technical report agrochemical residue field trials first 3 ... · coresta agrochemical analysis...

Agrochemical Residue Field Trials Sub-Group

Technical Report

Agrochemical Residue Field Trials

First 3-year Programme

September 2017

Sub-Group Co-ordinator and Author:

Keisuke Nakayama

Japan Tobacco Inc., Japan

https://www.coresta.org/groups/agrochemical-residue-field-trials

Table of Contents

1. Introduction ....................................................................................................................... 3

2. Achievements .................................................................................................................... 3

2.1 List of CPAs............................................................................................................. 3

2.2 Formal protocol ....................................................................................................... 4

2.3 Participants, tobacco types and CPAs included in the field trials

as of December 31, 2015 ......................................................................................... 4

2.4 Collation of results under formal protocol .............................................................. 6

2.5 Collection of already available residue trial data .................................................... 6

2.6 Additional achievements ......................................................................................... 6

3. Future Plans ...................................................................................................................... 7

4. Acknowledgements ........................................................................................................... 7

5. Appendix I ........................................................................................................................ 8

RFT-049-CTR First 3-Year Programme of Trials – September 2017 3/14

1. Introduction

Guidance Residue Levels (GRLs)1 have been developed by the CORESTA Agro-Chemical

Advisory Committee (ACAC) to provide guidance to tobacco growers and those in the

tobacco industry with interest in the application of Crop Protection Agents (CPAs) that are in

compliance with the implementation of Good Agricultural Practices (GAP). Residue data

from field trials complying with label instructions are an essential part of the process to

establish GRLs. To this end, ACAC proposed the creation of a new Task Force, the

Agrochemicals Field Trials Task Force (RFT TF)2, with the objectives listed below. Seven

meetings have been held since the establishment of this TF to the end of 2015. In this report,

the main achievements through to December 31st 2015 are described in the light of the

objectives.

Objectives:

1. In consultation with ACAC, to prepare and maintain a list of CPAs necessary to sustain

successful leaf production and for which GRLs have to be set or reviewed.

2. To produce a formal protocol for trial and testing procedures.

3. To promote participation in this programme globally.

4. To collate results of trials done under the formal protocol and make them available to

ACAC.

5. To collect already available field residue trial data from various sources and make them

available to ACAC.

Meetings:

Inaugural meeting, Vienna, Austria, June 30, 2012

2nd

meeting: Sapporo, Japan, September 22, 2012

3rd

meeting: Lexington, KY, USA, January 20, 2013

4th

meeting: Brufa di Torgiano, Italy, October 12, 2013

5th

meeting: Raleigh, NC, USA, January 11, 2014

6th

meeting: Quebec, Canada, October 11, 2014

7th

meeting: Izmir, Turkey, October 24, 2015

2. Achievements

2.1 List of CPAs

CPAs for the first series of trials were selected by the TF from a list of priorities determined

by ACAC (shown in Table 1).

1 CORESTA Guide No. 1 - Agrochemical Guidance Residue Levels (GRLs)

2 This TF was transformed to a Sub-Group (RFT SG) in 2016


Table 1. GRL candidates

The residue definition (target analytes) of each CPA was confirmed in collaboration with the

CORESTA Agrochemical Analysis Sub-Group (AA SG) and the testing laboratory JT R&D

completed method validation.

In addition to the CPAs listed in Table 1, field trials for selected additional CPAs, not yet

defined as candidates for GRLs, were conducted by some executors, as agreed by ACAC, the

RFT, and the testing laboratory. Among these are valifenalate, benthiavalicarb-isopropyl,

fluopicolide, sulfentrazone and mandipropamid.

2.2 Formal protocol

TF members and meeting participants started with the discussion on essential elements3 of

the study design at the inaugural meeting, and finalised a study protocol (version 4 as of

December 31, 20154) following discussions at subsequent RFT meetings.

