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Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This thesis was submitted as part of the requirement for the degree of Doctor of Philosophy at The University of Western Australia February 2014 Australian Research Council Centre of Excellence in Plant Energy Biology School of Chemistry and Biochemistry

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Page 1: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

Characterising the response of rice and wheat coleoptiles to anoxia and

re-oxygenation

Rachel Shingaki-Wells

This thesis was submitted as part of the requirement for the degree of Doctor of Philosophy at The University of Western Australia

February 2014

Australian Research Council Centre of Excellence in Plant Energy Biology School of Chemistry and Biochemistry

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Declaration

The examination of this thesis is an examination of the work of Rachel

Shingaki-Wells. The work has been substantially conducted by Rachel

Shingaki-Wells during enrolment in the degree of Doctor of Philosophy at

The University of Western Australia.

This thesis contains published work and/or work prepared for publication,

some of which has been co- authored. The bibliographical details of the

work and where it appears in the thesis are outlined on the next page. A

description for each publication that clarifies the contribution of Rachel

Shingaki-Wells follows. Signed consent from each co-author are provided

at the back of this thesis.

Rachel Shingaki-Wells

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Publications

Thesis Chapter 1: Shingaki-Wells RN,, Millar AH, Whelan J, Narsai R (2013) What

happens to plant mitochondria under low oxygen? An omics review of the responses to low oxygen and re-oxygenation. Plant Cell and Environment. Reviewed and returned with minor corrections.

Chapter 2: Shingaki-Wells RN, Huang S, Taylor NL, Carroll AJ, Zhou W,

Millar AH (2011) Differential molecular responses of rice and wheat coleoptiles to anoxia reveal novel metabolic adaptations in amino acid metabolism for tissue tolerance. Plant Physiology 156:1706-24

Chapter 3: Shingaki-Wells RN, Huang S, Alexova R, Millar AH (2014) Wheat

genotype responses to anoxia are temperature and tissue dependent. Unpublished.

Chapter 4: Shingaki-Wells RN, Huang S, Millar AH (2014) Proteome and

metabolome responses in cereals subjected to short-term anoxia followed by re-oxygenation. Unpublished.

Additional Addendum: Shingaki-Wells RN, Huang S, Taylor NL, Millar AH (2011)

Pursuing the identification of O2 deprivation survival mechanisms in plants related to selective mRNA translation, hormone-independent cellular elongation and preparation for the arrival of oxygen. Plant Signaling and Behavior 6: 1612-5

Research: Huang S, Jacoby RP, Shingaki-Wells RN, Li L, Millar AH (2013)

Differential induction of mitochondrial photorespiratory machinery by light intensity is linked to changes in respiratory metabolism in rice leaves. New Phytologist 198: 103- 115

Review: Huang S, Shingaki-Wells RN, Taylor NL, Millar AH (2013) The rice

mitochondria proteome and its response during development and to the environment. Frontiers in Plant Proteomics 4:16-21

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Author contributions This thesis contains publications/manuscripts as outlined on page IV. The contributions of each co-author are as follows: Introduction 1. Shingaki-Wells RN: writing, figure preparation, editing. 2. Millar AH: writing, editing. 3. Whelan J: editing. 4. Narsai R: writing, figure preparation, editing. Study I 1. Shingaki-Wells RN: experimental work, data analysis, writing, figure

preparation, editing. 2. Huang S: lab guidance, experimental design, writing, editing. 3. Taylor NL: iTRAQ runs and analysis, editing. 4. Carroll AJ: Metabolite computational analysis, metabolite table preparation,

writing, editing. 5. Zhou W: Metabolite analysis. 6. Millar AH: concept, experimental design, writing, editing. Study II 1. Shingaki-Wells RN: experimental work, experimental design, data analysis,

writing, figure preparation. 2. Huang S: lab guidance, experimental design, writing, editing. 3. Alexova R: metabolite analysis guidance. 4. Millar AH: concept, experimental design, editing. Study III 1. Shingaki-Wells RN: experimental work, data analysis, writing, figure

preparation. 2. Huang S: lab guidance, experimental design, figure guidance, editing. 3. Millar AH: concept, experimental design, editing.

The consent of each co-author is provided on page 199 of this thesis.

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Acknowledgements I would like to take this opportunity to sincerely thank my supervisors Harvey

Millar and Shaobai Huang for their invaluable encouragement and advice. I

appreciate your patience and calming words when I made the silliest of mistakes.

Even though both of you had many more things on your plate than I ever did, I

thank you for always making time for me without hesitation.

Thanks to other members of Plant Energy Biology for your advice, assistance

and friendship: Owen Duncan, Holger Eubel, Julia Grassl, Cristian Holzmann,

Connie Hooper, Sandi Kerbler, Szymon Kubiswevski-Jakubiak, Simon Law, Alex

Lee, Lei Li, Josh Linn, Reena Narsai, Ellen Paynter, Yan Peng, Hafiz Che

Othman, Adriana Pruzinska, Jordan Radomiljac, Michelle Sew, Cory Solheim,

Elke Stroher, Yew-Foon Tan, Tiago Tomaz and Aaron Yap.

Thank you to DAFWA for the wheat seed donations. Special mention to Richard

Jacoby for facilitating seed collection and for your valuable advice over the years.

I would like to thank Wenxu Zhou for running my first samples on the GC-MS. I

am grateful to Adam Carroll for analysing my metabolite samples in the early

days and for explaining program-related details with me. Thanks to Nic Taylor for

his work on the iTRAQ experiments and helpful discussions over the years.

Thanks to Rali Alexova for always taking to time to listen and help. Thanks to

Clark Nelson for your helpful discussions on statistics. Thank you to Jenny Gillett,

Jude Moyle, Deb Yeoman, Allan McKinley, Hayden Walker, Rosie Farthing and

Geetha Shute for making administrative life pleasant and smooth. Thanks to Alice

Trend for all of your support, laughs, encouragement and science outreach

opportunities. Thanks to Ben Gully for your patience, presence and for getting

me through.

I am grateful to the Australian government and the GRDC (GRS183) for providing

me scholarships. Thank you to the Australian Research Council via the Centre of

Excellence in Plant Energy Biology for the positive environment and financial

support for this project. …

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Abbreviations

1,3-PGA 1,3-bisphosphoglycerate 2-PGA 2-phosphoglycerate 2D- PAGE two-dimensional polyacrylamide gel electrophoresis 3-PGA 3-phosphoglycerate 3-PGDH D-3-phosphoglycerate dehydrogenase ACC oxidase 1-aminocyclopropane carboxylic acid ACN acetonitrile ADH alcohol dehydrogenase AdoMet S-adenosylmethionine ADP adenosine diphosphate AK adenylate kinase AlaAT alanine aminotransferase ALDH aldehyde dehydrogenase AMP adenosine monophosphate AMPS ammonium persulfate ANOVA analysis of variance ANPs anaerobic proteins AOX alternative oxidase Apx ascorbate peroxidase Arabidopsis Arabidopsis thaliana ATE Arg-tRNA protein transferases

ATP adensosine triphosphate BAC basic amino acid carrier BBTI Bowman-Birk-type trypsin inhibitor CHAPS 3-[(3-Cholamidopropyl)dimethylammonio]-1-propanesulfonate CoA coenzyme A CHCA α-cyano-4-hydroxycinnamic acid Da dalton ddH2O double-distilled water DHAP dihydroxyacetone phosphate DHAP dihydroxyacetonephosphate DiGE differential in gel electrophoresis DNA deoxyribonucleic acid

DTT DL-dithiothreitol EDTA ethylenediaminetetraacetic acid ERF ethylene response factor ESI electrospray ionization ETC electron transport chain

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Fig. figure FK fructokinase Fru-1,6-B2 fructose-1,6-bisphosphate Fru-6-P fructose-6-phosphate

FW fresh weight

G-3-P glyceraldehyde-3-phosphate GABA gamma-aminobutyric acid GAPDH glyceraldehyde-3-phosphate dehydrogenase GC gas chromatography GlnSyn glutamine synthetase Glu-1-P glucose-1-phosphate Glu-6-P glucose-6-phosphate GSH reduced glutathione

GSSG oxidised glutathione H+-ATPase ATP hydrolysing proton pump H+-PPiase pyrophosphtase proton pump HK hexokinase HPLC high performance liquid chromatography HRE hypoxia responsive ERF (ethylene response factor) IAA indole-acetic acid IEF isoelectric focussing ILR1 indole-acetic acid amino acid hydrolase 1 iPGAM 2,3-bisphosphoglycerate-independent phosphoglycerate mutase kDa kilo Dalton Km Michaelis constant

LDH lactate dehydrogenase LEA late embryonogenesis abundant m/z mass to charge MALDI-TOF matrix assisted laser desorption time of flight MDH malate dehydrogenase MDHA monodehydroascorbic acid MES 2-(N-morpholino)ethanesulfonic acid MetSyn cobalamin-indepdendent methionine synthase MM molecular mass MOWSE molecular weight search mRNA messenger RNA

MS mass spectrometry mt mitochondrial n number of biological replicates n/s not significant

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NAD+ nicotinamide adenine dinucleotide (oxidized form) NADH nicotinamide adenine dinucleotide (reduced form) NDPK nucleotide diphosphate kinase NERP N-end rule pathway

NiR nitrite reductase NL non linear NO nitric oxide NR nitrate reductase NTP nucleotide triphosphate OAA oxaloacetate Os Oryza sativa (prefix for rice gene) PDC pyruvate decarboxylase PDH pyruvate dehydrogenase PDLP plasmodesmata-located protein PEP phosphoenolpyruvate PFK-ATP ATP-dependent phosphofructokinase PFK-PPi PPi-dependent phosphofructokinase PGI phosphoglucoseisomerase PGK phosphoglyceratekinase PGM phosphoglyceratemutase Pi inorganic phosphate pI isoelectric point PK pyruvate kinase PPDK pyruvate phosphate dikinase PPi pyrophosphate Prx peroxiredoxin PSAT phosphoserine aminotransferase Put putrescine rad reduced alcohol dehydrogenase activity mutant line RAP related to AP2 RNA ribonucleic acid ROS reactive oxygen species rpm rotations per minute S significant SDH succinate dehydrogenase SDS sodium dodecyl sulphate SHMT serine hydroxymethyltransferase Sig. significant SMM saturated matrix mix SOD superoxide dismutase

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SS sucrose synthase SSA succinic semialdehyde Sub1A-1 Submergence1-A allele SUS sucrose synthase gene TCA tricarboxylic acid TEMED tetramethylethylenediamine TES N-Tris(hydroxymethyl)methyl-2-aminoethanesulfonic acid TFA trifluoroacetic acid TGA transformed geometric mean TPI triosephosphate isomerase TPP thiamine pyrophosphate UDP uridine diphosphate UDP-Gluc-PPiase UDP-glucose pyrophosphorylase V-PPase vacuolar pyrophosphatase v/v volume to volume w/v weight to volume WT wild type x g times the force of gravity

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Abstract

Floods are estimated to affect 17 million km2 of land worldwide, threatening the

productivity of several major crops. A key consequence of this is the creation of a

physical barrier that causes oxygen deprivation in plants and thus inhibition of

aerobic respiration, the most efficient means of ATP production. As a result,

plants must rely on glycolysis, a less efficient means of ATP synthesis, in order to

survive. Crop anoxia tolerance is highly variable; on one end of the spectrum is

rice (Oryza sativa), which has been known to survive for weeks without oxygen,

showing exceptional abilities to germinate, develop a coleoptile and grow under

strict anoxia. In contrast, species such as wheat (Triticum aestivum), a dry-land

winter crop, can endure anoxia for only a short period of time, and fails to

germinate or grow when oxygen deprived.

While biochemical comparisons between rice and wheat responses to anoxia

exist, little information was available at the proteomic and metabolomic level.

Furthermore, research on the consequences of re-oxygenation, an inevitable

event for plant survival, is scarcely described. Thus, the research presented in

this thesis aimed to characterise the molecular responses of rice and wheat

coleoptiles to anoxia and re-oxygenation.

In Study I, rice (cv. Amaroo) and wheat (cv. Calingiri) coleoptile responses to

anoxia were compared at the physiological, proteome and metabolome level.

This analysis revealed a large proteomic response to anoxia in rice, which

contrasted to that of wheat. For example, rice showed large increases in proteins

involved in glycolysis, a response likely to improve ATP production under

anaerobic conditions. In general, amino acids rapidly accumulated in anoxic rice,

but not in wheat. Most surprisingly, wheat failed to accumulate alanine, a

standard plant response to anoxia. Supplementation of key amino acids,

including alanine, appeared to reduce electrolyte leakage in anoxic wheat. This

result was not apparent in rice.

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Study II took a multi-genotype approach to understanding wheat responses to

anoxia. Four genotypes with purported variation in anoxia tolerance were

compared to the original genotype of interest, Calingiri. Growth recovery, alcohol

dehydrogenase induction, electrolyte leakage and metabolomes were compared

between the five genotypes. Temperature and tissue variations revealed the

sensitive dependence that anoxic responses have on these factors. Thus, the

reported inconsistencies relating to the anoxia tolerance of certain wheat

genotypes appears to be strongly linked with experimental differences.

In Study III, the responses of rice and wheat (cv. Calingiri) to re-oxygenation were

examined. Proteins involved in cell wall re-modelling, oxidative stress and

fermentation were shown to change under these stresses. The large amino acid

accumulation observed in rice was rapidly reversed upon re-oxygenation. This

was not the case in wheat.

Overall, these studies show the highly variable responses that these species

exhibit during anoxia and re-oxygenation. In contrast to wheat, the ability of rice

to tolerate anoxia appears to be linked with its rapid response to this stress.

Amino acid metabolism appears to play an important, but as yet poorly defined

role in both anoxia and re-oxygenation. While wheat is generally anoxia

intolerant, inter-genotype responses to anoxia are variable, and highly dependent

on the tissue and temperature.

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Contents

Declaration........................................................................................ II Publications....................................................................................... III Author contributions......................................................................... IV Acknowledgements.......................................................................... V Abbreviations.................................................................................... VI Abstract ............................................................................................ X Contents............................................................................................ XII Chapter 1: Introduction..................................................................... 1 Foreword to literature review............................................................... 2 Literature review.................................................................................. 4 Chapter 2: Rice and wheat responses to anoxia............................ 49 Foreword to Study I............................................................................ 50 Study I................................................................................................ 51 Supplemental data for Study I............................................................. 70 Chapter 3: Wheat genotype responses to anoxia 75 Foreword to Study II........................................................................... 76 Study II............................................................................................... 77 Figures………………………............................................................... 106 Tables................................................................................................. 114 Supplemental data for Study II............................................................ 117 Chapter 4: Rice and wheat responses to re-oxygenation.............. 136 Foreword to Study III........................................................................... 137 Study IIII.............................................................................................. 138 Figures………………………............................................................... 166 Supplemental data for Study III........................................................... 186 Chapter 5: General Discussion....................................................... 191 Co-author consent........................................................................... 199

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Chapter 1 Introduction

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Foreword to literature review The following literature review has been submitted as an invited review of

the ‘omics’ literature that relates to how plants respond to anoxia as well

as re-oxygenation (Shingaki-Wells et al., 2014). This review contains

information reported in the first results chapter, which is published

research (Shingaki-Wells et al., 2011).

Plants that are flooded can be rapidly deprived of oxygen, resulting in

hypoxia or anoxia. The purpose of this project is to determine how two

cereals, Oryza sativa (rice) and Triticum aestivum (wheat), respond to low

oxygen at the physiological and molecular level. Since rice is typically a

flood-tolerant crop, and wheat a flood-intolerant crop, it was suspected

that the molecular responses of these species would be highly divergent.

Rice is especially interesting in that it can germinate under anoxia, a

feature that is absent in wheat. The growth of rice when germinated under

anoxia is aberrant however, with the coleoptile as the only tissue to

develop in young seedlings. This tissue has therefore been the subject of

much research, since it is an example of a tissue with exceptional anoxia

tolerance.

For plants to survive a low-oxygen event, they must also endure the

added consequences that come with re-oxygenation. Typically, oxidative

stress becomes a factor, and plants must appropriately deal with the

molecular damage that ensues.

This project explored three major questions:

A. How do rice and wheat coleoptiles respond to short-term anoxia at

the physiological, proteomic and metabolomic level? Do these

differences underlie the contrasting tolerance of these species to

anoxia?

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B. How great is the variation in anoxia tolerance between different

wheat genotypes? How do other environmental factors affect

anoxia tolerance?

C. How do rice and wheat respond to re-oxygenation after short-term

anoxia? Do the differences seen between these species, in terms

of their response to anoxia, affect metabolism post-anoxia?

Point A, B and C are discussed in Chapters 2, 3 and 4, respectively. They

are formatted as published, or as manuscripts to be submitted to a

scientific journal. The last section of this thesis, Chapter 5, will draw

general conclusions about this project.

References

Shingaki-Wells RN, Huang S, Taylor NL, Carroll AJ, Zhou W, Millar AH (2011) Differential molecular responses of rice and wheat coleoptiles to anoxia reveal novel metabolic adaptations in amino acid metabolism for tissue tolerance. Plant Physiology 1156: 1706-1724

Shingaki-Wells RN, Millar AH, Whelan J, Narsai R (2014) What happens to plants under low oxygen? An omics review of the responses to low oxygen and re-oxygenation. Plant, Cell & Environment Submitted.

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What happens to plants under low oxygen? An omics

review of the responses to low oxygen and re-

oxygenation

Rachel Shingaki-Wells1, A. Harvey Millar1, James Whelan1,2, Reena Narsai1,3

1ARC Centre of Excellence in Plant Energy Biology, MCS Building M316

University of Western Australia, 35 Stirling Highway, Crawley 6009, Western

Australia, Australia. 2Department of Botany, School of Life Science, La Trobe

University, Bundoora, Victoria 3086, Australia. 3Centre for Computational

Systems Biology, MCS Building M316 University of Western Australia, 35

Stirling Highway, Crawley 6009, Western Australia, Australia.

Abstract

Floods can rapidly submerge plants, limiting oxygen to the extent that oxidative

phosphorylation no longer generates adequate ATP supplies. Low oxygen

tolerant plants, such as rice, are able to adequately respond to low oxygen by

successfully re-modelling primary and mitochondrial metabolism to partially

counteract the energy crisis that ensues. In this review, we discuss how plants

respond to low oxygen stress at the transcriptomic, proteomic, metabolomic

and enzyme activity level, particularly focussing on mitochondria and interacting

pathways. The role of reactive oxygen species and nitrite as an alternative

electron acceptor as well as their links to respiratory chain components is

discussed. By making intra-kingdom as well as cross-kingdom comparisons,

conserved mechanisms of anoxia tolerance are highlighted as well as tolerance

mechanisms that are specific to anoxia-tolerant rice. We discuss re-

oxygenation as an often overlooked, yet essential stage of this environmental

stress and consider the possibility that changes occurring during low oxygen

may also provide benefits upon re-aeration. Finally, we consider what it takes to

be low-oxygen tolerant and argue that alternative mechanisms of ATP

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production, glucose signalling as well as reverse-metabolism of fermentation

end-products promote the survival of rice after this debilitating stress.

Introduction

Flooding events deprive plants of oxygen, posing a considerable threat to crop

productivity. The volume of research that focuses its attention on the molecular

consequences of hypoxia or anoxia is both vast and diverse. At the centre of

such study lies a commonality; plants that are deprived of oxygen need to rely

on anaerobic metabolism to maintain adequate ATP production. Different

plants can have significantly different levels of tolerance to low oxygen, with

some plants able to tolerate only hours, while others, such as rice, can even

survive weeks under flooding conditions. As a result, it is not surprising that

different survival tactics have evolved, with some plants adopting rapid-growth

avoidance strategies and others only involving significant metabolic shifts to

ensure survival (Voesenek et al., 2006; Salavati et al., 2012).

Whether in plants or animals, it can be seen that many molecular responses to

low oxygen are conserved, including the induction of fermentation and

glycolysis (Mustroph et al., 2010). Several studies in recent years have even

shown how altering components directly or indirectly involved in these

pathways alters low oxygen tolerance. For example in the last decade, studies

have shown a role for group VII ethylene responsive factors, namely

RAP2.12/RAP2.2, HRE1/HRE2, SNORKEL1/2 and SUB1A-1, in regulating

sugar metabolism, fermentation and/or growth in plants under low oxygen

conditions (Xu et al., 2006; Hattori et al., 2009; Hinz et al., 2010; Licausi et al.,

2010). Furthermore, substantial evidence towards important roles for nitric

oxide (NO) and reactive oxygen species (ROS) signalling have also been

presented in the last decade (Igamberdiev et al., 2010; Gupta and Igamberdiev,

2011) with studies revealing an important role of the mitochondrial respiratory

components facilitating this signalling (Blokhina and Fagerstedt, 2010).

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Given that the genes encoding the mitochondrial respiratory components are

largely conserved across different plants, with the known exception of complex

II in rice (Huang et al., 2010), it is probable that it is not the presence of unique

genes in tolerant species that facilitates survival. Instead, it is more likely that

specific regulation at the transcriptomic, proteomic and metabolomic levels

occurs in low-oxygen tolerant species, which allows sufficient continuation of

respiratory metabolism and ATP production. Additionally, unlike mammals,

plants contain chloroplasts, which also produce energy, facilitating low-oxygen

tolerance. For example, it has been shown that light exposure reduces the

need for fermentation and extends survival during anaerobiosis in rice and

wheat seedlings (Mustroph et al., 2006). Hence, a common thread that

underlies the degree of low-oxygen tolerance in plants is the ability to

successfully shift metabolism in favour of energy production under these

conditions.

It is important to note that while different plant species show significant

variation in their level of tolerance to low-oxygen stress, many plant species can

survive a short period, as may occur during brief water-logging periods.

Adapting to post-anoxic stress is integral to surviving a flood event, yet this

stage is rarely considered. The few studies that have examined this stage

reveal rapid changes in transcript and metabolite abundances, shifting

metabolism back towards aerobic respiration and increased energy production

(Branco-Price et al., 2008; Narsai et al., 2009). Thus, when studying anoxia it is

useful to consider that changes made under low oxygen are not only relevant

for anoxic survival but can also be essential for the survival success of plants

upon return to aerobic conditions. In mammals for example, studies looking at

hypoxia responses in the human heart not only examine the ischemic episode,

leading to the reduced oxygen supply, but also examine the substantial

damage invoked during rapid re-oxygenation (Schaub et al., 2009). Similarly,

for flood-prone farmland to remain economically productive, crop plants must

be able to maintain seed production when floodwaters recede. The question is

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how or even whether plants prepare for this second round of stress, which

often includes a ROS challenge as well as dehydration (Fukao et al., 2011).

In this review, we will take a systems biology approach to discuss the

responses of plants to low oxygen, from organelle morphology to the molecular

response, with a focus on central and mitochondrial metabolism at the

transcript and protein levels, to help answer the question: What happens to

mitochondria under low oxygen conditions? Specifically, we discuss the

interactions of ROS and NO signalling with the mitochondrial respiratory

pathways and reveal differences between low-oxygen tolerant and non-tolerant

plant species. We also discuss the effects of re-oxygenation on plants and

distinguish between the different ways recovery has been examined, i.e.

oxygenation shock and re-oxygenation. Metabolic trends of recovery in

different plant species are also highlighted, and compared across kingdoms.

DNA, RNA and proteins under low oxygen

Before even considering in depth the significant mitochondrial and metabolic

changes known to occur under low oxygen in different species (Gibbs and

Greenway, 2003; Greenway and Gibbs, 2003; Magneschi and Perata, 2009;

Narsai et al., 2011; Narsai and Whelan, 2013), one of the most obvious

differences between low-oxygen tolerant and intolerant species is the ability to

survive and therefore sustain the machinery to carry out DNA replication,

transcription and protein synthesis under low oxygen. Without at least some

function of these, low oxygen survival would not be possible.

The DNA level

Under low oxygen, ATP synthesis is substantially lower than in aerobic

conditions in rice (Mustroph and Albrecht, 2003). However, it has been

proposed that energy “budgeting” occurs under low oxygen in rice, dedicating

specific amounts of ATP to different cellular functions (Edwards et al., 2012).

When the rates of DNA synthesis and energy expenses related to this were

measured under hypoxia and anoxia in rice, it was observed that DNA

synthesis still occurred, but at half the rate of that occurring under normoxia

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(Edwards et al., 2012). This is further supported by the continued, but slower,

rate of cell division and elongation that occurs under low oxygen in rice

(Takahashi et al., 2011). This is in contrast to intolerant species where these

mechanisms are not able to be sustained.

The RNA level - transcription under low oxygen

Due to the ‘energy crisis’ that occurs when oxygen is limited (Huang et al.,

2008), it is plausible that energy usage for regulating relatively large numbers of

transcripts could be restricted. However, in anoxia-tolerant rice or even anoxia-

intolerant species such as Arabidopsis, transcriptional processes do not

appear to be limited (Narsai and Whelan, 2013). In fact, the transcriptomic

responses to low oxygen are within the range of other abiotic stress responses,

with thousands of genes showing differential expression (Lasanthi-Kudahettige

et al., 2007; Branco-Price et al., 2008; Narsai et al., 2009; Narsai and Whelan,

2013). Selective polysome loading is a factor that regulates low oxygen gene

expression (Branco-Price et al., 2008). For example, hypoxic stress in

Arabidopsis resulted in a reduction of polysome content by approximately

50 %, a decrease that was almost entirely reversed upon re-oxygenation

(Branco-Price et al., 2008). Additionally, it is clear that regulation at the

transcript level is extremely crucial under low oxygen, with many ethylene-

responsive transcription factors (ERFs) showing important function under

hypoxia (Bailey-Serres et al., 2012). The critical role of the gaseous hormone

ethylene in low oxygen signalling was first implied based on the observed

increase in its levels under low oxygen (reviewed in (Voesenek and Sasidharan,

2013)). The synthesis of ethylene requires oxygen at the level of ACC oxidase

(Kende, 1993). However, achieving anoxia requires a transition through

hypoxia, meaning functional ethylene concentrations may exist even in anoxic

cells. Among the most well-known ERFs is the group VII ERF, which is thought

to be involved in regulating the expression of genes encoding enzymes involved

in carbohydrate consumption, ethanolic fermentation and cell expansion in

anoxia-tolerant rice (Fukao et al., 2006). Ethylene signalling and the role of

group VII ERFs under low oxygen also appears to be conserved in several

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species, with studies in the last couple of years demonstrating their role in

affecting the low-oxygen tolerance in the anoxia-intolerant Arabidopsis thaliana

(Arabidopsis).

The protein level - protein synthesis under low oxygen

Protein synthesis is energetically costly, especially in light of the reduced

capability of plants to produce ATP when oxygen is unavailable (Mustroph and

Albrecht, 2003). Expending energy on protein synthesis should therefore be an

investment with considerable return. Interestingly, the decreased rates of

protein synthesis observed in anoxic rice coleoptiles is less than the decrease

in calculated ATP synthesis rates (Edwards et al., 2012). In fact, the proportion

of ATP used for protein synthesis was highest in anoxic coleoptiles (52%),

followed by normoxic and hypoxic coleoptiles at 19% and 14%, respectively

(Edwards et al., 2012). This suggests the importance of a responsive - or at

least maintained - proteome during adaptation to anoxia. A high-return

investment could include catabolic proteins that increase glycolytic ATP

production, contributing to the observed Pasteur effect during anoxia (Gibbs

and Greenway, 2003). This is also supported by the significant changes in the

proteomes observed under anoxia, including the increased protein abundance

observed for a number of glycolysis and fermentation-associated proteins

(Millar et al., 2004; Howell et al., 2007; Shingaki-Wells et al., 2011). Thus,

despite decreases in the rates of ATP, DNA and protein synthesis (Mustroph

and Albrecht, 2003; Edwards et al., 2012) continued function of these is what

facilitates survival under low oxygen.

Mitochondrial morphology under low oxygen

Survival under low-oxygen conditions is directly linked with the ability to

produce energy (ATP) under these circumstances. The double membrane

structure of mitochondria contains the crucial components of the respiratory

pathway and facilitates the required membrane potential for effective energy

production. Some of the earliest studies examining mitochondria under

anaerobic conditions have been performed in yeast (Nagata et al., 1975). It was

revealed that under anaerobic conditions, there are a significantly smaller

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number of mitochondria present and these also show differences in their

ultrastructure compared with mitochondria in aerobically grown yeast (Nagata

et al., 1975). Specifically, it was seen that under anaerobic conditions,

mitochondria fail to develop cristae (Figure 1) (Nagata et al., 1975). Similarly,

studies in human cells have also revealed that under hypoxia, significant

changes in mitochondrial shape and ultrastructure occur (Figure 1). When

H9C2 cells were examined during hypoxia under glucose-free conditions, it

was seen that mitochondria swell and become donut-shaped (toroidal) (Figure

1) (Liu and Hajnoczky, 2011). This was also seen upon re-oxygenation in the

presence of glucose (Liu and Hajnoczky, 2011). It is thought that this occurs in

order to better tolerate matrix volume increases and produce mitochondria that

can regain mitochondrial membrane potential (Liu and Hajnoczky, 2011). In

addition to these, a recent study in protists, looking at the mitochondrial

structure of hypoxically-grown choanoflagellates also revealed several

peculiarities under these conditions, including mitochondria showing tubular

cristae, which has never been seen before in choanoflagellates (Figure 1)

(Wylezich et al., 2012).

Ultrastructure under continuous anoxia and in transition to or from

anoxia

In plants, low oxygen studies have involved different experimental designs to

reflect the circumstances faced specifically by plants. Early studies examining

semi-aquatic plants under anoxia revealed mitochondrial degeneration and

developmental failure in the absence of oxygen (Ueda and Tsuji, 1971;

Vartapetian et al., 1976; Oliveira, 1977; Fox and Kennedy, 1991). However,

plants can often undergo brief periods of anaerobic conditions, such as those

that may occur during a brief flood. One study examined 4-day old (anoxia

intolerant) wheat seedlings that were subjected to 90 min of anoxia, before

mitochondrial ultrastructure was examined in the coleoptiles (Vartapetian et al.,

1985). Mitochondrial deterioration was revealed under these conditions, in that

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Figure 1. Mitochondrial morphology under anoxia.

Structural changes under low-oxygen in yeast (Saccharomyces cerevisiae –

JYD 56-G strain), human (Homo sapiens – H9C2 cells), protists (Codosiga

balthica n. sp. strain IOW94), plants; anoxia tolerant (tol) barnyard grass

(Echinochloa phyllopogon) and rice (Oryza sativa) as well as anoxia intolerant

wheat (Triticum aestivum) are shown.

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the matrix appeared less dense and cristae, less dilated (Figure 1) (Vartapetian

et al., 1985). Interestingly, the damage was seen to be reversed upon transfer

back to aerated conditions provided the duration of anoxia was relatively small

(Vartapetian et al., 1985). Such flexibility would be advantageous if stress

conditions are transient in nature. Mitochondrial ultrastructure has been linked

to supercomplex formation in the electron transport chain (Dudkina et al.,

2006). The relevance of this to low oxygen is currently unknown, but it is

certainly interesting that ATP synthase dimerization and subsequent

oligermerisation is hypothesised to contribute to cristae formation and

mitochondrial morphology (Dudkina et al., 2006). Whether or not ATP synthase

interactions are responsible for these changes in mitochondrial ultrastructure

under low oxygen is yet to be investigated.

For some plant species, the anaerobic conditions offered by their habitat can

last for extended periods of time and these species have evolved mechanisms

that allow mitochondrial survival even under these conditions. When anoxia-

tolerant plant species including Echinochloa phyllopogon and Echinochloa

crus-galli (barnyard grasses) were examined, it was seen that mitochondrial

size, shape and ultrastructure remained unchanged even under anaerobic

conditions (Kennedy et al., 1980). Similarly, embryos of anoxia-tolerant rice

develop mature mitochondria from promitochondria under both aerobic or

anaerobic conditions (Howell et al., 2007), which further supported the relatively

high level of conservation seen in the transcriptomic responses during both

aerobic and anaerobic germination in rice (Narsai et al., 2009; Narsai and

Whelan, 2013). However, this type of maintenance of mitochondrial structure or

ultrastructure is not consistent throughout rice development or in all anoxia-

tolerant plant species. For example, there does appear to be tissue-specific

differences in mitochondrial morphology under anoxia at the later stages of rice

development.

Specifically, in anaerobic-tolerant rice shoots, anaerobic mitochondria have less

dense matrices but more cristae (Figure 1) (Couee et al., 1992). It has also

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been shown that excised rice coleoptiles (that no longer receive the

endosperm’s sugar supply) are more sensitive to anoxia, with abnormal

mitochondria observed after 1 day of anoxia, and after 2 days rupturing can

occur (Vartapetian et al., 1976). This effect was lost when glucose was

externally supplied, suggesting that mitochondria are sensitive to low oxygen in

a sugar-dependent manner. It is well known that starch mobilisation occurs via

alpha-amylase induction in anoxic rice and that this response is somewhat

unique to anaerobic tolerance (Guglielminetti et al., 1995; Guglielminetti et al.,

1995), whereby this response is absent in anoxic wheat, which fails to

germinate under anoxia. Thus it appears that metabolic adaptation, rather than

quiescence, is important for the upkeep of anoxic mitochondria in these rice

coleoptiles. Nitrite supplementation under low oxygen also appears to benefit

rice in that mitochondria show increased ATP synthesis (Stoimenova et al.,

2007), a phenomenon discussed in greater detail below. Rice seedlings

germinated and grown under anoxia appear to retain mitochondrial function in

coleoptiles, as these consume oxygen rapidly upon the transfer to aerated

conditions, albeit less efficiently compared to aerated controls (Millar et al.,

2004; Shingaki-Wells et al., 2011). Again, respiratory capacity is restored after

just 1 day of re-oxygenation following 6 days of anoxia (Millar et al., 2004).

Responses to low oxygen

Responses to low oxygen are being increasingly characterised, with

technological advances improving quality and quantity of data from DNA and

RNA to protein and metabolite analysis. It is the combined regulation and

control at each of these levels, which contributes to differences in low oxygen

survival across different plant species. Figure 2 visualises the known molecular

responses, to date, summarising the systems-level responses to low oxygen in

anaerobic tolerant rice, focussing on mitochondrial functions and interacting

pathways. The responses in Figure 2 reflect findings from previous

transcriptomic studies (Lasanthi-Kudahettige et al., 2007; Narsai et al., 2009;

Mustroph et al., 2010; Narsai and Whelan, 2013), proteomic studies (Millar et

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+

+

+

+

+

--

+ -

+

+

-

-

+

Figure 2. The rice mitochondrial system under anoxia. Full caption follows on the next page.

14

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Figure 2. The rice mitochondrial system under anoxia. Schematic

diagram visualising transcriptomic, proteomic, metabolomic and enzymatic

activities known to date (to our knowledge, through a systematic pubmed

search), and coloured based on their response to anoxia in rice. Note that for

some pathways shown, not all components and their responses have been

experimentally verified in terms of sub-cellular location or function under anoxia

(in black font). Figure on the previous page.

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al., 2004; Huang et al., 2005; Howell et al., 2007; Sadiq et al., 2011; Shingaki-

Wells et al., 2011), metabolite studies (Mustroph et al., 2006; Narsai et al.,

2009; Shingaki-Wells et al., 2011) and enzyme activity studies (Fox and

Kennedy, 1991; Couee et al., 1992; Mujer et al., 1993; Carystinos et al., 1995;

Gibbs et al., 2000; Mustroph and Albrecht, 2003).

Fermentation

One of the earliest and most well-characterised responses to low oxygen is the

up-regulation of fermentation pathways as well as changes to the glycolytic

pathway, which were first observed in anaerobically grown yeast (Barnett,

2003). Cross-kingdom analysis reveals that not only are these pathways

conserved across different species, but that there are several commonalities in

their responses to low oxygen. In yeast as well as both tolerant and intolerant

plant species, an increase in alcohol dehydrogenase activity and subsequent

ethanol accumulation is observed (Waters et al., 1991; Guglielminetti et al.,

2001; Barnett, 2003; Branco-Price et al., 2008; Shingaki-Wells et al., 2011). In

the anoxia-intolerant species, Arabidopsis, alcohol dehydrogenase (ADH) is

significantly up-regulated at the transcript level in response to low oxygen

(Branco-Price et al., 2008; Narsai et al., 2011). In contrast, several genes

encoding alcohol dehydrogenase are down-regulated in rice, with the

exception of LOC_Os11g10510.1, which is induced in response to low oxygen

(Lasanthi-Kudahettige et al., 2007; Narsai et al., 2009) and shows significantly

higher expression during submergence in the SUB1A-containing cultivar

(M202(Sub1)) compared to the submergence-intolerant japonica M202 line

(Fukao et al., 2006; Mustroph et al., 2010). SUB1A has been shown to

regulate genes encoding enzymes involved in carbohydrate metabolism (Fukao

et al., 2006).

The comparison of tolerant and intolerant plant species does reveal strong

inter-species conservation in the up-regulation of pyruvate decarboxylase

(PDC) under low oxygen at the transcript level (Mustroph et al., 2010; Narsai

and Whelan, 2013). This is further supported by the finding that while over-

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expression of ADH1 does not increase flood tolerance in Arabidopsis, the over-

expression of PDC1 and PDC2 does increase survival, supporting a more

active role for PDC in flood tolerance or supporting the notion that PDC activity

is the limiting factor for ethanol production (Ismond et al., 2003). In rice, it can

be seen that PDC is induced, at both the transcript and protein levels (Figure 2)

(Neljubov, 1901; Mustroph et al., 2010; Sadiq et al., 2011; Shingaki-Wells et

al., 2011; Narsai and Whelan, 2013). Interestingly, PDC is also expressed at

significantly higher levels in the SUB1A anoxia-tolerant rice line compared to

the intolerant M2O2 line (Mustroph et al., 2010). In terms of enzyme activity, it

has also been shown that ATP-dependent phosphofructokinase (PFK),

pyrophosphate-dependent phosphofructokinase (PFP), PDC, and ADH are all

increased in response to anoxia in rice coleoptiles (Figure 2) (Gibbs et al.,

2000). However, given that many of these inductions are conserved in both

tolerant and intolerant species, the up-regulation of fermentation alone cannot

confer tolerance.

Glycolysis

Across low oxygen studies in different species, it has been observed how the

presence of an energy source affects the low oxygen response (Nagata et al.,

1975; Liu and Hajnoczky, 2011). In plants specifically, it has even been shown

that anoxic survival is improved upon exposure to light (Mustroph et al., 2006).

Despite lower levels of ATP under anaerobic compared to aerobic conditions,

overall, it was shown that ATP levels were more stably maintained during

anaerobiosis in the light compared to the dark in both rice and wheat

seedlings, and light also had the effect of reducing the rate of fermentation in

these plants (Mustroph and Albrecht, 2003; Mustroph et al., 2006). The

combined effect of light inducing photosynthesis as a source of ATP and as a

localised source of oxygen to fuel respiration is likely to underlie these changes.

Nevertheless, survival was better in rice compared to the anaerobic intolerant

wheat. Thus, maintaining the rates of energy production and flux, via regulated

changes to the glycolytic and fermentation pathways is crucial for anaerobic

tolerance.

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In rice, it is well known that energy stores, such as those in the form of starch

allow increased anoxia survival as rice maintains a functioning starch

metabolism, via active alpha-amylase induction and function under low oxygen

conditions (Figure 2) (Guglielminetti et al., 1995; Guglielminetti et al., 1995). It

has been shown that many genes encoding proteins involved in starch

metabolism and glycolysis are induced in rice, with sucrose synthase, aldolase,

triosephosphate isomerase and pyruvate phosphate dikinase (PPDK) also

significantly induced at the protein level (Figure 2) (Ricard et al., 1991; Lasanthi-

Kudahettige et al., 2007; Narsai et al., 2009; Shingaki-Wells et al., 2011). In

anaerobic tolerant species like rice, it has been observed that a pyrophosphate

(PPi)-dependent step in glycolysis is induced under low oxygen conditions

(Huang et al., 2005; Huang et al., 2008). Many PPi-utilising enzymes use PPi

bound to Mg2+, rather than free PPi (Horder, 1974). With decreasing ATP under

low oxygen, Mg2+ concentrations rise through liberation from ATP, and this

increases the activity of PPi-dependent enzymes, whose abundances are also

elevated under low oxygen (Horder, 1974; Lasanthi-Kudahettige et al., 2007;

Igamberdiev and Kleczkowski, 2011). PPDK and pyruvate kinase (PK) reactions

may work in a cyclical manner, with PK working in the direction of pyruvate

formation and PPDK working in the direction of pyruvate consumption

(Igamberdiev and Kleczkowski, 2011). Operation of this cycle would result in

PPi production, aiding conservation of ATP via the use of PPi-dependent

glycolytic reactions involving PPi-phosphofructokinase (PFK) and UDP-glucose

pyrophosphorylase as opposed to those that are ATP dependent (Igamberdiev

and Kleczkowski, 2011).

Thus, the induction of PPDK and increased activity of pyrophosphate-

dependent phosphofructokinase (PFK-PPi) is seen under anoxia in rice (Figure

2). Additionally, it is thought that the tonoplast H+-PPiase consumes PPi under

anaerobic conditions, as part of the “switch” to PPi as an alternate to ATP, and

that this activity contributes to cytosolic pH regulation (Huang et al., 2008). This

is also supported by the significant transcript induction of this gene (Lasanthi-

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Kudahettige et al., 2007) and increased enzymatic activity (Carystinos et al.,

1995) observed under anoxia (Figure 2).

While many other genes encoding glycolytic enzymes are induced under anoxia

in rice, phosphoglycerate mutase, enolase and lactate dehydrogenase are not

induced at the transcript level (Figure 2). Interestingly, despite this,

phosphoglycerate mutase and enolase protein abundance increases under

anoxia (Shingaki-Wells et al., 2011) and lactate dehydrogenase activity is also

known to slightly increase under anoxia (Mustroph and Albrecht, 2003). This

suggests that regulation occurs at the post-transcriptional, post-translational

and enzymatic activity level during anoxia (Figure 2). It is likely that transcript,

protein and enzymatic activity induction (Figure 2) contribute to the 1.4-1.7 fold

faster rate of glycolysis (“Pasteur effect”) seen under anoxia in rice, compared

to under aerobic conditions (Gibbs et al., 2000). It is important to point out here

that many of these enzymes were also activated under low oxygen in anoxia-

intolerant species, such as maize and wheat. However, sucrose accumulation

still occurred and viability was lost, an observation likely to be caused by the

lack of a functional alpha-amylase under anoxia (Perata et al., 1992; Mustroph

and Albrecht, 2003). Similarly, whilst many of these glycolytic enzymes are also

induced at the transcript level in anoxia-intolerant Arabidopsis (Narsai et al.,

2011), this alone, clearly does not lead to survival under anoxia.

Mitochondrial responses

Towards the end of the glycolytic pathways, pyruvate and acetaldehyde are

produced and can be imported into the mitochondria, for use as substrates in

the Tricarboxylic acid (TCA) cycle. It has been observed that the response to

low oxygen involves changes at the mRNA, protein, and enzyme activity levels

for these components, with several studies reporting significant changes under

anoxia (Couee et al., 1992; Howell et al., 2007; Narsai et al., 2011), and this

facilitates oxidation of these products during re-aeration (Tsuji et al., 2003).

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The TCA cycle

At the transcript level, studies have shown that there are several common

expression responses to low oxygen in different plant species for genes

encoding components of the TCA cycle (Mustroph et al., 2010; Narsai et al.,

2011). Overall, transcripts encoding several TCA cycle enzymes are down-

regulated in response to anoxia, in poplar, rice and Arabidopsis (Narsai et al.,

2011). Upon entry into the mitochondria, pyruvate can be metabolised by

pyruvate dehydrogenase to form acetyl CoA (Figure 2). Under anoxia, pyruvate

dehydrogenase and malate dehydrogenase are down-regulated both at the

transcript and protein levels in coleoptiles from rice seedlings germinated and

grown under anoxia, relative to aeration (Figure 2) (Millar et al., 2004; Howell et

al., 2007; Lasanthi-Kudahettige et al., 2007; Narsai et al., 2009; Shingaki-Wells

et al., 2011). This is not surprising, given that other TCA cycle enzymes and

their corresponding metabolites decrease in abundance under anoxia in rice

(Figure 2). Among these is the TCA cycle enzyme 2-oxoglutarate

dehydrogenase, which can metabolise 2-oxoglutarate to form succinyl-CoA

through reduction of NAD+. The well-recognized accumulation of alanine under

low oxygen (Narsai et al., 2011) when catalysed by alanine aminotransferase

can also result in the co-production of 2-oxoglutarate, providing substrate for

2-oxoglutarate dehydrogenase (Rocha et al., 2010). Rocha and colleagues

(2010a) propose that 2-oxoglutarate can be converted to Succinyl CoA, which

can be further metabolised to generate ATP and succinate. The NAD+ required

for 2-oxoglutarate production could be provided by via malate dehydrogenase

activity in reverse direction (Rocha et al., 2010). However, malate

dehydrogenase protein levels are significantly reduced in anoxic rice coleoptiles

relative to aeration (Shingaki-Wells et al., 2011). In Lotus japonicus, malate

dehydrogenase activity in the OAA-utilising direction during waterlogging is

about a third of that in control conditions, which could be a limiting factor in

sustaining the 2-oxoglutarate dehydrogenase reaction (Rocha et al., 2010).

This does not necessarily rule out the mechanism proposed by Rocha and

colleagues, but could suggest a lower level of malate dehydrogenase activity

during waterlogging, or higher level of ethanolic fermentation, is sufficient to

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sustain these reactions. Overall, the TCA cycle, from the lowered fumarase

activity (Couee et al., 1992) to the lowered succinyl CoA ligase protein

abundance (Howell et al., 2007) is repressed under anoxia in rice (Figure 2).

However, not all components of the TCA cycle are repressed under anoxia.

Barnyard grass seedlings (Echinochloa phyllopogon (Stapf.) Koss), are an

extremely successful anoxia-tolerant weed of cultivated rice, having anaerobic

mitochondria that outperform those of rice in that TCA cycle enzyme activities

approached their maxima earlier and remain higher for longer during anaerobic

germination, characteristics that also correlate with the unaffected

mitochondrial ultrastructure under anoxia (Figure 1) and the weed-like ability of

Echinochloa to germinate more rapidly under anoxia (Fox and Kennedy, 1991).

Exposure of both rice and Echinochloa to anoxia resulted in most TCA cycle

enzyme activities approaching those of air (Fox and Kennedy, 1991). However,

interestingly, the activity of fumarate reductase, which converts fumarate to

succinate, is almost negligible in aerobic and anaerobic Echinochloa compared

to the 20-fold higher activity found in rice (Figure 2) (Fox and Kennedy, 1991).

As the substrate of complex II in the mETC, succinate probably accumulates

when the ubiquinone pool is saturated with electrons due to the absence of the

terminal electron acceptor O2 (Rocha et al., 2010) and despite being lower,

succinate dehydrogenase activity is present in anoxic rice shoots (Couee et al.,

1992). Thus, as well as being a product of ETC blockage, this increased

fumarate reductase activity may also help to explain why anoxic succinate

accumulation in rice is so rapid (Shingaki-Wells et al., 2011). The accumulation

of succinate is a known response to anoxia in rice (Menegus et al., 1989;

Narsai et al., 2009; Shingaki-Wells et al., 2011). In rice, succinate accumulates

3.5 fold in rice coleoptiles after just one day of anoxia (Shingaki-Wells et al.,

2011). Similarly, fumarate significantly increased during anoxic germination,

with higher levels observed from as early as just 3 h of imbibition to 2-d

germinated seeds (Figure 2) (Narsai et al., 2009). Interestingly, fumarate did not

increase in abundance after 1 d anoxia in coleoptiles (Shingaki-Wells et al.,

2011), suggesting that this response may only occur in the early anoxic growth

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stages. Using 14C labelling, it has been demonstrated that succinate is

metabolised under anoxia (Rumpho and Kennedy, 1983). The exact pathway(s)

responsible for anoxic succinate accumulation is as yet unclear, but it has been

suggested that GABA shunt is partially responsible. A clearer answer on the

mechanism of anoxic succinate production awaits further flux analysis

(Lakshmanan et al., 2013). Overall, these observations highlight the presence of

at least a partially functional anaerobic TCA cycle in both Echinochloa and rice,

with subtle differences that might correlate with Echinochloa’s increased

success in an oxygen-deprived environment.

A special role for alanine during anoxia

In addition to succinate, alanine accumulation has also been observed under

anoxia (Menegus et al., 1989; Narsai et al., 2009; Shingaki-Wells et al., 2011).

In Arabidopsis, alanine accumulates during oxygen deprivation, even in alanine

aminotransferase (AlaAT) mutants (Miyashita et al., 2007) or GABA-T knockouts

(Miyashita and Good, 2008) and even despite nitrogen starvation (Rocha et al.,

2010). It has been proposed that the production of Ala is beneficial by

consuming the excess pyruvate under anaerobic conditions to prevent

respiratory oxygen consumption (Zabalza et al., 2009). Diversion of pyruvate

into the Ala synthesis pathway could be beneficial as the alternatives, lactate

and ethanol, can be toxic or rapidly diffuse out of the cell, respectively (Figure

2).

In addition to alanine, the AlaAT reaction produces 2-oxoglutarate, which is a

substrate for the GABA shunt pathway (Figure 2). Interestingly, metabolite

analysis has shown that although 2-oxoglutarate abundance decreases under

anoxia, GABA and succinate both increase in abundance under anoxia in rice

(Narsai et al., 2009). In Arabidopsis, when glutamate decarboxylase and GABA

transaminase mutants were examined, the initial rapid alanine accumulation

was not significantly affected (Miyashita and Good, 2008). However, the later,

slower phase of alanine accumulation was partially inhibited in these mutants

suggesting that the GABA shunt, or more specifically, the conversion of GABA

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and pyruvate to alanine and succinic semialdehyde, does contribute to alanine

accumulation under low oxygen conditions (Miyashita and Good, 2008).

