Acetamiprid Summary of Analytical Chemistry and Residue Data Barcode D394779

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Summary of Submitted Residue Chemistry Studies

OPPTS 860 Series 

Guideline

MRID 

Number

Title

860.1500 48590101 48590101 Samoil, K. (2011) Acetamiprid: Magnitude of the Residue on Asparagus. 

Project Number: 09939, 09939/08/MIR04. Unpublished study prepared by Interregional 

Research Project No. 4. 162 p.

48590102 48590102 Samoil, K. (2011) Acetamiprid: Magnitude of the Residue on Mustard Greens. 

Project Number: 09271, 09271/09/CAR05. Unpublished study prepared by Interregional 

Research Project No. 4, University of Arkansas and U.S. Dept. of Agriculture, Agr. Res. 

Serv. 147 p.

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 Unpublished study prepared by Interregional 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 Unpublished study 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 {(1E)-N-[(6-chloro-3-pyridinyl)methyl]-N'-cyano-Nmethylethanimidamide} for post-emergent foliar use on asparagus; Brassica leafy greens,

subgroup 5B, and turnip greens; and sweet corn. In addition, IR-4 is proposing to update crop 

group definitions for established tolerances for vegetable, fruiting, group 8-10; fruit, citrus, group 

10-10; and fruit, pome, group 11-10. 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).

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 

asparagus, brassica leafy vegetables and turnip greens, and sweet corn. Maximum seasonal rates 

and preharvest intervals (PHIs), respectively, are: 0.2 pounds active ingredient per acre (lb ai/A)

and 1 day for asparagus, 0.375 lb ai/A and 3 days for Brassica leafy vegetables and turnip 

greens, and 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 has submitted studies depicting residues of 

acetamiprid in/on asparagus, mustard greens, and sweet corn kernel + cob with husks removed 
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(K+CWHR), forage, and stover. The asparagus and mustard greens field trials were conducted 

in the U.S. and reflect application of the 70% WP formulation. The asparagus field trials were 

conducted with and without a non-ionic surfactant (NIS), whereas all mustard greens field trials 

included an NIS. 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 formulation applied as four applications without an adjuvant. 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). Stover samples from the 

Canadian trials were allowed to dry before harvest, while samples from the U.S. trials were 

harvested at the target PHIs and dried after harvest in a dryer or at ambient temperatures in the 

field or test facility.

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

The submitted crop field trial data for asparagus and mustard greens are adequate to support the 

proposed uses and are sufficient for establishing tolerances at 0.80 ppm in asparagus, and 15 

ppm in Brassica leafy greens, subgroup 5B, and turnip greens. Residues (and per trial averages) 

of acetamiprid were 0.11-0.43 (0.12-0.41) ppm in/on asparagus and 0.20-10 (0.30-9.2) ppm in/on 

mustard greens. 

HED has concluded that insufficient data have been submitted to support the use on sweet corn. 

Although 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, it is not possible to 

combine the two sets 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. Furthermore, although the use patterns were similar between the 

U.S. and Canadian trials for K+CWHR and forage (four applications, 1- to 2-day PHI), 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. Additional crop field trial data are 

required to support the proposed uses. 

Regulatory Recommendations

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

and establishing tolerances in asparagus, Brassica leafy greens, subgroup 5B and turnip greens. 

The labels for the 70% WP and 30% SG formulations should be modified to prohibit the harvest 

of turnip roots for food/feed purposes, and to specify use of an NIS as adjuvant for applications 

to asparagus, brassica leafy greens, and turnips. Furthermore, it was noted that the draft label for 

the 30% SG formulation includes the following error in the “Site” column: “Pome Fruit (within 

Crop Group 11)” instead of “Pome Fruit (within Crop Group 11-10)”. This error should be 

corrected on the label.
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There are no residue chemistry considerations which would preclude granting registration of the 

70% WP and 30% SG formulations for use on asparagus, Brassica leafy greens, subgroup 5B 

and turnip greens. It is noted that all of the submitted field trials for asparagus and mustard 

greens used the 70% WP 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, 12/1/09). Therefore bridging 

data to support the use of the 30% SG formulation on these commodities are not required. 

With the establishment of a tolerance in Brassica, leafy greens, subgroup 5B, the established 

tolerance in vegetable, Brassica, leafy, group 5, should be removed, and a new tolerance should 

be established in Brassica, head and stem, subgroup 5A, at 1.2 ppm. No additional data are 

required to support this tolerance, as adequate residue data were previously submitted and 

reviewed (D264154, 12/31/01, M. Doherty). This petition requests a revised use pattern for 

subgroup 5B commodities, specifically a shorter PHI; therefore, a higher U.S. tolerance of 15 

ppm is required. 

