Document ID: EPA-HQ-OPP-2008-0945-0010
Agency: epa
Document Type: Supporting & Related Material
Title: 
Posted Date: 2009-12-09T05:00Z

UNITED STATES ENVIRONMENTAL PROTECTION AGENCY

WASHINGTON, D.C.  20460

	OFFICE OF PREVENTION, PESTICIDE

	AND TOXIC SUBSTANCES

  SEQ CHAPTER \h \r 1 MEMORANDUM

Date:  5 August 2009

SUBJECT:	Clothianidin; Petitions for Tolerances and Seed Treatment Uses
on Root and Tuber Vegetables, Bulb Vegetables, Leafy Greens, Brassica
Leafy Vegetables, Fruiting Vegetables, Cucurbit Vegetables, and Cereal
Grains (except rice).  Summary of Analytical Chemistry and Residue Data.

PC Code:  044309	DP Barcodes:  D357454, D357455

Decision Nos.:  399488, 399566 	Registration Nos.:  264-RNIR; 264-RNIE

Petition Nos.:  8F7416, 8F7413	Regulatory Action:  Section 3
Registrations

Risk Assessment Type:  NA	Case No.:  NA

TXR No.:  NA	CAS No.:  210880-92-5

MRID No.:  See MRID Summary Table	40 CFR:  180.586

		              									Ver.Apr.08

FROM:	Michael A. Doherty, Ph.D., Chemist

		Risk Assessment Branch II

		  SEQ CHAPTER \h \r 1 Health Effects Division (7509P)

THROUGH:	Richard A. Loranger, Ph.D., Senior Scientist

		Risk Assessment Branch II

		  SEQ CHAPTER \h \r 1 Health Effects Division (7509P)

		

TO:		Kable Davis/Venus Eagle (Team 01)

		Insecticide/Rodenticide Branch

		Registration Division (7505P)  SEQ CHAPTER \h \r 1   SEQ CHAPTER \h \r
1 	

MRID Summary Table

MRID No.	Study Type	Comments

47483006	860.1340 RAM	New DER; 47483006.der.doc

47483007	860.1340 ILV

	47483008	860.1360 MRM	New DER; 47483008.der.doc

47483009	860.1380 Storage Stability	New DER; 47483009.der.doc

47483012	860.1500 Potato	New DER; 47483012.der.doc (U.S. field trial
data)

47483013	860.1500 Potato	New DER; 47483013.der.doc (Canadian filed trial
data)

47483014	860.1500 Root vegetables	New DER; 47483014.der.doc

47483015	860.1500 Bulb vegetables	New DER; 47483015.der.doc

47483017	860.1500 Leafy greens	New DER; 47483017.der.doc

47483018	860.1500 Brassica leafy vegetables	New DER; 47483018.der.doc

47483019	860.1500 Fruiting vegetables	New DER; 47483019.der.doc

47483020	860.1500 Cucurbit vegetables	New DER; 47483020.der.doc

47483021	860.1500 Wheat	New DER; 47483021.der.doc

47483022	860.1520 Potato	New DER; 47483022.der.doc

47483023	860.1520 Tomato	New DER; 47483023.der.doc

47483024	860.1520 Wheat	New DER; 47483024.der.doc

47524001	860.1900 Soybean	New DER; 47524001.der.doc

  SEQ CHAPTER \h \r 1 This document was originally prepared under
contract by Dynamac Corporation (1910 Sedwick Road, Building 100, Suite
B; Durham, NC 27713).  The document has been reviewed by the Health
Effects Division (HED) and revised to reflect current Office of
Pesticide Programs (OPP) policies.

Executive Summary

Clothianidin,
(E)-N-[(2-Chloro-5-thiazolyl)methyl]-N’-methyl-N”-nitroguanidine, is
a broad spectrum, systemic neonicotinoid insecticide (Group 4A
insecticide).  It is currently registered to Bayer CropScience for seed
treatment uses on canola (rapeseed), cotton, corn, sorghum, and sugar
beet, and to Valent USA Corporation for seed treatment uses and for
direct soil or foliar applications to grapes, pome fruits, potatoes and
tobacco.  Permanent tolerances are established for residues of
clothianidin per se in or on plant commodities at 0.01-1.0 ppm and in
milk at 0.01 ppm [40 CFR §180.586(a)], and time-limited tolerances are
established for clothianidin residues in sugar beet roots and tops at
0.02 ppm [40 CFR §180.586(b)].  Tolerances are also established for the
indirect residues of clothianidin at 0.02 ppm in nongrass animal feeds;
forage, fodder, and straw of cereal grains; forage, fodder, and hay of
grasses; and soybean forage and hay [40 CFR §180.586(d)].  

Bayer CropScience (Bayer) has submitted petitions (PP# 8F7413 and
8F7416) proposing the use of a multiple active ingredient (MAI),
wettable powder (WP) formulation containing 56.25% clothianidin and
18.75% imidacloprid (Sepresto 75WS, EPA Reg. No. 264-RNIR) for use as a
seed treatment for the control of various insects on the following
crops/crop groups:  root and tuber vegetables, bulb vegetables, leafy
green vegetables, Brassica leafy vegetables, fruiting vegetables,
cucurbit vegetables, and cereal grains, except rice.  The proposed uses
on vegetables crops (except potato) are for seed treatments at maximum
use rates of 0.1-1.2 g ai/1000 seed, and the proposed maximum use rate
for potatoes is 12.5 g ai/100 kg seed pieces.  For cereal grains (except
rice), the proposed maximum use rate is 70 g ai/100 kg seed.  The WP
formulation is slurried with water and a seed colorant, and applied
using commercial seed treatment equipment.  Bayer is also proposing use
of another MAI formulation for seed treatment of wheat, barley and
triticale (Proceed™ Optimum; EPA Reg. No. 264-RNIE).  This FlC
formulation contains 0.128 lb/gal of clothianidin along with three
fungicides (prothioconazole, tebuconazole, and metalaxyl).  The proposed
use rate for the FlC formulation is 7.5 g ai clothianidin/100 kg seed. 
In conjunction with these uses, Bayer is proposing the following
permanent tolerances for residues of clothianidin per se in/on the
following crop groups and commodities:

Vegetable, fruiting, Group 8	0.01 ppm

Vegetable, cucurbit, Group 9	0.01 ppm

Grain, cereal, except rice, Group 15	0.01 ppm

Wheat, forage	0.35 ppm

Wheat, hay	0.07 ppm

Wheat, straw	0.04 ppm

Bayer is also proposing permanent tolerances for the combined residues
of clothianidin and its metabolite TMG in/on the following crops or crop
groups:

Vegetable, root, except sugar beet, Subgroup 1B	0.6 ppm

Vegetable, tuberous and corm, Subgroup 1C	0.2 ppm

Vegetable, bulb, Group 3	0.2 ppm

Vegetable, leafy greens, except Brassica, Subgroup 4A	1.1 ppm

Vegetable, Brassica, leafy, Group 5	0.35 ppm

Potato	0.6 ppm

  SEQ CHAPTER \h \r 1 The nature of clothianidin residues in plants has
been adequately delineated based on the acceptable corn, sugar beet,
apple, and tomato metabolism studies.  Parent compound is the only
residue of concern in primary crops for both tolerance setting and risk
assessment purposes, except in leafy vegetables and root crops.  In
these crops, the residues of concern also include the metabolite
thiazolylmethylguanidine (TMG) for purposes of risk assessment.  The
nature of the residue in livestock is also understood based on the
acceptable goat and hen metabolism studies.  For risk assessment, the
residues of concern in ruminants include parent and the metabolites TZU,
TZG, TZNG, and ATMG-Pyruvate, and the residues of concern in poultry
include parent and the metabolites TZU, TZG, TZNG, and ATG-Acetate. 
However, only parent needs to be included in the tolerance expression
for animal commodities.

  SEQ CHAPTER \h \r 1 Adequate LC-MS/MS methods are available for
enforcing tolerances of clothianidin in plant commodities (Bayer Methods
00552, 00552-M001, and 109240-1) and livestock commodities (Bayer Method
00624).  The validated limit of quantitation (LOQ) for clothianidin in
plant commodities is 0.01 ppm, except in wheat straw (0.02 ppm), while
the validated LOQs are 0.01 ppm in milk, and 0.02 ppm in livestock
tissues.  Bayer has also submitted a LC-MS/MS method (Method No.
TI-002-P05-001) for enforcing recommended tolerances for the combined
residues of clothianidin and TMG on root and tuber vegetables and leafy
vegetables.  This method was adequately validated and has undergone a
successful independent laboratory validation (ILV) trail.  However, a
separate enforcement method including analysis of TMG is not required at
the present time, as the tolerance expression includes only
clothianidin.

 

Adequate LC-MS/MS methods are also available for collecting data on
residues of clothianidin and its metabolites TMG and TZNG in plant
commodities.  An adequate LC-MS/MS method (Method No. TI-002-P05-001)
was used for determining residues of clothianidin and TMG in root
vegetables, leafy vegetables, potatoes, and potato processed
commodities.  The validated LOQ for both analytes is 0.01 ppm in each
plant commodity.  Another LC-MS/MS method (Method No. T1-004-P07-01) was
used for determining residues of clothianidin per se in/on fruiting
vegetables, cucurbit vegetables and wheat commodities and in tomato and
wheat processed commodities.  The validated method LOQ for clothianidin
is 0.01 ppm in each plant matrix.  Residues of clothianidin per se in
the potato field trials from Canada and residues of clothianidin and
TZNG in soybean commodities from the rotational crop field trial were
determined using slightly modified versions of a tolerance enforcement
method (Method No. 00552/M001).  The validated method LOQ for
clothianidin and TZNG was 0.01 ppm in each commodity.

Storage stability data are available indicating that clothianidin is
stable under frozen storage conditions for up to 24 months in sugar beet
roots, canola seed, and field corn grain, forage and straw, 15 months in
apples and apple juice, 12 months in tomatoes and spinach, and ~6 months
in grapes and potato.  Data are also available indicating that the
metabolite TMG is stable under frozen storage conditions for up to 24
months in sugar beet leaves and potato tubers, flakes and chips, and ~6
months in grapes.  These data adequately support the sample storage
conditions and durations from the submitted field trials and processing
studies.  However, no data are available supporting the stability of the
metabolite TZNG in soybean commodities from the rotational crop field
trial.

The submitted field trial data for clothianidin are adequate and support
the propose seed treatment uses for the WP formulation.  An adequate
number of field trials were conducted on the required representative
crops in the appropriate geographic regions.  All field trials were
conducted at ~1x the maximum proposed use rates, with the exceptions of
the potato and wheat field trials.  The U.S. potato field trials were
conducted at 1.6x the proposed rate and the wheat field trials were
conducted at 1.8x the maximum proposed rate.  The appropriate number and
types of plant commodities were collected from each test at the earliest
possible commercial harvest, and samples of each commodity were analyzed
for the residues of concern using adequate LC-MS/MS methods.  The field
trial data are also supported by the available storage stability data. 
The submitted wheat field trial data for the 56% WP formulation will
also support the use of the 0.128 lb/gal FlC formulation, as the use
rate for this formulation is considerably lower (0.1x) than for the 56%
WP formulation.

As requested by the Agency, samples of all root and leafy vegetables
were analyzed for both clothianidin and the TMG metabolite.  Residues of
TMG were <LOQ in all samples of carrots, radish roots, potatoes, bulb
onions and cabbage.  For the crop samples having quantifiable residues
of both clothianidin and TMG, the ratio of clothianidin:TMG residues was
3.2x-4.8x for lettuce, spinach and broccoli, 1.9x for radish tops, 6.1x
for green onions, and 0.6x for mustard greens.

The submitted potato, tomato, and wheat processing studies are adequate.
 Because clothianidin residues were <LOQ in/on tomatoes and wheat grain
following seed treatments at ≥5x the proposed use rates, quantifiable
residues are unlikely to occur in tomato and wheat processed
commodities; therefore, separate tolerances for processed tomato and
wheat commodities are not required.  In the potato processing study,
residues of TMG were <LOQ in/on tuber and all processed fractions;
however residues of clothianidin were shown to concentrate by 1.4x in
wet peel, 2.6x in chips, and 6.3x in flakes/granules (the theoretical
maximum for flakes/granules is 4.7x).  Based on the highest average
field trial (HAFT) residues for potatoes from the Canadian trials and
the above processing factors, separate tolerances are required for
potato chips at 0.6 ppm and flakes/granules at 1.5 ppm.

Adequate livestock feeding studies are available for clothianidin, and
tolerances for clothianidin residues in animal commodities were recently
assessed in conjunction with petitions for uses on grapes, potatoes,
sorghum and cotton.  As the proposed uses will not increase the dietary
exposure of livestock to clothianidin residues, reassessment of animal
tolerances is not required for the current petitions.

An adequate confined field rotational crop study is available for
clothianidin.  The metabolism of clothianidin in rotational crops is
similar to the metabolism in primary crops, and HED has concluded that
parent, TZNG and MNG are the residues of concern in rotational crops for
purposes of risk assessment.  However, only parent needs to be included
in the tolerance expression.  The available field rotational crop
studies are adequate and support the existing tolerances for rotational
crops.  The submitted soybean rotational crop field trials are also
adequate and support the 30-day plant-back interval (PBI) specified for
soybeans and dried beans and peas on the proposed label for the 56% WP
formulation.

  SEQ CHAPTER \h \r 1 Regulatory Recommendations and Residue Chemistry
Deficiencies

No major deficiencies were noted in the subject petition that would
preclude establishing permanent tolerances for residues of clothianidin
on the proposed commodities and crop groups.  However, the petitioner
should resolve the following minor deficiencies:  

	•	Information is required clarifying the proposed use rates for
potatoes and cereal grains on the label for the 56% WP formulation (see
Use Directions Section).

	•	The use direction for “Root Vegetables” should be corrected to
read “Root and Tuber Vegetables.” 

	•	The label should be amended to prohibit the use of treated seeds
for food, feed, or oil purposes, including the production of seed
sprouts.

	•	The final reports depicting the frozen storage stability of
clothianidin in spinach and tomatoes are required for evaluation by HED.
 Submission of this report should be a condition of registration.

	•	To support the submitted soybean field rotational crop trials, data
are required demonstrating the stability of the TZNG method in frozen
soybean commodities for up to 18 months.  Submission of these data
should be a condition of registration.

	•	A revised Section F is required incorporating the changes to the
proposed tolerances recommended by HED (see Table 8).

Based on all the available residue data, HED recommends for establishing
permanent tolerances for clothianidin as detailed in Table 8.  Note that
HED has recently evaluated other petitions for clothianidin requesting
registration of foliar uses.  Some of the use sites overlap and,
generally, the recommended tolerance level is governed by the foliar
uses.  The tolerance expression for clothianidin should be revised to be
as follows:  

Tolerances are established for residues of the insecticide clothianidin,
including its metabolites and degradates, in or on the commodities in
the table below as a result of the application of clothianidin. 
Compliance with the tolerance levels specified below is to be determined
by measuring only clothianidin
[(E)-N-[(2-Chloro-5-thiazolyl)methyl]-N’-methyl-N”-nitroguanidine]
in or on the commodity.

Human health risk assessments for clothianidin are forthcoming.

