Acetamipri d Summary of Analytical Chemi stry and R esidue Data DP Barcode D409727



### UNIT ED STATES ENVIRONMENTAL PROTECTION AGENCY

WA SHINGTON

, D

. C

. 20460

OFFICE OF CHEMICAL SAFETY AND

POLLUTION PREVENTION 

### MEMORANDUM



### D ate: March 12

, 2013

Subject: Ace tamiprid. P et i tio n for the Establishment of Pe rmane nt Tolerances and Registra tion for Use on Sweet Corn. Summar y of Analytical Chem istry and R esidue

Data.

From:

Thr ough:

T o: P C Code : 099050

MRJD Nos .: (Se e MRJD summary )

Pet ition Nos.: l E7919

Assessme n t Type: NA

TXRNo.: NA

Decision Nos

. : 474870 DP Bar code: D409727

R egistration Nos.: 80 33-23

, 8033-36 Regulato ry Action: Section 3 Registrati on Case No.: 7617

CAS No.: 135410

- 20-7

40 C FR § 18 0.57 8



### E li za beth Holman, Physical Scientist**~** t}/--



### Ri sk Assess m ent B r anc h II

Health Effects Division (7509P)

W illiam T. 

### Dre w,

# Chemist~)**~** Ri sk Assessment Branch II



### Health Eff ec ts Division (7509P)

Andrew Ertman

, Che mical Review Mana ger Ri sk Integration M in or Use

, and Emergency R esponse Branch

Re g i s trat i on D ivisio n (7505P )

And



### J ennife r UrbanskiNenus Eagle ( Team 01)

I nsecticide/Rodenticide Br anch

Re gis tr at ion Di visio n (7505P)

Page 1 of25Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode 0409727



## Table of Contents

Background

. .. ............... . ...... . ........................ . .. .. . .. .. . ... .. .. .. .. . ... . ... .. .. . .............................. . ........ . ........ 3

Executive Summary

............. . ....... .. .. . .. .. .. . ... . .. .. .. . ... .. .. . ... .. .. . .. .. .. .. ......................... . ... . ................... . .. 3

Regulatory Recommendations

........... .. .. ...... .. . .. .. .. .. .. . ... . .. ... .. . ... . .. .. .. ... . ....... . ... .. .. ............. . ........ . ..... 4

Tolerance Considerations

....................... . .. .. .. . ... .. .. . ...... . ... . ... ...... .. .. ...... .. ........... . ............................. 5

Analytical Me t hod

..................... . ... . ......... .. ...... . ... . ... . .. .. .. .. .. . ... . ... .. .. .. ....... . .................................. 5

Recommended Tolerances

........... .. ...... . ...... .. .. .. .. .. .. .. .. . ... . ... .. . .. ... . .. .. ... .. . ... .................................. 5

International Harmonization

. . ... . ................. .. ...... . ... . .. . ... . ... . ... . ... . ... . ... . ... .. .. . ... . ............................ 6

Revisions to Petitioned-For Tolerances

........................................ .. ...... . .... . ....... ... . .. ... .. .. .. .. .. ... .. . 6

Residue Profi l e

................................................................................................................................ 6

Residue Chemistry Guidelines

...... . ... . .......... . ... .. .. .. ................. .. ............................................... .. ..... 8

Directions for Use (860.1200)

........................................ . ........................................................... 8

Nature of the Residue (860.1300/1850)

...................................................................................... 8

Residue Analytical Methods (860.1340)

..................................................... . ................. .. ........... 9

Multiresidue Methods (860.1360)

............................................................................................ 11

Storage Stability (860.1380)

.......... .. ..................... .. ...... . .............. .. ........................................... 11

Water, Fish, and Irrigated Crops (860.1400)

................................................................... . ........ 11

Food Handling (860.1460)

................................................ . ............................... . ............... .. ...... 11

Meat, Milk, Poultry, and Eggs (860

. 1480)

....... .. .. . .......... . ........... . ....... . ... . ....... . ... .. ... . ... .. ....... . .. 12

<;rop Field Trials (860.1500)

. . ... .. .. . ... . .. . ... . .. .. .. . ... . ... . ...... . ... .. .. ... . .. ... .. . .. ... . ....... . ........... . ..... . ...... 13

Processed Food and Feed (860

. 1520)

... . .. .. .. .. . ... . ... .. ......... .. .. .. ......... ... . ... .. ...... .. ... . ....... .. ........... 17

, '(

, 

### Submittal of Analytical Reference Standards (860

. 1650)

.. ...... .. . ... . .. ... . ... .. . ... .. .. . ... .. ... .. .. ... .. .. .. 17

Rotational Crops (Field; 860.1900)

........ . .................. .. ........... . .. . ............... .. ...... . .... . ... . .... .. .. . .... 17

Tolerance Derivation

.................................................................... .. ... .. ..... ... .. .. ....... .. .. ... .. .. .. .. ... .. .. . 18

References

.............................................................................. . .............. .. .. . ... .. ... . .. .. ... . ... .. ... . ... .. ... . 18

Attachment 1. International Maximum Residue Limits

- Acetarniprid

........... . ....... .. .. ... .. .. ....... . 19

Appendix I. 

### Field Trial Geographic Distribution

. . ... . .. .. .......... ... ................. .. .. . ..................... ... ... 19

Appendix II. Tolerance Assessment Calculations

.................. ............... ........... . .......................... 22

Page 2 of25Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 3 of 25 Summary of Submitted Residue Chemistry Studies

OPPTS 860 Series

Guideline MRID

Number Title

860.1500 48590103 48590103 Samoil , K. (2011) Acetamiprid: Magnitude of the Residue on Sweet Corn. Project Number: 10216, 10216/09/CAR01. Unpublished study prepared by Interregional Research Project No. 4, University of California and University of Florida. 232 p.

48590104 48590104 Lonsbary, S. (2010) Acetamiprid: Magnitude of the Residue on Sweet Corn:

Final Report. Project Number: AAFC06/034R, AAFC06/034R/297. Unpublished study prepared by University of California, Davis. 398 p.



## Background

The Agency has received a petition from the Interregional Research Project No. 4 (IR

- 4) to register the insecticide acetamiprid { CAS name (1 E )

- N

- [(6

- chloro

- 3

- pyridinyl)methyl]

- N '

- cyano

N

- methylethanimidamide } for post

- emergen t foliar use on sweet corn. T he end

- use products under consideration for the new uses are the 70% wettable powder (WP) formulation, Assail® 70

WP Insecticide (EPA Reg. No. 8033

- 23), and the 30% water soluble granule (SG) formulation,

Assail® 30 SG Insecticide (EPA Reg. No. 8033

- 36). Under an earlier petition (Petition

# 1E7919 ), this request for use on sweet corn was found to have inadequate residue data and the Agency requested additional residue data prior to registration and the establishment of

tolerances.

Acetamiprid is regis tered for use on a number of crops, and permanent tolerances have been established (40 CFR § 180.578) ranging from 0.01 ppm to 50 ppm in plant commodities

, and from 0.010 ppm to 0.20 ppm in livestock commodities. The residue definition for risk

assessment and tolerance enforcement is the parent compound for plant commodities, and combined residues of the parent compound and Metabolite IM

- 2

- 1 for livestock commodities (plus Metabolite IM

- 2

- 1

- amide in ruminant muscle for risk assessment purposes only). Accep table analytical methods are available to enforce tolerances for residues of acetamiprid in plant and livestock commodities.



## Executive Summary

The petitioner is proposing to use acetamiprid as post

- emergence foliar applications to sweet

corn. The m aximu m seasonal rate and preharvest interv als (PHIs), respectively, are 0.21 lb ai/A and 7 days (following two applications) or 1 day (following four applications) for sweet corn.