The available residue chemistry data for acetamiprid are insufficient for assessing risk and 

establishing tolerances for use of the 30% SG and 70% WP formulations on sweet corn. Until 

the requested sweet corn field trial data have been submitted, this use should be removed from 

both labels. Tolerances in sweet corn K+CWHR, forage, and stover will not be established until 

the outstanding data have been received. The registrant has been made aware of this data gap 

and will be submitting additional field trial data at a later date. 

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 data currently 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 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. HED 

recommends that the tolerances not be revised at this time, but be re-evaluated when the 

outstanding data for sweet corn have been submitted and reviewed.

The established tolerances in vegetable, fruiting, group 8; fruit, citrus, group 10; and fruit, pome, 

group 11, can be updated to the current crop group definitions (with no accompanying data) to 

vegetable, fruiting, group 8-10; fruit, citrus, group 10-10; and fruit, pome, group 11-10.

Pre-Registration Data Needs

Asparagus; Brassica leafy vegetables, group 5 and subgroups 5A and 5B; and turnip greens

The petitioner should submit a revised Section F, specifying the recommended tolerances in 

Table 1, below.
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Sweet corn

Five additional crop field trials should be conducted in the U.S. with the 30% SG formulation 

and an adjuvant in Zones 1 (1 trial), 5 (3 trials), and 12 (1 trial) to provide a full set of field trial 

data for this formulation. Each trial should include an additional side-by-side treated plot 

reflecting application of the 70% WP formulation with an adjuvant. Although the available data 

suggest that residues are similar following application according to the four-application/1-day 

PHI use pattern and the two-application/7-day PHI use pattern, HED recommends that each use 

pattern be represented in at least two of the required trials. The registrant has been made aware 

of these issues and intends to complete the required trials during the 2012 growing season. 

When the outstanding data for sweet corn have been submitted and reviewed, the established 

tolerances in milk and the fat, meat, and meat byproducts of cattle, goat, horse, and sheep should 

be re-evaluated. 

Tolerance Considerations

Analytical Method

Approved tolerance enforcement methods for crops are available for acetamiprid, including gas 

chromatography with electroconductivity 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 spectrometry 

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)

Asparagus 0.8 0.80

Brassica, leafy greens, subgroup 5B 15 15

Turnip greens 15 15 Turnip, greens

Vegetable, brassica, leafy, group 5 1.20 None With the establishment of the 

separate 5B tolerance, the 
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Table 1. Tolerance Summary for Acetamiprid.

Commodity Established/Proposed 

Tolerance (ppm)

Recommended 

Tolerance (ppm)

Comments (Correct 

Commodity Definition)

group 5 tolerance should be 

removed. 

Brassica, head and stem, subgroup 

5A

-- 1.2 Using the existing group 5 

tolerance and available data, 

this separate 5A tolerance can 

be established without 

additional data. 

Corn, sweet, kernel plus cob with 

husks removed

0.01 To be determined Insufficient data are available 

to support the proposed 

use/tolerances for sweet corn 

at this time.

Corn, sweet, forage 10

Corn, sweet, stover 30

Vegetable, fruiting, group 8 0.20 None

Fruit, citrus, group 10 0.50 None

Fruit, pome, group 11 1.0 None

Vegetable, fruiting, group 8-10 0.20 0.20

Fruit, citrus, group 10-10 0.50 0.50

Fruit, pome, group 11-10 1.0 1.0

International Harmonization

There are currently no established Codex, Canadian, or Mexican maximum residue limits 

(MRLs) for acetamiprid on asparagus and no established Codex MRLs on any Brassica

vegetables; therefore, there are no issues of harmonization. Canadian MRLs are established for 

residues of acetamiprid at 1.2 ppm in/on Chinese cabbage (Bok choy), cabbages, broccoli raab, 

collards, kale, mustard greens, mustard spinach, and rape greens. With the establishment of 

separate tolerances in leafy greens, subgroup 5B, and Brassica head and stem, subgroup 5A, the 

Canadian MRLs for Bok choy Chinese cabbages, broccoli raab, collards, kale, mustard greens, 

mustard spinach, and rape greens will no longer be harmonized with U.S. tolerances. This 

petition requests a revised use pattern for subgroup 5B commodities, specifically a shorter PHI; 

therefore, a higher U.S. tolerance of 15 ppm is required. (Subgroup 5B includes bok choy 

Chinese cabbage, broccoli raab, collards, kale, mustard greens, mustard spinach, and rape 

greens.) 

Revisions to Petitioned-For Tolerances

No revisions relative to the petitioned-for tolerances are necessary for asparagus; Brassica leafy 

greens, subgroup 5B; or turnip greens. In keeping with HED conventions for tolerance rounding 

and significant figures, the proposed tolerance for asparagus was changed from 0.8 ppm to 0.80 

ppm. 