Background

Clothianidin is a broad spectrum, systemic insecticide belonging to both
the chloronicotinyl (neonicotinoid) and nitroguanidine classes of
chemicals.  It is also a major metabolite of thiamethoxam.  Clothianidin
acts by binding with the nicotinic acetylcholine receptor sites in
insects (Group 4A insecticide), interfering with neural transmission of
stimuli and eventually inhibiting reproduction of the insect. 
Clothianidin Technical Insecticide was first registered in the U.S.
during 2003 by Takeda with Bayer acting as their Agent.  Bayer currently
has seven end-use products containing clothianidin that are registered
only for seed treatment uses on corn, canola, cotton, rapeseed, sorghum,
and sugar beet.  Clothianidin end-use products with direct foliar and/or
soil uses on grapes, pome fruits, potatoes and tobacco were originally
registered to Arvesta (now known as Arysta).  However, these
products/uses have been transferred to Valent, which is now the Agent
for Sumitomo Chemical Co. which owns the current registration for
Technical Clothianidin.

 MAI formulation for seed treatment of wheat, barley and triticale
(Proceed™ Optimum; EPA Reg. No. 264-RNIE).  This FlC formulation
contains 0.128 lb/gal of clothianidin along with three fungicides
(prothioconazole, tebuconazole, and metalaxyl).

The chemical structure and nomenclature of clothianidin and its
metabolite, TMG, are listed in Table 1, and the physicochemical
properties of technical grade clothianidin are listed in Table 2. 

Table 1.	Clothianidin Nomenclature.

Parent Compound	

Common name	Clothianidin

Company experimental name	TI-435, V-10066

IUPAC name
(E)-1-(2-Chloro-1,3-thiazol-5-ylmethyl)-3-methyl-2-nitroguanidine

CAS name
(E)-N-[(2-Chloro-5-thiazolyl)methyl]-N’-methyl-N”-nitroguanidine

CAS registry number	210880-92-5 (formerly 205510-53-8)

Molecular wt.	249.68

End-use product (EP)	56.25% WP Seed Treatment (Sepresto® 75 WS)

Metabolite	

Common name	Thiazolylmethylguanidine

Company experimental name	TMG

IUPAC name	N-(2-chlorothiazol-5-yl)-N´-methylguanidine

CAS Name	N-(2-chlorothiazol-5-yl)-N´-methylguanidine

CAS registry number	635283-91-9

Molecular wt.	204.68

Table 2.	Physicochemical Properties of Clothianidin.

Parameter	Value	Reference

Melting point (ºC)	176.8	D335355, W. Drew, 10/16/07

pH at 23ºC	6.24 (1% solution/suspension)

	Density (g/cm3)	1.61 (PAI)*, 1.59 (TGAI)

	Water solubility (g/L at 20ºC)	0.327

	Solvent solubility (g/L at 25ºC)	Acetone	15.2	Dichloromethane	1.32

Ethyl acetate	2.03	Heptane 	<0.00104

Methanol	6.26	Octanol	0.938

Xylene	0.0128

	Vapor pressure (Pa at 20ºC)	1.3 x 10 -10

	Dissociation constant, pKa at 20ºC	11.09

	Octanol/water partition coefficient, Log(KOW) at 25ºC	0.7

	UV/visible absorption spectrum (Maximum, nm)	265.5 (acidic or neutral)

246.0 (basic)

	*PAI = Purified Active Ingredient; TGAI = technical grade active
ingredient.

860.1200  Directions for Use

The proposed use directions are summarized below in Table 3.

Table 3.	Summary of Directions for Use of Clothianidin Seed Treatments.

Applic. Timing, Type, and Equip.	Form.

[EPA Reg. No.]	Application Rates 1	Use Directions and Limitations 3

g ai/1000 seeds 	oz ai/1000 seeds	lb ai/A 2

	Root Vegetables (Group 1) 4

Seed treatment using commercial seed treatment equipment only	56.25% WP

[264-RNIR] 	Radish:  0.45

Carrot:  0.118	Radish:  0.01575 

Carrot:  0.0042	Radish: 0.50-0.67

Carrot:  0.10-0.25	Do not use treated seed for food, feed or oil
processing.

Bulb Vegetables (Group 3)

Seed treatment using commercial seed treatment equipment only	56.25% WP 

[264- RNIR]	Bulb onion:  0.18 

Green onion:  0.106

Leek: 0.20	Bulb onion:  0.006 

Green onion:  0.0037

Leek: 0.0071	Bulb onion:  0.06-0.19 

Green onion:  0.23-0.42

Leek: 0.30-0.35	Do not use treated seed for food, feed or oil
processing.

Leafy Green Vegetables (Subgroup 4A)

Seed treatment using commercial seed treatment equipment only	56.25% WP

[264- RNIR] 	Head Lettuce:  0.798 

Leaf Lettuce: 0.64 

Spinach: 0.16	Head Lettuce:  0.028 

Leaf Lettuce: 0.0225 

Spinach: 0.0055	Head Lettuce:  0.70-2.25

Leaf Lettuce:  0.68-2.26

Spinach:  0.09-0.21	Do not use treated seed for food, feed or oil
processing.

Brassica Leafy Vegetables (Group 5)

Seed treatment using commercial seed treatment equipment only	56.25% WP 

[264- RNIR]	Cabbage:  1.193

Broccoli:  1.193

Mustard Greens: 0.0995 	Cabbage: 0.0416

Broccoli:  0.0416

Mustard Greens: 0.0035	Cabbage:  0.06-0.44

Broccoli:  0.39-0.42

Mustard Greens: 0.03-0.16	Do not use treated seed for food, feed or oil
processing.

Fruiting Vegetables (Group 8)

Seed treatment using commercial seed treatment equipment only	56.25% WP

[264- RNIR] 	Tomato:  0.099

Pepper: 0.495	Tomato:  0.0035

Pepper: 0.0174 	Tomato:  0.02-0.06

Pepper:  0.04-0.21	Do not use treated seed for food, feed or oil
processing.

Cucurbit Vegetables (Group 9)

Seed treatment using commercial seed treatment equipment only	56.25% WP

[264- RNIR] 	Squash:  0.995

Melon:  0.995

Cucumber:  0.995	Squash:  0.034

Melon:  0.034

Cucumber:  0.034	Squash:  0.04

Melon:  0.02-0.11

Cucumber:  0.04-0.16	Do not use treated seed for food, feed or oil
processing.

Cereal Grains, except rice (Group 15)

Seed treatment using commercial seed treatment equipment only	56.25% WP 

[264- RNIR]	70 g ai/100 kg seed	1.125 oz ai/100 lbs seed 

	Corn:  0.007-0.011

Sorghum: 0.001-0.007

Millet:  0.011-0.025

Barley:  0.035-0.067

Oats:   0.034-0.090

Wheat:   0.021-0.105	Do not use treated seed for food, feed or oil
processing.

Wheat, Barley and Triticale

Seed treatment using on farm or commercial seed treatment equipment.  
0.128 lb/gal FlC

[264-RNIE]	7.5 g ai/100 kg seed	0.12 oz ai/100 lb seed	Barley: 
0.004-0.007

Wheat:   0.002-0.011	Do not use treated seed for food, feed or oil
processing.

Forage may be grazed or harvested 31 days after seeding.

Potato 

Seed treatment using commercial seed treatment equipment only	56.25% WP

[264- RNIR]	12.5 g ai/100 kg seed pieces	0.20 oz ai/100 lb seed pieces
potato:  0.163-0.325	Do not use treated seed for food, feed or oil
processing.

1	The seed treatment rates are expressed in g ai/1000 seed and oz
ai/1000 seed are the maximum use rates, unless otherwise indicated. 
Although the use directions cover entire crop groups, the use rates for
individual crops in each group were listed under each group.

2	The range of potential application rates expressed on a lb ai/A basis
were calculated by the reviewer using the maximum seed treatment rate
for each crop and information on the number of seeds/lb and planting
rates (lbs seed/A) from the ExposSAC SOP 15 memo (3/2/2004).

3	For all uses, the label for the 56% WP specifies a maximum use rate of
0.375 lb ai/A per cropping cycle for clothianidin, regardless of
application type (seed, soil or foliar).  The label also specifies the
following rotational crop restrictions:  Areas planted with treated seed
may be replanted immediately with any crop having uses or tolerances for
clothianidin and imidacloprid.  Areas may also be replanted 30 days
later with soybeans, dried beans or dried peas.  Do not plant any other
crops in treated areas for at least one year after the treated seeds are
planted.   No maximum seasonal use rate or rotational crop restrictions
are specified on the label for the 0.128 lb/gal FlC.

4	Although the label specifies directions for “Root Vegetables”, the
label also cites Crop Group 1 and includes all vegetables in the Root
and Tuber Vegetables Crop Group. 

Conclusions.  The proposed label directions for the 56% WP formulation
are adequate and are supported by the available field trial data. 
However, HED noted that the field trial data on wheat and potatoes (U.S.
trials) would support higher use rates than those currently specified on
the proposed label.

The proposed use rate for potato seed pieces is 0.0125 lb ai/100 lb seed
(12.5 g ai/100 kg seed); however, the use rate for clothianidin in the
U.S. potato field trials was 0.019 lb ai/100 lb seed (19 g ai/100 kg
seed; 1.5x rate).  For a typical potato planting density of 2000 lb seed
pieces/A, the proposed rate would be equivalent to 0.25 lb ai/A and the
field trial rate would be equivalent to 0.38 lb ai/A. Based on the
information and data submitted with the rotational soybean field trials,
it appears that Bayer is supporting the higher use rate of 0.019 lb
ai/100 lb seed for potatoes.  This is also suggested by the fact that
the maximum seasonal use rate on the label is 0.374 lb ai/A, which is
equivalent to the field use rate for potatoes.

For cereal grains, the proposed use rate is 0.07 lb ai/100 lb seed (70 g
ai/100 kg seed); however, the use rate in the wheat field trials was
0.125 lb ai/100 lb seed (1.8x).  Considering that the label specifies a
maximum application rate of 2 oz product/100 lb seed (0.125 lb
product/100 lb seed), it appears that there is an error in the
application rate for cereal grains on the proposed label.  The
petitioner should clarify the proposed application rates for both
potatoes and cereals grains.

In addition, the label currently lists uses for “Root Vegetables”
and then specifies all the crops listed under Crop Group 1, including
all the tuberous and corm crops.  The use directions should be amended
to specify the use on “Root and Tuber Vegetables”.

With the respect to the label for the 0.128 lb/gal FlC (Proceed
Optimum), the submitted wheat field trial data will adequately cover the
proposed use as the use rate of the FlC is one tenth that of the WP
formulation.

860.1300 Nature of the Residue - Plants	

  SEQ CHAPTER \h \r 1 MARC Memo, D282449, Y. Donovan, 4/25/03

DP#D282446, Y. Donovan, 5/1/03

Adequate plant metabolism studies are available reflecting the
application of [14C]-clothianidin as a seed treatment to corn and sugar
beets, as foliar applications to apples, and as soil and foliar
applications to tomatoes.  Based on these metabolism studies, the
Metabolism Assessment Review Committee (MARC) concluded that the nature
of the residue has been adequately delineated, and that parent only is
the residue of concern to be used in risk assessment and the tolerance
expression for most primary crops.  However, the MARC also determined
that future uses on root crops and/or leafy vegetables will require
analysis of TMG along with parent in field trial samples.  The metabolic
profiles in the tested primary crops were similar in that the highest
level residue was the parent, clothianidin, with the exception of mature
sugar beet tops.  TMG is being included as a residue of concern for this
risk assessment.

860.1300 Nature of the Residue - Livestock

  SEQ CHAPTER \h \r 1 MARC Memo, D282449, Yan Donovan, 4/25/03

DP# D282446, Yan Donovan, 5/1/03

The nature of clothianidin residues in livestock is understood based on
the adequate goat and hen metabolism studies.  In these studies, a goat
was dosed orally for 3 days with [14C]-clothianidin at levels equivalent
to roughly 200 ppm in the diet, and hens were dosed orally for 3 days
with [14C]-clothianidin at levels equivalent to 140 ppm in the diet. 
For ruminants, the MARC concluded that the residues of concern include
parent, TZU, TZG, TZNG, and ATMG-Pyruvate and that these residues should
be included in risk assessments.  For poultry, the MARC concluded that
the residues of concern include parent, TZU, TZG, TZNG and ATG-Acetate
for risk assessment purposes.  However, for purposes of tolerances, the
MARC recommended that only parent needs to be included in the tolerance
expression for animal commodities.  

860.1340 Residue Analytical Methods

DP# D303164, W. Drew, 2/1/06

47483006.der.doc 

Enforcement Methods

Adequate LC-MS/MS methods are available for enforcing tolerances for
clothianidin residues in plant (Bayer Methods 00552 and 109240-1) and
animal (Bayer Method 00624) commodities.  The LOQ for clothianidin in
plant commodities is 0.01 ppm, except for wheat straw (0.02 ppm), and
the validated LOQs are 0.01 ppm in milk and 0.02 ppm in animal tissues. 
All three of these methods were reviewed by BEAD’s Analytical
Chemistry Laboratory, approved for tolerance enforcement, and forwarded
to FDA for inclusion in PAM Volume II.

In addition, Bayer has submitted a method description and validation
data for an LC-MS/MS method (Method No. TI-002-P05-001) for determining
residues of clothianidin and its metabolite
N-(2-chlorothiazol-5-yl)-N´-methylguanidine (TMG) in plant commodities.
 This method is being proposed as a possible enforcement method for
determining clothianidin and TMG residues in/on root and tuber
vegetables and leafy vegetables.   

For this method, residues are extracted from plant samples (2 g/sample)
twice with acetonitrile (ACN) and then twice with ACN:water (1:1, v:v). 
The extracts are centrifuged, and the resulting supernatants are
combined and diluted with 0.045% acetic acid.  Deuterated (d3-methyl)
internal standards of clothianidin (TI-435d3) and TMG (TMG-d3) are then
added, and residues are purified by elution through a C18 solid phase
extraction (SPE) cartridge.  The resulting eluate is concentrated to
near dryness, and redissolved in 0.1% acetic acid:ACN (90:10, v/v) and
filtered.  Residues are analyzed by LC-MS/MS using the m/z 250→169.16
transition for clothianidin, and residues the m/z 206.86→134.06
transition for TMG.  The retention times for clothianidin and TMG are
approximately 8.0 and 5.2 minutes, respectively.  The validated limit of
quantitation (LOQ) is 0.01 ppm for each analyte in/on root and leafy
vegetable matrices, and the limits of detection (LODs) are 0.002-0.003
ppm.  Residues are expressed in terms of each analyte.

This method was adequately validated using control samples of potato
tubers and turnip tops fortified with clothianidin or TMG, each at 0.01
and 0.10 ppm.  The recoveries of clothianidin and TMG were acceptable. 
Average recoveries (±S.D.) for clothianidin were 79 ± 5% from potato
tubers and 75 ± 10% from turnip tops.  Average recoveries (±S.D.) for
TMG were 87 ± 10% from potato tubers and 77 ± 7% from turnip tops. 
Apparent residues of clothianidin and TMG were <LOD ppm in/on all
control samples.

The LC-MS/MS method has also undergone a successful independent
laboratory validation (ILV) trial using control samples of potatoes
fortified with TMG at 0.01, 0.02 and 0.1 ppm.  Recoveries of TMG in the
first ILV trial averaged 89-96% with standard deviations of 2-3%. 
However, no radiovalidation data were provided for the method.

Data Collection Methods

In the root vegetable, bulb vegetable, leafy green vegetable, Brassica
vegetable, and potato (U.S. trials) field trials and the potato
processing study, residues of clothianidin and TMG in/on each plant
commodity were determined by using above LC-MS/MS method (Method No.
TI-002-P05-001).  The method was adequately validated in conjunction
with the analysis of the samples from each field trial and processing
study.  Adequate sample calculations and example chromatograms were
provided, and the fortification levels used for the method recoveries
bracketed the measured residue levels.  Apparent residues of
clothianidin and TMG were <LOQ in/on control samples, with the
exceptions of one control sample of potato having apparent residues of
clothianidin at 0.032 ppm and one control sample of radish roots having
apparent residues of clothianidin at 0.014 ppm.  The validated LOQ is
0.01 ppm for both analytes in each commodity and the calculated LODs are
0.001-0.003 ppm.

