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Agricultural Sciences in China

2007,

6(12):

1487-1493

Study on Aroma Components in Fruit From Three Different Satsuma Mandarin

Varieties

QIAO

Yu,

XIE

Bi-jun,

ZHA NG Yan, ZHOU Hai-yan and PAN Si-yi

Col lege of Food Science

and

Technology, Huazhong Agricultural Universi ty , Wuhan 430070 P.R.China

Abstract

Fruit aroma of Guoqing 1, Miyagawa Wase, and Owari from three different Satsuma mandarin varieties were investigated

by headspace solid phase microextraction (HS -SPM E) combined with GC-MS . The results showed that there were 73, 71,

and 66 aroma com ponents in the three varieties, and the total contents we re 584.67, 505.29, and 494.63 yg g-1, respectively.

Total 29 constituents were comm on in the three varieties. It was also found that Guoqing

1,

Miyagawa Wase, and Owari

had 12,

5,

and 2 unique components, respectively. The key aroma compon ents were limonene, linalool, y-terpinene, p

myrcene, a-p inen e, and octanal in the three fruits. Guoqing 1 contained more key aroma compounds than Miyagawa

Wase and Owari.

Key words: Satsuma mandarins, fruit, volatile com pounds, aroma

INTRODUCTION

Aroma is one of the mo st important quality attributes

of citrus fruit and the most significant parameter of

quality in both eatable and proce ssed products.

In

or-

der to improve the fruit quality and modify the arom a

formation, information on the flavor constitution present

in fruit is needed and important for cultivar breeding

and further processing. Researche s

on

citrus aroma

have been performed for many years in western

countries. Aroma of grapefruit juice and sweet orange

juice which were the major processing cultivars has

been extensively investigated and reviewed (N6nez

et

al.

1985; Nisperos-Carried0 and Shaw 1990; Shaw

and Moshon as 1997; Jia

et

al. 1998; Tgnder

et

al. 1998;

Bazemore et

al.

1999; Jordan et

al.

2001, 2003; Lin

et

al. 2002; Rega

et

al. 2003; Moufida and Marzouk

2003; Selli

et al.

2004; A llegrone et

al.

2006; Arena

et

al.

2006). Many studies

on

aroma of juice and es-

sential oil have been cond ucted on Satsuma mandarins

(Yajima et

al.

1979; Ohta et

al.

1982; Moshonas and

Shaw 1997; Minh

et

al. 2002; PCrez

et

al. 2005; PCrez-

L6pez and Carbonell-Barrachina 2006), but few data

exist on the fruit aroma. Elmaci and Altug (2005) de-

tected 26 volatile compou nds in the three mand arin cul-

tivars from Turkey using dy namic headspace and found

the key aroma impact compounds w ere limonene, y-

terpinene, p-cymene, m yrcene, a-pinen e, P-pinene, and

a-terpinolene in all sam ples by sensory evaluation.

In China , Sa t sum a mandar ins , o r ig ina t ing i n

Huangyan and Wenzhou of Zhejiang P rovince, are dis-

tributed widely and have the highest yield. Man darins

are primarily consum ed as fresh fruit and processed

into tin cans in industry. Although Satsuma mandarins

possess the imp ortant economic values with respect to

the citrus industry in China, only volatile compounds

of essential oil from Satsuma mandarins were previ-

This paper is translated from its Chinese version in Scientia Agricultura Sinica.

QIAO Yu.Ph D candidate, E-mail: [email protected];Correspondence PAN Si-yi, Professor, Tel: +86-27-87283778, E-mail: pansiyiOmail.hzau.edu.cn

02007 CAAS.

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Published

by

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2/7

1488

QIAO Yu et

al.

ously reported (Huang and Wu 1998; Shan and Li 200 6;

Zhang

et

al. 2007; Zhou

et al.

2007). Relatively little

information is available

on

the flavor of Chinese Sat-

suma m andarins (Zhou

et

al. 2007), especially the na-

tive cultivar grown in China.

In the present study, aroma of Guoqing

1,

Miyagawa

Wase, and Owa ri, the three different Satsuma manda-

rin varieties from the Songzi region of Ch ina, were in-

vestigated by headspace solid phase microextraction

(HS-SPME) combined with GC-MS. By determining

the volatile componen ts from the three fruits, we can

have a better perspective on the characteristic aroma

compounds in different cultivars and get some infor-

mation on cultivar breeding and juice processing.

MATERIALS AND METHODS

Materials

The samples of Guoqing

1 Citrus unshiu

Marc. cv .