It has also been suggested that Ala synthesis could prevent cytoplasmic

acidification that would otherwise occur if all pyruvate was metabolised into

lactate (Reggiani et al., 1988). Interestingly, it has been observed that the

supplementation of Medicago root hairs with alanine (and serine; both of which

are glucogenic amino acids) leads to alkalinisation of the cytoplasm (Felle,

1996). Alanine is a neutral amino acid, with a methyl group side chain. It is

possible that this increase in pH is caused by alanine metabolism, possibly

through conversion to other amino acids or via proton-consuming

gluconeogenesis. However, it was shown that the rapid Ala synthesis that

occurs during the first 90 minutes of oxygen deprivation does not significantly

regulate cytoplasmic pH in maize root tips (Roberts et al., 1992). Whether or

not Ala metabolism contributes to pH regulation during long-term hypoxia is yet

to be determined.

Basic amino acid metabolism in plant mitochondria under anoxia

Mitochondria in rice are also involved in specific aspects of branch chain amino

acid metabolism in anaerobic conditions. An anaerobic-enhanced basic amino

acid carrier (BAC) has been identified in rice and shows a concomitant increase

with mitochondrial arginase and elevation of Arginine and Ornithine in anaerobic

rice tissues, consistent with an anaerobic role of mtBAC (Taylor et al., 2010).

The role for these components in facilitating mitochondrial arginine metabolism

and the plant urea cycle during anoxic growth of rice and in nitrate assimilation

under anaerobic conditions has been presented (Taylor et al., 2010).

Putrescine, synthesised from Arg, is also more abundant in rice during

anaerobic growth (Reggiani et al., 1989). Its synthesis is linked to the ethylene-

enhanced elongation of rice cells (Lee and Chu, 1992). Notably, Pro, which is a

product of Orn, is significantly higher in abundance in anaerobic than aerobic-

germinated rice embryos (Narsai et al., 2009). Pro synthesis occurs very early in

the germination of rice embryos under anaerobic conditions as a major product

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of seed nitrate assimilation (Reggiani et al., 1993; Reggiani et al., 2000), prior to

the breakdown and degradation of amino acids in storage proteins. Ornithine-

Arginine-Citrate metabolism by mitochondria could therefore be enhanced

during anoxia leading to putrescine-stimulated cell elongation and anaerobic

proline synthesis in rice. This pathway is not common to all plants, for example,

there is no report of hypoxic or anaerobic metabolism using BACs in

Arabidopsis, and AtmBAC1 or AtmBAC2 are not enriched on polysomes

during hypoxia in Arabidopsis (Branco-Price et al., 2008).

Respiratory chain

Overall, the mitochondrial proteomes of aerated, anoxic and post-anoxic rice

coleoptiles were similar (Millar et al., 2004). However, closer examination

revealed that fewer respiratory complexes containing cytochrome were found in

anoxic rice coleoptiles, which likely explains the reduced capacity to respire

under these conditions (Millar et al., 2004). Monitoring respiratory capacity of

coleoptiles from rice seedlings germinated and grown under anoxia shows that

mitochondria are equipped to respire should oxygen become available (Millar et

al., 2004; Shingaki-Wells et al., 2011) and also in the anoxia-tolerant barnyard

grass (Kennedy et al., 1987). Thus, while the respiratory chain is generally

down-regulated under anoxia, there is likely to still be some function (Figure 2).

A previous study comparing the transcript responses to low oxygen in

germinating rice, Arabidopsis and poplar revealed several divergences in the

responses of genes encoding components of the respiratory and alternative

pathways (Narsai et al., 2011). Specifically, it was shown that while AOX and

several components of the electron transport chain are induced under low

oxygen in Arabidopsis, this is not seen in rice and the flood-tolerant poplar

(Narsai et al., 2011). It is possible that the up-regulation of these components in

Arabidopsis suggests that this is a response that aims to counteract the energy

crisis during oxygen deprivation. In the case of AOX, it has been shown that

NO production, which occurs under low oxygen, can result in the inhibition of

acontiase activity and subsequent citrate accumulation. Citrate causes an

increase in AOX protein abundance and capacity (Gupta et al., 2012).

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Expression of these genes would be futile and energetically burdensome if

oxygen remains a limiting factor. Thus, the inability of Arabidopsis to prevent

expression of certain genes that do not confer tolerance might underlie its

intolerance to anaerobic conditions.

However, the induction of Complex II components was seen in both

Arabidopsis and rice (Narsai et al., 2011). As a component of both the electron

transport chain and TCA cycle, complex II has a vital role in mitochondrial

metabolism. It has previously been shown that there are significant functional

and compositional differences between mitochondrial complex II between

Arabidopsis and rice (Huang et al., 2010), although it is not yet fully understood

exactly how this may contribute to anaerobic tolerance in rice. Additionally,

recent studies are now revealing a link between the respiratory components

and reactive oxygen species (ROS) as well as nitric oxide (NO) metabolism

(Gupta et al., 2009; Gleason et al., 2010; Gupta and Igamberdiev, 2011)

uncovering new involvement of respiratory components in these pathways

under anoxia.

Roles for NO and ROS in anoxia

Nitrite-dependent ATP production and regulation of nitric oxide (NO)

In recent years, the evidence supporting an important role(s) for NO under low

oxygen has been building (Gupta et al., 2011; Stoimenova et al. 2007). NO

production can occur enzymatically via the activity of nitrate reductase (NR) or

through deoxyhemeprotein-catalysed nitrite reduction (Figure 2) (Huang et al.,

2005). Under anoxia, the NR transcript is significantly induced in rice coleoptiles

(Figure 2) (Lasanthi-Kudahettige et al., 2007). Several studies have tried to

elucidate the role of NO under low oxygen (Planchet et al., 2005; Gupta &

Igamberdiev 2011; Horchani 2011; Stoimenova et al. 2007). Nitrate-

supplemented NR-free tobacco mutants do not produce NO, but when

supplied with nitrite under anoxia, substantial amounts of NO can be produced

(Planchet et al., 2005). This suggests that NO production is nitrite-dependent

under anoxia. In contrast, nitrite reductase-deficient tobacco mutants still show

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NO production (Planchet et al., 2005). It has also been shown that when root

mitochondria from tobacco NR double mutants are supplemented with NADH

and nitrite, NO is generated, and this is exacerbated by falling oxygen

concentrations, supporting a strong link between oxygen and NO (Gupta and

Igamberdiev, 2011). This link is further supported by the finding that electron

transport chain inhibitors inhibit NO production and nitrite supplementation

increases the ATP/ADP ratio in legume nodules (Horchani, 2011).

The addition of nitrite to anaerobic NADH-supplemented barley and rice

mitochondria has also been shown to result in increased ATP synthesis, relative

to nitrite-free anaerobic samples, whilst the same increase in response to nitrite

was not seen in the aerobic counterparts (Stoimenova et al., 2007). Inhibitor

experiments also revealed that nitrite-driven ATP synthesis is sensitive to

uncouplers, myxothiazol (Qo site of complex III) and KCN (complex IV),

suggesting the involvement of proton translocation (Gupta and Igamberdiev,

2011). Stoimenova and colleagues (2007) also reported that nitrite-dependent

ATP production under oxygen deprivation was sustained for longer periods of

time in anoxia-tolerant rice when compared to the less tolerant barley

mitochondria. This may be one factor that underlies the exceptional tolerance

of rice seedlings to anoxia.

As a free radical, NO levels must be regulated to prevent excessive cellular

damage. NO can diffuse out of the mitochondrion into the cytosol to be

converted to nitrate by oxygenated class 1 hemoglobins (Figure 2), which are

up-regulated at the transcript level under low oxygen in Arabidopsis and rice

coleoptiles (Taylor et al., 1994; Lasanthi-Kudahettige et al., 2007; Branco-Price

et al., 2008). This entire cycle oxidizes NADH/NAD(P)H to promote the

maintenance of NAD+/NADP+ levels, which is likely to be important for glycolytic

energy production (Igamberdiev and Hill, 2004). Non-symbiotic hemoglobins

are down-regulated under anoxia during germination, suggesting that this

mechanism of NO scavenging may not come into play until the later stages of

anoxic rice development (Narsai et al., 2011). These non-symbiotic

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hemoglobins are able to stay oxygenated due to their high affinity for oxygen,

even when oxygen falls below the concentration required for complex IV

saturation (Igamberdiev et al., 2010). Oxygenated hemoglobin can oxidise NO

to form nitrate (Figure 2). The resulting met-hemoglobin is then reduced to form

hemoglobin, which can then be re-oxygenated (Igamberdiev et al., 2010). The

nitrate formed can be reduced by NR to nitrite to start the cycle again and

promote ATP synthesis under oxygen deprivation. The pathways relating to NO

that are shown in Figure 2 reflect the suggested pathway from Gupta and

colleagues under low oxygen (Gupta et al., 2011).

Reactive Oxygen Species metabolism and the Ascorbate Glutathione

cycle

In addition to NO, there is also a role for the established links between ROS

and the mitochondrial electron transport chain (mETC). Hydrogen peroxide

(H2O2) production during anoxia has been documented in rice, wheat and

garden iris, but with the plasma membrane NADPH oxidase activity responsible

for a substantial amount of its production (Blokhina et al., 2001). Hypoxia-

induced H2O2 production has also been reported in wheat (Biemelt et al.,

2000). Superoxide production at the mETC also occurs under low oxygen

(Blokhina et al., 2003). In rice coleoptiles, a mitochondrial Mn superoxide

dismutase (MnSOD) has been observed to accumulate under anoxia at the

protein level (Figure 2) (Shingaki-Wells et al., 2011). This MnSOD may act to

detoxify O2- into H2O2 (Figure 2), which can be subsequently reduced to form

water by the mitochondrial ascorbate peroxidase (Xu et al., 2011). This latter

reaction is linked to the oxidation of ascorbic acid to the radical

monodehydroascorbic acid (MDHA), which can disproportionate to

dehydroascorbic acid (DHA) or ascorbic acid (Noctor and Foyer, 1998).

Reduction of MDHA can also be catalysed by MDHA reductase. Reduced

glutathione (GSH) is involved in the next step in the pathway resulting in its

oxidation (GSSG) (Foyer and Halliwell, 1976; Noctor and Foyer, 1998).

Glutathione reductase completes the ascorbate/glutathione cycle by reducing

GSSG to GSH and oxidizing NADPH to NADP+ (Figure 2). H2O2 may also leave

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mitochondria to be metabolized in the cytosol or peroxisome. Notably,

cytosolic peroxiredoxin protein abundance is also increased in anoxic rice

coleoptiles that have never been exposed to oxygen post-imbibition (Figure 2)

(Shingaki-Wells et al., 2011).

While the role of the ascorbate glutathione cycle and ROS metabolism is not

fully characterised under low oxygen conditions in rice, there is some evidence

suggesting involvement of these enzymes during oxygen limitation and

recovery in other plant species. For example, flood-tolerant species such as

Spartina anglica, Menyanthes trifoliata and Phragmites australis show increases

in the activities of dehydroascorbate reductase (DHAR) during post-anoxia

(Wollenweber-Ratzer and Crawford, 1994). This observation is reversed in

flood-intolerant Iris germanica and the anoxia tolerant Acorus calamus. For

MDHA reductase, Acorus calamus, Spartina anglica and Menyanthes trifoliate

showed higher activity post-anoxia relative to a pre-anoxic control

(Wollenweber-Ratzer and Crawford, 1994). Iris germanica showed a reduction

in MDHA reductase activity. This suggests that anoxia-tolerant plants had at

least one enzyme whose activity increased during post-anoxia (Wollenweber-

Ratzer and Crawford, 1994). For glutathione, the data were less clear, with

tolerant plants showing lower levels of GSH and GSSG, and an intolerant plant

only showing decreases in GSH post-anoxia (Wollenweber-Ratzer and

Crawford, 1994). Anoxia-tolerant A. calamus showed an increase in GSSG, but

there was little change in the pool size of total glutathione. Ascorbic acid, on

the other hand, did increase in abundance in this anoxia tolerant species

(Wollenweber-Ratzer and Crawford, 1994). However, as Blokhina and

colleagues (2003) discuss, the overall literature correlating antioxidant status

with tolerance is often internally contradictory (Blokhina et al., 2003).

Lastly, although the link between ROS and the ETC is not fully understood in

rice, it is known that transcripts encoding complex II, succinate

dehydrogenase, are induced under low oxygen (Narsai et al., 2011).

Interestingly, recent studies have shown a link between mitochondrial complex

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II and ROS in both humans (Moreno-Sánchez et al., 2013) and plants (Gleason

et al., 2011). Specifically, in Arabidopsis, it was shown that SDH1-1 mutants

had phenotypes associated with lowered mitochondrial ROS production,

providing evidence that the ETC contributes to localized mitochondrial ROS

production (Gleason et al., 2011). If this link is conserved in rice, a functional

complex II under anoxia may contribute to specific ROS-related signalling or

gene expression (Fukao and Bailey-Serres, 2004), both while under anoxia and

possibly even in preparation for re-oxygenation. Alternatively, a role for reverse

electron flow through succinate dehydrogenase is worthy of consideration

(Hohl et al., 1987; Igamberdiev and Hill, 2009), but this still requires more

evidence that it occurs and is physiologically relevant in plants.

Re-oxygenation in plants

It is important to note that different plant species have adapted to different

levels of tolerance to anaerobic conditions, whereby several species are able to

survive relatively short bursts of hypoxia and recover. For example, despite

significant mitochondrial damage observed in wheat seedlings upon exposure

to low oxygen (Figure 1), mitochondrial recovery does occur when seedlings

are re-oxygenated, provided the duration of low oxygen treatment is brief

(Vartapetian et al., 1985). While this is the case for most species, rice can

survive extended periods of anoxia as a result of specific adaptations. One of

these includes coleoptile elongation, which in some cases is more rapid under

anoxia when compared to aerobically-germinated seedlings (Alpi and Beevers,

1983). Additionally, primary leaves fail to grow and root growth is hindered

under anaerobic conditions. This response of trying to grow in order to reach

the aerobic surface is called the Snorkel effect (Kordan, 1974), reflecting how

rice is re-introduced to oxygen, even after flooded germination. However,

literature searches reveal that the molecular responses to re-oxygenation are

not as well characterised as the response to low oxygen alone.

Re-oxygenated samples can reflect plants germinated and grown under anoxia

that are then switched to an aerated environment. This provides the

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opportunity to study oxygen-independent development and the capacity of a

naïve plant to adapt to oxygenation shock. However, it is limited by the fact that

relatively few plants can germinate under oxygen deprivation. For example, rice

but not wheat, will germinate in the complete absence of oxygen, so

comparing these species will require aerated conditions at the germination

stage for wheat. Hence, post-anoxic plants can also reflect plants that were

grown under aerated conditions, are subsequently switched to either a

complete or near anaerobic environment to then be re-exposed to oxygen for

‘recovery’, as may occur under a period of brief flood.

Both approaches can use two types of control treatments including (1)

continuously aerated samples as well as (2) samples that are either

continuously anoxic or where the last treatment was anoxia. Using both types

of control treatments could be useful in defining re-oxygenation specific

responses as opposed to those responses that are simply oxygen-dependent.

For example, a transcript or protein that is detected only during recovery, but

not in continuously anoxic or aerated samples could be considered specific to

post-anoxia.

Transcriptomic responses to re-oxygenation

Post-anoxic transcriptome data, although limited in the published literature,

could provide clues into how, and the degree to which, metabolism is re-

modelled when oxygen becomes available. Using a three-way experimental

design including 1) aerobic v anaerobic germination, 2) 24 h aerobic

germination switched to anaerobic conditions for up to 6 h, and 3) 24 h

anaerobic germination switched to aerobic condition for up to 6 h, it was

possible to identify core aerobic and anaerobically responsive transcripts

(Narsai et al., 2009). When rice was germinated for 24 h under anoxia and then

switched to aerobic conditions, significant transcriptome reprogramming was

observed (Narsai et al., 2009). Over 4000 genes were induced within only 6 h

of exposure to air, and over 50% of those had higher expression under aerobic

germination compared to anaerobic germination, indicating a rapid shift

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towards aerobic growth (Narsai et al., 2009). Another 15% represented genes

specifically responsive to re-oxygenation, whereby these were not higher during

aerobic germination, but were down-regulated in response to switching from

aerobic to anaerobic conditions, indicating oxygen-treatment specific regulation

(Narsai et al., 2009).

In anoxia-intolerant Arabidopsis, selective mRNA translation was examined in

seedlings subjected to hypoxia and subsequently returned to aeration (Branco-

Price et al., 2008). As discussed above, Arabidopsis seedlings subjected to

hypoxia had a 50% reduction in polysome content and increases in 80S

monosomes and ribosome subunits, observations that were reversed upon re-

oxygenation for 1 hour (Branco-Price et al., 2008). Transcripts encoding

proteins involved in cell wall formation, transcription, signalling, cell division,

hormone metabolism and lipid metabolism were translationally repressed under

hypoxia, whereas after 1 hour of re-oxygenation, translational repression was

relieved (cluster 4 (Branco-Price et al., 2008)). A specific example of this is a

protein annotated as a eukaryotic translation initiation factor 4F (At5g57870).

Polysomal mRNA was isolated from Arabidopsis seedlings treated with

hypoxia, re-oxygenation or no stress at all to deduce a putative oxygen

responsive translatome. Indeed, many polysome-associated mRNAs were

induced during hypoxic treatment. Interestingly, 80% of the polysomal mRNAs

that were highly induced after 9 h hypoxia did not significantly decrease after

1h re-oxygenation, an observation in-line with translational repression under

hypoxia (Branco-Price et al., 2008). It is unclear what exactly the biological

significance of this is, but it is possible that some hypoxia-induced transcripts

are important for re-oxygenation, or that 1 h is too short a time for dissociation

of ribosomes and mRNAs in Arabidopsis. Alternatively, there may have been an

evolutionary benefit in delaying polysome dissociation if hypoxia was a frequent

and recurring threat. This is further supported by the identification of a cluster

of genes that were induced during hypoxia, but only associating with

ribosomes during re-oxygenation (cluster 3; (Branco-Price et al., 2008)).

Nevertheless, it is also possible that the observed low oxygen intolerance in

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Arabidopsis may be contributed to by its delayed response to re-oxygenation.

Re-oxygenation effects on fermentation, TCA cycle and glycolysis

It is very well known that under low-oxygen conditions, fermentation is induced

in many plant species, where pyruvate is first converted to acetaldehyde, which

can enter the mitochondria or remain in the cytosol where it is converted to

ethanol (Figure 2) (Davies et al., 1974; Guglielminetti et al., 2001; Narsai et al.,

2009; Mustroph et al., 2010). However, overall, anaerobic activities result in

decreased ATP and increased cytoplasmic acidity, which can hinder recovery

upon re-oxygenation (Menegus et al., 1991; Felle, 2005). In rice, an aldehyde

dehydrogenase (Aldehyde dehydrogenase 2a - LOC_Os02g49720.1) is

induced at the transcript level under anoxia in coleoptiles and during

germination (Lasanthi-Kudahettige et al., 2007; Narsai et al., 2009). However,

at the protein level, it is reduced in rice embryo mitochondria as well as

coleoptiles under anoxia (Howell et al., 2007; Sadiq et al., 2011). Thus, the

regulation of ALDH2b is contradictory at the transcript and protein levels, with

further investigation necessary to deduce the reasons for this.

Mitochondrial aldehyde dehydrogenases oxidise aldehydes to form acetate. In

rice leaves ALDH2a protein increases slightly after 24 h submergence, despite

the large mRNA induction in the same tissue (Tsuji et al., 2003). ALDH2a then

continues to accumulate post-submergence, reaching its peak at 4 h and then

decreasing by 24 h, an endpoint protein abundance that is higher than before

or immediately after submergence (Tsuji et al., 2003). ALDH2b decreases after

submergence and during re-oxygenation levels reach a minimum at 1.5 h but

show consistent increases up to 24 h (Tsuji et al., 2003). Even though levels of

acetaldehyde and ethanol were high after 24 h submergence, ALDH activity

was only induced during the re-oxygenation phase with concomitant decreases

in acetaldehyde levels (Tsuji et al., 2003). Taken together with the shown

reverse activity of ADH and catalases in ethanol metabolism in young poplar

plants (Kreuzwieser et al., 2001), it has been proposed that upon re-

oxygenation, ethanol produced during anaerobiosis may converted back to

acetaldehyde by peroxidation through catalases or reverse ADH activity

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(Kreuzwieser et al., 2001; Tsuji et al., 2003). Thus, acetaldehyde oxidation

could aid the post-anoxic re-generation of acetyl-CoA, a TCA cycle substrate,

as well as the complex I substrate NADH, both of which are integral to

respiratory metabolism. Further supporting this is the finding that within only 3 h

of exposure to air after 24 h of anaerobic germination, genes encoding TCA

cycle components are significantly induced and subsequent metabolites

including citrate and 2-oxoglutarate, are also increased in abundance, whilst

succinate and fumarate are depleted, suggesting a rapid response to reinstate

the aerobic TCA cycle (Narsai et al., 2009).

In addition to the TCA cycle, significant changes to the expression of glycolytic

enzymes were also observed upon 3 h of aeration after 24 h of anaerobic

germination, including the induction of phosphoglycerate mutase and enolase

encoding genes (down-regulated under anoxia; Figure 2), as well as increases

in fructose and glucose metabolite content (Narsai et al., 2009). Other

metabolites identified to accumulate under re-oxygenation included

carbohydrates arabinose and trehalose, suggesting a restoration of

carbohydrate pools when the energy crisis presented by anoxia is relieved.

Alanine and post-anoxia

As discussed above, alanine accumulation is seen under anaerobic conditions

(Kato-Noguchi, 2006; Kato-Noguchi and Ohashi, 2006; Shingaki-Wells et al.,

2011). Additionally, this accumulation is thought to also be beneficial during re-

oxygenation (Rocha et al., 2010). The Arabidopsis knockout AlaAT1 sustains

hypoxic accumulation of alanine, however upon the return of oxygen, these

plants show defective rates of Ala consumption relative to WT plants (Miyashita

et al., 2007). This could result in glutamate and pyruvate synthesis, the latter of

which could be metabolised into Acetyl CoA for TCA cycle/ETC operation.

Interestingly, when tracking alanine and AlaAT levels in waterlogged plants,

increases in AlaAT continued to occur beyond the point at which levels of

alanine reached a plateau (de Sousa and Sodek, 2003). Support for a vital role

of AlaATs is demonstrated by the steep declines in Ala during re-oxygenation

(de Sousa and Sodek, 2003). Alanine may be thought of as a transportable

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energy source, much like lactic acid in the Cori cycle of animals or sucrose of

plants, as its transport through xylem has been shown previously (de Sousa

and Sodek, 2003). Like lactic acid, alanine can be metabolised into pyruvate,

which can subsequently enter the gluconeogenesis pathway or be metabolised

into Acetyl CoA.

Interestingly, the coleoptiles of anoxia-intolerant wheat seedlings subjected to

1d of anoxia did not accumulate alanine, unlike that of anoxia-tolerant rice

(Shingaki-Wells et al., 2011). However, upon supplementation of anoxic

seedlings with alanine, electrolyte leakage was reduced in wheat but not in rice,

whose leakage was already low relative to wheat. Thus, it appears, that alanine

has a significantly beneficial role under anoxia itself and thus the production of

a rice plant defective in alanine synthesis could reveal the regulation and

pathways responsible for the steep alanine accumulation that occurs, even

when plants are deficient of nitrogen (Rocha et al., 2010).

Vacuolar H+-pyrophosphatase (V-PPase)

Anoxically-treated rice seedlings show increased V-PPase protein activity,

which is thought to hydrolyse PPi, as opposed to scarcely abundant ATP, to

pump protons from the cytosol to the vacuole (Figure 2) (Carystinos et al.,

1995). This induction would be useful in the context of anoxia, where Mg2+

concentrations rise as a result of falling ATP, to promote Mg-PPi complex

formation (Igamberdiev and Kleczkowski, 2011). As discussed in detail by

Igamberdiev and Kleczkowski (2011) these conditions would promote the

function of PPi-dependent enzymes. The induction of V-PPase is also seen in

cold-treated seedlings (Carystinos et al., 1995). Re-oxygenation for two days

results in a decrease of V-PPase to levels that are barely detectable and

comparable to pre-anoxic seedlings. The activity of V-PPase also mirrored

these protein abundance changes (Carystinos et al., 1995). Relative to V-

PPase, the activity of the ATP-dependent proton pump increased slightly

during anoxia. Similarly, this activity returned to pre-anoxic levels upon re-

oxygenation. Whether or not V-PPase proton pumping counteracts anoxic

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cytoplasmic acidification is debatable, since anoxic rice vacuoles show

increases in their pH (Menegus et al., 1991), with alternative purposes thought

to include the maintenance of tonoplast energisation as a preventative cell

death measure (Carystinos et al., 1995).

Post-anoxic decreases in the activities of V-PPase and V-ATPase suggest a

reduction in the need for proton transport across the vacuolar membrane. In

another study, rice seedlings overexpressing V-PPase (OVP1) show increased

survival after cold treatment compared to wild type seedlings, and this

correlates with a decrease in markers for membrane damage as well as higher

proline levels in cold-treated transgenic seedlings (Zhang et al., 2011). The

significance of anoxic V-PPase induction in rice is yet to be fully elucidated.

However, it is worth noting that anoxic rice seedlings rapidly accumulate proline

(Figure 2) and show no significant increase in electrolyte leakage, a marker for

membrane damage, when transferred to anoxia. Anoxic wheat, which is

relatively intolerant to anoxia, accumulates proline, albeit to a lesser extent, and

shows large and significant increases in electrolyte leakage (Shingaki-Wells et

al., 2011). The level of anoxic V-PPase induction in wheat is yet to be

determined.

Respiratory components

Mitochondria isolated from the coleoptiles of rice seedlings grown under anoxia

for 7 days show significantly lower rates of oxygen consumption than their

aerobically-grown counterparts (Millar et al., 2004). When 6 day old anoxic

seedlings are switched to air for 1 day, the rate of oxygen consumption

recovers to levels comparable to those seen in continuous aeration (Millar et al.,

2004). This is also supported by the rapid and significant induction of genes

encoding respiratory chain components, and alternative pathway components

within 3 h of aerobic treatment after 24 h of anaerobic germination (Narsai et

al., 2009). Re-oxygenated coleoptile samples were unique, in that they were

able to respire in a KCN-insensitive manner, attributed to AOX protein induction

also observed upon re-oxygenation (Millar et al., 2004). Soluble mitochondrial

protein profiles of continuously anoxic and re-oxygenated rice coleoptiles are

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remarkably similar, indicating that the synthesis and maintenance of many

mitochondrial components can occur in an oxygen-independent manner.

Analysis of whole mitochondrial proteomes revealed an enrichment of

chaperones and proteins involved in carbon metabolism during re-oxygenation

of coleoptiles, but on the whole, anoxic and post-anoxic proteomes were

largely similar (Millar et al., 2004).

Complex I and ATP synthase protein abundances did not differ significantly

when comparing anoxic and re-oxygenated samples. Other membrane

proteins that were part of the b/c1 complex (III) and cytochrome c oxidase (IV)

complex were clearly more abundant during the re-oxygenation phase (Millar et

al., 2004). These observations are consistent with the higher cytochrome

content, heme and cytochrome c during air adaptation (Millar et al., 2004).

Post-anoxic AOX induction is seen both at the transcript and protein levels

upon re-oxygenation (Millar et al., 2004; Narsai et al., 2009). This induction may

prevent over-reduction of the respiratory chain in a situation where heme

abundance was previously limited. It is also likely that the high level of

mitochondrial biogenesis that takes place in anoxic rice seedlings aids a rapid

response to re-oxygenation shock (Millar et al., 2004; Howell et al., 2007).

Soybean re-oxygenation responses

The first large-scale re-oxygenation proteomics study focused on the roots of

soybean seedlings (Salavati et al., 2012). Two-day-old seedlings subjected to

one day of flooding were sampled four days after de-submergence and

compared to seven-day-old seedlings kept under continuous aeration.

Seedlings were also sampled immediately after flooding and compared to 3-

day-old continuously aerated controls. Of the seven proteins whose

abundances did not return to control levels during re-oxygenation, six

increased and one decreased during recovery. These six were also significantly

more abundant immediately after the flooding stress. Of interest is 1-Cys

peroxiredoxin (Prx), a protein that detoxifies H2O2, and whose abundance

immediately after flooding was 3 fold higher than that of seedlings grown under

continuous aeration. Prx remained significantly more abundant in de-

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submerged seedlings compared to its control. Sustained elevation during re-

oxygenation could lend support to the hypothesis that anoxic induction of Prx

is a preparatory measure for the threat of oxidative stress posed during post-

anoxia. Interestingly, Prx induction is also conserved in anoxic rice coleoptiles

and fresh water low oxygen tolerant turtles (Krivoruchko and Storey, 2010;

Shingaki-Wells et al., 2011).

It is important to note that the submerged soybean seedlings were grown

under a light regime (Salavati et al., 2012). Thus, it is likely that the conditions

were not fully anoxic, facilitating ROS production and therefore hypoxic Prx

function is a possibility. However, the conserved response between flooded

soybean, anoxic rice and even anoxic freshwater turtles (Krivoruchko and

Storey, 2010; Shingaki-Wells et al., 2011), in addition to the sustained elevation

of Prx during de-submergence, makes it tempting to speculate that Prx

functions broadly in both plants and animals to detoxify ROS during re-

oxygenation. It is possible that the high abundance of Prx under low oxygen

may also be a result of delayed protein degradation, which would otherwise

occur in aeration, as has been shown in flooded soybean seedlings (Nishizawa

and Komatsu, 2011). The lack of flood-induced Prx mRNA induction also

supports this notion (Nishizawa and Komatsu, 2011).

The classical anaerobic proteins alcohol dehydrogenase and pyruvate

decarboxylase are elevated in re-oxygenated samples compared to aerated

controls (Salavati et al., 2012). This could be a result of a delay in return to

metabolic equilibrium post-hypoxia (i.e. a remnant hypoxic response) or could

indicate the necessity of these proteins after a flood, especially if this event is

likely to re-occur. An overview of re-oxygenated samples treated with 1, 2 or 3

days of flooding also reveals an up-regulation of proteins involved in protein

folding, cell wall biosynthesis, cell expansion and cytoskeletal organization.

Down-regulated proteins were involved in amino acid metabolism, proteolysis

and glycolysis (Salavati et al., 2012). Notably, these proteins are up-regulated in

anoxic rice coleoptiles (Shingaki-Wells et al., 2011), thus the down-regulation of

these during re-oxygenation may represent an attempt to return to equilibrium.

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Such observations highlight the importance of considering multiple stages of

this plant stress to identify re-oxygenation-specific responses.

Which mitochondrial functions help to make rice an

anoxia survivor?

As an anoxia-tolerant species, rice has many adaptations that allow survival

under both relatively long periods of continuous anoxia, as well as during re-

oxygenation stress, which is known to further hinder survival in other plant

species. Based on the literature we propose some prominent mitochondrial

adaptations and/or responses in this species that may be important survival

traits, and these are summarised below.

• Nitrite-dependent ATP production is sustained for longer

Roles for NO production and scavenging in plant mitochondria under anoxia

have been proposed based on the NO production observed under low oxygen

(Benamar et al., 2008); reviewed in (Gupta et al., 2011)). Using nitrite as an

electron acceptor, it has been shown that anaerobic ATP production in this

manner is sustained for almost twice as long in anoxia-tolerant rice, compared

to anoxia-intolerant barley (Stoimenova et al., 2007). While ATP production

under anaerobic conditions is less than 25% of what is seen in aerobic

conditions, this is still significantly higher than in anoxia-intolerant species such

as maize and wheat under anoxia (Mustroph and Albrecht, 2003). Therefore,

between activating PPi-dependent pathways (Huang et al., 2008) and having

increased nitrite-dependent ATP production (Stoimenova et al., 2007) more

energy is produced under anoxia in rice compared to anoxia-intolerant species.

• Anaerobic arginine metabolism for cell elongation and amino

acid synthesis

The anaerobic enhancement of BAC and arginase in rice mitochondria (Taylor

et al., 2010) provides a role of mitochondria during anoxia in altering amino acid

content of anoxic tissues and even contributing to cell elongation processes in

rice coleoptiles. There are potential links between this process and the N-

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based electron transport chain metabolism, noted above, that remain to be

explored.

• Aldehyde dehydrogenase functions in low oxygen and re-

oxygenation

The rice mitochondrial ALDH2 oxidises aldehyde to form acetate and is

induced under anoxia in coleoptiles and during anaerobic germination in rice

(Tsuji et al., 2003; Lasanthi-Kudahettige et al., 2007; Narsai et al., 2009). In

contrast, its Arabidopsis orthologue is not induced under low oxygen

(Kursteiner et al., 2003). Given that ALDH2 does not decrease in abundance for

a few hours following re-oxygenation in flood tolerant rice and poplar, it has

been proposed that the ethanol produced during anaerobiosis may be

converted back to acetaldehyde by peroxidation through catalases or ADH

activity (Kreuzwieser et al., 2001; Tsuji et al., 2003). Acetaldehyde may then be

entering the mitochondria for conversion into acetate by ALDH2 (Tsuji et al.,

2003). Thus, this modified fermentative metabolism may contribute to re-

oxygenation survival in low oxygen tolerant species such as rice and poplar.

• Separate response to anoxia from those to other abiotic stresses

A recent study compared low oxygen stress to other abiotic stress (drought,

salt, cold and heat) responses in rice and Arabidopsis, in order to gain insight

into the uniqueness of the low oxygen response (Narsai and Whelan, 2013).

This study showed that several genes associated with oxidative stress (as

identified in (Gadjev et al., 2006) are down-regulated under heat stress but

induced under anoxia in Arabidopsis, whereas their rice orthologues are down-

regulated under anoxia (Banti et al., 2008; Narsai and Whelan, 2013). This

supports the observations that pre-treating Arabidopsis seedlings with heat,

improves low oxygen survival (Banti et al., 2008). For example, the

mitochondrial dicarboxylate carrier 2 (AtDIC2 - AT4G24570) is induced under

anoxia and abiotic stress in Arabidopsis, whereas its rice orthologue

(LOC_Os08g37370.1), annotated as a mitochondrial 2-oxoglutarate/malate

carrier, showed repressed gene expression under anoxia and unchanging

expression under abiotic stress (Narsai et al., 2013b). Similarly, several WRKY

transcription factor encoding genes that were induced under low oxygen in

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Arabidopsis, were also repressed or unchanging under anoxia in rice,

suggesting that for some stress-responsive pathways, Arabidopsis may

perceive low oxygen stress similarly to other abiotic stresses, whereas, this

does not appear to be the case in rice (Narsai et al., 2013b).

Conclusions

As a major site for energy production, regulation of the mitochondrial system is

essential for survival, from the level of maintaining ultrastructure for membrane

potential (Figure 1) to the transcript, protein, enzyme activity and metabolite

levels that need to be intricately regulated (Figure 2). This functionality is even

more crucial under low oxygen conditions when there is an energy deficit.

Hence, not all species can survive under low oxygen. Anoxia-tolerant rice

represents a relativity unique and increasingly characterised model for low-

oxygen tolerance. In the last decade, much more knowledge has been gained

pertaining to the mechanisms relating to low oxygen survival. In terms of

mitochondria, a complex picture is emerging showing important functional links

between the respiratory pathway and sugar/starch signalling in anoxic rice (Lu

et al., 2007; Cho et al., 2009; Park et al., 2010). Additionally, there is growing

evidence for respiratory chain components being involved in NO and ROS

signalling under low oxygen (Blokhina et al., 2003; Gupta et al., 2011). Thus, in

addition to being the powerhouses for oxidative phosphorylation, mitochondria

are also important organelles in helping to ensure survival under anoxia.

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References

Alpi A, Beevers H (1983) Effects of O2 Concentration on Rice Seedlings. Plant Physiology 71: 30-34 Bailey-Serres J, Fukao T, Gibbs DJ, Holdsworth MJ, Lee SC, Licausi F, Perata P, Voesenek LA, van Dongen JT (2012) Making sense of low oxygen sensing. 17: 129-138 Banti V, Loreti E, Novi G, Santaniello A, Alpi A, Perata P (2008) Heat acclimation and cross-tolerance against anoxia in Arabidopsis. Plant, Cell and Environment 31: 1029-1037 Barnett JA (2003) A history of research on yeasts 5: the fermentation pathway. Yeast 20: 509-543 Benamar A, Rolletschek H, Borisjuk L, Avelange-Macherel MH, Curien G, Mostefai HA, Andriantsitohaina R, Macherel D (2008) Nitrite-nitric oxide control of mitochondrial respiration at the frontier of anoxia. Biochim Biophys Acta 1777: 1268-1275 Biemelt S, Keetman U, Mock H-P, Grimm B (2000) Expression and activity of isoenzymes of superoxide dismutase in wheat roots in response to hypoxia and anoxia. Plant, Cell & Environment 23: 135-144 Blokhina O, Fagerstedt KV (2010) Oxidative metabolism, ROS and NO under oxygen deprivation. Plant Physiology and Biochemistry 48: 359-373 Blokhina O, Virolainen E, Fagerstedt KV (2003) Antioxidants, Oxidative Damage and Oxygen Deprivation Stress: a Review. Annals of Botany 91: 179-194 Blokhina OB, Chirkova TV, Fagerstedt KV (2001) Anoxic stress leads to hydrogen peroxide formation in plant cells. Journal of Experimental Botany 52: 1179-1190 Branco-Price C, Kaiser KA, Jang CJH, Larive CK, Bailey-Serres J (2008) Selective mRNA translation coordinates energetic and metabolic adjustment to celluar oxygen deprivation and reoxygenation in Arabidopsis thaliana. The Plant Journal 56: 743-755 Carystinos GD, MacDonald HR, Monroy AF, Dhindsa RS, Poole RJ (1995) Vacuolar H(+)-translocating pyrophosphatase is induced by anoxia or chilling in seedlings of rice. Plant Physiol 108: 641-649 Cho JI, Ryoo N, Eom JS, Lee DW, Kim HB, Jeong SW, Lee YH, Kwon YK, Cho MH, Bhoo SH, Hahn TR, Park YI, Hwang I, Sheen J, Jeon JS (2009) Role of the rice hexokinases OsHXK5 and OsHXK6 as glucose sensors. Plant Physiology 149: 745-759 Couee I, Defontaine S, Carde J-P, Pradet A (1992) Effects of anoxia on mitochondrial biogenesis in rice shoots. Modification of in Organello translation characteristics. Plant Physiology 98: 411-421 Davies DD, Grego S, Kenworthy P (1974) The control of the production of lactate and ethanol by higher plants. Planta 118: 297-310 de Sousa CAF, Sodek L (2003) Alanine metabolism and alanine aminotransferase activity in soybean (Glycine max) during hypoxia of the root system and subsequent return to normoxia. Environmental and Experimental Botany 50: 1-8

Page 54: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

42

Dudkina NV, Heinemeyer J, Sunderhaus S, Boekema EJ, Braun HP (2006) Respiratory chain supercomplexes in the plant mitochondrial membrane. TRENDS in Plant Science 11: 232-240 Edwards JM, Roberts TH, Atwell BJ (2012) Quantifying ATP turnover in anoxic coleoptiles of rice (Oryza sativa) demonstrates preferential allocation of energy to protein synthesis. Journal of Experimental Botany 63: 4389-4402 Felle HH (1996) Control of cytoplasmic pH under anoxic conditions and its implication for plasma membrane proton transport in Medicago sativa root hairs. Journal of Experimental Botany 47: 967-973 Felle HH (2005) pH Regulation in Anoxic Plants. Annals of Botany 96: 519-532 Fox TC, Kennedy RA (1991) Mitochondrial enzymes in aerobically and anaerobically germinated seedlings of Echinochloa and rice. Planta 184: 510-514 Foyer CH, Halliwell B (1976) The presence of glutathione and glutathione reductase in chloroplasts: A proposed role in ascorbic acid metabolism. Planta 133: 21-25 Fukao T, Bailey-Serres J (2004) Plant responses to hypoxia - is survival a balancing act? TRENDS in Plant Science 9: 449-456 Fukao T, Xu K, Ronald PC, Bailey-Serres J (2006) A variable cluster of ethylene response factor-like genes regulates metabolic and developmental acclimation responses to submergence in rice. The Plant Cell 18: 2021-2034 Fukao T, Yeung E, Bailey-Serres J (2011) The Submergence Tolerance Regulator SUB1A Mediates Crosstalk between Submergence and Drought Tolerance in Rice. The Plant Cell 23: 412-427 Gadjev I, Vanderauwera S, Gechev TS, Laloi C, Minkov IN, Shulaev V, Apel K, Inze D, Mittler R, Van Breusegem F (2006) Transcriptomic footprints disclose specificity of reactive oxygen species signaling in Arabidopsis. Plant Physiology 141: 436-445 Gibbs J, Greenway H (2003) Mechanisms of anoxia tolerance in plants. I. Growth, survival and anaerobic catabolism. Functional Plant Biology 30: 1–47 Gibbs J, Morrell S, Valdez A, Setter TL, Greenway H (2000) Regulation of alcoholic fermentation in coleoptiles of two rice cultivars differing in tolerance to anoxia. Journal of Experimental Botany 51: 785-796 Gleason C, Huang S, Thatcher LF, Foley RC, Anderson CR, Caroll AJ, Millar AH, Singh KB (2010) Reactive oxygen species signalling from mitochondria links pathogen perception to plant defence. Proc Natl Acad Sci U S A 108: 10768-10773 Greenway H, Gibbs J (2003) Mechanism of anoxia tolerance in plants. II. Maintenance requirements for energy and energy consuming processes. Functional Plant Biology 30: 999-1036 Guglielminetti L, Busilacchi HA, Perata P, Alpi A (2001) Carbohydrate-ethanol transition in cereal grains under anoxia. New Phytologist 151: 607-612

Page 55: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

43

Guglielminetti L, Perata P, Alpi A (1995) Effect of anoxia on carbohydrate metabolism in rice seedlings. Plant Physiology 108: 735-741 Guglielminetti L, Yamauchi M, Perata P, Alpi A (1995) Amylotic activities in cereal seeds under aerobic and anaerobic conditions. Plant Physiology 109: 1069-1076 Gupta HS, Igamberdiev AU, Manjunatha G, Segu S, Moran JF, Neelawarne B, Bauwe H, Kaiser WM (2011) The emerging roles of nitric oxide (NO) in plant mitochondria. Plant Science 181: 520-526 Gupta KJ, Igamberdiev AU (2011) The anoxic plant mitochondrion a a nitrite: NO reductase. Mitochondrion 11: 537-543 Gupta KJ, Shah JK, Brotman Y, Jahnke K, Willmitzer L, Kaiser WM, Bauwe H, Igamberdiev AU (2012) Inhibition of aconitase by nitric oxide leads to induction of the alternative oxidase and to a shift of metabolism towards biosynthesis of amino acids. Journal of Experimental Botany 63: 1773-1784 Gupta KJ, Zabalza A, van Dongen JT (2009) Regulation of respiration when the oxygen availability changes. Physiologia Plantarum 137: 383-391 Hattori Y, Nagai K, Furukawa S, Song X, Kawano R, Sakakibara H, Wu J, Matsumoto T, Yoshimura A, Kitano H (2009) The ethylene response factors SNORKEL1 and SNORKEL2 allow rice to adapt to deep water. Nature 460: 1026-1030 Hinz M, Wilson IW, Yang J, Buerstenbinder K, Llewellyn D, Dennis ES, Sauter M, Dolferus R (2010) Arabidopsis RAP2.2: an ethylene response transcription factor that is important for hypoxia survival. Plant Physiology 153: 757-772 Hohl C, Oestreich R, Rosen P, Wiesner R, Grieshaber M (1987) Evidence for succinate production by reduction of fumarate during hypoxia in isolated adult rat heart cells. Archives of biochemistry and biophysics 259: 527-535 Horchani F, Prevot, M., Boscari, A., Evangelisti, E., Meilhoc, E., Bruand, C., Raymond, P., Boncompagni, E., Aschi-Smiti, S., Puppo, A., Brouquisse, R. (2011) Both plant and bacterial nitrate reductases contribute to nitric oxide production in Medicago truncatula nitrogen-fixing nodules. . Plant Physiol. 155: 1023–1036 Horder M (1974) Complex formation or inorganic pyrophosphate with magnesium influence of ionic strength, supporting medium and temperature. Biochim Biophys Acta 358: 319-328 Howell KA, Cheng K, Murcha MW, Jenkin LE, Millar AH, Whelan J (2007) Oxygen initiation of respiration and mitochondrial biogenesis in rice. Journal of Biological Chemistry 282: 15619-15631 Huang K, Keszler A, Patel N, Patel R, Gladwin M, Kim-Shapiro D, Hogg N (2005) The reaction between nitrite and deoxyhemoglobin. Reassessment of reaction kinetics and stoichiometry. Journal of Biological Chemistry 280: 31126-31131 Huang S, Colmer TD, Millar AH (2008) Does anoxia tolerance involve altering the energy currency towards PPi? Trends in Plant Science 13: 221-227

Page 56: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

44

Huang S, Greenway H, Colmer T, Millar H (2005) Protein synthesis by rice coleoptiles during prolonged anoxia: implications for glycolysis, growth and energy utilization. Annals of Botany 96: 703–715 Huang S, Taylor NL, Narsai R, Eubel H, Whelan J, Millar AH (2010) Functional and composition differences between mitochondrial complex II in Arabidopsis and rice are correlated with the complex genetic history of the enzyme. Plant Molecular Biology 72: 331-342 Igamberdiev AU, Bykova NV, Shah JK, Hill RD (2010) Anoxic nitric oxide cycling in plants: participating reactions and possible mechanisms. Physiologia Plantarum 138: 393-404 Igamberdiev AU, Hill RD (2004) Nitrate, NO and haemoglobin in plant adaptation to hypoxia: an alternative to classic fermentation pathways. Journal of Experimental Botany 55: 2473-2482 Igamberdiev AU, Hill RD (2009) Plant mitochondrial function during anaerobiosis. Annals of botany 103: 259-268 Igamberdiev AU, Kleczkowski LA (2011) Magnesium and cell energetics in plants under anoxia. The Biochemical Journal 437: 373-379 Ismond KP, Dolferus R, De Pauw M, Dennis ES, Good AG (2003) Enhanced low oxygen survival in Arabidopsis through increased metabolic flux in the fermentative pathway. Plant Physiology 132: 1292-1302 Kato-Noguchi H (2006) Pyruvate metabolism in rice coleoptiles under anaerobiosis. Plant Growth Regulation 50: 41-46 Kato-Noguchi H, Ohashi C (2006) Effects of anoxia on amino acid levels in rice coleoptiles. Plant Production Science 9: 383-387 Kende H (1993) Ethylene biosynthesis. Annual Review of Plant Physiology and Plant Molecular Biology 44: 283-307 Kennedy RA, Barrett SCH, Vander Zee D, Rumpho ME (1980) Germination and seedling growth under anaerobic conditions in Echinochloa crus-galli (barnyard grass). Plant, Cell & Environment 3: 243-248 Kennedy RA, Fox TC, Siedow JN (1987) Activities of isolated mitochondria and mitochondrial enzymes from aerobically and anaerobically germinated barnyard grass (Echinochloa) seedlings. Plant Physiology 85: 474-480 Kordan HA (1974) Patterns of shoot and root growth in rice seedlings germinating under water. Journal of Applied Ecology 11: 685-690 Kreuzwieser J, Harren FJM, Laarhoven LJJ, Boamfa I, te Lintel-Hekkert S, Scheerer U, Huglin C, Rennenberg H (2001) Acetaldehyde emission by the leaves of trees – correlation with physiological and environmental parameters. Physiologia Plantarum 113: 41-49 Krivoruchko A, Storey KB (2010) Forever young: mechanisms of natural anoxia tolerance and potential links to longevity. Oxidative medicine and cellular longevity 3: 186-198 Kursteiner O, Dupuis I, Kuhlemeier C (2003) The pyruvate decarboxylase1 gene of Arabidopsis is required during anoxia but not other environmental stresses. Plant Physiology 132: 968-978 Lakshmanan M, Zhang Z, Mohanty B, Kwon JY, Choi H-Y, Nam H-J, Kim D-I, Lee D-Y (2013) Elucidating Rice Cell Metabolism under Flooding

Page 57: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

45

and Drought Stresses Using Flux-Based Modeling and Analysis. Plant Physiol 162: 2140–2150 Lasanthi-Kudahettige R, Magneschi L, Loreti E, Gonzali S, Licausi F, Novi G, Beretta O, Vitulli F, Alpi A, Perata P (2007) Transcript profiling of the anoxic rice coleoptile. Plant Physiology 144: 218-231 Lee TM, Chu C (1992) Ethylene-Induced Polyamine Accumulation in Rice (Oryza sativa L.) Coleoptiles. Plant physiology 100: 238-245 Licausi F, van Dongen JT, Giuntoli B, Novi G, Santaniello A, Geigenberger P, Perata P (2010) HRE1 and HRE2, two hypoxia-inducible ethylene response factors, affect anaerobic responses in Arabidopsis thaliana. The Plant Journal 62: 302-315 Liu X, Hajnoczky G (2011) Altered fusion dynamics underlie unique morphological changes in mitochondria during hypoxia–reoxygenation stress. Cell Death and Differentiation 18: 1561-1572 Lu CA, Lin CC, Lee KW, Chen JL, Huang LF, Ho SL, Liu HJ, Hsing YI, Yu SM (2007) The SnRK1A protein kinase plays a key role in sugar signaling during germination and seedling growth of rice. The Plant Cell 19: 2484-2499 Magneschi L, Perata P (2009) Rice germination and seedling growth in the absence of oxygen. Annals of Botany 103: 181-196 Menegus F, Cattaruzza L, Chersi A, Fronza G (1989) Differences in the anaerobic lactate-succinate production and in the changes of cell sap pH for plants with high and low resistance to anoxia. Plant Physiology 90: 29-32 Menegus F, Cattaruzza L, Mattana M, Beffagna N, Ragg E (1991) Response to anoxia in rice and wheat seedlings. Changes in pH of intracellular components, glucose-6-phosphate level, and metabolic rate. Plant Physiology 95: 760-767 Millar AH, Trend AE, Heazlewood JL (2004) Changes in the mitochondrial proteome during the anoxia to air transition in rice focus around cytochrome-containing respiratory complexes. The Journal of Biological Chemistry 279: 39471-39478 Miyashita Y, Dolferus R, Ismond KP, Good AG (2007) Alanine aminotransferase catalyses the breakdown of alanine after hypoxia in Arabidopsis thaliana. The Plant Journal 49: 1108-1121 Miyashita Y, Good AG (2008) Contribution of the GABA shunt to hypoxia-induced alanine accumulation in roots of Arabidopsis thaliana. Plant & Cell Physiology 49: 92-102 Mujer CV, Rumpho ME, Lin JJ, Kennedy RA (1993) Constitutive and Inducible Aerobic and Anaerobic Stress Proteins in the Echinochloa Complex and Rice. Plant Physiol 101: 217-226 Mustroph A, Albrecht G (2003) Tolerance of crop plants to oxygen deficiency stress: fermentative activity and photosynthetic capacity of entire seedlings under hypoxia and anoxia. Physiologia Plantarum 117: 508-520 Mustroph A, Boamfa EI, Laarhoven LJ, Harren FJ, Albrecht G, Grimm B (2006) Organ-specific analysis of the anaerobic primary metabolism in rice and wheat seedlings. I: Dark ethanol production is dominated by the shoots. Planta 225: 103-114

