Document ID: EPA-HQ-OPP-2011-0985-0007
Agency: epa
Document Type: Supporting & Related Material
Title: 
Posted Date: 2012-11-14T05:00Z

UNITED STATES ENVIRONMENTAL PROTECTION AGENCY

WASHINGTON, D.C.  20460

	OFFICE OF CHEMICAL SAFETY

	AND POLLUTION PREVENTION

  SEQ CHAPTER \h \r 1 MEMORANDUM

Date:  October 2, 2012

SUBJECT:	REVISED.  Flonicamid.  Petition for the Establishment of
Permanent Tolerances and Registration for Use on Berry Low-Growing
Subgroup 13-07G, Cucumber for Greenhouse Use Only, and Rapeseed
Sub-group 20A.   Summary of Analytical Chemistry and Residue Data.

PC Code:  128016	DP Barcode:  D396902 

Decision No.: 457726	Registration No.:  71512-10, 71512-9

Petition No.:  1E7942	Regulatory Action:  Section 3 Registration

Assessment Type: Single Chemical	Case No.:  NA

TXR No.:  NA	CAS No.:  158062-67-0

MRID No.:  See Table Below	40 CFR:  180.613

		              									

FROM:	Amelia M. Acierto, Chemist			

		Risk Assessment Branch III (RAB3)

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

	

THROUGH:	Stephen Funk, Senior Scientist

		Risk Assessment Branch III (RAB3)

		Health Effects Division (HED; 7509P)

		

TO:		Barbara Madden/Sydney Jackson, RM #5

		Risk Integration, Minor Use and Emergency Response Branch (RIMUERB)

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

Note: The DER for greenhouse use on cucumber was originally prepared by
the Pest Management Regulatory Agency (PMRA) of Health Canada and DERs
for berry and canola were originally prepared under contract by Versar,
Inc. (6850 Versar Center, Springfield, VA 22151; submitted 4/3/12).   
SEQ CHAPTER \h \r 1 The DERs have been reviewed by HED and revised to
reflect current Office of Pesticide Programs (OPP) policies.

MRID Summary Table

MRID No.	Study Type	Comments

48657101	860.1500 	New DER; 48657101.der.doc Strawberry

48657102	860.1500 	New DER; 48657102.der.doc Cucumber

48657103 de.1	860.1500 	New DER; 48657103.de.1.doc Canola

48657103 de.2	860.1520 	New DER; 48657103.de.2.doc Canola processed food

Table of Contents

  TOC \o "1-3" \h \z \u    HYPERLINK \l "_Toc324945615"  Executive
Summary	  PAGEREF _Toc324945615 \h  3  

  HYPERLINK \l "_Toc324945616"  Regulatory Recommendations	  PAGEREF
_Toc324945616 \h  5  

  HYPERLINK \l "_Toc324945617"  Pre-Registration Data Needs	  PAGEREF
_Toc324945617 \h  6  

  HYPERLINK \l "_Toc324945618"  Condition-of-Registration Data Needs	 
PAGEREF _Toc324945618 \h  6  

  HYPERLINK \l "_Toc324945619"  Tolerance Considerations	  PAGEREF
_Toc324945619 \h  6  

  HYPERLINK \l "_Toc324945620"  Analytical Method	  PAGEREF
_Toc324945620 \h  6  

  HYPERLINK \l "_Toc324945621"  Recommended Tolerances	  PAGEREF
_Toc324945621 \h  6  

  HYPERLINK \l "_Toc324945622"  International Harmonization	  PAGEREF
_Toc324945622 \h  7  

  HYPERLINK \l "_Toc324945623"  Revisions to Petitioned-For Tolerances	 
PAGEREF _Toc324945623 \h  7  

  HYPERLINK \l "_Toc324945624"  Residue Profile	  PAGEREF _Toc324945624
\h  7  

  HYPERLINK \l "_Toc324945625"  Residue Chemistry Guidelines	  PAGEREF
_Toc324945625 \h  9  

  HYPERLINK \l "_Toc324945626"  Directions for Use (860.1200)	  PAGEREF
_Toc324945626 \h  9  

  HYPERLINK \l "_Toc324945627"  Nature of the Residue in Plants and
Livestock (860.1300)	  PAGEREF _Toc324945627 \h  10  

  HYPERLINK \l "_Toc324945628"  Residue Analytical Methods (860.1340)	 
PAGEREF _Toc324945628 \h  11  

  HYPERLINK \l "_Toc324945629"  Multiresidue Methods (860.1360)	 
PAGEREF _Toc324945629 \h  11  

  HYPERLINK \l "_Toc324945630"  Storage Stability (860.1380)	  PAGEREF
_Toc324945630 \h  11  

  HYPERLINK \l "_Toc324945631"  Food Handling (860.1460)	  PAGEREF
_Toc324945631 \h  12  

  HYPERLINK \l "_Toc324945632"  Meat, Milk, Poultry, and Eggs (860.1480)
  PAGEREF _Toc324945632 \h  12  

  HYPERLINK \l "_Toc324945633"  Crop Field Trials (860.1500)	  PAGEREF
_Toc324945633 \h  13  

  HYPERLINK \l "_Toc324945634"  Strawberry
………………………………………………………………
………….…........  PAGEREF _Toc324945634 \h  13  

Cucumber………………………………………………………
………………………...... 15

  HYPERLINK \l "_Toc324945636"  Canola	  PAGEREF _Toc324945636 \h  16  

  HYPERLINK \l "_Toc324945637"  Processed Food and Feed (860.1520)	 
PAGEREF _Toc324945637 \h  18  