In the fruiting vegetable, cucurbit vegetable and wheat field trials and
the tomato and wheat processing studies, residues of clothianidin in/on
each commodity were determined using an LC-MS/MS method (Bayer Method
No. T1-004-P07-01), which is a modified version of Bayer Method 00552. 
For this method, residues were extracted with ACN:water (2:1, v/v) and
filtered, and a deuterated internal standard of clothianidin is added. 
The extract is then diluted with 0.1% acetic acid and residues were
cleaned up by elution through a C18 SPE cartridge.  The eluate is
diluted with 0.1% acetic acid and residues of clothianidin were
determined by LC-MS/MS using the internal standard.  The m/z 250→169
ion transition was used for quantitation of clothianidin residues.

Method No. T1-004-P07-01 was adequately validated in conjunction with
the analysis of the samples from each field trial and processing study,
and the fortification levels used for the method recoveries bracketed
the measured residue levels.  Apparent residues of clothianidin were
<LOQ in/on control samples.  The validated LOQ is 0.01 ppm for each
crop, and the calculated LODs are 0.002-0.005 ppm. 

m/z 250→169 ion transition for quantitation of clothianidin residues. 
The validated LOQ is 0.02 ppm, and the estimated LOD is 0.01 ppm.  This
method was also adequately validated in conjunction with the analysis of
the field trial samples.

In the soybean rotational crop field trial, soybean commodities were
analyzed for residues of clothianidin and its metabolite TZNG using
another LC-MS/MS method, which is also a slightly modified version of
Bayer Method 00552/M001.  For this method, residues were extracted with
ACN:water (2:1, v/v) and filtered.  Stable isotopes of [2H3]
clothianidin and [13C, 15N] TZNG were then added to the extract as
internal standards.  The extract was concentrated to remove the ACN, and
then eluted through a ChemElut CE 1010 cartridge with cyclohexane:ethyl
acetate (1:1, v/v).  Residues were concentrated to dryness, redissolved
in ACN, diluted with water, and then analyzed by LC-MS/MS using the
internal standards for quantitation.  The m/z 250→169 and 236→132
ion transitions were used for quantifying clothianidin and TZNG,
respectively.  This method was adequately validated in conjunction with
the analysis of the field trial samples.  The validated LOQ is 0.01 ppm
for clothianidin and TZNG in all soybean matrices.  The statistically
calculated LODs for both analytes are 0.002-0.004 ppm.

Conclusions. Adequate methods are available for enforcing tolerances for
residues of clothianidin on plant commodities.  The residue data on
clothianidin, TMG and TZNG in the submitted field trials, processing
studies, and rotational crop field trials were collected using adequate
LC-MS/MS methods.

Bayer has proposed an adequate LC-MS/MS method (Method No.
TI-002-P05-001) for enforcing possible tolerances for the combined
residues of clothianidin and TMG in/on root and tuber vegetables, leafy
vegetables, and Brassica vegetables.   Adequate validation data were
provided for this method, and the method has undergone a successful ILV
trial.  However, HED has concluded that only clothianidin needs to be
included in the tolerance expression for both primary and rotational
crops and for animal commodities.  Residues of TMG will be used only for
risk assessment.  Therefore, a separate tolerance enforcement method is
not required for TMG residues at the present time. 

860.1360 Multiresidue Methods

DP# D282446, Yan Donovan, 5/1/03

47483008.der.doc

Multiresidue method testing of clothianidin and its metabolites MNG,
TZG, TZNG, TZU, and ATMG-Pyr have been previously submitted.  
Clothianidin and its major metabolites are not adequately recovered
using any of the multiresidue methods.  These data were forwarded to the
US FDA for further evaluation.  With the current petitions, Bayer has
also submitted data indicating that the TMG metabolite is not recovered
using FDA multiresidue methods.  The TMG metabolite is not a residue of
concern for tolerance enforcement purposes; therefore, the multiresidue
data for TMG will not be forwarded to FDA.

860.1380 Storage Stability

47483009.der.doc (TMG in potato and sugar beet tops)	

Adequate storage stability data are available indicating that
clothianidin is stable at ≤-18°C for up to 24 months in sugar beet
roots, canola seed, and field corn grain, forage and straw (DP# 282446,
Y. Donovan, 5/1/03) and 15 months in apples and apple juice (DP# 287182,
W. Cutchin, 7/13/04).  Data are also available indicating that both
clothianidin and TMG are stable at -20°C for up to 5.3 months in grapes
and 6 months in potatoes (DP# 303164, W. Drew, 2/1/06).  

In appendices to the leafy green and fruiting vegetable field trials
(MRIDs 47483017 and 47483019), Bayer also provided preliminary storage
stability data for clothianidin in frozen spinach and tomatoes from an
ongoing study (Bayer Crop Science No. RATIY019).  In this study, control
samples of tomatoes and spinach were fortified with clothianidin at 0.25
ppm and stored at -10°C.  Triplicate fortified samples were analyzed
immediately after fortification (0-day), and duplicate stored samples
were analyzed after approximately 1, 3, 6 and 12 months of storage,
along with control samples and two freshly fortified samples.  The
average corrected recovery for clothianidin after 12 months of frozen
storage was 94% from tomatoes and 92% from spinach, indicating that
clothianidin is stable at -10°C for up to 12 months in tomatoes and
spinach.

nd stored at ≤-10°C.  Three fortified replicates of each matrix were
analyzed prior to storage on Day zero, and two fortified samples of each
matrix were reanalyzed after approximately 0, 1, 3, 6, 12, 21, and 24
months of frozen storage.  At each sampling interval, control samples
and two freshly fortified control samples of each matrix were analyzed
along with the stored samples using an adequate LC-MS/MS method (Method
No. TI-002-P05-001), which has a validated LOQ of 0.01 ppm for TMG. 
Average corrected recoveries for TMG after ~24 months of frozen storage
were 96% from potato tubers, 92% for potato flakes, 94% for potato
chips, and 89% for sugar beet leaves.  These data indicate that TMG is
stable in potato tubers, flakes and chips, and sugar beet leaves stored
at ≤-10°C for up to 24.6 months.

The storage durations and conditions of samples from the crop field
trials and processing studies submitted to support these petitions are
presented in Table 4.  

Table 4.	Summary of Storage Conditions and Durations of Samples from
Crop Field Trial and Processing Studies.  

Matrix 	Storage Temperature  (°C)	Actual Storage Duration (days)
Interval of Demonstrated Storage Stability (days) 1

Potato (U.S. trials)	<-15	309	720 (clothianidin – sugar beet roots)

750 (TMG – potato)

Potato (Canadian trials)	-10	496-516	720 (clothianidin – sugar beet
roots)

Carrot roots	<0	33-299	720 (clothianidin – sugar beet roots)

750 (TMG – potatoes and sugar beet leaves)

Radish roots

9-349

	Radish tops

8-356

	Bulb onion	<0	17-411	720 (clothianidin – sugar beet roots)

750 (TMG – potato)

Green onion

237-287

	Head lettuce	<0	43-250	368 (clothianidin – spinach)

750 (TMG – sugar beet leaves)

Leaf lettuce

146-311

	Spinach

143-225

	Broccoli	<0	89-305	368 (clothianidin – spinach)

750 (TMG – sugar beet leaves)

Cabbage

39-261

	Mustard greens

197-373

	Tomato	<0	13-219	368 (clothianidin – tomato)

Bell pepper 

13-247

	Non-Bell pepper

15-223

	Cucumber	<-15	223-294	368 (clothianidin – tomato)

Muskmelon

196-268

	Summer squash

212-307

	Wheat forage	<-15	148-421	720 (clothianidin – corn grain, forage and
stover)

Wheat grain

112-373

	Wheat hay

86-374

	Wheat straw

86-344

	Potato tuber (RAC)	<-15	487	720 (clothianidin – sugar beet roots)

≤-9	210	368 (clothianidin – tomato)

Wheat grain (RAC)	≤-9	210	720  (clothianidin – corn grain)

1	The relevant commodity and analyte for the supporting storage
stability data are listed in parentheses.

Conclusions.  The available storage stability data are adequate and
indicate that clothianidin is stable at ≤0°C for at least 24 months
in sugar beet roots, canola seed, and corn grain, forage and stover, 15
months in apples and apple juice, 12 months in spinach and tomatoes, and
5-6 months in grapes and potatoes.  The metabolite TMG is also stable at
≤0°C for up to 5.3 months in grapes and 24.6 months in sugar beet
leaves and potato tubers, flakes and chips.  The available storage
stability data adequately support the storage conditions and durations
for samples from the submitted field trials and processing studies.

860.1400 Water, Fish, and Irrigated Crops

There are no proposed uses that are relevant to this guideline topic.

860.1460 Food Handling

There are no proposed uses that are relevant to this guideline topic.

860.1480 Meat, Milk, Poultry, and Eggs

DP# D282446, Y. Donovan, 5/1/03

DP# D309473, W. Drew, 2/1/06

Adequate livestock feeding studies are available for clothianidin, and
tolerances for clothianidin residues in animal commodities were recently
assessed in conjunction with petitions for uses on grapes, potatoes,
sorghum and cotton (DP# D309473).  The maximum dietary burdens (MDB) of
livestock for clothianidin residues were calculated at that time to be
0.321 ppm for beef cattle, 0.287 ppm for dairy cattle, 0.020 ppm for
poultry, and 0.035 ppm for swine.  For this petition, the dietary
exposure of livestock to clothianidin residues were recalculated using
the maximum reasonably balanced diets (MRBD) for livestock (ChemSAC
memo, 6/30/08), the established tolerances, and the tolerances
recommended for feedstuffs in a concurrent clothianidin petition from
Valent (PP# 8F7395 and 8E7460, DP# 355896 and 360842).  The recalculated
residues in the MRBDs were 0.291 ppm for beef cattle, 0.289 ppm for
dairy cattle, 0.012 ppm for swine and 0.013 ppm for poultry (Table 5). 

As the proposed uses will not increase the dietary exposure of livestock
to clothianidin residues, reassessment of animal tolerances is not
required for these petitions.  The current 0.01 ppm tolerance for milk
is adequate and tolerances are not required for eggs or fat, meat, and
meat byproducts of cattle, goats, hogs, horses, sheep and poultry.

Table 5.   Calculation of Dietary Burdens for Clothianidin Residues to
Livestock.

Feedstuff	Dietary Component	% Dry Matter 1	% Diet 1	Residues  (ppm) 2
Dietary Contribution (ppm) 3

Beef Cattle

Field corn forage	R	40	10	0.10	0.025

Cotton gin byproducts	R	90	5	4.5	0.250

Sugar beet molasses	CC	75	10	0.05	0.007

Field corn grain	CC	88	70	0.01	0.008

Cottonseed meal	PC	89	5	0.02 4	0.001

TOTAL BURDEN	100

0.291

Dairy Cattle

Field corn forage	R	40	35	0.1	0.088

Almond, hulls	R	90	10	1.5	0.167

Sugar beet molasses	CC	75	10	0.05	0.007

Field corn grain	CC	88	35	0.01	0.004

Cottonseed	PC	88	10	0.20	0.023

TOTAL BURDEN	100

0.289

Poultry 

Field corn grain	CC

75	0.01	0.008

Cottonseed meal	PC

20	0.02 4	0.004

Soybean seed	PC

5	0.02	0.001

TOTAL BURDEN	100

0.013

Swine 

Field corn grain	CC

85	0.01	0.009

Cottonseed meal	PC

15	0.02 4	0.003

TOTAL BURDEN	100

0.012

1	Potential dietary burdens for livestock were determined using recent
Agency guidance on calculating the maximum reasonably balanced diets for
livestock (memo, 6/30/2008).

2	The tolerance level for the RAC was used for any associated processed
fractions unless otherwise indicated.

3	Contribution = ([tolerance /% DM] X % diet) for beef and dairy cattle;
contribution = ([tolerance] X % diet) for poultry and swine.

4	A residue level of 0.02 ppm was used for cottonseed meal, as the
cotton processing study indicated that residues are reduced in meal by
0.1x.

860.1500 Crop Field Trials

47483012.der.doc (potato)	47483014.der.doc (carrot and radishes)
47483015.der.doc (onions)

47483017.der.doc (leafy greens)	47483018.der.doc (Brassica vegetables)
47483019.der.doc (fruiting vegetables) 47483020.der.doc (cucurbits)
47483021.der.doc (wheat)	

Bayer has submitted field trial data on carrots, radishes, green and dry
bulb onions, lettuce, spinach, broccoli, cabbage, mustard greens,
tomatoes, Bell and non-Bell peppers, cucumbers, squash, muskmelons and
wheat to support proposed seed treatment uses of a MAI WP formulation
containing 56% clothianidin.    SEQ CHAPTER \h \r 1 The results from
these field trials are discussed below and the residue data are
summarized in Table 6.  

Table 6.	Summary of Residue Data from Crop Field Trials Using Seed
Treatments of Clothianidin (WP or FlC).

Crop matrix	Analyte	Applic. Rate 1	PHI (days)	Residue Levels (ppm) 2

n	Min.	Max.	HAFT 3	Median	Mean	Std. Dev.