With the establishment of a tolerance in Brassica leafy greens, subgroup 5B, the established 

tolerance in vegetable, Brassica, leafy, group 5, should be removed, and a new tolerance should 

be established in Brassica, head and stem, subgroup 5A, at 1.2 ppm. 
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Insufficient data are available to support the proposed tolerances in corn, sweet, kernel plus cob 

with husks removed; corn, sweet, forage; and corn, sweet, stover. Until the outstanding field 

trial data are received, no tolerances will be established. 

No revisions are necessary relative to the petitioned-for tolerances updating the crop group 

definitions for vegetable, fruiting, group 8-10; fruit, citrus, group 10-10; and fruit, pome, group 

11-10. The existing tolerances for the old crop group definitions should be removed. 

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)

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, 

N N

H

Cl

CH3

N

O

NH2

N N

H

C

l

CH3

N

CN

N N

CH3

C

l

CH3

N

CN
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Table 3. Physicochemical Properties of Technical-Grade Acetamiprid.

Parameter Value Reference

pH 6.08 (Aqueous solution at 20 C) 10/23/2007

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.

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

Asparagus

Post-emergence, 

Broadcast, 

Aerial (≥5 

gal/A) or

ground, (≥20 

gal/A)

Assail®

70 WP

[8033-23]

0.05-0.1 2 0.2 1 Minimum RTI = 10 days

Assail®

30 SG

[8033-36]

0.047-0.1

Head and Stem Cole Crops (Crop Subgroup 5A):

Broccoli, Chinese broccoli (gai lon), Brussels sprouts, Cabbage, Chinese Cabbage (bok choy, napa), Chinese 

mustard cabbage (gai choy), Cavalo broccolo, Cauliflower, Kohlrabi

No change from established use pattern for Cole Crops (within Group 5)3
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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

Leafy Cole Crops (Crop Subgroup 5B) and Turnip Greens:

Broccoli raab (rapini), Collards, Kale, Mizuna, Mustard greens, Mustard spinach, Rape greens, Turnip greens

Post-emergence, 

Broadcast, 

Aerial (≥5 

gal/A) or

ground, (≥30 

gal/A)

Assail®

70 WP

[8033-23]

0.035-0.1 4 0.375 3 Minimum RTI = 7 days

Assail® 

30SG

[8033-36]

0.038-0.1

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)

Fruiting Vegetables (within Crop Group 8-10):

Eggplant (including African, pea, scarlet), Cocona, Garden huckleberry, Goji berry, Groundcherry, Martynia, 

Naranjilla, Okra, Pepino, Pepper (bell, nonbell), Roselle, Sunberry, Tomato (including bush, currant, tree), 

Tomatillo & Cultivars, varieties and/or hybrids of these

No change from established use pattern for Fruiting Vegetables (within Crop Group 8)3

Citrus (within Crop Group 10-10):

Calamondin, Citron, Citrus Hybrids, Grapefruit, Japanese summer grapefruit, Kumquat, Lemon, Lime (including 

Australian desert, Australian finger, Australian round, Brown River finger, Mount White, Russell River, sweet, 

Tahiti, New Guinea Wild), Mandarin (Mediterranean, Satsuma), Orange (sweet, sour, tachibana, trifoliate), 

Pummelo, Tangelo, Tangor, Uniq fruit & Cultivars, varieties and/or hybrids of these

No change from established use pattern for Citrus (within Crop Group 10)3

Pome Fruit (within Crop Group 11-10):

Apple, Azarole, Crabapple, Loquat, Mayhaw, Hook, Medlar, Pear (including Asian), Quince (including Chinese, 

Japanese), Tejocote & Cultivars, varieties, and/or hybrids of these.

No change from established use pattern for Pome Fruit (within Crop group 11)3

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 a NIS, methylated seed oil, or horticultural oil, is recommended 

for use on orchard and vine crops, except on grapes. With regard to adjuvant use, the labels state 

“Please see specific crop use directions.” The specific crop use directions for asparagus do not 

mention the use of an adjuvant. For leafy cole crops (subgroup 5B), the specific use directions 

recommend the use of an adjuvant (type not specified) for control of whiteflies. 
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It was noted that the use on the draft label for cabbage, Chinese bok choy, which is a member of 

subgroup 5B, will be covered under subgroup 5A with the established use pattern for cole 

(Brassica) crops. 

Conclusions. The labels are adequate to allow evaluation of the residue data relative to the 

proposed uses on asparagus; Brassica leafy greens, subgroup 5B, and turnip greens; and sweet 

corn. 

The asparagus and mustard greens field trials were conducted in the U.S. and reflect application 

of the 70% WP formulation with and without an NIS for asparagus, and with an NIS for mustard 

greens. 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, except that the Canadian sweet corn field trials reflected a significantly 

longer PHI for stover (38-89 days).