To support the proposed uses, the petitioner previously submitted studies depi cting residues of acetamiprid in/on sweet corn kernel + cob with husks removed (K+CWHR), forage, and stover. Sweet corn field trials were conducted in the U.S. with the 30% SG formulation applied as both two and four applications with a non

- ionic surfacta nt ( NIS ) adjuvant, and in Canada with the 70% WP formulation applied as four applications without an adjuvant. In the earlier review of

th is residue data, it was noted that a pplications were made in accordance with the proposed labeling a t all trials, exc ept that the Canadian sweet corn field trials reflected a significantly longer PHI for stover (38

- 89 days).Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 4 of 25 

### The earlier 2012 review of the sweet corn residue data also cited adjuvant issues as a discrepancy in the use pattern between the U.S. and Canadian field trials, with the U.S. trials being conducted with an adjuvant

, and the Canadian trials not including an adjuvant (D394 779, E. Holman, 03/06/2012) . However, since this decision was made, HED’s ChemSAC concluded that the inherent variability in field trials, coupled with the characteristics and conservative nature of the

OECD tolerance calculation method exceeds the variab ility seen with the use of adjuvants

. Therefore, the adjuvant differences observed in the U.S. and Canadian field trials are no longer

considered to be an issue. HED previously concluded that there is evidence to support residue equivalency for the 70% W P formulation and the 30% SG formulation

, and the combination of

trials conducted with these two formulations provide for an adequate number of trials with sufficient geographic variation

.

Consequently, based on the conclusions of ChemSAC on adjuvant dif ferences and the equivalency of the formulations , the previously identified deficiencies in the sweet corn residue

field trial data have been sufficiently resolved. No additional sweet corn field trial data are required. The available, previously submitted residue data are adequate to support the proposed use and are sufficient for establishing tolerances at 0.01 ppm in sweet corn (kernel plus cob with

hus ks removed), 15 ppm in sweet corn forage, and 30 ppm in sweet corn stover. In addition, the use on sweet corn has increased the anticipated livestock dietary burden and thus necessitates

increases in the livestock tolerances in milk

, as well as the tolera nces in the fat, meat, and meat byproducts of cattle, goat, horse, and sheep. These recommended increases are summarized below in the Regulatory Recommendations section, which match the tolerance values proposed in the petition currently under review.

The residue data are supported by appropriate analytical method and storage stability data.



## Regulatory Recommendations

The available residue chemistry data for acetamiprid are sufficient for purposes of assessing risk

and establis hing tolerances i n sweet corn

.

There are no residue chemistry considerations which would preclude granting registration of the

70% WP and 30% SG formulations for use on sweet corn

. It is noted that all of the submitted

U.S. field trials for sweet corn used the 70% WP f ormulation , whereas the Canadian trials used

the 30% SG formulation . The registrant is requesting the use of both the 70% WP and the 30%

SG formulation. Normally, consistent with OCSPP and OECD Crop Field Trial Guidance,

a dditional bridging data would be required to support the use of the 30% SG formulation.
However, during a previous assessment, a similar situation was encou ntered and the registrant provided additional information on the SG formulation. As a result, HED concluded that such

data were not necessary, agreeing that due to high water solubility both products are likely to produce a solution of acetamiprid (D369474, D. McNeilly, 12/ 0 1/ 20 09)

. Therefore bridging data to support the use of the 30% SG formulation on sweet corn is not required

.

The proposed use of acetamiprid on sweet corn will result in a significant increase in the maximum reasonable dietary burden for ruminants as a result of dietary contributions from sweet corn forage and cannery waste. Based on the available data , the tolerance in milk should beAcetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 5 of 25 

### increased from 0.10 to 0.30 ppm, and the tolerances in the fat, meat and meat byproducts of cattle, goat, horse and sheep should be increased as follow s : F rom 0.10 to 0.20 ppm in fat; from 0.10 to 0.30 ppm in meat; and from 0. 20 to 0.70 ppm in meat byproducts.

In addition, an error has been identified with a commodity definition listing in the existing 40

CFR §180.578 , which currently lists “vegetable, tuberous and corm, group 1.” In a future action associated with acetamip rid, this listing should be revised to read “Vegetable, tuberous and corm, subgroup 1C.”



## Tolerance Considerations

Analytical Method

Approved tolerance enforcement methods for crops are available for acetamiprid, including gas chromatography with el ectro n capture detection (GC/ECD) for vegetables and non

- citrus fruits ; high performance liquid chromatography with ultraviolet detection (HPLC/UV) for citrus fruits only ; and high performance liquid chromatography with tandem mass spectrometr ic detection (LC/MS/MS; Method #KP

- 216R0 and its modification Method #KP

- 216R1) for vegetables and

non

- citrus fruits. The GC/ECD and HPLC/UV methods have undergone acceptable petition method validation (PMV) trials

. Following the submission of acceptable independent laboratory

validation (ILV) data

, and the addition of a second daughter ion specific to acetamiprid to be monitored for analysis of acetamiprid, the LC/MS/MS method was previously determined to be

suitable for tolerance enforcement. The GC/ECD and LC/MS/MS methods use methanol extraction followed by partitioning into dichloromethane, and Florisil/silica gel column cleanup

. The HPLC/UV method use s acetonitrile (ACN) extraction, partitioning into hexane and dichloromethane, and Florisil/C18 cleanup. The limit of quantitation (LOQ) for vegetables and

non

- citrus fruits is 0.01 ppm. The LOQ for citrus fruits is 0.05 ppm. An approved HPLC/UV

toleran ce enforcement method for livestock matrices is available. The LOQ is 0.01 ppm for meat, fat, milk, and eggs, and 0.05 ppm for liver and kidney.



## Recommended Tolerances

Table 1. Tolerance Summary for Acetamiprid.

Commodity Established/Proposed Tolerance (ppm) Recommended

Tolerance (ppm) Comments ( Correct

Commodity Definition )

Corn, sweet, kernel plus cob with

husks removed 0.01 0.01

Corn, sweet, forage 1 5 1 5

Corn, sweet, stover 30 30

Milk 0.30 0.30

Cattle, fat 0.20 0.20

Cattle, meat 0.30 0.30

Cattle, meat byproducts 0.70 0.70

Goat, fat 0.20 0.20

Goat, meat 0.30 0.30

Goat, meat byproducts 0.70 0.70Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 6 of 25 Table 1. Tolerance Summary for Acetamiprid.

Commodity Established/Proposed Tolerance (ppm) Recommended

Tolerance (ppm) Comments ( Correct

Commodity Definition )

Horse, fat 0.20 0.20

Horse, meat 0.30 0.30

Horse, meat byproducts 0.70 0.70

Sheep, fat 0.20 0.20

Sheep, meat 0.30 0.30

Sheep, meat byproducts 0.70 0.70



## International Harmonization

There are currently no established Codex, Canadian or Mexican MRLs for acetamiprid on sweet corn; therefore, there are no issues of harmonization. There are Codex and Canadian MRLs on livestock commodities, with the revised livestock tolerances for the U.S. being higher than both

the Codex and Canadian values. Given the requested use on sweet corn, these higher U.S. livestock commodity tolerances are warranted. However, this is not considered to be a significant trade irritant, as livestock commodities are rarely shipped internationally.



## Revisions to Petitioned

- For Tolerances

No revisions relative to the petitioned

- for tolerances are necessary for sweet corn or for the

associated livestock commodities.



## Residue Profile

Table 2. Acetamiprid Nomenclature.