Root Vegetables:  proposed use = carrot – 0.118 g ai/1000 seed, radish
– 0.45 g ai/1000 seed

Carrot	Clothianidin	0.12

(0.023-0.342)	90-196

90-196	16	<0.00	0.011	0.011	0.010	0.010	<0.001

	TMG

	16	<0.01	<0.01	<0.010	0.010	0.010	NA

Radish roots	Clothianidin	0.50

(0.087-0.429)	34-60

34-60	10	<0.01	0.625	0.528	0.016	0.124	0.219

	TMG

	10	<0.01	<0.01	<0.01	0.010	0.010	NA

Radish tops	Clothianidin	0.50

(0.087-0.429)	34-60

34-60	10	<0.01	0.343	0.339	0.050	0.114	0.130

	TMG

	10	<0.01	0.113	0.112	0.058	0.057	0.040

Potato – 12.5 g ai/100 kg seed pieces or 0.0125 lb ai/100 lb seed
pieces

Potato 

(U.S. tests)	Clothianidin	19-24 g ai/100 kg seed pieces

(0.33-0.42)	79-143	32	<0.010	0.101	0.086	0.029	0.037	0.026

	TMG

	32	<0.010	<0.010	0.010	0.010	0.010	NA

Potato (Canadian tests)	Clothianidin	12 g ai/100 kg seed pieces 	90	10
<0.020	0.240	0.225	0.050	0.079	0.079

Bulb Vegetables:  proposed use = bulb onion – 0.18 g ai/1000 seed,
green onion – 0.106 g ai/1000 seed

Bulb onion	Clothianidin	0.20

(0.019-0.094)	106-269	12	<0.01	0.017	0.014	0.010	0.011	0.002

	TMG

106-269	12	<0.01	<0.01	<0.01	0.010	0.010	NA

Green onion 	Clothianidin	0.12

(0.028-0.145)	90-153	6	0.013	0.142	0.128	0.068	0.074	0.048

	TMG

90-153	6	<0.01	0.022	0.017	0.012	0.014	0.005

Leafy Greens (Subgroup 4A): proposed uses = head lettuce – 0.8 g
ai/1000 seed, leaf lettuce – 0.64 g ai/1000 seed, spinach -
0.16 g ai/1000 seed)

Head lettuce	Clothianidin	0.792-0.804

(0.027-0.508)	53-143	12	<0.01	0.091	0.082	0.010	0.022	0.028

	TMG

53-143	12	<0.01	0.024	0.023	0.010	0.012	0.005

Leaf lettuce	Clothianidin	0.644-0.654

(0.079-1.41)	45-67	12	0.033	0.349	0.315	0.010	0.085	0.125

	TMG

45-67	12	<0.01	0.155	0.149	0.027	0.042	0.051

Spinach	Clothianidin	0.161

(0.033-0.106)	47-96	12	<0.01	0.078	0.066	0.013	0.026	0.023

	TMG

47-96	12	<0.01	0.021	0.017	0.010	0.011	0.003

Brassica Leafy Vegetables:   proposed uses = broccoli and cabbage - 1.19
g ai/1000 seed, mustard greens - 0.1 g ai/1000 seed

Broccoli	Clothianidin	1.19-1.21

(0.046-0.339)	74-195

74-195	12	<0.01	0.409	0.329	0.010	0.063	0.129

	TMG

	12	<0.01	0.130	0.103	0.010	0.026	0.038

Cabbage	Clothianidin	1.21

(0.046-0.330)	74-177

74-177	12	<0.01	<0.01	<0.01	0.010	0.010	NA

	TMG

	12	<0.01	<0.01	<0.01	0.010	0.010	NA

Mustard greens	Clothianidin	0.100-0.101

(0.015-0.132)	28-62

28-62	10	<0.01	0.011	0.010	0.010	0.010	0.0

	TMG

	10	<0.01	0.024	0.018	0.010	0.013	0.005

Fruiting Vegetables:  proposed use = tomato – 0.1 g ai/1000 seed,
pepper – 0.5 g ai/1000 seed

Tomato	Clothianidin	0.10

(0.0008-0.0038)	112-174	24	<0.01	<0.01	<0.01	0.01	0.01	NA

Bell pepper

0.50

(0.002-0.036)	90-196	12	<0.01	<0.01	<0.01	0.01	0.01	NA

Non-Bell pepper (fresh)

0.50

(0.011-0.016)	119-149	6	<0.01	<0.01	<0.01	0.01	0.01	NA

Non-Bell pepper (dried)

	130-149	6	<0.01	0.013	0.013	0.010	0.011	0.001

Cucurbit Vegetables:  proposed use = 1.0 g ai/1000 seeds

Cucumber	Clothianidin	1.0

(0.005-0.081)	46-53	12	<0.01	<0.01	0.01	0.01	0.01	NA

Muskmelon

1.0

(0.014-0.064)	75-98	12	<0.01	<0.01	0.01	0.01	0.01	NA

Summer squash

1.0

(0.010-0.062)	41-49	10	<0.01	<0.01	0.01	0.01	0.01	NA

Wheat:  proposed use = 70 g ai/100 kg seed

Wheat forage	Clothianidin	125 g ai/100 kg seed 

(0.067-0.171)	31-245	40	<0.01	0.273	0.253	0.076	0.087	0.075

Wheat hay

	56-277	40	<0.01	0.085	0.071	0.011	0.019	0.016

Wheat grain

	86-307	40	<0.01	<0.01	<0.01	0.010	0.010	NA

Wheat straw

	86-307	40	<0.01	0.043	0.040	0.010	0.014	0.009

1	Except for wheat and potatoes, the application rates are expressed in
g ai/1000 seed.  The value in parentheses is the equivalent field use
rates (lb ai/A) which were calculated by the reviewer based on the
planting densities (seeds/A) used in the field trials.  Regardless of
application type (seed, soil or foliar) the label-specified maximum
seasonal use rate for clothianidin is 0.375 lb ai/A.

2	The LOQ is 0.01 ppm.  Residues <LOQ were estimated to be 0.01 ppm for
all calculations.  

3	HAFT = Highest Average Field Trial.

NA= Not applicable

Root Vegetables, Except Sugarbeet (Group 1B)

Thirteen field trials were conducted on carrots (8 tests) and radishes
(5 tests) in the United States in Zones 1, 3, 5, 6, 10 and 11 during
2006-2008.  For each test, clothianidin (3.33 lb/gal FlC) was applied to
seeds at rates of 0.12 g ai/1000 seed for carrots (1x proposed rate) and
0.50 g ai/1000 seed for radishes (1.1x proposed rate).  The formulation
was mixed with water and applied using commercial seed treatment
equipment.  Based on the planting densities (seeds/A) at the field
sites, the equivalent field use rates for clothianidin were 0.023-0.342
lb ai/A for carrots and 0.087-0.429 lb ai/A for radishes.  HED notes
that the maximum seasonal use rate (0.375 lb ai/A) was exceeded at one
of the radish field sites (0.429 lb ai/A).  Single control and duplicate
treated samples of carrot roots and radish roots and tops were harvested
at commercial maturity (BBCH 49), which was at 90-196 days after
planting (DAP) for carrot and 34-60 DAP for radish.  

≥LOQ.  Residues of TMG were <LOD in/on all 16 carrot root samples. 
Average residues were 0.01 ppm for clothianidin and TMG, and the highest
average field trial (HAFT) residues were 0.011 ppm for clothianidin and
<0.01 ppm for TMG.

In the five radish field trials conducted at a 1x rate, clothianidin
residues were <0.010-0.625 ppm in/on 10 root samples and <0.010-0.343
ppm in/on 10 top samples harvested at 34-60 DAP.  Clothianidin residues
were <LOQ in/on 4 root samples and 1 top sample.  Residues of TMG were
<LOQ in/on all radish root samples and were <0.01-0.113 ppm in/on the 10
radish top samples.  Average residues in/on radish roots and tops were,
respectively, 0.124 and 0.114 ppm for clothianidin and 0.010 and 0.057
ppm for TMG.  The HAFT residues in/on root and tops were, respectively,
0.528 and 0.339 ppm for clothianidin and <0.01 and 0.112 ppm for TMG. 
For samples of radish tops having quantifiable residues of both
analytes, the ratio of clothianidin:TMG residues was 1.9x.

Sugar beets

Adequate field trial data are available supporting the existing use for
clothianidin (3.33 lb/gal SE) as a seed treatment for sugar beets (DP#
335355, W. Drew, 10/16/07).  The field trial data support a seed
treatment use rate of 0.132 lb ai/100,000 seeds (0.6 g ai/1000 seeds),
which is higher than the proposed uses on root vegetables (0.45 g
ai/1000 seeds).  The available data support the current 0.02 ppm
tolerance for sugar beet roots. 

Potatoes

U.S. Field Trials:  In sixteen field trials conducted in the United
States in Zones 1, 2, 3, 5, 9, 10 and 11 during 2004-2005, clothianidin
(5 lb/gal FlC) was applied to potato seed pieces at rates of 0.019-0.024
lb ai/100 lb seed pieces (1.6x proposed rate).  Based on the planting
density of the potatoes, these application rates were equivalent to a
field use rate of 0.33-0.42 lb ai/A.  HED notes that the maximum
seasonal use rate (0.375 lb ai/A) was exceeded in eight of the potato
field trials (0.38-0.42 lb ai/A).  Applications were made by spraying or
syringe injection, and the formulation was applied either directly or
after dilution with water; no adjuvants were used.  Single control and
duplicate treated samples of potato tubers were harvested at commercial
maturity (BBCH 49) from each test, which was at 79-143 DAP.  

The sample storage conditions and durations for this study are supported
by the available storage stability data, and residues of clothianidin
and TMG in/on potatoes were determined using an adequate LC-MS/MS method
(Method No. TI-002-P05-001).  The validated LOQ is 0.01 ppm for each
analyte in/on potatoes, and the LOD was 0.002 ppm for each analyte.

Following a seed piece treatment with clothianidin (FlC) to potatoes at
0.019-0.024 lb ai/100 lb of seed pieces (1.6x rate), clothianidin
residues were <0.01-0.101 ppm in/on 32 samples of potato harvested
79-143 DAP.  Residues of TMG were ND (<0.002 ppm) on 29 potato samples
and <LOQ on the remaining 3 potato samples.  Average residues were 0.037
ppm for clothianidin and <0.01 ppm for TMG, and the HAFT residues were
0.086 ppm for clothianidin and <0.01 ppm for TMG.

Canadian Field Trials:  In five field trials conducted in Canada in
Zones 1A and 12 during 2004, clothianidin (5 lb/gal FlC) was applied to
potato seed pieces at rates of 11.8-12.0 g ai/100 kg seed pieces (0.012
lb ai/ 100 lb), which is 1x the proposed use rate.  As planting
densities (lb seed pieces/area) were not reported, the equivalent field
use rate could not be calculated.  For application, the formulation was
diluted with water and applied to seed pieces in plastic bags, and the
bags were then shaken to evenly distribute the test substance.  Single
control and duplicate treated samples of potato tubers were harvested
from each site at commercial maturity, 90 DAP.  At one site, samples
were also harvested at 83, 90, 97, and 103 DAP to assess residue
decline.

The sample storage conditions and durations are supported by the
available storage stability data, and residues of clothianidin in/on
potatoes were determined using an adequate LC-MS/MS method (Bayer Method
00552/M001)  The validated LOQ is 0.01 ppm for clothianidin in/on
potatoes, and the estimated LOD was 0.01 ppm.

Following a seed piece treatment of clothianidin (FlC) to potatoes at
0.012 lb ai/100 lb seed (1x rate), clothianidin residues were <0.02-0.24
ppm in/on 10 samples of potatoes harvested at 90 DAP.  The average
clothianidin residue was 0.079 ppm and the HAFT residue was 0.225 ppm. 
In the residue decline test, clothianidin residues remained relatively
steady at 0.03-0.07 ppm from 83-103 DAP.  Samples were not analyzed for
residues of the TMG metabolite.

Bulb Vegetables (Group 3)

Nine field trials were conducted on bulb onions (6 tests) and green
onions (3 tests) in the United States in Zones 1, 6, 8 10 and 11 during
2006-2007.  For each test, clothianidin (3.33 lb/gal FlC) was applied to
seeds at rates of 0.20 g ai/1000 seed for bulb onions (1.1x proposed
rate) and 0.12 g ai/1000 seed for green onions (1.1x proposed rate). 
The formulation was mixed with water and then applied using commercial
seed treatment equipment.  Based on the planting densities (seeds/A) at
the various field sites, the equivalent field use rates of clothianidin
were 0.019-0.094 lb ai/A for bulb onions and 0.028-0.145 lb ai/A for
green onions.  Single control and duplicate treated samples of bulb and
green onions were harvested at commercial maturity (BBCH 47), which was
at 106-296 DAP for bulb onions and 90-153 DAP for green onions.  

The sample storage conditions and durations are supported by the
available storage stability data, and the residues of clothianidin and
metabolite TMG in/on onions were determined using an adequate LC-MS/MS
method (Method No. TI-002-P05-001).  The validated LOQ is 0.01 ppm for
each analyte, and the LODs are 0.002 ppm for clothianidin and 0.001 ppm
for TMG.

In the six bulb onion field trials conducted at a 1.1x rate,
clothianidin residues were <0.01-0.017 ppm in/on 12 samples harvested at
106-269 DAP, with only one sample having residues >LOQ.  Residues of TMG
were <LOD in/on all samples.  Average residues in/on bulb onions were
0.011 ppm for clothianidin and 0.01 ppm for TMG, and the HAFT residues
were 0.014 ppm for clothianidin and <0.01 ppm for TMG.

In the three green onions field trials conducted at a 1.1x rate,
clothianidin residues were 0.013-0.142 ppm in/on 6 samples harvested at
90-153 DAP.  Residues of TMG were <0.010-0.022 ppm, with one sample
having TMG residues at <LOQ.   Average residues were 0.074 ppm for
clothianidin and 0.014 ppm for TMG, and HAFT residues were 0.128 ppm for
clothianidin and 0.017 ppm for TMG.  In samples with quantifiable
residues of both clothianidin and TMG, the average ratio of
clothianidin:TMG was 6.1x.

Leafy Greens (Subgroup 4A)

A total of 18 field trials were conducted on head lettuce (6 tests),
leaf lettuce (6 tests) and spinach (6 tests) in the United States in
Zones 1, 2, 3, 6, 9 and 10 during 2007.  In each test, clothianidin (56%
WP) was applied to seeds at rates of 0.79-0.80 g ai/1000 seed for head
lettuce (1x rate), 0.64-0.65 g ai/1000 seed for leaf lettuce (1x rate),
and 0.16 g ai/1000 seed for spinach (1x rate).  The formulation was
slurried with water (1:1, w/w) and applied using commercial seed
treatment equipment.  Based on the planting densities (seeds/A) for the
three crops at the various field sites, the equivalent field use rates
for clothianidin were 0.027-0.508 lb ai/A for head lettuce, 0.079-1.41
lb ai/A for leaf lettuce, and 0.033-0.106 lb ai/A for spinach.  HED
notes that the maximum seasonal use rate (0.375 lb ai/A) was exceeded at
one of the head lettuce field sites (0.508 lb ai/A) and at four of the
leaf lettuce field sites (0.435-1.41 lb ai/A).  Single control and
duplicate treated samples of head and leaf lettuce and spinach were
harvested at commercial maturity (BBCH 47-49), which was at 53-143 DAP
for head lettuce, 45-67 DAP for leaf lettuce, and 47-96 DAP for spinach.
 

The sample storage conditions and durations are supported by the
available storage stability data, and the residues of clothianidin and
its metabolite TMG in/on leafy greens were determined using an adequate
LC-MS/MS method (Method No. TI-002-P05-001).  The validated LOQ is 0.01
ppm for each analyte, and the LODs are 0.0026 ppm for clothianidin and
0.0018 ppm for TMG.

In five of the six head lettuce field trials conducted at the 1x rate,
clothianidin and TMG residues were each <LOQ (<0.01 ppm) in/on 10
samples harvested at 53-142 DAP.  However, in one field trial, residues
in/on the two lettuce samples harvested at 143 DAP were 0.091 and 0.072
ppm for clothianidin and 0.024 and 0.022 ppm for TMG.  For the two
samples having quantifiable residues of both analytes, the ratio of
clothianidin:TMG residues was 3.5x.  For all six head lettuce field
trials, average residues were 0.022 ppm for clothianidin and 0.012 ppm
for TMG.  The HAFT residues were 0.082 ppm for clothianidin and 0.023
ppm for TMG.

In the six leaf lettuce field trials conducted at the 1x rate, residues
of clothianidin were 0.033-0.349 ppm in/on 12 samples harvested at 45-67
DAP, and residues of TMG were <0.01-0.155 ppm.  Average residues in/on
leaf lettuce were 0.085 and 0.042 ppm for clothianidin and TMG,
respectively, and HAFT residues were 0.315 and 0.149 ppm for
clothianidin and TMG, respectively.  For samples having quantifiable
residues of both analytes, the average ratio of clothianidin:TMG
residues in leaf lettuce was 4.4x.

 having residues ≥LOQ.  The average TMG residue was 0.011 ppm and HAFT
residue was 0.017 ppm.  In the two samples with quantifiable residues of
both analytes, the ratio of clothianidin:TMG was 4.8x.

Brassica (Cole) Leafy Vegetables (Group 5)

  Samples were stored at ≤-10°C for up to 261-373 days prior to
extraction for analysis.  

The sample storage conditions and durations are supported by the
available storage stability data.  Residues of clothianidin and
metabolite TMG in/on Brassica vegetables were determined using an
adequate LC-MS/MS method (Method No. TI-002-P05-001).  The validated LOQ
is 0.01 ppm for each analyte. The LODs for broccoli are 0.0026 ppm for
clothianidin and 0.0014 ppm for TMG, and the LODs for cabbage and
mustard greens are 0.0022 ppm for clothianidin and 0.0031 ppm for TMG. 