HED has concluded that insufficient data have been submitted to support the use of either the 

70% WP or the 30% SG formulation on sweet corn. Until the requested crop field trial data have 

been submitted, use on sweet corn should be removed from both labels. 

In support of the proposed use on turnip greens, the label(s) should be revised to prohibit the 

harvest of turnip root for food/feed purposes because use on turnip root is not supported by 

residue data or an established tolerance. 

In support of the proposed use on Brassica leafy greens, subgroup 5B, the label(s) should be 

revised to include Chinese Bok Choy with the subgroup 5B commodities. Chinese Bok Choy is 

currently misplaced on the labels with subgroup 5A commodities. 

The labels should specify use of an NIS as adjuvant for the asparagus, Brassica leafy greens and 

turnip greens uses because other adjuvant types were not tested. 

It was noted that the draft label for the 30% SG formulation includes the following error in the 

“Site” column: “Pome Fruit (within Crop Group 11)” instead of “Pome Fruit (within Crop 

Group 11-10)”. This error should be corrected on the label. 

Nature of the Residue (860.1300/1850)

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

MARC Decision Memo, DP# 278652, 11/13/2001, M. Doherty

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

MARC Decision Memo, DP# 278652, 11/13/2001, M. Doherty

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

Residue Chemistry Memo DP# 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 to be little translocation of 

acetamiprid following foliar application. In cabbage, there was uptake and translocation of 
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acetamiprid to the above-ground portions of the plant following a soil application. Due to the 

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 (>90% 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 DP#s 342549 & 355773, 11/05/2008, W. Drew

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

Residue Chemistry Memo DP# 303623, 11/05/2004, W. Drew (PP#4F6833)

Residue Chemistry Memo DP# 264154, 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 
Acetamiprid Summary of Analytical Chemistry and Residue Data Barcode D394779

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analysis of vegetables and non-citrus fruits (DP#s 342549 & 355773). A summary of the 

available methods is presented in Table 6.

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 asparagus, mustard greens, and 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 Canada 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 asparagus, mustard greens, and 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.
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Conclusions. The methods used in the submitted asparagus, mustard green, and 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 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 DP# 264154, 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 asparagus for intervals of up to 426 days

(14.2 months), mustard greens for up to 394 days (13.0 months), and 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, 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 860.1380(d)(6)(i)].

The storage durations and conditions of samples from the asparagus, mustard green, and 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

Asparagus -20 70-473 days (2.3-15.6 months) Up to 426 days (14.0 months) in/on asparagus

Mustard greens 160-382 days (5.3-12.6 months) Up to 394 days (13.0 months) in/on mustard 

greens

Sweet corn, K+CWHR 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 asparagus, mustard greens, and 

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 on storage are needed.
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Water, Fish, and Irrigated Crops (860.1400)

This guideline topic is not relevant to the proposed uses.

Food Handling (860.1460)

This guideline topic is not relevant to the proposed uses.

Meat, Milk, Poultry, and Eggs (860.1480)

Residue Chemistry Memo DP# 264154, 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. There are no significant livestock feedstuffs associated with 

the proposed uses on asparagus; Brassica leafy greens, subgroup 5B; and turnip greens.

Although additional crop field trial data are required for sweet corn to support the proposed use, 

the maximum reasonable dietary burdens of acetamiprid to ruminants, based on the addition of 

sweet corn forage and cannery waste, are calculated herein for informational purposes (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
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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

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. 

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 currently 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. The tolerances should not be revised at this time, but be reevaluated when the outstanding data for sweet corn have been submitted and reviewed.

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.
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Crop Field Trials (860.1500)

DER References: 48590101.der (Asparagus)

48590102.der (Mustard greens)

48590103.der (Sweet corn, U.S. trials)

48590104.der (Sweet corn, Canada trials).

Asparagus

IR-4 has submitted field trial data for acetamiprid on asparagus. During the 2008-2009 growing 

season, 8 U.S. field trials were conducted in the following North American Free Trade

Agreement (NAFTA) Growing Zones: 2 (MD; 1 trial); 5 (MI; 2 trials); 10 (CA; 3 trials); and 11 

(ID and WA; 2 trials). The 2 MI trials and 2 of the CA trials were conducted by the same Field 

Research Directors (FRDs) at the same trial locations and used the same variety of asparagus. 

Careful examination of the field trial records indicates that the only differences between the two 

trials were use of different tank mixes for all applications, and a 7-day (CA trials) or 21-day (MI 

trials) offset in application dates. HED has concluded that the differences between these CA 

trials are insufficient to classify them as separate trials; therefore, this pair of trials constitutes a 

single trial with replicate samples for purposes of OCSPP 860.1500 data requirements. In the 

case of the MI trials, HED has concluded that while not ideal, the 21-day offset in application 

dates is sufficiently different to be classified as independent field trials. The adjustment in trial 

numbers results in a total of seven field trials, with two trials total conducted in NAFTA Zone 

10. 