Chemical Structure

Common Name Acetamiprid

Molecular Formula C 10 H 11 ClN 4 Molecular Weight 222.68
Company Experimental Name EXP

- 61842A, AEF124370, NI

- 25

IUPAC Name ( E )

- N 1

- [(6

- chloro

- 3

- pyridyl)methyl]

- N 2

- cyano

- N 1

- methylacetamidine

CAS Name (1 E )

- N

- [(6

- chloro

- 3

- pyridinyl)methyl]

- N'

- cyano

- N

- methylethanimidamide

CAS Registry Number 135410

- 20

- 7

End

- use Products (EPs) Assail® 70 WP Insecticide (EPA Reg. No. 8033

- 23)

Assail® 30 SG Insecticide ( EPA Reg. No. 8033

- 36)Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 7 of 25 Table 2. Acetamiprid Nomenclature.

Chemical Structure of Acetamiprid Metabolite

IM

- 2

- 1

N 1

- [(6

- chloro

- 3

- pyridyl )methyl]

- N 2

- cyano

- acetamidine

Chemical Structure of Acetamiprid Metabolite

IM

- 2

- 1

- amide (also referred to as IM

- 2

- 2)

N 2

- aminocarbonyl

- N 1

- [(6

- chloro

- 3

- pyridyl)methyl]acetamidine

Table 3. Physicochemical Properties of Technical

- Grade Acetamiprid.

Parameter Value Reference

Melting Point/Range ( C) 98.9 DP Barcode D328216, W. Drew,

10/23/2007 pH 6.08 (Aqueous solution at 20 C)
Density (g/cm 3 ) 1.33 (at 20 C)
Water Solubility (g/L) 4.25 (at 25 C)

Solvent Solubility (at 25 C) Acetone >20 g/100 g

Methanol >20 g/100 g

Ethanol >20 g/100 g

Dichloromethane >20 g/100 g

Chloroform >20 g/100 g

Acetonitrile >20 g/100 g Tetrahydrofuran >20 g/100 g

Benzene 2.44 g/100 g Xylene 4.01 g/100 g

n

- Hexane 6.54 ppm

Carbon disulfide 507 ppm

Vapor Pressure (mm Hg) 7.5 x 10 - 9 (at 25 C) DP Barcode D 264154, M. Doherty;

12/31/2001

Dissociation Constant, pK

a 0.7 (at 25 C) DP Barcode D328216, W. Drew,

10/23/2007 Octanol/Water Partition Coefficient, Log K OW 0.8 (at 25 C)

UV/Visible Absorption Spectrum Not available



### The residue chemistry database for acetamiprid is complete and acceptable for supporting recommended tolerance levels and conducting human health risk assessments. The available metabolism data and information regarding physicochemical properties do not indicate that there are any special concerns with this chemical in terms of bioaccumulation, exposure, or other risk

assessment considerations. N N H Cl

C H 3



### N

O N H 2 

### N N

H C

l

C H 3



### N C NAcetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 8 of 25 

## Residue Chemistry Guidelines

Directions for Use (860.1200)

Table 4. Summary of Proposed Directions for Use of Acetamiprid. 1

Applic. Timing, Type, and Equip. Formulation

[EPA Reg.
No.] Applic.

Rate (lb ai/A) Max. No.

Applic. per

Season Max. Seasonal

Applic. Rate (lb ai/A) PHI

(days) Use Directions and

Limitations 2

Sweet corn

Post

- emergence, Broadcast, Aerial (≥5 gal/A) or ground, (≥20 gal/A) Assail®

70 WP [8033

- 23]

Assail®

30 SG [8033

- 36] 0.075

- 0.1 2 0.21 7 Minimum RTI = 14 days

0.04

- 0.054 4 1 Minimum RTI = 7 days (if applied in a rotation or

tank mixture with another insecticide)

1 From draft labels dated 8/25/11 for Assail® 70 WP and 8/24/11 for Assail® 30 SG

2 RTI = Re

- treatment interval

3 Refer to accept ed labels dated 6/29/11 for both Assail® 70 WP and Assail® 30 SG.



### Adjuvant use : The draft labels for the 70% WP and 30% SG formulations state that an adjuvant,

such as a non

- ionic or silicone surfactant or methylated seed oil, is recommended on certain row crops. For the control of whiteflies on row crops, an adjuvant is recommended for vegetables (except legumes) and cotton . The draft labels for the 70% WP and 30% SG formulations also state that an adjuvant, such as an NIS , methylated seed oil, or horticultural oil, is recommended for use on orchard and vine crops, except on grapes.

Conclusions

. The labels are adequate to allow evaluation of the residue data relative to the proposed use on sweet corn.

Sweet corn field trials were conducted in the U.S. with the 30% SG formulation applied as both two and four applications with an NIS

, and in Ca nada with the 70% WP applied as four applications without an adjuvant. Applications were made in accordance with the proposed labeling a t all trials.



## Nature of the Residue (860.1300/1850)

Plants: Residue Chemistry Memo D 264154, 12/31/2001, M. Doherty (PP#0F6082)

MARC Decision Memo, D278652, 11/13/2001, M. Doherty

Livestock: Residue Chemistry Memo D 264154, 12/31/2001, M. Doherty (PP#0F6082)

MARC Decision Memo, D278652, 11/13/2001, M. Doherty

Rotational: Residue Chemistry Memo D328216, 10/23/2007, W. D rew (PP#6F7051 and PP#6E7163)

Residue Chemistry Memo D 264154, 12/31/2001, M. Doherty (PP#0F6082)



### Radiolabeled metabolism studies are available for carrot, cabbage, cotton, apple, eggplant, lactating goat, laying hen, and rat. In plants, there appears t o be little translocation of acetamiprid following foliar application. In cabbage, there was uptake and translocation of acetamiprid to the above

- ground portions of the plant following a soil application. Due to theAcetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 9 of 25 

### rapid dissipation of acetamiprid in the field, root uptake is not considered to be a likely source of residues in plants. Parent acetamiprid is the predominant residue at >90% of the total radioactive residues ( TRR) in three of the five metabolism studies. Confined rotational crop studies sho wed no residues of acetamiprid at the 30

- day plant

- back interval.

Acetamiprid and metabolite IM

- 2

- 1 are the major residues in all ruminant tissues except muscle,

where IM

- 2

- 1

- amide accounts for nearly 50% of the TRR. IM

- 2

- 1

- amide was not found in any

oth er ruminant tissue. Metabolite IM

- 2

- 1 is the major residue in poultry tissues and eggs (50

- 80% TRR). IM

- 2

- 5 is also a major residue in eggs (~20% TRR). Parent acetamiprid was not detected in poultry tissues or eggs. The metabolism of acetamiprid in lac tating goat was similar to the profile observed in laying hen and rat. The initial transformation appears to be demethylation of the parent compound. The most abundant metabolite identified (both sexes) resulted from the removal of the cyanoacetamide gro up from demethylated parent. This removal (and direct removal of the group from the parent) resulted in cyanoacetamide metabolites.

Conclusions

. The nature of the residue for acetamiprid is considered to be adequately understood for target crops, rotational crops, and livestock. The residue definitions for tolerance expression and risk assessment are summarized in Table 5.

Table 5. Risk Asses sment and Tolerance Enforcement Residue Definitions for Acetamiprid.