Page 58: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

46

Mustroph A, Boamfa EI, Laarhoven LJJ, Harren FJM, Pors Y, Grimm B (2006) Organ specific analysis of the anaerobic primary metabolism in rice and wheat seedlings II: light exposure reduces needs for fermentation and extends survival during anaerobiosis. Planta 225: 139-152 Mustroph A, Lee SC, Oosumi T, Zanetti ME, Yang H, Ma K, Yaghoubi-Masihi A, Fukao T, Bailey-Serres J (2010) Cross-Kingdom comparison of transcriptomic adjustments to low-oxygen stress highlights conserved and plant-specific responses. Plant Physiology 152: 1484-1500 Nagata I, Furuya E, Yoshida Y, Kanaseki T, Tagawa K (1975) Development of Mitochondrial Membranes in Anaerobically Grown Yeast Cells. The Journal of Biochemistry 78: 1353-1364 Narsai R, Howell KA, Carroll A, Ivanova A, Millar AH, Whelan J (2009) Defining core metabolic and transcriptomic responses to oxygen availability in rice embryos and young seedlings. Plant Physiology 151: 306-322 Narsai R, Rocha M, Geigenberger P, Whelan J, Van Dongen JT (2011) Comparative analysis between plant species of transcriptional and metabolic responses to hypoxia. New Phytologist 190: 472-487 Narsai R, Whelan J (2013) How unique is the low oxygen response? An analysis of the anaerobic response during germination and comparison with abiotic stress in rice and Arabidopsis. Frontiers in Plant Science 4: 349-362 Neljubov D (1901) Ueber die horizontale Nutation der Stengel vonPisum sativum und einiger anderen. . Pflanzen Beih Bot Zentralbl10: 128-139 Nishizawa K, Komatsu S (2011) Characteristics of soybean 1-Cys peroxiredoxin and its behavior in seedlings under flooding stress. Plant Biotechnology 28: 83-88 Noctor G, Foyer CH (1998) Ascorbate and glutathione: keeping active oxygen under control. Annual Review of Plant Physiology and Plant Molecular Biology 49: 249-279 Oliveira L (1977) Changes in the ultrastructure of mitochondria of roots of Triticale subjected to anaerobiosis. Protoplasma 91: 267-280 Park M, Yim HK, Park HG, Lim J, Kim SH, Hwang YS (2010) Interference with oxidative phosphorylation enhances anoxic expression of rice alpha-amylase genes through abolishing sugar regulation. Journal of Experimental Botany 61: 3235-3244 Perata P, Pozueta-Romero J, Akazawa T, Yamaguchi I (1992) Effect of anoxia on starch breakdown in rice and wheat seeds. Planta 188: 611-618 Planchet E, Gupta KJ, Sonoda M, Kaiser WM (2005) Nitric oxide emission from tobacco leaves and cell suspensions: rate limiting factors and evidence for the involvement of mitochondrial electron transport. The Plant Journal 41: 732-743 Reggiani R, Cantu CA, Brambilla I, Bertani A (1988) Accumulation and interconversion of amino acids in rice roots under anoxia. Plant and Cell Physiology 29: 981-987 Reggiani R, Hochkoeppler A, Bertani A (1989) Polyamines in Rice Seedlings under Oxygen-Deficit Stress. Plant physiology 91: 1197-1201

Page 59: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

47

Reggiani R, Mattana M, Aurisano N, Bertani A (1993) Utilization of stored nitrate during the anaerobic germination of rice seeds. Plant & cell physiology 34: 379-383 Reggiani R, Nebuloni M, Mattana M, Brambilla I (2000) Anaerobic accumulation of amino acids in rice roots: role of the glutamine synthetase/glutamate synthase cycle. Amino Acids 18: 207-217 Ricard B, Rivoal J, Spiteri A, Pradet A (1991) Anaerobic stress induces the transcription and translation of sucrose synthase in rice. Plant Physiology 95: 669-674 Roberts JKM, Hooks MA, Miaullis AP, Edwards S, Webster C (1992) Contribution of malate and amino acid metabolism to cytoplasmic pH regulation in hypoxic maize root tips studied using nuclear magnetic resonance spectroscopy. Plant Physiology 98: 480-487 Rocha M, Licausi F, Araújo WL, Nunes-Nesi A, Sodek L, Fernie AR, van Dongen JT (2010) Glycolysis and the tricarboxylic acid cycle are linked by alanine aminotransferase during hypoxia Induced by waterlogging of Lotus japonicus. Plant Physiology 152: 1501-1513 Rocha M, Sodek L, Licausi F, Hameed MW, Dornelas MC, van Dongen JT (2010) Analysis of alanine aminotransferase in various organs of soybean (Glycine max) and in dependence of different nitrogen fertilisers during hypoxic stress. Amino Acids 39: 1043-1053 Rumpho ME, Kennedy RA (1983) Anaerobiosis in Echinochloa crus-galli (barnyard grass) seedlings: Intermediary metabolism and ethanol tolerance. Plant Physiology 72: 44-49 Sadiq I, Fanucchi F, Paparelli E, Alpi A, Bachi A, A. A, Perata P (2011) Proteomic identification of differentially expressed proteins in the anoxic rice coleoptile. Journal of Plant Physiology 168: 2234-2243 Salavati A, Khatoon A, Nanjo Y, Komatsu S (2012) Analysis of proteomic changes in roots of soybean seedlings during recovery after flooding. J Proteomics 75: 878-893 Schaub MC, Lucchinetti E, Zaugg M (2009) Genomics, transcriptomics, and proteomics of the ischemic heart. Heart Metabolism 42: 4-9 Shingaki-Wells RN, Huang S, Taylor NL, Carroll AJ, Zhou W, Millar AH (2011) Differential molecular responses of rice and wheat coleoptiles to anoxia reveal novel metabolic adaptations in amino acid metabolism for tissue tolerance. Plant Physiology 156: 1706-1724 Stoimenova M, Igamberdiev AU, Gupta KJ, Hill RD (2007) Nitrite-driven anaerobic ATP synthesis in barley and rice root mitochondria. Planta 226: 465-474 Taylor E, Nie X, MacGregor A, Hill R (1994) A cereal haemoglobin gene is expressed in seed and root tissues under anaerobic conditions. Plant Molecular Biology 24: 853-862 Taylor NL, Howell KA, Heazlewood JL, Tan TY, Narsai R, Huang S, Whelan J, Millar AH (2010) Analysis of the rice mitochondrial carrier family reveals anaerobic accumulation of a basic amino acid carrier involved in arginine metabolism during seed germination. Plant physiology 154: 691-704

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48

Tsuji H, Meguro N, Suzuki Y, Tsutsumi N, Hirai A, Nakazono M (2003) Induction of mitochondrial aldehyde dehydrogenase by submergence facilitates oxidation of acetaldehyde during re-aeration in rice. FEBS Letters 546: 369-373 Ueda K, Tsuji H (1971) Ultrastructural changes of organelles in coleoptile cells during anaerobic germination of rice seeds. Protoplasma 73: 203-215 Vartapetian BB, Andreeva IN, Kozlova GI (1976) The resistance to anoxia and the mitchondrial fine structure of rice seedlings. Protoplasma 88: 215-224 Vartapetian BB, Zakhmylova NA, Generozova IP (1985) Ultrastructure of wheat coleoptile mitochondria at short-term anoxia and post-anoxia. Plant Cell and Environment 8: 65-67 Voesenek LACJ, Colmer TD, Pierik R, Millenaar FF, Peeters AJM (2006) How plants cope with complete submergence. New Phytologist 170: 213-226 Voesenek LACJ, Sasidharan R (2013) Ethylene – and oxygen signalling – drive plant survival during flooding. Plant Biology 15: 426-435 Waters I, Morrell S, Greenway H, Colmer TD (1991) Effects of anoxia on wheat seedlings. II Effect of O2 supply prior to anoxia on tolerance to anoxia, alcoholic fermentation, and sugar levels. Journal of Experimental Botany 42: 1437-1447 Wollenweber-Ratzer B, Crawford CMM (1994) Enzymatic defence against post anoxic injury in higher plants. Proceedings of the Royal Society of Edinburgh 102B: 381-390 Wylezich C, Karpov SA, Mylnikov AP, Anderson R, Jurgens K (2012) Ecologically relevant choanoflagellates collected from hypoxic water masses of the Baltic Sea have untypical mitochondrial cristae. BMC Microbiology 12: 271-283 Xu K, Xu X, Fukao T, Canlas P, Maghirang-Rodriguez R, Hueer S, Ismail AM, Bailey-Serres J, Ronald PC, Mackill DJ (2006) Sub1A is an ethylene-response-factor-like gene that confers submergence tolerance to rice. Nature 442: 705-708 Zabalza A, Van Dongen JT, Froehlich A, Oliver SN, Faix B, Gupta KJ, Schmalzlin E, Igal M, Orcaray L, Royuela M, Geigenberger P (2009) Regulation of respiration and fermentation to control the plant internal oxygen concentration. Plant Physiology 149: 1087-1098 Zhang J, Li J, Wang X, Chen J (2011) OVP1, a vacuolar H+-translocating inorganic pyrophosphatase (V-PPase), overexpression improved rice cold tolerance Plant Physiology and Biochemistry 49: 33-38

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Chapter 2 Rice and wheat responses to anoxia

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Foreword to Study I

The first study of this thesis aimed to characterise the physiological, proteomic

and metabolomic responses of rice and wheat coleoptiles to anoxia. Since

rice has historically been cultivated in flooded, anaerobic soils, many rice

cultivars are anoxia tolerant to the extent that they can germinate under

complete oxygen deprivation. In contrast, wheat is typically a dry-land, winter

crop, rendering it relatively anoxia intolerant.

Coleoptiles were chosen as the sample of interest, since anaerobically

germinated rice fails to develop any other tissue. Since wheat does not

germinate without oxygen, we used several treatment regimes. For rice, we

used anoxic germination, as well as aerobic germination and growth, followed

by a one-day anoxic shock. For wheat, only the latter treatment was used.

Study I provided a multi-faceted understanding of the molecular responses

these species exhibit when treated with anoxia. At the protein level, rice had a

strong response to anoxia, in stark contrast to wheat. At the metabolite level,

anoxic amino acid metabolism appeared to strongly contrast between the two

species, corroborating the response differences seen in the proteomics

analysis. Consequently, it was hypothesised that interfering with wheat amino

acid metabolism would affect fitness outcomes. In the absence of genetic

mutants, seedlings were supplemented with a few key amino acids that

showed inter-species response differences. Using a measure for cell integrity,

wheat coleoptiles, unlike rice coleoptiles, appeared to benefit from amino acid

supplementation. Thus, the results of Study I provide a basis for further

investigation of the benefits of amino acid accumulation under anoxia.

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Differential Molecular Responses of Rice and WheatColeoptiles to Anoxia Reveal Novel MetabolicAdaptations in Amino Acid Metabolism forTissue Tolerance1[W][OA]

Rachel N. Shingaki-Wells, Shaobai Huang, Nicolas L. Taylor, Adam J. Carroll,Wenxu Zhou, and A. Harvey Millar*

Australian Research Council Centre of Excellence for Plant Energy Biology (R.N.S.-W., S.H., N.L.T., W.Z.,A.H.M.), Centre for Comparative Analysis of Biomolecular Networks (R.N.S.-W., S.H., N.L.T., A.H.M.), andCentre of Excellence for Plant Metabolomics (W.Z.), University of Western Australia, Crawley, WesternAustralia 6009, Australia; and Australian Research Council Centre of Excellence for Plant Energy Biology,Australian National University, Canberra, Australian Capital Territory 2601, Australia (A.J.C.)

Rice (Oryza sativa) and wheat (Triticum aestivum) are the most important starch crops in world agriculture. While bothgerminate with an anatomically similar coleoptile, this tissue defines the early anoxia tolerance of rice and the anoxiaintolerance of wheat seedlings. We combined protein and metabolite profiling analysis to compare the differences in responseto anoxia between the rice and wheat coleoptiles. Rice coleoptiles responded to anoxia dramatically, not only at the level ofprotein synthesis but also at the level of altered metabolite pools, while the wheat response to anoxia was slight in comparison.We found significant increases in the abundance of proteins in rice coleoptiles related to protein translation and antioxidantdefense and an accumulation of a set of enzymes involved in serine, glycine, and alanine biosynthesis from glyceraldehyde-3-phosphate or pyruvate, which correlates with an observed accumulation of these amino acids in anoxic rice. We show a positiveeffect on wheat root anoxia tolerance by exogenous addition of these amino acids, indicating that their synthesis could be linkedto rice anoxia tolerance. The potential role of amino acid biosynthesis contributing to anoxia tolerance in cells is discussed.

Rice (Oryza sativa) and wheat (Triticum aestivum) areeconomically important crops that are adversely af-fected by multiple environmental stresses. Both thesemonocotyledon grasses operate similar central meta-bolic processes yet notably differ in aspects of theirdevelopment and anatomy as well as in their optimalgrowth conditions: rice is typically cultivated in trop-ical regions on flooded/anaerobic soils, whereas wheatis almost exclusively a dry-land winter crop (Nagai andMakino, 2009). Despite these differences, their criticalrole as the main source of nutrition for humanity

makes the comparative study of these crops underyield-reducing stresses important. Furthermore, thestudy of two species, as opposed to two cultivars of thesame species, may be useful in highlighting mecha-nisms of anoxia adaptation in plants differing in thecontexts of their domestication. Rice is an ideal modelspecies for elucidating the mechanisms of anoxia toler-ance in plants; its full genome sequence is available (Yuet al., 2002), it can survive under prolonged anoxia, andit can even display elongation of its coleoptiles underanoxic conditions (Menegus et al., 1991; Perata et al.,1997). A critical aspect of rice anoxia tolerance is theinduction of the starch-degrading enzyme a-amylaseunder anoxia, providing a continuing supply of sub-strates for metabolism (Perata et al., 1992). Rice growthunder anoxia is largely restricted to the coleoptile,with root and leaf development halted in the absenceof oxygen (Opik, 1973). From an evolutionary perspec-tive, successful coleoptile growth under anoxia pro-vides rice seedlings with the opportunity to reach moreair-saturated conditions above anaerobic mud or stand-ing water (Kordan, 1974), thus increasing the chance ofsurvival. In some regions of the world, wheat also en-counters waterlogging, causing oxygen deficiency, butunlike rice, this normally leads to major or even totalyield losses (Setter and Waters, 2003). Compared withrice seedlings, wheat seedlings are widely consideredto be anoxia intolerant, despite possessing an anatom-

1 This work was supported by the Grains Research and Devel-opment Corporation and an Australian Postgraduate Award Ph.D.scholarship (to R.N.S.-W.), by a University of Western AustraliaResearch Development Award (to S.H.), by the Australian ResearchCouncil through the Australian Research Council Centre of Excel-lence in Plant Energy Biology (grant no. CE0561495), and by anAustralian Research Council Australian Professorial Fellowship (toA.H.M.).

* Corresponding author; e-mail [email protected] author responsible for distribution of materials integral to the

findings presented in this article in accordance with the policydescribed in the Instructions for Authors (www.plantphysiol.org) is:A. Harvey Millar ([email protected]).

[W] The online version of this article contains Web-only data.[OA] Open Access articles can be viewed online without a sub-

scription.www.plantphysiol.org/cgi/doi/10.1104/pp.111.175570

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ically similar coleoptile tissue under normal growthconditions (Menegus et al., 1991). Although wheatseeds are starchy like rice, they cannot germinate andgrow a coleoptile under anoxia due to an absence ofthe starch-degrading enzyme a-amylase in anaerobicseeds (Perata et al., 1992).Without oxygen, the glycolytic pathway that is linked

with ethanolic fermentation is the predominant mech-anism of energy production in plants (Gibbs et al., 2000;Bailey-Serres and Voesenek, 2008). However, there isstill much less energy production during anoxia thanin aeration per unit of carbohydrate metabolized. As aconsequence, the synthesis rate of macromoleculessuch as proteins decreases well below that seen inaerated tissues (Alpi and Beevers, 1983). Even so, ricecoleoptiles still exhibit a complex pattern of newlysynthesized proteins under anoxia (Mocquot et al.,1981; Ricard and Pradet, 1989; Huang et al., 2005).Along with the classical anaerobic proteins first re-ported in maize (Zea mays; Sachs et al., 1996), anoxicrice coleoptiles also synthesize a range of proteins withunknown functions (Huang et al., 2005). To date, theidentified anoxically synthesized protein data set in ricedoes not form complete biochemical pathways (Ricardet al., 1991; Huang et al., 2005). Evidently missing fromthis set are a range of enzymes in glycolysis and theenzymes that could explain the observed amino acidaccumulation in rice coleoptiles under anoxia (Fanet al., 1997; Kato-Noguchi and Ohashi, 2006). It remainsunclear whether these dramatically induced amino acidpools are derived from specific protein degradationunder anoxia or de novo amino acid synthesis. Withthe improved techniques in protein identification us-ing peptide mass spectrometry, it is feasible to analyzeproteins on a large scale using combinations of gel-based or non-gel-basedmethods to address these issuesand provide an in-depth understanding of the mech-anism(s) of anoxia tolerance. Direct comparisons ofproteome responses that occur during anoxia in toler-ant rice coleoptiles and intolerant wheat coleoptilesalso provide an opportunity to differentiate proteomechanges under anoxia associated with cellular stressand damage from those associated with continuedgrowth and adaptation.At the metabolite level, the accumulation of fermen-

tation end products such as ethanol, lactate, and Alahas been extensively studied in plants responding tooxygen deprivation (Raymond et al., 1985; Meneguset al., 1989, 1991; Gibbs and Greenway, 2003). A recentmetabolomic analysis of Lotus japonicus suggests thatthe accumulation of succinate and Ala under lowoxygen might function to generate ATP that is addi-tional to what the glycolytic pathway offers (Rochaet al., 2010). In rice coleoptiles, the anaerobic assimila-tion of inorganic nitrogen into amino acids, particularlyAla and g-aminobutyrate/Glu, may serve to supple-ment ethanolic fermentation in sustaining glycolyticenergy production (Fan et al., 1997). There are alsoseveral studies that report changes of carbohydrates(Suc, Glc, Fru) and sugar phosphates in coleoptiles and

shoots (composed of both leaves and coleoptiles) ofrice seedlings in response to anoxia (Menegus et al.,1991; Guglielminetti et al., 1995; Huang et al., 2003). Ananalysis of the early germination stages of rice embryosat the metabolite level highlighted sets of 10 and 13metabolites, respectively, as aerobic and anaerobic re-sponders (Narsai et al., 2009). However, a broad pic-ture of the changes of metabolites in the anoxic ricecoleoptile itself remains unclear, and measuring only afew compounds, as has been reported in most of theearlier studies (Menegus et al., 1989, 1991), makes it hardto understand the flow of both carbon and nitrogen be-tweenmetabolic pools under anoxia. Furthermore, thereare no reported studies on how wheat coleoptiles re-spond to anoxia across a broad set of metabolite pools.

In this study, we combined protein and metabolite-profiling analyses to compare the differences in responseto anoxia between anoxia-tolerant rice coleoptiles andanoxia-intolerant wheat coleoptiles. Rice coleoptiles,but not wheat coleoptiles, responded to anoxia dra-matically, not only at the level of new protein synthesisbut also at the level of altered metabolite pools. Wealso found significant increases in anoxic rice coleop-tile proteins related to protein translation, such as 40Sribosomal proteins and elongation factors. The possi-bility of selected mRNA translation and protein turn-over in anoxic rice coleoptiles, but not in anoxic wheatcoleoptiles, which are remarkably unchanged, is dis-cussed in light of the observed low correlation betweenprotein abundance and reported gene expression data.A set of enzymes that increased in abundance in anoxicrice, a change that was not apparent in wheat, are in-volved in Ser, Gly, and Ala biosynthesis from glyco-lytic metabolites. This correlates with the observedaccumulation of these amino acids in anoxic rice cole-optiles. The potential role of amino acid biosynthesiscontributing to anoxia tolerance is discussed, and weshow a positive effect on tolerance upon exogenoussupplementation of these amino acids in wheat butnot in rice.

RESULTS

Physiological Analyses Highlight Differences betweenResponses of Rice and Wheat Seedlings to Anoxia

Germination of the rice and wheat seeds used in thisstudy under anoxic conditions replicated widely re-ported differences that rice can germinate and grow itscoleoptile under anoxia while wheat seeds fail to ger-minate under similar conditions (Alpi and Beevers,1983; Supplemental Fig. S1A). We compared rice cole-optiles from seedlings germinated and grown underanoxia for 6 d with those under aeration for 4 d tocharacterize rice metabolism under prolonged anoxia.Rice coleoptiles from seedlings grown under aerationfor 4 d followed by a 1-d switch to anoxia were alsostudied. This allowed a comparison to be made be-tween prolonged protein changes from germination

Rice and Wheat Anoxia Responses

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and more rapid changes associated with the loss ofoxygen from aerobic tissue. The treatment involving aswitch to anoxia also generated a data set comparableto publicly available microarray data characterizingcoleoptiles from 4-d-old anoxically germinated riceseedlings (Lasanthi-Kudahettige et al., 2007). As theyare unable to germinate under anoxia, we were con-strained to studying wheat seedlings that were germi-nated and grown under aeration for 4 d and thenswitched to 1 d of anoxia. By using the Evans blue vi-ability stain, a distinction in the anoxia tolerance of riceand wheat was confirmed in that the viability of ricerootswasmuch greater than that of wheat after a switchfrom aeration to anoxia (Supplemental Fig. S1B).

Detailed study of the 24-h anoxic response in riceandwheat coleoptiles was performed tracking growth,sugar content, and metabolic activities (Table I). Thisshowed that aerobically grown rice coleoptiles, but notwheat coleoptiles, displayed significant elongation after1 d of anoxia (Table I). Sugars are the primary carbonsource for energy production via glycolysis and etha-nolic fermentation. The sugar content of rice coleoptilesunder anoxia for 6 d was considerably lower than thatmeasured in 4-d-old aerobic coleoptiles (Table I). Thesugar content of coleoptiles, leaves, and roots of bothrice and wheat seedlings was also significantly lowereven after a 1-d switch from aeration to anoxia (Table I).Induction of alcohol dehydrogenase (ADH) is a keystep in the switch to anaerobic energy production, forit is ethanolic fermentation that regenerates NAD+, anoxidant necessary for the continuation of glycolysis. Inboth anoxic rice and wheat coleoptiles, ADH activitywas induced compared with the aerated control (Table

I). However the apparent inducibility of ADH activityduring anoxia was greater in coleoptiles of rice (3.4-fold) than those of wheat (2.4-fold; Table I). The highestADH activity recorded was observed in rice coleoptilesafter 6 d under anoxia (Table I). In the leaves and rootsof both rice and wheat seedlings, ADH activities werealso induced by anoxia, but the final specific activity ofADH was 5- to 10-fold higher in rice than in wheat(Table I).

The 6-d-old anoxic rice coleoptiles were shorter thanthose from seedlings germinated and grown underaeration for 4 d (Table I). This contrasts with previousreports that rice coleoptiles grown under anoxia weremuch longer than aerated ones (Atwell et al., 1982; Alpiand Beevers, 1983). The explanation for this differencecould be the different cultivars used or the use of N2bubbling as a means to achieve anoxia, rather than thestagnant conditions used in other studies (Magneschiet al., 2009). Bubbling removes other gases such as CO2and even ethylene produced by coleoptiles if traceamounts of oxygen are available, reducing the com-plexity of comparing anoxic and aerated conditions.

We also monitored the capacity for mitochondrialrespiratory function by measuring tissue oxygen con-sumption rate. The rate of oxygen consumption incoleoptiles from seedlings continuously grown underanoxia, but returned to aeration for the measurements,was significantly less than that of continuously aeratedcoleoptiles (Table I). This is consistent with the needfor oxygen for the biosynthesis of heme groups for thecytochromes of the plant respiratory chain (Millaret al., 2004). The oxygen consumption rate capacityin roots and leaves from rice and wheat seedlings was

Table I. Growth, sugar concentration, oxygen consumption rate, and ADH activity of coleoptiles from rice and wheat seedlings exposed toaeration or anoxia

Rice seeds were germinated and grown under aeration for 4 d (control), anoxia for 6 d (anoxically germinated; 6 d N2), or subsequently switchedto 1 d of anoxia (anoxically switched; 4 d air + 1 d N2) or 1 d of air (aerobically switched; 6 d N2 + 1 d air). Wheat seeds were treated withcontrol conditions or were anoxically switched.

Parameters TreatmentsRice Wheat

Coleoptiles Leaves Roots Coleoptiles Leaves Roots

Growth (mm) 4 d air 11.9 6 0.9 – – 28.1 6 2.7 – –4 d air + 1 d N2 14.2 6 1.0a – – 26.2 6 1.5 – –

6 d N2 7.1 6 0.7a – – – – –6 d N2 + 1 d air 9.7 6 0.7b – – – – –

Sugar concentration(mg hexose g21

4 d air 44.8 6 1.4 55.8 6 2.1 28.0 6 2.8 37.0 6 0.7 64.9 6 2.5 12.4 6 1.24 d air + 1 d N2 21.6 6 0.9a 31.3 6 0.7a 13.5 6 0.7a 26.4 6 1.2a 40.4 6 1.0a 3.4 6 0.3a

fresh wt) 6 d N2 3.5 6 0.2a – – – – –6 d N2 + 1 d air 7.7 6 1.1b – – – – –

Oxygen consumptionrate (nmol min21

4 d air 126.3 6 5.1 302.2 6 10.8 398.8 6 20.2 140.6 6 6.0 478.8 6 36.2 436.8 6 14.44 d air + 1 d N2 104.7 6 2.8a 132.7 6 20.0a 82.1 6 1.2a 146.1 6 8.9 336.7 6 10.1 177.3 6 1.0a

g21 fresh wt) 6 d N2 67.4 6 6.0a – – – – –6 d N2 + 1 d air 134.0 6 11.8b – – – – –

ADH activity (unitsmg21 protein)

4 d air 0.75 6 0.06 0.94 6 0.07 0.94 6 0.05 0.25 6 0.01 0.09 6 0.01 0.32 6 0.024 d air + 1 d N2 2.68 6 0.13a 3.42 6 0.04a 5.22 6 0.70a 0.59 6 0.01a 0.28 6 0.01a 1.08 6 0.01a

6 d N2 6.61 6 0.48a – – – – –6 d N2 + 1 d air 4.38 6 0.24b – – – – –

aThe value of continuously anoxic/anoxically switched samples is P , 0.05 when compared with continuously aerated samples. bThe value ofaerobically switched samples is P , 0.05 when compared with continuously anoxic samples.

Shingaki-Wells et al.

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significantly lowered by 1 d of anoxia (Table I), indi-cating tissue adaptation to anoxia and/or damage orloss of mitochondrial function. Interestingly, this effectwas more dramatic in rice than in wheat tissues. Incomparison, the respiratory capacity of wheat coleop-tiles was not significantly affected by 1 d of anoxia andin rice the reduction was significant yet slight (Table I),suggesting minimal mitochondrial damage occurredduring this period of anoxia and the immediate abilityof mitochondrial function to return upon the aerationrequired for the measurements to be carried out. Inconclusion, rice coleoptiles grown continuously underanoxia or aeration had significant differences in all theparameters investigated. When switched from aeratedto anoxic conditions, coleoptiles of rice responded toanoxia to a greater degree than those of wheat. Incomparison, leaves and roots of rice and wheat seed-lings responded to anoxia similarly in all parametersinvestigated, distinct from the coleoptile response inboth species, and despite the longer term differencesnoted from Evans blue viability staining of roots (Sup-plemental Fig. S1B).

Quantitative Proteomic Analysis of Coleoptiles Shows a

Significant Rice Response But a Minimal WheatResponse to Anoxia

A number of molecular responses that underlie thedifferences noted in Table I have been investigated inpublished reports (Menegus et al., 1991; Perata et al.,1992). There are also a number of studies on global geneexpression in response to anoxia or oxygen deficiencyin plants including rice (Lasanthi-Kudahettige et al.,2007; Narsai et al., 2009) and Arabidopsis (Arabidopsisthaliana; Klok et al., 2002; Branco-Price et al., 2005; Liuet al., 2005; Loreti et al., 2005; Mustroph et al., 2010).But so far, information on the changes of protein abun-dance in response to anoxia is limited (Mocquot et al.,1981; Ricard and Pradet, 1989; Huang et al., 2005). Be-cause there were such dramatic differences at thephysiological level between 4-d aerated and 6-d anoxiccoleoptiles (Table I), we started analyzing differencesin protein profiles using differential in-gel electropho-resis (DIGE), which is based on staining protein sam-ples with different fluorescent dyes (Fig. 1A). Out of1,259 protein spots detected on isoelectric focusing(IEF)/SDS-PAGE gels (pI range, 3–10), 164 (13%) pro-tein spots met the criteria of significant 2-fold differ-ences in protein abundance on three replicate gels (P,0.05). A total of 107 of these protein spots were moreabundant under anoxia and 57 were more abundantunder aeration (Fig. 1A). This suggested a significantdifference in the protein profiles of samples from 6-danoxic and 4-d aerated rice coleoptiles. We also com-pared rice coleoptiles from 4-d aerated seedlings withthose grown in the same control conditions butswitched to an additional 1 d of anoxia (Fig. 1B). Therewere 1,245 protein spots detected, and 67 (5%) of thesemet the above-mentioned significance criteria (Fig. 1B).Eighty-five percent of these changing protein spots

were more abundant in coleoptiles subjected to theanoxic switch (Fig. 1B), suggesting a rapid 24-h re-sponse to anoxia at the protein level. This is in agree-ment with the results of van Dongen and colleagues(2009), who reported a tendency for gene expression toincrease in response to 0.5 to 48 h of hypoxia as opposedto cessation of transcription in roots of Arabidopsisseedlings. We then compared coleoptile proteomes ofwheat using the same anoxic-switch experimental setupused in rice (Fig. 1C). According to the same significancecriteria, only five (0.4%) of the 1,245 protein spots de-tected differed in abundance between the two treat-ments (Fig. 1C), suggesting a very limited response toanoxia at the protein level in wheat coleoptiles.

We then conducted two additional independentanalyses to further quantify the difference between4-d aerated and 6-d anoxic coleoptiles in order toovercome limitations of the pH 3 to 10 nonlinear (3-10NL) DIGE analysis. We used a broader pH range toshow more basic protein spots in a DIGE analysis(using pI 3–11 gels) and a non-gel-based iTRAQ (forisobaric tag for relative and absolute quantitation)experiment to remove the bias against protein size andsolubility that is inherent to IEF-based analysis. Out ofthe 1,007 spots detected in the pI 3 to 11 DIGE, 140(13.9%) spots met the criteria of significance. Forty-sixof these prospective proteins were more abundantunder anoxia and 94 were more abundant under aer-ation (Supplemental Figs. S2 and S4). Using iTRAQanalysis, we identified 142 proteins, 126 of whichcould be quantified in a three-biological-replicate ex-periment comparing coleoptile proteomes extractedfrom 6-d anoxic and 4-d aerated rice seedlings (Sup-plemental Table S1). Among them, 34 were signifi-cantly more abundant under anoxia and 29 weresignificantly more abundant under aeration (Supple-mental Fig. S2). The fold differences in protein abun-dance as revealed by iTRAQ were proportional tothose revealed by the DIGE analysis, with the r2 being0.61 (Supplemental Fig. S3A). However, the DIGE anal-ysis resolved much larger fold differences between thetwo treatments than those calculated in the iTRAQanalysis (Supplemental Fig. S3A). For example, accord-ing to the DIGE analysis, peroxiredoxin (Os07g44430.1)was reported to be 3.38- to 22.69-fold more abundantin 6-d anoxic rice coleoptiles than in the 4-d aeratedcontrol, whereas this difference was only 2.48-foldaccording to the iTRAQ analysis (Table II). Similardiscrepancies between the linearity of responses by thetwomethods have been previously reported (Wu et al.,2006).

Identified Proteins in Rice Coleoptiles with Changes inAbundance under Anoxia

The identified proteins with significant changes inabundance between aerated and anoxic treatments arelisted in Table II. The protein identification evidencefrom all protein analysis is shown in SupplementalTable S1, and further details for iTRAQ data analysis

Rice and Wheat Anoxia Responses

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are provided in Supplemental Table S2. We have incor-porated microarray data (4-d-old anoxic and 4-d-oldaerobic rice coleoptiles from Lasanthi-Kudahettigeet al. [2007]) into Table II and Supplemental Table S1for further comparison. The enzymes detected, whichare involved in glycolysis, fermentation, and aminoacid biosynthesis, were also incorporated into a metab-olite pathway map in Figure 2. We could not identifythe five protein spots that were significantly differentbetween treatments in wheat coleoptiles due to theirvery low abundance on gels.

Enzymes Involved in Glycolysis andEthanolic Fermentation

We identified the accumulation of enzymes involvedin ethanolic fermentation such as ADH1 (Os11g10480)and pyruvate decarboxylase 1 (Os05g39310) in anoxic

rice coleoptiles (Table II; Fig. 2), consistent with pub-lished reports (Mocquot et al., 1981; Ricard and Pradet,1989; Bailey-Serres and Chang, 2005; Huang et al., 2005;van Dongen et al., 2009). Proteins significantly in-creasing in abundance and involved in multiple stepsof glycolysis were also identified and listed in Table IIand Figure 2. Those enzymes were pyrophosphate (PPi)-Fru-6-P 1-phosphotransferase b-subunit (Os06g13810),Fru-bisP aldolase (Os05g33380, Os01g67860, Os10g08022),triosephosphate isomerase (Os01g05490), glyceraldehyde-3-phosphate dehydrogenase (Os04g40950, Os02g38920,Os08g03290), phosphoglycerate kinase (Os02g07260),phosphoglucomutase (Os03g50480), 2,3-bisphospho-glycerate-independent phosphoglycerate mutase(Os01g60190), and enolase (Os10g08550; Table II; Fig.2). Exceptions to these anoxia increases were fructoki-nase 2 (Os08g02120), which was observed to decreasein abundance under anoxia, as well as discrepancies in

Figure 1. DIGE on two-dimensional IEF/SDS gels. A and B, Comparisons were made between coleoptile proteomes of riceseedlings treated with 4 d of aeration versus 6 d of anoxia (A) as well as 4 d of aeration with an additional 1 d under anoxia (B). C,Wheat responses to anoxia were also analyzed by comparing coleoptiles from seedlings treated in the same way as in B. The toppanels are gel images of each fluorescence signal, and the bottom panel is a combined image electronically overlaid usingImageQuant TL software (GE Healthcare). Yellowish spots represent proteins of equal abundance between the two samples. Thenumbered arrows indicate proteins identified by MS (listed in Table II) with abundances that were significantly different betweentreatments (identified in all nine gel images; P , 0.05; abundance difference . 1.5). Below the DIGE image is a Venn diagramrepresenting the percentage of protein spots significantly changing in abundance between the two treatments. The percentage ofprotein spots significantly more abundant under anoxia or aeration is shown on the left or right side in each Venn diagram,respectively. The percentage of proteins that did not significantly differ in abundance is shown in the middle.

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Table II. Proteomic analysis of rice coleoptiles in response to anoxia or switch from air to anoxia

Proteins selected from DIGE corresponding to Figure 1, A and B, and iTRAQ (Supplemental Table S2) were identified by MS/MS (Protein ID) withcorresponding rice gene numbers (Os Gene No.). Details of the matched protein size, number of peptides identified, and percentage coverage areshown in Supplemental Table S1. Transcript abundance differences between anoxic (4 d) and aerated (4 d) rice coleoptiles derived from independentmicroarray data (Lasanthi-Kudahettige et al., 2007) have been incorporated (significant increase [positive, boldface], significant decrease [negative,boldface italic]). Protein spots chosen for MS/MS analysis met the following criteria in at least one analysis: a protein abundance difference of 1.5 orgreater where proteins were higher in anoxic samples (positive, boldface) and those higher in aeration (negative, boldface italic), P , 0.05, and anabundance high enough on preparative gels for subsequent MS identification. FAD, Fold abundance difference; GAPDH, glyceraldehyde-3-phosphate dehydrogenase; iPGAM, 2,3-bisphosphoglycerate-independent phosphoglycerate mutase; MetSyn, cobalamin-independent Met syn-thase; N/S, not significant; 3-PGDH, D-3-phosphoglycerate dehydrogenase; PSAT, phospho-Ser aminotransferase; S, significant; SHMT, Serhydroxymethyltransferase; Sig., significantly different from 1 or not; TGM, transformed geometric mean; X, no data.

Functional

CategoryOs Gene No. Protein ID

DIGE: 3-10NL DIGE: 3-11NL DIGE: 3-10NL iTRAQ Array

6 d N2/4 d Air 6 d N2/4 d Air 4 d Air 1 d N2/4 d Air 6 d N2/4 d Air 4 d N2/4 d Air

Spot FAD P Spot FAD P Spot FAD P TGM Sig. FAD

Sugar metabolism, Os03g28330.1 Suc synthase – X X – X X – X X 1.6 S 2

glycolysis, Os06g09450.1 Suc synthase – X X – X X – X X 1.7 S 2

fermentation, Os01g60190.1 iPGAM 31 3.3 4.E-04 20 5.7 5.E-04 27 1.3 1.E-01 21.0 N/S 2

and TCA cycle Os01g60190.1 iPGAM 32 4.3 4.E-06 21 6.1 3.E-05 26 1.5 9.E-03 21.0 N/S 2

Os10g08550.1 Enolase 33 7.5 5.E-09 18 5.7 9.E-04 28 2.4 7.E-04 1.2 S 2

Os10g08550.1 Enolase 34 2.2 3.E-05 19 2.8 2.E-03 29 1.5 8.E-04 1.2 S 2

Os08g02120.1 Fructokinase-2 – X X – X X – X X 22.2 S 22

Os05g33380.1 Aldolase 16 4.7 5.E-06 – X X 5 2.1 3.E-04 2.0 S N/S

Os01g67860.1 Aldolase – X X – X X – X X 2.2 S N/S

Os10g08022.1 Aldolase – X X – X X – X X 2.3 S X

Os04g40950.1 GAPDH 6 2.2 7.E-04 6 2.4 2.E-03 4 1.1 8.E-02 1.4 S N/S

Os04g40950.1 GAPDH 10 3.6 7.E-05 – X X 11 1.0 7.E-01 1.4 S N/S

Os04g40950.1 GAPDH – X X 8 2.6 1.E-03 – X X 1.4 S N/S

Os02g38920.1 GAPDH 18 13.2 5.E-06 – X X 9 1.7 2.E-03 1.8 S 3

Os02g38920.1 GAPDH 17 6.7 4.E-08 – X X 8 1.7 1.E-02 1.8 S 3

Os08g03290.1 GAPDH 15 2.5 6.E-04 – X X 6 1.2 4.E-02 X X N/S

Os08g03290.2 GAPDH – X X – X X – X X 1.3 S N/S

Os03g50480.1 Phosphoglucomutase 14 6.3 2.E-05 – X X 25 2.7 2.E-03 21.1 S N/S

Os02g07260.1 Phosphoglycerate kinase 28 5.3 1.E-04 – X X 31 2.4 1.E-02 1.2 S 2

Os01g05490.1 Triosephosphate isomerase 40 2.9 5.E-05 – X X 36 1.2 9.E-03 1.4 S 4 and N/S

Os06g13810.1 PPi-phosphofructokinase 23 2.8 2.E-02 – X X 19 2.1 9.E-04 1.4 S 2

Os05g39310.1 Pyruvate decarboxylase 1 – X X – X X – X X 2.0 S 594

Os11g10480.1 ADH1 12 6.0 2.E-05 – X X 12 3.6 4.E-05 2.2 S 4

Os01g46070.1 Malate dehydrogenase – X X – X X – X X 21.1 S N/S

Amino acid

synthesis

Os02g50240.1 Gln synthetase 38 22.3 7.E-05 – X X 34 21.3 3.E-04 22.3 N/S 22

Os12g42884.1 MetSyn – X X – X X – X X 21.7 S 22 and N/S

Os12g42876.1 MetSyn 25 2.3 2.E-03 – X X 17 3.3 2.E-03 21.7 S X

Os12g42876.1 MetSyn 26 1.1 6.E-01 – X X 18 2.7 3.E-03 21.7 S X

Os03g06200.1 PSAT 5 4.7 9.E-07 5 6.5 1.E-03 – X X 1.7 N/S 5

Os03g06200.1 PSAT – X X 9 5.6 1.E-03 – X X 1.7 N/S 5

Os12g22030.1 SHMT 19 1.6 9.E-02 – X X 14 2.0 4.E-04 X X N/S

Os04g55720.1 3-PGDH 24 5.8 2.E-05 – X X 20 2.0 1.E-03 1.9 S 4

Os10g25130.1 Ala aminotransferase – X X 15 2.5 4.E-03 – X X X X N/S

Stress responsive Os07g44430.1 Peroxiredoxin 4 5.5 6.E-05 4 11.0 5.E-05 – X X 2.5 S 32

Os07g44430.1 Peroxiredoxin 3 3.4 2.E-03 3 22.7 1.E-06 – X X 2.5 S 32

Os05g25850.1 Manganese-superoxide dismutase 1 1.6 1.E-02 1 1.9 1.E-02 – X X 1.4 N/S N/S

Os03g17690.1 Ascorbate peroxidase 39 24.6 3.E-06 – X X 13 22.3 1.E-04 21.8 S N/S

Os07g49400.1 Ascorbate peroxidase – X X – X X – X X 21.9 S N/S

Os03g07180.1 Embryotic protein DC-8 – X X 10 3.5 4.E-05 – X X X X X

Os03g07180.1 Embryotic protein DC-8 – X X 11 3.9 3.E-05 – X X X X X

Os03g07180.1 Embryotic protein DC-8 – X X 12 3.6 4.E-05 – X X X X X

Os03g07180.1 Embryotic protein DC-8 – X X 13 4.7 1.E-04 – X X X X X

Os05g46480.1 LEA group 3 2 4.1 7.E-07 2 7.1 2.E-04 – X X X X 22

Os02g15250.1 LEA domain containing – X X 14 5.9 8.E-05 – X X – X X

Translation Os03g14530.1 S10/S20 ribosomal protein – X X – X X – X X 1.3 S 2

Os11g29190.1 40S ribosomal protein S5 – X X – X X – X X 21.3 S 2

Os03g08010.1 Elongation factor 1-a – X X – X X – X X 1.3 S N/S

Os01g52470.1 Elongation factor – X X – X X – X X 1.4 S X

Os02g32030.1 Elongation factor – X X – X X – X X 21.1 S N/S

Miscellaneous Os08g04210.1 Protein kinase – X X – X X – X X 3.2 S 1,007

Os08g04250.1 Protein kinase – X X – X X – X X 2.3 S 248

Os08g04240.1 Protein kinase – X X – X X – X X 2.8 S 525

Os04g56430.1 CRK5 – X X – X X – X X 21.9 S 3

Os01g03340.1 BBTI4 11 26.0 2.E-06 – X X – X X 21.9 S 23 and 22

Os01g03360.1 BBTI5 – X X – X X – X X 1.1 S 22

Os03g62060.1 IAA-amino acid hydrolase 36 25.3 3.E-04 17 24.6 6.E-03 32 21.0 4.E-01 23.0 S 2271

Os05g04510.1 S-Adenosyl-Met synthetase – X X – X X – X X 21.6 S N/S

Rice and Wheat Anoxia Responses

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the direction of change for phosphoglucomutase(Os03g50480) between the DIGE and iTRAQ analyses.

We also identified two Suc synthase enzymes(Os03g28330, Os06g09450) that were significantly moreabundant in rice coleoptiles of anoxically germinatedseedlings (Table II). Our data agree with reports thatunder anoxia, there is a switch from invertase to Sucsynthase as a means of degrading Suc into sugars thatcan then enter the glycolytic pathway (Guglielminettiet al., 1995).

These observations reinforced the evidence for gen-eral enhancement of glycolysis and ethanolic fermen-tation for rice coleoptiles during adaptation to anoxiaand highlight the gene-specific identification of chang-ing proteins that would promote a Pasteur effect. Onlyabout two-thirds of the transcripts for these glycolyticproteins are transcriptionally more abundant underanoxia in rice (Lasanthi-Kudahettige et al., 2007). Butnotably, the decreased abundance of fructokinase 2 wasalso seen at the transcript level under anoxia (Table II).

Figure 2. Effect of prolonged anoxia on carbohydrate metabolism, glycolysis, fermentation, amino acid metabolism, and theTCA cycle in rice coleoptiles. Rice seeds were germinated and grown under anoxia for 6 d or aeration for 4 d. The green and redboxes represent metabolites significantly more abundant under aeration and anoxia, respectively (P , 0.05). The yellow boxesrepresent metabolites whose abundances are unchanged. Enzyme names on arrows are also colored in this fashion. The numberson the top left side of each box represent the response value (RV) of the corresponding metabolite (anoxic/aerated) in ricecoleoptiles. All data were extracted from Tables II and III. Metabolite abbreviations are as follows: DHAP, dihydroxyacetone-phosphate; GABA, g-aminobutyrate; G-3-P, glyceraldehyde-3-phosphate; PEP, phosphoenolpyruvate; 1,3-PGA, 1,3-bisphos-phoglycerate; 2-PGA, 2-phosphoglycerate; 3-PGA, 3-phosphoglycerate; SSA, succinic semialdehyde. Protein abbreviations areas follows: ADH, alcohol dehydrogenase; AlaAT, Ala aminotransferase; aldolase, Fru-bisP aldolase; FK, fructokinase; GAPDH,glyceraldehyde-3-phosphate dehydrogenase; GlnSyn, Gln synthetase; iPGAM, 2,3-bisphosphoglycerate-independent phos-phoglycerate mutase; MDH, malate dehydrogenase; MetSyn, 5-methyltetrahydropteroyltri-Glu-homo-Cys methyltransferase(cobalamin-independent Met synthase); PDC, pyruvate decarboxylase; PFK-PPi, PPi-Fru-6-P 1-phosphotransferase; 3-PGDH,D-3-phosphoglycerate dehydrogenase; PGK, phosphoglycerate kinase; PGM, phosphoglucomutase; PSAT, phospho-Ser amino-transferase; SHMT, Ser hydroxymethyltransferase; SS, Suc synthase; TPI, triosephosphate isomerase.

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Enzymes Involved in Amino Acid Metabolism

We identified several enzymes involved in the syn-thesis of Ser and Gly that increased in abundance underanoxic stress, notably, D-3-phosphoglycerate dehydro-genase (Os04g55720), phospho-Ser aminotransferase(Os03g06200), and Ser hydroxymethyltransferase(Os12g22030; Table II; Fig. 2). Ala aminotransferase 2(Os01g25130) was also more abundant in anoxic ricecoleoptiles. Gln synthetase root isozyme 3 (Os02g50240)was less abundant under anoxia when compared withaeration, and different isoforms of 5-methyltetrahy-dropteroyltri-Glu-homo-Cys methyltransferase (Metsynthase; Os12g42876 up in DIGE, Os12g42876/Os12g42884 down in iTRAQ) showed discrepancies intheir direction of change. Met generation is particu-larly interesting, as this amino acid is involved in thesynthesis of ethylene, a plant hormone involved insubmergence-induced gene expression (Fukao et al.,2006; Xu et al., 2006). With the exception of 6-d anoxiasamples that showed anoxic accumulation, Met tendedtoward a higher abundance under aerobic conditionsin rice (Table III). The enzyme involved in the firststep of ethylene production, S-adenosyl-Met synthase(Os05g04510), was also detected in our iTRAQ analy-sis (Table II). However, it was significantly less abun-dant in coleoptiles of anoxically germinated rice, anobservation in line with the oxygen dependence of theethylene biosynthetic pathway.