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

foliar broadcast applications of a 70% WP formulation of acetamiprid (Assail® 70 WP) at 0.099-

0.103 lb ai/A/application for a total seasonal rate of 0.200-0.204 lb ai/A (~1x the maximum 

proposed seasonal application rate). Applications were made at 10- to 14-day retreatment 

intervals (RTIs) using ground equipment in spray volumes of 20-36 gal/A. In five of eight trials, 

an NIS was added to each spray mixture (second application only at one of the trials); an 

adjuvant was not added to the spray mixtures at the remaining trial sites. Samples of asparagus 

were harvested at maturity at a PHI of 1 day. In one CA trial, additional samples were harvested 

at PHIs of 0, 4, 8, and 11 days to assess residue decline.

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 asparagus field trials are presented in Table 10. Following two foliar broadcast 

applications of the 70% WP formulation of acetamiprid at a total rate of 0.200-0.204 lb ai/A, 

residues of acetamiprid (and per trial averages) were 0.11-0.43 (0.12-0.41) ppm in/on asparagus 

spears at a 1-day PHI.

When residues are compared for trials conducted with and without an adjuvant, residues were 

generally higher following applications made with an NIS (0.21-0.43 ppm; average 0.28 ppm) 

than following applications made without an adjuvant (0.11-0.26 ppm; average 0.18 ppm). 
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In the residue decline trial, residues of acetamiprid declined with increasing PHI.

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

Commodity Total 

Applic. Rate

(lb ai/A)

PHI 

(days)

Residue Levels

(ppm)1

n Sample 

Min.

Sample 

Max.

LAFT2 HAFT2 Median Mean Std. 

Dev.

ASPARAGUS (proposed use = 0.2 lb ai/A total application rate, 1-day PHI)

Asparagus 0.200-0.204 1 7 0.11 0.43 0.12 0.41 0.26 0.25 0.09

1

 Except for sample min/max, values reflect per trial averages; n = no. of field trials. 

2

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

Conclusions. The submitted residue data for asparagus are acceptable. An acceptable method 

was used for residue quantitation, and the study is supported by adequate storage stability data. 

The study reflects the maximum proposed use pattern for the 70% WP formulation for 

asparagus. Owing to the designation of one pair of residue trials as a single trial with replicate 

samples, geographic representation is inadequate from NAFTA Zone 10 per OCSPP 860.1500

(refer to Appendix I). However, given the requested PHI of 1 day, the maximum anticipated 

residues are going to be driven by application parameters and not meteorological or cultural 

practices. Furthermore, the available residue data is tightly grouped around the mean, with a 

small observed standard deviation. Therefore, it is highly unlikely that additional residue data 

from Zone 10 would have a significant impact on the recommended tolerance. Consequently 

HED is not requesting additional field trials for asparagus. 

It is noted that all of the submitted field trials used the 70% WP 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, 

12/1/09). Therefore bridging data to support the use of the 30% SG formulation on asparagus 

are not required. The data are sufficient for establishing tolerances on asparagus associated with 

the requested registration of the 70% WP and 30% SG formulations. 

Mustard greens

IR-4 has submitted field trial data for acetamiprid on mustard greens. During the 2009 growing 

season, 8 U.S. field trials were conducted in the U.S. in the following North American Free 

Trade Agreement (NAFTA) Growing Zones: 2 (GA, NC, and SC; 3 trials); 4 (AR; 1 trial); 5 

(OH; 1 trial); 6 (TX; 1 trial); and 10 (CA; 2 trials). The 2 CA trials were conducted by the same 

FRD at the same trial locations. Examination of the field trial records indicates that there were 

sufficient differences between the trials, including use of different tank mixes for all 

applications, a 60-day offset in initiation, different crop varieties, and different spray equipment. 

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

foliar broadcast or directed applications of a 70% WP formulation of acetamiprid (Assail® 70 
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WP) at 0.074-0.080 lb ai/A for the first application and at 0.097-0.104 lb ai/A for subsequent 

applications, for a total seasonal rate of 0.374-0.384 lb ai/A (~1x the maximum proposed 

seasonal application rate). A fifth application was made at the GA trial at 0.101 lb ai/A because 

the crop was not mature after four applications; the total seasonal rate for this trial was 0.476 lb 

ai/A. Applications were made at 6- to 8-day RTIs using ground equipment in spray volumes of 

27-47 gal/A. An NIS was added to each spray mixture. Samples of mustard greens were 

harvested at maturity at PHIs of 2-4 days.

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 mustard greens field trials are presented in Table 11. Following four or five 

foliar broadcast or directed applications of the 70% WP formulation of acetamiprid at a total rate 

of 0.374-0.476 lb ai/A, residues of acetamiprid (and per trial averages) were 0.20-10 (0.30-9.2) 

ppm in/on mustard greens at PHIs of 2-4 days. Residues at the GA trial that received five 

applications were well within the range of residues at the remaining trials.

