Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D409727 

UNITED STATES ENVIRONMENTAL PROTECTION AGENCY 

WASHINGTON, D.C. 20460 

OFFICE OF CHEMICAL SAFETY AND 

POLLUTION PREVENTION 

MEMORANDUM 

Date: March 12, 2013 

Subject: Acetamiprid. Petition for the Establishment of Permanent Tolerances and 

Registration for Use on Sweet Corn. Summary of Analytical Chemistry and Residue 

Data. 

From: 

Through: 

To: 

PC Code: 099050 

MRJD Nos.: (See MRJD summary) 

Petition Nos.: l E7919 

Assessment Type: NA 

TXRNo.: NA 

Decision Nos.: 474870 

DP Barcode: D409727 

Registration Nos.: 8033-23, 8033-36 

Regulatory Action: Section 3 

Registration Case No.: 7617 

CAS No.: 135410-20-7 

40 CFR § 180.578 

Elizabeth Holman, Physical Scientist ~ t}/--

Risk Assessment Branch II 

Health Effects Division (7509P) 

William T. Drew, Chemist~) ~ Risk Assessment Branch II 

Health Effects Division (7509P) 

Andrew Ertman, Chemical Review Manager 

Risk Integration Minor Use, and Emergency Response Branch 

Registration Division (7505P) 

And 

Jennifer UrbanskiNenus Eagle (Team 01) 

Insecticide/Rodenticide Branch 

Registration Division (7505P) 

Page 1 of25 
Acetamiprid 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 Method ......................... ............ ................................................................................. 5 

Recommended Tolerances .......................................................................................................... 5 

International Harmonization ....................................................................................................... 6 

Revisions to Petitioned-For Tolerances .......................................... ............................................ 6 

Residue Profile ................................................................................................................................ 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 

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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 (1E)-N-[(6-chloro-3-pyridinyl)methyl]-N'-cyanoN-methylethanimidamide} for post-emergent foliar use on sweet corn. The 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 registered 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). 

Acceptable 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 maximum seasonal rate and preharvest intervals (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 depicting 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 surfactant (NIS) adjuvant, and in Canada with the 

70% WP formulation applied as four applications without an adjuvant. In the earlier review of 

this residue data, it was noted that applications were made in accordance with the proposed 

labeling at all trials, except 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 D409727

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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 (D394779, 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 variability 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% 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 geographic variation.

Consequently, based on the conclusions of ChemSAC on adjuvant differences 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 

husks 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 tolerances 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 establishing tolerances in 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 formulation, 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, 

additional bridging data would be required to support the use of the 30% SG formulation. 

However, during a previous assessment, a similar situation was encountered 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, 12/01/2009). 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 be 
Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D409727

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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 follows: 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. 

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 acetamiprid, 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 electron 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 spectrometric 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 uses 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 

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. 

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 15 15

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 0.70
Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D409727

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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 C10H11ClN4

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 (1E)-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)

N N

CH3

Cl

CH3

N

CN
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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/cm3) 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 D264154, M. Doherty; 

12/31/2001

Dissociation Constant, pKa 0.7 (at 25 C) DP Barcode D328216, W. Drew, 

Octanol/Water Partition 10/23/2007

Coefficient, Log KOW

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

CH3

N

O

NH2

N N

H

C

l

CH3

N

CN
Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D409727

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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 

Limitations2

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 accepted 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 Canada with the 70% WP applied as four 

applications without an adjuvant. Applications were made in accordance with the proposed 

labeling at all trials.

Nature of the Residue (860.1300/1850)

Plants: Residue Chemistry Memo D264154, 12/31/2001, M. Doherty (PP#0F6082)

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

Livestock: Residue Chemistry Memo D264154, 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. Drew (PP#6F7051 and PP#6E7163)

Residue Chemistry Memo D264154, 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 to 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 the 
Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D409727

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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 showed 

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 

other 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 lactating 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 group 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 Assessment 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 & D355773, 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 D264154, 12/31/2001, M. Doherty (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/UV). 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 

alternative 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 confirmatory 

analysis of vegetables and non-citrus fruits (D342549 & D355773). A summary of the available 

methods is presented in Table 6.
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Table 5. Table 6. Summary of Validated Analytical Methods for Acetamiprid.

Target 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 

Canadian field trials were analyzed for residues of acetamiprid using an 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 analysis.

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 LCFlorisil 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 

identical to established 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 method validation and concurrent 
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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 Methods (860.1360)

Residue Chemistry Memo D264154, 12/31/2001, M. Doherty (PP#0F6082)

Data concerning the recovery of residues of acetamiprid using FDA multiresidue method 

protocols (PAM Volume I) were submitted in conjunction with the original acetamiprid 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 

were 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). No 0-day data were provided for any study. These data 

are acceptable to support the storage conditions and durations of samples from the submitted 

field trials; however, the 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 Residue 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 D409727

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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. 

The 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 Type1 % Dry 

Matter2 % Diet2

Established

Tolerance or HR3

(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 -- 35 -- --

Cotton, undelinted seed PC 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

 Contribution = [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 to dairy cattle. 
Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D409727

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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 

level1

Residues adjusted to 1x feeding level for 

dairy cattle

6 18 60 0.5x 1.4x 4.7x

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 LOQs 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 dietary 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 tissues.