In five of the broccoli field trials conducted at the 1x rate,
clothianidin and TMG residues were each <0.01 ppm in/on 10 samples
harvested at 74-195 DAP.  However, in one field trial, residues in/on
the two broccoli samples harvested at 143 DAP were 0.249 and 0.409 ppm
for clothianidin and 0.076 and 0.130 ppm for TMG.  The ratio of
clothianidin:TMG residues in this field trial was 3.2x.  For all six
field trial, average residues were 0.063 ppm for clothianidin and 0.026
ppm for TMG.  The HAFT residues were 0.329 ppm for clothianidin and
0.103 ppm for TMG.

In the six cabbage field trials conducted at the 1x rate, clothianidin
and TMG residues were <0.01 ppm in/on all 12 samples of cabbage
harvested at 74-177 DAP, and average residues were 0.01 ppm for both
clothianidin and TMG.   

 10 samples having residues ≥LOQ.  Average clothianidin residues were
0.01 ppm and HAFT residues were 0.01 ppm.  Residues of TMG were
<0.01-0.024 ppm, with 4 of the 10 samples having of residues ≥LOQ. 
Average TMG residues were 0.013 ppm and HAFT residues were 0.018 ppm. 
In samples with quantifiable residues of both clothianidin and TMG, the
ratio of clothianidin:TMG was 0.55x.

Fruiting Vegetables, Except Cucurbits (Group 8)

Twenty-one field trials were conducted on tomatoes (12 tests), Bell
peppers (6 tests) and non-Bell peppers (3 tests) in the United States in
Zones 1, 2, 3, 5, 6 and 10 during 2006 and 2007.  For each test,
clothianidin (3.33 lb/gal FlC) was applied to seeds at rates of 0.10 g
ai/1000 seed for tomatoes (1x rate) and 0.50 g ai/1000 seed for peppers
(1x rate).  The formulation was mixed with water and then applied using
commercial seed treatment equipment.  Based on the planting densities
(seeds/A) at the field sites, the equivalent field use rates for
clothianidin were 0.0008-0.0038 lb ai/A for tomatoes, 0.002-0.036 lb
ai/A for Bell peppers, and 0.011-0.016 lb ai/A for non-Bell peppers. 
Single control and duplicate treated samples of each crop of were
harvested at commercial maturity, which was at 112-174 DAP for tomatoes
and 90-196 DAP for peppers.  Additional non-bell pepper samples were
harvested at 130-149 DAP and were allowed to dry for 4-19 days before
sampling.  

The sample storage conditions and durations are supported by the
available storage stability data.  Residues of clothianidin in/on
tomatoes and peppers were determined using an adequate LC-MS/MS method
(Method No. T1-004-P07-01).  The validated LOQ for clothianidin is 0.01
ppm and the LOD is 0.002 ppm for peppers and 0.003 ppm for tomatoes.

For the tests conducted at the 1x rate, clothianidin residues were <LOD
in/on all 24 samples of tomatoes harvested at 112-174 DAP and in/on all
12 samples of Bell peppers harvested at 90-196 DAP.  For non-Bell
peppers, clothianidin residues were <LOQ in/on all 6 samples of fresh
non-bell peppers and in/on 4 of the 6 samples of dried non-Bell peppers.
 Quantifiable residues were found in only 2 dried pepper samples at
0.012 and 0.013 ppm.  The average residues and the HAFT residues were
0.01 ppm for tomatoes, fresh bell peppers, and fresh non-bell peppers. 
For dried non-bell peppers, the average and HAFT residues were 0.011 and
0.013 ppm, respectively.

Cucurbit Vegetables (Group 9)

Seventeen field trials were conducted on cucumbers (6 tests), muskmelons
(6 tests) and summer squash (5 tests) in the United States in Zones 1,
2, 3, 5, 6 and 10 during 2006.  For each test, clothianidin (3.33 lb/gal
FlC) was applied to seeds at a rate of 1.0 g ai/1000 seed (1x rate). 
The formulation was mixed with water and applied using commercial seed
treatment equipment.  Based on the planting densities (seeds/A) at the
various field sites, the equivalent field use rates for clothianidin
were 0.005-0.081 lb ai/A for cucumbers, 0.014-0.064 lb ai/A for
muskmelons, and 0.010-0.062 lb ai/A for summer squash.  Single control
and duplicate treated samples of each crop of were harvested at
commercial maturity, which was at 41-53 DAP for cucumber and summer
squash and at 75-98 DAP for muskmelons.  

The sample storage conditions and durations are supported by the
available storage stability data, and residues of clothianidin in/on
cucurbit vegetables were determined using an adequate LC-MS/MS method
(Method No. T1-004-P07-01).  The validated LOQ for clothianidin is 0.01
ppm and the LOD is 0.002 ppm.

For the 1x rate field trials, clothianidin residues were <0.01 ppm in/on
all 12 samples of muskmelons harvested at 75-98 DAP and all 10 samples
of summer squash harvested at 41-49 DAP.  Residues were also <0.01 ppm
in/on 11 of the 12 cucumber samples harvested at 46-53 DAP.  Only one
cucumber sample had quantifiable residues (0.01 ppm) of clothianidin. 
The average residues and the HAFT residues for clothianidin were 0.01
ppm for cucumbers, muskmelon, and summer squash.

Cereal Grains (Groups 15 and 16) 

Wheat Forage, Wheat Hay, and Wheat Straw

Twenty wheat field trials were conducted in the United States in Zones
2, 4, 5, 6, 7, 8, and 11 during 2005 and 2006 using both spring wheat (8
tests) and winter wheat (12 tests) varieties.  For each trial,
clothianidin (5 lb/gal FlC) was applied to wheat seeds at a rate of
0.125 lb ai/100 lb seed (125 g ai/100 kg); this use rate is 1.8x the
proposed use rate of 70 g ai/100 kg seed.  The formulation was diluted
with water and then applied using commercial seed treatment equipment. 
Based on the seeding rates at the various field sites (717,200-2,015,000
seeds/A), the equivalent field use rates for clothianidin were
0.067-0.171 lb ai/A.  Single control and duplicate treated samples of
each commodity were harvested from each test at the appropriate stage. 
Wheat forage was collected at BBCH 24-36 growth stage (31-245 DAP), and
wheat hay was cut at BBCH 61-85 (56-277 DAP) and allowed to field-dry
for 1-8 days prior to sampling.  Wheat grain and straw were harvested at
normal crop maturity, BBCH 89 (86-307 DAP).  

The sample storage conditions and durations are supported by the
available storage stability data, and residues of clothianidin in/on
wheat commodities were determined using an adequate LC-MS/MS method
(Method No. TI-004-P07-01).  The validated LOQ is 0.01 ppm for
clothianidin in all wheat matrices. The calculated LODs are 0.003 in
forage, 0.002 ppm in grain, and 0.005 ppm in hay and straw.

 40 samples of forage, <0.01-0.085 ppm in/on 40 samples of hay, ≤0.002
ppm in/on all 40 samples of grain, <0.01-0.043 ppm in/on 40 samples of
straw.  Clothianidin residues averaged 0.087 ppm for forage, 0.019 ppm
for hay, <0.01 ppm for grain, and 0.014 ppm for straw.  The HAFT
residues were 0.253 ppm for forage, 0.071 ppm for hay, <0.01 ppm for
grain, and 0.040 ppm for straw. 

Sorghum

Adequate field trial data are available supporting the existing use of
clothianidin (5 lb/gal FlC) as a seed treatment for sorghum at a rate of
0.25 lb ai/100 lb seed or 250 g ai/100 kg seed (DP# D303164, W. Drew,
2/01/06).  The field trial data support the current 0.01 ppm tolerances
for sorghum grain, forage and stover, which were set at the method LOQ.

Corn (field, pop and sweet)

Adequate field corn and sweet corn field trial data are available
supporting the existing use of clothianidin (5 lb/gal FlC) as a seed
treatment for corn at a rate of 1.25 mg ai/seed (DP# D282446, Y.
Donovan, 5/01/03).  This use rate is equivalent to 0.358 lb ai/100 lb
seed or 358 g ai/100 kg seed.  The available field trial data were
conducted at a use rate of 2 mg ai/seed (1.6x rate).  As residues were
<LOQ in/on all grain and C+KWHR samples, the tolerance for these
commodities is set at the LOQ (0.01 ppm).  The tolerances for corn
forage and stover are set at 0.1 ppm.

Conclusions.  The submitted field trial data reflecting seed treatment
applications of clothianidin using WP or FlC formulations are adequate. 
An adequate number of field trials were conducted on the required
representative crops in the appropriate geographic regions.  All tests
were conducted at ~1x the proposed use rates, with the exceptions of the
potato and wheat field trials.   The U.S. potato field trials were
conducted at 1.6x the proposed rate, the Canadian potato field trials
were conducted at 1x the proposed rate, and the wheat field trials were
conducted at 1.8x the proposed rate.  Samples of each RAC from all the
field trials were analyzed using adequate LC-MS/MS methods, and
available storage stability data support the sample storage durations
and conditions.  

As requested by the Agency, samples from the root vegetable, potato,
bulb vegetable, leafy greens, and Brassica vegetable field trials were
also analyzed for the TMG metabolite using an adequate LC-MS/MS method. 
Residues of TMG were <LOQ in all samples of carrots, radish roots,
potatoes, bulb onions and cabbage.  For the crop samples having TMG
residues ≥LOQ, TMG residues levels were compared to clothianidin
residue levels.  The ratios of clothianidin:TMG residues were 3.2x-4.8x
for lettuce, spinach and broccoli, 1.9x for radish tops, 6.1x for green
onions, and 0.6x for mustard greens. (Note: although TMG residue data
will be used for risk assessment, the tolerance for primary crops uses
will continue to include only parent)

The available field trial data will support tolerances of clothianidin
per se at 0.8 ppm for root vegetables, except sugar beet (Subgroup 1B),
0.3 ppm for tuberous and corm vegetables (Subgroup 1C), 0.6 ppm for
leaves of root and tuber vegetables (Group 2), 0.45 ppm for bulb
vegetables (Group 3), 0.7 ppm for leafy greens (Subgroup 4A), 0.4 ppm
for Brassica leafy vegetables (Group 5), 0.01 ppm for fruiting
vegetables (Group 8), and 0.01 ppm for cucurbit vegetables (Group 9). 
The Agency has received a petition for foliar uses of clothianidin on
some of these crops.  Those uses may supersede the tolerances supported
by the seed treatment field trials.  See Section 860.1550 regarding
proposed tolerances.

Based on the all the reviewed field trial data for field corn, sweet
corn, sorghum and wheat, the residue data support a 0.01 ppm tolerance
for clothianidin on cereal grains, Group 15, except rice.  The field
trial data will also support general tolerances for the forage, fodder,
and straw of the cereal grains crop group (Group 16).  The corn and
sorghum field trial data support a tolerance of 0.1 ppm for stover, and
the wheat field trial data support tolerances of 0.35 ppm for forage,
0.07 ppm for hay, and 0.05 ppm for straw.

860.1520 Processed Food and Feed

47483022.der.doc (Potato)

47483023.der.doc (Tomato)

47483024.der.doc (Wheat)

In support of the proposed uses on tuberous and corm vegetables,
fruiting vegetables and wheat, Bayer has submitted processing studies on
potato, tomato, and wheat.  The results of these studies are discussed
below, and the observed processing factors for the various processed
commodities are listed in Table 7.

Potato.  In a field trial conducted in MN during 2004, clothianidin (5
lb/gal FlC) was applied to potatoes as a seed piece treatment at a rate
of 0.095 lb ai/100 lb seed (7.6x proposed rate).  Based on a field
planting rate of 2012 lb seed pieces/acre, this seed treatment rate is
equivalent to a field use rate of 1.91 lb ai/A.  The application was
made using a cement mixer, and no adjuvants were used.  Single control
and treated bulk samples of potatoes were harvested at commercial
maturity (115 DAP) and processed into washed potatoes, cooked potatoes,
flakes, chips, and wet peel using simulated commercial practices.  

Adequate storage stability data are available supporting the sample
storage conditions and durations.  Residues of clothianidin and TMG
in/on potatoes were determined using an adequate LC-MS/MS method (Method
No. TI-002-P05-001).  The validated LOQ is 0.01 ppm for each analyte
in/on potatoes, and the calculated LODs for potatoes and potato
processed fractions are 0.015-0.023 ppm for clothianidin and 0.002-0.015
ppm for TMG.

Average clothianidin residues were 0.176 ppm in/on whole potatoes (RAC),
0.377 ppm in washed potatoes, 0.252 ppm in wet peel, 0.464 ppm in chips,
0.181 ppm in cooked potatoes, and 1.123 ppm in flakes/granules.  Average
TMG residues were <LOQ in whole potatoes and all processed fractions;
therefore, processing factors were not calculated for TMG residues.

The processing factors for clothianidin residues are 1.4x for wet peel,
2.6x for chips, 1.0x for cooked potatoes and 6.3x for potato
flakes/granules.  The theoretical concentration factors for potato
processed fractions are 4.0x for processed waste (wet peel) and 4.7x for
flakes/granules. 

Tomato.  In a field trial conducted in CA during 2006, clothianidin
(3.33 lb/gal FlC) was applied to tomato seeds at a rate of 0.50 g
ai/1000 seed (5x proposed rate).  The formulation was mixed with water
and applied using commercial seed treatment equipment.  Based on the
planting density used for tomatoes in the field trial (29,870 seeds/A),
the equivalent field use rate for clothianidin was 0.033 lb ai/A. 
Single control and treated bulk samples of tomatoes were harvested at
commercial maturity, at 122 DAP, and processed into puree and paste
using simulated commercial practices.  The sample storage conditions and
durations for tomatoes are supported by the available storage stability
data.

Residues of clothianidin in/on tomatoes were determined using an
adequate LC-MS/MS method (Method No. T1-004-P07-01).  The validated LOQ
for clothianidin is 0.01 ppm and the LOD is 0.003 ppm for tomatoes.

Residues of clothianidin were <LOD (<0.003 ppm) in/on tomatoes grown
from seeds treated with clothianidin (FlC) at 0.50 g ai/1000 seeds.  As
residues were non-detectable in the whole fruit (RAC) following
treatment at a 5x rate, samples of paste and puree were not analyzed.

Wheat.  In a field trial conducted in MN during 2006, clothianidin (5
lb/gal FlC) was applied to wheat seeds at a rate of 0.625 lb ai/100 lb
seed (8.9x proposed rate).  The formulation was diluted with water and
applied using commercial seed treatment equipment.  Based on the seeding
rate used in the field trial (926,718 seeds/A), the equivalent field use
rate for clothianidin was 0.462 lb ai/A.  Single control and treated
bulk samples of wheat grain were harvested at normal maturity, at 97
DAP.  

The sample storage conditions and durations are supported by the
available storage stability data.  

Residues of clothianidin in/on wheat grain were determined using an
adequate LC-MS/MS method (Method No. TI-004-P07-01).  The validated LOQ
is 0.01 ppm, and the calculated LOD is 0.002 ppm in grain.

Following a seed treatment of clothianidin at 0.625 lb ai/100 lb seed
(8.9x rate), residues of clothianidin were nondetectable (<0.002 ppm)
in/on grain harvested at normal crop maturity.  As residues in/on grain
were <LOD following a 8.9x application, the grain was not processed in
wheat bran, flour, middlings, shorts, and germ.

≥5x use rate.

Conclusions.  The submitted potato, tomato, and wheat processing studies
are adequate.  Because residues were <LOQ in/on the tomato and wheat
grain RACs following a seed treatment at ≥5x the proposed use rate,
tolerances for processed tomato and wheat commodities are not required.