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

required because sufficient residue decline data are available for acetamiprid, indicating that 

residues do not increase with increasing harvest intervals (refer to DP# 264154, 12/31/01, M. 

Doherty and others).

Table 11. Summary of Residue Data from Mustard Greens Crop Field Trials with Acetamiprid.

Commodity Total 

Applic. Rate

(lb ai/A)

PHI 

(days)

Residue Levels

(ppm)1

n Sample 

Min.

Sample 

Max.

LAFT2 HAFT2 Median Mean Std. 

Dev.

BRASSICA, LEAFY GREENS, SUBGROUP 5B and TURNIP GREENS

(proposed use = 0.375 lb ai/A total application rate, 3-day PHI)

Mustard greens 0.374-0.476 2-4 8 0.20 10 0.30 9.2 1.9 2.6 2.8

1

 Except for sample min/max, values reflect per trial averages; n = no. of field trials. 

2

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

Conclusions. The submitted residue data for mustard greens are acceptable. The study reflects 

the maximum proposed use pattern for the 70% WP formulation for Brassica leafy greens, 

subgroup 5B and turnip greens, and the number and location of the field trials are in accordance 

with OCSPP 860.1500 for mustard greens (refer to Appendix I). An acceptable method was 

used for residue quantitation, and the study is supported by adequate storage stability data.

The submitted residue data are adequate to support use of both the 70% WP and 30% SG 

formulations of acetamiprid on Brassica leafy greens and turnip greens. It is noted that all of the 

submitted field trials used the 70% WP formulation. The registrant is requesting the use of both 

the 70% WP and 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, 

12/1/09). Therefore bridging data to support the use of the 30% SG formulation on Brassica
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leafy greens and turnip greens are not required. The data are sufficient for establishing 

tolerances on Brassica leafy greens and turnip greens associated with the requested registration 

of the 70% WP and 30% SG formulations (see below). 

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 (41- to 89-day PHIs). The application rates used in 

the studies are equivalent to ~1x the maximum proposed seasonal application rate.

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 12 (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 
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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 Canada sweet corn field trials indicated that residues of acetamiprid generally 

declined with increasing PHI in sweet corn forage and stover.

Canada 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 conducted in NAFTA Zone 5B.

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).
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The results of the sweet corn field trials are presented in Table 12 (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 41-89 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 ~22%, residues in these samples were still included 

in the summary data calculations. 

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 12. 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 0.213-0.219

(238.5-245.4)

41-89 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 concluded that insufficient data have been submitted 

to support the use on sweet corn. Although there is evidence to support residue equivalency for 

the 70% WP formulation and the 30% SG formulation and the combination of trials conducted 
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with these two formulations provide for an adequate number of trials with sufficient geographic 

variation, it is not possible to combine the two sets 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. Furthermore, although the 

use patterns were similar between the U.S. and Canadian trials for K+CWHR and forage (four 

applications, 1- to 2-day PHI), 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. Additional crop field trial data are required to support the proposed uses. 

Based on the crop field trial study designs, the U.S. use pattern appears to be less restrictive for 

stover (1- or 7-day PHI in the U.S. vs. harvest at maturity in Canada); therefore, to support the 

proposed uses on sweet corn, five additional crop field trials must be conducted in the U.S. with 

the 30% SG formulation and an adjuvant in Zones 1 (1 trial), 5 (3 trials), and 12 (1 trial) to 

provide a full set of field trial data for this formulation. Each trial should include an additional 

side-by-side treated plot reflecting application of the 70% WP formulation with an adjuvant. 

Although the available data suggest that residues are similar following application according to 

the four-application/1-day PHI use pattern and the two-application/7-day PHI use pattern, HED 

recommends that each use pattern be represented in at least two of the required trials. 

HED concludes that the available data are insufficient for establishing tolerances associated with 

the requested registration at this time. 

Processed Food and Feed (860.1520)

There are no significant processed commodities associated with the proposed uses on asparagus; 

Brassica leafy greens, subgroup 5B and turnip greens; or 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 communication 

between T. Cole, of BEAD’s Analytical Chemistry Branch (ACB), and Versar, 11/30/11. Please 

note that the acetamiprid metabolite IM-1-2 has expired (8/1/2009) and an updated certificate of 

analysis (COA) or a new standard for this compound should be sent in. The analytical reference 

standard for metabolite IM-1-2 should be supplied and supplies replenished as requested by the 

Repository, or an updated COA should be supplied. 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:
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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.

Tolerance Derivation

Residue Chemistry Memo DP# 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 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. HED has concluded that the available data for sweet corn are insufficient to 

establish tolerances at this time; therefore, the data were not entered into the OECD tolerance 

calculation procedure, and the proposed tolerances were not assessed.