Enzymes or Proteins Involved in Reactive OxygenSpecies Detoxification

Reactive oxygen species (ROS) play an important rolein signaling under oxygen deficiency (Baxter-Burrellet al., 2002; Bailey-Serres and Chang, 2005). We iden-tified several proteins involved in ROS degradationthat changed in abundance. As examples, peroxire-doxin (Os07g44430) was significantly more abundantin rice coleoptiles derived from 6-d-old anoxic seed-lings than in 4-d-old aerated seedlings (Table II). Inconcordance, the transcript for this gene was 32-foldhigher in abundance in anoxic rice coleoptiles (Lasanthi-Kudahettige et al., 2007). Peroxiredoxin is an antioxidantenzyme that can reduce both hydrogen peroxide (H2O2)and alkyl hydroperoxides. In contrast, we identifiedanother H2O2-decomposing enzyme, ascorbate peroxi-dase (Os03g17690, Os07g49400), that was less abundantin anoxic coleoptiles (Table II). The Bowman-Birk-typetrypsin inhibitor (BBTI; Os01g03340) found to decreasein abundance under anoxia may have other functionsbeyond its role in proteolysis. BBTIs have been re-ported to act as monodehydroascorbate reductasesand dehydroascorbate reductases in etiolated mungbean (Vigna radiata) seedlings (Hou et al., 2000) androots of sweet potato (Ipomoea batatas; Hou and Lin,1997) and thus can be involved in the regeneration ofascorbate. These results suggest that rice coleoptilesmay use different detoxification systems under anoxia/hypoxia and reaeration from those used during con-tinual aeration. It has been reported that anoxia can

cause an increase in H2O2 in the rice root apoplast andplasma membrane (Blokhina et al., 2001), suggesting aprotective function of these antioxidant defense en-zymes in anoxic rice coleoptiles. However, we havepreviously measured markers for lipid oxidation anddemonstrated that damage was lower in anoxic cole-optiles relative to aerobic or reoxygenated coleoptiles(Millar et al., 2004), suggesting that either (1) oxidativestress under anoxia is minimal and that peroxiredoxinhas a protective role upon the return of oxygen or (2)peroxiredoxin has a function under anoxia that wehave not anticipated. The former seems more likely,given that oxygen is necessary for the formation ofROS. Interestingly, manganese-superoxide dismutasewas detected in two DIGE analyses, and althoughstatistically significant in its accumulation under 6 d ofanoxia (P , 0.05), manganese-superoxide dismutasedid not meet all of the criteria set for significance;specifically, the abundance change did not exceed 2(Table II), indicating the quantitatively differential roleof peroxiredoxin in responding to the availability ofoxygen. What is clear from the literature is that oxygendeprivation perturbs the redox status of cells, whetherit be ROS levels (Blokhina et al., 2001), oxidative damage(Blokhina et al., 1999; Millar et al., 2004), or regulationof genes and small-molecule antioxidants involved inredox regulation (Yan et al., 1996; Biemelt et al., 1998;Blokhina et al., 2000, 2003; van Dongen et al., 2009).

Proteins Involved in the Process of Translation

Selective translation of cytoplasmic mRNAs in plantsunder oxygen deficiency has been discussed (Bailey-Serres, 1999).We identified several proteins in the iTRAQanalysis involved in translation processes, which weremore abundant in 6-d-old anoxic coleoptiles relativeto the control. Those proteins were elongation factor1-a (Os03g08010), elongation factor 2 (Os01g52470),and S10/S20 domain-containing ribosomal protein(Os03g14530; Table II). Others involved in translationthat were less abundant under anoxia were 40S ribo-somal protein S5 (Os11g29190) and elongation factor(Os02g32030). Whether these abundance changes inthe translational machinery are responsible for theperturbations in the levels of glycolytic, amino acidbiosynthetic, and ROS-defense proteins is currentlyunknown.

Other Proteins of Interest

The lower abundance of indole-3-acetic acid (IAA)-amino acid hydrolase precursor (ILR1; Os03g62060)we report under anoxia can be related to a long historyof research on auxin-regulated coleoptile elongationdating back to the famous experiment of Went (1942).The IAA-amino acid hydrolase is involved in thecleavage of conjugates between IAA and amino acids(Bartel and Fink, 1995). The dramatic decrease of ILR1(Table II) could indicate that IAA is maintained in itsconjugate form under anoxia. Microarray data also

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Table III. Metabolomic analysis of rice and wheat coleoptiles in response to anoxia

Rice plants were grown under (1) 4 d of aeration, (2) 6 d of anoxia, (3) 4 d of aeration and then 4 h of anoxia, or (4) 4 d of aeration and then 1 d ofanoxia. Wheat plants were grown under all treatments except number 2. Coleoptile tissues were separated from leaves for analysis. Complex polarmetabolite extracts were taken from all tissues and analyzed by GC-MS. Raw GC-MS data processing and statistical analyses were then carried outusing MetabolomeExpress software (version 1.0; http://www.metabolome-express.org). Metabolite signal intensity ratios were calculated by dividingthe mean tissue mass- and internal standard-normalized signal intensity for each metabolite in treated samples by its corresponding value in controlsamples (RV columns). The statistical significance of each ratio was tested by Welch’s t test (P , 0.05; n = 5). Values highlighted in boldface aresignificantly more abundant in anoxic coleoptiles, whereas negative boldface italic indicates a metabolite that is more abundant under aeration, withvalues that meet a threshold for significance of P , 0.05. N/D, No data; RV, response value.

Sample Metabolite

6 d N2/4 d air 4 d Air + 1 d N2/4 d Air 4 d Air + 4 h N2/4 d Air

Rice Rice Wheat Rice Wheat

RV P RV P RV P RV P RV P

Amino acids

and polyamines

L-Pro 98.6 5.8E-06 8.7 2.5E-02 2.6 1.7E-03 0.5 4.9E-01 0.5 1.4E-01

L-Leu 43.8 1.1E-05 11.6 1.7E-03 0.6 6.6E-02 0.6 4.6E-01 0.1 6.0E-01

b-Ala 43.4 1.4E-08 0.7 2.6E-01 1.0 3.3E-03 0.9 4.4E-01 0.9 4.9E-04

L-Ala 42.6 2.3E-06 43.2 8.1E-04 0.1 6.3E-01 6.9 1.5E-03 0.5 3.5E-01

L-Glu 36.5 1.7E-06 211.7 6.9E-02 20.9 5.8E-02 239.2 7.7E-02 20.4 2.8E-01

L-Tyr 22.5 4.4E-06 21.2 4.3E-03 0.4 2.7E-01 22.3 9.6E-02 0.2 3.0E-01

2-Aminoadipic acid 17.3 6.6E-07 21.0 8.1E-02 20.1 7.4E-01 0.1 7.4E-01 20.4 1.6E-01

L-Arg 15.6 1.2E-05 20.7 2.7E-03 0.7 1.0E-01 0.0 9.6E-01 0.1 5.7E-01

L-Homo-Ser 15.5 1.9E-02 20.9 1.0E-02 0.6 3.2E-01 20.9 9.6E-02 20.2 3.2E-01

L-Ile 12.0 3.2E-05 5.2 6.6E-04 0.7 1.1E-01 0.3 4.7E-01 0.3 3.3E-01L-Lys 10.9 3.6E-05 22.0 3.1E-03 1.5 3.5E-02 21.8 1.1E-01 0.5 1.0E-01

L-Val 10.2 5.8E-07 5.5 3.4E-07 20.1 6.6E-01 20.1 8.8E-01 0.3 4.2E-01

L-Ser 9.0 5.9E-12 2.0 2.3E-03 20.8 4.4E-03 0.1 8.3E-01 20.4 4.2E-01

g-Aminobutyric acid 8.9 1.5E-08 8.1 1.2E-03 0.4 3.5E-03 2.3 1.4E-01 0.6 8.6E-04

L-Met 6.0 2.8E-02 21.9 3.9E-02 0.6 1.4E-01 2123.6 5.4E-02 20.2 4.4E-01

L-Trp 5.2 1.8E-05 4.6 1.7E-02 0.6 1.9E-01 20.4 3.5E-01 0.5 8.8E-02

L-Thr 2.4 1.1E-06 2.1 6.4E-06 0.1 4.3E-01 0.6 1.4E-01 0.5 1.2E-01

Gly 1.9 2.5E-03 3.7 1.2E-03 1.4 4.4E-03 0.6 1.9E-01 0.4 2.0E-01

L-Gln 1.8 4.6E-04 20.5 4.4E-03 21.4 9.0E-02 20.2 2.3E-01 21.5 2.0E-03

4-Hyp 1.4 1.1E-06 20.1 4.9E-01 20.1 4.9E-01 0.1 5.0E-01 20.9 2.2E-02

Orn 0.6 3.5E-03 21.3 2.8E-04 0.4 1.8E-01 210.0 4.3E-02 20.9 1.2E-01

L-Asn 20.6 4.5E-01 0.0 9.7E-01 20.2 5.9E-01 240.0 4.7E-02 0.1 6.1E-01

L-Asp 21.5 1.5E-01 216.6 2.2E-01 21.7 3.7E-02 2448.4 4.7E-02 23.2 1.2E-03

L-Phe N/D N/D 22.1 1.5E-01 0.9 5.3E-03 20.2 2.1E-01 0.4 6.6E-02

L-a-Aminobutyric acid N/D N/D 2.5 1.5E-04 22.7 2.7E-01 0.2 4.6E-01 21.2 2.4E-03

Putrescine 52.4 6.9E-08 7.9 1.1E-04 1.7 4.2E-03 0.2 5.9E-01 20.2 1.5E-01

Sugars and

glycolytic substrates

6-Phosphogluconate 9.7 1.0E-03 20.8 3.6E-01 21.6 1.1E-01 21.4 3.9E-02 21.0 1.0E-02

D-Rib 20.8 9.2E-05 21.2 9.2E-04 21.3 3.1E-03 20.5 2.9E-04 20.6 1.3E-02

Trehalose 21.0 2.3E-02 22.1 3.1E-02 21.6 3.3E-04 20.3 1.8E-01 20.9 1.9E-03D-Xyl 22.7 5.8E-06 20.5 1.4E-01 0.1 6.4E-01 0.1 2.2E-01 0.1 4.0E-01

3-Phosphoglyceric acid 18.0 1.3E-04 20.5 5.5E-01 20.2 7.6E-01 20.3 5.6E-01 20.2 1.2E-01

Suc 4.8 3.4E-04 0.7 9.3E-02 25.6 3.6E-05 20.3 1.3E-01 211.5 1.5E-03

Fru-6-P 2.9 2.9E-04 0.1 8.7E-01 20.3 2.8E-01 20.2 3.4E-01 21.2 8.8E-03

Glc-6-P 2.8 4.4E-05 20.2 6.9E-01 20.5 1.0E-01 20.1 1.7E-01 21.4 2.2E-03

D-Fru 22.4 9.9E-07 20.3 1.7E-05 20.4 3.9E-01 0.0 8.1E-01 20.4 3.8E-02

D-Glc 24.2 2.1E-05 20.4 8.8E-05 20.3 6.3E-03 20.1 2.0E-01 0.1 4.9E-01

TCA cycle substrates

and other acids

Succinate 116.5 1.8E-08 3.5 4.2E-03 1.0 1.1E-03 6.5 1.5E-03 21.1 2.7E-03

Fumarate 7.0 2.9E-07 20.7 2.7E-01 20.2 1.6E-01 1.1 5.1E-02 20.4 1.7E-01

Aconitate 4.3 5.3E-04 22.8 3.2E-02 20.5 1.5E-01 21.6 1.1E-02 20.2 2.4E-01

Citrate 2.5 4.0E-05 211.7 5.5E-02 21.5 8.3E-03 23.2 1.3E-02 20.7 1.4E-04

Malate 0.0 1.5E-01 22.2 8.8E-05 21.0 3.1E-05 20.1 9.2E-02 0.0 7.5E-01

Isocitrate 20.1 1.9E-01 22.1 8.7E-02 20.5 3.7E-02 25.3 6.0E-03 20.5 1.1E-03

2-Oxoglutarate 22.2 1.3E-03 23.8 2.6E-02 20.3 1.8E-01 224.5 6.4E-04 20.8 2.8E-03

Glycerate 21.8 1.3E-04 21.5 2.6E-06 20.9 7.3E-03 20.5 1.6E-02 20.2 8.9E-03

Threonate 2118.6 1.0E-05 21.1 7.0E-04 20.2 4.3E-03 0.3 8.7E-03 20.2 2.0E-01

Ascorbate N/D N/D 21.8 3.8E-04 1.2 2.2E-01 20.1 2.0E-01 20.1 2.7E-01

Glucarate 0.9 1.1E-04 20.3 3.0E-02 20.4 3.9E-03 20.2 1.9E-01 20.2 2.1E-01Citramalate 20.5 5.7E-02 20.8 1.9E-02 20.2 6.8E-02 0.2 6.1E-02 21.4 4.9E-03

4-Hydroxycinnamate N/D N/D 20.1 3.0E-01 0.5 1.2E-03 0.2 2.2E-02 0.8 8.0E-04

Urate 561 2.1E-06 0.2 5.8E-01 15.2 2.9E-03 21.4 3.3E-01 15.4 3.4E-04

Other Shikimic acid 20.7 1.0E-03 20.1 4.1E-01 4.5 6.2E-02 0.0 9.3E-01 3.4 1.5E-01

Phosphate 1.6 5.5E-08 0.3 2.9E-02 20.1 6.0E-01 20.1 6.2E-01 20.2 2.4E-01

Cytosine N/D N/D 21.6 2.0E-04 20.6 1.5E-05 20.2 4.0E-01 20.3 3.0E-01

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suggest that the transcript of this protein was dramat-ically down-regulated (271-fold) in anoxic rice coleop-tiles (Lasanthi-Kudahettige et al., 2007). This supportsthe observation that auxin-binding activities were de-creased in anoxic coleoptiles (Mapelli and Locatelli,1995) and that there was no synergistic effect of IAA andanaerobiosis on rice coleoptile elongation (Pegoraroet al., 1988). The repressive effect of anoxia on auxin-related genes has also been observed in Arabidopsisthrough a global gene expression analysis (Loreti et al.,2005).Also of interest was the finding that several proteins

with unknown functions accumulated under anoxia.These proteins are annotated as protein kinases thatcontain the domain of unknown function 26. Theirtranscript fold increases under anoxia range from 248-to 1,007-fold (Os08g04250, Os08g04210, Os08g04240;Lasanthi-Kudahettige et al., 2007). In addition, theArabidopsis ortholog (At5g48540; Supplemental TableS3) is up-regulated in response to 2 and 9 h of hypoxiaboth within the total and polysomal mRNA pools ofArabidopsis seedlings (Branco-Price et al., 2008). Nota-bly, we found anoxic accumulation of two group 3 lateembryogenesis abundant proteins (LEA; Os05g46480,Os02g15250) as well as embryonic protein DC-8(Os03g07180). LEAs are hydrophilic unstructured pro-teins rich in Gly, Ala, and Ser (Baker et al., 1988;Campos et al., 2006). It has been reported that a LEAprotein (Os04g52110) accumulates in anoxic rice em-bryos (Howell et al., 2007), and other groups havedemonstrated the inducibility of GUS reporters whenfused to a carrot (Daucus carota) group 3 LEA promoterunder hypoxia, salinity, and dehydration (Siddiquiet al., 1998). Recently, it was shown that SUB1A in-creased the accumulation of transcripts encoding forproteins involved in dehydration tolerance. Most in-terestingly, the LEA3 transcript level increased to agreater degree during desubmergence in M202(Sub1)rice relative to wild-type M202 (Fukao et al., 2011).This is especially interesting given that dehydration is astress inherent to desubmergence. This LEA3 transcriptactually showed a decrease during submergence, achange in opposition to what we have found. This maybe attributable to the use of different cultivars, themeasurement of transcript levels and not proteinabundance levels, and that submergence and anoxiaare not perfectly comparable. Despite these differences,in our experimental system, it is tempting to speculatethat LEA up-regulation is a response that provides aprotective and anticipatory function for when plantsreturn to air. Clearly, LEAs are stress responsive; how-ever, the role of these proteins in anoxic environmentsawaits further insights into their molecular function.

Metabolomic Analysis Reveals a Greater Response toAnoxia in Rice Than in Wheat Coleoptiles

To investigate the impact of the changes in primarymetabolism on metabolite pools, we considered theoverall changes in the gas chromatography-mass spec-

trometry (GC-MS) profiles of primary metabolites inwheat and rice coleoptiles exposed to anoxia. Consis-tent with the physiological and proteomic data, therewere dramatic differences in metabolite profiles be-tween rice coleoptiles derived from 4-d-old aeratedand 6-d-old anoxic seedlings, with very high accumu-lation of amino acids under anoxia (Table III; Fig. 2).Many of these responses were also observed in ricecoleoptiles that were switched to anoxia for 1 d, al-though these tended to be considerably more subtle(Table III; Fig. 3).

A number of major differences observed in 6-d-oldanoxic seedling coleoptiles relative to 4-d-old aerobicseedling coleoptiles were not observed at all as re-sponses in switched seedling coleoptiles (e.g. 17- to45-fold increases in 3-phosphoglycerate, b-Ala, and2-aminoadipate and a remarkable 560-fold increase inurate; Supplemental Table S7). Moreover, some me-tabolites responded in opposite directions to the twotreatments (e.g. Arg, homo-Ser, Lys, and Tyr; Supple-mental Table S7). These discrepancies are consistentwith oxygen-dependent biogenesis of cellular com-ponents involved in the regulation of thesemetabolitesin rice.

The wheat coleoptile metabolite profile also respondedto anoxia (Table III; Fig. 3; Supplemental Table S4). Certainfeatures were found to be common to responses ofwheat and rice coleoptiles to 1-d anoxic transfer. Theseincluded accumulations of g-aminobutyrate, Gly, Ile,Pro, Thr, succinate, and putrescine and decreases inAsp, Fru, Rib, trehalose, citrate, isocitrate, citramalate,glucarate, malate, glycerate, threonate, and cytosine(Table III; Supplemental Table S5). However, in wheat,these responses tended to be much less pronouncedthan those observed in anoxically switched rice cole-optiles (Table III; Fig. 3).

While some metabolite responses to the 1-d anoxicshift were common to both species (Fig. 3; Table III),we did identify a number of species-specific responsesthat may be linked to the differential anoxia toleranceof these species (Supplemental Tables S5 and S6). Rice-specific responses included moderate to strong in-creases in Ser, Ala, Leu, and Trp and decreases in Arg,Met, Tyr, Orn, 6-phosphogluconate, and aconitate (withthe aconitate response being themost consistently strongbetween experiments). Wheat-specific responses in-cluded moderate increases in b-Ala, 4-hydroxycinna-mate, and shikimate, strong increases in urate, andmoderate decreases in 4-Hyp and Suc. Interestingly, asmall number of metabolites responded moderatelystrongly in opposite directions between the two spe-cies. For example, a-aminobutyrate and phosphate in-creased in rice while decreasing in wheat; conversely,Lys, Phe, Xyl, and ascorbate decreased in rice whileincreasing in wheat. The distinctive and significantaccumulation of Ala and Ser in rice was consistent withour evidence of increased abundance of enzymes inthese pathways in rice (Fig. 3).

Surprisingly, L-Ala did not significantly differ inabundance between control and anoxically switched

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wheat coleoptiles (Table III), contradictory to a previ-ous report where Ala levels accumulated in wheatshoots to the same degree as that of rice shoots after 8 hof anoxia (Menegus et al., 1989) as well as a range ofreports from other species (van Dongen et al., 2009;Narsai et al., 2011). Such a difference might be ex-plained by differences in the experimental system, thespecific dissection of the coleoptile tissue used in thisreport, or the timing of the amino acid accumulation.For example, accumulation of Ala in roots of Arabi-dopsis was found by treatment with 48 h of 4% and 8%oxygen but not when the concentration of oxygen wasreduced to 1% (van Dongen et al., 2009). To considerthe last of these, we repeatedmetabolite profiling at 4 hafter the switch to anoxia in both rice and wheat, but

again we saw an increase in L-Ala in rice but not inwheat (Table III).

In addition to changes in amino acids, variations inintermediates in the tricarboxylic acid (TCA) cyclewere also observed. In the TCA cycle, the step con-verting succinate into fumarate by succinate dehydro-genase requires the operation of an electron transportchain and reduction of oxygen to water. Withoutoxygen, the TCA cycle will stop at succinate dehydro-genase and succinate will accumulate, as we observedin both rice and wheat coleoptiles (Table III; Fig. 3) andas other studies have reported (Menegus et al., 1991;Fan et al., 1997; Rocha et al., 2010). This claim was alsosupported by the decrease in other TCA cycle inter-mediates such as malate and citrate in both anoxically

Figure 3. Effect of a 1-d anoxic switch on carbohydrate metabolism, glycolysis, fermentation, amino acid metabolism, and theTCA cycle in rice and wheat coleoptiles. Rice and wheat seeds were germinated and grown under aeration for 4 d or for 4 d witha switch to 1 d of anoxia. Green or red boxes represent metabolites significantly more abundant during aeration or the anoxicswitch, respectively (P, 0.05). The yellow boxes represent metabolites whose abundances are unchanged. Enzyme names thataccompany arrows are also colored in this fashion for the rice response only (anoxia-responsive proteins were not identified inwheat). The numbers on the top left and right side of each square represent the response value (RV) of the correspondingmetabolite (anoxia/aeration) in rice and wheat coleoptiles, respectively. All data were extracted from Tables II and III. (Forabbreviations, see Fig. 2 legend).

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switched cereals, yet it was contradicted when observ-ing 6-d-old anoxic rice coleoptiles (Table III; Figs. 2 and3) and suggests that the other intermediates in theTCA cycle were utilized under anoxia. The advantageof the accumulation of succinate under anoxia hasbeen widely discussed in the context of the extra ATPproduction that can result (Gibbs and Greenway, 2003;Bailey-Serres and Voesenek, 2008; Rocha et al., 2010).Under prolonged anoxia, higher abundances of Suc,

Glc-6-P, and Fru-6-P in rice coleoptiles were observed(Table III; Fig. 3). Rice coleoptiles treated with shorterperiods of anoxia (24 or 4 h) revealed no significantdifferences in these sugars between stress and controltreatments. In wheat, however, a 4-h anoxic treatmentresulted in significant decreases in all three sugars,and the 24-h treatment resulted in a decrease of Suc(Table III; Fig. 3). Decreases in the levels of the trans-portable sugar Suc as well as decreases in glycolyticintermediates might be indicative of a delayed transi-tion to anaerobic metabolism in wheat when com-pared with rice.

Database-Driven Metabolic Phenotype Analysis RevealsConserved and Divergent Responses to Low Oxygen in

Rice and Wheat

Having established that wheat and rice coleoptilesdisplay differential responses to oxygen deprivation, wethought it would be informative to compare these re-sponses with those previously observed in other species.To this end, we used the PhenoMeter tool ofMetabolome-Express (https://www.metabolome-express.org; fordetails, see “Materials and Methods”) to search theMetabolomeExpress database of metabolic pheno-types, MetaPhenDB (see “Materials and Methods”),for previously reported metabolic phenotypes of sta-tistically significant qualitative overlap (codirectionalresponses) or inverse overlap (opposite direction re-sponses) with the rice and wheat responses to anoxiathat we report.As expected, the metabolic responses of rice and

wheat coleoptiles to anoxic transfer retrieved signifi-cant hits (P , 0.05; Fisher’s exact test) to a number ofpreviously reported responses to oxygen deprivation(Gibon et al., 2002; Narsai et al., 2009, 2011; Rocha et al.,2010; summarized in Supplemental Table S9) whileretrieving very few matches to any of the many otherfunctionally less closely related metabolic responses inthe MetaPhenDB database (for detailed results, in-cluding Fisher’s exact test P values, see SupplementalTable S9). In addition, a number of species-specificpositive and negative hits were also observed to di-verse treatments (Supplemental Table S8). For exam-ple, rice gave highly significant positive hits to theresponses of Arabidopsis cell suspensions to inhibi-tion of the mitochondrial electron transport chaincomplex I (Garmier et al., 2008), while wheat did notgive any significant hits to this phenotype. Conversely,only wheat gave significant positive hits to low-oxygenresponses of potato (Solanum tuberosum) tubers

(Geigenberger et al., 2000), castor bean (Ricinus com-munis) phloem (van Dongen et al., 2003), or the sulfurdepletion-mediated hypoxia response of the Chlamy-domonas reinhardtii stm6 mutant (Timmins et al., 2009;Supplemental Table S8). In two cases, waterloggingof Populus 3 canescens roots (Kreuzwieser et al., 2009)and low-oxygen treatment of Arabidopsis roots (vanDongen et al., 2009), rice gave positive hits whilewheat gave inverse hits (Supplemental Table S8), in-dicating significant divergence between rice and wheatin metabolites that define these responses. Given thelarge difference that these two species display in theirresponses to anoxia at the metabolite level, we wantedto consider whether the ability to generate a particularmetabolite pool contributes to anoxia tolerance and weset out to test this hypothesis.

Amino Acid-Induced Improvement of Cell Integrity inWheat under Anoxia

A range of reports in mammalian cells have high-lighted that exogenous addition of Gly, Ser, and/orAla can enhance the survival of cells to oxygen dep-rivation (Brecht and Groot, 1994; Tijsen et al., 1997;Wang et al., 2010). To test whether the differentialaccumulation of these amino acids could be part ofplant anoxia tolerance and to define the functionalimportance of the divergence of rice and wheat met-abolic responses to anoxia, we supplemented themedium used for rice and wheat growth under anoxia.We supplemented with a combination of amino acidsand assessed plant performance with the Evans blueroot cell viability assay after 3 d in anoxia (Fig. 4A).This showed that amino acid supplementation signif-icantly increased cell viability in wheat but not in riceroots, consistent with the differential accumulation ofthese amino acids in rice. To confirm this finding fromwhole wheat seedlings, we used the measurement ofelectrical conductivity as a direct indicator of electro-lyte leakage, and thus cell integrity, from anoxicallytreated seedlings in the presence or absence of thesethree amino acids in several different combinations(Fig. 4B). This showed that the combination of Ser/Ala/Gly significantly lowered electrolyte leakage, asdid Ser/Ala, but the presence of only one of the aminoacids did not protect wheat seedlings from electrolyteleakage (P , 0.01). We also confirmed the absence ofthis positive effect in anoxia-tolerant rice seedlings. Thissuggests that the disparity between rice and wheatmetabolite pool responses (Fig. 3) may contribute to thedegree of anoxia tolerance and that partial generation ofthese pools (via exogenous supplementation) in sensi-tive plants can improve cellular integrity.

DISCUSSION

We have analyzed the differential responses of co-leoptiles from rice and wheat seedlings to anoxia at thephysiological, metabolomic, and proteomic levels. Our

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data suggest that despite wheat having an anatomi-cally similar coleoptile, it responds to anoxia to a lesserdegree at the molecular level than the coleoptiles ofrice. Our findings are consistent with previous reportsthat rice seedlings were much more tolerant to anoxiathan wheat seedlings and that this involves an adap-tive response (Menegus et al., 1989, 1991). Our results

also suggest that the changes in the capacity of met-abolic pathways, via alterations in protein synthesis ordegradation rates, are important at least in the ricecoleoptile for anoxia tolerance.

Transcriptional Versus Translational Control of RiceAnoxia Response

There is an increasing body of literature on thetranscriptional response of rice to anoxia that showsgreat complexity in the response (Howell et al., 2007;Lasanthi-Kudahettige et al., 2007; Narsai et al., 2009),and the role of differential translation of only an activepool of RNAs during germination and anoxia furthercomplicates its interpretation (Branco-Price et al., 2008).We have extracted published gene expression data from4-d-old anoxic and aerobic rice seedlings (Lasanthi-Kudahettige et al., 2007) to make comparisons withour protein profiling data here. Overall, the correlationbetween differences in protein abundance and differ-ences in mRNA expression in anoxically germinatedrice versus aerated rice was poor (r2 = 0.39 when com-paring log10 ratios; Supplemental Fig. S3B). However,there were some positive correlations observed wherethe direction of change in response to anoxia or aerationwas the same for both the protein and its transcript(Table II). For example, peroxiredoxin (Os07g44430) andprotein kinases (Os08g04250, Os08g04210, Os08g04240)were highly accumulated under anoxia alongside clearup-regulation of the corresponding transcripts (TableII). The BBTI (Os01g03340) and ILR1 (Os03g62060)were less abundant under anoxic conditions, whichwas in concordance with the extracted transcript dataindicating their strong down-regulation (Table II). Suchresults suggest that these particular proteins might beregulated at the transcriptional level. However, anotherBBTI (Os01g03360) was reported as more abundant in6-d anoxic coleoptiles according to iTRAQ quantitation,despite its transcript showing the opposite direction ofchange under anoxia (Table II).

Selective mRNA translation under oxygen deficiencyhas been previously observed in plants (Bailey-Serres,1999). In Arabidopsis, it was recently reported thatselective mRNA translation coordinates “energetic andmetabolic adjustments” to oxygen deficiency and re-covery (Branco-Price et al., 2008). This claim was alsosupported by our proteomic data for the accumulationof proteins from the glycolytic pathway in anoxic ricecoleoptiles (Table II; Fig. 3). For example, Fru-bisPaldolase (Os05g33380) and glyceraldehyde-3-phosphatedehydrogenase cytosolic 3 (Os04g40950, Os08g03290)were significantly more abundant at the protein level,while the extracted microarray data indicated thatboth genes were not responsive to anoxia (Table II).Other isoforms of glyceraldehyde-3-phosphate dehy-drogenase cytosolic 3 (Os02g38920) showed abundancedifferences that were in agreement at the protein andmRNA levels. This suggests that the selected transla-tion of different mRNAs might require modification ofthe cytosolic ribosome. However, the actual mechanism

Figure 4. The effect of exogenous amino acid feeding on cell integrityafter prolonged anoxia in wheat and rice seedlings. A, Rice and wheatseeds were germinated and grown under 4 d of aeration. Fresh culturemedium in the presence or absence of 10 mM Ala, Ser, and/or Gly wasthen added to seedlings. Seedlings were returned to 3 d of aeration(green) or transferred to 3 d of anoxia (nonsupplemented in red;supplemented in dark red). Roots were then analyzed using the Evansblue viability stain (n = 3). An increase in cell death is proportional toincreasedA600. B, Cell membrane permeability in whole rice andwheatseedlings was also analyzed (n = 10–23). This was done by measuringelectrical conductivity after seedlings were incubated in distilled,deionized water for 1 h (C1). A second measurement was taken aftersample boiling (C2) to obtain the proportion of cell leakage in differentsamples. Larger C1/C2 values indicate higher electrolyte leakage andthus lower cell integrity. *** P , 0.001, ** P , 0.01, * P , 0.05 whencomparedwith anoxic seedlings that were not supplemented (red bars).

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of selective translation in plants remains unknown.Matching of the rice genes studied here to their Arabi-dopsis orthologs showed no apparent correlation be-tween the rice proteins, whose abundance was notreflected in rice transcript data, and the ribosomalloading of orthologous mRNA under anoxia in Arabi-dopsis (Supplemental Table S3). Exceptions includesome proteins with unknown functions as well asclassical anaerobic proteins.Alternatively, difference in protein abundance be-

tween treatments could be accounted for by alterationsof the rate of synthesis and/or degradation of eachprotein. The abundance of cytosolic ascorbate perox-idase (Os03g17690) was significantly decreased with-out any apparent change in gene expression (Table II),suggesting that the translation of this gene was in-hibited by some downstream consequence of anoxia orthat this protein underwent selective degradation. Themechanism of selective protein degradation under an-oxia also deserves further investigation. Because thewheat coleoptile proteome was largely unchangedeven after 24 h of anoxia (Fig. 1C), selective mRNAtranslation or protein degradation might not be occur-ring as frequently in this species as is apparent in ricecoleoptiles. The consequence of a smaller upstreamresponse for the regulation of translation and proteinturnover in wheat coleoptiles under anoxia was alsoreflected in metabolic and physiological responses.

Amino Acid Metabolism Is Perturbed during Anoxia

The accumulation of amino acids in anoxic rice andwheat coleoptiles is consistentwith thewell-documentedobservation of this phenomenon when plants are ex-posed to differing degrees of oxygen deprivation (Fanet al., 1997; Kato-Noguchi and Ohashi, 2006; Narsaiet al., 2009; van Dongen et al., 2009; Rocha et al., 2010).We also detected the accumulation of enzymes involvedin Ala, Ser, and Gly biosynthesis concomitant with theaccumulation of those amino acids (Fig. 2). The pro-posed benefit of the accumulation of Ala under oxygendeprivation in different plant species has been dis-cussed in detail (Gibbs and Greenway, 2003; Bailey-Serres and Voesenek, 2008). Also, Ala synthesis throughAla aminotransferase 2 does not contribute to the oxi-dation of NADH, as does lactate or ethanol produc-tion, but rather serves as a retainable carbon sourceupon return to air (Good and Crosby, 1989; Miyashitaet al., 2007). However, the role of Gly and Ser accu-mulation is less clear. The transcripts for a number ofthese biosynthetic proteins are more abundant underanoxia (Lasanthi-Kudahettige et al., 2007; Table II),indicating that amino acid synthesis rather than proteindegradation is likely to be responsible. But, to ourknowledge, direct evidence for the benefits of feedingexogenous amino acids to seedlings growing underanoxia in an anoxia-intolerant but not an anoxia-tolerantspecies (Fig. 4) has not previously been reported.We initiated these exogenous feeding experiments

on the basis of an intriguing report on the positive

effects of Gly, Ser, and Ala on mammalian cells underhypoxic stress. Of the 23 standard amino acids tested,only Gly, L-Ala, and L-Ser provided significant protec-tion from hypoxic injury of cultured hepatocytes (Brechtand Groot, 1994). For some years, hypoxic or energydeficiency injury to hepatocytes and kidney tubuleshas been treated with Gly as a method of cell preser-vation (Weinberg et al., 1991; Carini et al., 1997; Tijsenet al., 1997). Although the literature agrees that pro-tection by Gly is not simply an enhancement of theenergetic state of the hypoxic cells, the mechanism ofprotection is still unclear. Research favors two differ-ent mechanisms associated with the modification ofthe rise in intracellular Na+ during hypoxia due toenergy-induced loss of Na+-K+-ATPase activity: indi-rectly via the activation of Gly receptor neurotrans-mitters (Carini et al., 1997) or directly by blockingnonselective sodium transport (Frank et al., 2000).

Subsequent literature examination also shows thatwhile the addition of a range of amino acids into ex-ternal medium can result in cytoplasmic acidificationof plant cells (Felle, 1981), the addition of Ala and Serdoes not acidify the cytoplasm but instead results in apH increase of some 0.2 to 0.3 units (Felle, 1996). Thissuggests a selective benefit of these amino acids inavoiding cytoplasmic acidification under anoxia. Addi-tionally, Ser is the entry point for sphingolipid biosyn-thesis in plants. The transcript of the gene controllingthe first step of sphingolipid biosynthesis, the conden-sation of palmitate and Ser to form 3-keto-dihydro-sphingosine (Ser palmitoyltransferase [Os01g70370]),was up-regulated 20-fold in anoxic coleoptiles (Lasanthi-Kudahettige et al., 2007) and was classified as a coreanaerobic responder in germinating rice embryos(Narsai et al., 2009). Recent research in Caenorhabditiselegans (Crowder, 2009; Menuz et al., 2009) suggeststhat ceramides play a critical role in anoxia tolerance.The possible role of Ser in ceramide biosynthesisthrough Ser palmitoyltransferase in plant adaptationto anoxia deserves further investigation to identifynovel mechanisms conferring anoxia tolerance.

Hence, there are a range of possible explanations forthe beneficial effects of combinations of Ala/Ser/Glyon plant cell anoxia tolerance through the retention ofcarbon skeletons, modification of biosynthetic processes,and cellular ion balance.

CONCLUSION

In summary, our study reinforced the importance ofglycolysis and ethanolic fermentation in the adapta-tion to anaerobiosis and suggests that glycolysis mightalso be important in providing substrates for amino acidsynthesis. Rice, but not wheat, coleoptiles respondedto anoxia dramatically at the physiological, proteomic,and metabolomic levels, in concordance with the re-spective tolerance and intolerance of these speciesto anoxia. Further investigation into the role of machin-ery differences in selected mRNA translation and/or

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protein turnover between rice and wheat coleoptiles isneeded based on the targets identified here. We providenovel protein and metabolite evidence of the enhance-ment of Ser/Gly biosynthesis as well as support obser-vations that Ala accumulates in anoxic rice. We alsoshow a benefit for wheat by exogenous application ofthese amino acids and highlight a range of mechanismsthat could be responsible for conferring anoxia toler-ance.

MATERIALS AND METHODS

Plant Material

Dehulled rice (Oryza sativa ‘Amaroo’) and wheat (Triticum aestivum

‘Calingiri’) seeds were surface sterilized for 10 min using 50% (v/v) NaOCl

and then thoroughly rinsed with distilled, deionized water. Fifty to 75 seeds

were placed in conical flasks containing 250 mL of culture medium (0.5 mM

MES, 0.4 mM CaSO4, pH 6.5) and bubbled with air or N2 (6–7 L min21). Plastic

tubing delivered the gas to the seeds, and the system was sealed using

Parafilm and aluminum foil. Seedlings were grown in the dark at 30�C for (1)

4 d under aeration, (2) 4 d under aeration with an additional 1-d switch to

anoxia, or (3) 6 d under anoxia. To ensure that stress conditions were anoxic,

oxygen concentrations were monitored, and after 10 min of N2 bubbling, the

oxygen concentration was below the level of detection. This was measured

using the LabQuest Vernier oxygen meter with a sensitivity of 0.01% oxygen.

Rice seed was kindly provided by the New South Wales Department of

Primary Industries and wheat seed by the Western Australian Department of

Agriculture and Food.

Evans Blue Viability Stain

This protocol was adapted from the method described by Baker and Mock

(1994). Fresh tissues were excised from seedlings, weighed (0.05–0.1 g), and

placed in a 10-mL Falcon tube containing 100 mL of distilled, deionized water.

Two milliliters of 0.25% (w/v) Evans blue was added to each sample, and

horizontally lying tubes were shaken at room temperature for 20 min at 300

rpm. The stain was rinsed from tissues in a sieve until the water ran clear, snap

frozen, and then ground in a 2-mL Eppendorf microfuge tube containing a

carborundum ball for 3min at 17 shakes s21. A total of 0.5 mL of 1% (w/v) SDS

was added, and samples were ground for 3 min again. One milliliter of

distilled, deionized water was added to samples, which were then centrifuged

at 8,800g for 3 min. The absorbance of diluted supernatants (1:3) was measured

at 600 nm. The average masses of tissue samples (0.075 g) were used to nor-

malize absorbance measurements so that different samples could be com-

pared (n = 3).

Measurement of Electrical Conductivity

We measured electrical conductivity as an estimation of membrane integ-

rity (Yan et al., 1996). This was done in whole rice and wheat seedlings

germinated and grown for 4 d in aeration and subsequently transferred to

anoxia or air for 3 d in fresh culture medium (0.5 mM MES, 0.4 mM CaSO4, pH

6.5). Some samples were supplemented with the amino acids L-Ala, L-Ser,

and/or Gly at 10 mM concentrations. Seedlings were then washed with

distilled, deionized water, patted dry with tissue paper, and placed in 15-mL

Falcon tubes containing 10 mL of distilled, deionized water for 1 h at 19.5�C.The electrical conductivity of these solutions was measured (C1; TPS Aqua-C

conductivity TDS temperature meter). Samples were then microwaved for 2

min. Care was taken to ensure boiling of each sample. After 1 h, the electrical

conductivity was measured again (C2) at 19.5�C and used as the denominator

in the calculation of percentage electrolyte leakage.

ADH Activity

Measurement of ADH activity was performed as described byWaters et al.

(1991). Briefly, protein was extracted by grinding approximately 70 mg

of snap-frozen plant tissue with acid-washed sand and 1 mL of extraction

buffer (125 mM MES, 110 mM NaCl, 1 mM EDTA, 0.5 mM thiamine PPi, 2.5 mM

MgSO2, and freshly added dithiothreitol at 2 mM, pH 6.8). After centrifugation

at 10,000g for 4 min at 4�C, the supernatant was removed for analysis. The

ADH activity was measured at 340 nm in a 1-mL cuvette in reaction medium

(10 mM acetaldehyde, 50 mM TES, 0.17 mM NADH, pH 7.5).

Carbohydrate Measurement

Carbohydrate levels were measured using a modified method (Trevelyan

and Harrison, 1952). Tissue extracts were prepared by heating 20-mg samples

submerged in 2 mL of 80% ethanol at 70�C for 20 min in a tightly sealed tube.

Extracts were then removed from tissue, and 100 mL of extract was added into

1 mL of freshly prepared anthrone reagent (mixture of 0.2 g of anthrone to 100

mL of 70% [v/v] sulfuric acid). After vortexing, samples were boiled at 100�Cfor 10 min exactly, promptly placed in an icy-water bath for 5 min, and then

removed and stored at room temperature for 5 min before measuring A627.

Oxygen Uptake Measurements

Oxygen uptake measurements followed a procedure described previously

(Lee et al., 2008) using a computer-controlled Clark-type oxygen electrode

unit. Slight modifications include the use of approximately 90 mg of fresh

tissue and 2 mL of oxygen-saturated buffer composed of 5 mM KH2PO4, 10 mM

TES, 10 mM NaCl, and 2 mM MgSO4, pH 7.2.

Protein Purification

Snap-frozen coleoptiles were ground with acid-washed sand and a solu-

bilizing solution (7% [w/v] SDS, 125 mM Tris-HCl, and 10% [w/v] b-mercap-

toethanol at a 5:8 [w/v] ratio, pH 7). Protein purification was carried out using

the chloroform-methanol method (Wessel and Flugge, 1984). Protein pellets

were then incubated with 80% acetone for 1 h at 220�C. The solution was

centrifuged at 14,000 rpm for 10 min at 4�C, and the pellets were air dried.

Protein was resolubilized with rehydration buffer (6 M urea, 2 M thiourea, 2%

[w/v] CHAPS, 2% [v/v] immobilized pH gradient buffer, and 18 mM

dithiothreitol) for preparative gels or lysis buffer (6 M urea, 2 M thiourea, 2%

[w/v] CHAPS, and 40 mM Tris) for DIGE gels by shaking in an orbital rocker at

1,400 rpm at 25�C for 45 min. Centrifugation at 20,000g for 15 min was then

carried out. Protein was quantified using the 2D Quant Kit (GE Healthcare).

IEF/SDS-PAGE Gel Separations

For preparative gels, 800 mg of protein resolubilized in rehydration buffer

containing equal amounts of both samples was loaded onto IEF strips (3-10NL,

3-11NL, 24 cm; GE Healthcare) and separated for 24 h (up to 50 mA per strip,

5 W, 21�C). Six-step program parameters were as follows: 30 V for 12 h and

hold (step and hold [stp]), 500 V for 1-h stp, 1,000 V for 1-h gradient, 3,000 V

for 2-h gradient, 8,000 V for 2-h gradient, and 8,000 V for 6-h stp). IEF strips

were then dipped in 13 gel buffer, placed on top of a 12% acrylamide gel, and

run at 45 mA per gel for 6 to 7 h. For DIGE gels (Eubel et al., 2007), 50 mg of

treated, control, and a 1:1 internal standard mixture of the above-mentioned

coleoptile proteins was labeled separately with 400 mM fluorescent CyDye. The

labeling procedure was carried out according to the recommendations of GE

Healthcare. Samples were pooled and separated in the same manner that

preparative gels were. DIGE gels were scanned using a Typhoon laser scanner

(GE Healthcare), and quantitative analysis was carried out using the DeCyder

software package (version 6.5; GE Healthcare). Three independent dye-

swapping replicates were carried out. Statistically significant spots were

selected for MS identification according to their appearance in nine of nine

fluorescent images, a ratio of abundance difference of 2 or greater, and a value

of P # 0.05. Both DIGE and preparative gels were Coomassie Brilliant Blue

stained and destained.

Protein Identification Using MS

Selected protein spots were excised from gels and digested in gel as

described previously (Taylor et al., 2005). Vacuum-dried samples were

redissolved in 5% (v/v) acetonitrile and 0.1% (v/v) formic acid for analysis

on an XCT Ultra Ion Trap mass spectrometer (Agilent Technologies), and MS/

MS spectra were exported for data analysis. MS spectra were examined

against an in-house rice database of The Institute for Genomic Research Rice

Pseudomolecules and Genome Annotation and mitochondrial and plastid

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protein sets (Rice version 6) using version 2.2.03 (Matrix Science) of theMascot

search engine. The following settings were selected for searching: MS error

tolerance of 61.2 D, MS/MS error tolerance of 60.6 D, maximum missed

cleavages tolerated as one, two variable modifications including carbamido-

methyl (C) and oxidation (M), peptide charge as 2+ and 3+, and finally, the

instrument selected as ESI-TRAP. After results were retrieved from theMascot

search engine, “Require bold red” and “Standard scoring” checkboxes were

selected with the ion score cutoff set at 37, the “Significance threshold”

set at P , 0.05, and the “Max. number of hits” set at AUTO. MS spectra

files are available for analysis via the Proteome Commons Tranche Project

under hashWiq7A0erU/p/zv9IJSKf+5pyjbFZXnERbYRQYwrglOB3N/kmT/

Sp9qJ4ksGmr9J76AmipUl3xMLTO1I07LFWa19V0K8AAAAAAAACEg = =.

Metabolite Extraction, GC-MS Sample, andData Analysis

Metabolite extraction from coleoptiles followed a modified procedure

described previously (Howell et al., 2009). Tubes containing ground tissue

samples (100 mg of stressed or nonstressed coleoptiles) and grinding balls

(cooled) were placed in a liquid N2-cooled solid rack. Cold metabolite

extraction medium (0.5 mL; 85% [w/v] HPLC-grade methanol, 15% [w/v]

untreated MilliQ water, and 100 ng mL21 ribitol) was added to each tube,

immediately vortexed, and then shaken at 1,400 rpm for 20 min at 65�C.To pellet cell debris, samples were centrifuged at 20,000g for 10 min. Aliquots

(60 mL) of extract were dried in a vacuum centrifuge for approximately 2 h.

Twenty microliters of 20 mg mL21 methoxylamine-HCl (98% purity; Sigma)

was added to each of the dried samples. Samples were then shaken at 1,400

rpm for 90 min at 30�C. To each sample, 30 mL of N-methyl-N-(trimethylsilyl)-

trifluoroacetamide (derivatization grade; Sigma) was added, followed by

shaking again at 1,400 rpm for 30 min at 37�C. After this, 10 mL of n-alkane

standard mix (0.029% [v/v] n-dodecane, 0.029% [v/v] n-pentadecane, 0.029%

[w/v] n-nonadecane, 0.029% [w/v] n-docosane, 0.029% [w/v] n-octacosane,

0.029% [w/v] n-dotriacontane, and 0.029% [w/v] n-hexatriacontane dissolved

in anhydrous pyridine) was added and vortexed. Samples were transferred to

GC-MS amber vials with screw-top seals and low-volume inserts (Agilent

Technologies). These were then incubated for 4 h at room temperature for

equilibration. Analysis of samples on the GC-MS device followed the proce-

dure described previously (Howell et al., 2009). GC-MS data were collected

using Chemstation GC/MSD Data Analysis Software (Agilent Technologies).

Raw GC-MS data preprocessing and statistical analysis were performed using

MetabolomeExpress software (version 1.0; http://www.metabolome-express.

org). Detailed methods have been reported (Carroll et al., 2010).

Metabolic Phenocopy Analysis Using theMetabolomeExpress PhenoMeter

To systematically characterize relationships between the metabolic phe-

notypes observed in this study and metabolic phenotypes reported in previ-

ous studies, we used the PhenoMeter tool of MetabolomeExpress (https://

www.metabolome-express.org) to search the MetabolomeExpress metabolic

phenotype database, MetaPhenDB, for metabolic phenotypes having statisti-

cally significant qualitative overlap with the responses observed in this study

(submitted as a batch of “bait” responses). The PhenoMeter uses the following

procedure for each bait response. The bait response is compared with each

and every reference response in MetaPhenDB, one at a time. Each comparison

is done by first counting (1) the number of metabolites increased (i.e. having a

greater than 1-fold change) in both bait and reference; (2) the number of

metabolites decreased in both bait and reference; (3) the number of metab-

olites increased in bait but decreased in reference; and (4) the number of

metabolites decreased in bait but increased in reference. These counts were

then used as input in a two-tailed Fisher’s exact test to calculate the P value of

obtaining the observed positive (codirectional) or negative (inverse) response

overlap by chance alone. P. 0.05 was used to indicate statistically significant

overlaps or inverse overlaps. To minimize biases caused by the presence of

different sets of “unknown” metabolites in metabolic phenotypes acquired

from different studies, only metabolites of known structure (and hence having

the same name in each study) were considered in comparisons. Only metab-

olites present in both bait and reference were considered. So that the anoxia

responses observed in this study could be compared with previously

published plant responses to anoxia and hypoxia, we added the complete

set of 36 metabolic phenotypes associated with seven peer-reviewed publica-

tions (Geigenberger et al., 2000; Gibon et al., 2002; van Dongen et al., 2003,

2009; Branco-Price et al., 2008; Timmins et al., 2009; Rocha et al., 2010) from

other groups presented in a recent review (Narsai et al., 2011) of the topic to

MetaPhenDB prior to PhenoMeter analysis. At the time of analysis, Meta-

PhenDB contained 12,379 publicly available metabolite response statistics

representing 116 metabolic phenotypes, including oxygen deprivation-related

metabolic phenotypes for a total of six plant species (Arabidopsis [Arabidopsis

thaliana], potato [Solanum tuberosum], Lotus japonicus, Populus 3 canescens,

castor bean [Ricinus communis], and rice) in addition to metabolic phenotypes

associated with a wide variety of other environmental, developmental, and

genetic perturbations.

iTRAQ Analysis

Proteins were purified and quantified as described above. For each sample,

a total of 100 mg of protein was precipitated by the addition of 4 volumes of

cold acetone and stored in 220�C overnight. The precipitated protein was

then resuspended in dissolution buffer and denatured, and Cys residues were

blocked according to the manufacturer’s instructions (AB Sciex). Each sample

was then digested with 20 mL of 0.25 mg mL21 trypsin (Invitrogen) at 37�Covernight and labeled with the iTRAQ tags in triplicate. iTRAQ reagents were

resuspended in 50 mL of 2-propanol and added to each sample, pH adjusted,

and allowed to incubate at room temperature for 2 h. The labeled samples

were pooled prior to further analysis. To remove excess labeling reactants and

to reduce the interference of salts during liquid chromatography-MS/MS

analysis, the pooled samples were diluted 4-fold with strong cation-exchange

buffer A (10 mM KH2PO4 in 25% acetonitrile, pH 3.0) and subjected to strong

cation-exchange chromatography using an OPTI-LYNX cartridge (Optimize

Technologies). The eluent was dried in a vacuum concentrator and stored at

220�C for liquid chromatography-MS/MS analysis.