2.3 Participants, tobacco types and CPAs included in the field trials as of

December 31, 2015

25 executors from 17 countries (Figure 1)

North & Central America: USA, Mexico, Cuba and Guatemala

South America: Argentina and Brazil

Asia: India, Philippines and Thailand

Africa: Malawi and Zimbabwe

Europe: Germany, Italy, Bulgaria, Greece, Macedonia and Turkey

3 Trial duration, the number of replicates, planting condition, application of CPA (rate, number of applications,

application intervals, pre-harvest interval), sampling, curing, sample shipment, etc.

4 This version was further updated to version 5.2 in October 2016 (see Appendix I)

# C P A # C P A # C P A

1 Azoxystrobin 9 Ethion 17 Spirotetramat

2 Difenoconazole 10 Triazophos 18 Bitertanol

3 Indoxacarb 11 Fenamidone 19 Iprobenfos

4 Propamocarb 12 Flubendiamide 20 Thiacloprid

5 Tebuconazole 13 Clothianidin 21 Chlorfenapyr

6 Chlorantraniliprole 14 Dicofol 22 Prothiofos

7 Triflumuron 15 Teflubenzuron 23 Quinalphos

8 Triadimefon /Triadimenol 16 Iprovalicarb


Figure 1. Trial Map and Executors

Tobacco types included (Table 2):

Flue-cured Virginia (FCV)

Burley (BLY)

Oriental (ORT)

Dark air-cured (DAC)

Dark fire-cured (DFC)

CPAs tested and the number of trials conducted (Table 2)

As of Dec. 2015, 83 % of Priority 1 CPAs, 38 % of Priority 2 CPAs and 0 % of

Priority 3 CPAs had been tested.

Table 2. CPAs tested and the number of trials conducted

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Ipro

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Benth

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-iso

pro

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Flu

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Sulfentr

azo

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Mandip

ropam

ide

Curing

type

Flue-

curedVirginia 9 7 4 12 7 4 8 6 8 4 3 6 10 5

Air-cured Burley 8 4 11 2 6 5 8 2 2 4 6 1

Dark 4 2 2 2

Fire-

curedDark 2 2 2

23 7 8 35 9 14 13 16 20 5 6 5 10 16 6

As of December, 2015

Sun Air-

cured

*: The number of trials were counted based on the completion of chemical analysis as of Dec 2015

Unclassified

Tobacco

type1 2 3 4 5 6 7 8-1

1st priority 2nd 3rd

198-2 9 10 11 12 13 14 15 16 17 18 26 27 28

Oriental 10

20 21 22 23 24 25

5

Total number of trials* 5

5 10

83% covered (10/12) 38% covered (3/8) 0% (0/3) 60% (3/5)


2.4 Collation of results under formal protocol

All the test results were compiled and submitted to ACAC with comments by the

RFT executive office.

Comments: The RFT Executive office investigated executor reports carefully to

determine if there were protocol/label violations, as these comments would be

useful for data selection by ACAC.

2.5 Collection of already available residue trial data

Some field residue trials were conducted outside of this CORESTA activity for

different purposes with different protocols. Some of the data were provided to

the RFT executive office, compiled, and submitted to ACAC.

These data providers were Bayer CropScience and ANITTA (Association

Nationale Interprofessionnelle et Technique du Tabac).

Some trials were conducted with CPAs for which GRLs have already been

established and/or GRL candidates, others were not. Data for CPAs with

established GRL could be used to verify these GRL values.

2.6 Additional achievements

The advantage of having CPA residue samples from the trials was taken for:

A residue degradation study was conducted for 12 CPAs to better

understand/interpret residue data. As a result, all CPAs tested were considered

stable within 12 months after grinding5,6

. Results will be provided to the

CORESTA Agrochemical Analysis Sub-Group (Table 3).

In addition to the degradation study, the rest of the samples were used for FAPAS

Proficiency tests arranged by CORESTA AA SG as agronomically incurred

samples (Project #097, 2016 Proficiency Test FAPAS FT0112). Nine CPAs were

targeted (Table 3).