  HYPERLINK \l "_Toc324945638"  Canola	  PAGEREF _Toc324945638 \h  18  

  HYPERLINK \l "_Toc324945639"  Confined Accumulation in Rotational
Crops (860.1850)	  PAGEREF _Toc324945639 \h  20  

  HYPERLINK \l "_Toc324945640"  Field Accumulation in Rotational Crops
(860.1900)	  PAGEREF _Toc324945640 \h  20  

  HYPERLINK \l "_Toc324945641"  Proposed Tolerances (860.1550)	  PAGEREF
_Toc324945641 \h  20  

  HYPERLINK \l "_Toc324945642"  Appendix I	  PAGEREF _Toc324945642 \h 
23  

  HYPERLINK \l "_Toc324945643"  International Residue Limits	  PAGEREF
_Toc324945643 \h  23  

  HYPERLINK \l "_Toc324945644"  Appendix II	  PAGEREF _Toc324945644 \h 
24  

  HYPERLINK \l "_Toc324945645"  Tolerance Assessment Calculations	 
PAGEREF _Toc324945645 \h  24  

  HYPERLINK \l "_Toc324945646"  Berry, Low growing, Subgroup 13-07G	 
PAGEREF _Toc324945646 \h  24  

  HYPERLINK \l "_Toc324945647"  Cucumber (Greenhouse, Foliar)	  PAGEREF
_Toc324945647 \h  24  

Cucumber (Greenhouse,
Chemigation)……………………………………………………
 24

  HYPERLINK \l "_Toc324945648"  Rapeseed, Subgroup 20A	  PAGEREF
_Toc324945648 \h  25  

 

Executive Summary

Flonicamid is a systemic insecticide that immediately suppresses the
feeding of sucking insects on plants.  From its chemical structure
(including the nicotinic acid structure), it would be expected to
exhibit the same mode of action as similarly structured neo-nicotinoid
pesticides.  However, flonicamid has not been found to activate
acetylcholine esterase (OP's and carbamates), or nicotinic acetylcholine
receptors (neo-nicotinoids).  Flonicamid has been described as a new
chemistry (cyanomethyl trifluoromethyl nicotinamide) with a novel (but
undefined) mode of action, different from other commercially available
products.  

The Interregional Research Project No. 4 (IR-4) has submitted crop field
trial and greenhouse data generated during 2008 and 2009 growing season
from the North American Free Trade Agreement (NAFTA) Growing Zones in
support of the petition for the establishment of permanent tolerances
for the combined residues of flonicamid
[N-(cyanomethyl)-4-trifluoromethylnicotinamide] and its metabolites TFNA
(4-trifluoromethylnicotinic acid), TFNA-AM
(4-trifluoromethylnicotinamide), and TFNG
[N-(4-trifluoromethylnicotinoyl)glycine], in or on the following raw
agricultural commodities (RACs):

	Berry low-growing subgroup 13-07G ……. . …. …1.4 ppm

	Cucumber *  ………………………………… ……1.3 ppm

	Rapeseed subgroup 20A ………………….… …….1.5 ppm

            * To increase tolerance on cucumber for greenhouse use only.

The petitioner proposes Section 3 registration of Beleaf™ 50SG (EPA
Reg. No. 71512-10) and Flonicamid 50WG (EPA Reg. No. 71512-9) for use on
the berry subgroup 13-07G, cucumber for greenhouse use, and the rapeseed
subgroup 20A.  Beleaf™ 50SG and Flonicamid 50WG are 50% water soluble
granule (SG) formulations of flonicamid (containing 0.5 pound active
ingredient per pound of formulated product).

The end-use products can be applied with ground, aerial and chemigation
equipment at the total rate of 0.267- 0.269 lb ai/acre (equivalent rate
calculated/plant for greenhouse use).  A non-ionic surfactant was used
in the crop trials except for canola and for greenhouse cucumber treated
by chemigation. The proposed pre-harvest intervals (PHIs) range from
0-days for strawberry and cucumber to 6-8 days for canola.

Tolerances are established for residues of flonicamid under 40 CFR
§180.613(a)(1) on various raw agricultural commodities (RACs) at levels
ranging from 0.2 ppm on fruit, pome, group 11 and vegetable, tuberous
and corm, subgroup 1C to 16.0 ppm on turnip greens; Brassica leafy
greens subgroup 5B; and raddish, tops.  Tolerance on cucumber is
currently included in the vegetable, cucurbit, group 9 at 0.40 ppm. 
Tolerances have also been established under §180.613(a)(2) on livestock
commodities including egg and milk at levels ranging from 0.03 ppm on
fat of cattle, goat, horse, poultry, and sheep to 0.08 ppm on meat
byproducts of cattle, goat, horse, poultry, and sheep.

The nature of the residue in plants and livestock is adequately
understood for purposes of this petition.  The metabolism of flonicamid
in plant and livestock are identical.  The main pathway of metabolism
involves hydrolysis of the cyano and amide functional groups in the
molecule.  The residues of concern in plants for the tolerance
expression and risk assessment are flonicamid, TFNA, TFNA-AM and TFNG
(D290386, A.M. Acierto, 4/22/2005).  The HED’s RARC (RARC Sec. 3.0,
4/20/05) has determined that the residues of concern in livestock
commodities for the tolerance expression and risk assessment are
flonicamid, TFNA and TFNA-AM.