Samples were analyzed on an Agilent 6510 quadrupole-time-of-flight

(Q-TOF) mass spectrometer with an HPLC Chip Cube source. The chip

consisted of a 160-nL enrichment column (Zorbax 300SB-C18 5mm) and a

150-mm separation column (Zorbax 300SB-C18 5mm) driven by an Agilent

Technologies 1100 series nano/capillary liquid chromatography system. Pep-

tides were loaded onto the trapping column at 4 mL min21 in 5% (v/v)

acetonitrile and 0.1% (v/v) formic acid with the chip switched to enrichment

and using the capillary pump. The chip was then switched to separation, and

peptides were eluted during a 1-h gradient (5%–60% [v/v] acetonitrile) using

the nano pump at 300 nL min21 directly into the mass spectrometer. The

Q-TOF mass spectrometer was run in positive ion mode, and MS scans were

run over a mass-to-charge ratio range of 275 to 1,500 and at 4 spectra s21.

Precursor ions were selected for auto-MS/MS at an absolute threshold of 500

and a relative threshold of 0.01, with a maximum of three precursors per cycle

and active exclusion set at two spectra, and released after 1 min. Precursor

charge-state selection and preference was set to [M+H]2+ and then [M+H]3+,

and precursors were selected by charge and then abundance. Resulting MS/

MS spectra were searched against The Institute for Genomic Research Rice

Pseudomolecules and Genome Annotation and mitochondrial and plastid

protein sets (Rice_osa6) using version 2.2.03 (Matrix Science) of the Mascot

search engine. The following settings were selected for database searching:MS

error tolerance of 6100 ppm; MS/MS error tolerance of 60.5 D; maximum

missed cleavages tolerated as one; fixed modifications methylthio (C),

iTRAQ8plex (N-term), iTRAQ8plex (K); variable modifications carbamido-

methyl (C) and oxidation (M) iTRAQ8plex (Q), peptide charge of 2+ or greater;

and finally, the instrument selected as ESI-Q-TOF. The resulting searches were

then exported, and all peptides identified (P , 0.05) were extracted to create

an exclusion list for the subsequent run. All five runs were performed

and combined using mzdata Combinator version 1.0.4 (West Australian Centre

of Excellence in Computational Systems Biology) for database searching

as outlined below. MS spectra files are available for analysis via the Prote-

ome Commons Tranche Project under hash 5AJQpzyi1I5adgPNIGdJ+

oQf8nlIoXnjLVhePv9x39srDtRpuZe9gQu9ij62NLKetNEdx6t1MqirlvSglVAA-

UHcQZAYAAAAAAAABcA = =.

Quantitation was carried out using default settings in Mascot version

2.2.03 (Matrix Science) for protein identifications as outlined above and

quantitation on isobaric mass tags (iTRAQ) at the peptide level. In more detail,

ratios for individual peptide matches were obtained from peptides meeting

the minimum criteria outlined above and were then combined to determine

ratios for protein hits using a weighted average. Outlier removal was carried

out by Dixon’s method for up to 25 data points per protein or by Rosner’s

method, where more than 25 data points were present and normalization was

carried out by median ratio. Values are reported as geometric means with SD,

and those significantly different from 1 at a 95% confidence interval are

Rice and Wheat Anoxia Responses

Plant Physiol. Vol. 156, 2011 1721 www.plant.org on December 28, 2013 - Published by www.plantphysiol.orgDownloaded from

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marked with asterisks (Supplemental Table S1). For proteins reported to have

a nonnormal distribution, the geometric SD was determined manually. Here, a

geometric mean for the individual peptide ratios and a 95% confidence

interval window was calculated as a t test in Analyze-it version 2.21.

Supplemental Data

The following materials are available in the online version of this article.

Supplemental Figure S1. Germination, growth, and cell integrity of rice

and wheat under anoxia.

Supplemental Figure S2. Number of protein spots detected in each

proteomic analysis that significantly differed in abundance between

treatments.

Supplemental Figure S3. Correlations between protein abundance de-

tected from iTRAQ and DIGE and between transcript and protein

abundance differences between continuously anoxic and aerated rice

coleoptiles.

Supplemental Figure S4.DIGE on two-dimensional 3-11NL IEF/SDS gels.

Supplemental Table S1. Entire list of rice coleoptile proteins significantly

changing between treatments that were identified by DIGE and iTRAQ

proteomic analyses.

Supplemental Table S2. Quantitative analysis of protein abundance from

4-d aerated and 6-d anoxic rice coleoptiles using iTRAQ.

Supplemental Table S3. Comparison of steady-state and polysomal

Arabidopsis mRNAs under aeration and hypoxia, whose genes are

orthologous to rice genes encoding proteins significantly changing in

abundance in at least one of our rice proteome analyses.

Supplemental Table S4. Whole set of relative metabolite levels in wheat

and rice coleoptiles under aerated and anoxic conditions.

Supplemental Table S5. Comparison of metabolite responses between

wheat and rice coleoptiles from seedlings switched to 1 d of anoxia in

two independent experiments.

Supplemental Table S6. Grouping of metabolite responses in coleoptiles

of 4-d-old rice and wheat seedlings transferred to anoxia for 1 d (anoxic

switch conditions).

Supplemental Table S7. Comparison of metabolite responses in coleop-

tiles of anoxically switched and anoxically germinated rice seedlings.

Supplemental Table S8.Metabolic phenocopy analysis: comparison of the

low-oxygen responses of rice and wheat coleoptiles with low-oxygen

and respiratory-perturbation responses in other species and tissues.

Supplemental Table S9. Expanded results of MetabolomeExpress Pheno-

Meter analysis.

Received March 2, 2011; accepted May 12, 2011; published May 27, 2011.

LITERATURE CITED

Alpi A, Beevers H (1983) Effects of O2 concentration on rice seedlings.

Plant Physiol 71: 30–34

Atwell B, Waters I, Greenway H (1982) The effect of oxygen and turbulence

on elongation of coleoptiles of submergence-tolerant and -intolerant rice

cultivars. J Exp Bot 33: 1030–1044

Bailey-Serres J (1999) Selective translation of cytoplasmic mRNAs in

plants. Trends Plant Sci 4: 142–148

Bailey-Serres J, Chang R (2005) Sensing and signaling in response to

oxygen deprivation in plants and other organisms. Ann Bot (Lond) 96:

507–518

Bailey-Serres J, Voesenek LACJ (2008) Flooding stress: acclimations and

genetic diversity. Annu Rev Plant Biol 59: 313–339

Baker CJ, Mock NM (1994) An improved method for monitoring cell death

in cell suspension and leaf disc assays using Evans blue. Plant Cell

Tissue Organ Cult 39: 7–12

Baker J, Steele C, Dure L (1988) Sequence and characterization of 6 Lea

proteins and their genes from cotton. Plant Mol Biol 11: 277–291

Bartel B, Fink GR (1995) ILR1, an amidohydrolase that releases active

indole-3-acetic acid from conjugates. Science 268: 1745–1748

Baxter-Burrell A, Yang Z, Springer PS, Bailey-Serres J (2002) RopGAP4-

dependent Rop GTPase rheostat control of Arabidopsis oxygen depri-

vation tolerance. Science 296: 2026–2028

Biemelt S, Keetman U, Albrecht G (1998) Re-aeration following hypoxia or

anoxia leads to activation of the antioxidative defense system in roots of

wheat seedlings. Plant Physiol 116: 651–658

Blokhina O, Virolainen E, Fagerstedt KV (2003) Antioxidants, oxidative

damage and oxygen deprivation stress: a review. Ann Bot (Lond) 91:

179–194

Blokhina OB, Chirkova TV, Fagerstedt KV (2001) Anoxic stress leads to

hydrogen peroxide formation in plant cells. J Exp Bot 52: 1179–1190

Blokhina OB, Fagerstedt KV, Chirkova TV (1999) Relationships between

lipid peroxidation and anoxia tolerance in a range of species during

post-anoxic reaeration. Physiol Plant 105: 625–632

Blokhina OB, Virolainen E, Fagerstedt KV, Hoikkala A, Wahala K,

Chirkova TV (2000) Antioxidant status of anoxia-tolerant and -intoler-

ant plant species under anoxia and reaeration. Physiol Plant 109:

396–403

Branco-Price C, Kaiser KA, Jang CJH, Larive CK, Bailey-Serres J (2008)

Selective mRNA translation coordinates energetic and metabolic ad-

justments to cellular oxygen deprivation and reoxygenation in Arabi-

dopsis thaliana. Plant J 56: 743–755

Branco-Price C, Kawaguchi R, Ferreira RB, Bailey-Serres J (2005)

Genome-wide analysis of transcript abundance and translation in

Arabidopsis seedlings subjected to oxygen deprivation. Ann Bot

(Lond) 96: 647–660

Brecht M, Groot H (1994) Protection from hypoxic injury in cultured

hepatocytes by glycine, alanine, and serine. Amino Acids 6: 25–35

Campos F, Zamudio F, Covarrubias AA (2006) Two different late embryo-

genesis abundant proteins from Arabidopsis thaliana contain specific

domains that inhibit Escherichia coli growth. Biochem Biophys Res

Commun 342: 406–413

Carini R, Bellomo G, Grazia De Cesaris M, Albano E (1997) Glycine

protects against hepatocyte killing by KCN or hypoxia by preventing

intracellular Na+ overload in the rat. Hepatology 26: 107–112

Carroll AJ, Badger MR, Harvey Millar A (2010) The MetabolomeExpress

Project: enabling Web-based processing, analysis and transparent dis-

semination of GC/MS metabolomics datasets. BMC Bioinformatics 11:

376–388

Crowder CM (2009) Ceramides: friend or foe in hypoxia? Science 324:

343–344

Eubel H, Lee CP, Kuo J, Meyer EH, Taylor NL, Millar AH (2007) Free-flow

electrophoresis for purification of plant mitochondria by surface charge.

Plant J 52: 583–594

Fan TW-M, Higashi RM, Frenkiel TA, Lane AN (1997) Anaerobic nitrate

and ammonium metabolism in flood-tolerant rice coleoptiles. J Exp Bot

48: 1655–1666

Felle H (1981) Stereospecificity and electrogenicity of amino acid transport

in Riccia fluitans. Planta 152: 505–512

Felle HH (1996) Control of cytoplasmic pH under anoxic conditions and its

implication for plasma membrane proton transport in Medicago sativa

root hairs. J Exp Bot 47: 967–973

Frank A, Rauen U, de Groot H (2000) Protection by glycine against hypoxic

injury of rat hepatocytes: inhibition of ion fluxes through nonspecific

leaks. J Hepatol 32: 58–66

Fukao T, Xu K, Ronald PC, Bailey-Serres J (2006) A variable cluster of

ethylene response factor-like genes regulates metabolic and develop-

mental acclimation responses to submergence in rice. Plant Cell 18:

2021–2034

Fukao T, Yeung E, Bailey-Serres J (2011) The submergence tolerance

regulator SUB1A mediates crosstalk between submergence and drought

tolerance in rice. Plant Cell 23: 412–427

Garmier M, Carroll AJ, Delannoy E, Vallet C, Day DA, Small ID, Millar

AH (2008) Complex I dysfunction redirects cellular and mitochondrial

metabolism in Arabidopsis. Plant Physiol 148: 1324–1341

Geigenberger P, Fernie AR, Gibon Y, Christ M, Stitt M (2000) Metabolic

activity decreases as an adaptive response to low internal oxygen in

growing potato tubers. Biol Chem 381: 723–740

Gibbs J, Greenway H (2003) Mechanisms of anoxia tolerance in plants. I.

Growth, survival and anaerobic catabolism. Funct Plant Biol 30: 1–47

Gibbs J, Morrell S, Valdez A, Setter TL, Greenway H (2000) Regulation of

Shingaki-Wells et al.

1722 Plant Physiol. Vol. 156, 2011 www.plant.org on December 28, 2013 - Published by www.plantphysiol.orgDownloaded from

Copyright © 2011 American Society of Plant Biologists. All rights reserved.

Page 80: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

alcoholic fermentation in coleoptiles of two rice cultivars differing in

tolerance to anoxia. J Exp Bot 51: 785–796

Gibon Y, Vigeolas H, Tiessen A, Geigenberger P, Stitt M (2002) Sensitive

and high throughput metabolite assays for inorganic pyrophosphate,

ADPGlc, nucleotide phosphates, and glycolytic intermediates based on

a novel enzymic cycling system. Plant J 30: 221–235

Good AG, Crosby WL (1989) Anaerobic induction of alanine aminotrans-

ferase in barley root tissue. Plant Physiol 90: 1305–1309

Guglielminetti L, Perata P, Alpi A (1995) Effect of anoxia on carbohydrate

metabolism in rice seedlings. Plant Physiol 108: 735–741

Hou WC, Lin YH (1997) Dehydroascorbate reductase and monodehy-

droascorbate reductase activities of trypsin inhibitors, the major sweet

potato (Ipomoea batatas [L] Lam) root storage protein. Plant Sci 128:

151–158

Hou WC, Wang YT, Lin YH, Hsiao LJ, Chen TE, Wang CW, Dai H (2000) A

complex containing both trypsin inhibitor and dehydroascorbate re-

ductase activities isolated from mitochondria of etiolated mung bean

(Vigna radiata L. (Wilczek) cv. Tainan no. 5) seedlings. J Exp Bot 51:

713–719

Howell KA, Cheng K, Murcha MW, Jenkin LE, Millar AH, Whelan J

(2007) Oxygen initiation of respiration and mitochondrial biogenesis in

rice. J Biol Chem 282: 15619–15631

Howell KA, Narsai R, Carroll A, Ivanova A, Lohse M, Usadel B, Millar

AH, Whelan J (2009) Mapping metabolic and transcript temporal

switches during germination in rice highlights specific transcription

factors and the role of RNA instability in the germination process. Plant

Physiol 149: 961–980

Huang S, Greenway H, Colmer TD (2003) Anoxia tolerance in rice

seedlings: exogenous glucose improves growth of an anoxia-‘intoler-

ant’, but not of a ‘tolerant’ genotype. J Exp Bot 54: 2363–2373

Huang S, Greenway H, Colmer TD, Millar AH (2005) Protein synthesis by

rice coleoptiles during prolonged anoxia: implications for glycolysis,

growth and energy utilization. Ann Bot (Lond) 96: 703–715

Kato-Noguchi H, Ohashi C (2006) Effects of anoxia on amino acid levels in

rice coleoptiles. Plant Prod Sci 9: 383–387

Klok EJ, Wilson IW, Wilson D, Chapman SC, Ewing RM, Somerville SC,

Peacock WJ, Dolferus R, Dennis ES (2002) Expression profile analysis

of the low-oxygen response in Arabidopsis root cultures. Plant Cell 14:

2481–2494

Kordan HA (1974) The rice shoot in relation to oxygen supply and root

growth in seedlings germinating under water. New Phytol 73: 695–697

Kreuzwieser J, Hauberg J, Howell KA, Carroll A, Rennenberg H, Millar

AH, Whelan J (2009) Differential response of gray poplar leaves and

roots underpins stress adaptation during hypoxia. Plant Physiol 149:

461–473

Lasanthi-Kudahettige R, Magneschi L, Loreti E, Gonzali S, Licausi F,

Novi G, Beretta O, Vitulli F, Alpi A, Perata P (2007) Transcript profiling

of the anoxic rice coleoptile. Plant Physiol 144: 218–231

Lee CP, Eubel H, O’Toole N, Millar AH (2008) Heterogeneity of the

mitochondrial proteome for photosynthetic and non-photosynthetic

Arabidopsis metabolism. Mol Cell Proteomics 7: 1297–1316

Liu FL, Vantoai T, Moy LP, Bock G, Linford LD, Quackenbush J (2005)

Global transcription profiling reveals comprehensive insights into

hypoxic response in Arabidopsis. Plant Physiol 137: 1115–1129

Loreti E, Poggi A, Novi G, Alpi A, Perata P (2005) A genome-wide analysis

of the effects of sucrose on gene expression in Arabidopsis seedlings

under anoxia. Plant Physiol 137: 1130–1138

Magneschi L, Kudahettige RL, Alpi A, Perata P (2009) Comparative

analysis of anoxic coleoptile elongation in rice varieties: relationship

between coleoptile length and carbohydrate levels, fermentative me-

tabolism and anaerobic gene expression. Plant Biol (Stuttg) 11: 561–573

Mapelli S, Locatelli F (1995) The relation of rice coleoptiles, auxin-binding

protein, and protein-biosynthesis to anoxia and indoleacetic-acid. Russ J

Plant Physiol 42: 624–629

Menegus F, Cattaruzza L, Chersi A, Fronza G (1989) Differences in the

anaerobic lactate-succinate production and in the changes of cell sap pH

for plants with high and low resistance to anoxia. Plant Physiol 90: 29–32

Menegus F, Cattaruzza L, Mattana M, Beffagna N, Ragg E (1991) Response

to anoxia in rice and wheat seedlings: changes in the pH of intracellular

compartments, glucose-6-phosphate level, and metabolic rate. Plant

Physiol 95: 760–767

Menuz V, Howell KS, Gentina S, Epstein S, Riezman I, Fornallaz-

Mulhauser M, Hengartner MO, Gomez M, Riezman H, Martinou J-C

(2009) Protection of C. elegans from anoxia by HYL-2 ceramide syn-

thase. Science 324: 381–384

Millar AH, Trend AE, Heazlewood JL (2004) Changes in the mitochondrial

proteome during the anoxia to air transition in rice focus around

cytochrome-containing respiratory complexes. J Biol Chem 279:

39471–39478

Miyashita Y, Dolferus R, Ismond KP, Good AG (2007) Alanine amino-

transferase catalyses the breakdown of alanine after hypoxia in Arabi-

dopsis thaliana. Plant J 49: 1108–1121

Mocquot B, Prat C, Mouches C, Pradet A (1981) Effect of anoxia on energy

charge and protein synthesis in rice embryo. Plant Physiol 68: 636–640

Mustroph A, Lee SC, Oosumi T, Zanetti ME, Yang H, Ma K, Yaghoubi-

Masihi A, Fukao T, Bailey-Serres J (2010) Cross-kingdom comparison

of transcriptomic adjustments to low-oxygen stress highlights con-

served and plant-specific responses. Plant Physiol 152: 1484–1500

Nagai T, Makino A (2009) Differences between rice and wheat in temper-

ature responses of photosynthesis and plant growth. Plant Cell Physiol

50: 744–755

Narsai R, Howell KA, Carroll A, Ivanova A, Millar AH, Whelan J (2009)

Defining core metabolic and transcriptomic responses to oxygen avail-

ability in rice embryos and young seedlings. Plant Physiol 151: 306–322

Narsai R, Rocha M, Geigenberger P, Whelan J, van Dongen JT (2011)

Comparative analysis between plant species of transcriptional and

metabolic responses to hypoxia. New Phytol 190: 472–487

Opik H (1973) Effect of anaerobiosis on respiratory rate, cytochrome

oxidase activity and mitochondrial structures in coleoptiles of rice

(Oryza sativa L.). J Cell Sci 12: 725–739

Pegoraro R, Mapelli S, Torti G, Bertani A (1988) Indole-3-acetic acid and

rice coleoptile elongation under anoxia. J Plant Growth Regul 7: 85–94

Perata P, Guglielminetti L, Alpi A (1997) Mobilization of endosperm

reserves in cereal seeds under anoxia. Ann Bot (Lond) 79: 49–56

Perata P, Pozueta-Romero J, Akazawa T, Yamagushi J (1992) Effect of

anoxia on starch breakdown in rice and wheat seeds. Planta 188: 611–618

Raymond P, Al-Ani A, Pradet A (1985) ATP production by respiration and

fermentation, energy charge during aerobiosis and anaerobiosis in

twelve fatty and starchy germinating seeds. Plant Physiol 79: 879–884

Ricard B, Pradet A (1989) Anaerobic protein synthesis in different organs of

germinating rice seeds. Plant Physiol Biochem 27: 761–768

Ricard B, Rivoal J, Spiteri A, Pradet A (1991) Anaerobic stress induces the

transcription and translation of sucrose synthase in rice. Plant Physiol

95: 669–674

Rocha M, Licausi F, Araujo WL, Nunes-Nesi A, Sodek L, Fernie AR, van

Dongen JT (2010) Glycolysis and the tricarboxylic acid cycle are linked

by alanine aminotransferase during hypoxia induced by waterlogging

of Lotus japonicus. Plant Physiol 152: 1501–1513

Sachs M, Subaiah C, Saab I (1996) Anaerobic gene expression and flooding

tolerance in maize. J Exp Bot 47: 1–15

Setter TL, Waters I (2003) Review of prospects for germplasm improve-

ment for waterlogging tolerance in wheat, barley and oats. Plant Soil

253: 1–34

Siddiqui NU, Chung H-J, Thomas TL, Drew MC (1998) Abscisic acid-

dependent and -independent expression of the carrot late-embryogenesis-

abundant-class gene Dc3 in transgenic tobacco seedlings. Plant Physiol 118:

1181–1190

Taylor NL, Heazlewood JL, Day DA, Millar AH (2005) Differential impact

of environmental stresses on the pea mitochondrial proteome. Mol Cell

Proteomics 4: 1122–1133

Tijsen MJH, Peters SMA, Bindels RJM, van Os CH, Wetzels JFM (1997)

Glycine protection against hypoxic injury in isolated rat proximal

tubules: the role of proteases. Nephrol Dial Transplant 12: 2549–2556

Timmins M, Zhou W, Rupprecht J, Lim L, Thomas-Hall SR, Doebbe A,

Kruse O, Hankamer B, Marx UC, Smith SM, et al (2009) The metab-

olome of Chlamydomonas reinhardtii following induction of anaerobic

H2 production by sulfur depletion. J Biol Chem 284: 23415–23425

Trevelyan WE, Harrison JS (1952) Studies on yeast metabolism. I. Frac-

tionation and microdetermination of cell carbohydrates. Biochem J 50:

298–303

van Dongen JT, Frohlich A, Ramırez-Aguilar SJ, Schauer N, Fernie AR,

Erban A, Kopka J, Clark J, Langer A, Geigenberger P (2009) Transcript

and metabolite profiling of the adaptive response to mild decreases in

oxygen concentration in the roots of Arabidopsis plants. Ann Bot (Lond)

103: 269–280

van Dongen JT, Schurr U, Pfister M, Geigenberger P (2003) Phloem

Rice and Wheat Anoxia Responses

Plant Physiol. Vol. 156, 2011 1723 www.plant.org on December 28, 2013 - Published by www.plantphysiol.orgDownloaded from

Copyright © 2011 American Society of Plant Biologists. All rights reserved.

Page 81: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

metabolism and function have to cope with low internal oxygen. Plant

Physiol 131: 1529–1543

Wang G-H, Jiang Z-L, Chen Z-Q, Li X, Peng L-L (2010) Neuroprotective

effect of L-serine against temporary cerebral ischemia in rats. J Neurosci

Res 88: 2035–2045

Waters I, Morrels S, Greenway H, Colmer T (1991) Influence of O2 supply

prior to anoxia on tolerance to anoxia, alcoholic fermentation, and sugar

levels. J Exp Bot 42: 1437–1447

Weinberg JM, Nissim I, Roeser NF, Davis JA, Schultz S, Nissim I (1991)

Relationships between intracellular amino acid levels and protec-

tion against injury to isolated proximal tubules. Am J Physiol 260:

F410–F419

Went FW (1942) Growth, auxin and tropisms in decapitated Avena cole-

optiles. Plant Physiol 17: 236–249

Wessel D, Flugge UI (1984) A method for the quantitative recovery of

protein in dilute solution in the presence of detergents and lipids. Anal

Biochem 138: 141–143

Wu WW, Wang G, Baek SJ, Shen R-F (2006) Comparative study of three

proteomic quantitative methods, DIGE, cICAT, and iTRAQ, using 2D

gel- or LC-MALDI TOF/TOF. J Proteome Res 5: 651–658

Xu K, Xu X, Fukao T, Canlas P, Maghirang-Rodriguez R, Heuer S, Ismail

AM, Bailey-Serres J, Ronald PC, Mackill DJ (2006) Sub1A is an

ethylene-response-factor-like gene that confers submergence tolerance

to rice. Nature 442: 705–708

Yan B, Dai Q, Liu X, Huang S, Wang Z (1996) Flooding-induced membrane

damage, lipid oxidation and activated oxygen generation in corn leaves.

Plant Soil 179: 261–268

Yu J, Hu S, Wang J, Wong GK, Li S, Liu B, Deng Y, Dai L, Zhou Y, Zhang X,

et al (2002) A draft sequence of the rice genome (Oryza sativa L. ssp.

indica). Science 296: 79–92

Shingaki-Wells et al.

1724 Plant Physiol. Vol. 156, 2011 www.plant.org on December 28, 2013 - Published by www.plantphysiol.orgDownloaded from

Copyright © 2011 American Society of Plant Biologists. All rights reserved.

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Supplemental Tables

For supplemental tables to Study I, please see the CD fixed to the back page

of this thesis.

Alternatively, visit http://www.plantphysiol.org/content/156/4/1706/suppl/DC1

to download your copy.

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Chapter 3 Wheat genotype responses to anoxia

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Foreword to Study II

Having observed large differences in the way that rice and wheat respond to

anoxia (Study I), we were interested in determining whether the responses

seen in wheat were representative of several genotypes or a peculiarity

specific to our original genotype of interest (Calingiri). Of particular interest was

the absence of anoxic alanine accumulation in wheat, a response common to

many species treated with low oxygen.

Literature searches revealed a published report showing differential anoxia

tolerance among 11 wheat genotypes (Goggin and Colmer, 2007). Of those,

four were selected for further analysis under treatment regimes previously

employed in Study I. To allow more direct comparisons to this research,

several variables were modified; a 15˚ C temperature treatment was added to

supplement our original 28˚ C treatment, and roots as well as coleoptiles were

harvested.

Growth, electrolyte leakage, alcohol dehydrogenase activity and metabolite

profiles were analysed in all five genotypes. The results of Study II suggest a

strong dependence of the anoxic response on temperature, genotype and

tissue. The difficulty in assessing relative anoxia tolerance of different

genotypes is also discussed.

References Goggin DE, Colmer TD (2007) Wheat genotypes show contrasting abilities

to recover from anoxia in spite of similar anoxic carbohydrate metabolism. Journal of Plant Physiology 164: 1605-1611

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Wheat genotype responses to anoxia are tissue and

temperature-dependent

Rachel N. Shingaki-Wells, Shaobai Huang, Ralitza Alexova & A. Harvey Millar.

ARC Centre of Excellence in Plant Energy Biology, Centre for Comparative Analysis of

Biomolecular Networks, Bayliss Building M316 University of Western Australia, 35 Stirling

Highway, Crawley 6009, Western Australia, Australia.

Abstract

Wheat seedlings were compared to assess the variation in responses to anoxia

caused by temperature, tissue and genotype. Growth, electrolyte leakage and

alcohol dehydrogenase activity were measured and compared to metabolome

responses under anoxia. These analyses revealed that responses to anoxia are

highly dependent on context; not only do measurement types affect how anoxia

tolerance is defined, but so too does the tissue, temperature and genotype. In

our previous analysis, we found the absence of alanine accumulation in anoxic

wheat, a surprising result in light of the fact that alanine accumulation is

considered a classical anaerobic response. This study showed that this is not

specific to wheat, but is temperature, tissue and genotype-dependent. The role

of alanine in anoxia tolerance remains unclear. In general, seedlings performed

better at 15˚ C than at 28˚ C, and coleoptiles performed better than roots. This

study highlights the difficulty of assessing anoxia tolerance, partially because no

gold standard measurement of tolerance exists, and any apparent tolerance

appears to be highly dependent on other experimental factors.

Introduction

Environmental oxygen deprivation can result from flooding, water logging, or high

soil microbial activity. Rice (Oryza sativa) is a model crop, and is especially useful

in understanding mechanisms of tolerance to oxygen deprivation. Rice is highly

tolerant to anoxia in that it is able to survive and up-regulate enzymes involved in

anaerobic ATP production, namely glycolysis and ethanolic fermentation (Gibbs

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and Greenway, 2003). In contrast, wheat (Triticum aestivum) is relatively anoxia

intolerant (Perata et al., 1992; Perata et al., 1997), failing to rapidly adjust its

proteome in order to respond to an anaerobic environment (Shingaki-Wells et al.,

2011). The historical cultivation and environmental adaptation of these crops

might explain these differences; rice frequently grows in flooded and/or

anaerobic lowland soils whereas wheat is a dry-land winter crop. Additionally, the

increased rate of glycolysis known to occur under low oxygen is smaller in wheat

than in rice, suggesting energy metabolism is at least partially to blame for the

intolerance of wheat to O2 deprivation (Waters et al., 1991). Flooding is expected

to increase in frequency as a consequence of climate change (Bailey-Serres and

Voesenek, 2008), and thus it is expected that crops other than rice will be

affected by floods, with economic consequences such as yield loss. In 2011, for

example, floods in Queensland, Australia affected a landmass equal to the size of

both France and Germany (Perata et al., 2011). Other records indicate a

worldwide flood effect on 17 million km2 of land (Perata et al., 2011). Studying

highly utilised crops such as wheat will be useful for future improvement

strategies should they be required when flooding events become more common.

Compared to the model plants rice and Arabidopsis, the genome of wheat is

sizeable, complex and largely un-annotated. In addition, mutants are not easily

obtainable, making genetic research a challenge. Possible alternatives include

the use of pre-existing genetic variants, such as cultivars, which are often

accompanied by purported differences in tolerance to various stresses such as

waterlogging (Setter et al., 2009). Goggin and Colmer (2007) compared eleven

genotypes of wheat, which differed in seminal root elongation and degree of root

tissue K+ concentration recovery during resupply of O2 after 72 h of anoxia.

Despite differences in recovery ability, the genotypes did not differ in starch

content, soluble carbohydrate or activity of alpha-amylase in seeds, nor did they

differ in soluble carbohydrate content in roots (Goggin and Colmer, 2007).

However, it remains unclear how different wheat varieties respond to anoxia at

the metabolomic level. Not only does tolerance to anoxia differ between species

but it also differs between tissues. For example, rice roots are sensitive to anoxia

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whereas coleoptiles are highly tolerant, being the only tissue to grow in rice

seedlings never before exposed to oxygen. Anoxic rice roots respire at rates far

lower than that of coleoptiles, suggesting mitochondrial dysfunction, which might

be disadvantageous during re-oxygenation (Shingaki-Wells et al., 2011). Rice

root growth is inhibited by lower concentrations of ethanol when compared to

coleoptiles, even though both tissues show rapid ethanol accumulation during

anoxia as well as ADH induction (Kato-Noguchi and Kugimiya, 2001; Shingaki-

Wells et al., 2011). The above contrasts between roots and coleoptiles suggest

that understanding anoxia tolerance mechanisms will be tissue dependent. Due

to the well-documented anoxia tolerance of the rice coleoptile, we focus on

changes of metabolites in wheat coleoptiles.

We have previously investigated the metabolomic response of anoxic coleoptiles

from a wheat variety known as Calingiri. Surprisingly, alanine failed to accumulate

during anoxia, which was in dramatic contrast to rice coleoptiles (Shingaki-Wells

et al., 2011). This is particularly interesting because alanine classically

accumulates in anaerobic plant species (Gibbs and Greenway, 2003). Alanine

production is catalysed by an anoxia-inducible enzyme, Alanine

Aminotransferase, using the glycolytic end-product, pyruvate, as well as

glutamate. It is thought that alanine serves as an alternative end-product to

ethanol, which could easily diffuse out of membranes, to be a lost carbon

skeleton for the cell (Rocha et al., 2010). When oxygen returns, alanine could be

converted back to pyruvate, for eventual assimilation into aerobic metabolic

processes. It is also hypothesised that alanine has an important role in

consumption of pyruvate which would otherwise activate alternative oxidase or

interfere with respiration inhibition and consume what little oxygen is left in the

cell (Gupta et al., 2009; Zabalza et al., 2009; Rocha et al., 2010). This thinking

however, is not applicable when plants are anoxic. Alanine synthesis produces 2-

oxoglutarate, whose metabolism is a result of partial TCA cycle operation, and

this could result in the production of an extra ATP during the succinate synthesis

step (Rocha et al., 2010). We also found that upon supplementation with

alanine, only anoxic wheat showed a significant reduction in cell injury (Shingaki-

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Wells et al., 2011), indicating that alanine itself, not just its production or

metabolism, has some beneficial effect on anoxic cells. These findings prompted

our comparison of several wheat genotypes to see whether the stability of

alanine levels upon transition to anoxia was unique to the genotype we were

studying.

In this study we demonstrate variation in response to anoxia and post-anoxia in

five wheat genotypes previously studied by Goggin and Colmer (2007). We see

how metabolite profiles correlate with physiological parameters like recovery of

growth, tissue damage and induction of fermentation. We also introduced two

treatment temperatures, 28˚ C as an optimal growth temperature for rice used

previously (Shingaki-Wells et al., 2011) and 15˚ C, which may be more suitable

for wheat growth (Goggin and Colmer, 2007). We demonstrate the strong

influence that temperature has on tissue responses to O2 deprivation, and

discuss how these and other factors complicate the process of ranking genotype

tolerance to anoxia.

Materials and Methods

Plant Material

We obtained wheat varieties of Ducula-4, SARC, Spear, Carnamah, Calingiri

from the Department of Agriculture and Food of Western Australia (DAFWA).

Ducula-4, SARC, Spear, Carnamah have been previously tested by Goggin and

Colmer (2007). Calingiri was used in our previous study to compare with rice

(Shingaki-Wells et al., 2011).

Plant growth

Plants were grown according to previous studies (Shingaki-Wells et al., 2011).

Briefly, approximately fifty seeds of each genotype were placed in a 250 mL

growth vessel. Seeds were sterilised by adding 6 % [w/v] NaOCl for 10 min. After

rinsing three times with ddH2O, 200 mL culture solution was added (0.5 mM 2-

(N-morpholino) ethanesulfonic acid (MES), 0.4 mM CaSO4, pH 6.5). Lids

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containing a gas delivery tube and a gas outlet hole were screwed on tightly.

Compressed air was bubbled throughout each vessel for four days, in a 28˚ C or

15˚ C dark growth chamber. Anoxic treatments lasted for one day, by using high

purity nitrogen gas. Post-anoxic treatments were obtained by bubbling with

compressed air for 1 or 3 days.

Tissue length measurements and calculations

Root, leaf and coleoptile lengths were measured using a ruler at several stages of

development with or without an anoxic stress. Measurements were taken at the

same time every day. There were 5-10 seedlings for each genotype /

temperature / treatment combination; and each experiment was repeated three

times for proportional growth calculations. The observed seedlings were treated

as follows: 4 d air; 4 d air 1 d N2 (Anx5d); 4 d air 1 d N2 1d air (Re-ox6d); 4 d air 1 d

N2 3d air (Re-ox8d); 5 d air (Air5d); 6 d air (Air6d); 8 d air (Air8d). For a 1 d recovery

treatment the proportional growth calculation was: [(Re-ox6d) - (Anx5d)] / (Anx5d)

*100. For a 3 d recovery treatment: [(Re-ox8d) - (Anx5d)]/ (Anx5d) *100. Control

calculations were: [(Air6d) - (Air5d)] / (Air5d) *100 or [(Air8d) - (Air5d)] / (Air5d) *100, for 1

d or 3 d of elongation, respectively.

Metabolite extraction and GCMS analysis

Metabolites were extracted by placing 25 ± 5 mg tissue into 2 mL Eppendorf

tubes containing a stainless steel grinding bead. Samples were snap frozen in

liquid nitrogen. Tubes were placed in a liquid nitrogen-cooled mill rack for

homogenisation twice at 15 shakes sec-1 for 2 minutes. Cold metabolite

extraction medium (500 μL; -20˚ C; 85 % [w/v] HPLC-grade methanol, 15 %

[w/v] untreated MilliQ water, and 100 ng μL-1 ribitol) was added to each sample,

which was then mixed at 1400 rpm for 20 min at 65˚ C using a thermomixer.

Samples were centrifuged at 20, 000 x g for 3 minutes at room temperature. 60

μL of supernatant was transferred to a low-volume insert and this was dried

down in a vacuum centrifuge. Inserts were transferred to 2 mL eppendorf tubes

for storage at -80˚ C. Derivatisation was carried out on samples that were re-

dried for 30 min. 20 μL of 20 mg mL-1 methoxyamine hydrochloride in anhydrous

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pyridine was added to each sample for incubation at 30˚ C for 90 min at 1400

rpm. Then, 30 μL room temperature MSTFA was added and incubated at 37˚ C

for 30 min at 1400 rpm. After this, 10 μL of an n-alkane mix was added (0.029%

[v/v] n-dodecane, 0.029% [v/v] n-pentadecane, 0.029% [w/v] n-nonadecane,

0.029% [w/v] n-docosane, 0.029% [w/v] n-octacosane, 0.029% [w/v] n-

dotriacontane, and 0.029% [w/v] n-hexatriacontane dissolved in anhydrous

pyridine). Samples were incubated at room temperature for 30 minutes prior to

GC-MS analysis, the methods of which have been described previously (Howell

et al., 2009). Briefly, 1 μL of sample was injected into an Agilent 7890 GC fitted

with an Agilent 5975 MSD. The carrier gas, helium, had a constant flow of 1

mL.min-1. The inlet temperature was 300˚ C and the initial oven temperature was

set at 70˚ C for 1 min. The oven temperature was increased to 76˚ C at 1˚ C. min-

1, then to 325˚ C at a rate of 6˚ C.min-1. This temperature was held for 8 minutes.

The capillary column used was a Varian Factor 4 (VF-5ms, 30 m x 0.25 mm,

0.25 μm; 10 m EZ-Guard). The MSD transfer line heater was set at 300˚ C, the

MS quadrupole at 150˚ C and the source at 230˚ C. The mass detection range

was set at 40-600 atomic mass units.

The generated data was collected and analyzed using Chemstation GC/MSD

Data Analysis Software (Agilent Technologies). Peak retention time and mass

spectra were manually inspected and checked against National Institute of

Standards and Technology (NIST) mass spectra library. Peak areas were

normalised to tissue weight and ribitol signal. ANOVAs were performed on

normalised and log-transformed data to give Tukey post-hoc p-values. Ratios

were calculated between anoxic and aerated samples using data normalised to

tissue mass and the peak area of a ribitol quantifier ion.

ADH

Protein extracts from snap frozen tissue were placed in 2 mL tubes with stainless

steel beads for homogenisation in cooled racks at 15 shakes/s for 2 mins. This

was repeated with racks turned around. Extraction buffer was added to tissue at

a 14:1 ratio (125 mM MES, 110 mM NaCl, 1 mM ethylenediaminetetraacetic acid

(EDTA), 0.5 mM thiamine pyrophosphate (TPP), 2.5 mM MgSO4.7H2O and

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freshly added 2 mM dithiothreitol (DTT)). This was mixed for 2 mins at 15

shakes/s with care taken to ensure racks were cold. The homogenate was then

centrifuged at 16, 000 x g for 4 min at 4˚ C and the resulting supernatant

transferred to a new tube and stored on ice. ADH activity was measured at 25˚ C

spectrophotometrically at 340nm in a 1 mL reaction volume.

880 μL of a solution containing N-Tris(hydroxymethyl)methyl-2-

aminoethanesulfonic Acid (TES) and acetaldehyde (pH 7.5) was added so that

final assay concentrations were 50 mM and 10 mM, respectively. Next, 100 μL of

a freshly-made solution containing reduced nicotinamide adenine dinucleotide

(NADH) was added to the cuvette so that the final assay concentration was 0.17

mM. Finally, 20 μL of ADH extract was added and promptly mixed using a

pipette before taking spectrophotometric measurements. To control for ADH-

independent NADH oxidation, absorbance in the absence of acetaldehyde or

ADH extract was measured for six minutes with absorbance changes (if there

were any) subtracted from sample measurements. The spectrophotometer

model used was a U- 2810 spectrophotometer (Hitachi High-Technologies

Corporation, Tokyo, Japan) with the measurements processed by computer

software (Hitachi UV Solutions Application, program no. 1344331-08, build 414).

To calculate the specific activity of ADH, total protein concentration of the tissue

extract was measured using the Bradford method (Bradford, 1976).

Cell leakage assays

Cell leakage assays were adapted from a previous study (Yan et al., 1996).

3 seedlings were submerged in 25 mL ddH2O in a 50 mL falcon tube. Samples

were placed in the dark at room temperature (approximately 19˚ C) for 1 hour.

Samples were gently mixed and electrical conductivities measured and recorded

as C1. Samples were boiled, then placed in an icebox for 20 minutes and allowed

to equilibrate to room temperature. A second measurement of electrical

conductivity was taken (C2). The ratio of C1 to C2 was calculated as a proxy for

cell leakage.

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Results

Assessment of anoxia tolerance using recovery growth

To understand the impact of anoxia and temperature on wheat growth, we

measured length of coleoptiles, leaves, primary roots and seminal roots in

aerated seedlings as well as seedlings subjected to one day of anoxia followed

by one and three days of re-oxygenation. These experiments were performed

three times, allowing the calculation of elongation rates (n=10, n=10, n=5). The

absolute growth data with length at different time points are given in

Supplemental Figure 1. Figure 1 represents relative growth rate, comparing

seedlings recovering from anoxia to those kept under constant aeration. We

calculated proportional growth of seedlings that were 6 or 8 days of age, as a

percentage of tissue length of seedlings that were 5 days of age (4d air 1d N2 for

the treatment; or 5d air for the control). Details on calculations are described in

the methods section.

Temperature has a significant impact on the length of all tissues measured (p-

val<0.001 for all tissues), with seedlings at 15˚ C showing apparent

developmental delays when compared with seedlings at 28˚ C (Supplemental

Figure 1a-d). After three days of re-oxygenation, a 28˚ C anoxic treatment

strongly inhibited the recovery of primary root elongation in Ducula-4, Spear and

Carnamah (Figure 1d), presumably due to the cell death in elongating root tips.

Looking from a more immediate perspective (1d re-oxygenation), only Calingiri

failed to show significant anoxic growth inhibition at 28˚ C, although this could be

due to large replicate variation (Figure 1c). In terms of the 3 d recovery of

seminal root elongation at 28˚ C, only Spear showed significant inhibition, with

Ducula-4 showing significant inhibition after 1 d recovery but not at 3 (Figure 1c-

d).

After a 28˚ C anoxia treatment, only the coleoptiles of Calingiri and Spear showed

higher proportional growth than control seedlings (Figure 1c-d). However, these

data should be interpreted with caution because Calingiri is developmentally

delayed compared to the other four genotypes (4d air; p<0.001; Supplemental

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Table 1a), with Carnamah and Ducula-4 coleoptiles at their maximum length at

four days of age (Supplemental Figure 1a; Supplemental Table 1b). We also

measured leaf elongation at a developmental stage where leaves were beginning

to emerge out of coleoptiles. One day of anoxia had less of an impact on the

recovery of leaves, demonstrated by the fact that proportional growth

measurements after 3 days of re-oxygenation are not significantly different

between seedlings kept under control conditions and those treated with anoxia

(Figure 1d). Leaf lengths are considerably larger in all genotypes by 3 d re-

oxygenation when compared to leaf lengths immediately after anoxia (4d air 1d

N2; Supplemental Table 2b). However, leaves from 8 d old control seedlings

were still significantly larger than those from seedlings treated with anoxia and re-

oxygenated for 3 days (at both temperatures), with the exception of 15˚ C

Calingiri leaves (Supplemental Figure 1b, Supplemental Table 2a).

At 15˚ C, SARC was the only genotype to show growth rate inhibition of leaves

and primary roots after 1 d re-oxygenation, but by 3 d re-oxygenation this

inhibition was no longer significant (Figure 1a-b). For 15˚ C seminal roots, only

Spear showed growth rate inhibition one day post-anoxia, but again, this lost its

statistical significance after three days of re-oxygenation (Figure 1a-b). 15˚ C

coleoptiles recovering from anoxia for 3 days showed significantly higher

proportional growth compared to aerated controls in all genotypes except SARC

(Figure 1b). Impressively, 15˚ C coleoptiles, which still have growth capacity at 4

days of age (Supplemental Table 1b), were not significantly shorter when

subjected to anoxia/re-oxygenation, compared to continuously aerated controls

(Supplemental Figure 1a; Supplemental Table 2a). The same is true for 28˚ C

coleoptiles (Supplemental Figure 1a; Supplemental Table 2a) but this is

complicated by the fact that at 4 days of age, coleoptiles are close to or at their

maximum length. Coleoptiles at 15˚ C show rapid growth resumption post-

anoxia (Supplemental Figure 1a; Supplemental Table 2b). At both temperatures,

the coleoptile is the only tissue where all genotypes have equivalent lengths

when comparing 8-d-old seedlings subjected to control treatments with those

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under anoxia/re-oxygenation (Supplemental Table 2a; Supplemental Figure 1).

This growth data suggests that the coleoptile is the most anoxia tolerant tissue.

Assessment of anoxia tolerance using electrolyte leakage measurements

We measured electrolyte leakage as an independent measure of anoxia

tolerance in wheat varieties grown at 15˚ C and 28˚ C (Figure 2). The ratio of

electrolyte leakage by whole seedlings after 1 h incubation (C1) and after boiling

(C2) can be used as a proxy for cell damage. At 28˚ C, all genotypes except

Calingiri had significantly higher leakage values after one day of anoxia,

compared to the aerated control (Figure 2b), suggesting that Calingiri is more

anoxia tolerant than the other genotypes. At 15˚ C, anoxia did not increase

electrolyte leakage in any of the genotypes (Figure 2a). These results suggest

that anoxia at higher temperatures is more stressful for wheat seedlings,

however, it must be noted that leakage levels for aerated seedlings at 15˚ C are

higher than seedlings grown at 28˚ C. The electrolyte leakage after boiling (C2) is

much lower at 15˚ C when compared to 28˚ C, which could explain the high

C1/C2 values in 15˚ C seedlings (data not shown). Although speculative, it is

possible that this discrepancy in apparent electrolyte levels is caused by

developmental differences between the smaller seedlings grown at 15˚ C. In

conclusion, results of our cell leakage suggest Calingiri is exceptional in terms of

its anoxia tolerance.

Assessing responses to anoxia by measuring ADH activity in coleoptiles

To check whether our measures for anoxia tolerance were linked to induction of

other classical responses to anoxia, we estimated the rate of activity for alcohol

dehydrogenase (ADH) in wheat coleoptiles. ADH is an important enzyme in the

transition to anaerobic metabolism, since the NAD+ produced could promote

maintenance of NAD+-dependent glycolytic reactions. Overall, ADH activity is 4-

11 fold higher at 28˚ C when compared to 15˚ C (Figure 3). At 28˚ C, Ducula-4

coleoptiles treated with anoxia have almost twice the activity of those kept under

aeration (Figure 3b). All other genotypes do not show significant induction,

although Calingiri is significant at the 94% confidence level (Supplemental Table

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3). At 15˚ C, only Calingiri shows significant induction (54%) during anoxia

(Figure 3a). These results suggest that anoxic alcohol dehydrogenase induction

is temperature-dependent, and if ADH induction is a measure of anoxia

tolerance, then Calingiri and Ducula-4 stand out as particularly tolerant.

Metabolite profiles of coleoptiles and roots

The shift from air to anoxia causes dramatic changes to the metabolome of rice

and wheat coleoptiles (Shingaki-Wells et al., 2011). We were interested in

investigating whether wheat genotypes, which apparently differ in their sensitivity

to anoxia (Goggin and Colmer, 2007), have distinct metabolite profiles that

underlie or correlate with tolerance to oxygen deprivation. We conducted

metabolomic analysis of coleoptiles and roots (seminal and primary) from all five

wheat varieties in response to anoxia at 15˚ C and 28˚ C. Table 1 shows the fold

changes (anoxia/air) of individual metabolites belonging to different

classifications.

Overall, the depletion of sugars, TCA cycle-related metabolites and accumulation

of amino acids were observed in roots and coleoptiles across varieties after

anoxic treatment (Table 1). This pattern is much more obvious at 15˚ C than at

28˚ C (Table 1), suggesting that such a shift of metabolism is linked to the

improved anoxia tolerance as observed above.

There was no metabolite in this set that showed a consistent direction of change

across tissues, genotypes and temperatures. GABA shows significant and large

increases under anoxia in 15˚ C roots and coleoptiles. Although the ratios range

from 4.76-17.98 at 28˚ C, no ratios at this temperature reached the significance

threshold due to large variation within the five biological replicates (Supplemental

Figure 2). Individual samples could not be considered outliers since the other

metabolite signals in those replicates were typical in their intensities.

At 15˚ C, alanine significantly accumulates under anoxia in the roots and

coleoptiles of all genotypes (Table 1). At 28˚ C, only the coleoptiles of Carnamah

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showed anoxic alanine accumulation, and in roots, accumulation was seen in

SARC, Spear and Calingiri. These results suggest that our prior study, in which

we reported the surprising observation that 28˚ C Calingiri coleoptiles fail to

accumulate alanine (Shingaki-Wells et al., 2011), is a response that is

temperature and genotype dependent rather than a feature of wheat itself.

Calingiri coleoptiles at 15˚ C are the only samples in this experiment to show

accumulation of fructose under anoxia (Table 1). All other samples show no

significant difference or rapid depletion of this sugar. Roots at 28˚ C, are the

most extreme in their depletion, followed by roots at 15˚ C. Calingiri is the only

genotype to not show significant depletion of fructose in 15˚ C roots. In 28˚ C

roots, fructose decreases by about 2.5 fold in anoxic Calingiri, whereas the other

genotypes show decreases ranging from 12 (Carnamah) to 63 fold (Ducula-4).

Glucose depletion is also most apparent in 28˚ C roots, followed by 15˚ C roots.

Glucose responses in Calingiri fail to stand out from other genotypes.