5 Criteria of the stability; <30%

COMMUNICATION OF THE EUROPEAN COMMUNITIES Directorate General for Agriculture VI B II-1

(7032/VI/95 rev.5) 6 Ground samples were stored in plastic bags in the dark under 25 ºC until analysis.


Table 3. GRL candidates used for the Degradation Study and the FAPAS Proficiency Test

3. Future Plans

In collaboration with ACAC and AA SG:

Encourage current executors and new trial executors who can cover new GRL

candidates not tested so far.

Define appropriate residue definition (target analytes) and identify problematic CPAs

for determining residue definition.

Continue to use samples for FAPAS Proficiency test as “agronomically incurred

samples”.

Collect useful information on the trend of supervised field residue trials for setting

legislative MRLs (Maximum Residue Levels) for food/feed in order to reinforce the

current protocol, if needed.

4. Acknowledgements

Field trials were conducted by local executors on a voluntary basis, and samples were

analysed by JT R&D colleagues. We would like to express our gratitude to them for

supporting this project.

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1 2 3 4 5 6 7 8-1 8-2 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28

Degradation Study X X X X X X X X X X X X

FAPAS FT0112 X X X X X X X X X

1st priority 2nd 3rd

Study

Unclassified


5. Appendix I

PROTOCOL

Agrochemical Residue Field Trial (RFT)

(version 5.2, updated Oct., 2016)

Prepared by:

Naoto Yamaguchi and Keisuke Nakayama

Japan Tobacco Inc.

JT Bldg. 2-1, Toranomon 2-chome

Minato-ku, Tokyo, 105-8422, JAPAN

(RFT executive office)


1. Preface

CORESTA has recently established the Agrochemical Residue Field Trial Task Force (RFT

TF) within the Agronomy & Leaf Integrity Study Group. The main objective of the RFT TF

is to obtain residue data of agrochemicals identified by ACAC as candidates for GRL

establishment.

Residue data from supervised field trials are one of the key elements for setting GRLs. Very

little information is available for new agrochemical candidates (see Table 1) and for this

reason CORESTA has decided to implement the new task force. Residue data obtained from

this program will assist ACAC in defining GRL’s for some of the most important

agrochemicals used worldwide in tobacco production.

For more information on the objectives, please visit:

http://www.coresta.org/

Task Force members have been discussing study design, which is stipulated in the protocol.

This protocol defines the study design.

2. Study Design

2.1 Duration

3 years

2.2 Planting and growing conditions (see Figures 1-1 & 1-2)

Minimum 3 treated rows per active ingredient and 1 untreated row for the control per

trial.

Use a minimum of 2 guard rows at each side of the treated rows to provide sufficient

distance to prevent contamination (Figure 1-2).

For oriental tobacco, a greater number of guard rows and/or more spacing between

guard rows and untreated rows (at least 1.5-2.5 m) should be utilized to prevent

contamination.

Guard rows may be treated with active ingredients not under evaluation

All agrochemicals applied to treated rows and guard rows should be recorded in the

executor report.

Follow local recommendations for the application of agrochemicals not under

evaluation for GRL establishment.

Avoid cross contamination when agrochemicals are applied to adjacent fields,

specifically if applied agrochemicals are being evaluated in the RFT TF trial.

2.3 Plot size

Sufficient to provide a representative treated sample (A minimum of 40 plants should be

harvested from the middle row for residue sampling purposes: 2 kg lamina

sample/replicate, see Fig. 1)

Guard rows and untreated row(s), should contain the same number of plants as treated

rows (A minimum of 40 plants per 1 row).

http://www.coresta.org/


2.4 Agrochemicals to be tested

Only locally registered or authorized tobacco agrochemicals listed in Table 1, unless

legal exceptions are available locally

A photograph or copy of the original label and summary of the critical label information

should be sent to the executive office of the TF (Naoto Yamaguchi and Keisuke

Nakayama). Label summaries should be prepared in English.