An adequate enforcement method is available which uses high performance
liquid chromatography with tandem mass spectrometric detection
(LC/MS/MS) adapted from FMC No. P-3561M.  The method has been used for
data collection and enforcement for plant commodities.  The method
determines flonicamid and its metabolites TFNA, TFNA-AM and TFNG and has
been sufficiently validated in five diverse crops.  A number of minor
modifications to the method were made for the petitioned crops including
changes in clean-up procedures, reagents, and sample sizes.  An LC-MS
method similar to the LC/MS/MS method was used for cucumber. Method
validation and concurrent recoveries in strawberry, cucumber and canola
were conducted using untreated control samples fortified separately with
flonicamid and its metabolites at 0.02, 0.20 and 2.0 ppm.  The
fortification levels were adequate to bracket expected residue levels in
the strawberry and cucumber.  The quantifiable residues were converted
to parent equivalents by the study reviewer using molecular weight
conversion factors of 1.20, 1.21, and 0.92 for TFNA, TFNA-AM, and TFNG,
respectively.  The LOQ (determined as the LLMV) was 0.02 ppm for each
analyte and the LOD was calculated as 1/3 the LOQ.

In canola, poor method validation recoveries and poor concurrent
recoveries were reported using the HPLC/MS/MS method for each analyte at
the 0.02 ppm fortification level. The petitioner noted that this is
caused by ion suppression due to matrix interference.  HED recommends
raising the limit of quantitation (LOQ) for each analyte to 0.2 ppm or
about 0.9 ppm for the combined residues of flonicamid and its
metabolites, calculated as flonicamid 

(ChemSAC Minutes, 4/2/12).

Three enforcement methods are used for livestock commodities: an
LC/MS/MS method RCC No. 844743 (for the determination of residues in
eggs and livestock tissues), LC/MS method RCC No. 842993 (for
determination of residues in milk) and LC/MS/MS method FMC No. P-3580,
which includes an acid hydrolysis step (for determination of residues in
meat and meat products (muscle, kidney and liver) of cattle, goat, hog,
horse, and sheep.

The multi-residue methods requirement has been fulfilled.  Flonicamid
and TFNA-AM were completely recovered using Protocol D (with no cleanup)
but were not recovered using Protocols E and F.  Metabolites TFNA and
TFNG were not recovered using Protocols B, D, E and F.  

  

Available storage stability data demonstrate that flonicamid and its
metabolites TFNA, TFNA-AM, and TFNG are relatively stable in/on oil
seed, non-oily grain, root and tuber crops, leafy vegetables, and
fruiting vegetables in frozen storage for ~23 months.  Storage stability
data demonstrate that processed commodities are also stable for ~23
months.  The current storage stability data demonstrate that residues of
flonicamid, TFNA, TFNA-AM, and TFNG are stable in/on the RAC samples of
berry, cucumber and canola stored frozen for up to 460, 336 and 735
days, respectively.  The available data on the five diverse crops (oil
seed, non-oily grain, root and tuber crop, leafy vegetables, and
fruiting vegetables) are adequate to support the storage conditions and
durations of the RAC samples from the submitted field trials.

Adequate field trial data were submitted supporting the use of the
flonicamid 50SG formulation on the proposed crop/crop groups.  An
adequate number of field trials were conducted on the required
representative crops in the appropriate geographic regions.  The crop
field trial data reflect the proposed multiple application rates and
pre-harvest intervals (PHIs).  The Organization of Economic Cooperation
and Development (OECD) spreadsheet calculation procedure was used to
determine appropriate tolerance levels. The proposed tolerance for
berry, low-growing, subgroup 13-07G is 1.4 ppm; the proposed tolerance
for greenhouse cucumber is 1.3 ppm.  Based on the OECD spreadsheet
calculation procedure, the proposed tolerances for berry and cucumber as
a member of the cucurbit vegetable group should be raised to 1.5 ppm. 
Therefore, a revised Section F is required to reflect this
determination.  The recommended tolerance of 1.5 ppm will replace the
existing tolerance of 0.40 ppm for the cucurbit vegetable group 9 under
40 CFR §180.613 (a)(1).  The proposed tolerance of 1.5 ppm for rapeseed
is appropriate.

Field trial decline studies demonstrate that the combined residues of
flonicamid and its metabolites in strawberry decline with increasing
pre-harvest intervals.  Residue decline was observed in greenhouse grown
cucumber treated by foliar spray but not in crops treated by chemigation
where the residues increased from the 0- to 7-day PHIs.  No decline
study was reported for canola.

Adequate processing studies in/on canola are available.  The processing
data indicate that the combined residues of flonicamid, TFNG, TFNA, and
TFNA-AM do not concentrate in canola meal and canola oil (each have
0.27x average processing factor).  The reported processing factors do
not exceed the theoretical concentration factor of 1.0x for canola meal
and 3.0x for canola oil (OCSPP §860.1520, Table 3).  Based on these
results, the tolerances for livestock commodities will not change.

  

No new rotational crop data were submitted and none are required with
the use of flonicamid on rapeseed, cucumber and berry (OCSPP 860.1850). 

There are currently no Codex or Canadian maximum residue limits (MRLs)
established for residues of flonicamid in crop or livestock commodities.
 

The analytical standards for flonicamid, and its metabolites (TFNA,
TFNA-AM and TENG) are available at the EPA National Pesticide Standards
Repository with expiration dates from 2014 - 2016.

  SEQ CHAPTER \h \r 1 Regulatory Recommendations 

Provided the revisions to the Section B/label and Section F are made as
requested below (in the Pre-Registration Data Needs section), the
available residue chemistry data are adequate to support registration of
the crop/crop group commodities requested by the petitioner at the
tolerance levels recommended in Table 1 below (in the Recommended
Tolerances section).