Based on the HAFT residues for potatoes from the Canadian trials (0.225
ppm) and the processing factors for wet peel (1.4x), chips (2.6x) and
flakes/granules (4.7x; theoretical), the maximum expected clothianidin
residues are 0.32 ppm in wet peel, 0.58 ppm in chips and 1.1 ppm in
flakes/granules.  A separate tolerance is not required for wet peel, as
the maximum expected residues are below the recommended tolerance. 
However, separate tolerances are required for potato chips at 0.6 ppm
and potato flakes/granules at 1.5 ppm.  These values are harmonized with
Canadian MRLs for potato.

  SEQ CHAPTER \h \r 1 860.1650 Submittal of Analytical Reference
Standards

An analytical standard for clothianidin, with an expiration date of
12/14/2013, is currently available in the EPA National Pesticide
Standards Repository (personal communication with Dallas Wright, ACB,
9/15/08).

860.1850 Confined Accumulation in Rotational Crops

DP# D282446, Y. Donovan, 5/1/03

An adequate confined rotational crop study is available and was reviewed
in conjunction with the petition for use on canola and corn (DP#
D282446).  Rotational crops of turnips, Swiss chard, and wheat were
planted approximately 1, 5, and 10 months following a single soil
application of [14C]-clothianidin at the rate of 0.293 lb ai/A (0.8x
maximum proposed seasonal rate) and samples of the appropriate RACs were
harvested at maturity.  The metabolism of clothianidin in rotational
crops was similar to the primary crops and the MARC concluded that
parent, TZNG and MNG are the residues of concern in rotational crops and
that only parent needs to be included in the tolerance expression.  

  SEQ CHAPTER \h \r 1 860.1900 Field Accumulation in Rotational Crops

DP# D282446, Y. Donovan, 5/1/03

47524001.der.doc (soybeans)

Limited field rotational crop studies are available and were reviewed in
conjunction with the petition for seed treatment uses on canola and corn
(DP# D282446).  In these studies, 10-11 trials were conducted in which
mustard greens, turnips, and wheat were planted 1, 4, 8, and 12 months
following a single seed treatment to corn at rates equivalent to 0.144
to 0.171 lb ai/A.  

Based on the residue data from these field rotational crop field trails,
tolerances were established for clothianidin residues at 0.02 ppm in/on
non-grass animal feeds (Group 18), the forage, fodder and straw of
cereal grains (Group 16), grass forage, fodder and hay (Group 17), and
soybean forage and hay.  These tolerances and the previously reviewed
rotational crop residue data supported rotational crop restrictions of
30 days for the above crop/crop groups and a 1-year restriction for any
other crops without registered clothianidin uses.

However, the proposed label for the 56% WP formulation allows for a
maximum seasonal use rate of up to 0.375 lb ai/A, which is 2.2-2.6x
higher then the rates previously used to generate the limited field
trial data.

The rotational crop restrictions on the proposed label specify that
areas planted with treated seed may be immediately replanted with
cotton, canola, rapeseed, sorghum, sugar beets, potato, cereal grains
(except rice), root vegetables (Group 1), bulb vegetables (Group 3),
leafy greens (Subgroup 4A), Brassica vegetables (Group 5), fruiting
vegetables (Group 8), and cucurbit vegetables (Group 9).  These areas
may also be replanted after 30 days with soybeans, dried beans or dried
peas.  Other crops cannot be planted for at least one year after the
treated seeds are planted.   

HED notes that all the crops or crop groups for which immediate
replanting is allowed have proposed or existing uses and tolerances for
clothianidin.  The only crops without registered uses that have a PBI of
<1 year are soybeans, dried beans and peas.

In order to support a 30-day PBI for soybeans following application of
clothianidin at rates up to 0.375 lb ai/A (420 g ai/ha), Bayer has
submitted a new field rotational crop study examining residues of
clothianidin and TZNG in/on rotated soybean commodities from a 30-day
PBI.  

In six field rotational crop trails conducted in Zones 2, 4, and 5
during 2005, clothianidin (5 lb/gal FlC) was applied as a single
broadcast soil application at 0.370-0.385 lb ai/A (1x maximum seasonal
rate) to fields typically used for growing potatoes. The applications
were made using ground equipment and no adjuvants were used.  A
rotational crop of soybeans was planted at each site 26-30 days after
treatment, and was grown according to standard agricultural practices.

Single control and duplicate treated samples of soybean forage, hay,
immature seeds (with and without pods), and mature seeds were collected
from each test.  Forage samples were collected at 36-65 DAP.  Hay was
cut at 46-94 DAP (BBCH 65-75) and allowed to field dry for 3-14 days
prior to collection.  Immature seed samples were collected at 78-102
DAP, and mature seed samples were collected at 104-120 DAP.  Samples
were stored frozen for 419-526 days prior to analysis.  Adequate data
are available supporting the stability of clothianidin in frozen soybean
matrices for these storage intervals; however, the available storage
stability data for TZNG are insufficient to support the storage
intervals from the current field trials.

Samples were analyzed for residues of clothianidin and its metabolite
TZNG using an adequate LC-MS/MS method, which is a modified version of
Bayer Method 00552/M001.  The validated LOQ was 0.01 ppm for
clothianidin and TZNG (expressed as parent) in each soybean matrix.  The
LODs for clothianidin residues were 0.003 ppm for hay and mature seed,
and 0.002 ppm for forage and immature seeds (with and without pods). 
The LODs for TZNG residues were 0.004 ppm for immature seed with pod,
0.003 ppm for hay, 0.002 ppm for immature seed without pod, and 0.001
ppm for forage and mature seed.

At PBIs of 26-30 days following a single soil application of
clothianidin at 0.370-0.385 lb ai/A (1x rate), residues of clothianidin
and TZNG were each <LOQ (<0.01 ppm) in/on 12 samples each of soybean
forage, immature seeds (with and without pods), and mature seeds.   For
the 12 hay samples, residues of clothianidin and TZNG were also <LOQ,
except in 1 sample having quantifiable residues of clothianidin at 0.011
ppm and 3 samples having residues of TZNG at 0.012-0.015 ppm.  Average
residues of clothianidin and TZNG were each 0.01 ppm in/on soybean
forage, immature and mature seeds.  For hay, average residues were 0.01
ppm for clothianidin and 0.011 ppm for TZNG.  The HAFT residues for
clothianidin and TZNG were <0.01 ppm in forage and immature and mature
seeds, and HAFT residues for hay were <0.01 ppm for clothianidin and
0.014 ppm for TZNG.

Conclusions.  Provided that acceptable supporting storage stability data
are submitted for metabolite TZNG, the submitted soybean rotational crop
field trials are adequate.  The data support a 30-day PBI for soybeans,
dried beans and dried peas following clothianidin applications up to
0.375 lb ai/A.  The data also indicate that the existing rotational crop
tolerances of 0.02 ppm for soybean forage and hay are adequate and that
rotational crop tolerances are not required for seeds of soybeans or
dried beans and peas.  In addition, the rotational crop restrictions
specified on the label for the proposed 56% WP are adequate.  

The available residue data on clothianidin and TZNG from the field
rotational crop studies will be used for risk assessment.  If levels of
the metabolite MNG are needed for risk assessment, MNG residues will be
estimated using ratios from the confined rotational crop study.

860.1550 Proposed Tolerances

For purposes of setting tolerances, the Agency has determined that only
clothianidin needs to be included in the tolerance expression for both
primary and rotational crops and for animal commodities.  The submitted
data for the metabolite TMG will not be included in the tolerance
expression, but will be used for risk assessment.  The proposed and
recommended tolerances for this petition are listed in Table 8.  The
tolerance expression for clothianidin should be revised to be as
follows:  

Tolerances are established for residues of the insecticide clothianidin,
including its metabolites and degradates, in or on the commodities in
the table below as a result of the application of clothianidin. 
Compliance with the tolerance levels specified below is to be determined
by measuring only clothianidin
[(E)-N-[(2-Chloro-5-thiazolyl)methyl]-N’-methyl-N”-nitroguanidine]
in or on the commodity.

The recommended tolerances for the root vegetables, except sugar beet
(Subgroup 1B), tuberous and corm vegetables (Subgroup 1C), leaves of
root and tuber vegetables (Group 2), bulb vegetables (Group 3), leafy
greens, except Brassica (Subgroup 4A) and wheat forage, hay and straw
were determined using the Agency’s SOP “Guidelines for Setting
Pesticide Tolerances Based on Field Trial Data” and the tolerance
harmonization spreadsheet (Appendix I).  Calculating recommended
tolerances for each of the representative crops separately, the
recommended tolerances are 0.8 ppm for the root vegetables (Subgroup
1B), 0.3 ppm for the tuberous and corm vegetables (Subgroup 1C), 0.6 ppm
for leaves of root and tuber vegetables (Group 2), 0.45 ppm for bulb
vegetables (Group 3), 0.7 ppm for leafy greens, except Brassica
(Subgroup 4A), 0.35 ppm for wheat forage, 0.07 ppm for wheat hay and
0.05 ppm for wheat straw.

The tolerance spreadsheet could not be used to calculate recommended
tolerances for the Brassica leafy vegetables (Group 5), fruiting
vegetables (Group 8), cucurbit vegetables (Group 9) or wheat grain as
clothianidin residues were <LOQ in/on the majority of the samples from
these crops/commodities.  For the Brassica leafy vegetables (broccoli,
cabbage and mustard greens), clothianidin residues were <LOQ in/on all
cabbage samples and <LOQ in/on ≥80% of the broccoli and mustard greens
samples.  Therefore, the recommended tolerance of 0.4 ppm is based on
the maximum observed residue value from all three crops.  For fruiting
and cucurbit vegetables and wheat grain, clothianidin residues were <LOQ
in/on all samples; therefore, the recommended tolerances equal the
method LOQ of 0.01 ppm.

Bayer is proposing a crop group tolerance on cereal grains, except rice.
 In that clothianidin residues were <0.01 ppm in/on all samples of wheat
grain from the current field trials and in/on all grain samples from the
field corn and sorghum field trials from earlier petitions, the
available data will support the proposed 0.01 ppm tolerance for cereal
grains, except rice.  

There are currently separate tolerances for corn forages (sweet and
field) and stovers (field, sweet and pop) and for sorghum forage and
stover, and Bayer is now proposing separate tolerances for wheat forage,
hay and straw.  However, because the proposed seed treatment use is for
all cereal grains, except rice, the appropriate crop group tolerances
should be established to cover forage and fodders of all cereal grain
crops.  The available residue data on wheat forage, hay and straw, corn
forage and stover, and sorghum forage and stover will support
establishing crop group tolerances for cereal grain forage, fodder and
straw.  The residue data from wheat forage, hay and straw will support
tolerances of 0.35 ppm for cereal grain forage, 0.07 ppm for cereal
grain hay, and 0.05 ppm for cereal grain straw, and the existing residue
data on field corn stover and sorghum stover will support a tolerance of
0.1 for cereal grain stover.  Once the cereal grain crop group
tolerances are established, the separate tolerances on corn grain (field
and pop), corn forage (sweet and field), corn stover (field, sweet and
pop) and sorghum grain, forage and stover can be deleted.  HED also
notes that with the establishment of direct tolerances on the cereal
grain forage, fodder and straw group, the 0.02 ppm tolerance for
inadvertent residues on the cereal grain forage, fodder and straw group
can be deleted.

HED notes that tolerances for clothianidin on leafy vegetables, except
Brassica (Group 4), Brassica leafy vegetables (Group 5), fruiting
vegetables (Group 8) and cucurbit vegetables (Group 9) are currently
pending under another petition (PP# 8F7395, DP# 355896, under review)
supporting the use of foliar applications of clothianidin on the above
crop groups.  As these tolerances are higher than the tolerances being
proposed by Bayer, they will supersede Bayer’s proposed tolerances if
they are approved.

≥5x the proposed use rate.  For potatoes, clothianidin residues were
shown to concentrate in wet peel (1.4x), chips (2.6x) and
flakes/granules (6.3x; 4.7x theoretical).  Based on the HAFT residues of
0.225 ppm for potatoes and the processing factors, the maximum expected
clothianidin residues are 0.32 ppm in wet peel, 0.58 ppm in chips and
1.1 ppm in flakes/granules.  A separate tolerance is not required for
wet peel, as the maximum expected residue is below the recommended
tolerance.  However, separate tolerances are required for potato chips
at 0.6 ppm and potato flakes/granules at 1.5 ppm.  These values are
harmonized with Canadian MRLs for potato.  

Because the proposed uses will not increase the dietary exposure of
livestock to clothianidin residues, the current 0.01 ppm tolerance for
milk is adequate and tolerances are not required for eggs or fat, meat,
and meat byproducts of cattle, goats, hogs, horses, sheep and poultry.

Except for potatoes, corn grains (field, pop) and peach/stone fruit (not
in subject petitions) there are currently no established or proposed
Codex, Canadian, or Mexican maximum residue limits (MRLs) for
clothianidin on the requested crops/crop groups.  For potato and
peach/stone fruit commodities, HED’s recommended tolerances are in
accord with established/recommended Canadian MRLs.  Therefore,
harmonization with international MRLs is not an issue with this
petition.  An International Residue Limit Status Sheet is attached.

Table 8. 	Tolerance Summary for Clothianidin

Commodity	Proposed Tolerance (ppm)	Recommended Tolerance (ppm) 1
Comments; 

Correct Commodity Definition

Vegetable, root, except sugar beet, Subgroup 1B	0.6	0.8	Adequate seed
treatment data are available on carrot and radish roots.

Vegetable, tuberous and corm, Subgroup 1C 	0.2	0.3	Adequate seed
treatment data are available on potato.  The recommended tolerance is in
accord with the current Canadian MRL.

Vegetable, leaves of root and tubers, Group 2	None	0.6	Adequate seed
treatment data are available on radish tops.

Vegetable, bulb, Group 3	0.2	0.45	Adequate data seed treatment data are
available on bulb and green onions.

Vegetable, bulb, Group 3-07

Vegetable, leafy greens, except Brassica, Subgroup 4A	1.1	0.7 2

(3.0)	Adequate seed treatment data are available on lettuce (head and
leaf), and spinach.

Vegetable, Brassica, leafy, Group 5	0.35	0.4 2,3

(1.9)	Adequate seed treatment data are available on broccoli, cabbage,
and mustard greens.

Vegetable, fruiting, Group 8	0.01	0.01 2,4

(0.20)	Adequate seed treatment data are available on tomatoes and
peppers.  Residues were <LOQ in/on all pepper and tomato samples.

Vegetable, cucurbit, Group 9	0.01	0.01 2,4

(0.06)	Adequate seed treatment data are available on cucumbers,
muskmelons and summer squash. Residues were <LOQ in/on all samples of
each crop.

Grain, cereal, except rice, Group 15	0.01	0.01 4	Adequate residue data
are available on grain from corn, sorghum and wheat.  Residues were <LOQ
in/on all samples of each crop.

Wheat, forage	0.35	None	Tolerances for wheat commodities will be covered
under the general tolerances for cereal grain forage, fodder and hay.

Wheat, hay	0.07	None

	Wheat, straw	0.04	None

	Grain, cereal, forage, fodder and hay, Group 16, forage	None	0.35
Considering the available wheat, corn and sorghum field trial data, the
tolerance was calculated using the spreadsheet and the data on wheat
forage.  Separate tolerances for corn and sorghum forage may be deleted.

Grain, cereal, forage, fodder and hay, Group 16, hay	None	0.07	The
tolerance was calculated using the tolerance spreadsheet and the wheat
hay residue data.