We also observed genotypic responses to anoxia across tissues and

temperatures. For example, citric acid, 2-oxoglutaric acid, malic acid, 4-

hydroxyproline, aspartic acid, shikimic acid and threitol/erythritol depletion

occurs in all temperature/tissue combinations of Ducula-4 (Supplemental Table

4). The TCA cycle metabolites, with the exception of succinate, appear to show

greater depletion in Ducula-4 than in Calingiri. In Calingiri and Carnamah, there

were no metabolites that showed a consistent response across tissues and

temperatures. Metabolite responses in 28˚ C Calingiri coleoptiles strongly

contrast to 28˚ C roots and 15˚ C coleoptiles/roots of Calingiri in that their

responses were much more subtle. The latter three sample types showed

consistent responses in 2-oxoglutaric acid (down) alanine (up) and proline (up).

Compared to these samples, which had 17-27 metabolites displaying significant

responses under anoxia, 28˚ C Calingiri coleoptiles only had 3 significant

metabolite responses. These metabolites were sucrose (down), aspartic acid

(down) and glycerol (up).

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Succinate is the only TCA cycle metabolite that shows accumulation, albeit

inconsistently. For example, succinate accumulates in all genotypes at 28˚ C in

roots. It also accumulates in 15˚ C Carnamah roots and the 28˚ C coleoptiles of

Ducula-4 and Carnamah. Surprisingly, anoxic succinate depletion was also

observed. The 15˚ C roots of SARC, Spear and Calingiri, as well as the 15˚ C

coleoptiles of SARC and Spear had up to 2.8 fold less succinate under anoxia

when compared to air.

Amino acid responses to anoxia vary widely among tissues and temperatures

(Table 1). At 15˚ C, coleoptiles show significant increases in many metabolites,

with beta-alanine, alanine, glycine, isoleucine, leucine, lysine, threonine, tyrosine

and GABA showing consistent increases across all five genotypes. Amino acids

decreasing in anoxic coleoptiles at 15˚ C did so inconsistently across genotypes.

Glutamine decreased in all genotypes except Spear. Other depleted amino acids

like 4-hydroxyproline and aspartic acid decreased in Ducula-4/Spear and

Ducula-4/SARC/Carnamah, respectively. 15˚ C roots show the second strongest

amino acid response under anoxia, with alanine and GABA significantly

increasing across all genotypes. Amino acids that decreased under anoxia were

not limited to 4-hydroxyproline and aspartic acid, but also glutamate in Ducula-4,

SARC and Spear as well as phenylalanine in Ducula-4.

In conclusion, metabolite profiles in wheat roots and coleoptiles at low and high

temperature responded differentially to anoxia, presumably contributing to

variation in anoxia tolerance. Higher temperatures appear to dampen the strong

amino acid responses that typically occur during anoxia, and promote the

depletion of sugars and TCA cycle metabolites. When comparing tissues, it

appears that roots show stronger depletion of sugars/TCA cycle intermediates,

with the exception of succinate. It is more difficult to detect patterns of difference

in the responses of amino acids across tissues. From a genotypic perspective,

the metabolite responses to anoxia in Ducula-4 greatly contrast to that of

Calingiri. Ducula-4 shows stronger depletion of sugars/TCA cycle intermediates

as well as fewer significant increases in many amino acids, with the exception of

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4-hydroxyproline and aspartic acid, which deplete more rapidly in anoxic Ducula-

4 when compared to Calingiri.

Discussion

It is a complicated process to assess mechanisms of anoxia tolerance in

plants.

Assessing anoxia tolerance in plants can be simplified to observing how long

plants survive a low-oxygen event and how productivity is affected. Assessing

the molecular mechanisms underlying this success is considerably more

complicated. We set out to look at various factors such as growth resumption,

seedling damage, fermentative capacity and metabolome re-modelling, in an

attempt to define what a successful and unsuccessful response to anoxia entails.

The anoxia tolerance of rice can be attributed to a large list of responses and

factors. Furthermore, there are different rice varieties that vary in their

mechanisms of anoxia tolerance. For instance, some varieties may exercise

metabolic acclimation at the transcript or protein level and others might undergo

rapid shoot growth when submergence threatens contact to air (Voesenek et al.,

2006). The availability of light for photosynthesis might alter O2 availability as well

as other factors like aerenchyma formation (Gibbs and Greenway, 2003). These

factors, as well as variation in treatment regimes and developmental stages,

make assessing the anoxia tolerance of different plants complicated. In the case

of anoxic coleoptile elongation, differences in length could not be explained by

carbohydrate content or the expression of transcripts encoding glycolytic/

fermentation enzymes and expansins (Magneschi et al., 2009; Magneschi et al.,

2009). Ethanol production on the other hand, correlated with anoxic coleoptile

elongation (Magneschi et al., 2009). This apparent contradiction might be

explained by the selective translation that occurs under low oxygen in

Arabidopsis (Branco-Price et al., 2008). Nevertheless, elongation itself might only

be advantageous in genotypes where the benefit outweighs any energetic cost.

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Considerable variation in the anoxia-tolerance of the wheat variety Ducula-4 has

been reported (Setter et al., 2009). Initial trials conducted in Obregon, Mexico,

showed the high tolerance of Ducula-4 to waterlogging (vanGinkel et al., 1992;

Sayre et al., 1994), whereas trials conducted in Australia showed many other

genotypes outperforming Ducula-4 (Setter, 2000; Setter et al., 2009). Personal

observations indicate that the performance of Ducula-4 in Kaithal, India, is very

poor in waterlogged conditions (Setter et al., 2009). Setter and colleagues (2009)

attribute this performance difference to the more optimal conditions found in

Mexico, including optimal temperatures, better nutrition and absence of post-

submergence drought. This hypothesis requires further study. It is also proposed

that waterlogging tolerance is accompanied by a set of consequences that are

rarely considered, that is, the threat posed by element toxicities (e.g. Na, Mn, Fe)

(Setter et al., 2009). Such toxicities can make experiments on different varieties

hard to replicate in the field (Setter et al., 2009). It was recently shown that the

transcription factor SUB1A not only acts to improve submergence tolerance but

also post-submergence dehydration stress (Fukao et al., 2011). Thus, the

discrepancies seen in low oxygen research might be a product of differences in

field conditions that exert large and unintended co-stresses. Furthermore,

practical characteristics of the experiment such as what is measured, stress

duration and developmental stage are also likely to contribute to large variation

between research groups.

A comparison of our data to prior research.

In our current study we used electrolyte leakage, ADH induction, growth recovery

and metabolite profiling to determine the relative anoxia tolerance of five wheat

genotypes. This study was inspired by our previous research, which compared

rice (cv. Amaroo) and wheat coleoptiles (cv. Calingiri) at 28˚ C (Shingaki-Wells et

al., 2011). We were surprised to find that Calingiri coleoptiles did not accumulate

alanine under anoxic stress, as this is a widely-reported response under low

oxygen (Narsai et al., 2011). Furthermore, the shoots of the wheat variety MEK

86, at 25˚ C, showed anoxic accumulation of alanine (Menegus et al., 1989). We

were interested in knowing if this was unique to wheat coleoptiles or to Calingiri

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specifically, and set out to assess the metabolome, among other measures, in

various wheat genotypes.

With a myriad of varieties to choose from, we searched the literature to reduce

our genotype selection down to five. Goggin and Colmer (2007) had published a

comprehensive comparison of 11 wheat genotypes, measuring seminal root

elongation, root recovery of K+ concentration, root ethanol production as well as

seed starch and alpha-amylase activity. We included our prior genotype of

interest, Calingiri, which was not included in Goggin and Colmer’s research, and

chose Ducula-4/SARC as our top performers, Carnamah as our middle, and

Spear as our bottom performer in terms of post-anoxic root elongation and K+

recovery (Goggin and Colmer, 2007).

Although anoxic Ducula-4 seedlings showed some of the highest EL in our

study, this was only significantly different to Calingiri seedlings, which had the

lowest EL, at the 94% confidence level (p-val=0.054). We are able to conclude

that 28˚ C Calingiri seedlings, which was the only genotype to show no significant

increase in EL when transferred to anoxia, is a unique genotype in this

characteristic. Goggin and Colmer (2007) on the other hand, did not study

Calingiri and found 15˚ C Ducula-4 to be a top performer in that after 3 days of

anoxia and subsequent re-aeration, it showed the highest recovery of tissue K+

concentrations in the expanded zone of the roots. The complexity of comparing

our results with those of Goggin and Colmer’s can arise from their use of

different tissues (seedling vs. roots in their study), the presence of a hypoxic pre-

treatment (absent in our study), age (4-5d vs. ~6-7d in their study), duration of

anoxia (1d vs. 3d in their study) as well as measurement types (electrolyte

leakage vs. K+ in their study).

Goggin and Colmer analysed ethanol production in 15˚ C excised anoxic roots

supplemented with glucose and found that there was no difference between

genotypes and over the time spent under anoxia (24-96h). This is consistent with

our work on ADH activity in 15˚ C coleoptiles, where Ducula-4, SARC, Spear and

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Carnamah show no significant difference in ADH activity, independent of

genotype or O2 availability (Figure 3A). Calingiri, which was not studied by Goggin

and Colmer, was an exception showing significant induction under 24h anoxia

(Figure 3A). Although ethanol production may not contribute to the differences in

anoxia tolerance between Ducula-4, SARC, Spear and Carnamah (Goggin and

Colmer, 2007), ADH activity induction could explain the success of 15˚ C

Calingiri, provided pyruvate decarboxylase activity was not limiting. At 28˚ C, the

coleoptiles of Ducula-4 showed significant ADH induction under anoxia (mean

difference -1.24 units; p-val=0.049; Figure 3b, Supplemental Table 3), with

Calingiri not meeting the significance threshold due to replicate variation (mean

difference -0.89 units; p-val=0.308; Supplemental Table 3). In our previous

study, 28˚ C Calingiri coleoptiles, leaves and roots all showed significant ADH

induction after 24 h anoxia (Shingaki-Wells et al., 2011).

Post-anoxic root elongation retention (72h anoxia then 72 h recovery) at 15˚ C

relative to continuously aerated controls was highest in SARC (100 %), followed

by Ducula-4 (72 %), Carnamah (22 %) and Spear (0 %) (Goggin and Colmer,

2007). For 15˚ C seminal root sums, post-anoxic (4d air, 1d anoxia, 3d air)

Ducula-4 seminal roots were 72 % of the length of their aerated controls (8d air).

SARC, Carnamah, Calingiri and Spear followed at 60, 49, 49 and 45 %,

respectively (Supplemental Figure 1C). The order of length retention is consistent

between studies, even though treatments and measurement types (sum vs.

average in their study) differed. Using the measure of proportional growth we see

no significant difference between control and stressed seedlings in any of the

genotypes (Figure 1b).

Goggin and Colmer also compared 15˚ C seedlings treated with a hypoxic pre-

treatment and 72 h anoxia to see whether they differed in root and seed soluble

carbohydrate, seed starch and alpha amylase activity. They found minimal

genotypic differences and concluded that carbohydrate metabolism cannot

explain recovery ability variation between genotypes (Goggin and Colmer, 2007).

Surprisingly, soluble carbohydrate concentrations in roots decreased more

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during 72 h aeration than during 72 h anoxia. Seed starch was lower under

anoxia, and in concordance, seed soluble carbohydrates were higher, even

though alpha amylase activity was lower under anoxia (Goggin and Colmer,

2007). A lack of alpha-amylase induction in anoxic wheat seedlings is thought to

underlie the failure of wheat to anoxically germinate (Perata et al., 1992). Our

metabolomics analyses showed that the 15˚ C roots (primary and seminal) of

Ducula-4, SARC, Spear and Carnamah showed significant reductions in

fructose, but for glucose, anoxic reductions were limited to Ducula-4, Carnamah

and Calingiri (Table 1). Sucrose was significantly depleted in SARC and Calingiri

only (Table 1). This data suggests that the four genotypes included in Goggin

and Colmer’s study do differ in terms of 15˚ C root carbohydrate metabolism, at

least for the conditions we studied (24 h anoxia). Although, it is important to note

that metabolome analysis may have differed if seminal and primary roots were

separated.

The importance of ADH: is it a predictor of performance under anoxia?

When rice is transformed with an antisense Adh1 construct so that its activity is

only 4-8% of untransformed plants, seedlings show reduced anaerobic ethanol

production and coleoptile elongation (Matsumura et al., 1998; Rahman et al.,

2001). Although we are unaware of any wheat ADH mutants, the adh null

mutants of other intolerant species such as Arabidopsis, barley and maize show

reduced tolerance to low oxygen including increased sensitivity to acetaldehyde

as well as reduced seed viability and germination during submergence

(Schwartz, 1969; Harberd and Edwards, 1982; Jacobs et al., 1988; Johnson et

al., 1994).

It is also believed that a hypoxic pre-treatment of wheat roots, which increases

activity of PDC and ADH, improves tolerance in subsequent anoxia treatments

(Waters et al., 1991). Pyruvate decarboxylase appears to be rate-limiting in

ethanolic fermentation (Waters et al., 1991). For example, Arabidopsis PDC over-

expressers, but not ADH over-expressers, show improved survival under hypoxia

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(Ismond et al., 2003). All this suggests that low ADH activity under low oxygen is

likely to confer reduced tolerance to anoxia.

In this study, the only genotype to show anaerobic ADH activity induction in 15˚

C coleoptiles was Calingiri. For 28˚ C coleoptiles, only Ducula-4 showed

significant induction. In our previous study, Calingiri did show significant ADH

activity induction (Shingaki-Wells et al., 2011). The question is whether Calingiri

and Ducula-4 coleoptiles at 15˚ C and 28˚ C, respectively, are top performers in

the other measurements that were made to determine anoxia tolerance.

Tissue anoxia tolerance, the influence of temperature and the validity of

the electrolyte leakage assay

Responses to anoxia were conditional on the temperature at which seedlings

were grown in. This has been reported previously, where wheat roots lose

elongation potential at 25˚ C after only 10 h anoxia compared to seedlings at 15˚

C, where after 20 h anoxia, 50-70 % of the elongation potential remained

(Waters et al., 1991). In our study, 15˚ C seminal roots showed no significant

difference in 3 d proportional growth between post-anoxic and aerated controls

(Figure 1b). At 28˚ C, the case was similar, except for Spear, which did show a

significant reduction in 3 d proportional growth post-anoxia (Figure 1d). 28˚ C

primary roots appeared to be more sensitive to anoxia than seminal roots, in that

Ducula-4, Spear and Carnamah showed significant proportional growth inhibition

post-anoxia (Figure 1d). At 15˚ C, primary roots did not show proportional growth

consequences (Figure 1b). Coleoptiles and leaves at 28˚ C appeared better off

than roots, showing no proportional growth consequences across all five

genotypes post-anoxia. In concordance, at 15˚ C, the coleoptiles and leaves

were the only tissues to show higher post-anoxic proportional growth,

suggesting coleoptiles are more tolerant to anoxia than roots. The greater anoxia

tolerance of coleoptiles relative to roots has been documented. For example,

anoxic growth suppression is high in rice roots but not coleoptiles, whereas ATP

levels, ADH activity, ethanol production and sugar concentrations are higher in

anoxic coleoptiles (Kato-Noguchi et al., 2011).

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While no significant differences were seen between 15˚ C anoxic and aerated

seedlings, the leakage of aerated seedlings was higher at 15˚ C than at 28˚ C

(Figure 2). The growth data of this study and that of older studies (Waters et al.,

1991) indicates that anoxia at 28˚ C is a harsher stress than at 15˚ C (Figure 1).

Thus if electrolyte leakage is indicative of cell damage, it is expected that anoxic

leakage values would be higher in the 28˚ C treatment compared to the 15˚ C

treatment. On the other hand, cell leakage increases in anoxic seedlings are only

evident at 28˚ C, which is consistent with the idea that anoxia at warmer

temperatures is more stressful than at cooler temperatures.

Electrolyte leakage is a standard measure of cell damage in much research

(Patterson et al., 1976; Yan et al., 1996), yet we are left with the question of

whether this assay measures exclusively what it is purported to. Recent research

has revealed that senescing leaves of barley show increased electrolyte leakage

(EL) despite the fact that there was no significant increase in membrane damage.

The lines of evidence that indicate this include (1) selective leakage of ammonium

when K+ was more abundant (2) absent increase in a cell death stain that is

dependent on membrane damage and (3) increased EL in leaves that were

reversing senescence, a response that requires maintenance of cellular

compartmentalisation (Rolny et al., 2011). Since EL does not appear to

exclusively measure membrane damage, this may explain why 15˚ C control

seedlings show higher EL than 28˚ C seedlings. Interestingly, sterol content is

lower in 28˚ C anoxic roots of all five genotypes, compared to aeration (Table 1).

If this is indicative of membrane damage or membrane composition changes,

alterations in EL could result. However, as this study measured EL of whole

seedlings, the individual contribution of each tissue to EL is unknown.

It is known that there is a net K+ and phosphate uptake when coleoptiles

supplemented with exogenous glucose are treated with anoxia for 60 h (Colmer

et al., 2001). K+ is important for maintaining osmotic pressure, which in turn

promotes elongation of anoxic coleoptile cells (Menegus et al., 1984). Growth of

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shoots and roots also occurs during re-aeration. In contrast, when coleoptiles

are not supplemented with glucose, post-anoxic recovery was reduced and K+ /

phosphate losses were apparent (Colmer et al., 2001). Reduced tolerance to

anoxia in the absence of exogenous glucose is also inferred via pronounced

degeneration of anoxic mitochondria (Vartapetian et al., 1976), reduced ATP

concentrations (Huang et al., 2005) and a reduction in elongation potential

(Waters et al., 1991). Additionally, rates of net uptake of K+ and phosphate are

associated with ethanol production rates by anoxic rice coleoptiles. Conversely,

losses in K+ and Cl- occurred where glucose was not supplied and during re-

aeration, net rates of uptake were stunted in sugar-deprived samples (Huang et

al., 2005). In our previous study, we showed electrolyte leakage of 28˚ C wheat

seedlings subjected to 3 d of anoxia to be far greater than that of rice, which

correlated with the known tolerance of rice to low oxygen (Shingaki-Wells et al.,

2011). All this suggests that ion leakage and uptake is associated with,

respectively, reduced and improved tolerance to anoxic stress.

These measurements are complicated by the fact that the whole seedling was

used, as opposed to excised coleoptiles, as in the ADH assay. The decision to

keep seedlings intact was a precaution that was taken to minimise the

contribution that excision would have to electrolyte leakage.

Anoxia tolerance of Calingiri and Ducula-4

As discussed above, we set out to determine whether Calingiri was a unique

wheat genotype to explain the surprising result that alanine did not accumulate in

28˚ C rice coleoptiles subjected to anoxia (Shingaki-Wells et al., 2011). Calingiri

seedlings at 28˚ C performed well in terms of electrolyte leakage, and its

coleoptiles significantly increased ADH activity under anoxia at 15˚ C, only just

failing to meet the significance threshold at 28˚ C. 15˚ C growth regimes revealed

the coleoptiles of Calingiri as among three other genotypes to show significant

increases in proportional growth (3 d) post-anoxia relative to continuous aeration.

In contrast, Calingiri leaves were alone in maintaining growth rates (Figure 1b). At

28˚ C, Calingiri and Spear showed higher proportional growth rates (3d) than

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their respective controls and in primary roots, Calingiri was the only genotype to

not show significant losses in proportional growth post-anoxia. These results

suggest relative anoxia tolerance of Calingiri compared to the other genotypes,

although this tolerance was not consistent across all treatment combinations.

Assigning anoxia-intolerance judgements to the other genotypes has proved

more difficult.

Whilst Ducula-4 coleoptiles showed promise at 28˚ C in the ADH assays (Figure

3b), it also showed significant increases in cell leakage at 28˚ C under anoxia

(Figure 2b). Ducula-4 tissues only show anoxia tolerance in 15˚ C coleoptiles in

terms of growth maintenance, but Ducula-4 is among three other genotypes also

showing this response (Figure 1b). This ranking is further complicated by the

apparent high performance of Ducula-4 at 15˚ C in seminal roots, primary roots

and coleoptiles in terms of % elongation retention when comparing the length of

tissues after 3 d re-oxygenation compared to 8 d old aerated controls

(Supplemental Figure 1e). This demonstrates how different ways of looking at

data can have a profound influence on our interpretations. Using % elongation

retention, Goggin and Colmer (2007) reported Ducula-4 to be among their

anoxia-tolerant genotypes.

Our metabolite analysis highlighted some important differences in metabolism

between genotypes, temperatures and tissues. We were interested in the

benefits of carbohydrate preservation as well as the response of succinate and

amino acids since these metabolites have been shown to strongly and

differentially respond to low oxygen in different species (Narsai et al., 2011).

a. Importance of preservation of CHO: some references in rice and

other plant species

Across genotypes, 15˚ C coleoptiles seem to stand out in their maintenance of

sugar supplies under anoxia (Table 1). 15˚ C coleoptiles of Calingiri are the only

samples to show accumulation of fructose under anoxia. Higher fructose levels

might be due to mobilisation of starch reserves or prevention of sugar

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exhaustion. In an anoxia-intolerant cultivar of rice (IR22), soluble sugar

concentrations were lower after germination and growth under anoxia than in a

more tolerant cultivar (cv. Amaroo) (Huang et al., 2003). Exogenous sugar supply

improved fresh weight and coleoptile extension of the IR22 (Huang et al., 2003).

Interestingly, when seeds were germinated under air and hypoxically pre-treated,

the tolerance differences between cultivars reduced, with IR22 even showing

higher glucose concentrations and faster growth than a cultivar with intermediate

tolerance (cv. Calrose) (Huang et al., 2003). Furthermore, when IR22 and

Amaroo coleoptiles were excised and supplied with glucose, anoxia tolerance

and ethanol production rates were similar, suggesting anoxia intolerance can be

a function of sugar availability (Huang et al., 2003). The importance of sugar

under anoxia, and the uniqueness of 15˚ C Calingiri coleoptiles in terms of its

fructose response and anoxic ADH induction suggests this sample is relatively

anoxia tolerant (Table 1).

b. Anoxic responses of succinate and GABA

In 15˚ C coleoptiles, Calingiri was the only genotype to maintain citric acid and

malic acid levels, with all other genotypes showing depletion under anoxia (Table

1). Steady citric acid and malic acid levels could be useful in maintaining the

synthesis of amino acids that branch off the TCA cycle via 2-oxoglutarate and

oxaloacetate. The depletion of 2-oxoglutarate and accumulation of alanine and

GABA in all genotypes of 15˚ C coleoptiles suggests operation of the GABA

shunt pathway, whereby 2-oxoglutaric acid is converted to glutamate, which

shows no significant change in all genotypes, which is subsequently

decarboxylated to product GABA (Shelp et al., 1995). Transamination of GABA

with pyruvate produces alanine and succinic semialdehyde, which then

generates succinate. The first and last reaction of GABA shunt produce and

consume NAD+, respectively, meaning this pathway is ‘NAD+ neutral’. This is in

contrast to TCA cycle-derived succinate production, which consumes NAD+, a

cofactor necessary to maintain glycolysis under low oxygen. Succinate did not

change in Ducula-4, Carnamah or Calingiri, and even more surprisingly, was

depleted in SARC and Spear. This leads us to ask what the metabolic fate of

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succinate is under low oxygen or question whether succinate leakage from cells

is a possibility. Succinate leakage, however, would challenge the idea that anoxic

plants synthesise alanine in preference to ethanol, which can be easily lost from

the cell (Rocha et al., 2010).

b. Alanine responses under anoxia

When oxygen returns, alanine could be converted back to pyruvate, for eventual

assimilation into aerobic metabolic processes (Miyashita et al., 2007). Despite the

fact that its production has no role in NAD+ generation, alanine is likely an

important compound since its accumulation does not decline in the event of low

nitrogen availability (Rocha et al., 2010). In anaerobic roots of barley, the activity

of alanine aminotransferase parallels that of alcohol dehydrogenase, that is, their

activities are induced over days under low oxygen (Good and Crosby, 1989). It

was also shown that alanine aminotransferase activity was induced in the

anaerobic roots of maize, rye and wheat, but not leaves (Good and Crosby,

1989). Alanine aminotransferase also increases in abundance in anoxic rice

coleoptiles (Shingaki-Wells et al., 2011).

It is hypothesised that alanine has an important role in consumption of pyruvate

which would otherwise activate alternative oxidase or interfere with respiration

inhibition and consume what little oxygen is left in the cell (Gupta et al., 2009;

Zabalza et al., 2009; Rocha et al., 2010). This thinking however, is not applicable

when plants are truly anoxic. Alanine production may also be useful in diverting

carbon backbones from excessive production of ethanol, which can diffuse out

of the cell or pose a threat of toxicity (Rocha et al., 2010). Alanine production

produces 2-oxoglutarate, whose metabolism as a result of partial TCA cycle

operation, could result in the production of an extra ATP during the succinate

synthesis step (Rocha et al., 2010). Confirming our previous metabolomics

experiments (Shingaki-Wells et al., 2011), Calingiri coleoptiles at 28˚ C did not

accumulate alanine (Table 1). Only Carnamah showed accumulation in 28˚ C

coleoptiles, and in 28˚ C roots, SARC, Spear and Calingiri were the only

genotypes to show increases in alanine. Across all genotypes, 15˚ C roots and

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coleoptiles accumulated alanine during anoxia (Table 1). ANOVA analyses

indicate that treatment and temperature interact to have a significant impact on

alanine signals, with alanine levels being higher at 15˚ C and under anoxia (p-

val<0.001). Additionally, coleoptiles have higher levels of alanine than roots (p-

val<0.001), and Calingiri has the highest alanine levels, with Ducula-4 having the

lowest alanine levels (genotype p-val<0.001) (Supplemental Table 6).

Alanine levels are higher at 15˚ C than at 28˚ C, and this might be due to the fact

that alcohol dehydrogenase activity levels are much higher at 28˚ C than at 15˚ C

(Figure 3), meaning more pyruvate can be directed towards the ethanol

fermentation pathway rather than the alanine synthesis pathway at higher

temperatures. This could mean that 15˚ C tissues have a higher capacity to

synthesise alanine due to pyruvate availability.

Conclusions

These analyses have revealed the complexity of ranking genotypes for tolerance

to anoxia. Calingiri, however, might have a slight tolerance advantage: it shows

alcohol dehydrogenase activity induction under anoxia, low cell leakage, superior

growth recovery in some respects, and sugar pools that appear more stable than

other genotypes. We found that an absent alanine response under anoxia is not

specific to wheat, but is temperature, tissue and genotype-dependent. The

specific role of alanine under anoxia is unclear, and requires further investigation.

Root sensitivity to anoxia was confirmed, as was the sensitivity of wheat at higher

temperatures. The large influence that temperature and tissue type have on the

metabolic responses of wheat to anoxia are likely to partially contribute to the

tolerance discrepancies reported in the literature.

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Bibliography

Bailey-Serres J, Voesenek LACJ (2008) Flooding stress: acclimations and genetic diversity. Annual Review of Plant Biology 59: 313-339

Bradford MM (1976) A Rapid and Sensitive Method for the Quantitation of Microgram Quantities of Protein Utilizing the Principle of Protein-Dye Binding. Analytical Biochemistry 72: 248-254

Branco-Price C, Kaiser KA, Jang CJH, Larive CK, Bailey-Serres J (2008) Selective mRNA translation coordinates energetic and metabolic adjustment to celluar oxygen deprivation and reoxygenation in Arabidopsis thaliana. The Plant Journal 56: 743-755

Colmer TD, Huang S, Greenway H (2001) Evidence for down-regulation of ethanolic fermentation and K+ effluxes in the coleoptile of rice seedlings during prolonged anoxia. Journal of Experimental Botany 52: 1507-1517

Fukao T, Yeung E, Bailey-Serres J (2011) The Submergence Tolerance Regulator SUB1A Mediates Crosstalk between Submergence and Drought Tolerance in Rice. The Plant Cell 23: 412-427

Gibbs J, Greenway H (2003) Mechanisms of anoxia tolerance in plants. I. Growth, survival and anaerobic catabolism. Functional Plant Biology 30: 1–47

Goggin DE, Colmer TD (2007) Wheat genotypes show contrasting abilities to recover from anoxia in spite of similar anoxic carbohydrate metabolism. Journal of Plant Physiology 164: 1605-1611

Good AG, Crosby WL (1989) Anaerobic induction of alanine aminotransferase in barley root tissue. Plant Physiology 90: 1305-1309

Gupta KJ, Zabalza A, van Dongen JT (2009) Regulation of respiration when the oxygen availability changes. Physiologia Plantarum 137: 383-391

Harberd NP, Edwards KJR (1982) The effect of a mutation causing alcohol dehydrogenase deficiency on flooding tolerane in barley. New Phytologist 90: 631-644

Howell KA, Narsai R, Carroll A, Ivanova A, Lohse M, Usadel B, Millar AH, Whelan J (2009) Mapping metabolic and transcript temporal switches during germination in rice highlights specific transcription factors and the role of RNA instability in the germination process. Plant Physiology 149: 961-980

Huang S, Greenway H, Colmer TD (2003) Anoxia tolerance in rice seedlings: exogenous glucose improves growth of an anoxia-‘intolerant’, but not of a ‘tolerant’ genotype. Journal of Experimental Botany 54: 2363-2373

Huang S, Ishizawa K, Greenway H, Colmer TD (2005) Manipulation of ethanol production in anoxic rice coleoptiles by exogenous glucose determines rates of ion fluxes and provides estimates of energy

Page 115: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

103

requirements for cell maintenance during anoxia. J Exp Bot 56: 2453-2463

Ismond KP, Dolferus R, De Pauw M, Dennis ES, Good AG (2003) Enhanced low oxygen survival in Arabidopsis through increased metabolic flux in the fermentative pathway. Plant Physiology 132: 1292-1302

Jacobs M, Dolferus R, Van Den Bossche D (1988) Isolation and biochemical analysis of ethyl methanesulfonate induced alcohol dehydrogenase null mutants of Arabidopsis thaliana (L.) Heynh. Biochemical Genetics 26: 105-122

Johnson JR, Cobb BG, Drew MC (1994) Hypoxic Induction of Anoxia Tolerance in Roots of Adh1 Null Zea mays L. Plant Physiology 105: 61-67

Kato-Noguchi H, Kugimiya T (2001) Effects of ethanol on growth of rice seedlings. Plant Growth Regulation 35: 93-96

Kato-Noguchi H, Yasuda Y, Sasaki R (2011) Anoxia tolerance and sugar level in roots and coleoptiles of aerobically germinated rice. Plant Production Science 14: 325-330

Magneschi L, Kudahettige RL, Alpi A, Perata P (2009) Comparative analysis of anoxic coleoptile elongation in rice varieties: relationship between coleoptile length and carbohydrate levels, fermentative metabolism and anaerobic gene expression. Plant Biology 11: 561-573

Magneschi L, Kudahettige RL, Alpi A, Perata P (2009) Expansin gene expression and anoxic coleoptile elongation in rice cultivars. Journal of Plant Physiology 166: 1576-1580

Matsumura H, Takano T, Takeda G, Uchimiya H (1998) Adh1 is transcriptionally active but its translational product is reduced in a rad mutant of rice (Oryza sativa L.), which is vulnerable to submergence stress. Theoretical and Applied Genetics 97: 1197-1203

Menegus F, Brambilla I, Bertani A (1984) Nutrient translocation pattern and accumulation of free amino acids in rice coleoptile elongation under anoxia. Physiologia Plantarum 61: 203-208

Menegus F, Cattaruzza L, Chersi A, Fronza G (1989) Differences in the anaerobic lactate-succinate production and in the changes of cell sap pH for plants with high and low resistance to anoxia. Plant Physiology 90: 29-32

Miyashita Y, Dolferus R, Ismond KP, Good AG (2007) Alanine aminotransferase catalyses the breakdown of alanine after hypoxia in Arabidopsis thaliana. The Plant Journal 49: 1108-1121

Narsai R, Rocha M, Geigenberger P, Whelan J, Van Dongen JT (2011) Comparative analysis between plant species of transcriptional and metabolic responses to hypoxia. New Phytologist 190: 472-487

Patterson BD, Murata T, Graham D (1976) Electrolyte leakage induced by chilling in Passiflora species tolerant to different climates. Australian Journal of Plant Physiology 3: 435-442

Page 116: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

104

Perata P, Armstrong W, Voesenek LACJ (2011) Plants and flooding stress. New Phytologist 190: 269-273

Perata P, Guglielminetti L, Alpi A (1997) Mobilization of endosperm reserves in cereal seeds under anoxia. Annals of Botany 79: 49–56

Perata P, Pozueta-Romero J, Akazawa T, Yamaguchi I (1992) Effect of anoxia on starch breakdown in rice and wheat seeds. Planta 188: 611-618

Rahman M, Grover A, Peacock WJ, Dennis ES, Ellis MH (2001) Effects of manipulation of pyruvate decarboxylase and alcohol dehydrogenase levels on the submergence tolerance of rice. Australian Journal of Plant Physiology 28: 1231-1241

Rocha M, Licausi F, Araújo WL, Nunes-Nesi A, Sodek L, Fernie AR, van Dongen JT (2010) Glycolysis and the tricarboxylic acid cycle are linked by alanine aminotransferase during hypoxia Induced by waterlogging of Lotus japonicus. Plant Physiology 152: 1501-1513

Rolny N, Costa L, Carrion C, Guiamet JJ (2011) Is the electrolyte leakage assay an unequivocal test of membrane deterioration during leaf senescence? Plant Physiology and Biochemistry 49: 1220-1227

Sayre KD, van Ginkel M, Rajaram S, Ortiz-Monasterio I (1994) Tolerance to water-logging losses in spring bread wheat: effect of time of onset on expression. In CS University, ed, Annual Wheat Newsletter, pp 165-171

Schwartz D (1969) An example of gene fixation resulting from selective advantage in suboptimal conditions. The American Naturalist 103: 479-481

Setter TL (2000) Farming systems for waterlogging prone sandplain soils of the South Coast. In Final report to the Grains Research and Development Corporation on project DAW 292

Setter TL, Waters I, Sharma SK, Singh KN, Kulshreshtha N, Yaduvanshi NPS, Ram PC, Singh BN, Rane J, McDonald G, Khabaz-Saberi H, Biddulph TB, Wilson R, Barclay I, McLean R, Cakir M (2009) Review of wheat improvement for waterlogging tolerance in Australia and India: the importance of anaerobiosis and element toxicities associated with different soils. Annals of Botany 103: 221-235

Shelp BJ, Walton CS, Snedden WA, Tuin LG, Oresnik IJ, Layzell DB (1995) GABA shunt in developing soybean seed is associated with hypoxia. Physiologia Plantarum 94: 219-228

Shingaki-Wells RN, Huang S, Taylor NL, Carroll AJ, Zhou W, Millar AH (2011) Differential molecular responses of rice and wheat coleoptiles to anoxia reveal novel metabolic adaptations in amino acid metabolism for tissue tolerance. Plant Physiology 156: 1706-1724

vanGinkel M, Rajaram S, Thijssen M (1992) Waterlogging in wheat: germ- plasm evaluation and methodology development. In The Seventh Wheat Workshop for Eastern, Central and Southern Africa, Nakuru, Kenya, pp 115-124

Page 117: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

105

Vartapetian BB, Andreeva IN, Kozlova GI (1976) The resistance to anoxia and the mitchondrial fine structure of rice seedlings. Protoplasma 88: 215-224

Voesenek LACJ, Colmer TD, Pierik R, Millenaar FF, Peeters AJM (2006) How plants cope with complete submergence. New Phytologist 170: 213-226

Waters I, Kuiper PJC, Watkin E, Greenway H (1991) Effects of anoxia on wheat seedlings: I. Interaction between anoxia and other environmental factors. Journal of Experimental Botany 42: 1427-1435

Waters I, Morrell S, Greenway H, Colmer TD (1991) Effects of anoxia on wheat seedlings. II Effect of O2 supply prior to anoxia on tolerance to anoxia, alcoholic fermentation, and sugar levels. Journal of Experimental Botany 42: 1437-1447

Yan B, Dai Q, Liu X, Huang S, Wang Z (1996) Flooding-induced membrane damage, lipid oxidation and activated oxygen generation in corn leaves. Plant and Soil 179: 261-268

Zabalza A, Van Dongen JT, Froehlich A, Oliver SN, Faix B, Gupta KJ, Schmalzlin E, Igal M, Orcaray L, Royuela M, Geigenberger P (2009) Regulation of respiration and fermentation to control the plant internal oxygen concentration. Plant Physiology 149: 1087-1098

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Figures

Figure 1. Proportional growth of wheat tissues.

Figure 2. Electrolyte leakage of whole wheat seedlings.

Figure 3. Specific ADH activity of wheat coleoptiles.

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Figure 1. Proportional growth of wheat tissues at 15˚ C (A-B) or 28˚ C (C-D) subjected to one day of anoxia and then one (A, C) or three (B, D) days of re-oxygenation, relative to continuously aerated controls. Full figure caption and Figure 1C-D on following page.

Me

an

Elo

ng

ati

on

_R

ate

T issue Treatment

*

*

**

Me

an

Elo

ng

ati

on

_R

ate

*

*

*

*

**

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Figure 1. Proportional growth of wheat tissues at 15˚ C or 28˚ C subjected to one day of anoxia and then one or three days of re-oxygenation, relative to continuously aerated controls. A. 15˚ C, 1 d proportional growth. B. 15˚ C, 3 d proportional growth. C. 28˚ C, 1 d proportional growth. D. 28˚ C, 3 d proportional growth. Briefly, the difference between the length of seedlings immediately after anoxia was subtracted from the length of seedlings after 1 or

Me

an

Elo

ng

ati

on

_R

ate

T issue Treatment

***

**

****

*

*

***

Me

an

Elo

ng

ati

on

_R

ate

T issue

*

**

***

*

* ***

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109

3 d re-oxygenation. This difference was calculated as a proportion of the length of seedlings immediately after anoxia. Control values were calculated using continuously aerated samples at the same ages. See methods for full calculations. *** indicates p-val <0.001; ** indicates p-val<0.01 and * indicates a p-val<0.05. Error bars represent +/- 1 standard error. Figure 1A-B on prior page.

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Figure 2. Electrolyte leakage of whole wheat seedlings after an hour of incubation as a ratio of maximum electrolyte leakage after sample boiling (3 seedings per replicate, n=11-16). Air indicates a treatment of air for 4 days. Anoxia indicates a treatment of four days of air followed by one say of anoxia. A. 15˚ C seedlings. B. 28˚ C seedlings. *** indicates p-val <0.001; ** indicates p-val<0.01 and * indicates a p-val<0.05. Error bars represent +/- 1 standard error. Figure 2B follows on the next page.

Genotype

Me

an

Ele

ctro

lyte

Le

aka

ge

(C

1/C

2)

TreatmentA

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Figure 2. Electrolyte leakage of whole wheat seedlings at 15˚ C (A) and 28˚ C (B). For full figure caption, see previous page.

BB

Genotype

Me

an

Ele

ctro

lyte

Le

aka

ge

(C

1/C

2)

Treatment*** *** ***

*

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Figure 3. Specific Alcohol Dehydrogenase (ADH) activity of wheat coleoptiles before and after anoxia. Air indicates a treatment of air for 4 days. Anoxia indicates a treatment of four days of air followed by one say of anoxia. A. 15˚ C coleoptiles. B. 28˚ C coleoptiles. *** indicates p-val <0.001; ** indicates p-val<0.01 and * indicates a p-val<0.05. Error bars represent +/- 1 standard error. Figure 3B follows on the next page.

Genotype

Sp

ec

ific

Ac

tiv

ity

(u

mo

l/m

in/m

g p

rote

in)

Treatment ***

A

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Figure 3. Specific ADH activity of wheat coleoptiles before and after anoxia. A. 15˚ C coleoptiles. B. 28˚ C coleoptiles. Figure 3A on previous page.

Genotype

Me

an

Sp

ec

ific

Ac

tiv

ity

(u

mo

l/m

in/m

g p

rote

in)

Treatment

*

B

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Tables Table 1. Metabolite profiling of anoxic tissues.

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Tab

le 1

. Met

abol

ite p

rofil

ing

of a

noxi

c tis

sues

. Ful

l tab

le c

aptio

n an

d se

cond

par

t of t

able

follo

ws

on th

e ne

xt p

age.

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Tab

le 1

. Con

tinue

d. M

etab

olite

pro

filin

g of

roo

ts (p

rimar

y /s

emin

al) a

nd c

oleo

ptile

s fro

m a

ll fiv

e ge

noty

pes

at 1

5˚ C

and

28˚

C. N

umbe

rs

repr

esen

t m

etab

olite

res

pons

e va

lue

ratio

s w

ith a

noxi

cally

-tre

ated

sam

ples

as

the

num

erat

or, a

nd a

erat

ed s

ampl

es a

s th

e de

nom

inat

or

(4 d

air

1 d

anox

ia d

ivid

ed b

y 4

d ai

r). B

lue

colo

rs in

dica

te m

etab

olite

s th

at s

igni

fican

tly d

eple

te d

urin

g an

oxia

, an

d gr

een

repr

esen

ts

met

abol

ites

that

sig

nific

antly

acc

umul

ate

unde

r an

oxia

. Firs

t par

t of t

his

tabl

e is

on

the

prev

ious

pag

e.

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Supplemental Figures Supplemental Figure 1. Growth profiles of tissues from seedlings treated with anoxia/re-oxygenation compared to continuous aeration. Supplemental Figure 2. GABA signal normalised to tissue mass and ribitol in 28˚ C coleoptiles and roots.

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S

upp

lem

enta

l Fig

ure

1. G

row

th p

rofil

es o

f tis

sues

from

see

dlin

gs tr

eate

d w

ith a

noxi

a/re

-oxy

gena

tion

com

pare

d to

con

tinuo

us

aera

tion.

A. C

oleo

ptile

leng

th. B

. Lea

f len

gth.

C. L

engt

h of

sum

of s

emin

al r

oots

. D. P

rimar

y ro

ot le

ngth

. E. %

ret

entio

n gr

owth

of

anox

ic v

s. c

ontin

uous

ly a

erat

ed s

ampl

es a

t 8 d

old

. Sup

plem

enta

l Fig

ures

1B

-E fo

llow

on

the

next

pag

es.

0 10

20

30

40

50

4d air (for air)

5d air

6d air

8d air

4d air (for anoxia)

4d air 1d N2

4d air 1d N2 1d air

4d air 1d N2 3d air

4d air (for air)

5d air

6d air

8d air

4d air (for anoxia)

4d air 1d N2

4d air 1d N2 1d air

4d air 1d N2 3d air

15˚ C

15

˚ C

28˚ C

28

˚ C

Length (mm) C

oleo

ptile

Duc

ula

SA

RC

Spe

ar

Car

nam

ah

Cal

ingi

ri

SF

1a

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119

S

upp

lem

enta

l Fig

ure

1. G

row

th p

rofil

es o

f tis

sues

from

see

dlin

gs tr

eate

d w

ith a

noxi

a/re

-oxy

gena

tion

com

pare

d to

con

tinuo

usae

ratio

n. A

. Col

eopt

ile. B

. Lea

f. C

. Sum

of s

emin

al r

oots

. D. P

rimar

y ro

ots.

E. %

ret

entio

n gr

owth

of a

noxi

c vs

. con

tinuo

usly

aer

ated

sa

mpl

es a

t 8 d

old

.

0 20

40

60

80

100

120

140

160

4d air (for air)

5d air

6d air

8d air

4d air (for anoxia)

4d air 1d N2

4d air 1d N2 1d air

4d air 1d N2 3d air

4d air (for air)

5d air

6d air

8d air

4d air (for anoxia)

4d air 1d N2

4d air 1d N2 1d air

4d air 1d N2 3d air

15˚ C

15

˚ C

28˚ C

28

˚ C

Length (mm)

Leaf

Duc

ula

SA

RC

Spe

ar

Car

nam

ah

Cal

ingi

ri

SF

1b

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120

Sup

ple

men

tal F

igur

e 1.

Gro

wth

pro

files

of t

issu

es fr

om s

eedl

ings

trea

ted

with

ano

xia/

re-o

xyge

natio

n co

mpa

red

to c

ontin

uous

ae

ratio

n. A

. Col

eopt

ile. B

. Lea

f. C

. Sum

of s

emin

al r

oots

. D. P

rimar

y ro

ots.

E. %

ret

entio

n gr

owth

of a

noxi

c vs

. con

tinuo

usly

aer

ated

sa

mpl

es a

t 8 d

old

. 0 50

100

150

200

250

4d air (for air)

5d air

6d air

8d air

4d air (for anoxia)

4d air 1d N2

4d air 1d N2 1d air

4d air 1d N2 3d air

4d air (for air)

5d air

6d air

8d air

4d air (for anoxia)

4d air 1d N2

4d air 1d N2 1d air

4d air 1d N2 3d air

15˚ C

15

˚ C

28˚ C

28

˚ C

Length (mm) S

um o

f Sem

inal

Roo

ts

Duc

ula

SA

RC

Spe

ar

Car

nam

ah

Cal

ingi

ri

SF

1c

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Sup

ple

men

tal F

igur

e 1.

Gro

wth

pro

files

of t

issu

es fr

om s

eedl

ings

trea

ted

with

ano

xia/

re-o

xyge

natio

n co

mpa

red

to c

ontin

uous

ae

ratio

n. A

. Col

eopt

ile. B

. Lea

f. C

. Sum

of s

emin

al r

oots

. D. P

rimar

y ro

ots.

E. %

ret

entio

n gr

owth

of a

noxi

c vs

. con

tinuo

usly

aer

ated

sa

mpl

es a

t 8 d

old

. 0 20

40

60

80

100

120

4d air (for air)

5d air

6d air

8d air

4d air (for anoxia)

4d air 1d N2

4d air 1d N2 1d air

4d air 1d N2 3d air

4d air (for air)

5d air

6d air

8d air

4d air (for anoxia)

4d air 1d N2

4d air 1d N2 1d air

4d air 1d N2 3d air

15˚ C

15

˚ C

28˚ C

28

˚ C

Length (mm) P

rimar

y R

oot

Duc

ula

SA

RC

Spe

ar

Car

nam

ah

Cal

ingi

ri

SF

1d

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122

S

upp

lem

enta

l Fig

ure

1. G

row

th p

rofil

es o

f tis

sues

from

see

dlin

gs tr

eate

d w

ith a

noxi

a/re

-oxy

gena

tion

com

pare

d to

con

tinuo

usly

ae

ratio

n. A

. Col

eopt

ile. B

. Lea

f. C

. Sum

of s

emin

al r

oots

. D. P

rimar

y ro

ots.

E. %

ret

entio

n gr

owth

of a

noxi

c vs

. con

tinuo

usly

aer

ated

sa

mpl

es a

t 8 d

old

. 0 20

40

60

80

100

120

15˚ C

28

˚ C

15˚ C

28

˚ C

15˚ C

28

˚ C

15˚ C

28

˚ C

Sum

Sem

inal

Roo

ts

Prim

ary

Roo

t C

oleo

ptile

Le

af

% Retention of growth at 8 days of age (post-anoxia/air)

Duc

ula

SA

RC

Spe

ar

Car

nam

ah

Cal

ingi

ri

120

SF

1e

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123

S

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l Fig

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2. G

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Supplemental Tables Supplemental Table 1. P-values and mean differences associated with length comparisons between different tissues at the beginning of the experiment (4 d air) and at other time points. Supplemental Table 2. P-values and mean differences associated with length comparisons made between seedlings treated anoxia and samples at other time points. Supplemental Table 3. Alcohol dehydrogenase assay p-values. Supplemental Table 4. Genotype-centric representation of Table 1 (metabolite data). Supplemental Table 5A. Average length of tissues at different time points and % growth retention calculations. Supplemental Table 6. ANOVA interaction data for alanine signals.

Page 137: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

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Page 142: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

130

Supplemental Table 4. Genotype-centric representation of Table 1. Metabolite profiling of roots (primary /seminal) and coleoptiles from all five genotypes at 15˚ C and 28˚ C. Numbers represent metabolite response values with anoxically-treated samples as the numerator, and aerated samples as the denominator (4 d air 1 d anoxia divided by 4 d air). Blue colours indicate metabolites that significantly deplete during anoxia, and green represents metabolites that significantly accumulate under anoxia.