Pre-Registration Data Needs

The submitted labels for Beleaf™ 50SG Insecticide and Flonicamid 50WG
have a restriction prohibiting greenhouse use.  The labels should be
revised to: “Do not use this product in greenhouses, except on
cucumbers”. 

The registrant needs to submit a revised section F in which the
recommended tolerances and commodity definitions listed in Table 1 are
proposed. 

Condition-of-Registration Data Needs

No residue chemistry conditional registration data needs are associated
with this tolerance petition.

Tolerance Considerations

Analytical Method

Adequate enforcement methods are available to enforce the proposed
tolerances for flonicamid and the major metabolites in plants and
livestock.  The proposed method for plants uses LC/MS/MS (FMC No.
P-3561M) to determine the residues of flonicamid and its major
metabolites, TFNA-AM (4-trifluoromethylnicotinamide), TFNA
(4-trifluoromethylnicotinic acid), and TFNG
[N-(4-trifluoromethylnicotinoyl)glycine].  The reported LOQ was 0.02 ppm
and the reported LOD was calculated as 1/3 the LOQ.   This LOQ was
demonstrated for cucumber and strawberry, but not for canola.   Based on
the poor results in the method validation and concurrent recoveries for
canola at 0.02 ppm fortifications per analyte, it is required to raise
the LOQ to 0.2 ppm per each analyte (3/14/12).  Recoveries were
consistently acceptable at the 0.2 ppm per analyte fortification level. 

Recommended Tolerances

Tolerances should be established in 40 CFR §180.613 with the following
tolerance expression, as per the Steve Knizner memo dated 5/27/09:

Tolerances are established for the residues of the insecticide
flonicamid including its metabolites and degradates, in or on the
commodities in the following table.  Compliance with the tolerance
levels specified in the following table is to be determined by measuring
only the sum of flonicamid
[N-(cyanomethyl)-4-(trifluoromethyl)-3-pyridinecarboxamide] and its
metabolites TFNA (4-trifluoromethylnicotinic acid), TFNA-AM
(4-trifluoromethylnicotinamide), and TFNG
[N-(4-trifluoromethylnicotinoyl)glycine], calculated as the
stoichiometric equivalent of flonicamid, in or on the following
commodities.

 

HED recommends for establishment of tolerances on the commodities in
Table 1 using the same tolerance expression as above at the tolerance
levels recommended in Table 1 below: 

Table 1.  Tolerance Summary for Flonicamid

Commodity	Established/Proposed Tolerance

(ppm)	Recommended Tolerance (ppm)	Comments (correct commodity
definition)

Berry, low growing, subgroup 13-07G	1.4	1.51

	Cucumber for greenhouse use only 9	1.3	1.52	Vegetable, cucurbit, group
9

Rapeseed subgroup 20A	1.5	1.53

	1 The representative commodity for the berry, low growing, subgroup
13-07G is strawberry.  The Organization of Economic Coordination and
Development (OECD) spreadsheet calculation procedure gave a value of 1.5
ppm for strawberry.

2 A tolerance was established on cucumber at 0.4 ppm (as a member of the
cucurbit vegetable group 9).  The current petition is to increase the
tolerance to 1.3 ppm for cucumber grown in greenhouse only.  The OECD
spreadsheet calculation procedure gave a value of 1.5 ppm for cucumber
grown in the greenhouse treated at the proposed label rate by foliar
spray.  The OECD spreadsheet calculation procedure gave a value of 0.7
ppm for cucumber treated by chemigation. This tolerance value and the
existing tolerance of 0.40 ppm in 40 CFR §180.613 will be covered under
the foliar spray treatment in greenhouse.  

 3 The representative commodity for the rapeseed, subgroup 20A is
canola.  The OECD spreadsheet calculation procedure gave a value of 1.5
ppm for canola.

No tolerances are required for the processed commodities of canola based
on the demonstrated processing factor of <0.27x for each canola meal and
canola oil.  The maximum theoretical concentration factors for canola
meal and canola oil are 1.9x and 3.0x, respectively (OCSPP 860.1520,
Table 3). 

International Harmonization

There are no Codex or Canadian maximum residue limits (MRLs) on the
proposed crops.  

Revisions to Petitioned-For Tolerances

Based on the OECD spreadsheet calculation procedure, HED recommends
increasing the proposed tolerance from 1.4 ppm to 1.5 ppm for berry, low
growing, subgroup 13-07G and from 1.3 ppm to 1.5 ppm for greenhouse
grown cucumber (as a member of the cucurbit vegetable group).

Residue Profile

The chemical structure and nomenclature of flonicamid and its
metabolites TFNA, TFNA-AM, and TFNG, and the physicochemical properties
of the technical grade of flonicamid are presented in Tables 2 and 3.  

TABLE 2.	Test Compound Nomenclature.

Compound	

Common name	Flonicamid

Company experimental name	IKI-220

IUPAC name	N-cyanomethyl-4-(trifluoromethyl)nicotinamide

CAS name	N-(cyanomethyl)-4-(trifluoromethyl)-3-pyridinecarboxamide

CAS registry number	158062-67-0

End-use product (EP)	50% SG formulation; Beleaf 50 SG (EPA Reg. No.
71512-10)

Compound	

Common name	TFNA

Chemical name	4-trifluoromethylnicotinic acid

Compound	

Common name	TFNA-AM

Chemical name	4-trifluoromethylnicotinamide

Compound	

Common name	TFNG

Chemical name	N-(4-trifluoromethylnicotinoyl)glycine

TABLE 3.	Physicochemical Properties of the Technical Grade Test Compound
Flonicamid.