Matrix Residues included in Risk Assessment Residues included in Tolerance Expression

Plants Primary Crop Acetamiprid Acetamiprid

Rotational Crop Not applicable None at this time

Livestock Ruminant Acetamiprid + IM

- 2

- 1+ IM

- 2

- 1

- amide (ruminant muscle only) Acetamiprid and IM

- 2

- 1

Poultry Acetamiprid and IM

- 2

- 1 Acetamiprid and IM

- 2

- 1

Drinking Water Acetamiprid Not Applicable



## Residue Analytical Methods (860.1340)

Residue Chemistry Memo D342549 & D 355773, 11/05/2008, W. Drew Residue Chemistry Memo D328216, 10/23/2007, W. Drew (PP#6F7051 and PP#6E7163) Residue Chemistry Memo D303623, 11/05/2004, W. Drew (PP#4F6833) Residue Chemistry Memo D 264154, 12/31/2001, M. Doher ty (PP#0F6082)



### Enforcement methods : Adequate residue analytical methods (GC/ECD and HPLC/UV) are available for the enforcement of established tolerances on plant commodities. The method LOQs are 0.01 ppm for vegetables and non

- citrus fruits (GC/ECD), and 0.05 ppm for citrus fruits (HPLC/U V). These methods have undergone successful PMV trials. Under PP#4F6833, Nisso America proposed that the LC/MS/MS method utilized for data collection and confirmatory analysis (Method #KP

- 216R0 or its modification, Method #KP

- 216R1) be designated an

alte rnative to the established GC/ECD tolerance enforcement method. With submission of acceptable ILV data and the ability to analyze two daughter ions specific to acetamiprid, the

LC/MS/MS method was determined to be suitable for tolerance enforcement and co nfirmatory analysis of vegetables and non

- citrus fruits (D342549 & D 355773). A summary of the available methods is presented in Table 6

.Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 10 of 25 Table 5. Table 6. Summary of Validated Analytical Methods for Acetamiprid.

T arget Matrices Method Description LOQ (ppm) Method Validation

Fortification Levels (ppm) Recovery

Range (%)

Vegetables and

Non

- Citrus Fruits Methanol extraction, residues partitioned into

dichloromethane, Florisil/silica gel column cleanup, and LC/MS/MS determination. 0.010 0.010, 0.020 72

- 80

Vegetables and

Non

- Citrus Fruits Methanol extraction, residues partitioned into

dichloromethane, Florisil/silica gel column cleanup, and GC/ECD determination. 0.010 0.010, 0.050 68

- 112

Citrus Fruits Acetonitrile extraction, co

- extractives partitioned

into hexane, residues partitioned into dichloromethane, Florisil/C18 column cleanup,

and HPLC/UV determination. 0.050 0.050, 0.250 77

- 100



### An approved HPLC/UV tolerance enforcement method for livestock matrices is available. The LOQ is 0.01 ppm for meat, fat, milk, and eggs, and 0.05 ppm for liver and kidney.

Data collection methods : Samples of sweet corn commodities from the U.S. field trials were analyzed for residues of acetamiprid using an LC/MS/MS method based on the LC/MS/MS tolerance enforcement method (Method KP

- 216R1). Samples of sweet corn matrices from the

Canad ian field trials were analyzed for residues of acetamiprid using a n LC/MS/MS method based on the GC/ECD enforcement method. The LOQ was 0.01 ppm (determined as the lowest level of method validation, LLMV) for residues of acetamiprid in/on all matrices

.

For sweet corn commodities from the U.S. field trials, samples were extracted with

methanol / water (1:1, v:v), then vacuum filtered. The extract was brought to volume with

methanol / water (1:1, v:v or 1:3 , v:v), and an aliquot was applied to a Waters Oasis HLB solid phase extraction (SPE) column or Strata

- X SPE column. Residues were eluted with ACN. The resulting eluate was adjusted to volume with water and diluted as needed with ACN / water ( 1:1

, v:v) or evaporated to near dryness under nitrogen and diluted with ACN / water ( 1:1 , v:v), then

filtered for LC/MS/MS a nalysis.

For sweet corn commodities from the Canadian field trials, samples were extracted with methanol, then vacuum filtered. The extract was combined with 5% sodium chloride and partitioned with hexane followed by methylene chloride (2x ). The methylene chloride phases were dried through anhydrous sodium sulfate and combined. The combined extracts were evaporated to dryness, redissolved in 20% acetone/hexane, and applied to a Supelclean LC

Florisil SPE column; residues were eluted with 50% acetone/hexane. The resulting eluate was evaporated to near dryness and adjusted to volume with 50% methanol/water, then filtered for LC/MS/MS analysis.

Conclusions . The methods used in the submitted sweet corn crop field trials are essentially

iden tical to establishe d tolerance enforcement methods; these methods are therefore suitable for data collection. In addition, acceptable method validation and concurrent recovery data were submitted with all studies, and the fortification levels used in meth od validation and concurrentAcetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 11 of 25 

### recovery were adequate to bracket expected residue levels in all crop matrices. Concurrent recoveries and residues in treated samples were not corrected for residues in controls in any of

the submitted studies.



## Multiresidue M ethods (860.1360)

Residue Chemistry Memo D 264154, 12/31/2001, M. Doherty (PP#0F6082)



### D ata concerning the recovery of residues of acetamiprid using FDA multiresidue method protocols (PAM Volume I) were submitted in conjunction with the original acetamipri d petition (PP#0F6082). Based on the results of the testing, the multiresidue methods are not appropriate for determining acetamiprid residues of concern. The Biological and Economic Analysis Division (BEAD) is currently working on a multi

- residue method for the neonicotinoids.



## Storage Stability (860.1380)

Concurrent storage stability studies were conducted with the crop field trial studies on asparagus, mustard greens, and sweet corn (U.S. trials). The data demonstrate that residues of acetamiprid

wer e stable during frozen storage in/on samples of sweet corn K+CWHR, forage, and stover for

up to 384

- 391 days (12.6

- 12.9 months) . N o 0

- day data were provided for any study . These data are acceptable to support the storage conditions and durations of sampl es from the submitted field trials; however, t he Agency reminds the petitioner that storage stability studies should always include a 0

- day sampling interval to establish the residue levels present at the time samples are placed into storage [see OCSPP Res idue Chemistry Test Guideline 860.1380(d)(6)(i)].

The storage durations and conditions of samples from the sweet corn crop field trials are presented in Table 7.

Table 7 . Summary of Storage Conditions and Durations of Samples from Crop Field Trial Studies.

Matrix Storage

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

Sweet corn, K+CWHR

- 20 144

- 363 days (4 .7

- 11.9 months) Up to 384

- 391 days (12.6

- 12.9 months) in/on sweet corn K+CWHR, forage, and stover Sweet corn, forage 168

- 360 days (5 .5

- 11.8 months)

Sweet corn, stover 142

- 377 days (4.7

- 12.4 months)



### Conclusions

. The submitted concurrent storage stability data for sweet corn commodities are adequate to support the submitted crop field trials. The data indicate that there are no storage stability issues, and no corrections for decline during storage are needed.



## Water, Fish, and Irrigated Crops (860.1400)

This guideline topic is not relevant to the proposed uses.



## Food Handling (860.1460)Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 12 of 25 

### This guideline topic is not relevant to the proposed uses.



## Meat, Milk, Poultry, and Eggs (860.1480)

Residue Chemistry Memo D264154, 12/31/01, M. Doherty DER Reference: 44988601.der, 12/14/01, H. Bietlot



### There are ruminant feedstuffs (forage, stover, and cannery waste) associated with the proposed use of acetamiprid on sweet corn.

T he maximum reasonable dietary burdens of acetamiprid to ruminants, based on the addition of sweet corn forage and cannery waste

, are calculated herein (Table 8).

With the addition of sweet corn feedstuffs, the dietary burdens are 1.132 ppm for beef cattle and 12.777 ppm for dairy cattle. The current livestock tolerances are based on a maximum theoretical dietary burden of 4.5 ppm.

Table 8

. Calculation of Dietary Burdens of Acetamiprid Residues to Cattle.