Updated crop group definitions. The established tolerances for vegetable, fruiting, group 8; 

fruit, citrus, group 10; and fruit, pome, group 11, can be updated to the current crop group 

definitions with no accompanying data to vegetable, fruiting, group 8-10 (at 0.20 ppm); fruit, 

citrus, group 10-10 (at 0.50 ppm); and fruit, pome, group 11-10 (at 1.0 ppm). 

Livestock commodities. The available field corn residue data indicate that the established 

tolerances on milk and the fat, meat, and meat byproducts of cattle, goat, horse, and sheep may 

be too low once use on sweet corn has been registered. The established tolerances will be 

reassessed when the outstanding sweet corn field trial data have been received.

Asparagus; Brassica, leafy greens, subgroup 5B; and turnip greens. Sufficient field trial data 

have been submitted for asparagus and mustard greens for establishing 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 0.80 ppm in asparagus and 15 

ppm in Brassica leafy greens, subgroup 5B and turnip greens. The OECD tolerance calculation 

procedure (March 2011 version) was utilized in determining the appropriate tolerance levels. 

Average values from the asparagus and mustard greens field trials were used.
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With the establishment of a tolerance in Brassica, leafy greens, subgroup 5B, the established 

tolerance in vegetable, Brassica, leafy, group 5 should be removed, and a new tolerance should 

be established in Brassica, head and stem, subgroup 5A, at 1.2 ppm. No additional data are 

required to support this tolerance because adequate residue data were previously submitted and 

reviewed under DP# 264154. 

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

asparagus and no established Codex MRLs on any Brassica vegetables; therefore, there are no 

issues of harmonization. Canadian MRLs are established for residues of acetamiprid at 1.2 ppm 

in/on Chinese cabbage (bok choy), cabbages, broccoli raab, collards, kale, mustard greens, 

mustard spinach, and rape greens. With the establishment of separate tolerances in Brassica

leafy greens, subgroup 5B, and Brassica head and stem, subgroup 5A, the Canadian MRLs for 

Bok choy Chinese cabbages, broccoli raab, collards, kale, mustard greens, mustard spinach, and 

rape greens will no longer be harmonized with U.S. tolerances. This petition requests a revised 

use pattern for subgroup 5B commodities, specifically a shorter PHI; therefore, a higher U.S. 

tolerance of 15 ppm is required. 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, DP# 278652, 11/13/2001, M. Doherty 

DER Reference: 44988601.der, 12/14/01, H. Bietlot

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

Residue Chemistry Memo DP# 303623, 11/05/2004, W. Drew (PP#4F6833)

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

Residue Chemistry Memo DP#s 342549 & 355773, 11/05/2008, W. Drew
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Attachment 1. International Maximum Residue Limits – Acetamiprid.

Acetamiprid (099050, Requested 14 November, 2011)

Summary of US and International Tolerances and Maximum Residue Limits 

Residue Definition:

US Canada Mexico2 Codex3

40 CFR 180.578:

Plants and Livestock:

N 1-[(6-chloro-3-

pyridyl)methyl]- N 2-cyanoacetamidine

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

pyridinyl)methyl]-N'-cyano-Nmethylethanimidamide

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

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

metabolite (E)-N-[(6-chloro-3-

pyridinyl)methyl]-N'-

cyanoethanimidamide

None

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

US Canada Mexico2 Codex3

Asparagus 0.8

Brassica, leafy greens, subgroup 

5B

15 1.2 (bok choy) Chinese 

cabbages, broccoli raab, 

collards, kale, mustard greens, 

mustard spinach, rape greens

Turnip greens 15

Corn, sweet, kernel plus cob with 

husks removed

0.01

Corn, sweet, forage 10

Corn, sweet, stover 30

Vegetable, fruiting, group 8-10 0.20 0.2 bell peppers, eggplants, 

groundcherries, non-bell 

peppers, pepinos, pepper 

hybrids, tomatillos, tomatoes

0.4 tomato paste

Fruit, citrus, group 10-10 0.50 0.5 calamondins, citrus 

citrons, citrus, hybrids, 

grapefruits, kumquats, lemons, 

limes, oranges, pummelos, 

satsuma mandarins, tangerines

1.2 dried citrus fruit pulp
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Summary of US and International Tolerances and Maximum Residue Limits 

Residue Definition:

US Canada Mexico2 Codex3

Fruit, pome, group 11-10 1.0 1.0 apples, Asian pears, 

crabapples, loquats, mayhaws, 

pears, quinces

Completed: M. Negussie; 11/16/2011

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 LOQ; 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.1. Trial Numbers and Geographical Locations for Asparagus.

NAFTA Growing Zones Asparagus

Submitted Requested1

Canada U.S.