Grain, cereal, forage, fodder and hay, Group 16, stover	None	0.1	The
tolerance is based on the existing field corn and sorghum field trial
data, and replaces separate tolerances on corn and sorghum stover.

Grain, cereal, forage, fodder and hay, Group 16, straw	None	0.05	The
tolerance was calculated using the tolerance spreadsheet and the wheat
straw residue data.

Potato, chips	None	0.6	Values are in accord with Canadian Maximum
Residue Limits (MRLs).

Potato, flakes	None	1.5

	1	Tolerances were calculated using the tolerance harmonization
spreadsheet unless otherwise indicated.

2	Higher tolerances (in parentheses) for these crop groups are currently
pending under another petition for foliar application uses (PP# 8F7395,
DP# 355896, under review).

3	Due to residues being <LOQ in/on most samples (≥80%), the tolerance
was assessed based on the maximum observed residue value.

4	Tolerance is based on the method LOQ (0.01 ppm) as residues were <LOQ
in all samples. 

References

DP Number:	D282446

Subject:	PP# 1F06315. TI-435 (Clothianidin) on Corn and Canola.  Summary
of Analytical Chemistry and Residue Data.

From:		Y. Donovan

To:		D. Kenny/M. Laws

Dated:		5/01/03

MRID(s):	45422527-35, 45422305-06, and 45422610-19

DP Number:	D287182

Subject:	Clothianidin.  Petition for the Permanent Tolerances for the
Uses on Apples and Pears and for the Use on Tobacco.  Summary of
Analytical Chemistry and Residue Data.  Petition Number 1F6342.

From:		W. Cutchin

To:		W. Cutchin

Dated:		7/13/04

MRID(s):	46027101, 45480402, 45480403

DP Numbers:	 D303164, D309473, D309474, D312449, D314533, and D318496

Subject:	Clothianidin.  Tolerance Petition Requesting Food Use of the
Insecticide Clothianidin on Grapes, Potatoes, Sorghum, and Cotton
(Section 3 Registration).  Summary of Analytical Chemistry and Residue
Data.

From:		W. Drew

To:		K. Davis/D. Kenny

Dated:		2/1/06

MRID(s):	46346801, 46346802, 46357301, 46357302, 46144901, 46144901,
46482308, 46482309 

DP Number:	D35355

Subject:	Clothianidin.  Tolerance Petition Requesting the Establishment
of Permanent Tolerances (Associated with Section 3 Registration) for
Food/Feed Use of the Insecticide as a Seed Treatment on Sugar Beets. 
Resolution of Rotational Crop Data Deficiency.  Summary of Analytical
Chemistry and Residue Data.  

From:		W. Drew

To:		K. Davis/V. Eagle

Dated:		10/16/2007

MRID(s):	47007809, 47007810, 46826901

DP Number:	355896 and 360842

Subject:	Clothianidin; Petitions for Tolerances and Uses on Berries
Subgroup 13-07H, Brassica Vegetables, Cotton, Cucurbit Vegetables,
Fruiting Vegetables, Leafy Vegetables, Peaches, Soybeans, and Tree Nuts.
 Summary of Analytical Chemistry and Residue Data.

From:		

To:		

Dated:		

MRID(s):	47471601-47471616, and 47578101-47578103

  SEQ CHAPTER \h \r 1 Attachments:  

International Residue Limit Status sheet

Appendix I - Tolerance Assessment Calculations

INTERNATIONAL RESIDUE LIMIT STATUS

Chemical Name:
(E)-N-[(2-Chloro-5-thiazolyl)methyl]-N’-methyl-N”-nitroguanidine
Common Name: Clothianidin	X Proposed tolerances

 Reevaluated tolerance

 Other	Date: 4/25/09

Codex Status (Maximum Residue Limits)	U. S. Tolerances

X No Codex proposal step 6 or above

 No Codex proposal step 6 or above for the crops requested 	Petition
Numbers: 8F7413 and 8F7416

DP Numbers: 357455 and 357454

Other Identifier: PC Code 044309

Residue definition (step 8/CXL):  NA	Reviewer/Branch: C. Swartz/RAB2

	Residue definition: Clothianidin

Crop (s)1	MRL (mg/kg)	Crop(s) 	Recommended Tolerance (ppm)

Vegetable, root, except sugar beet, Subgroup 1B	0.8

Vegetable, tuberous and corm, Subgroup 1C 	0.3

Leaves of root and tuber vegetables, Group 2	0.6

Vegetable, bulb, Group 3	0.45

Vegetable, leafy greens, Subgroup 4A	0.7

Vegetable, brassica, leafy, Group 5	0.4

Vegetable, fruiting, Group 8	0.01

Vegetable, cucurbits, Group 9	0.01

Grain, cereal, except rice, Group 15	0.01

Grain, cereal, forage, fodder and hay, Group 16, forage	0.35

Grain, cereal, forage, fodder and hay, Group 16, hay	0.07

Grain, cereal, forage, fodder and hay, Group 16, stover	0.10

Grain, cereal, forage, fodder and hay, Group 16, straw	0.05

Limits for Canada	Limits for Mexico

( No Limits

( No Limits for the crops requested	X  No Limits

(   No Limits for the crops requested

Residue definition: Clothianidin	Residue definition:  NA

Crop(s)	MRL (mg/kg)	Crop(s)	MRL (mg/kg)

  SEQ CHAPTER \h \r 1 Field corn grain	0.01

Popcorn grain	0.01

Rapeseed (canola)	0.01

Sweet corn kernel plus cob with husk removed	0.01

Milk	0.01

Notes/Special Instructions:  Potato commodities were recently given MRLs
by Canada, as follows:  Tubers (0.3 ppm), chips (0.6 ppm), and
granules/flakes (1.5 ppm).  PMRA (Canada) is currently reviewing a
petition to establish tolerances on stone fruit, which includes peaches.

Appendix I.  Tolerance Assessment Calculations.

For each of the crops/crop groups listed below, the Guidance for Setting
Pesticide Tolerances Based on Field Trial Data (SOP), along with the
tolerance spreadsheet, was used for calculating recommended tolerances. 
As specified in the SOP, the minimum of the 95% upper confidence limit
(UCL) on the 95th percentile and the point estimate of the 99th
percentile was selected as the tolerance value in cases when the dataset
was large (greater than 15 samples) and reasonably lognormal.  For
datasets that were small (≤15 samples) and reasonably lognormal, the
upper bound estimate of the 95th percentile based on the median residue
value was compared to the minimum of the 95% UCL on the 95th percentile
and the point estimate of the 99th percentile, and the minimum value was
selected as the tolerance value.  For datasets that were not lognormal,
the upper bound on the 89th percentile was selected as the tolerance
value (distribution-free method).  The rounding procedures specified in
the SOP were also used.

Root Vegetables, Except Sugarbeet, Subgroup 1B

The datasets used to establish a tolerance for clothianidin on the root
vegetables, except sugar beets (Subgroup 1B) consisted of field trial
data for the representative crops carrots and radishes. The seed
application rates were 0.12 g ai/1000 seed for carrots and 0.50 g
ai/1000 seed for radishes.  As specified by the SOP, the field trial
application rates are within 25% of the maximum label application rate. 
The residue values used to calculate the tolerance are provided in Table
I-1.

Because all but one (0.011 ppm) of the residues values for carrots were
<LOQ (<0.01 ppm), the tolerance harmonization spreadsheet could not be
used to calculate a recommended tolerance (Table I-1).  The maximum
likelihood estimation (MLE) procedures were needed to impute censored
values for radish roots because field trial sample results were below
LOQ for 4 of 12 samples.  The carrot and radish datasets were relatively
small (12-16 samples each).  The dataset for radish was entered into the
tolerance spreadsheet.  Visual inspection of the lognormal probability
plots for radish roots (Figure I-1) provided in the spreadsheet
indicated that the radish root dataset is not reasonably lognormal.  The
results from the approximate Shapiro-Francia test statistic (Figure I-2)
confirmed that the assumption of lognormality should be rejected for
radish. 

Using the tolerance spreadsheet, the recommended tolerance is 0.80 ppm
for radish roots.  The maximum residue value (0.011 ppm) was used to
determine a recommended carrot tolerance of 0.02 ppm.  Although the
recommended tolerances for radish and carrot roots differed by more than
5x, tolerances for both crops are quite low; therefore, a crop Subgroup
tolerance is considered appropriate for root vegetables, except
sugarbeet (Subgroup 1B).  The recommended value is 0.8 ppm, based on
radish.

Table I-1.	Residue data used to calculate tolerance for Clothianidin on
Root Vegetables.

Regulator:	EPA	EPA

Chemical:	Clothianidin	Clothianidin

Crop:	Carrot	Radish Roots (MLE)

PHI:	90-196 days 	34-60 days 

App. Rate:	0.12 g ai/1000 seed	0.5 g ai/1000 seed

Submitter:	Bayer CropScience	Bayer CropScience

MRID Citation:	MRID 47483014	MRID 47483014

	Residues of Clothianidin (ppm)

	0.010	0.016

	0.010	0.016

	0.010	0.036

	0.010	0.076

	0.010	0.010

	0.010	0.010

	0.010	0.010

	0.010	0.010

	0.010	0.625

	0.010	0.431

	0.010

0.010

0.010

0.010

0.010

0.011

	1	Residue values <LOQ (0.01 ppm) are listed in bold.

Figure I-1.  Lognormal probability plot of Clothianidin field trial
data for Radish Roots.

Figure I-2.   Tolerance spreadsheet summary of Clothianidin field trial
data for Radish Roots.

Leaves of Root Vegetables, Except Sugarbeet, Crop Group 2 

The datasets used to establish a tolerance for clothianidin on the
leaves of root vegetables crop group consisted of field trial data for
radish tops (the representative crop of leaves of root vegetables), and
represented a seed application rate of 0.50 g ai/1000 seed.  As
specified by the SOP, the field trial application rates are within 25%
of the maximum label application rate.  The residue values used to
calculate the tolerance are provided in Table I-2.

The radish dataset was relatively small (12 samples) and entered into
the tolerance spreadsheet. Visual inspection of the lognormal
probability plots for radish tops (Figure I-3) provided in the
spreadsheet indicated that the radish dataset were reasonably lognormal.
 The results from the approximate Shapiro-Francia test statistic (Figure
I-4) confirmed that the assumption of lognormality should not be
rejected for radish. 

Using the tolerance spreadsheet, the recommended value is 0.60 ppm for
radish tops.  The crop group tolerance is considered appropriate for
leaves of root vegetables (Group 2).  

Table I-2.	Residue data used to calculate tolerance for Clothianidin on
Leaves of Root Vegetables.

Regulator:	EPA

Chemical:	Clothianidin

Crop:	Radish Tops

PHI:	34-60 days 

App. Rate:	0.5 g ai/1000 seed

Submitter:	Bayer CropScience

MRID Citation:	MRID 47483014

	Residues of Clothianidin (ppm)

	0.010

	0.010

	0.011

	0.034

	0.036

	0.063

	0.122

	0.171

	0.335

	0.343

	0.360

	0.490

1	Residue values <LOQ (0.01 ppm) are listed in bold.

Figure I-3.  Lognormal probability plot of Clothianidin field trial data
for Radish Tops.

Figure I-4.   Tolerance spreadsheet summary of Clothianidin field trial
data for Radish Tops.

Tuberous and Corm Vegetables, Subgroup 1C 

The datasets used to establish a tolerance for clothianidin on the
tuberous and corm vegetables crop group consisted of field trial data
for potatoes (the representative crop of tuberous and corm vegetables),
representing seed application rates of 19-24 g ai/ 100 kg seed pieces. 
Although this application rate is 1.6x the proposed application rate of
12.5 g ai/100 kg seed, the residue data were used to assess a
recommended tolerance.  The residue values used to calculate the
tolerance are provided in Table I-3.

The potato dataset was not small (32 samples) and entered into the
tolerance spreadsheet (Table I-3).  Visual inspection of the lognormal
probability plots for potato tubers (Figure I-5) provided in the
spreadsheet indicated that the potato dataset were reasonably lognormal.
 The results from the approximate Shapiro-Francia test statistic (Figure
I-6) confirmed that the assumption of lognormality should not be
rejected for potato tubers. 

Using the tolerance spreadsheet, the recommended value is 0.15 ppm for
potato tubers.

The crop group tolerance based on potato tubers is considered
appropriate for tuberous and corm vegetables (Subgroup 1C).  

Table I-3.	Residue data used to calculate tolerance for Clothianidin on
Tuberous and Corm Vegetables.

Regulator:	EPA

Chemical:	Clothianidin

Crop:	Potato

PHI:	79-143 days 

App. Rate:	19-24 g ai/100 kg seed pieces

Submitter:	Bayer CropScience

MRID Citation:	MRID 47483012

	Residues of Clothianidin (ppm)

	0.010	0.029

	0.010	0.030

	0.010	0.035

	0.010	0.037

	0.012	0.043

	0.013	0.043

	0.015	0.048

	0.016	0.056

	0.018	0.057

	0.019	0.058

	0.020	0.060

	0.020	0.071

	0.020	0.077

	0.022	0.085

	0.028	0.092

	0.028	0.101

1	Residue values <LOQ (0.01 ppm) are listed in bold.

Figure I-5.  Lognormal probability plot of Clothianidin field trial data
for Potato Tubers.

Figure I-6.   Tolerance spreadsheet summary of Clothianidin field trial
data for Potato Tubers.

Bulb Vegetables, Crop Group 3

The datasets used to establish a tolerance for clothianidin on the bulb
vegetables crop group consisted of field trial data for bulb onion and
green onion (the representative crops of bulb vegetables), and
represented seed application rates of 0.20 g ai/1000 seed for bulb
onions and 0.12 g ai/1000 seed for green onions.  As specified by the
SOP, the field trial application rates are within 25% of the maximum
label application rate.  The residue values used to calculate the
tolerance are provided in Table I-4.

Because all but one (0.01 ppm) of the residues values for bulb onion
were <LOQ (<0.01 ppm), the tolerance harmonization spreadsheet could not
be used to calculate a recommended tolerance (Table I-4).  The bulb
onion and green onion datasets were both relatively small (6- samples
each).  The dataset for green onion was entered into the tolerance
spreadsheet.  Visual inspection of the lognormal probability plots for
radish roots (Figure I-7) provided in the spreadsheet indicated that the
green onion dataset were reasonably lognormal.  The results from the
approximate Shapiro-Francia test statistic (Figure I-8) confirmed that
the assumption of lognormality should not be rejected for green onion. 

Using the tolerance spreadsheet, the recommended tolerance is 0.45 ppm
for green onion.  The maximum residue value (0.017 ppm) was used to
assess a recommended tolerance of 0.025 ppm for bulb onions.  Although
the recommended tolerances for bulb and green onions differed by more
than 5x, tolerances for both crops are quite low; therefore, a crop
group tolerance is considered appropriate for bulb vegetables.  Based on
the green onion residue data, the recommended tolerance for bulb
vegetables is 0.45 ppm. 

Table I-4.	Residue data used to calculate tolerance for Clothianidin on
Bulb Vegetables.

Regulator:	EPA	EPA

Chemical:	Clothianidin	Clothianidin

Crop:	Bulb Onion	Green Onion

PHI:	106-269 days 	90-153 days 

App. Rate:	0.20 g ai/1000 seed	0.12 g ai/1000 seed

Submitter:	Bayer CropScience	Bayer CropScience

MRID Citation:	MRID 47483015	MRID 47483015

	Residues of Clothianidin (ppm)

	0.01	0.013

	0.01	0.038

	0.01	0.062

	0.01	0.073

	0.01	0.113

	0.01	0.142

	0.01

0.01

0.01

0.01

0.01

0.017

	1	Residue values <LOQ (0.01 ppm) are listed in bold.

Figure I-7.  Lognormal probability plot of Clothianidin field trial
data for Green Onion.