Feedstuff Type 1 % Dry

Matter 2 % Diet 2 Established

Tolerance or HR 3
(ppm) Dietary Contribution

(ppm) 4

Beef Cattle

Cotton gin byproducts R 90 5 20.0 1.111

R not registered R

-- 10

-- -- Potato processed waste CC 15 30 0.01 0.020

CC not registered CC

-- 50

-- --
Canola meal PC 88 5 0.01 0.001

TOTAL BURDEN

-- -- 100

-- 1.132

Dairy Cattle

Sweet corn forage R 48 45 10.0 9.375

Sweet corn cannery

waste CC 30 10 10.0 3.333

CC not registered CC

-- 3 5

-- -- Cotton, undelinted seed P C 88 10 0.60 0.068

TOTAL BURDEN

-- -- 100

-- 12.777

1 R = Roughage; CC = carbohydrate concentrate; PC = protein concentrate.

2 OCSPP 860.1000 Supplement (June 2008)

3 HR = Highest residue. HR used for sweet corn forage (and cannery waste); established tolerances used for remaining commodities.

4 Contribut ion = [tolerance or HR/% DM] X % diet



### In the cattle feeding study (refer to 44988601.der), the dietary feeding levels were 6, 18, and 60 ppm. Based on the data for sweet corn forage that are currently available, these correspond to 0.47x, 1.4x, and 4.7x the maximum reasonable dietary burden t o dairy cattle.Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 13 of 25 

### If the residues observed at the three dosing levels are adjusted to a 1x feeding level for dairy cattle (see Table 9 ), maximum expected combined residues of acetamiprid and IM

- 2

- 1 would be

0.28 ppm in milk, 0.61 ppm in kidney, 0. 56 ppm in liver

, 0.15 ppm in fat , and 0.24 ppm in

muscle.

Table 9

. Summary of Data from Cattle Feeding Study with Acetamiprid.

Matrix Maximum combined residues of acetamiprid and IM

- 2

- 1 at each dosing

level 1 Residues adjusted to 1x feeding level for dairy cattle

6 18 60 0.5x 1.4 x 4.7 x Milk (Days 4

- 27 ) 0.081 0.366 1.3 0.17 0.26 0.28

Fat <0.072 0.153 0.714 <0.15 0.11 0.15

Kidney <0.25 <0.86 2.54 <0.53 <0.61 0.54

Liver <0.15 0.64 2.65 <0.32 0.46 0.56

Muscle <0.050 0.289 1.11 <0.11 0.21 0.24

1 The LOQ s were 0.01 ppm for milk, fat, and muscle and 0.05 ppm for kidney and liver



### Conclusions. The proposed use of acetamiprid on sweet corn will result in a significant increase in the maximum reasonable dietary burden to ruminants as a result of die tary contributions from sweet corn forage and cannery waste. When the results of the dairy cattle feeding study are adjusted for the increased dietary burden, the maximum expected combined residues of acetamiprid and IM

- 2

- 1 increase in milk and all tissue s.

Based on the data available, the tolerance in milk should be increased from 0.10 to 0.30 ppm,

and the tolerances in the fat, meat, and meat byproducts of cattle, goat, horse, and sheep should be increased from 0.10 to 0.20 ppm in fat; from 0.10 to 0.30 ppm in meat; and from 0.20 to 0.70

ppm in meat byproducts.

Because sweet corn commodities are not significant feedstuffs for poultry or swine, no changes

are needed to the established tolerances in eggs, n or in poultry or hog tissues.



## Crop Field Trials (860.1500)

DER References: 48590103.der (Sweet corn, U.S. trials)

48590104.der (Sweet corn, Canad ian trials).



### Sweet corn

Seven sweet corn field trials were conducted in the U.S. during the 2009 growing season, and

five trials were conducted in Canada during the 2006 growing season. The use patterns were similar. In the U.S. trials, samples of K+CWHR, forage, and stover (dried after harvest) were

harvested at a 1

- day PHI following four applications of the 30% SG formulation at a total rate of

~ 0.21 lb ai/A or at a ~7

- day PHI following two applications of the 30% SG formulation at a total

rate of ~0.21 lb ai/A. In the Canadian trials, samples of K+CWHR and forage were harvested at

a 1

- to 2

- day PHI following four applications of the 70% WP formu lation at a total rate of ~0.21 lb ai/A, and stover was harvested at maturity ( 38

- to 89

- day PHIs). The application rates used in the studies are equivalent to ~1x the maximum proposed seasonal application rate.Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 14 of 25 

### U.S. Trials

IR

- 4 has submitted field trial data for acetamiprid on sweet corn. During the 2009 growing

season, 7 U.S. field trials w ere conducted in the following North American Free Trade Agreement (NAFTA) Growing Zones: 1 (NY; 1 trial); 2 (GA and SC; 2 trials); 3 (FL; 1 trial); 5A (WI; 1 trial); 10 (CA; 1 trial); and 11 (ID; 1 trial).

Each trial consisted of one untreated plot and two side

- by

- side treated plots. At each trial location, one treated plot (plot 2) received four foliar broadcast or directed applications o f a 30% SG formulation of acetamiprid ( Assail® 30 SG) at 0 .053

- 0.057 lb ai/A/application for a total

seasonal rate of 0.212

- 0.220 lb ai/A . A second plot (plot 3) received two foliar broadcast or directed applications of the same formulation at 0.094

- 0.109 lb ai/A/application for a total

seasonal rate of 0.195

- 0.214 lb ai/A. Applica tions were made at 4

- to 8

- da y RTIs (plot 2) or 12

- to 16

- day RTIs (plot 3) using ground equipment

, in spray volumes of 23

- 49 gal/A. An NIS was added to each spray mixture.

Sa mples of K+CWHR, forage, and stover were harvested from the side

- by

- side plots at PHIs of 1 day (plot 2) or 5

- 8 days (plot 3), except at the NY trial, where PHIs for stover were 28 and 35 days for plots 2 and 3, respectively. Stover was dried in a dr y er o r allowed to dry at ambient temperatures in the field or at the test facility for 2

- 18 days after harvest to a moisture content of

15

- 20%, except at the NY trial, where stover was allowed to dry prior to harvest.

Samples were analyzed for residues of acetamiprid using an adequate LC/MS/MS method, and the study is supported by acceptable storage stability data (see Table 7).

The results of the sweet corn field trials are presented in Table 1 0 (below)

. In samples of sweet corn harvested 1 day following four foliar broadcast or directed applications of the 30% SG formulation of acetamiprid at a total rate of 0.212

- 0.220 lb ai/A, acetamiprid residues (and per trial averages) were <0.01 (<0.01) in K+CWHR , 0.42

- 8.1 (0.54

- 7.3) in forage , and 0.12

- 16 (0.19

- 15 .5) ppm in stover. In samples of sweet corn harvested 5

- 8 days following two foliar broadcast or directed applications of the 30% SG formulation of acetamiprid at a total rate of

0.195

- 0.214 lb ai/A, acetamiprid residues (and per trial averages) were <0.0 1 (<0.01) in

K+CWHR , 0.39

- 10 (0.41

- 9.1) in forage , and 0.21

- 21 (0.21

- 20) ppm in stover. Results for stover from the NY trials, dried before harvest and reflecting PHIs of 28 and 35 days, were within the range of residue results for samples from the remain ing trials reflecting ~1 and ~7

- day PHIs and

post

- harvest drying.

Side

- by

- side comparison of residues in/on corn forage and stover harvested 1 day following four

foliar applications or 5

- 8 days following two foliar applications suggested that the use pat terns yielded similar residues in both matrices, with neither use pattern yielding consistently higher or

lower residues ; however, the data summary indicates that overall residues were slightly higher in both forage and stover following two applications wi th a 5

- to 8

- day PHI.