Parameter	Value	Reference1

Melting point	157.5 (C	MRID 45854601 

pH	4.5 (25 (C)

	Density	1.531 (20 (C)

	Water solubility	5.2 g/L (20 (C)

	Solvent solubility	Solvent	g/100 mL (20 (C)

acetone	17.32

acetonitrile	12.04

dichloromethane	0.40

ethyl acetate	3.57

hexane	0.00003

isopropyl alcohol	1.46

methanol	9.76

n-octanol	0.26

toluene	0.03	MRID 45656705

Vapor pressure	9.43 x 10-7 Pa (20 (C)

2.55 x 10-6 Pa (25 (C)	MRID 45854601

Dissociation constant, pKa	11.60 ± 0.03 (20 ± 1 (C)	MRID 45656705

Octanol/water partition coefficient, Log(KOW)	1.9 (Log POW = 0.3) (29.8
(C)	MRID 45854601

UV/visible absorption spectrum	Acidic and neutral aqueous solutions
exhibited similar spectra with an absorption maximum near 265 nm and a
molar absorptivity of 3,900 L/cm mol. A basic solution exhibited two
absorption peaks. The peak observed in acidic and neutral solutions was
present at a slightly longer wavelength, 270 nm, with an absorptivity of
4,200 L/cm mol. The second peak had an absorption maxima at 204 nm with
an absorptivity of 13,200 L/cm mol.

	1 RD Memo, DP# 285457, 9/30/2003, S. Mathur

Residue Chemistry Guidelines

Directions for Use (860.1200)

The petitioner has submitted amended labels for a 50SG formulation
(Beleaf 50SG Insecticide, EPA Reg. No. 71512-10) and for the 50WG
formulation (Flonicamid 50WG, EPA Reg. No. 71512-9).  A summary of the
proposed use patterns on berry, low growing (subgroup 13-07G),
greenhouse grown cucumbers, and rapeseed (subgroup 20B) is detailed in
Table 4.

Table 4.  Summary of Directions for Use of Flonicamid

Application, Timing, Type and Equipment	Formulation (EPA Reg. Nos.).
App. Rate 

(lb ai/A)

[fl oz /A]	Max. No. App. per Season	RTI

(days)	Max. Seasonal App. Rate

(lb ai/A)

[fl oz /A]	PHI

(days)	

Use Directions and other Limitations

Berry, low growing, subgroup 13-07G [Bearberry, bilberry, blueberry,
lowbush, cloudberry, cranberry, lingonberry, muntries partridgeberry,
strawberry, cultivars, varieties, and/or hybrids of these]1.

Foliar spray ground or air	Beleaf 50SG

(EPA Reg. No. 71512-10) or

Flonicamid 50WG (EPA Reg. No. 71512-9)	0.089

[2.8]	3	7	0.267

[8.4]	0	 Apply when Aphids or Lygus first appear in the field and before
populations reach high levels.  Flonicamid will stop Aphids or Lygus
feeding rapidly but it may take several days to see reduction in Aphids
or Lygus numbers.  Reapply when new insects are detected. Two sequential
applications of flonicamid result in better Aphids or Lygus control than
a single application.  Do not make more than 2 applications of
flonicamid without rotating to an insecticide with a different mode of
action. 

Greenhouse Cucumbers

Foliar directed

	Beleaf 50SG

(EPA Reg. No. 71512-10) or

Flonicamid 50WG (EPA Reg. No. 71512-9)	0.089

[2.8]	2	7	 4.28 oz/A or 0.1 oz per 1000 ft2

	0	1) For Aphids Plant Bugs. Begin applications before populations begin
to build and before damage is evident, according to local pest
management guidelines. Use LOWER RATE for building populations and
HIGHER RATE for greater populations and/or dense foliage.  Rapidly
growing plants may need retreatment.  Check plants often and retreat as
necessary to maintain population below damaging levels.

2) For Greenhouse Whitefly. Apply when adult whiteflies first appear. Do
not allow population to increase unchecked before making the first
application. Application provides SUPPRESSION only.  Apply in
combination with other effective products for control. Check plants
often and retreat as necessary to maintain population below damaging
levels.                                                                 
                                                                        
                                                 

Chemigation (to soil or growth media)

	Beleaf 50SG

(EPA Reg. No. 71512-10) or

Flonicamid 50WG (EPA Reg. No. 71512-9)	0.089

[2.8]	2	7	4.28 oz/A or 2.8 g/1000 ft2	0	Begin applications before
populations begin to build and before damage is evident according to
local pest management guidelines.  Apply using a drench by hand, drip
irrigation or with motorized calibrated irrigation equipment to the base
of the plants.2

Rapeseed Subgroup 20A [Borage, crambe, cuphea, echium, flax seed, gold
of pleasure, hare’s ear mustard, lesquerella, lunaria, meadowfoam,
milkweed, mustard seed, oil raddish, poppy seed, rapeseed, sesame, sweet
rocket, cultivars varieties, and/or hybrids of these].

Foliar spray ground or air	Beleaf 50SG

(EPA Reg. No. 71512-10) or

Flonicamid 50WG (EPA Reg. No. 71512-9)	0.089

[2.8]	3	7	0.267

[8.4]	7	Apply when Aphids or Lygus first appear in the field and before
populations reach high levels.  Flonicamid will stop Aphids or Lygus
feeding rapidly but it may take several days to see reduction in Aphids
or Lygus numbers.  Reapply when new insects are detected. Two sequential
applications result in better Aphids or Lygus control than a single
application.  Do not make more than 2 applications of flonicamid without
rotating to an insecticide with a different mode of action.3

1 Spray adjuvants may improve coverage but do not use binder or
sticker-type surfactants. Only use adjuvants known to be safe on
strawberries.