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, nor in poultry or hog tissues.

Crop Field Trials (860.1500)

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

48590104.der (Sweet corn, Canadian 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 formulation 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.
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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 were 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 of 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. Applications were made at 4- to 8-day 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.

Samples 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 dryer or 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 10 (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 <0.01 (<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 remaining 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 patterns 

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 with a 5- to 8-day PHI. 

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

submitted with the Canadian sweet corn field trials indicated that residues of acetamiprid 

generally declined with increasing PHI in sweet corn forage and stover.
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Canadian trials 

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

season, 8 field trials were 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 Zones 5B, 7A and 12.

Each trial consisted of one untreated plot and one treated plot. The treated plots received four 

foliar broadcast applications of a 70% WP formulation 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 seasonal 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-day RTIs using 

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 and forage 

were harvested at PHIs of 1-2 days; stover samples were harvested at maturity at PHIs of 38-89 

days. To assess residue decline, in 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 presented in Table 10 (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 and 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 noted that 

the highest residues in stover (0.22 and 0.35 ppm) were observed in/on samples from the 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 application rates within 25% of the target. Excluding this AB trial from the 

tolerance calculations would have no impact on the final result. 
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In the residue decline trial, residues of acetamiprid generally declined with increasing PHI in 

sweet corn forage and stover. Residues in K+CWHR were below the LOQ at all harvest 

intervals; therefore, residue decline could not be assessed.

Table 10. Summary of Residue Data from Sweet Corn Crop Field Trials with Acetamiprid.

CommodityNo. 

Apps.

Total Applic. 

Rate

(lb ai/A)

PHI 

(days)

Residue Levels (ppm)1

n Sampl

e Min.

Sample 

Max.

LAFT2 HAFT2 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 0.213-0.281

(238.5-314.7)

38-89 5 <0.01 0.35 0.011 0.285 0.050 0.082 0.095

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 results 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 proposed 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). Acceptable methods were used for residue quantitation, 

and the studies are supported by adequate storage stability data.

In considering the available data, HED has now concluded that sufficient data have been 

submitted to support the use on sweet corn. There 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 geographic 

variation. In the previous review of this dataset, HED 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, residues (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 days in the U.S. trials, then allowed to dry in the field or in the test facility prior to analysis. 
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In contrast, in the Canadian trials the stover was allowed to dry in the field, a process which took 

41-89 days, prior to harvesting and analysis. 

The 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 difference noted in the 2012 HED 

review was the use of adjuvants. The 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 recently 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 observed in the U.S. and Canadian field trials are no longer considered to be an issue. 

HED concludes 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, and 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 soon 

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 Branch/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.
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Tolerance Derivation

Residue Chemistry Memo D264154, 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 be 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 ppm 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 commodities. 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: 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. See earlier section on Meat, Milk, Poultry, and Eggs (860.1480) for 

additional information on the derivation 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, 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 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 the 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#

Residue Chemistry Memo D264154, 12/31/2001, M. Doherty (PP#0F6082)

Residue Chemistry Memo D303623, 11/05/2004, W. Drew (PP#4F6833)

Residue Chemistry Memo D328216, 10/23/2007, W. Drew (PP#6F7051 and PP#6E7163)

Residue Chemistry Memo D342549 & D355773, 11/05/2008, W. Drew
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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 Mexico2 Codex3

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: (1E)-N-[(6-chloro-3-

pyridinyl)methyl]-N'-cyano-Nmethylethanimidamide

Livestock:(1E)-N-[(6-chloro-3-

pyridinyl)methyl]-N'-cyano-Nmethylethanimidamide, including 

the metabolite (1E)-N-[(6-chloro3-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. 

Commodity1 Tolerance (ppm) /Maximum Residue Limit (mg/kg)

US Canada Mexico2 Codex3

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 D409727

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Summary of US and International Tolerances and Maximum Residue Limits 

Residue Definition:

US Canada Mexico2 Codex3

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. MRLs indicated as proposed have not been finalized by the CCPR and the CAC.
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Appendix I. Field Trial Geographic Distribution.

Table I.3. Trial Numbers and Geographical Locations for Sweet Corn.

NAFTA Growing Zones Sweet Corn

Submitted Requested1

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 crop 

group/subgroup tolerance 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 860.1500 data requirements.
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Appendix II. Tolerance Assessment Calculations.

The 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 95th percentile of the underlying 

residues distribution. The average residue values used to calculate the tolerances are provided in 

Table I-1. 

Table II-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 Days 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 0.285
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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 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 II-1. Residues of acetamiprid were not quantifiable 

(LOQ = 0.01 ppm) in/on all samples of 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 D409727

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, respectively. The average residue values used to 

calculate the tolerance are provided in Table II-1. Residues of acetamiprid were quantifiable 

(LOQ = 0.01 ppm) in/on all samples of sweet corn forage. Using the OECD tolerance 

calculation procedure, the recommended 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 15
Acetamiprid Summary of Analytical Chemistry and Residue Data DP Barcode D409727

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 II1. Residues of acetamiprid were quantifiable (LOQ = 0.01 ppm) in/on 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