Figure I-8.   Tolerance spreadsheet summary of Clothianidin field trial
data for Green Onion.

Leafy greens, except Brassica, Subgroup 4A

The datasets used to establish a tolerance for clothianidin on the leafy
greens Subgroup 4A consisted of field trial data for head lettuce, leaf
lettuce, and spinach (the representative crops of leafy greens) and
represented seed application rates of 0.8 g ai/1000 seed for head
lettuce, 0.65 g ai/1000 seed for leaf lettuce, and 0.16 g ai/1000 seed
for spinach.  As specified by the SOP, the field trial application rates
are within 25% of the maximum label application rate.  The residue
values used to calculate the recommended tolerances are provided in
Table I-5.

Because all but two (0.072-0.091 ppm) of the residues values for head
lettuce were <LOQ (<0.01 ppm), the tolerance harmonization spreadsheet
could not be used to calculate a recommended tolerance (Table I-5).  The
maximum likelihood estimation (MLE) procedures were needed to impute
censored values for spinach because field trial sample results were
below LOQ for 2 of 12 samples.  The head lettuce, leaf lettuce, and
spinach datasets were relatively small (12 samples each).  The dataset
for leaf lettuce and spinach were entered into the tolerance
spreadsheet.  Visual inspection of the lognormal probability plots for
leaf lettuce and spinach (Figures I-9 and I-11, respectively) provided
in the spreadsheet indicated that the leaf lettuce and spinach datasets
were reasonably lognormal.  The results from the approximate
Shapiro-Francia test statistic (Figures I-10 and I-12, respectively)
confirmed that the assumption of lognormality should not be rejected for
leaf lettuce and spinach.  

Using the tolerance spreadsheet, the recommended tolerances are 0.70 ppm
for leaf lettuce and 0.08 ppm for spinach.  Based on the maximum residue
value of 0.091 ppm for head lettuce, the recommended tolerance for head
lettuce would be 0.10 ppm.  Although the recommended tolerances for
lettuce and spinach differed by more than 5x, tolerances for all three
crops are quite low; therefore, a crop group tolerance is considered
appropriate for leafy greens Subgroup 4A.  

The recommended value is 0.70 ppm, which is the highest of the
recommended tolerances on the individual crops.

Table I-5.	Residue data used to calculate tolerance for Clothianidin on
Leafy Vegetables.

Regulator:	EPA	EPA	EPA

Chemical:	Clothianidin	Clothianidin	Clothianidin

Crop:	Head Lettuce	Leaf Lettuce	Spinach (MLE)

PHI:	53-143 days 	45-67 days 	47-96 days 

App. Rate:	0.79-0.80 g ai/1000 seed	0.64-0.65 g ai/1000 seed	0.16 g
ai/1000 seed

Submitter:	Bayer CropScience	Bayer CropScience	Bayer CropScience

MRID Citation:	MRID 47483017	MRID 47483017	MRID 47483017

	Residues of Clothianidin (ppm)

	0.010	0.033	0.01

	0.010	0.042	0.01

	0.010	0.051	0.010

	0.010	0.058	0.011

	0.010	0.064	0.012

	0.010	0.067	0.013

	0.010	0.132	0.013

	0.010	0.191	0.015

	0.010	0.201	0.042

	0.010	0.233	0.043

	0.072	0.280	0.054

	0.091	0.349	0.078

1	Residue values <LOQ (0.01 ppm) are listed in bold.

Figure I-9.  Lognormal probability plot of Clothianidin field trial
data for Leaf Lettuce.

Figure I-10.   Tolerance spreadsheet summary of Clothianidin field trial
data for Leaf Lettuce.

Figure I-11.  Lognormal probability plot of Clothianidin field trial
data for Spinach.

Figure I-12.   Tolerance spreadsheet summary of Clothianidin field trial
data for Spinach.

Brassica Leafy Vegetables, Crop Group 5

The datasets used to establish a tolerance for clothianidin on the
brassica leafy vegetables crop group consisted of field trial data for
broccoli, cabbage, and mustard greens (the representative crops of
brassica leafy vegetables) and represented seed application rates of
1.19-1.21 g ai/1000 seed for broccoli and cabbage and 0.10 g ai/1000
seed for mustard greens.  As specified by the SOP, the field trial
application rates are within 25% of the maximum label application rate. 
The residue values used to calculate the tolerance are provided in Table
I-6.

Because all but four (0.011-0.409 ppm) of the residues values for the 34
samples of broccoli, cabbage, and mustard greens were <LOQ (<0.01 ppm),
the tolerance harmonization spreadsheet could not be used to calculate a
recommended tolerances (Table I-6).  Therefore, the maximum residue
value for all three crops (broccoli - 0.409 ppm) was used to assess the
tolerance.  The recommended tolerance for brassica leafy vegetables is
0.4 ppm.

Table I-6.	Residue data used to calculate tolerance for Clothianidin on
Brassica Leafy Vegetables.

Regulator:	EPA	EPA	EPA

Chemical:	Clothianidin	Clothianidin	Clothianidin

Crop:	Broccoli	Cabbage	Mustard Greens

PHI:	74-195 days 	74-177 days 	28-62 days 

App. Rate:	1.19-1.21 g ai/1000 seed	1.21 g ai/1000 seed	0.10 g ai/1000
seed

Submitter:	Bayer CropScience	Bayer CropScience	Bayer CropScience

MRID Citation:	MRID 47483018	MRID 47483018	MRID 47483018

	Residues of Clothianidin (ppm)

	0.010	0.010	0.010

	0.010	0.010	0.010

	0.010	0.010	0.010

	0.010	0.010	0.010

	0.010	0.010	0.010

	0.010	0.010	0.010

	0.010	0.010	0.010

	0.010	0.010	0.010

	0.010	0.010	0.011

	0.010	0.010	0.011

	0.249	0.010

0.409	0.010

	1	Residue values <LOQ (0.01 ppm) are listed in bold.

Fruiting Vegetables, Crop Group 8

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 seed application rates of 0.1 g ai/1000 seed for tomatoes and 0.5 g
ai/1000 seed for peppers.  As specified by the SOP, the field trial
application rates are within 25% of the maximum label application rate. 
The residue values used to estimate the tolerance are provided in Table
I-7.

Because all of the residues values for the 24 samples of tomato, 12
samples of bell pepper, and 6 samples of non-bell pepper were <LOQ
(<0.01 ppm), the tolerance harmonization spreadsheet could not be used
to calculate a recommended tolerances (Table I-7).  Therefore, the LOQ
value (0.01 ppm) was used as the recommended tolerance for fruiting
vegetables.

Table I-7.	Residue data used to calculate tolerance for Clothianidin on
Fruiting Vegetables.

Regulator:	EPA	EPA	EPA

Chemical:	Clothianidin	Clothianidin	Clothianidin

Crop:	Tomato	Bell Pepper	Non-Bell Pepper

PHI:	112-174 days 	90-196 days 	119-149 days 

App. Rate:	0.1 g ai/1000 seed	0.5 g ai/1000 seed	0.5 g ai/1000 seed

Submitter:	Bayer CropScience	Bayer CropScience	Bayer CropScience

MRID Citation:	MRID 47483019	MRID 47483019	MRID 47483019

	Residues of Clothianidin (ppm)

	0.010	0.010	0.010	0.010

	0.010	0.010	0.010	0.010

	0.010	0.010	0.010	0.010

	0.010	0.010	0.010	0.010

	0.010	0.010	0.010	0.010

	0.010	0.010	0.010	0.010

	0.010	0.010	0.010

0.010	0.010	0.010

0.010	0.010	0.010

0.010	0.010	0.010

0.010	0.010	0.010

0.010	0.010	0.010

	1	Residue values <LOQ (0.01 ppm) are listed in bold.

Cucurbit Vegetables, Crop Group 9

The datasets used to establish a tolerance for clothianidin on the
cucurbit vegetables crop group consisted of field trial data for
cucumber, muskmelon, and summer squash (the representative crops of
cucurbit vegetables) and represented seed application rates of 1.0 g
ai/1000 seed for all three crops.  As specified by the SOP, the field
trial application rates are within 25% of the maximum label application
rate.  The residue values used to estimate the tolerance are provided in
Table I-8.

Because all but one (0.01 ppm) of the residues values for the 12 samples
each of cucumber and muskmelon, and 10 samples of summer squash, the
tolerance harmonization spreadsheet could not be used to calculate a
recommended tolerances (Table I-8).  Therefore, the maximum residue
value (0.01 ppm) was used to determine the tolerance.  The recommended
tolerance for cucurbit vegetables is 0.01 ppm.

Table I-8.	Residue data used to calculate tolerance for Clothianidin on
Cucurbit Vegetables.

Regulator:	EPA	EPA	EPA

Chemical:	Clothianidin	Clothianidin	Clothianidin

Crop:	Cucumber	Muskmelon	Summer Squash

PHI:	46-53 days 	75-98 days 	41-49 days 

App. Rate:	1.0 g ai/1000 seed	1.0 g ai/1000 seed	1.0 g ai/1000 seed

Submitter:	Bayer CropScience	Bayer CropScience	Bayer CropScience

MRID Citation:	MRID 47483020	MRID 47483020	MRID 47483020

	Residues of Clothianidin (ppm)

	0.010	0.010	0.010

	0.010	0.010	0.010

	0.010	0.010	0.010

	0.010	0.010	0.010

	0.010	0.010	0.010

	0.010	0.010	0.010

	0.010	0.010	0.010

	0.010	0.010	0.010

	0.010	0.010	0.010

	0.010	0.010	0.010

	0.010	0.010

0.010	0.010

	1	Residue values <LOQ (0.01 ppm) are listed in bold.

Cereal Grains, except rice, Crop Group 15

The datasets used to establish a tolerance for clothianidin on the
cereal grains crop group consisted of field trial data for wheat,
representing seed application rates of 0.125 g ai/100 kg seed.  Although
the use rate for wheat was 1.8x the proposed use rate of 70 g ai/100 kg
seed, these data were used to assess a recommended tolerance as residues
at the 1.8x rate were <LOQ in/on all samples of wheat grain (Table I-9).
 Because all of the residues values for the 40 samples of wheat grain
were <LOQ (<0.01 ppm), the tolerance harmonization spreadsheet could not
be used to calculate a recommended tolerances (Table I-9).  Therefore,
the LOQ value (0.01 ppm) was used as the recommended tolerance for wheat
grains.  In addition, the existing field trial data on field corn and
sorghum (DP# D303164, W. Drew, 2/01/06; and DP# D282446, Y. Donovan,
5/01/03) support tolerances of 0.01 ppm for corn grain and sorghum
grain.  Therefore, the residue data on field corn, sorghum and wheat
will together support a 0.01 ppm tolerance on cereal grains, except
rice.

Table I-9.	Residue data used to calculate tolerance for Clothianidin on
Cereal Grains.

Regulator:	EPA

Chemical:	Clothianidin

Crop:	Wheat Grain

PHI:	86-307 days 

App. Rate:	125 g ai/100 kg seed

Submitter:	Bayer CropScience

MRID Citation:	MRID 47483021

	Residues of Clothianidin (ppm)

	0.010	0.010

	0.010	0.010

	0.010	0.010

	0.010	0.010

	0.010	0.010

	0.010	0.010

	0.010	0.010

	0.010	0.010

	0.010	0.010

	0.010	0.010

	0.010	0.010

	0.010	0.010

	0.010	0.010

	0.010	0.010

	0.010	0.010

	0.010	0.010

	0.010	0.010

	0.010	0.010

	0.010	0.010

	0.010	0.010

1	Residue values <LOQ (0.01 ppm) are listed in bold.

Wheat Forage, Hay, and Straw

The datasets used to assess tolerances for clothianidin consisted of
field trial data for wheat forage, hay, and straw, representing a seed
application rate of 125 g ai/100 kg seed (1.8x proposed rate).  The
residue values used to calculate the tolerance are provided in Table
I-10.

The maximum likelihood estimation (MLE) procedures were needed to impute
censored values for wheat hay because field trial sample results were
below LOQ for 15 of 40 samples, and wheat straw because field trial
sample results were below LOQ for 19 of 40 samples.  The datasets for
wheat forage, hay (MLE) and straw (MLE) were entered into the tolerance
spreadsheet (Table I-10).  Visual inspection of the lognormal
probability plots for wheat forage, hay, and straw (Figures I-13, I-15
and I-17, respectively) provided in the spreadsheet indicated that the
wheat forage, hay, and straw datasets were not lognormal.  The results
from the approximate Shapiro-Francia test statistic (Figures I-14, I-16
and I-18, respectively) confirmed that the assumption of lognormality
should be rejected for wheat forage, hay, and straw.  

Using the tolerance spreadsheet, the recommended tolerances are 0.35 ppm
for wheat forage, 0.07 ppm for wheat hay, and 0.05 ppm for wheat straw.

Table I-10.	Residue data used to calculate tolerance for Clothianidin on
Wheat Forage, Hay, and Straw.

Regulator:	EPA	EPA	EPA

Chemical:	Clothianidin	Clothianidin	Clothianidin

Crop:	Wheat Forage	Wheat Hay (MLE)	Wheat Straw (MLE)

PHI:	31-245 days 	56-277 days 	86-307 days 

App. Rate:	125 g ai/100 kg seed	125 g ai/100 kg seed	125 g ai/100 kg
seed

Submitter:	Bayer CropScience	Bayer CropScience	Bayer CropScience

MRID Citation:	MRID 47483021	MRID 47483021	MRID 47483021

	Residues of Clothianidin (ppm)

	0.010	0.077	0.006	0.011	0.005	0.010

	0.010	0.083	0.007	0.011	0.006	0.010

	0.010	0.088	0.007	0.011	0.006	0.010

	0.010	0.094	0.007	0.011	0.007	0.010

	0.010	0.094	0.008	0.014	0.007	0.010

	0.010	0.098	0.008	0.014	0.007	0.010

	0.015	0.113	0.008	0.016	0.008	0.010

	0.015	0.122	0.008	0.016	0.008	0.010

	0.021	0.131	0.009	0.017	0.008	0.010

	0.022	0.132	0.009	0.021	0.008	0.011

	0.023	0.156	0.009	0.022	0.008	0.013

	0.024	0.158	0.009	0.027	0.008	0.014

	0.030	0.160	0.009	0.031	0.008	0.015

	0.033	0.181	0.009	0.032	0.009	0.015

	0.033	0.182	0.010	0.035	0.009	0.018

	0.034	0.186	0.010	0.038	0.009	0.019

	0.034	0.211	0.010	0.040	0.009	0.031

	0.042	0.212	0.010	0.041	0.009	0.038

	0.044	0.232	0.011	0.056	0.009	0.041

	0.075	0.273	0.011	0.085	0.010	0.043

1	Residue values <LOQ (0.01 ppm) are listed in bold.

Figure I-13.  Lognormal probability plot of Clothianidin field trial
data for Wheat Forage.

Figure I-14.   Tolerance spreadsheet summary of Clothianidin field trial
data for Wheat Forage.

Figure I-15.  Lognormal probability plot of Clothianidin field trial
data for Wheat Hay.

Figure I-16.   Tolerance spreadsheet summary of Clothianidin field trial
data for Wheat Hay.

Figure I-17.  Lognormal probability plot of Clothianidin field trial
data for Wheat Straw.

Figure I-18.   Tolerance spreadsheet summary of Clothianidin field trial
data for Wheat Straw.

Clothianidin	Summary of Analytical Chemistry and Residue Data	DP#: 
357455

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