2 Use a minimum of 25 gal/1000 plants but do not exceed the holding
capacity of soil or growth media. Do not apply more than 4.28 oz/A (0.44
oz/1000 plants based on 1 plant/4.5 ft2 or 9712 plants/A) of flonicamid
per application. 

3 Spray adjuvants may improve coverage but do not use binder or
sticker-type surfactants. Only use adjuvants known to be safe on canola

The submitted labels for Beleaf™ 50SG Insecticide and Flonicamid 50WG
have a restriction for greenhouse use.  The labels should be revised to
change the statement “Do not use this product in greenhouses” to
“Do not use this product in greenhouses, except for cucumber”. 

Conclusions.  The submitted labels (EPA Reg. Nos. 71512-10 and 71512-9)
are adequate to allow evaluation of the residue data relative to the
proposed use.  Revised labels are required to delete the restriction for
greenhouse use for cucumber.

Nature of the Residue in Plants and Livestock (860.1300)

No new metabolism data were submitted in support of this petition and
none are required.  The nature of the residue in plants and livestock is
adequately understood.  Based on the metabolism studies conducted in
plants, the major metabolic pathway of flonicamid in plants involves
hydrolysis of the cyano (-CN) and amide (-CONH) functional groups and
ring hydroxylation.  The residues of concern in plants for tolerance and
risk assessment are flonicamid and its metabolites TFNA, TFNA-AM, and
TFNG (D290386, A.M. Acierto, 4/22/2005).  In livestock commodities, HED
has determined that the residues of concern for the tolerance expression
and risk assessment are flonicamid, TFNA and TFNA-AM (HED/RARC Sec. 3.0,
4/20/05).

Residue Analytical Methods (860.1340)

The method entitled “Analytical Methodology for IKI-220 (F1785) and
its Major Metabolites in/on Peach, Potato Tuber, and Wheat Straw” (FMC
No. P-3561M) was used with some modifications to determine residues of
flonicamid and its metabolites TFNA-AM (4-trifluoromethylnicotinamide),
TFNA (4-trifluoromethylnicotinic acid), and TFNG
[N-(4-trifluoromethylnicotinoyl)glycine] in/on strawberry and canola. 
Cucumber fruit samples were analyzed for the residues of flonicamid and
the three major metabolites, using a liquid chromatography with mass
spectroscopic detection (LC-MS) working method entitled “Residue
Analysis of Flonicamid, TFNA, TFNG, TFNA-AM by LC/MS,  Version #3”.  A
number of minor modifications to the methods were made, including
changes in clean-up procedures, reagents, and sample sizes.  To
calculate the total of all flonicamid, TFNA, TFNA-AM and TFNG residues
(the residue definition in plant matrices), residues of the 3
metabolites above the lowest level of method validation (LLMV) were
converted to flonicamid equivalents (MW flonicamid = 229.17 g/mol) prior
to summing using the following conversion factors:  1.2 for TFNA (MW =
191.11 g/mol), 1.21 for TFNA-AM (MW = 190.12 g/mol); and, 0.92 for TFNG
(MW = 248.2 g/mol).  The LOQ (determined as the LLMV) was 0.02 ppm for
each analyte, except in canola.   For canola matrices, poor recoveries
were obtained at the 0.02 ppm fortification for canola matrices. 
Satisfactory recoveries were obtained at a fortification level of 0.2
ppm for each of the four analytes.  The limit of detection (LOD) was
calculated as 1/3 the LOQ.

Multiresidue Methods (860.1360)

The multi-residue method (MRM) data were reviewed previously and the
testing data have been forwarded to FDA for inclusion in PAM, Vol. I. 
The multi-residue methods requirement has been fulfilled.  Flonicamid
and TFNA-AM were completely recovered using Protocol D (with no cleanup)
but were not recovered using Protocols E and F.  Metabolites TFNA and
TFNG were not recovered using Protocols B, D, E and F.

Flonicamid and its metabolites TFNA (4-trifluoromethylnicotinic acid),
TFNA-AM (4-trifluoromethylnicotinamide), and TFNG
[N-(4-trifluoromethylnicotinoyl)glycine] were analyzed according to the
FDA Multi-Residue Method Test guidelines in PAM, Vol. I (dated 1/94). 
Flonicamid and its metabolites were tested through Protocols A and C,
and as a result of Protocol C testing, all compounds were tested through
Protocols D and E.  Based on the results of Protocol E testing, testing
under Protocol F was not required.  Since methylated TFNA and TFNG
provided good response on at least one of the column/detector
combinations outlined in Protocol C, additional testing was performed
with these compounds under Protocol B.  

Storage Stability (860.1380)

DER Reference: 48657101 der doc (strawberry)

	           48657102 der.doc (cucumber)

                           48657103 de 1.doc (canola) 

	           48657103 de 2 doc (canola processed commodities)

To support the sample storage intervals, untreated control RAC samples
(strawberry, cucumber and canola) and processed canola commodities
(canola meal and oil) were fortified with each analyte (flonicamid,
TFNA, TFNA-AM and TFNG) at 0.2 ppm.  The samples were extracted
according to the method described under the analytical method and stored
at <-15 to ~-21oC from collection to extraction.  Samples were analyzed
within 1- 14 days of extraction.  The data demonstrate that residues of
flonicamid, TFNA, TFNA-AM, and TFNG are stable in/on the RAC samples of
strawberry, cucumber and canola stored frozen for up to 460, 336 and 735
days, respectively.  The available data on five diverse crops (oil seed,
non-oily grain, root and tuber crop, leafy vegetables, and fruiting
vegetables) are adequate to support the storage conditions and durations
of the RAC samples for the subject petition.  Results of the storage
study are summarized in Table 5.  