Guo qing 1). Miyag awa Wase Citrus unshiu Marc. cv

Miyagawa Wase), and O wari

Citrus unshiu

Marc. cv.

Ow ari) fruits from citrus garden , located in the S ongzi

region of Hubei Province, China, were collected on Oc-

tober 11, October 31, and November 9 in 2006,

respectively. The total soluble solids of Guoqing 1 ,

Miyagawa Wase, and Owari were 9, 11, and 12.5

and total so luble solids/total acidity ratioes (TSS/TA)

were 1 3.24, 14.67, and 12.25, respectively. Analysis

of volatile compounds was carried out after 24 h in the

wake of postharvest.

Methods

Determination of the volatile compounds

of

Sat-

suma m andarins

4

kg

fruit of each cultivar were

peeled and reamed in a centrifuge uice extraction. The

3 g pulp with 3.6

g

NaC1, prev iously add ed to 1 p L of

IS solution (cyclohexanoe), was placed into a 20-mL

vial containing a m icrostirring bar. The SPME manual

device equipped with a 5 0/30

pm

DVB/CAR/PDMS fi-

ber (Supelco, Bellfonte, PA, USA) was u sed for ex-

traction of orange juice. The fiber was conditioned in

GC injector port at 270C for 1 h prior to use. The

sample was equilibrated at 40C for 1 5 min and e x-

tracted by D VB/CAR /PDMS fiber for 40 min at the

same tempe rature under stirring. After extraction, the

fiber was inserted into the injection port of G C to des-

orb the ana lytes for 5 m in.

GC-MS analysis GC-MS was carried out using a HP

5975C quadropole mass selective detector at 150C

(Agilent Technologies, USA). Mass spectral ionization

was set at 230C. The mass spectrometer was oper-

ated in the electron ionization mode at a voltage of 70

eV. The flow rate of helium on HP-5 column (30 m x

0.25

mm

i . dx 0.25 pm film thickness, J&W S cientific,

Folsom, CA, USA) is

1

mL min-'. Analysis was per-

formed in the splitless mode and injector temp erature

was 250C. The column was held at 35C for 5 min,

then increased from

35

to 180C at 3C min-I, held at

180C for 1 min, and finally increased to 240C at a

rate of 5C m i d , held for

5

min.

Volatile compone nts were tentatively iden tified by

comp aring their mass sp ectra with the m ass spectra of

l i b ra r i e s (NISTOS, WILEY7.0) and r e f e rences

(Moshonas and Shaw 1997; Jordan et al. 2001,2003;

Lin

et

al. 2002). Semiquantification

of

compounds iden-

tified in this study was calculated by com paring the

peak area of each compound with that of the internal

standard.

RESULTS

Total ionic chromatograms of volatile compounds in

the three different Satsuma mandarin fruits are shown

in Fig. and Table 1, indicating the quality and qua ntity

results of components.

The aroma compounds

of

the three different

Satsuma mandarins

The identified volatile compounds and their relative

amounts are given in Tables 1 and 2. Differences in the

composition of volatile molecules from Guoqing 1,

Miyagawa Wase, and Ow ari were observed.

A total of 65 com ponents were identified in Guoqing 1

fruit and their total concentration was 584.67 pg g- . The

highest amounts of volatile compound s were limonen e,

linalool, y-terpinene, P-myrcene, octanal, decanal,

terpinen-4-01, and (E)-Zhexen-l-ol.

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Study on Aroma Components in Fruit From Three Different Satsuma Mandarin Varieties

1489

Table 1 Volatile comp ounds from thre e different Satsuma mandarin varieties

Compounds

Content pg g-1)

