Technical Report Agrochemical Residue Field Trials First 3 ... · CORESTA Agrochemical Analysis Sub-Group (AA SG) and the testing laboratory JT R&D completed method validation. In
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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
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
RFT-049-CTR First 3-Year Programme of Trials – September 2017 4/14
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
RFT-049-CTR First 3-Year Programme of Trials – September 2017 5/14
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
Azo
xyst
robin
Difenoco
nazo
le
Indoxaca
rb
Pro
pam
oca
rb
Tebuco
nazo
le
Chlo
rantr
anilip
role
Triflum
uro
n
Triadim
efo
n
Triadim
enol
Eth
ion
Triazo
phos
Fenam
idone
Flu
bendia
mid
e
Clo
thia
nid
in
Dic
ofo
l
Teflubenzu
ron
Ipro
valica
rb
Spirote
tram
at
Bitert
anol
Ipro
benfo
s
Thia
cloprid
Chlo
rfenapyr
Pro
thio
fos
Quin
alp
hos
Valif
enala
te
Benth
iava
licarb
-iso
pro
pyl
Flu
opic
olid
e
Sulfentr
azo
ne
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)
RFT-049-CTR First 3-Year Programme of Trials – September 2017 6/14
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.
RFT-049-CTR First 3-Year Programme of Trials – September 2017 7/14
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.
Az
ox
ys
tro
bin
Dif
en
oc
on
az
ole
Ind
ox
ac
arb
Pro
pa
mo
ca
rb
Te
bu
co
na
zo
le
Ch
lora
ntr
an
ilip
role
Tri
flu
mu
ron
Tri
ad
ime
fon
Tri
ad
ime
no
l
Eth
ion
Tri
az
op
ho
s
Fe
na
mid
on
e
Flu
be
nd
iam
ide
Clo
thia
nid
in
Dic
ofo
l
Te
flu
be
nz
uro
n
Ipro
va
lic
arb
Sp
iro
tetr
am
at
Bit
ert
an
ol
Ipro
be
nfo
s
Th
iac
lop
rid
Ch
lorf
en
ap
yr
Pro
thio
fos
Qu
ina
lph
os
Va
life
na
late
Be
nth
iav
ali
ca
rb-i
so
pro
py
l
Flu
op
ico
lid
e
Dim
eth
om
orp
h
Ma
nd
ipro
pa
mid
e
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
RFT-049-CTR First 3-Year Programme of Trials – September 2017 8/14
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)
RFT-049-CTR First 3-Year Programme of Trials – September 2017 9/14
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).
RFT-049-CTR First 3-Year Programme of Trials – September 2017 10/14
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.
RFT-049-CTR First 3-Year Programme of Trials – September 2017 11/14
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.
RFT-049-CTR First 3-Year Programme of Trials – September 2017 12/14
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
RFT-049-CTR First 3-Year Programme of Trials – September 2017 13/14
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
RFT-049-CTR First 3-Year Programme of Trials – September 2017 14/14
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 kiyoshi.oyama@jt.com
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