TABLE 5.	Stability of Flonicamid and its Metabolites in Strawberry,
Cucumber and Canola,

Strawberry

Matrix	Analyte	Spike Level

(ppm)	Storage interval1

(days)	Fresh Fortification Recoveries (%) 	Recovered Residues (ppm)	Mean
Recovered Residues (ppm)	Mean Recovery (%)	Corrected % Recovery2,3

Strawberry	Flonicamid	0.20	460	100	0.19, 0.20, 0.20	0.20	98	98

	TFNA	0.20	460	90	0.17, 0.18, 0.18	0.18	88	98

	TFNA-AM	0.20	460	80	0.16, 0.17, 0.17	0.17	83	104

	TFNG	0.20	460	80	0.15, 0.16, 0.16	0.16	78	98

Cucumber	Flonicamid	0.2	336	90, 90, 105	0.18, 0.18, 0.21	0.19	95	100

	TFNA	0.2	336	80, 85, 95	0.16, 0.17, 0.19	0.17	85	102

	TFNA-AM	0.2	336	80, 80, 90	0.16, 0.16, 0.18	0.17	85	104

	TFNG	0.2	336	75, 80, 90	0.15, 0.16, 0.18	0.16	84	103

Canola (seed)	Flonicamid	0.2	735	82	0.16, 0.16, 0.17	0.16	81	98

	TFNA	0.2	735	74	0.12, 0.15,  0.16	0.14	72	97

	TFNA-AM	0.2	735	82	0.16, 0.16, 0.16	0.16	81	99

	TFNG	0.2	735	85	0.15, 0.17, 0.16	0.16	79	93

1 Interval from fortification to extraction.  Samples were analyzed
within 0 - 14 days of extraction.

2 Corrected for mean recovery in freshly fortified samples.

3 Corrected by dividing the mean freezer storage stability recoveries by
the corresponding concurrent recovery. 

Conclusions.  The submitted storage stability data demonstrate that
residues of flonicamid, TFNA, TFNA-AM, and TFNG are stable in/on the RAC
samples of strawberry, cucumber and canola stored frozen for up to 460,
336 and 735 days, respectively.  The available data on five diverse
crops (oil seed, non-oily grain, root and tuber crop, leafy vegetables,
and fruiting vegetables) support the storage conditions and durations on
strawberry, cucumber and canola.  

Food Handling (860.1460)

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

Meat, Milk, Poultry, and Eggs (860.1480)

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

Crop Field Trials (860.1500)

Strawberry

DER Reference:  48657101

The IR-4 has submitted field trial data for flonicamid on strawberries. 
Eight field trials were conducted in the United States during the 2008
growing season in the North American Free Trade Agreement (NAFTA)
Growing Zones 1 (NY; 1 trial), 2 (NC; 1 trial), 3 (FL; 1 trial), 5 (WI;
1 trial), 10 (CA; 3 trials), and 12 (OR; 1 trial).  

Two trials [CA*59 and CA*60 (Salinas, CA)] were conducted at the same
location by the same field research director (FRD).  The differences
between the trials were:  use of different tank mixes for all
applications; a 60- to 62-day off-set in application dates; and use of
different application equipment (in two of three applications).  HED has
concluded that the differences are insufficient to classify the trials
as two separate trials (ChemSAC, 11/2/2011).  The number of independent
trials is seven.

Each trial consisted of one untreated plot and one treated plot.  At
each trial location, the treated plot received three foliar broadcast or
directed applications of a 50% water soluble granule (SG) formulation of
flonicamid (Beleaf 50 SG) at 0.086-0.094 lb ai/A/application, for a
total seasonal rate of 0.263-0.280 lb ai/A.  Applications were made at
the blooming to mature fruit stage with retreatment intervals (RTI)
between 6- to 8-days, except at trials OR12 and FL24, where one
application at each trial was made at an RTI of 10-11 days due to rain. 
Applications were made using ground equipment in spray volumes of 27-53
gal/A.  Except for one trial, a nonionic surfactant (NIS) was added to
the spray mixture for each of the applications.

 

Samples were harvested from all trials at a 0-day pre-harvest interval
(PHI); additional samples of strawberries were collected at PHIs of 3,
5, and 7 days from one trial (NC13) to assess residue decline.  

Samples were analyzed for residues of flonicamid and metabolites TFNA,
TFNA-AM, and TFNG using a high performance liquid chromatography method
with tandem mass spectrometric detection (LC/MS/MS) adapted from FMC No.
P-3561M.  The quantifiable residues of TFNA, TFNA-AM, and TFNG were
converted to parent equivalents using molecular weight conversion
factors of 1.20, 1.21, and 0.92, respectively (MW of flonicamid 229.17
÷ MW of TFNA 191.11, MW of TFNA-AM 190.12, or MW of TFNG 248.2).  The
limit of quantitation (LOQ; determined as the lowest level of method
validation, LLMV) was 0.02 ppm for each analyte.  The method was
adequate for data collection based on acceptable method validation and
concurrent recovery data.  The fortification levels used in method
validation and concurrent method recovery were adequate to bracket
expected residue levels.  Concurrent recoveries and residues in the
treated samples were not corrected for residues in controls.  The LOD
for each matrix was calculated by multiplying the standard deviation of
recovery measurements at the LLMV by the one-tailed t-statistic
(confidence level not reported) for six to seven replicates, and the LOQ
was defined as 3x the LOD.  The calculated LOQs in strawberries were
0.0094, 0.0153, 0.0134, and 0.0104 ppm, respectively, for flonicamid,
TFNA, TFNA-AM, and TFNG; corresponding calculated LOD values were
0.0031, 0.0051, 0.0045, and 0.0035 ppm. 