Guoaine

1

Mivaeawa Wase Owari

Hydrocarbons

a-Thujene

a-Pinene

Camphene

Sahinene

P-Pinene

P-Myrcene

3-Carene

a-Terpinene

D-Limonene

Z)-b-Ocimene

y-Terpinene

Terpinolene

l-Methyl-4- 1 methylethenyl)-henzne

GElemene

a-Cuhehene

Copaene

P-Cubebene

P-Elemene

Junipene

P-Caryophyllene

p-Gurjunene

a-Caryophyllene

Isoledene

y-Muurolene

Cermacrene

D

P-Humulene

Valencene

a-Selinene

a-Amorphene

GAmorphene

A

coho

s

Ethyl alcohol

Z)-Z-Hexen-1 01

E)-Z-Hexen-1 01

I-Octanol

Linalool

trans-p-Mentha-2.8-diene-

1-01

Isopulegol

P-Terpinol

Borneo1

0.17

0.90

0.02

0 50

0.84

8.95

462.89

I

.93

21.12

1.28

0.3

0.07

0.16

0.26

0.09

0.39

0.03

0.23

0.04

0.12

0.04

0.05

0.24

0.06

0.70

0.13

0.05

0.25

0.71

2.13

1.34

50.54

1.20

0.33

0 05

0.34

.oo

0.59

1.29

8.41

0.46

0.55

422.31

1.71

19.10

1.56

0.23

0.3

0.1

1.13

0.17

.42

26.45

0.46

0.28

0.14

0.79

0.02

0.36

0.74

7.76

400.60

1.60

17.30

1.02

0 05

0.04

0.10

0.17

0.06

0.19

0.14

0.06

0.03

0.20

0.21

1.15

0.26

5.39

0.95

36.36

0.44

0.28

0.08

-.not found

or

not exist.

There were

36

components found in Miyagawa

Wase fruit and the concentration of the total volatiles

was 505.29 pg

g-I.

The most abundant compounds

were limonene, Iinalool, y-terpinene, P-myrcene, octan al,

terpinen-4-01, (Z)- p-ocimene, terpino lene, and deca nal.

Fifty-five compounds were determined in O wari fruit

and the total concentration was 494.63

pg

g-*. The

major vo latile comp ounds were limonen e, linalool, y-

terpinen e, P-m yrcene, oc tanal, (E)-2-he xen- 1-01,

terpinen-4-01, and decanal.

Guoqing

1

had the most kinds and greatest amo unts

of

aroma compounds in all samples. Total 29

common

constituents were found in the three varieties. Guoqing

1 had 12 unique compoun ds, which were P-gurjunene,

isoledene, germacrene

D,

P-humulene, a-selinene,

a

amorphene, borneol,

1

nonan ol, nerol, undecanal, bu-

Content

(pg g- )

Compounds

Guoqing Miyagawa Wase Owari

I-Nonanol

4-Terpineol

a-Terpineol

cis-Carveol

Nerol

Citronellol

Geraniol

Thymol

Aldehydes

Hexanal

E)-Z-Hexenal

Heptanal

Octanal

Nonanal

Citronella1

Decanal

Neral

Z)-2-Decenal

E)-Z-Decenal

Geranial

Perillal

Undecanal

2-Undecenal

E,E)-Zd-Decadienal

Esters

Butyl hutanoate

Ethyl hexanoate

Ethyl octanoate

Linalyl acetate

Citronellyl acetate

Neryl acetate

Geranyl acetate

Isopropyl Myristate

Ketones

Camphor

Carvone

Z)-6, O-Dimethyl-5 9-undecadien-2-one

@)-6,1

-Dimethyl-5 9-undecadien-2-one

Acids

Acetic acid

0.21

2.49

2.95

0.40

0.37

0.47

0.27

0.18

1.19

0.43

0.14

8.81

0.21

3.07

0.84

0.12

0.64

0.34

0.11

0.25

0.42

0.1

0.29

0.20

0.66

0.32

0.17

0.73

0.02

0.13

I .84

1.15

1.02

0.14

7.93

0.98

1.49

0.52

0.34

0.23

0.16

0.54

0.24

0.72

0.27

0.65

2.06

1.98

0.24

0.25

0.15

0.06

0.68

0.10

0.16

7.05

0.08

I .76

0.48

0.07

0.39

0.25

0.42

0.08

0.21

0.12

0.41

0.2

I

0.16

0.59

0.12

0.07

tyl butanoate, and

(2)-6,1O-dimethyl-5 9-undecadien-

2-one. 3-Carene, a-terpine ne, nonanal, 2-undecenal,

and (E,E)-2,4-decadienal were foun d only in M iyagawa

Wase, while (Z)-2-hexen-

1-01

and P-terpinol were de-

tected only in O wari fruit.

Comparison of volatile constitution in the three

different Satsuma mandarin varieties

Hydrocarbons

Hydrocarbons, especially the monot-

erpene hydrocarb ons, are the highest am ount group in

citrus aroma. The most abund ant group of vo latile com-

pounds in the three selected Satsuma mandarin fruits

were hydrocarbons, and the monoterpene hydrocar-

bons presented in higher qu antities than sesq uiterpene

hydrocarbons.

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4/7

1490

Q I A O Yu

et

11.

A

3 800000

3 600

3 400000

3 200000

3 000

000

2800000

2600000

u

2400000

2200000

B

2000000

8

1800000

z

1600000

-

I400000

2

1200000

1000 000 i

B

Time (min)

I

0

50.00

55.00

60.00

Time (min)

C

Time (min)

Fig.