No residue decline data were included in the submission; however, residue decline data

submitted with the Canad ian sweet corn field trials indicated that residues of acetamiprid generally declined with increasing PHI in sweet corn forage and stover.Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 15 of 25 

### Canad ian trials

IR

- 4 has submitted field trial data for acetamiprid on sweet corn. During the 2006 growing

season, 8 field trials w ere conducted in Canada in the following North American Free Trade Agreement (NAFTA) Growing Zones: 5 (ON; 4 trials); 5B (QC; 2 trials); 7A (AB; 1 trial); and 12 (BC; 1 trial). The two pairs of ON trials and the two QC trials were conducted by the same

FRDs at the same trial locations. Careful examination of the field trial records indicates that the only differences between the two trials in each pair were the use of different tank mixes for all applications, different crop varieties, and a 6

- to 7

- day offset in application dates (ON trials). HED has concluded that the differences between the trials are insufficient to classify them as separate trials; therefore, each trial pair constitutes a single trial with replicate samples for

purposes of OCSPP 860.1500/PMRA Regulatory Directive 98

- 2 data requirements. The adjustment in trial numbers results in a total of five field trials, with two trials conducted in

NAFTA Zone 5 and one trial each conducted in NAFTA Zone s 5B , 7A and 12

.

Each trial consisted of one untreated plot and one treated plot. T he treated plots received four foliar broadcast applications of a 70% WP f ormulation of acetamiprid (Assail® 70 WP) at 0.052

- 0.056 lb ai/A/application (58.7

- 62.6 g ai/ha/application) for a total seaso nal rate of 0.213

- 0.219 lb ai/A (238.5

- 245.4 g ai/ha) . Due to an oversight by field personnel, the first three applications

at the AB trial site were made at 0.074

- 0.077 lb ai/A (82.7

- 86.6 g ai/ha), which resulted in a total

seasonal rate of 0.281 lb ai/A (314.7 g ai/ha). Applications were made at 6

- to 8

- da y RTIs u sing ground equipment

, in spray volumes of 20.8

- 77.0 gal/A (194

- 720 L/ha). An adjuvant was not added to the spray mixtures at any of the trial sites. Samples of sweet corn K+CWHR an d forage

w ere harvested at PHIs of 1

- 2 days; stover samples were harvested at maturity at PHIs of 38

- 89 days. To assess residue decline, i n one ON trial, additional samples were harvested at PHIs of 0, 3, and 7 days for K+CWHR and forage, and at 70, 83, and 90 days (target PHI = 76 days) for

stover.

Samples were analyzed for residues of acetamiprid using an adequate LC/MS/MS method, and the study is supported by acceptable storage stability data (see Table 7).

The results of the sweet corn field trials are present ed in Table 1 0 (below)

. Following four foliar broadcast applications of the 70% WP formulation of acetamiprid at a total rate of 0.213

- 0.281 lb ai/A (238.5

- 314.7 g ai/ha), acetamiprid residues (and per trial averages) were <0.01 (<0.01) ppm

in/on K+CWHR a nd 0.23

- 1.1 (0.43

- 0.82) ppm in/on forage harvested at PHIs of 1

- 2 days, and

<0.01

- 0.35 (0.011

- 0.285) ppm in/on stover harvested at PHIs of 38

- 89 days. It was note d that the highest residues in stover (0.22 and 0.35 ppm) were observed in/on samples from th e AB trial which received a total seasonal application rate of 0.281 lb ai/A (314.6 g ai/ha). Although this rate exceeded the target application rate by ~ 33 %, which is higher than the general HED policy

to only include application rates within 25% of the target, residues in these samples were still included in the summary data calculations

. As summarized in Table 10, the maximum stover residues observed in the Canadian trials are far exceeded by those in the U.S. trials, with the U.S. trials all having ap plication rates within 25% of the target. Excluding this AB trial from the tolerance calculations would have no impact on the final result.Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 16 of 25 

### In the residue decline trial, residues of acetamiprid generally declined with increasing PHI in

sweet corn fora ge and stover. Residues in K+CWHR were below the LOQ at all harvest intervals; therefore, residue decline could not be assessed.

Table 1 0

. Summary of Residue Data from Sweet Corn Crop Field Trials with Acetamiprid.

Com

modity No.

Apps. Total Applic.

Rate (lb ai/A) PHI

(days) Residue Levels (ppm) 1

n Sampl

e Min. Sample

Max. LAFT 2 HAFT 2 Median Mean Std.

Dev.

SWEET CORN (proposed use = 0.21 lb ai/A total application rate; 4 applications with a 1

- day PHI or 2 applications with a 7

- day PHI)

U.S. Trials (30% SG formulation)

K+CWHR 4 0.212

- 0.220 1 7 <0.01 <0.01 0.01 0.01 0.01 0.01 N/A

2 0.195

- 0.214 5

- 8 7 <0.01 <0.01 0.01 0.01 0.01 0.01 N/A

Forage 4 0.212

- 0.220 1 7 0.42 8.1 0.54 7.3 1.3 3.0 2.8

2 0.195

- 0.214 5

- 8 7 0.39 10 0.41 9.1 1.4 2.9 3.1

Stover 4 0.212

- 0.220 1 3 7 0.12 16 0.19 15.5 4.1 5.7 5.7

2 0.195

- 0.214 5

- 8 3 7 0.21 21 0.21 20 2.8 5.3 7.0

Canada Trials (70% WP formulation)

K+CWHR 4 0.213

- 0.281

(238.5

- 314.7) 1

- 2 5 <0.01 <0.01 0.01 0.01 0.01 0.01 N/A

Forage 4 5 0.23 1.1 0.43 0.82 0.61 0.60 0.15

Stover 4 0.213

- 0.2 81

(238.5

- 314.7 ) 38

- 89 5 <0.01 0. 35 0.011 0. 285 0.0 50 0.0 82 0.0 95

1 Except for sample min/max, values reflect per trial averages; n = no. of field trials. N/A = Not applicable

2 LAFT = lowest average field trial; HAFT = highest average field trial.

3 Including PHIs of 28 and 35 days for stover from plots 2 and 3 of the NY trail , respectively. Although the PHIs

from this trial differed by >25%, this data was included in the summary re sults because the residues were within the range of those in the other trials, and the use pattern was consistent with typical stover harvest

.



### Conclusions . The submitted residue data for sweet corn are acceptable. The study reflects the maximum propos ed use patterns for sweet corn, and, if the U.S. and Canadian field trials are combined, the number and location of the field trials are in accordance with OCSPP 860.1500 for sweet corn (refer to Appendix I ). A cceptable methods were used for residue quant itation,

and th e studies are su pported by adequate storage stability data.

In considering the available data, HED has now concluded that sufficient data have been submitted to support th e use on sweet corn. T here is evidence to support residue equivalency for

the 70% WP formulation and the 30% SG formulation and the combination of trials conducted with these two formulations provide for an adequate number of trials with sufficient geographi c variation. In the previous review of this dataset, HE D concluded that the U.S. and Canadian trial

dataset could not be combined due to the significant differences in the stover PHIs between the

U.S. and Canadian trials. These differences are reflected in the residue data for stover. In the U.S. trials, res idues (and per trial averages) of acetamiprid were <0.01 (<0.01) in K+CWHR,

0.39

- 10 (0.41

- 9.1) in forage, and 0.12

- 21 (0.19

- 20) ppm in stover. In the Canadian trials, residues (and per trial averages) were <0.01 (<0.01) in K+CWHR, 0.23

- 1.1 (0.43

- 0.82) in forage,

and <0.01

- 0.35 (0.011

- 0.285) ppm in stover. Specifically, stover was harvested with a PHI of 1 to 2 day s in the U.S. trials, then allowed to dry in the field or in the test facility prior to analysis.Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 17 of 25 

### In contrast, in the Canadian trials the stove r was allowed to dry in the field, a process which took

41

- 89 days, prior to harvesting and analysis.