Ducula SARC Spear Carnamah Calingiri

Root Coleoptile Root Coleoptile Root Coleoptile Root Coleoptile Root Coleoptile 15˚ C 28˚ C 15˚ C 28˚ C 15˚ C 28˚ C 15˚ C 28˚ C 15˚ C 28˚ C 15˚ C 28˚ C 15˚ C 28˚ C 15˚ C 28˚ C 15˚ C 28˚ C 15˚ C 28˚ C

Sugars / Glycolysis

Sucrose 0.93 0.01 0.73 0.21 0.69 0.16 0.83 0.17 0.76 0.11 1.09 0.10 0.80 0.17 0.79 0.90 0.61 0.35 0.88 0.26 D-Fructose 1 0.29 0.02 0.74 0.44 0.54 0.03 1.18 0.52 0.49 0.07 1.12 0.28 0.36 0.08 1.35 0.80 0.76 0.43 2.19 0.54 D-Fructose 2 0.26 0.02 0.70 0.40 0.51 0.03 1.17 0.45 0.47 0.07 1.13 0.25 0.33 0.07 1.37 0.74 0.76 0.39 2.23 0.53 D-Glucose 0.66 0.05 0.53 0.71 0.87 0.26 0.78 0.64 0.75 0.10 0.53 0.39 0.72 0.12 0.77 0.86 0.62 0.13 1.47 0.61 D-Glucose or Galactose 0.53 0.05 0.43 0.54 0.77 0.23 0.74 0.37 0.70 0.08 0.53 0.26 0.65 0.10 0.75 0.66 0.58 0.08 1.61 0.54 D-Fructose-6-Phosphate 0.26 1.58 0.58 0.06 0.85 1.47 0.62 0.29 0.70 0.47 0.76 0.26 0.79 0.09 0.79 3.51 1.53 0.27 0.90 1.19 D-Glucose-6-Phosphate 0.27 0.82 0.52 0.05 0.86 1.48 0.51 0.34 0.72 0.22 0.73 0.28 0.74 0.21 0.69 3.38 1.16 0.25 0.81 1.06 Trehalose 0.73 0.14 0.64 0.88 0.81 0.21 0.85 0.79 0.74 0.75 0.60 0.37 0.93 0.55 0.59 0.91 0.45 0.57 0.62 0.58 Galactose 0.66 0.05 0.53 0.71 0.87 0.26 0.78 0.64 0.75 0.10 0.53 0.39 0.72 0.12 0.77 0.86 0.62 0.13 1.47 0.61

TCA Cycle

Citric Acid 0.25 0.02 0.30 0.19 1.12 0.06 0.43 0.23 1.61 0.28 0.50 0.30 0.52 0.29 0.38 0.71 0.94 0.33 0.62 0.63 Isocitric Acid 0.29 0.10 0.42 0.16 0.77 0.08 0.43 0.28 1.10 0.33 0.86 0.74 0.70 0.27 0.62 0.96 0.64 0.26 0.50 0.56 Fumaric acid 0.91 0.37 0.36 0.71 0.86 0.46 0.59 0.11 0.75 0.50 0.39 0.66 1.18 0.55 0.55 0.58 0.79 1.32 0.70 0.79 2-oxoglutaric acid 0.19 0.01 0.29 0.04 0.33 0.07 0.20 0.12 0.55 0.10 0.27 0.32 0.51 0.10 0.18 1.49 0.44 0.18 0.21 1.08 Succinate 0.96 2.21 0.68 3.66 0.61 2.59 0.56 0.64 0.58 3.39 0.36 1.80 1.52 3.08 0.64 2.40 0.74 4.41 1.16 1.92 Malic Acid 0.39 0.07 0.16 0.11 0.44 0.08 0.34 0.03 0.61 0.12 0.32 0.37 0.50 0.14 0.33 0.34 0.44 0.33 0.74 0.53

Amino Acids

4-Hydroxyproline 0.34 0.03 0.48 0.31 0.86 0.05 0.65 0.23 0.75 0.15 0.55 0.28 0.62 0.23 0.80 0.84 0.81 0.47 1.06 1.01 Aspartic Acid 0.21 0.00 0.22 0.07 0.39 0.01 0.27 0.04 0.58 0.11 0.44 0.12 0.35 0.28 0.38 0.29 0.28 0.18 0.80 0.20 L-Glutamate 0.16 0.62 0.44 0.04 0.45 1.10 0.45 0.06 0.73 0.41 1.05 0.10 0.37 0.29 0.66 1.32 0.80 0.97 1.01 0.61 L-Glutamine 0.58 0.18 0.12 0.06 1.01 0.17 0.05 0.01 0.70 0.29 0.20 0.03 1.11 0.19 0.15 0.75 1.09 0.93 0.15 0.58 beta-Alanine 1.38 0.20 5.19 1.38 4.30 0.72 9.32 1.23 4.72 0.74 6.49 1.61 3.35 1.82 5.70 2.37 5.15 2.94 7.93 2.22 Glycine 1.68 1.18 3.62 1.39 2.58 3.49 5.92 1.76 3.11 5.01 5.39 1.76 4.25 3.06 5.73 3.63 3.77 4.38 5.87 1.40 L-Alanine 2.83 0.82 7.52 1.09 9.13 4.14 6.00 1.22 7.00 9.47 13.18 1.90 9.89 1.98 5.77 6.48 9.55 9.41 4.23 1.71 L-Asparagine 0.85 0.01 0.31 0.15 1.43 0.08 0.24 0.06 1.67 0.04 0.52 0.53 1.87 0.32 1.07 0.56 2.97 0.43 1.04 0.72 L-Isoleucine 0.93 0.07 2.08 0.56 1.35 0.70 3.00 0.51 1.35 1.05 5.72 1.02 2.33 1.10 4.21 1.33 2.04 2.10 4.15 1.04 L-Leucine 0.88 0.08 2.49 1.54 1.34 0.85 4.81 0.94 1.36 1.17 8.08 1.35 2.34 1.04 6.48 3.93 2.25 2.30 6.36 1.36 L-Lysine 2.29 0.26 4.53 1.12 4.21 1.70 5.37 0.69 4.65 0.38 9.53 1.37 7.70 1.63 6.51 2.43 21.20 8.77 6.31 2.53 L-Methionine 0.70 0.00 1.17 0.19 0.88 0.05 0.97 0.20 1.25 0.71 5.40 0.93 1.02 1.90 1.67 1.31 1.30 1.29 1.93 0.62 L-Phenylalanine 0.48 0.05 1.42 1.04 1.17 0.08 2.22 0.59 2.65 1.36 6.54 0.70 1.46 1.52 4.46 4.34 2.70 2.50 3.21 1.46 L-Proline 1.79 0.13 6.12 4.23 6.35 3.93 6.57 1.64 4.62 8.82 36.85 3.76 7.32 7.88 5.65 11.42 13.11 8.18 5.48 1.87 L-Serine 0.61 0.01 1.00 0.48 1.56 0.46 0.59 0.26 2.26 0.90 1.64 0.34 1.58 0.84 1.33 1.18 2.16 1.43 1.68 0.54 L-Threonine (3 TMS) 0.98 0.03 2.55 0.42 1.85 0.62 2.64 0.29 2.28 1.20 5.73 0.92 2.25 1.14 3.37 1.34 2.93 1.77 3.19 0.84 L-Threonine (2 TMS) 0.97 0.08 2.38 0.46 1.55 0.36 2.96 0.56 1.59 1.00 6.68 1.30 1.28 0.77 3.03 1.36 2.24 1.14 2.61 1.21 L-Tryptophan 0.61 0.84 1.16 0.24 0.84 0.91 1.00 0.29 1.17 0.73 1.16 0.60 0.90 0.77 1.05 1.34 0.94 0.78 1.30 2.90 L-Tyrosine 0.53 1.33 2.51 0.68 1.15 1.11 4.12 0.33 1.32 0.52 10.84 0.70 3.28 1.11 6.69 3.43 6.99 1.07 6.74 1.50 L-Valine 0.90 0.14 1.90 0.47 1.54 0.68 2.69 0.47 1.22 1.06 4.99 1.05 1.96 1.03 2.82 1.33 2.07 2.10 3.22 0.97 Ornithine 1.00 0.15 0.70 0.77 1.03 0.32 0.61 0.60 1.58 0.52 0.79 0.64 2.06 0.45 0.95 1.29 1.82 0.64 1.10 0.95 GABA 18.01 4.76 19.80 6.17 25.45 12.64 30.31 12.61 50.89 12.19 13.11 6.94 40.45 14.22 44.11 11.88 34.59 17.98 40.60 9.54 2-Aminobutyric acid 0.68 0.57 0.62 0.52 1.38 0.56 0.49 0.29 0.96 0.86 0.65 0.20 0.56 0.54 0.68 1.76 1.30 1.61 0.63 0.42

Polyamine Putrescine 1.41 0.20 2.34 2.04 1.64 0.65 2.32 1.84 2.77 1.86 2.05 1.27 2.03 2.32 3.09 5.57 1.64 3.51 2.21 1.15

Sugar acid D-Gluconic acid 0.71 0.20 1.02 0.38 1.11 0.37 1.10 0.47 0.75 0.57 1.06 0.55 0.97 0.62 1.09 1.05 1.06 0.74 4.99 5.53 L-Threonic acid 0.51 0.09 0.56 0.40 0.61 0.19 0.83 0.61 0.66 0.39 0.45 0.80 0.70 0.51 0.98 1.56 0.61 0.51 1.29 1.19 Glyceric acid 0.73 0.08 0.83 0.39 1.24 0.10 0.85 0.40 1.12 0.34 0.60 0.75 1.00 0.37 1.04 0.72 1.05 0.55 0.95 0.59

Polyols

Mannitol/Sorbitol 2.89 0.61 5.34 0.57 3.04 1.12 0.81 0.62 0.67 1.24 0.35 0.60 0.42 0.73 0.46 0.83 0.79 0.61 1.65 1.10 Threitol/Erythritol 0.40 0.07 0.16 0.10 0.44 0.08 0.38 0.03 0.61 0.12 0.33 0.36 0.51 0.14 0.33 0.33 0.44 0.33 0.74 0.51 meso-Erythritol 0.40 0.08 0.17 0.11 0.45 0.08 0.36 0.04 0.61 0.13 0.33 0.37 0.51 0.15 0.33 0.35 0.45 0.34 0.74 0.53 Myo-Inositol 1.30 0.57 3.70 1.36 2.97 1.13 2.35 0.76 2.41 1.59 3.44 1.15 2.58 1.89 2.48 3.86 2.38 1.74 1.62 0.99 Glycerol 1.56 0.67 1.45 3.31 1.77 0.91 2.37 1.51 0.89 1.72 1.34 1.07 0.60 1.01 1.54 1.93 0.85 0.53 2.28 2.35 Shikimic acid 0.20 0.18 0.06 0.10 0.39 0.29 0.26 0.05 0.36 0.36 0.87 2.07 0.38 0.57 0.37 0.52 0.38 0.41 0.42 2.51

Sterol Campesterol 0.62 0.54 1.23 1.04 1.12 0.42 0.94 1.45 1.04 0.68 1.19 1.29 0.97 0.60 1.02 0.94 1.03 0.81 0.97 1.16 beta-Sitosterol 0.57 0.39 1.17 0.60 1.15 0.37 0.90 0.87 1.01 0.70 1.18 0.63 0.66 0.45 0.98 0.94 1.04 0.80 0.92 0.72

Misc.

Urea 0.73 0.08 1.27 1.64 1.76 0.17 0.82 1.97 0.86 0.66 1.37 0.53 1.24 0.29 1.06 1.12 1.77 1.07 1.00 0.49 Cinnamic acid 0.43 0.03 0.55 0.58 0.97 0.08 0.91 0.34 1.16 0.25 0.74 0.41 0.60 0.60 0.98 1.07 0.91 0.28 1.27 0.77 Nicotinic acid 0.70 0.07 1.06 1.14 1.08 0.32 1.11 0.56 0.97 0.90 0.80 1.06 0.87 0.81 1.02 0.95 1.10 1.40 0.98 1.03 Phosphoric acid 0.83 0.51 0.94 0.49 1.37 0.32 1.27 0.34 1.37 0.83 0.88 0.81 1.13 0.73 1.09 0.99 1.18 0.84 1.25 0.78

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Chapter 4 Rice and wheat responses to re-oxygenation

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137

Foreword to Study III

Since Study I reported rapid amino acid accumulation in anoxic rice, the fate

of these pools upon re-oxygenation was also questioned. The comparatively

subtle response of wheat to anoxia is also interesting, in light of the fact that

sucrose rapidly depletes in anoxic wheat. This suggests that anoxic wheat is

assimilating the carbon from sucrose into glycolysis, but in contrast to rice, is

unable to replenish it from endosperm starch reserves. Despite this, wheat

amino acid metabolism remains relatively stable.

In Study III, aerobically germinated rice and wheat seedlings were treated with

anoxia for one day, at 28˚ C. Re-oxygenation treatments followed and lasted

for one day. Proteome and metabolome changes in coleoptiles were analysed

in an attempt to understand whether these inter-species differences during

anoxia would continue upon re-oxygenation.

Indeed, the proteomic and metabolomic responses to anoxia and re-

oxygenation were generally subtler in wheat. The rapid accumulation of amino

acids seen in rice (Study I) was confirmed in Study III. Furthermore, rapid

responses of the rice metabolome were observed during re-oxygenation.

Specifically, amino acids were consumed post-anoxia. This was not the case

for wheat, which failed to anaerobically accumulate amino acids to the extent

seen in rice. In Study III, the role of amino acid consumption during re-

oxygenation is discussed.

Proteomics analysis revealed several inter-species similarities. For example,

the abundance of several antioxidant proteins was affected by anoxia/re-

oxygenation. Finally, the activity of two classes of antioxidant enzymes was

measured in an attempt to clarify the somewhat contradictory proteomics

data.

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Differential recovery of rice and wheat during re-

oxygenation after short-term anoxic stress

Rachel N. Shingaki-Wells, Shaobai Huang & A. Harvey Millar.

Australian Research Council Centre of Excellence in Plant Energy Biology, Centre for

Comparative Analysis of Biomolecular Networks, Bayliss Building M316 University of Western

Australia, 35 Stirling Highway, Crawley 6009, Western Australia, Australia.

Abstract

The metabolic responses of plants to anoxia are well documented, however,

comparatively little is known about the effects of re-oxygenation. This study

aimed to understand how two cereal crops, rice and wheat (Oryza sativa and

Triticum aestivum, respectively), respond to post-anoxia at the metabolomic

and proteomic level. We found considerable divergence in the metabolism of

these two species. Specifically, highly accumulating amino acids were rapidly

consumed during re-oxygenation in rice, but not in wheat. At the protein level,

we saw several similarities between these species. Both species exhibited

changes in proteins involved in cell structure re-modelling, translation and

oxidative stress defence. Overall, however, the response of rice to these

stresses appeared to be more pronounced than what was observed in wheat.

We discuss how this could be a result of the ability of rice to synthesise

sucrose during anoxia, to improve anaerobic ATP production, and indirectly

increase amino acid production, for improved fitness during re-oxygenation.

Introduction

Floods are expected to increase in frequency as a result of anthropological

climate change (Arnell and Liu, 2001; Bailey-Serres and Voesenek, 2008).

Submerged plants are quickly deprived of oxygen (Armstrong, 1979),

especially if microbial activity is high and light penetration is limited (Bailey-

Serres et al., 2012). Floods in Pakistan resulted in $4.45 billion worth of

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139

damage to rice, wheat and cotton, with rice being highly flood-threatened in

many parts of the world (Arshad and Shafi, 2010; Bailey-Serres et al., 2012).

The threat that floods pose to food security has been a motivator for much

research on crops that are both tolerant and intolerant to low oxygen. Plants

that survive floods are eventually returned to an oxygenated environment. Yet

most studies focus on the low-oxygen event alone, with little attention paid to

the stresses imposed when floodwaters recede. De-submergence can cause

drought stress (Branco-Price et al., 2008) as well as oxidative stress (Blokhina

et al., 1999) and thus the transcriptomes, proteomes and metabolomes of an

anoxic tissue are likely to influence the degree of tolerance a plant exhibits

when oxygen returns.

A study of polysomal mRNA populations in Arabidopsis seedlings treated with

hypoxia followed by re-oxygenation revealed that more than half of the mRNA

population was prevented from complexing with ribosomes during low oxygen,

without a change in the steady state abundance (Branco-Price et al., 2008).

This strongly suggests selective translation is involved in the resulting

proteome, a process that would promote ATP conservation under low oxygen

(Branco-Price et al., 2008). During re-oxygenation, repression of translation

was rapidly reversed, with 88 % recovery of polysome levels within 1 hour,

which could allow rapid proteome adjustment when O2 returns (Branco-Price

et al., 2008). Plants may also prepare for re-oxygenation, as evidenced by a

subset of transcripts that increase under hypoxia, but are only translated

when oxygen returns (Branco-Price et al., 2008).

More recently, the first plant proteomics study focussing on re-oxygenation

showed that soybean roots adjust their proteomes during a flooding event,

and that these changes remain present even during de-submergence (Salavati

et al., 2012). Our interests lie in what happens to rice and wheat during re-

oxygenation, since we previously showed the subtle response of the wheat

coleoptile proteome and metabolome relative to rice under anoxia (Shingaki-

Wells et al., 2011). The availability of oxygen determines the mode of energy

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140

metabolism and thus we expect many changes that occur under anoxia to be

reversed when oxygen is no longer limiting. Specifically, we are interested in

the fate of amino acids which so strongly accumulate in anoxic tissues (Kato-

Noguchi and Ohashi, 2006; Shingaki-Wells et al., 2011). In this study, we

analysed the proteomes and metabolomes of rice and wheat coleoptiles

subjected to air, anoxia and re-oxygenation to understand how anoxia-tolerant

and -intolerant species metabolically adjust to re-oxygenation. We also

studied the activity of two oxidative stress defence proteins, peroxidase and

catalase, to understand the role of these systems during the different phases

of anoxic stress.

Methods

Plant Growth Rice and wheat seedlings were grown at 28˚ C as described previously

(Shingaki-Wells et al., 2011). Four-day-old seedlings were germinated and

grown in the dark in a hydroponic-like system, and bubbled with air. The

coleoptiles of some seedlings were harvested at this stage and snap frozen in

liquid nitrogen. Other seedlings went on for a one-day anoxic treatment,

delivered by infusion with 99.9 % nitrogen gas. Re-oxygenation treatments

were given to some of these anoxic seedlings for one day. The details of this

growth regime are described by Shingaki-Wells and colleagues (2011).

Differential in Gel Electrophoresis (DIGE)

Protein isolation from rice and wheat coleoptiles was performed using the

chloroform/ methanol method as described previously (Wessel and Flügge,

1984; Shingaki-Wells et al., 2011). To compare air, anoxia and post-anoxia

treatments, six DIGE gels were run for both species, resulting in the

representation of each treatment by four biological replicates. Samples were

labelled with CyDyes as described previously (GE Healthcare) (Shingaki-Wells

et al., 2011) except one gel was loaded with 500 μg extra unlabelled protein

for downstream mass spectrometry analysis.

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Quantitative gel analysis

Fluorescent gels were scanned using a Typhoon™ laser scanner (GE

Healthcare) using three filter/laser combinations: 580 BP 30, Green (532 nm);

670 BP 30, Red (633 nm); and 520 BP 40, Blue (488 nm). The PMT was set

at 520 V, sensitivity set at normal and pixel size at 100 microns. Cy2 was

selected as the internal standard. Gels were cropped using ImageQuant TL to

exclude outer gel areas where proteins did not migrate. Then .gel files were

imported into Decodon Delta2D (v 4.3), black speckles removed at a setting of

2, and arranged in their respective treatment groups. The In-Gel Standard

Warping Strategy was chosen with ‘warp mode within gels’ set as identical

and ‘warp mode between gels’ set as automatic. The master gel is by default

the first gel image added to the project. Master gels were changed if the

default gel was not representative of other gels (i.e. it had smearing, or ran

differently). After automatic warpings were performed, match vectors were

reviewed for every automatically warped gel combination. If automatic warping

was unsatisfactory in a portion of the gel, all match vectors were removed in

that section for manual matching instead (exact warp mode). After warping, a

fusion image was generated. Problematic gels or gels with obvious distortion

were excluded from the image fusion. The chosen fusion type was ‘union’.

Internal standard gels were excluded from the image fusion. Other options

were left as default. Spot detection was then carried out on the fusion image.

Delta2D’s proposed detection parameters were left as default. Spots were

manually inspected on the fusion image. Spot editing tools were used to split

spots if it was clear in 3D images that the spots within the boundary were two

separate spots. 3D inspection also allowed calls to be made on whether two

spots should be joined, or an undetected spot should actually be a spot.

Detected spots in smear regions were cancelled. After spot editing, spots

were transferred from the fusion image. Boundary transfers were adapted to

actual spots on the target images by selecting ‘re-model spots after transfer’.

Transferred spot boundaries were manually inspected using the ‘Gel Image

Regions’ window. If editing was necessary, this was done on the fusion image,

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142

requiring re-transfer of spots again. Noisy spots were filtered out if the spot

quality (Q) was less than 0.02.

Statistics

Each spot intensity is calculated as a percentage of the signal intensity of the

entire gel (overall normalisation). This value is then normalised to the

corresponding Cy2 spot (horizontal normalisation). Ratios are calculated by

comparing these twice-normalised values between treatments. Delta2D

produces a ‘Quantitation Table’ listing various spot variables including ratio of

mean normalised volumes of treatment to treatment. For spot changes to be

considered significant, an ANOVA p-value had to be less than 0.05 and a ratio

change greater than 1.5.

MALDI-TOF/TOF analysis of peptides

Plugs were cut out of 2D gels and destained twice on an orbital rocker for 45

min with 50 μL 50 % ACN v/v, 25 mM NH4HCO3. Destaining solution was

removed to allow gel slices to dry at room temperature for 20 min. 12 μL

digestion solution (10 mM NH4HCO3, 3 μg/mL trypsin) was added to each

dried gel slice for incubation at 37˚ C for 16 h. Peptides were extracted from

gel slices using 12 μL 100 % v/v ACN for 15 minutes on an orbital rocker. The

supernatant was stored. Then 12 μL 50 % [v/v] ACN 5 % v/v formic acid was

added twice, for 15 min with all supernatants combined and stored. This was

then dried in a vacuum centrifuge and stored at -20˚ C for later use.

A saturated matrix mix (SMM) was made by adding powdered α-cyano-4-

hydroxycinnamic acid (CHCA) to 90 % ACN [v/v] 0.1 % TFA [v/v], briefly

vortexed and sonicated for 15 min. The solution was centrifuged at 10, 000 x

g for 5 mins to pellet residual matrix. The resulting supernatant was used as

the SMM.

Dried samples were re-constituted in 5 μL 5 % ACN [v/v] 0.1 % TFA [v/v].

After 10 mins, 2.5 μL of the sample was spotted on an MTP 384 MALDI target

plate and allowed to dry until approximately half was left. Then 2 μL spotting

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matrix (90 % ACN [v/v] 10 % SMM [v/v]) was mixed in with the sample and

allowed to dry completely. Spots were washed with 10 μL cold 10 mM

NH4H2PO4 in 0.1 % TFA [v/v] for 10 sec. The washing solution was then

removed and spots were allowed to dry.

Analysis of peptides was carried out with an UltraFlex III MALDI-TOF/TOF

mass spectrometer (Bruker Daltonics). The laser intensity used ranged from

30 % to 60 % with up to 1200 shots per spot for MS. Selected MS/MS ions

ranged from 700-4000 m/z using 3 % additional laser power. Data were

analysed using Biotools (Bruker Daltronics) and the Rice_6.1 or WheatTC

database. The Mascot search engine v 2.3 was used with error tolerances of

±1.2 Da for MS and ±0.6 Da for MS/MS, “Max Missed Cleavages” set at 1,

variable modifications set as Carbamidomethyl (C) and Oxidation (M). The

significance threshold was set at p<0.05 (score>49).

Enzyme activity assays

Enzyme extract preparation for peroxidase and catalase assays

Tissue was ground in liquid-nitrogen cooled racks with stainless steel beads

for 2 mins at 15 shakes/s. Cooled racks were turned around and

homogenisation repeated. Cooled extraction buffer (0.1 M KH2PO4, pH 7.4)

wad added to ground tissue samples at a 5:1 ratio. This was mixed twice for

2 min at 15 shakes/s ensuring the rack was kept cold but not so cold as to

freeze samples. Samples were centrifuged at 15, 000 x g for 20 min at 4˚ C.

Supernatant was stored on ice. Protein concentration was calculated using

the Bradford assay. Assays were performed at 25˚ C.

Assay for peroxidase activity

Peroxidase activity was measured using a modified method reported

previously (Abeles and Biles, 1991).To a 1 mL cuvette, 350 μL 0.2 M sodium

acetate buffer pH 5, 350 μL 1 % guaiacol and 350 μL 0.08 % H2O2 were

added. After mixing and setting to auto-zero, 17.5 μL enzyme extract was

mixed in, and absorbance at 470 nm is recorded for 110 seconds.

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Assay for catalase activity

Peroxidase activity was measured using a modified method reported

previously (Chance and Maehly, 1955). The spectrophotometer was auto

zeroed using 75 μM Na phosphate buffer, pH 7. To a 3 mL quartz cuvette, 1.9

mL 75 μM Na phosphate buffer, pH 7 was added followed by 100 μL enzyme

extract and then 1 mL 45 μM H2O2. The absorbance was read at 240 nm for

500 seconds.

Metabolomics

Coleoptiles of rice and wheat seedlings were harvested and rapidly snap

frozen in liquid nitrogen. Metabolites were extracted by placing 25 ± 5 mg

tissue into 2 mL Eppendorf tubes containing a stainless steel grinding bead.

Samples were snap frozen in liquid nitrogen. Metabolites were extracted and

run on a GC-MS as described previously (Howell et al., 2009; Shingaki-Wells

et al., 2011). The generated data were collected and analyzed using

Chemstation GC/MSD Data Analysis Software (Agilent Technologies),

according to earlier analyses (Shingaki-Wells et al., 2011). Data were

processed using MetabolomeExpress software, as described previously

(Carroll et al., 2010).

Results

The effect of anoxia/re-oxygenation on metabolism Four-day-old seedlings germinated and grown under aeration were

transferred to anoxia for one day and subsequently returned to air. The

metabolomic response of rice and wheat coleoptiles to anoxia/post-anoxia

contrast considerably.

During anoxia, rice increased the abundance of many amino acids, including,

Ser, Gly, Phe, Tyr, Ala, Leu, Val, Asn, Lys, Met, Homoserine, Thr, Ile, Glu, Pro,

Orn and GABA (Figure 1A, Supplemental Figure 1A). Notably, of the detected

amino acids, none were depleted in anoxic rice coleoptiles. All of the amino

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acids that increased under anoxia showed decreases during re-oxygenation,

with the exception of ornithine, whose levels were not significantly different to

that of anoxic samples (Figure 1A, Figure 3A). These amino acid levels

remained significantly higher in re-oxygenated samples compared to pre-

anoxic samples, except for Asn and Lys, the abundances of which did not

significantly differ between post-anoxic and pre-anoxic rice samples (Figure

1A, Supplemental Figure 1B).

Sucrose levels increased in anoxic rice, whereas glucose and fructose

remained unchanged (Figure 1B). During re-oxygenation, sucrose declined but

its levels remained higher than pre-anoxic samples (Figure 1B). Glucose and

fructose showed contrasting responses during post-anoxia; glucose

increased so that levels were comparable to pre-anoxia, and fructose

decreased post-anoxia, with levels lower than pre-anoxic samples (Figure 1B).

Both of the detected glycolytic intermediates, glucose-6-phosphate and 3-

phosphoglyceric acid (3-PGA), accumulated under low oxygen in rice (Figure

1B). Both of these metabolites decreased during re-oxygenation. TCA cycle

intermediates showed contrasting responses to anoxia in rice; citrate,

isocitrate and 2-oxoglutarate were depleted during anoxia whereas succinate

and fumarate accumulated (Figure 1C). Aconitate levels remained stable

during low oxygen. Citrate, aconitate, isocitrate and 2-oxoglutarate

accumulated during re-oxygenation, whereas succinate and fumarate

decreased (Figure 1C).

For wheat, the accumulation of some amino acids during anoxia was

accompanied by the depletion of others. Gly, Trp, Leu, Val, Lys, Ile, GABA,

Pro and Orn accumulated and Ser, Asp, Glu and Gln were consumed under

anoxia (Figure 2A, Supplemental Figure 2A). Ala, Phe, Tyr, Asn, Thr, Met,

Homoserine and Arg levels did not change under anoxia (Figure 2A).

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The levels of accumulated and depleted amino acids in anoxic wheat were

unchanged when oxygen returned. Of the non-responding amino acids in

wheat, only Ala changed, in the direction of accumulation during re-

oxygenation (Figure 2A). When comparing post-anoxic to pre-anoxic samples,

several amino acids were significantly different in abundance. Gly, Ala, Trp, Tyr,

Lys, Thr, GABA, Orn and Arg are higher whereas Asp, Asn, Glu and Gln are

lower in post-anoxic wheat compared to pre-anoxia (Figure 2A, Supplemental

Figure 2B). An interesting inter-species difference was observed in that post-

anoxic levels of sucrose were depleted in wheat (Figure 2B), whereas in rice,

sucrose levels were elevated during post-anoxia (Figure 1B). Glucose, fructose,

Glu-6-P and Fru-6-P remained stable in wheat, whereas 3-PGA decreased

under anoxia (Figure 2B). When oxygen returned, these metabolites remained

stable, except 3-PGA which accumulated post-anoxia (Figure 2B). However,

when looking at pre-anoxic levels, sucrose and glucose are higher when

compared to post-anoxic samples (Figure 2B).

Just as in rice, succinate accumulated in anoxic wheat, but fumarate

remained stable. Malate, citrate, aconitate and isocitrate decreased whereas

2-oxoglutarate levels did not change (Figure 2C). The abundances of several

TCA cycle metabolites remained perturbed during post-anoxia, compared to

pre-anoxic samples. For example, aconitate and malate were depleted in

post-anoxic samples relative to pre-anoxia (Figure 2C).

Re-oxygenation results in changes to the proteomes of rice and wheat

We analysed changes in the proteome of rice and wheat seedlings

germinated and grown under air for four days. Some seedlings were

subjected to a one-day anoxic switch and others were subsequently re-

oxygenated for one day. Protein spots significantly changing in abundance

can be seen in Figure 4A for rice and 4B for wheat. The abundances of these

proteins are represented in Figure 5 for wheat and Figure 6 for rice. Proteins

were categorised into three groups; those that significantly increased in

abundance under anoxia (Figure 5A, Figure 6A) those that did not change

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(Figure 5B, Figure 6B) as well as those that significantly decreased in

abundance when transferred to anoxia (Figure 5C, Figure 6C). Within each

group was a set of proteins with a variety of responses to re-oxygenation. We

detected six proteins that significantly increased in wheat coleoptiles under

anoxia (Figure 5A). These include a translation initiation factor 5A (IF; 1.96 X),

pyruvate decarboxylase isozyme 2 (PDC2; 1.82 X), NADP-dependent malic

enzyme (1.55 X), 12-oxophytodienoate reductase (OPR; 1.55) and two

proteins of unknown function (2.32 X, 1.63 X) (Figure 5A). During post-anoxia,

the translation IF (spot 7, Figure 4B; Supplemental table 1) did not significantly

differ in abundance to that of the anoxic treatment, but its levels became

comparable to the pre-anoxic abundance. Pyruvate decarboxylase (Spot 33,

Figure 5A; Supplemental table 1), a classical anoxia-inducible protein,

remained elevated after one day of re-oxygenation. NADP-dependent malic

enzyme, which converts malate to pyruvate, is annotated as chloroplastic

when searching against the rice genome (84 %) and remains elevated in post-

anoxic samples.

Several wheat protein spots decreased under anoxia, eight of which could be

identified by mass spectrometry (Figure 5C). Four are unknown function

proteins (-1.44 X to -2.71 X). The others included phenylalanine ammonia

lyase (-3.72 X), which converts phenylalanine to ammonia and trans-cinnamic

acid, as well as a translation initiation factor 5A (-2.44 X). This translation

initiation factor 5A (spot 24) has a gel pI that is 0.4 units more acidic than the

other initiation factor (spot 7), which showed an increase under anoxia. These

two proteins were identified using mass spectrometry as the same gene

product (CK198613; Supplemental table 1). Phenylalanine ammonia lyase

showed an increase in abundance during re-oxygenation, which suggests this

abundance change was highly dependent on oxygen availability (Figure 5C;

spot 15, Figure 4B). ATP synthase F0 subunit 1 (-2.37 X) and heat shock

protein 20 (-1.71 X) also decreased under anoxia, but their experimental

molecular weights were far smaller than the theoretical molecular weights,

suggesting less accumulation of protein degradation products (Supplemental

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table 1). Several proteins failed to significantly change in abundance when

transitioned to anoxia, but showed significant differences during re-

oxygenation (Figure 5B). Two of these proteins, beta-glucosidase and Hsp20

(spot 36 and 38, respectively), appeared to be protein degradation products.

A putative glycosyl hydrolase family 16 protein (spot 51, Figure 4B, Figure 5B)

has a post-anoxic abundance that is significantly less than pre-anoxic

samples. These proteins are known for their role in cell wall re-modelling

(Strohmeier et al., 2004). We also detected a putative polygalacturonase (spot

20, Figure 4B; Figure 5B), another protein involved in cell wall remodelling,

which significantly increased during re-oxygenation. A protein annotated as a

universal stress domain containing protein (spot 31, Figure 4B; Figure 5B) also

showed a high post-anoxic abundance, relative to anoxic samples. This

protein is homologous to the Adenine nucleotide alpha hydrolases-like

superfamily protein in Arabidopsis thaliana (AT3G53990) (Supplemental table

1). Notably, we detected a putative peroxidase precursor protein, which was

also significantly higher in abundance during re-oxygenation compared to pre-

anoxic samples (TC429713; Spot 28, Figure 4B; Figure 5B). Peroxidases are

involved in the reduction of a range of peroxides (Welinder et al., 2002).

We detected fifteen proteins that significantly increased during the transition to

anoxia in rice (Figure 6A; Figure 4A; Supplemental table 2). Five pyruvate

phosphate dikinase, chloroplast precursor (PPDK) spots were detected, with

differing isoelectric points (Os03g31750; pI=5.25-5.6; Spots 40-44)

(Supplemental table 2). These proteins are involved in the conversion of

phosphoenolpyruvate to pyruvate, and remain elevated during re-oxygenation

(Figure 6A). Thiamine pyrophosphate-dependent pyruvate decarboxylase in

spots 24-27 and glyceraldehyde-3-phosphate dehydrogenase in spot 20,

showed a similar response to PPDK (Figure 6A, Supplemental table 2). Among

the glycolytic enzymes that increased under anoxia, pyruvate kinase

significantly decreased during re-oxygenation (spot 22, Figure 6A).

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Pyruvate decarboxylase isozyme 2 (Os03g18220; spot 23, 45) and ascorbate

peroxidase (Os04g35520; spot 8) showed post-anoxic levels that were

comparable to pre-anoxic samples (Figure 6A).

Among the proteins that decreased in abundance in anoxic rice coleoptiles,

six were likely to be degradation products according to their gel molecular

mass (Spots 10, 16, 33-35, 6; Supplemental table 2, Figure 6C). This includes

two ATP synthase F0 subunit 1 spots, three tubulin-related protein spots and

an elongation factor. A peroxidase precursor (Os04g59150, spot 18) that

decreased under anoxia remained low in abundance during re-oxygenation

(Figure 6C). A GDSL-like lipase/acylhydrolase (Os06g06290, spot 5)

responded similarly to the peroxidase precursor (Figure 6C). Lipases are

involved in lipid hydrolysis and the Os06g06290 transcript in particular is

responsive to various a/biotic stresses (Jiang et al., 2012) and is down-

regulated in anoxic rice seedlings (Lasanthi-Kudahettige et al., 2007; Narsai et

al., 2009). Unlike the putative wheat peroxidase precursor protein, the rice

orthologue (Os04g59150) was lower in abundance under anoxia and

remained low during re-oxygenation (Spot 28; Supplemental table 2, Figure

4A, Figure 6C). A vesicle-fusing ATPase (Os05g44310) responded similarly to

the rice peroxidase. We also detected a 40A ribosomal protein S5 that

significantly decreased during anoxia, and appeared to stay low under post-

anoxia, except that the associated p-value did not meet the cut-off (p-

val=0.064).

Several rice proteins that decreased during anoxia then went on to

significantly increase during re-oxygenation (Figure 6C). These include actin

(spot 7, Os05g01600), ribosomal protein L6 (spot 11, Os09g31180), ribulose

bisphosphate carboxylase large chain (spot 57, Os01g58020) and three

phenylalanine ammonia lyase (spots 37-39, Os02g41630, pI 6.4-6.7) (Figure

6C, Supplemental table 2). Actin is a cytoskeletal protein and ribulose

bisphosphate carboxylase large chain is involved in photosynthesis. The

reversible abundance of these proteins suggests these proteins are true

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aerobic responders, whose functions are unnecessary or redundant enough

to afford O2-dependent degradation.

Lastly, we detected several rice proteins that did not significantly change

during anoxia, and instead showed significant changes during post-anoxia

when compared to anoxia or pre-anoxia (Figure 6B). However, it is suspected

that these proteins trended towards change, despite the fact that they did not

meet significance thresholds. For example, five Cysteine-rich proteins

appeared to increase during anoxia, yet their p-values ranged from 0.066-

0.21. During re-oxygenation, the abundances of these proteins failed to

significantly differ to anoxic samples, but compared to pre-anoxic samples,

their abundances were significantly higher (Spots 47, 51-54; Os08g04210,

Os08g04250, Os04g56430) (Supplemental table 2, Figure 6B). It is suspected

that biological variation was responsible for these observations. Nevertheless,

these proteins appear to show an apparent O2-dependent response in that

post-anoxic abundances are 2.8-4.2 fold higher than pre-anoxic abundances.

The transcripts of these proteins are also up-regulated under anoxia in

similarly aged rice coleoptiles (3-1007 X) (Lasanthi-Kudahettige et al., 2007) as

well as young rice seedlings (Narsai et al., 2009).

Several other proteins, whose apparent decrease in abundance failed to meet

the significance threshold upon the transition of rice to anoxia, showed a

significant increase during re-oxygenation (Figure 6B). This includes another

Cysteine-rich receptor-like protein kinase spot (spot 61, Os04g56430), a

glycolsyl hydrolase family 17 protein (spot 55, Os05g31140), an expansin

precursor (spot 56, Os01g60770) and (Figure 6B). The latter two proteins are

involved in cell re-modelling, and more specifically, expansins are known to be

involved in cell wall extension in O2-deprived rice (Huang et al., 2000; Lee and

Kende, 2001; Strohmeier et al., 2004). Interestingly, the expansin transcript

(Os01g60770) is significantly less abundant in young anoxic rice seedlings,

and also shows significant increases during re-oxygenation (Narsai et al.,

2009).

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Effect of oxygen availability of the activity of H2O2 –degrading enzymes

Re-oxygenation is likely to be accompanied by oxidative stress, so the activity

of two enzymes involved in antioxidant defence were measured. In wheat

coleoptiles, catalase activity was significantly higher in post-anoxic samples

compared to aerated samples (Figure 7A). The data suggest that an increase

in catalase activity starts to occur during the anoxic phase (p-val=0.12), but

the significance threshold is only met during re-oxygenation (p-val=0.01)

(Figure 7A). For rice, there was no significant difference between aerated,

anoxic and post-anoxic samples (Figure 7A). However, rice seedlings

germinated and grown under anoxia for six days show extremely low levels of

catalase activity (Figure 7A).

Wheat coleoptiles from post-anoxic and anoxic seedlings had significantly

higher peroxidase activity compared to aerated controls (Figure 7B). In rice,

post-anoxic coleoptiles had elevated activity compared to aeration (Figure 7B).

Once again, coleoptiles from seedlings under continuous anoxia had very low

peroxidase activity (Figure 7B).

Discussion

Similarities between the response of rice and wheat proteomes to

anoxia and re-oxygenation

While our previous study (Shingaki-Wells et al., 2011) failed to identify

significantly changing proteins in anoxic wheat coleoptiles, this study identified

several (Figure 6). This previous study set a strict ratio of change of at least

two, with few wheat proteins meeting that cut-off, and none that could be

identified. Here we focussed on significant p-value changes and undertook

more detailed analysis of gels to find any changes that might have gone

undetected previously.

We detected several similarities in the way that rice and wheat coleoptiles

respond to anoxia and re-oxygenation at the proteome level. For example,

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both species showed a decrease in phenylalanine ammonia lyase, a change

that was reversed during re-oxygenation (-3.72 X for anoxic wheat, -2.8 to –

5.05 X for rice) (Figure 6C, Figure 5C). However, Phe levels were only affected

in anoxic rice (Figure 1A, Figure 2A, Figure 3). In rice, anoxic Phe levels were

30 X that of aerated samples, and during re-oxygenation, Phe dropped by 10

X (Figure 1A). Wheat Phe levels remained remarkably stable (Figure 2A). A

decline in phenylalanine ammonia lyase might explain anoxic accumulation of

Phe in rice. An increase in this enzyme also supports declines in Phe during

post-anoxia. If Phe ammonia lyase contributes to the dynamics of

phenylalanine metabolism, it is unclear why Phe remains stable in wheat

coleoptiles. It is possible that Phe ammonia lyase requires post-translational

modification for full functionality, or that Phe metabolism in anoxic wheat is

controlled by other mechanisms.

A decrease in transcripts encoding Phe ammonia lyase under low oxygen

conditions has been reported in rice (Narsai et al., 2009). Potato tubers

accumulate this protein when bruised under aerated conditions but not

hypoxic conditions (Vayda and Schaeffer, 1988). Phe ammonia lyase is

involved in the polyphenolic production pathway, compounds that are

constituents of phytoalexins and lignins (Lamb et al., 1989; Rumeau et al.,

1990). Phytoalexin and lignin accumulation is a common response to

wounding (Rumeau et al., 1990). Hypoxic tubers that are wounded are also

more susceptible to bacterial soft rot (Rumeau et al., 1990). Even though

anaerobiosis interferes with the potato tuber wound response, the expression

of mRNAs encoding glycolytic enzymes is maintained, suggesting that the

response to low oxygen is prioritised over the wounding response (Butler et al.,

1990; Rumeau et al., 1990). The decreased abundance of this protein in rice

and wheat coleoptiles may be a product of inhibited mRNA or protein

synthesis, in combination with maintained degradation rates, since it is known

that selective transcription and translation occur under low oxygen (Branco-

Price et al., 2008; Narsai et al., 2009). Nevertheless, it is intriguing that this

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response is conserved between two species that differ so greatly in their

anoxia tolerance.

Rice and wheat also showed increases in pyruvate decarboxylase (PDC)

isozyme 2 under anoxia (Figure 6A, Figure 5A), suggesting operation of the

NAD+-producing ethanolic fermentation pathway. Post-anoxia saw a

divergence in response between these two species, with rice PDC trending

towards down-regulation during re-oxygenation so that post-anoxic levels

were comparable to pre-anoxia (spot 23, 45; Figure 6A). In wheat, PDC

remained elevated in post-anoxic coleoptiles (spot 33, Figure 5A). This could

suggest that elevated PDC activity is advantageous in post-anoxic wheat, or

that wheat, in contrast to rice, has an inadequate response to re-oxygenation.

Metabolomic datasets suggest that a subtle response to re-oxygenation is

likely, since metabolites whose abundances are highly responsive to oxygen in

rice do not appear to be so in wheat. In particular, the major trend observed

was a highly dynamic amino acid pool in rice, which in contrast to wheat,

trended towards rapid accumulation during anoxia and consumption during

re-oxygenation (Figure 1A, Figure 2A). Wheat showed many fewer changes in

amino acids during both anoxia and re-oxygenation (Figure 2A), in line with our

previous observation that the response of wheat coleoptiles to anoxia is

subdued and perhaps inadequate (Shingaki-Wells et al., 2011).

Differential regulation of translation-related proteins

The increase in a putative eukaryotic translation initiation factor in anoxic

wheat coleoptiles (spot 7, Figure 5A) is interesting in light of the fact that

overall protein synthesis rates are decreased in anoxic plants (Mocquot et al.,

1981). Rice also showed differential regulation of translation-related proteins,

specifically, a 40S ribosomal protein S5 (-2.02 X, spot 26, Figure 6C) and

elongation factors (Shingaki-Wells et al., 2011). Since selective translation is

known to occur in hypoxic Arabidopsis (Branco-Price et al., 2008), the up-

regulation of this translation initiation factor in anoxia-intolerant wheat

suggests specific factors may be required to direct translation under low

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oxygen. Although the post-anoxic abundance of this protein was not

significantly lower than that of the anoxic abundance, the final abundance is

not significantly different to pre-anoxic levels, suggesting specificity of this

factor under low oxygen. Although wheat had a weak proteomic response in

our previous study (Shingaki-Wells et al., 2011), protein abundance does

appear to be regulated by oxygen levels. The capacity for synthesis however,

appears to be greater in rice, with rice coleoptiles showing an average fold

change – for proteins significantly increasing in abundance – of 4.8 X, and

wheat showing an average of 1.8 X. Since protein synthesis is energetically

demanding, this may simply be a reflection of the ability of rice to mobilise

endosperm starch reserves under anoxia to enhance glycolytic rates

(Guglielminetti et al., 1995).

Proteins of unknown function respond to anoxia and re-oxygenation

We detected several proteins with unknown function, annotated as Cysteine-

rich repeat secretory proteins in rice (Spot 41, 51-52; Figure 6B; Os08g04210,

Os08g04250). These proteins did not show an increase under anoxia that

was significant, however post-anoxic abundances were significantly higher

than pre-anoxic abundances. In our previous study, these proteins were

significantly higher in the coleoptiles of six-day-old continuously anoxic rice

seedlings relative to four-day-old aerated seedlings (Shingaki-Wells et al.,

2011). The transcripts of these proteins are 248-1007 X higher in continuously

anoxic coleoptiles relative to aeration (Lasanthi-Kudahettige et al., 2007). As

discussed previously (Shingaki-Wells et al., 2011b), the Arabidopsis

orthologue (At5g48540) is also responsive to low oxygen (Branco-Price et al.,

2008). This protein contains two DUF26 domains (domains of unknown

function), common to the plasmodesmata-located protein family (PDLP1)

(Thomas et al., 2008). Knockout analysis revealed that these proteins are

involved in cell-to-cell crosstalk (Thomas et al., 2008). At5g48540, however,

lacks a transmembrane domain and instead forms large bodies in the

apoplast, thus differentiating this protein from the PDLP1 family (Thomas et al.,

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2008). The function of these low oxygen-responsive proteins awaits further

study.

Oxygen availability affects proteins involved in cell structure

Several proteins involved in cell wall re-modelling were detected in our study.

In rice, a glycosyl hydrolases family 17 protein (Os05g31140; spot 55) and an

expansin precursor (Os01g60770; spot 56, Figure 6B) showed low

abundance during anoxia, and strong increases during post-anoxia. The

corresponding expansin transcript is also lower in anoxic rice coleoptiles

(Lasanthi-Kudahettige et al., 2007). Transcripts of the expansin family vary in

their response to anoxia (Magneschi et al., 2009). Actin, a protein integral to

the actin cytoskeleton, also showed a decrease under anoxia in rice, which

was reversed during re-oxygenation (Os05g01600; spot 7, Figure 6C). In

wheat, a glycosyl hydrolases family 16 protein (spot 51, Figure 5B) showed a

significantly lower abundance during post-anoxia, relative to pre-anoxic

coleoptiles, and a polygalacturonase (spot 20, Figure 5B) showed a decrease

during re-oxygenation, relative to anoxia. In soybean roots, an actin protein

has been reported to increase during re-oxygenation, while others decreased,

which suggests differing and oxygen-dependent roles for these actins in cell

re-modelling (Salavati et al., 2012). Other proteins involved in cell wall

remodelling were also detected in soybean roots during re-oxygenation

(Salavati et al., 2012), indicating a perturbation of cell wall metabolism in

multiple species subjected to low oxygen stress. The proteins found in rice

trended towards a return to pre-anoxic levels. Glycosyl hydrolases family 16

protein in wheat remained significantly lower during re-oxygenation, and while

alternative explanations exist, this might suggest a failure to re-adjust

appropriately to the return of oxygen (Figure 5B).

Sugar metabolism contrasts in anoxic rice and wheat

Metabolite analysis revealed large differences in how rice and wheat re-model

metabolism during anoxia and re-oxygenation (Figure 1, Figure 2, Figure 3).

Sucrose is especially important under anoxia since it is a transportable sugar

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originating from the starchy endosperm of rice (Perata et al., 1997). The ability

of rice to increase sucrose during anoxia (Figure 1B), a response that was

absent in wheat (Figure 2B), aligns with observations that the Pasteur effect,

an increase in the glycolytic rate, is strong in rice and weak in wheat (Waters

et al., 1991). The consumption of sucrose in anoxic wheat appears to

maintain levels of glucose and fructose, to support glycolysis (Figure 2B).

During re-oxygenation, sucrose decreases in rice, but relative to pre-anoxic

levels, sucrose is still significantly higher (Figure 1B). A decrease in sucrose

post-anoxia is consistent with responses seen in other rice studies (Narsai et

al., 2009). In wheat, the low sucrose levels found under anoxia fail to increase

upon re-aeration, suggesting a failure of wheat coleoptiles to mobilise sugars

from starch within the first day of re-oxygenation (Figure 2B). Since aerobic

respiration is efficient in terms of ATP synthesis per sugar unit consumed

(Gibbs and Greenway, 2003), it is unknown whether a low level of sucrose

would affect energy metabolism in post-anoxic wheat. The decrease of post-

anoxic sucrose in rice suggests that starch metabolism is regulated rapidly by

changes in oxygen concentrations, a characteristic which probably

contributes to one aspect of anoxia tolerance. 3-phosphoglyceric acid, an

intermediate of glycolysis, shows contrasting responses between rice and

wheat (Figure 1B, Figure 2B). In rice, this metabolite increases during anoxia,

and is rapidly consumed during re-oxygenation. In wheat, 3-phosphyglyceric

acid decreases during anoxia, and partially recovers during post-anoxia.

These observations further support the large Pasteur effect in anoxic rice

relative to wheat (Waters et al., 1991). This is also supported by previous our

report where anoxic rice was able to increase the production of several

glycolytic enzymes by over two-fold (Shingaki-Wells et al., 2011).

In wheat, NADP-dependent malic enzyme, which converts malate to pyruvate,

increases during anoxia and stays elevated during re-oxygenation (Figure 5A).

The activity of this enzyme is probably activated by low pH (Edwards et al.,

1998), a well-documented consequence of anoxia in plants (Menegus et al.,

1989; Menegus et al., 1991). During the early stages of hypoxia, a six-fold

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157

increase in the activity of this enzyme in maize root tips is seen (Edwards et al.,

1998). Consistent with the hypothesis that malic enzyme acts to synthesise

pyruvate, is the decrease of malate seen in anoxic wheat (Figure 2C). Malate

remains at low levels during re-oxygenation in wheat (Figure 2C). The potential

role or consequence of pyruvate production in anoxic and post-anoxic wheat

is unknown, and awaits further investigation.

Amino acid pools respond strongly to oxygen availability in rice, but

not in wheat

As discussed above, the overall trend for rice was an accumulation of amino

acids under low oxygen (Figure 1A, Supplemental Figure 1A). Fewer amino

acids showed changes in anoxic wheat (Figure 2A, Supplemental Figure 2A).

Since many amino acids are directly or indirectly synthesised from

intermediates of glycolysis or the TCA cycle, it is possible that the high

glycolytic rate, permitted by high sucrose levels in rice (Figure 1B), contributes

to amino acid accumulation in the absence of a mitochondrial terminal

electron acceptor. Wheat, on the other hand, does not appear to have an

abundance of mobilised sugar substrate (Figure 1A), thus minimising the

branching off from glycolysis and/or the TCA cycle to synthesise amino acids.