1 -- -- --

1A -- -- --

2 1 -- 1/1

3 -- -- --

4 -- -- --

5 2 -- 2/2

5A -- -- --

5B -- -- --

6 -- -- --

7 -- -- --

7A -- -- --

8 -- -- --

9 -- -- --

10 2

2

-- 3/2

11 2 -- 2/1

12 -- -- --

13 -- -- --

14 -- -- --

15 -- -- --

16 -- -- --

17 -- -- --

18 -- -- --

19 -- -- --

20 -- -- --

21 -- -- --

Total 7

2

8/6

1 As per Table 5 of OCSPP 860.1500 for asparagus; 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 of the Zone 10 trials (CA35 and CA37) constitute a single trial with replicate samples for 

purposes of OCSPP 860.1500 data requirements.

Table I.2. Trial Numbers and Geographical Locations for Mustard Greens.

NAFTA Growing Zones Mustard Greens

Submitted Requested1

Canada U.S.

1 -- -- --

1A -- -- --

2 3

2

-- 2/1

3 -- -- 1/0
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Table I.2. Trial Numbers and Geographical Locations for Mustard Greens.

NAFTA Growing Zones Mustard Greens

Submitted Requested1

Canada U.S.

4 1 -- 1/1

5 1 -- 1/1

5A -- -- --

5B -- -- --

6 1 -- 1/1

7 -- -- --

7A -- -- --

8 -- -- --

9 -- -- --

10 2 -- 2/1

11 -- -- --

12 -- -- --

13 -- -- --

14 -- -- --

15 -- -- --

16 -- -- --

17 -- -- --

18 -- -- --

19 -- -- --

20 -- -- --

21 -- -- --

Total 8 8/5

1 As per Table 5 of OCSPP 860.1500 for mustard greens; the first number reflects the field trials required if a tolerance is sought 

on the crop subgroup leafy Brassica greens; the second number reflects the number of field trials required if a tolerance is sought 

only on mustard greens.

2 The petitioner noted that one of the Zone 2 trials (GA*06) was located near the border of Zone 3.

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

NAFTA Growing Zones Sweet Corn

Submitted Requested1

Canada U.S. Canada U.S.

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 asparagus; and Brassica leafy greens, subgroup 5B and turnip greens 

(based on data for mustard greens). 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 asparagus and mustard greens.

Regulator: EPA

Chemical: Acetamiprid

Crop: Asparagus Mustard greens

PHI: 1 Day 2-4 Days

App. Rate: 0.20 lb ai/A 0.375 lb ai/A

Submitter: IR-4 IR-4

MRID Citation: MRID 48590101 MRID 48590102

Acetamiprid (ppm)

0.21 9.2

0.21 2.65

0.405 1.55

0.12 2.15

0.27 1.2

0.26 0.30

0.26 1.7

-- 2.4

Asparagus

The dataset used to establish a tolerance for acetamiprid on asparagus consisted of field trial data 

representing application rates of 0.200-0.204 lb ai/A acetamiprid with a 1-day PHI. The field 

trial application rates and PHIs are 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 asparagus. Using the OECD tolerance calculation procedure, the recommended 

tolerance is 0.80 ppm.
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Mustard greens

The dataset used to establish a tolerance for acetamiprid on Brassica leafy greens, subgroup 5B 

and turnip greens consisted of field trial data on mustard greens representing application rates of 

0.374-0.476 lb ai/A acetamiprid with a 2- to 4-day PHI. The field trial application rates and 

PHIs are within 25% of the maximum label application rate (except for one field trial that 

received an extra application) 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 mustard greens. Using the OECD tolerance 

calculation procedure, the recommended tolerance is 15 ppm.

Total number of data (n) 7

Percentage of censored data 0%

Number of non-censored data 7

Lowest residue 0.120

Highest residue 0.405

Median residue 0.260

Mean 0.250

Standard deviation (SD) 0.087

Correction factor for censoring (CF) 1.000

Proposed MRL estimate

- Highest residue 0.405

- Mean + 4 SD 0.599

- CF x 3 Mean 0.750

Unrounded MRL 0.750

Rounded MRL 0.8

 High uncertainty of MRL estimate.

[Small dataset]

GAP

Acetamiprid

Asparagus

USA
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Percentage of censored data 0%

Number of non-censored data 8

Lowest residue 0.300

Highest residue 9.200

Median residue 1.925

Mean 2.644

Standard deviation (SD) 2.750

Correction factor for censoring (CF) 1.000

Proposed MRL estimate

- Highest residue 9.200

- Mean + 4 SD 13.645

- CF x 3 Mean 7.931

Unrounded MRL 13.645

Rounded MRL 15

0.375 lb ai/A, 3-day PHI

Acetamiprid

Mustard greens

U.S.A.