T he use patterns were similar between the U.S. and Canadian trials for K+CWHR and forage (four applications, 1

- to 2

- day PHI). Another use pattern dif ference noted in the 2012 HED review was the use of adjuvants. T he U.S. trials performed with the 30% SG formulation included an adjuvant, whereas the Canadian trials using the 70% WP formulation did not include an adjuvant. However, HED’s ChemSAC recent ly concluded that the inherent variability in field trials, coupled with the characteristics and conservative nature of the OECD tolerance calculation method exceeds the variability seen with the use of adjuvants . Therefore, the adjuvant

differences obser ved in the U.S. and Canadian field trials are no longer considered to be an issue.

HED conclude s that the available data are sufficient for establishing tolerances associated with the requested registration at this time. No additional data are required

.



## Processed Food and Feed (860.1520)

There are no significant processed commodities associated with the proposed uses on sweet corn

.



## Submittal of Analytical Reference Standards (860.1650)

Analytical standards for acetamiprid and metabolites IM

- 2

- 1, a nd IM

- 2

- 2 are currently available in the EPA National Pesticide Standards Repository, confirmed via personal email

communication with T. Cole, of BEAD’s Analytical Chemistry Branch (ACB), 02/26/13. However, there is only a small quantity of acetamiprid standard remaining. Therefore, 5 grams of the analytical reference standard for acetamiprid should be supplied to the Repository as soo n as possible. The reference standards should be sent to ACB, which is located at Fort Meade, to the attention of either Theresa Cole or Frederic Siegelman at the following address:

USEPA National Pesticide Standards Repository/Analytical Chemistry Bra nch/OPP 701 Mapes Road Fort George G. Meade, MD 20755

- 5350

(Note that the mail will be returned if the extended zip code is not used.)



## Rotational Crops (Field; 860.1900)

Residue Chemistry Memo DP# 328216, 10/23/2007, W. Drew (PP#6F7051 and PP#6E7163)



### No field rotational crop data have been submitted, and no rotational crop restrictions are established on the subject labels . The available confined rotational crop data indicate that no field rotational crop studies or label restrictions for rotational crops are required to support the proposed uses.Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 18 of 25 

## Tolerance Derivation

Residue Chemistry Memo D 264154, 12/31/2001, M. Doherty (PP#0F6082)



### Tolerances are currently established under 40 CFR §180.578(a)(1) for residues of the insecticide, acetamiprid, to b e determined by measuring only acetamiprid, in or on crop matrices. The tolerance expression proposed by IR

- 4 in this petition is consistent with 40 CFR §180.578(a)(1).

Sweet corn. Sufficient sweet corn field trial data have been submitted to establish tolerances associated with the requested registration of the 70% WP formulation and the 30% SG formulation. The available field trial data will support the proposed tolerances of 0.01 ppm in sweet corn (kernel plus cob with husks removed), 15 p pm in sweet corn forage, and 30 ppm in

sweet corn stover. The OECD tolerance calculation procedure (March 2011 version) was utilized in determining the appropriate tolerance levels. Average values from the sweet corn

field trials were used.

Livestock co mmodities . The available sweet corn residue data indicate that the established tolerances on milk and the fat, meat and meat byproducts of cattle, goat, horse and sheep will be

too low once the requested use on sweet corn has been registered. Therefore, HED recommends that the livestock tolerances be revised as follows to address the increased anticipated livestock dietary burden: t he tolerance in milk should be increased from 0.10 to 0.30 ppm, and the tolerances in the fat, meat and meat byproducts of ca ttle, goat, horse and sheep should be increased from 0.10 to 0.20 ppm in fat; from 0.10 to 0.30 ppm in meat; and from 0.20 to 0.70 ppm in meat byproducts. See earlier section on Meat, Milk, Poultry, and Eggs (860.1480) for

additional information on the de rivation of these recommended tolerances.

There are currently no established Codex, Canadian or Mexican MRLs for acetamiprid on sweet

corn ; therefore, there are no issues of harmonization

. There are Codex and Canadian MRLs on livestock commodities, wit h the revised livestock tolerances for the U.S. being higher than both

the Codex and Canadian values. Given the requested use on sweet corn, these higher tolerances in the U.S. are warranted. However, this is not considered to be a significant trade irritant, as livestock commodities are rarely shipped internationally. An International Residue Limit Status Sheet (IRLS) follows th e references in this document.

The proposed and recommended tolerances for acetamiprid as a result of the subject action are presented in Table 1

.

References

MARC Decision Memo, D278652, 11/13/2001, M. Doherty DER Reference: 44988601.der, 12/14/01, H. Bietlot Residue Chemistry Memo D394779, 03/06/2012, E. Holman (PP#

R esidue Chemistry Memo D 264154, 12/31/2001, M. Doherty (PP#0F6082) Residue Chemistry Memo D303623, 11/05/2004, W. Drew (PP#4F6833)

Residue Chemist ry Memo D328216, 10/23/2007, W. Drew (PP#6F7051 and PP#6E7163) Residue Chemistry Memo D342549 & D 355773, 11/05/2008, W. DrewAcetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 19 of 25 

### Attachment 1. International Maximum Residue Limits

– Acetamiprid

.



## Acetamiprid (PC Code 099050)

Summary of US and International Tolerances and Maximum Residue Limits Residue Definition :
US Canada Mexico 2 

### Codex 3

40 CFR 180.578:

Plants: acetamiprid (1 E )

- N

- [(6

- chloro

- 3

- pyridinyl)methyl]

- N ′

-

cyano

- N

– methylethanimidamide

Livestock: acetamiprid and (1 E )

- N

- [(6

- chloro

- 3

- pyridinyl)methyl]

- N ′

-

cyano

- N

- ethanimidamide Plants: (1 E )

- N

- [(6

- chloro

- 3

- pyridinyl)methyl]

- N'

- cyano

- N

methylethanimidamide

Livestock:(1 E )

- N

- [(6

- chloro

- 3

- pyridinyl)methyl]

- N'

- cyano

- N

methylethanimida mide, including the metabolite (1 E )

- N

- [(6

- chloro

3

- pyridinyl)methyl]

- N'

- cyanoethanimidamide Plants: acetamiprid

Livestock: sum of acetamiprid and its desmethyl (IM

- 2

- 1) metabolite, expressed as acetamiprid.

The residue is not fat

soluble.



### Commodity 1 

### Tolerance (ppm) /Maximum Residue Limit (mg/kg)

US Canada Mexico 2 

### Codex 3

Corn, sweet, kernel plus cob

with husks removed 0.01

Corn, sweet, forage 10
Corn, sweet, stover 30

Milk 0.30 0.1 0.02
Cattle, fat 0.20 0.1 0.02 Mammalian fats (except milk fats)
Cattle, meat 0.30 0.1 0.02 Meat from

mammals other than

marine mammals. Cattle, meat byproducts 0.70 0.3 0.05 Edible offal (mammalian)
Goat, fat 0.20 0.1 0.02 Mammalian fats (except milk fats)
Goat, meat 0.30 0.1 0.02 Meat from

mammals other than

marine mammals. Goat, meat byproducts 0.70 0.3 0.05 Edible offal (mammalian)
Horse, fat 0.20 0.1 0.02 Mammalian fats (except milk fats)
Horse, meat 0.30 0.1 0.02 Meat from

mammals other than

marine mammals. Horse, meat byproducts 0.70 0.3 0.05 Edible offal (mammalian) Sheep, fat 0.20 0.1 0.02 Mammalian fats (except milk fats) Sheep, meat 0.30 0.1 0.02 Meat from

mammals other than

marine mammals.Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 20 of 25 

### Summary of US and International Tolerances and Maximum Residue Limits Residue Definition :
US Canada Mexico 2 

### Codex 3

Sheep, meat byproducts 0.70 0.3 0.05 Edible offal (mammalian)

Completed: M. Negussie; 02/27/2013

1 Includes only commodities of interest for this action. Tolerance values should be the HED recommendations and not those proposed by the applicant.