The accumulation of alanine, for example, is thought of as an alternative, non-

toxic endpoint to ethanol and lactic acid production (Reggiani et al., 1988). In

cases where a limited amount of oxygen is available (hypoxia), production of

alanine may be beneficial in diverting pyruvate from processes involving

respiratory oxygen consumption, preventing a transition from hypoxia to

anoxia (Zabalza et al., 2009). Alternatively, amino acid production may simply

be a product of protein degradation, and amino acid inter-conversion

(Reggiani et al., 1988), although the increase in several enzymes involved in

amino acid synthesis in anoxic rice suggests de novo synthesis is also a

contributor (Shingaki-Wells et al., 2011). The absence of alanine production in

anoxic wheat could be a feature of glycolytic substrate limitation, or a failure to

appropriately regulate enzymes involved in alanine production. It has been

reported that rice accumulates more succinate than lactate under anoxia,

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whereas wheat accumulates much more lactate, which might contribute to

the cytoplasmic acidification observed in wheat (Menegus et al., 1989;

Menegus et al., 1991). The rapid accumulation of succinate in rice, but not

wheat, is consistent with our results (Figure 1C, Figure 2C). Amino acid

accumulation may also contribute to maintenance of osmotic pressure,

counteracting any decrease caused by rapid sugar consumption (Reggiani et

al., 1988).

Re-oxygenation resulted in major changes to the metabolome of rice,

specifically, 16 of the 17 amino acids accumulating under anoxia were

consumed post-anoxia, the exception being Orn (Figure 1A, Figure 3A). In

contrast, of the nine accumulating amino acids in anoxic wheat, none showed

significant decreases during re-oxygenation, relative to anoxia (Figure 2A,

Figure 3B). This might improve the success of rice seedlings recovering from

anoxia if the carbon skeletons of amino acids were directed into primary

energy metabolism. Indeed, citrate, aconitate, isocitrate and 2-oxoglutarate

accumulate post-anoxia, suggesting resumption of TCA cycle activity. Post-

anoxic conversion of Ala to pyruvate could contribute to this flow, as

suggested in Arabidopsis studies (Miyashita et al., 2007). It is worth pointing

out that the accumulation of Ala during anoxia is 98 X in rice, whereas in

wheat, Ala fails to accumulate (Figure 1A, Figure 2A), suggesting a higher

capacity of rice to engage in post-anoxic Ala metabolism. In line with this is

the observation that wheat coleoptiles accumulate Ala during post-anoxia

(Figure 2A).

Succinate accumulates rapidly in anoxic rice (34 X, Figure 1C), and less so in

wheat (1.4 X, Figure 2C). During re-oxygenation, succinate is rapidly

consumed in rice (Figure 1C), which is likely a result of oxygen-dependent

electron transport chain operation. Succinate is also consumed post-anoxia in

wheat (Figure 2C). Presumably, one day of anoxia is not long enough to inhibit

the re-initiation electron transport chain operation in both species when

oxygen returns.

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159

Oxidative stress defence and its role during recovery

The detection of multiple peroxidase enzymes changing in abundance under

anoxia and/or re-oxygenation suggests oxygen availability affects oxidative

defence status. In rice, a peroxidase precursor decreased under anoxia and

remained low in abundance after one day of re-oxygenation (Os04g59150;

spot 18, Figure 6C). In contrast, the stromal ascorbate peroxidase increased

in anoxic rice and remained elevated during post-anoxia (Os04g35520; spot 8.

Figure 6A). We previously detected two ascorbate peroxidases originating

from different genes that decreased in anoxic rice coleoptiles (Os03g17690,

Os07g49400) (Shingaki-Wells et al., 2011). Ascorbate peroxidase activity has

been shown to decrease under low oxygen in wheat roots, with a subsequent

return to pre-anoxic levels post-anoxia (Biemelt et al., 1998). In our

experiments however, we detected one peroxidase precursor in wheat,

whose post-anoxic abundance was significantly higher than pre-anoxic levels

(spot 28, Figure 5B).

Since oxidative stress is a known stress during re-oxygenation (Blokhina et al.,

2003), we wanted to measure the activity of two H2O2 decomposing enzymes

to clarify these apparent contradictions in rice. Wheat and rice peroxidase

activity significantly increased during re-oxygenation, relative to anoxia (Figure

7B). This agrees with the direction of change that the wheat peroxidase

precursor showed (spot 28, Figure 5B), but differs from what was seen in rice

(Os04g59150; spot 18, Figure 6C). Os04g59150 has been experimentally

shown to be located in etioplasts (Reiland et al., 2011) and is predicted to be

a secretory or endoplasmic reticulum protein (Narsai et al., 2013).

For stromal ascorbate peroxidase the activity data agrees to some extent,

except that activity did not increase under anoxia, while the abundance of

Os04g33520 did (spot 8, Figure 6A). The location of this protein is

experimentally verified in the chloroplast (Kleffmann et al., 2007; Narsai et al.,

2013; Xu et al., 2013). Overall, it is difficult to correlate protein abundance

data with peroxidase activity, since activity measurements are the sum of

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160

multiple peroxidases. It is possible that different peroxidases are regulated at

the post-translational level to affect their activity, and thus the changes will

influence the general peroxidase activity measurement.

A similar change in activity was seen in wheat catalase, but not rice (Figure

7A). The post-anoxic activity of catalase was not significantly different to

anoxic or aerated rice coleoptiles. In rice coleoptiles from seedlings

germinated and grown under continuous anoxia for 6 days, the activity of both

enzymes were extremely low, suggesting a role for oxygen exposure in the

regulation of these enzymes. Indeed, it has been shown that anti-oxidant

levels are affected by both low oxygen and re-aeration in wheat roots (Biemelt

et al., 1998). In summary, anoxia followed by re-oxygenation affects the status

of the anti-oxidant defence system, but the exact proteins responsible for

these changes are unknown.

Conclusion The response of rice and wheat to anoxia and re-oxygenation is highly

divergent, particularly at the metabolome level. While rice accumulates many

amino acids, wheat accumulates fewer amino acids at rates less rapid than

rice. Post-anoxia results in the consumption of amino acids in rice, which is

suspected to improve the retention of carbon skeletons, that would otherwise

be lost if pyruvate was diverted solely to ethanol production. Proteomes are

also affected by oxygen availability, including enzymes involved in glycolysis

and ethanolic fermentation. Generally, the degree of accumulation of proteins

in wheat was subtle, compared to rice. Further proteomic experiments

involving iTRAQ may be required to delve deeper into the post-anoxic

response. We conclude that active metabolic re-modelling in rice plays a role

in defence against anoxia and re-oxygenation, which may underlie its superior

tolerance to this stress.

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Bibliography

Abeles FB, Biles CL (1991) Characterization of peroxidases in lignifying peach fruit endocarp. Plant Physiology 95: 269-273

Arnell N, Liu CX (2001) Climate change 2001: hydrology and water resources. In Intergovernmental Panel on Climate Change,

Arshad RR, Shafi S (2010) Pakistan Floods 2010: Preliminary Damage and Needs Assessment. In Asian Development Bank and World Bank, Islamabad, Pakistan

Bailey-Serres J, Lee SC, Brinton E (2012) Waterproofing crops: effective flooding survival strategies. Plant Physiology 160: 1698-1709

Bailey-Serres J, Voesenek LACJ (2008) Flooding stress: acclimations and genetic diversity. 59: 313-339

Biemelt S, Keetman U, Albrecht G (1998) Re-aeration following hypoxia or anoxia leads to activation of the antioxidative defense system in roots of wheat seedlings. Plant Physiology 116: 651-658

Blokhina O, Virolainen E, Fagerstedt KV (2003) Antioxidants, Oxidative Damage and Oxygen Deprivation Stress: a Review. Annals of Botany 91: 179-194

Blokhina OB, Fagerstedt KV, Chirkova TV (1999) Relationships between lipid peroxidation and anoxia tolerance in a range of species during post-anoxic reaeration. Physiologia Plantarum 105: 625-632

Branco-Price C, Kaiser KA, Jang CJH, Larive CK, Bailey-Serres J (2008) Selective mRNA translation coordinates energetic and metabolic adjustment to celluar oxygen deprivation and reoxygenation in Arabidopsis thaliana. The Plant Journal 56: 743-755

Butler W, Cook L, Vayda ME (1990) Hypoxic stress inhibits multiple aspects of the potato tuber wound response. Plant Physiology 93: 264-270

Carroll AJ, Badger MR, Harvey Millar A (2010) The MetabolomeExpress Project: enabling web-based processing, analysis and transparent dissemination of GC/MS metabolomics datasets. BMC Bioinformatics 11: 376

Chance B, Maehly AC (1955) Assay of catalases and peroxidases. In S. P. Colowick and N. O. Kaplan, eds., Methods in Enzymology, Vol II. Academic Press, New York, pp 764-775

Edwards S, Nguyen BT, Do B, Roberts JKM (1998) Contribution of malic enzyme, pyruvate kinase, phosphoenolpyruvate carboxylase, and the krebs cycle to respiration and biosynthesis and to intracellular pH regulation during hypoxia in maize root tips observed by nuclear magnetic resonance imaging and gas chromatography-mass spectrometry. Plant Physiol 116: 1073-1081

Gibbs J, Greenway H (2003) Mechanisms of anoxia tolerance in plants. I. Growth, survival and anaerobic catabolism. Functional Plant Biology 30: 1–47

Page 175: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

163

Guglielminetti L, Yamauchi M, Perata P, Alpi A (1995) Amylotic activities in cereal seeds under aerobic and anaerobic conditions. Plant Physiology 109: 1069-1076

Howell KA, Narsai R, Carroll A, Ivanova A, Lohse M, Usadel B, Millar AH, Whelan J (2009) Mapping metabolic and transcript temporal switches during germination in rice highlights specific transcription factors and the role of RNA instability in the germination process. Plant Physiology 149: 961-980

Huang J, Takano T, Akita S (2000) Expression of -expansin genes in young seedlings of rice (Oryza sativa L.). Planta 211: 467-473

Jiang Y, Rongjun C, Dong J, Xu Z, Gao X (2012) Analysis of GDSL lipase (GLIP) family genes in rice (Oryza sativa). Plant Omics 5: 351-358

Kato-Noguchi H, Ohashi C (2006) Effects of anoxia on amino acid levels in rice coleoptiles. Plant Production Science 9: 383-387

Kleffmann T, von Zychlinski A, Russenberger D, Hirsch-Hoffmann M, Gehrig P, Gruissem W, Baginsky S (2007) Proteome dynamics during plastid differentiation in rice. Plant Physiol 143: 912-923

Lamb CJ, Lawton MA, Dron M, Dixon RA (1989) Signals and transduction mechanisms for activation of plant defenses against microbial attack. Cell 56: 215-224

Lasanthi-Kudahettige R, Magneschi L, Loreti E, Gonzali S, Licausi F, Novi G, Beretta O, Vitulli F, Alpi A, Perata P (2007) Transcript profiling of the anoxic rice coleoptile. Plant Physiology 144: 218-231

Lee Y, Kende H (2001) Expression of beta-expansins is correlated with internodal elongation in deepwater rice. Plant Physiology 127: 645-654

Magneschi L, Kudahettige RL, Alpi A, Perata P (2009) Expansin gene expression and anoxic coleoptile elongation in rice cultivars. Journal of Plant Physiology 166: 1576-1580

Menegus F, Cattaruzza L, Chersi A, Fronza G (1989) Differences in the anaerobic lactate-succinate production and in the changes of cell sap pH for plants with high and low resistance to anoxia. Plant Physiology 90: 29-32

Menegus F, Cattaruzza L, Mattana M, Beffagna N, Ragg E (1991) Response to anoxia in rice and wheat seedlings. Changes in pH of intracellular components, glucose-6-phosphate level, and metabolic rate. Plant Physiology 95: 760-767

Miyashita Y, Dolferus R, Ismond KP, Good AG (2007) Alanine aminotransferase catalyses the breakdown of alanine after hypoxia in Arabidopsis thaliana. The Plant Journal 49: 1108-1121

Mocquot B, Prat C, Mouches C, Pradet A (1981) Effect of anoxia on energy charge and protein synthesis in rice embryos. Plant Physiology 68: 636-640

Narsai R, Devenish J, Castleden I, Narsai K, Xu L, Shou H, Whelan J (2013) Rice DB: An Oryza Information Portal linking annotation, sub-cellular location, function, expression, regulation and evolutionary information for rice and Arabidopsis. Plant Journal

Page 176: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

164

Narsai R, Howell KA, Carroll A, Ivanova A, Millar AH, Whelan J (2009) Defining core metabolic and transcriptomic responses to oxygen availability in rice embryos and young seedlings. Plant Physiology 151: 306-322

Perata P, Guglielminetti L, Alpi A (1997) Mobilization of endosperm reserves in cereal seeds under anoxia. Annals of Botany 79: 49–56

Reggiani R, Cantu CA, Brambilla I, Bertani A (1988) Accumulation and interconversion of amino acids in rice roots under anoxia. Plant and Cell Physiology 29: 981-987

Reiland S, Grossmann J, Baerenfaller K, Gehrig P, Nunes-Nesi A, Fernie AR, Gruissem W, Baginsky S (2011) Integrated proteome and metabolite analysis of the de-etiolation process in plastids from rice (Oryza sativa L.). Proteomics 11: 1751-1763

Rumeau D, Maher EA, Kelman A, Showalter AM (1990) Extensin and phenylalanine ammonia-lyase gene expression altered in potato tubers in response to wounding, hypoxia, and Erwinia carotovora infection. Plant Physiology 93: 1134-1139

Salavati A, Khatoon A, Nanjo Y, Komatsu S (2012) Analysis of proteomic changes in roots of soybean seedlings during recovery after flooding. J Proteomics 75: 878-893

Shingaki-Wells RN, Huang S, Taylor NL, Carroll AJ, Zhou W, Millar AH (2011) Differential molecular responses of rice and wheat coleoptiles to anoxia reveal novel metabolic adaptations in amino acid metabolism for tissue tolerance. Plant Physiology 156: 1706-1724

Shingaki-Wells RN, Huang S, Taylor NL, Millar AH (2011b) Pursuing the identification of O2 deprivation survival mechanisms in plants related to selective mRNA translation, hormone-independent cellular elongation and preparation for the arrival of oxygen. Plant Signaling & Behavior 6: 1612-1615

Strohmeier M, Hrmova M, Fischer M, Harvey AJ, Fincher GB, Pleiss J (2004) Molecular modeling of family GH16 glycoside hydrolases: Potential roles for xyloglucan transglucosylases/hydrolases in cell wall modification in the poaceae. Protein Science 13

Thomas CL, Bayer EM, Ritzenthaler C, Fernandez-Calvino L, Maule AJ (2008) Specific targeting of a plasmodesmal protein affecting cell-to-cell communication. PLoS Biology 6: 180-190

Vayda ME, Schaeffer HJ (1988) Hypoxic stress inhibits the appearance of wound-response proteins in potato tubers. Plant Physiology 88: 805-809

Waters I, Morrels S, Greenway H, Colmer T (1991) Effects of anoxia on wheat seedlings. II. Influence of O2 supply prior to anoxia on tolerance to anoxia, alcoholic fermentation, and sugar levels. Journal of Experimental Botany 42: 1437-1447

Welinder KG, Justesen AF, Kjaersgård IV, Jensen RB, Rasmussen SK, Jespersen HM, Duroux L (2002) Structural diversity and transcription of class III peroxidases from Arabidopsis thaliana. European Journal of Biochemistry 269: 6063–6081

Page 177: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

165

Wessel D, Flügge UI (1984) A method for the quantitative recovery of protein in dilute solution in the presence of detergents and lipids. Analytical Biochemistry 138: 141-143

Xu L, Carrie C, Law SR, Murcha MW, Whelan J (2013) Acquisition, conservation, and loss of dual-targeted proteins in land plants. Plant Physiol 161: 644-662

Zabalza A, Van Dongen JT, Froehlich A, Oliver SN, Faix B, Gupta KJ, Schmalzlin E, Igal M, Orcaray L, Royuela M, Geigenberger P (2009) Regulation of respiration and fermentation to control the plant internal oxygen concentration. Plant Physiology 149: 1087-1098

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Figures

Figure 1. Relative metabolite signals in rice coleoptiles subjected to air, anoxia

and re-oxygenation.

Figure 2. Relative metabolite in wheat coleoptiles subjected to air, anoxia and

re-oxygenation.

Figure 3. Metabolite response ratios in rice and wheat coleoptiles from aerated

seedlings subjected anoxia and re-oxygenation.

Figure 4. Representative images of Differential in Gel Electrophoresis (DiGE)

using rice and wheat coleoptiles from aerated seedlings subjected anoxia and re-

oxygenation.

Figure 5. Relative protein abundance in wheat coleoptiles subjected to air,

anoxia and re-oxygenation.

Figure 6. Relative protein abundance in rice coleoptiles subjected to air, anoxia

and re-oxygenation.

Figure 7. Catalase and peroxidase activity in rice and wheat coleoptiles.

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7

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16

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xt p

age.

0 1 2 3 4 5 6 7 8 9 10 L-S

erine

Glyc

ine

L-Tryp

topha

n

L-Phe

nylal

anine

L-Tyro

sine L-A

lanine

L-Leu

cine

L-Vali

ne

L-Glut

amic

acid L-G

lutam

ine L-P

roline

Ornithi

ne Putr

escin

e L-Argi

nine

Gamma-A

minobu

tyric

acid

L-Asp

artic

acid L-A

spara

gine

L-Lys

ine

L-2-A

minoad

ipic a

cid

L-Hom

oseri

ne

L-Meth

ionine

L-Thre

onine

L-Iso

leucin

e W

heat

Normalised signal A

Page 182: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

17

0

Figu

re 2

. Rel

ativ

e m

etab

olite

sig

nals

in w

heat

col

eopt

iles

subj

ecte

d to

air

(dar

k bl

ue),

anox

ia (g

reen

) and

re-

oxyg

enat

ion

(ligh

t blu

e).

See

full

figur

e ca

ptio

n on

pre

viou

s pa

ge.

0 0.

2 0.

4 0.

6 0.

8 1 1.

2 1.

4 1.

6 1.

8

Sucros

e

D-Gluc

ose

D-Fruc

tose

Glucos

e 6-ph

osph

ate

Fructos

e 6-ph

osph

ate

3-Pho

spho

glyce

ric ac

id

Whe

at

Normalised signal

0 0.

5 1 1.

5 2 2.

5 3 3.

5 4 4.

5

Citric a

cid cis

-Aco

nitic

acid

Isocit

ric ac

id Oxoglu

taric

acid

Succin

ic ac

id Fum

aric a

cid

L-Mali

c acid

W

heat

Normalised signal

C

B

Page 183: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

17

1

.

Fig

ure

3. P

ost-

anox

ic m

etab

olom

es o

f ric

e (A

) and

whe

at (B

) col

eopt

iles.

Ful

l fig

ure

capt

ion

on fo

llow

ing

page

s.

Met

abol

ite R

espo

nse

Valu

es

Hig

her u

nder

ano

xia

Hig

her u

nder

pos

t-ano

xia

Unc

hang

ed (n

/s)

Not

det

ecte

d

glyc

olys

is TC

A cy

cle

sucr

ose

gluc

ose

fruct

ose

gluc

ose-

6-P

fruct

ose-

6-P

fruct

ose-

1,6-

bis-

P

G-3

-P

Cys

S

er

Gly

3-P

GA

PE

P

pyru

vate

acet

yl C

oA

citra

te

acon

itate

isoc

ritra

te

2-ox

oglu

tara

te

succ

inyl

-CoA

succ

inat

e

fum

arat

e

mal

ate

oxal

oace

tate

acet

alde

hyde

et

hano

l

Ala

Leu

Val

Asn

Asp

Lys

hom

oser

ine

Thr

Met

Ile

Glu

P

ro

Gln

H

is

GA

BA

SS

A

orni

thin

e

Arg

Phe

Tyr

Trp

shik

imat

e

2-am

inoa

dipi

c ac

id

putre

scin

e

DH

AP

1,3-

PG

A

2-P

GA

3-ph

osph

oser

ine

3-ph

osph

ohyd

ro

-pyr

uvat

e

UD

P-g

luco

se

chor

ism

ate

0.

4

0.1

0.

2

6.3

2.9

8.

2

12.6

0

.03

0

.2

1.

3

0

.3

1.2

0.2

0.

2

0.

6

0

.5

0.

4

0.3

0.

5

0.1

0.

3

0.

2

1.5

0.5

0.

3

0.

6

0.3

0.4

0.1

0.1

0

.6

1.7

0

.6

A

Page 184: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

17

2

Fig

ure

3.P

ost-

anox

ic m

etab

olom

es o

f ric

e (A

) and

whe

at (B

) col

eopt

iles.

Ful

lfig

ure

capt

ion

on fo

llow

ing

page

.

glyc

olys

is TC

A cy

cle

sucr

ose

gluc

ose

fruct

ose

gluc

ose-

6-P

fruct

ose-

6-P

fruct

ose-

1,6-

bis-

P

G-3

-P

Cys

S

er

Gly

3-P

GA

PE

P

pyru

vate

acet

yl C

oA

citra

te

acon

itate

isoc

ritra

te

2-ox

oglu

tara

te

succ

inyl

-CoA

succ

inat

e

fum

arat

e

mal

ate

oxal

oace

tate

acet

alde

hyde

et

hano

l

Ala

Leu

Val

Asn

Asp

Lys

hom

oser

ine

Thr

Met

Ile

Glu

P

ro

Gln

H

is

GA

BA

SS

A

orni

thin

e

Arg

Phe

Tyr

Trp

shik

imat

e

2-am

inoa

dipi

c ac

id

putre

scin

e

DH

AP

1,3-

PG

A

2-P

GA

3-ph

osph

oser

ine

3-ph

osph

ohyd

ro

-pyr

uvat

e

UD

P-g

luco

se

chor

ism

ate

1.2

1.3

2.6

1.

1

5.0

0.6

1.9

4.7

0

.6

0

.7

1.0

1

.7

1

.6

1.1

3.

6

0.

7

0.9

1

.1

1.

4

1

.4

1.1

0

.7

1.6

1.

1

1.

1

0.9

1.4

1.

3

1.

5

1.9

0.6

1.0

1.1

1.3

1

.3

0.8

0

.8

Met

abol

ite R

espo

nse

Valu

es

Hig

her u

nder

ano

xia

Hig

her u

nder

pos

t-ano

xia

Unc

hang

ed (n

/s)

Not

det

ecte

d

B

Page 185: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

17

3

Fig

ure

3. M

etab

olite

res

pons

e ra

tios

in r

ice

(A) a

nd w

heat

(B) c

oleo

ptile

s fro

m a

erat

ed s

eedl

ings

sub

ject

ed a

noxi

a an

d re

-oxy

gena

tion.

Met

abol

ites

in g

reen

are

mor

e ab

unda

nt u

nder

ano

xia

and

thos

e in

blu

e ar

e m

ore

abun

dant

dur

ing

post

-ano

xia.

Dar

k gr

ey in

dica

tes

no

sign

ifica

nt d

iffer

ence

bet

wee

n th

e si

gnal

s in

the

two

trea

tmen

ts a

nd li

ght g

rey

indi

cate

s th

at th

e m

etab

olite

was

not

det

ecte

d. N

umbe

rs

indi

cate

the

ratio

of c

hang

e th

at o

ccur

s du

ring

re-o

xyge

natio

n, r

elat

ive

to a

noxi

a. F

igur

es o

n pr

evio

us p

ages

.

Page 186: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

174

Figure 4. Representative images of Differential in Gel Electrophoresis (DiGE) using rice (A) and wheat (B) coleoptiles from aerated seedlings subjected anoxia and re-oxygenation. Full figure caption follows on next page.

A

Page 187: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

175

Figure 4. Representative images of Differential in Gel Electrophoresis (DiGE) using rice (A) and wheat (B) coleoptiles from aerated seedlings subjected anoxia and re-oxygenation. In this image, anoxic samples were labeled with Cy 5 (red) and post-anoxic samples with Cy 3 (green). An overlay of the image produces spots of differing colours, including red for proteins more abundant under anoxia, green for proteins more abundant under post-anoxia, and yellow for proteins that have the same abundance under both treatments. For details on DIGE, refer to the methods section. Delta2D (Decodon) was used to analyse gel images, and significantly changing spots (p-val<0.05) were selected for MALDI-TOF MS/MS analysis. Caption continued on next page.

B

Page 188: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

176

Figure 4. Caption continued. To see detail on spot identification, see Supplemental table 1 and 2 for wheat and rice, respectively, as well as Figures 5-6. Figures on previous pages.

Page 189: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

177

Figure 5. Relative protein abundance in wheat coleoptiles subjected to air (dark blue), anoxia (green) and re-oxygenation (light blue). Aerated protein abundances were normalised to 1 and compared to anoxic and post-anoxic samples. The numbers that precede protein identities indicate the spot numbers shown in Figure 4B. Proteins were split into three categories depending on the response during anoxia. A. Proteins that significantly increased from air to anoxia; B. Proteins that did not significantly change in abundance from air to anoxia; C. Proteins that significantly decreased under anoxia. Above each protein is a significance indicator; the first position indicates the p-val associated with the change from air to anoxia, the second position relates to the anoxia and post-anoxia comparison, and the third position relates to the post-anoxia and air comparison. * indicates the difference is significant (p-val<0.05); - indicates the difference is not significant; # indicates this is probably a protein degradation product. Figure 5B and Figure 5C on following pages.

0.0

0.5

1.0

1.5

2.0

2.5

3.0

7. Euk

ar. tra

nslat

ion IF

5A

43. e

xpres

sed p

rotein

18. 1

2-oxo

phyto

dieno

ate re

ducta

se

33. P

yr de

carbo

xylas

e iso

zyme 2

34. N

ADP-depe

nden

t mali

c enz

yme,

12. e

xpres

sed p

rotein

Nor

mal

ised

sig

nal

*/-/- */-/* */*/-

A

Page 190: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

17

8

Fig

ure

5. R

elat

ive

prot

ein

abun

danc

e in

whe

at c

oleo

ptile

s su

bjec

ted

to a

ir (d

ark

blue

), an

oxia

(gr

een)

and

re-

oxyg

enat

ion

(ligh

t bl

ue).

Full

figur

e ca

ptio

n on

pre

viou

s pa

ge.

0.0

0.5

1.0

1.5

2.0

2.5

3.0

26. e

xpres

sed p

rotein

29

. exp

resse

d prot

ein

32. N

t PPas

e/pho

spho

dieste

rase

36. b

-gluc

osida

se, e

xo-b-

gluca

nase

37

. exp

resse

d prot

ein

51. g

lycos

yl hy

drolas

es fa

mily 16

25. D

NA-bind

ing pr

otein

28. p

eroxid

ase p

recurs

or 20. p

olyga

lactur

onas

e

38. H

sp20

/a-cry

stallin

family

31. u

nivers

al str

ess p

rotein

domain

-/*/*

-/-/*

-/*/-

Normalised signal

#

#

B

Page 191: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

17

9

Fig

ure

5. R

elat

ive

prot

ein

abun

danc

e in

whe

at c

oleo

ptile

s su

bjec

ted

to a

ir (d

ark

blue

), an

oxia

(gr

een)

and

re-

oxyg

enat

ion

(ligh

t bl

ue).

Full

figur

e ca

ptio

n on

pre

viou

s pa

ge.

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4

1.6

1.8

47. e

xpres

sed p

rotein

30. e

xpres

sed p

rotein

6.

expre

ssed

prote

in

21. A

TP synth

ase F

0 sub

1

15. P

he am

monia-

lyase

24. E

ukar.

trans

lation

IF 5A

39. H

sp20

/a-cry

stallin

family

prote

in

48. e

xpres

sed p

rotein

*/-/*

*/

-/-

*/*/

-

Normalised signal #

#

C

Page 192: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

18

0

Fig

ure

6. R

elat

ive

prot

ein

abun

danc

e in

ric

e co

leop

tiles

sub

ject

ed to

air

(dar

k bl

ue),

anox

ia (g

reen

) and

re-

oxyg

enat

ion

(ligh

t blu

e).

Full

figur

e ca

ptio

n on

nex

t pag

es.

0 2 4 6 8 10

12

14

16

18

19. M

ito pr

oces

sing p

eptid

ase

22. p

yruva

te kin

ase

8. Stro

mal Asc

orbate

Pero

xidas

e

23. P

DC isoz

yme 2

45. P

DC isoz

yme 2

20. G

3PDH

24. th

iamine

PPi e

nzym

e

25. th

iamine

PPi e

nzym

e

26. th

iamine

PPi e

nzym

e

27. th

iamine

PPi e

nzym

e

40. P

PDK, chlo

roplas

t prec

ursor

41. P

PDK, chlo

roplas

t prec

ursor

42. P

PDK, chlo

roplas

t prec

ursor

43. P

PDK, chlo

roplas

t prec

ursor

44. P

PDK, chlo

roplas

t prec

ursor

Normalised signal

*/*/

-

*/-/-

*/-/*

A

Page 193: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

18

1

Fig

ure

6. R

elat

ive

prot

ein

abun

danc

e in

ric

e co

leop

tiles

sub

ject

ed to

air

(dar

k bl

ue),

anox

ia (g

reen

) and

re-

oxyg

enat

ion

(ligh

t blu

e).

Full

figur

e ca

ptio

n on

nex

t pag

es.0 1 2 3 4 5 6 7 8 9

47. C

ys-ric

h rep

eat s

ecret

ory pr

otein

51. C

ys-ric

h rep

eat s

ecret

ory pr

otein

52. C

ys-ric

h rep

eat s

ecret

ory pr

otein

53. C

ys-ric

h rec

eptor

-like p

rotein

kina

se

54. C

ys-ric

h rec

eptor

-like p

rotein

kina

se

55. g

lycos

yl hy

drolas

es fa

mily 17

56. e

xpan

sin pr

ecurs

or

61. C

ys-ric

h rec

eptor

-like p

rotein

kina

se

58. ri

bulos

e BisP

carbo

xylas

e small

chain

60. C

ys-ric

h rec

eptor

-like p

rotein

kina

se

62. P

DI

12

Normalised signal

-/-/*

-/*/-

-/*/*

B

Page 194: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

18

2

Fig

ure

6. R

elat

ive

prot

ein

abun

danc

e in

ric

e co

leop

tiles

sub

ject

ed to

air

(dar

k bl

ue),

anox

ia (g

reen

) and

re-

oxyg

enat

ion

(ligh

t blu

e).

Full

figur

e ca

ptio

n on

nex

t pag

e.

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4

5. GDSL-l

ike lip

ase/a

cylhy

drolas

e

18. p

eroxid

ase p

recurs

or

30. v

esicl

e-fus

ing ATPas

e

36. 4

0S rib

osom

al pro

tein S

5

10. A

TP synth

ase F

0 sub

unit 1

13. C

ys-ric

h rep

eat s

ecret

ory pr

otein

55

16. tu

bulin

/FtsZ do

main co

ntaini

ng pr

otein

33. tu

bulin

/FtsZ do

main co

ntaini

ng pr

otein

34. tu

bulin

/FtsZ do

main co

ntaini

ng pr

otein

35. A

TP synth

ase F

0 sub

unit 1

6. elo

ngati

on fa

ctor

7. ac

tin

11. ri

boso

mal pro

tein L

6

37. P

he am

monia-

lyase

38. P

he am

monia-

lyase

39. P

he am

monia-

lyase

57. ri

bulos

e BisP

carbo

xylas

e larg

e cha

in

Normalised signal

*/-/*

*/

-/-

*/*/

-

# #

# #

# #

C

Page 195: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

18

3

Fig

ure

6. R

elat

ive

prot

ein

abun

danc

e in

ric

e co

leop

tiles

sub

ject

ed t

o ai

r (d

ark

blue

), an

oxia

(gr

een)

and

re-

oxyg

enat

ion

(ligh

t bl

ue).

Aer

ated

pro

tein

abu

ndan

ces

wer

e no

rmal

ised

to

1 an

d co

mpa

red

to a

noxi

c an

d po

st-a

noxi

c sa

mpl

es.

The

num

bers

tha

t pr

eced

e pr

otei

n id

entit

ies

indi

cate

the

spo

t nu

mbe

rs s

how

n in

Fig

ure

4A.

Pro

tein

s w

ere

split

into

thr

ee c

ateg

orie

s de

pend

ing

on t

he r

espo

nse

durin

g an

oxia

. A. P

rote

ins

that

sig

nific

antly

incr

ease

d fro

m a

ir to

ano

xia;

B. P

rote

ins

that

did

not

sig

nific

antly

cha

nge

in a

bund

ance

from

ai

r to

ano

xia;

C.

Pro

tein

s th

at s

igni

fican

tly d

ecre

ased

und

er a

noxi

a. A

bove

eac

h pr

otei

n is

a s

igni

fican

ce i

ndic

ator

; th

e fir

st p

ositi

on

indi

cate

s th

e p-

val a

ssoc

iate

d w

ith th

e ch

ange

from

air

to a

noxi

a, th

e se

cond

pos

ition

rel

ates

to th

e an

oxia

and

pos

t-an

oxia

com

paris

on,

and

the

third

pos

ition

rel

ates

to

the

post

-ano

xia

and

air

com

paris

on.

* in

dica

tes

the

diffe

renc

e is

sig

nific

ant

(p-v

al<

0.05

); -

indi

cate

s th

e di

ffere

nce

is

not

sign

ifica

nt;

# in

dica

tes

this

is

pr

obab

ly

a pr

otei

n de

grad

atio

n pr

oduc

t. Fi

gure

s on

pr

evio

us

page

s.

Page 196: Characterising the response of rice and wheat coleoptiles ... · Characterising the response of rice and wheat coleoptiles to anoxia and re-oxygenation Rachel Shingaki-Wells This

184

Figure 7. Catalase (A) and peroxidase (B) activity in rice and wheat coleoptiles. Seedlings were germinated and grown under aeration for 4 days and subsequently transferred to anoxia and re-oxygenation for 1 day. Alternatively, rice seedlings were germinated and grown under anoxia for 6 days. Figure 7B on following page.

0

5

10

15

20

25

30

35

40

45

50

Air Anoxia Post-anoxia Air Anoxia Post-anoxia Continuous anoxia

Wheat Rice

Cat

alas

e ac

tivity

(mM

H2 O

2.min

-1.m

g-1 p

rote

in)

p=0.01 p=0.0009

p=0.02

(1 d) (1 d) (6 d)

A

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Figure 7. Catalase (A) and peroxidase (B) activity in rice and wheat coleoptiles. Seedlings were germinated and grown under aeration for 4 days and subsequently transferred to anoxia and re-oxygenation for 1 day. Alternatively, rice seedlings were germinated and grown under anoxia for 6 days. Figure 7B on following page. Figure 7A on previous page.

0

50

100

150

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Air Anoxia Post-anoxia Air Anoxia Post-anoxia Continuous anoxia

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Supplemental Figures

Supplemental Figure 1 (SF 1). Metabolite response ratios in rice coleoptiles

when comparing anoxia to air (A) and post-anoxia to air (B).

Supplemental Figure 2 (SF 2). Metabolite response ratios in wheat coleoptiles

when compared anoxia to air (A) and post-anoxia to air (B).

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Chapter 5 General Discussion

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General Discussion The overall aim of this thesis was to understand and identify key responses of

rice (cv. Amaroo) and wheat (cv. Calingiri) seedlings to anoxia as well as re-

oxygenation. In Study I, four-day-old aerated rice and wheat seedlings were

treated with anoxia for one day (Shingaki-Wells et al., 2011). Initial

experiments set out to confirm a physiological effect of anoxia on these

seedlings. Rice coleoptiles showed significant growth during anoxia, whereas

those of wheat did not. Both species showed significant decreases in

coleoptile sugar content, as well as significant increases in ADH activity after

one day of anoxia. Curiously, wheat coleoptiles did not show a significant loss

of respiratory capacity after one day of anoxia, despite evidence to the

contrary, where damage to wheat coleoptile mitochondria was shown after

only 1.5 hours of anoxia (Vartapetian et al., 1985). However, mitochondrial

ultrastructure was promptly repaired during re-aeration, but not if anoxia

lasted 36 hours (Vartapetian et al., 1985).

Since a physiological response to anoxia was observed in both species,

proteomics analysis was carried out to further explore the molecular

adaptations of these seedlings. Immediately evident was the comparatively

subtle response of wheat coleoptiles to anoxia. Whereas 4.6 % of the

detected proteins increased after one day of anoxia in rice, only 0.08 % did so

in wheat. Rice coleoptiles from seedlings germinated and grown under

continuous anoxia for six days had even larger differences to those of aerated

controls, with 8.5 % of the detected proteins being significantly higher in

abundance under anoxia, and 4.5 % being significantly lower, meaning 13 %

of the protein spots detected were affected by oxygen availability. Proteins

involved in glycolysis, fermentation, amino acid metabolism, oxidative stress

and translation were differentially regulated in anoxic rice, changes which were

mostly corroborated by other proteomic and transcriptomic studies (Lasanthi-

Kudahettige et al., 2007; Narsai et al., 2009; Sadiq et al., 2011). In remarkable

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similarity, Sadiq and colleagues (2011) found that 14 % of both transcripts

and proteins were significantly different in abundance between aerated and

continuously anoxic seedlings.

Metabolite analysis largely supported the idea that rice responses to anoxia

are strong, and those of wheat are weak. While many amino acids

accumulated during anoxia in rice, which was later confirmed by Study III,

comparatively few did so in wheat. The accumulation of free amino acids in

anoxic rice has been documented before, using three-day-old aerated

seedlings transferred to anoxia for up to 48 hours (Kato-Noguchi and Ohashi,

2006). It is interesting that amino acids continue to accumulate past the point

of our measurements, 24 hours, suggesting this response might not be

transient. Alanine and GABA made up 19 and 23 % of the amino acid pool,

respectively, in anoxic rice coleoptiles (Kato-Noguchi and Ohashi, 2006). While

anoxic alanine accumulation is considered a classical anaerobic response

(Narsai et al., 2011), the analyses of Study I showed no significant

accumulation of alanine in anoxic wheat coleoptiles. This contrasts to an

earlier study, which showed wheat shoots accumulating alanine faster than

rice at initial time points, and equally at later time points (8 h) (Menegus et al.,

1989).

While the benefits of anaerobic alanine accumulation are unknown, several

hypotheses have surfaced. As discussed more thoroughly in Chapter 1,

potential benefits include hypoxic pyruvate consumption to prevent anoxia

(Zabalza et al., 2009), carbon skeleton retention for post-anoxia (Miyashita et

al., 2007) or prevention of excessive cytoplasmic acidification through

diverting carbon skeletons away from lactic acid production (Reggiani et al.,

1988). None of these hypotheses, however, are able to explain why alanine

supplementation of anoxic wheat seedlings, but not rice seedlings, reduces

cell leakage (Study I) (Shingaki-Wells et al., 2011). It is important to point out,

however, that a combination of serine, glycine and alanine also had this effect,

but not serine or glycine alone (Shingaki-Wells et al., 2011). It is possible that

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the benefit of this supplementation is related to osmotic pressure, but it is also

possible that the inter-conversion of amino acids provides some benefit in

anoxic wheat.

Intrigued by these results, four more wheat genotypes were selected for

further analysis (Study II) and compared to our primary genotype of interest,

Calingiri. These four genotypes, SARC1, Ducula4, Carnamah and Spear, were

selected on the basis that the anoxia tolerance of their roots was highly

variable (Goggin and Colmer, 2007). For a more direct comparison to this

research, two variables were modified. This included the addition of a 15˚ C

temperature treatment to our original 28˚ C treatment used for Study I and III,

and analysis of roots as well as coleoptiles. An absent alanine response in 28˚

C anoxic coleoptiles of Calingiri seedlings confirmed the results of Study I.

However, it appeared that an anaerobic alanine response in Calingiri was

tissue dependent, with 28˚ C Calingiri roots showing significant accumulation

under anoxia. Additionally, all genotypes accumulated alanine in 15˚ C tissues

(coleoptiles and roots), indicating that temperature has a strong effect on

anoxic alanine accumulation, a finding that was confirmed by ANOVA

interaction analyses.

The focus on alanine was an attempt to identify whether its accumulation

could be used as a marker for anoxia tolerance, but this study, which

suggests Calingiri coleoptiles are among the top performers, challenges this

hypothesis. This analysis was further complicated by the difficulty in finding a

gold standard measure of anoxia tolerance. For example, there are several

ways to measure what could be considered the simplest of variables, growth,

which can lead to different conclusions. The vast differences identified in the

metabolomics analysis suggests that anoxia tolerance is likely to be sensitively

dependent on even subtle environmental or experimental differences, as

exemplified by the inconsistencies of the Ducula-4 literature (Setter et al.,

2009). Study II, therefore, contributes the finding that anoxia tolerance is

temperature and tissue dependent, and complicated by the fact that plants

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may achieve tolerance by different means. Employing other measurements of

cell integrity as alternatives to the electrolyte leakage assay could be useful in

clarifying the damage caused by anoxia in different wheat genotypes. This

includes cell stains such as propidium iodide (Rolny et al., 2011).

In Study III, our interest shifted to the consequences of re-oxygenation on the

coleoptiles of rice and wheat (Calingiri) seedlings, at 28˚ C. In relaxing our

significance thresholds for the proteomics analysis, we were able to detect

several wheat proteins that changed during anoxia, as well as re-oxygenation.

Proteins changing in anoxic wheat were involved in translation and pyruvate

metabolism. Confirming our results in Study I, these changes were mostly

below 2-fold, suggesting a relatively restrained response to anoxia. Re-

oxygenation resulted in changes common to both species, including a

decrease in phenylalanine ammonia lyase under anoxia, which was reversed

upon re-oxygenation. This protein is suspected to be involved in cell wall re-

modelling (Rumeau et al., 1990). In addition, post-anoxic changes in other

proteins involved in cell structure re-modelling were seen in rice and wheat.

This aligns with the findings reported in the first study to document proteomic

changes to re-oxygenation in plants (Salavati et al., 2012). Since low oxygen

events reduce the efficiency of ATP production (Gibbs and Greenway, 2003),

it follows that growth, which may lose preference to other critical processes,

would be aberrant under different oxygen concentrations.

Re-oxygenation caused large changes to the metabolome of rice, but less so

in wheat. The rapid accumulation of amino acids in anoxic rice, which was

also observed in Study I, was reversed during post-anoxia (Study III). The

hypothesis that alanine accumulation might be beneficial for post-anoxic

metabolism (Miyashita et al., 2007) may therefore also apply to other amino

acids. It is suspected that the inability of wheat to mobilise starch under

anoxic conditions (Guglielminetti et al., 1995) contributes to a lower glycolytic

flux (Waters et al., 1991), and thus a reduced capacity to accumulate amino

acids (Study I and III). This could negatively affect post-anoxic recovery in

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wheat, since the amylotic enzymes required for starch mobilisation would not

be immediately available during re-oxygenation, nor the amino acids whose

inter-conversion to pyruvate could allow prompt resumption of aerobic

respiration. As seen in Study II, anoxic amino acid accumulation is relatively

strong and sucrose levels relatively stable in 15˚ C coleoptiles, suggesting a

strong dependence of anoxic metabolism on temperature.

Future work

While general trends have been identified, the complex experimental design

outlined in Study II requires the development of a computational method to

systematically compare physiological measurements with metabolomics

analyses. Incorporating rice data into this analysis has the potential to identify

metabolic biomarkers of tolerance. This analysis will be carried out in the near

future. Proteomics analysis in re-oxygenated seedlings would be well

complemented by translatome or shotgun proteomics analysis to overcome

the shortfalls of gel analysis. Incorporating more treatment regimes, including

anoxically-germinated rice seedlings transferred to air for the first time, could

be useful in isolating post-anoxic shock responses. Such analysis could also

be useful in imitating the conditions often faced by lowland rice, which often

germinate under anaerobic conditions. While this has been done using anoxic

rice coleoptile mitochondrial samples (Millar et al., 2004), this analysis has not

been performed at the whole-cell level. Integration of this data with that of the

anoxia literature would provide a solid basis for identifying key responses to

low oxygen and re-aeration, two stresses that are often intertwined. Follow up

of these changes, through the development of genetic mutants would be

useful in understanding the role these genes play in low oxygen survival. For

example, targeting a set of enzymes involved in cell structure re-modelling

could clarify the importance of their role during re-oxygenation. Alternatively,

disrupting several reactions of amino acid metabolism in tolerant and

intolerant crop species could clarify any speculations made on the functional

importance of these pathways.

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References Gibbs J, Greenway H (2003) Mechanisms of anoxia tolerance in plants. I.

Growth, survival and anaerobic catabolism. Functional Plant Biology 30: 1–47

Goggin DE, Colmer TD (2007) Wheat genotypes show contrasting abilities to recover from anoxia in spite of similar anoxic carbohydrate metabolism. Journal of Plant Physiology 164: 1605-1611

Guglielminetti L, Yamauchi M, Perata P, Alpi A (1995) Amylotic activities in cereal seeds under aerobic and anaerobic conditions. Plant Physiology 109: 1069-1076

Kato-Noguchi H, Ohashi C (2006) Effects of anoxia on amino acid levels in rice coleoptiles. Plant Production Science 9: 383-387

Lasanthi-Kudahettige R, Magneschi L, Loreti E, Gonzali S, Licausi F, Novi G, Beretta O, Vitulli F, Alpi A, Perata P (2007) Transcript profiling of the anoxic rice coleoptile. Plant Physiology 144: 218-231

Menegus F, Cattaruzza L, Chersi A, Fronza G (1989) Differences in the anaerobic lactate-succinate production and in the changes of cell sap pH for plants with high and low resistance to anoxia. Plant Physiology 90: 29-32

Millar AH, Trend AE, Heazlewood JL (2004) Changes in the mitochondrial proteome during the anoxia to air transition in rice focus around cytochrome-containing respiratory complexes. The Journal of Biological Chemistry 279: 39471-39478

Miyashita Y, Dolferus R, Ismond KP, Good AG (2007) Alanine aminotransferase catalyses the breakdown of alanine after hypoxia in Arabidopsis thaliana. The Plant Journal 49: 1108-1121

Narsai R, Howell KA, Carroll A, Ivanova A, Millar AH, Whelan J (2009) Defining core metabolic and transcriptomic responses to oxygen availability in rice embryos and young seedlings. Plant Physiology 151: 306-322

Narsai R, Rocha M, Geigenberger P, Whelan J, Van Dongen JT (2011) Comparative analysis between plant species of transcriptional and metabolic responses to hypoxia. New Phytologist 190: 472-487

Reggiani R, Cantu CA, Brambilla I, Bertani A (1988) Accumulation and interconversion of amino acids in rice roots under anoxia. Plant and Cell Physiology 29: 981-987

Rolny N, Costa L, Carrion C, Guiamet JJ (2011) Is the electrolyte leakage assay an unequivocal test of membrane deterioration during leaf senescence? Plant Physiology and Biochemistry 49: 1220-1227

Rumeau D, Maher EA, Kelman A, Showalter AM (1990) Extensin and phenylalanine ammonia-lyase gene expression altered in potato tubers in response to wounding, hypoxia, and Erwinia carotovora infection. Plant Physiology 93: 1134-1139

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Sadiq I, Fanucchi F, Paparelli E, Alpi A, Bachi A, A. A, Perata P (2011) Proteomic identification of differentially expressed proteins in the anoxic rice coleoptile. Journal of Plant Physiology 168: 2234-2243

Salavati A, Khatoon A, Nanjo Y, Komatsu S (2012) Analysis of proteomic changes in roots of soybean seedlings during recovery after flooding. J Proteomics 75: 878-893

Setter TL, Waters I, Sharma SK, Singh KN, Kulshreshtha N, Yaduvanshi NPS, Ram PC, Singh BN, Rane J, McDonald G, Khabaz-Saberi H, Biddulph TB, Wilson R, Barclay I, McLean R, Cakir M (2009) Review of wheat improvement for waterlogging tolerance in Australia and India: the importance of anaerobiosis and element toxicities associated with different soils. Annals of Botany 103: 221-235

Shingaki-Wells RN, Huang S, Taylor NL, Carroll AJ, Zhou W, Millar AH (2011) Differential molecular responses of rice and wheat coleoptiles to anoxia reveal novel metabolic adaptations in amino acid metabolism for tissue tolerance. Plant Physiology 156: 1706-1724

Vartapetian BB, Zakhmylova NA, Generozova IP (1985) Ultrastructure of wheat coleoptile mitochondria at short-term anoxia and post-anoxia. Plant Cell and Environment 8: 65-67

Waters I, Morrels S, Greenway H, Colmer T (1991) Effects of anoxia on wheat seedlings. II. Influence of O2 supply prior to anoxia on tolerance to anoxia, alcoholic fermentation, and sugar levels. Journal of Experimental Botany 42: 1437-1447.

Zabalza A, Van Dongen JT, Froehlich A, Oliver SN, Faix B, Gupta KJ, Schmalzlin E, Igal M, Orcaray L, Royuela M, Geigenberger P (2009) Regulation of respiration and fermentation to control the plant internal oxygen concentration. Plant Physiology 149: 1087-1098

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Co-author consent This thesis contains publications/manuscripts as outlined on page III. The

consent of each co-author is provided on the following pages.

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I, Adam Carroll , approve the u se of the following publication, of which I am

a co -author, to be included in the thesis of Rachel Shingaki -Wells for the

degree of Doctor of Philosophy at The University of Western Australia.

1. Shingaki -Wells RN , H uang S, Taylor NL, Carro ll AJ, Zhou W, Millar AH. (2011) Differential molecular responses of rice and wheat coleoptiles to anoxia reveal novel metabolic adaptations in amino acid metabolism for tissue tolerance. Plant Physiology 156(4):1706 -24.

Signed __ _______________

Date ___________________________ 06/01/2014

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I, Wenxu Zhou, approve the use of the following publication, of which I am a

co-author, to be included in the thesis of Rachel Shingaki-Wells for the

degree of Doctor of Philosophy at The University of Western Australia.

1. Shingaki-Wells RN,, Huang S, Taylor NL, Carroll AJ, Zhou W, Millar AH. (2011) Differential molecular responses of rice and wheat coleoptiles to anoxia reveal novel metabolic adaptations in amino acid metabolism for tissue tolerance. Plant Physiology 156(4):1706-24.

Signed ________________________

Date ___________________________

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