2.5 Application

Only 1 evaluated agrochemical per treatment plot (at least 3 rows)

Agrochemicals required for crop management, but not evaluated for residues, may be

applied to the entire trial area

Adjust the conditions of application to obtain the expected highest residue per the

product label, taking into account the following7:

o Rate: highest labeled rate

o Number of applications: highest according to the label

o Application intervals: shortest according to the label but target harvest based on the

product’s labeled PHI

o Pre harvest interval (PHI):

Follow agrochemical label instruction

In the absence of PHI on the label, a PHI will be provided by the TF

Dosage (volume of spraying solution) when it applies:

o Follow agrochemical label instruction

o In the absence of dosage on the label, use appropriate volume (to be recorded in

executor report)

2.6 Harvesting

3-replicate samples to be taken from the middle of the treated rows (treated samples)

and 1-replicated sample to be taken from the untreated row (control sample) (see Fig. 1)

2 samples based upon stalk positions (one lower stalk sample, and one upper stalk

sample (see Fig. 2)

o Oriental tobacco: Upper sample (composite of 3+4; Ana+Uch alti harvest) and lower

sample (composite of 1+2; Ana, etc. harvests)

o FCV, BLY: upper sample (composite sample of leaf & tips = M/H + B+T) and lower

sample (composite sample of primings, lugs, & cutters = P+X+C)

Labeling at harvest (keep the control & treated samples separate during harvest and

curing)

Do not sample the guard rows

7 These parameters are optional in cases where these conditions are unrealistic. In the absence of tobacco

specific label information, the CPA has to be applied according to practical recommendations in

consideration of the points above. In this scenario, the TF executive office should be consulted prior to trial

initiation to ensure appropriate use of pattern.


Handling

o First and last plants of each treatment row/plot to be excluded (2-3 plants)

o Harvest and cure the treatment plot while maintaining identity

2.7 Curing

Follow local practices

Keep treated samples separate during curing to avoid cross contamination

If possible, place untreated tobacco between samples during curing

2.8 Sampling

Sample size

o For each replicate, collect a representative sample of at least 2 kg of cured whole

leaves for the respective stalk positions (i.e. [P+X+C] and [M/H+B+T])

o From the 2 kg of cured whole leaf, collect 0.5 kg of lamina for laboratory analysis

(whole leaf for Oriental only)

o Hand stripping – remove the stem/mid-rib

o Discard the stems/mid-ribs

o Retain the remainder of the whole leaves until the laboratory provides instructions

Remaining leaf will serve as a back-up sample in case of issues during sample

transportation and/or unsuccessful residue analysis

Testing laboratory requests samples be discarded once the analysis is completed

o Place de-stemmed lamina in paper bag and air-dry to lowest possible moisture

o After the sample is dried, and immediately prior to shipment, transfer it from the

paper bag to a plastic bag (example: zip-lock).

2.9 Samples storage at origin

Keep samples clean in order to avoid insect infestation. If possible keep the samples

in a freezer.

o If samples are infested by insects, the Japanese quarantine office requires

fumigation which takes time and great financial cost. If adequate sanitation cannot

be realized it is possible that samples could be discarded.

2.10 Packing, Labeling & Shipment (see Fig. 3)

Each tobacco sample should be delivered in a clean, clear plastic bag, which is

appropriately labeled and enclosed in a second bag to prevent accidental contamination

during transit.

Labeling: Stalk position, tobacco type, origin, a.i., treated/untreated, etc. (See file “RFT

TF_report_format_ver.5.xls.”)

Shipment (See file “RFT TF_report_ format_ver.5.xls.”

o Freight company: TNT Express or Nippon Express Co., Ltd

o Notify JT sample receiver of sample shipment

o Ship all samples in one package/box to minimize shipping cost and Japanese

import taxes/duties

o Shipment cost: to be paid by sender.


3. Field documentation and record keeping

See file “RFT TF_report_format_ver.5.xls.”

In “RFT TF_report_format ver.5. xls.”, there is other required information that does

not link directly to this protocol , e.g.:

o Trial CPA information,

o Crop and field information including “plot size”, “plant spacing”,

o Precise use pattern information and Field trial information,

o Other information including irrigation, precipitation, temperature, etc.