2 Mexico adopts US tolerances and/or Codex MRLs for its export purposes.

3 * = absent at the limit of quantitation; Po = postharvest treatment, such as treatment of stored grains. PoP = processed postharvest treated commodity, such as processing of treated stored wheat. (fat) = to be measured on the fat portion of the sample. MR Ls indicated as proposed have not been finalized by the CCPR and the CAC.Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 21 of 25 

### Appendix I . Field Trial Geographic Distribution

.

T able I .3. Trial Numbers and Geographical Locations for Sweet Corn

. NAFTA Growing Zones Sweet Corn

Submitted Requested 1

Canada U.S. Canada U.S.

1

-- 1

-- 2/1

1A

-- -- -- --
2

-- 2

-- 1/1

3

-- 1

-- 1/1

4

-- -- -- --
5 2 2

-- 4 5/3

5A

-- 1

-- --
5B 1 2

-- 2

--

6

-- -- -- --

7

-- -- -- --
7A 1

-- 1

--
8

-- -- -- --
9

-- -- -- --
10

-- 1

-- 1/1

11

-- 1

-- 1/1

12 1

-- 1 1/1

13

-- -- -- --
14

-- -- -- --
15

-- -- -- --
16

-- -- -- --
17

-- -- -- --
18

-- -- -- --
19

-- -- -- --
20

-- -- -- --
21

-- -- -- --

Total 5 7 8 12/9

1 As per Table 5 of OCSPP 860.1500 and Table 2 of PMRA Regulatory Directive 98

- 2 for sweet corn; the second number reflects a 25% reduction in the number of field trials allowed for the crop as a representative commodity in support of a cro p group/subgroup t olerance or when application results in no quantifiable residues.

2 HED has concluded that two pairs of the Zone 5 trials (131/132 and 133/134) and the two Zone 5B trials (136/137) each constitute a single trial with replicate samples for purposes of 86 0.1500 data requirements.Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 22 of 25 

### Appendix II. Tolerance Assessment Calculations

.

T he OECD tolerance calculation procedure (March 2011 version), was used for calculating

recommended tolerances in sweet corn . The statistical goal of the OECD tolerance calculation procedure is to produce a tolerance proposal in the region of the 95 th 

### percentile of the underlying residues distribution. The average residue values used to calculate the tolerances are provided in

Table I

- 1.

Table I I

- 1. Residue data used to calculate tolerance for acetamiprid in/on sweet corn (K+CWHR, forage, and stover)

. Regulator: EPA

Chemical: Acetamiprid

Crop: Sweet corn

(K+CWHR) Sweet corn, forage Sweet corn, stover

PHI: 1

- 2 Day s 1

- 2 Days 1

- 2 (U.S.);

38

- 89 (CAN)

App. Rate: 0. 195

- 0.281 lb ai/A 0. 195

- 0.281 lb ai/A 0. 195

- 0. 281 lb ai/A

Submitter: IR

- 4 IR

- 4 IR

- 4

MRID Citation: MRID 48590103,

48590104 MRID 48590103,

48590104 MRID 48590103,

48590104

Acetamiprid (ppm)



### <0.01 0.630 15.500



### <0.01 0.430 20.000



### <0.01 0.610 0.190



### <0.01 0.820 0.210



### <0.01 0.490 4.100



### <0.01 7.300 2.750



### <0.01 9.050 11.500



### <0.01 0.535 8.350



### <0.01 0.410 0.430



### <0.01 0.850 0.445



### <0.01 0.760 3.200



### <0.01 6.250 2.750



### <0.01 4.650 4.750



### <0.01 1.750 2.550



### <0.01 2.350 0.031



### <0.01 1.250 0.011



### <0.01 1.350 0.052



### <0.01 3.350 0.116



### <0.01 1.400 0.285Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 23 of 25 

### Sweet corn (K+CWHR)

The dataset used to establish a tolerance for acetamiprid on sweet corn (K+CWHR) consisted of field trial data representing application rates of 0.195

- 0.281 lb ai/A acetamiprid with a 1

- 2 day PHI. The field trial application rates and PHIs are generally w ithin 25% of the maximum label application rate and minimum label PHI, respectively. The average residue values used to calculate the tolerance are provided in Table I I

- 1. Residues of acetamiprid were not quantifiable (LOQ = 0.01 ppm) in/o n all samples o f sweet corn (K+CWHR)

. Using the OECD tolerance calculation procedure , the recommended tolerance is 0.01 ppm.

Acetamiprid

K+CWHR

USA and Canada

GAP

Total number of data (n) 19
Percentage of censored data 100%

Number of non

- censored data 0

Lowest residue 0.010

Highest residue 0.010

Median residue 0.010

Mean 0.010

Standard deviation (SD) 0.000
Correction factor for censoring (CF) 0.333

Proposed MRL estimate

- Highest residue 0.010

- Mean + 4 SD 0.010

- CF x 3 Mean 0.010

Unrounded MRL 0.010

Rounded MRL 0.01

High uncertainty of MRL estimate.

[High level of censoring]Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 24 of 25 

### Sweet corn forage

The dataset used to establish a tolerance for acetamiprid on sweet corn forage consisted of field trial data representing application rates of 0.195

- 0.281 lb ai/A acetamiprid with a 1

- 2 day PHI. The field trial application rates and PHIs are generally within 25% of the maximum label application rate and minimum label PHI, respectiv ely. The average residue values used to calculate the tolerance are provided in Table I I

- 1. Residues of acetamiprid were quantifiable (LOQ = 0.01 ppm) in/o n all samples of sweet corn forage

. Using the OECD tolerance calculation procedure , the recommende d tolerance is 15 ppm.

Acetamiprid

Forage

USA and Canada

GAP

Total number of data (n) 19
Percentage of censored data 0%

Number of non

- censored data 19

Lowest residue 0.410

Highest residue 9.050

Median residue 1.250

Mean 2.328

Standard deviation (SD) 2.600
Correction factor for censoring (CF) 1.000

Proposed MRL estimate

- Highest residue 9.050

- Mean + 4 SD 12.728

- CF x 3 Mean 6.984

Unrounded MRL 12.728

Rounded MRL 15Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D 409727

Page 25 of 25 

### Sweet corn stover

The dataset used to establish a tolerance for acetamiprid on sweet corn forage consisted of field trial data representing application rates of 0.195

- 0. 281 lb ai/A acetamiprid with a 1

- 2 day PHI in

the U.S. trials and a 38

- 89 day PHI in the Canadian trials

. The field trial application rates and

PHIs are generally within 25% of the maximum label application rate and minimum label PHI, respectively. The average residue values used to calculate the tolerance are provided in Table I I

1. Residues of acetamipri d were quantifiable (LOQ = 0.01 ppm) in/o n all samples of sweet corn

stover

. Using the OECD tolerance calculation procedure , the recommended tolerance is 30 ppm.

Acetamiprid

Stover

USA and Canada

GAP

Total number of data (n) 19

Percentage of censored data 0%

Number of non

- censored data 19

Lowest residue 0.011
Highest residue 20.000

Median residue 2.550

Mean 4.064

Standard deviation (SD) 5.774
Correction factor for censoring (CF) 1.000

Proposed MRL estimate

- Highest residue 20.000

- Mean + 4 SD 27.162

- CF x 3 Mean 12.193

Unrounded MRL 27.162

Rounded MRL 30