Total ionic chromatograms of vo latile compoun ds in the three different Satsuma m andarins fruits.

A,

Guoqing

1; B,

Miyagawa Wase;

c,

owari.

The most abundant compounds in the three man-

darin fruits were limone ne

(462.893, 422.313,

and

400.603

pg g- , respectively) followed by y-terpinene

and P-myrcene.

Valencene, which was detected

in

the highest amounts

in Miyagaw a Wase, was the sesquiterpene compo nent

found

in

greatest concentrations in all sam ples, repre-

senting about

0.04-0.22

f total contents.

Alcohols Alcoho ls have been described to be the most

important con tributors to citrus flavor, especially ter-

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5/7

Study

on Aroma Components

in

Fruit From Three Different Satsuma Mandarin Varieties

1491

Table 2

Compounds and contents

of

aroma components in the

three different Satsuma mandarin varieties

Compounds

Hydrocarbons

Content pg g-1)

Guoqing

1

Miyagawa Wase Owari

501.83 459.09 43 1.59

Monoterpenes 499.06 457.62 430.56

Sesquiterpenes 2.43 1.24 0.98

Others

0.34

0.23

0.05

Alcohols 63.64 31.77 49.63

Terpene alcohols 58.59 30.18 41.58

Others

0.66

0

0.3

I

Aliphatic aldehydes 13.87 12.8 9.82

Terpene aldehydes 2.03 0.57 1.19

Esters

2.26 0.4

I

1.46

Ketones 1.04

0 65

0.87

Acids 0 0 0.07

Total 584.67 505.29

494.63

Aliphatic alcohols

4.39 1.59 7.75

Aldehydes 15.90 13.37 11.01

pene alcohols hav e the characteristic aroma. The se

compou nds we r e f ound t o a ccoun t f o r 0 . 06 i n

Miyagaw a Wase, lower than in Gu oqing 1 and Owari.

The dom inant alcohol was linalool, with the highest

content in Guoqing 1 (50.54 pg g-I). Except for (E)-

2-hexen- 1-01, alcohol com ponents are fo und in higher

quantities in Guoqing 1 than other varieties. The key

aroma comp ounds of citrus such as cis-carveol, nerol,

c i t r o n e l l o l , a n d g e r a n i o l w e r e n o t d e t e c t e d i n

Miyagawa Wase.

Aldehydes Aldehydes are also the main aroma com -

pounds in citrus. Th e aliphatic aldehydes are found

in lower quantities than terpene aldehydes. Octana l

was found in considerable quantities (8.81, 7.93, and

7.05 pg g-I, respectively). Miyagaw a Wase contained

the lower quantitie s of terpene aldehydes, only rep-

resenting 0.11

.

The quantities of hexanal, decanal,

neral, and geranial in O wari were les s than those of

Guoqing 1. Moreover, several unsaturated aldehydes

wi th l ong ca r bona t e cha in s we r e f ound , such a s

undecanal in Guoqing 1and 2-undecenal in Miyagawa

Wase.

Esters

Esters presenting fruity note in trace am ounts

have been considered very impo rtant to citrus flavor.

The con tents of esters in the three variety fruits were

0.39, 0.08, and 0.30 , espectively. Ethyl hexanoate

and neryl acetate were detected in all samples. Ethyl

hexanoate was present about the same quanti ty in

Guoqing 1 and Ow ari and the lowest quanti t ies in

Miyagaw a Wase fruit. Neryl acetate was the most pre-

dominant among the ester compounds in all samples,

and it occurred in higher propo rtions in Miyagaw a Wase

fruit. Ethyl octanoate, linalyl acetate, citronellyl acetate,

and geranyl acetate were the four common esters found

in both Guoqing 1 and Owari, and they were detected

in higher quantity

in

Guoqing 1.

Ketones and acids

Ketones were believed to make a

positive contribution to the citrus flavor. The levels

of ketones in the three variety fruits were 0.18, 0.13,

and 0.18 , respectively. Carvone exhibited the high-

est concentration of ketones in all samples. Moreov er,

acetic acid was detected in Ow ari.

DISCUSSION

Arom a compound s will make different contributions to

the fruit because of their thresholds and the concentra-

tions in sample matrix. Th e contribution of chemical

compounds to food flavor is not judged by their con-

tent in sample. Only the compo und possessing intense

aroma value could be the key arom a to the fruit (Zhang

et

al.