4. Residue analysis

Testing lab: Japan Tobacco Inc. - Leaf Tobacco Research Center

Laboratory documentation and record keeping (See another file “RFT

TF_report_format_ver.5.xls.”)

Table 1. New GRL candidates

# Priority Guide N°1 CPA Company Active Ingredient

1

Priority 1

no Syngenta Azoxystrobin

2 no Syngenta Difenoconazole

3 no Du Pont Indoxacarb

4 no Bayer CropScience Propamocarb

5 no Bayer CropScience Tebuconazole

6 no Du Pont Chlorantraniliprole

7 no Bayer CropScience Triflumuron

8 no Bayer CropScience Triadimefon/Triadimanol

9 no Bayer CropScience Ethion

10 no Bayer CropScience Triazophos

11 no Bayer CropScience Fenamidone

12 no Bayer CropScience Flubendiamide

13

Priority 2

no Bayer CropScience Clothianidin

14 no DOW Dicofol

15 no BASF Teflubenzuron

16 no Bayer CropScience Iprovalicarb

17 no Bayer CropScience Spirotetramat

18 no Bayer CropScience Bitertanol

19 no Kumiai Iprobenfos

20 no Bayer CropScience Thiacloprid

21

Priority 3

no BASF Chlorfenapyr

22 no Bayer CropScience Prothiofos

23 no Syngenta Quinalphos


In addition to the above CPAs, others, not yet defined as candidates for GRLs, will also be

evaluated for residues by some executors. Among these are valiphenal, benthiavalicarb,

fluopicolid, sulfentrazone and mandipropamid

Fig. 1-1. Trial design for 1 CPA being tested in 1 location

Fig. 1-2. Trial design for 3 CPAs being tested in 1 location

2 kg

2 kg 2 kg

2 kg

G G T T T G G U G G

Sampling Sampling

3 replicates 1 replicate

G: Guard row

T: Treated (applied) row

U: Untreated row

Non harvest

Treatment CPA "A"

A A A

A A A

A A A

2kg 2kg 2kg

2kg 2kg 2kg 2kg

2kg 2kg 2kg

G G T T T G G T T T G G T T T G G U G G

3 replicates

G: Guard row

T: Treated (applied) row

U: Untreated (control) row

Non harvest

Treatment CPA "A"

Treatment CPA "B"

Treatment CPA "C"

C

A A A B B B C C C

C C

A A A B B B C C

1 replicates3 replicates 3 replicates

A A A B B B C

Sampling Sampling Sampling Sampling


Fig. 2. Stalk position (Upper and Lower)

Fig. 3. Packing, Labeling & Shipment

Upper leaves

Lower leaves

FCV, BLY: B+TORT: 3+4

FCV, BLY: P+X+CORT: 1+2

Label Form Example

Company Japan Tobacco Inc. Before sending the samples to Japan,

Country Japan 1. Attach the label to each pack of samples

Treated or Untreated Treated/Untreated 2. Send the electronic file of this label by e-mail to Receiver and

Testing Agrochemical Azoxystrobin TF executive office (see protocol).

Type of Tobacco FCV/BUR/ ORT Available Freight Company for sending tobacco samples to Japan

Domination/Varaiety Co-319 TNT Express http://www.tnt.com/express/en_us/site/home.html

Stalk Position Upper/Lower Nippon Express Co., Ltd http://www.nipponexpress.com/

Replication No. 1/2/3 If above companies are not available in the sender country,

Carrying Company TNT please contact receiver.

Air WayBill No. GD123456789WW

Sending Date 22-Sep-12 Shipping cost is covered by sender.

From (Sender) To (Receiver)

Name NameJapan Tobacco Inc.

Leaf Tobacco Research Center

Address Address1900 , Idei, Oyama, Tochigi, Japan

Zip Code:323-0808

Attention Attention Ichiro ATOBE, Kiyoshi OYAMA

Phone Phone +81-285-34-2651

Fax Fax +81-285-25-4460

e-mail e-mail [email protected]

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