2007). Elmaci and Altug 2005)detected 26 volatile

compounds in the three mandarin cultivars from Tur-

key using dynam ic headspace, and the key arom a im-

pact com pounds were limonene, y-terpinene, p-cymene,

myrcene, a-pinene, P-pinene, and a-terpinolene in all

samples by sensory evaluation.

Terpenic compounds

of

characteristic aroma in

Satsuma mandarin varieties

Limonene accounted for the major proportion in citrus

aroma. Tgnder

et al .

(1998) pointed ou t that the li-

monene presenting typical citrus aroma was the most

important compound in orange juice. Because of its

low threshold and high content, limonene was consid-

ered to be the key aroma compound in the three se-

lected Satsuma mandarin varieties.

Except for limonene, y-terpinene, P-myrcene, and

a-pine ne are the abundant monoterpenic com pounds

in Satsuma mandarin fruit. The odor thresholds of them

were low, and the three compo unds have a ci t rusy,

balsamic, and piney note (Ahmed et al. 1978; Tgnder

et

al.

1998; Plotto et

al.

2004). Elmaci and Altug 2005)

also found them to contribute to the mandarin fruit.

Therefore, y-terpinene, P-myrcene, and a- pin en e were

believed to be characteristic arom a compounds

of

se-

lected samples.

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1492

QI O Yu

et al.

Characteristic alcohol and aldehyde aroma

compounds

Alcohols and aldehydes are the major aroma compounds

in citrus fruit. Among the alcohols and aldelhydes pre-

sented in this paper, linalool and octanal ranked the high-

est in terms of quantity. Linalool with fruity aroma

w as th e k ey a ro m a co m p o n en t i n o ran g e ju i ce

(Nisperos-Carried0 and Shaw 1990). Linalool made a

positive contribution to orange flavor in combination as

per Ohta

et al .

(1982). Octanal is in general described

as the key aroma com ponent in orange juice because of

typical citrus odor (Nisperos-Carried0 and Shaw 1990).

The study performed by Tgnder et al . (1998) showed

that the thresholds of linalool and octanal were only

lower than those of limonene . Both of them could make

a positive contribution to Satsu ma mandarin flavor.

Other characteristic aroma compounds

Most of the esters exhibited fruity aroma, especially

some low boiled compounds, such as ethyl acetate and

ethyl butanoate. They have extreme ly low thresholds

but could not be detected in this study due to their high

volatility. Some ketones with lowe r quantities would

have effect

on

the aroma of Satsuma mandarin fruit.

The key aroma components were limonene, linalool,

y-terpinene, p-m yrcene, a-p ine ne , and octanal in the

three Satsuma mandarin fruits. The difference of con-

stitution in these compounds contributed to the varia-

tion of the overall aroma. By comparing the amounts

of these six key aroma compounds, we can see that

five compounds of them, except for a-p inen e, were

presented in the highest quantities in G uoqing 1, fol-

lowed by Miyagawa Wase and Owari . Therefore,

Guoqing 1 had relatively intense aroma, which is in ac-

cordance with the sensory evaluation. More over, the

total amounts and categories of arom a compounds in

Guoqing 1 were more than others. From these results,

it can be concluded that the aroma of Guoqing 1 was

the most prefered compared with Miyagawa Wase and

Owari.

Furthermore, the TSS/TA in M iyagawa W ase fruit

had higher quantities than other fruits, but the quantity

of aroma was lower than Guoqing 1 and Owari. The

correlation of taste and smell compounds will be still

studied further

CONCLUSION

Fruit aromas of different varieties were analyzed by

headspace solid phase microextraction combined with

GC-M S. The results showed that there were 73, 71,

and 66 aroma components in the three varieties, the

compounds and amounts of hydrocarbons, alcohols,

aldehydes, and esters were dominant in Guoqing 1. The

contents of alcohols, esters, and ketones were lowest

in Miyagawa Wase and the quantities of hydrocarb ons

and aldehydes were lowest in Owari. The key aroma

compone nts were limonene, linalool, y-terpinene,

p

myrcene, a-pinene , and octanal in the three fruits.

Guoqing

1

contained more amounts of key aroma com-

pounds than Miyagawa Wase and Owari.

Acknowledgements

The authors are grateful to the Wangchunhua Citrus

Valley

Co.,

Ltd., China, for supplying citrus fruits. This

work was suppo rted by the Project of Agriculture Struc -

ture Readjust of Ministry of Agriculture, China (04-09-

038) and the Major Key Technology R&D Program of

Hubei Province, China (2005AA201 C68).

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02007

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rights reserved.

Publishedby

Elsevier ltd.


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