Following three foliar broadcast or directed applications of the 50% SG
formulation of flonicamid at 0.263-0.280 lb ai/A, residues (and per
trial averages) of flonicamid, metabolites TFNA, TFNA-AM, TFNG, and
combined residues of the four analytes, respectively, in/on strawberries
harvested at a 0-day PHI were:  0.11-0.66 (0.13-0.54), <0.02-0.12
(<0.02-0.12), <0.02 (<0.02), <0.02-0.083 (<0.02-0.080), and <0.17-<0.79
(<0.19-<0.73) ppm.  

Data from the residue decline trial showed that residues of flonicamid
and combined residues decreased in strawberries with increasing PHIs;
however, residues of TFNA increased with increasing PHIs.  Residue
decline could not be assessed for TFNA-AM and TFNG because residues were
below the LOQ in/on all samples.

A summary of residue data from the strawberry field trials is presented
in Table 6.

TABLE 6.  Summary of Residue Data from Strawberry Field Trials with
Flonicamid.

Commodity	Analyte	Total

Rate

(lb ai/A)	PHI (days)	Residue Levels (ppm flonicamid equivalents)

n	Sample Min.	Sample Max.	LAFT1	HAFT1	Median	Mean	Std.  Dev.

Strawberry, Berries with caps removed	Flonicamid	0.263-0.280	0	7	0.11
0.66	0.13	0.54	0.34	0.34	0.16

	TFNA

<0.02	0.12	<0.02	0.12	0.052	0.051	0.035

	TFNA-AM

<0.02	<0.02	<0.02	<0.02	0.02	0.02	N/A

	TFNG

<0.02	0.083	<0.02	0.080	0.026	0.036	0.022

	Combined2

<0.17	<0.79	<0.19	<0.73	0.41	0.45	0.20

1 LAFT: Lowest average fielt trial;  HAFT: highest average field trial

2  Combined residues of flonicamid, TFNA, TFNA-AM, and TFNG

Conclusions.  The submitted strawberry field trial data are adequate. 
Following three foliar broadcast or directed applications of the 50% SG
formulation of flonicamid at 0.263-0.280 lb ai/A, residues (and per
trial averages) of flonicamid, metabolites TFNA, TFNA-AM, TFNG, and
combined residues of the four metabolites, respectively, in/on
strawberries harvested at a 0-day PHI were:  0.11-0.66, <0.02-0.12,
<0.02, <0.02-0.083, and <0.17-<0.79 ppm.  Data from the residue decline
trial showed that residues of flonicamid and total residues decreased in
strawberries with increasing PHIs; however, residues of TFNA increased
with increasing PHIs.  Residue decline could not be assessed for TFNA
and TFNG because residues were below the LOQ in/on all samples.

An acceptable method was used for residue quantitation, and adequate
data were submitted to support sample storage intervals and conditions.



Cucumber

	

DER Reference:  48657102

Four greenhouse cucumber trials were conducted in zones 2 (1 trial each
in MD and TN), 5 (1 trial in ON) and 9 (1 trial in CO) during 2008 and
2009.   Each trial site consisted of two treated plots and one untreated
control plot.  At one of the treated plots, two foliar ground
applications of flonicamid (Beleaf 50SG insecticide) were applied 6-7
days apart at rates ranging from 0.129-0.147 lb a.i./A (0.145-0.165 kg
a.i./ha) per application for total rates of 0.262-0.291 lb a.i./A
(0.294-0.326 kg a.i./ha) per season.  A nonionic surfactant was included
in the tank mix for the second foliar application at trial CO06
(Activator 90; 0.25% v/v) and in both foliar applications at trials TN04
(Co-Op; 0.25% v/v) and ON03 (Agral 90; 0.25% v/v).  The second treated
plot received two simulated chemigation applications of flonicamid to
the rock wool substrate in which the cucumber plants were grown using a
syringe, 6-7 days apart.  The rates (per acre [hectare]) determined
using an average plant density of 2.4 plants per square meter, ranged
from 0.130-0.134 lb a.i./A (0.146-0.150 kg a.i./ha) per application for
total rates of 0.264-0.269 lb a.i./A (0.296-0.302 kg a.i./ha) per
season.  No adjuvants were included in any of the chemigation- applied
mixtures.  Mature cucumber fruit samples were harvested from all treated
plots on the day of the last application, after the foliar spray had
dried (i.e., 0-day PHI). At the ON03 trial, samples were harvested from
both treated plots at additional PHIs of 3, 5, and 7 days to evaluate
any residue decline. 

Cucumber fruit samples were analyzed for the combined residues of
flonicamid and the three major metabolites, 4-trifluoromethylnicotinic
acid (TFNA), 4-trifluoromethylnicotinamid (TFNA-AM), and N-(4-trifluoro-
methylnicotinoyl)glycine (TFNG), using a liquid chromatography with mass
spectroscopic detection (LC-MS) working method entitled “Residue
Analysis of Flonicamid, TFNA, TFNG, TFNA-AM by LC/MS, Version #3”. 
This method is similar to the previously reviewed reference method No.
P-3561 entitled “Analytical Methodology for IKI-220 (F1785) and its
Major Metabolites in/on Peach, Potato Tuber, and Wheat Straw, FMC Corp.
P-3561M”.  The calculated limit of quantitation (LOQ) was 0.017 ppm
for flonicamid, 0.0094 ppm for TFNA, 0.011 ppm for TFNA-AM, and 0.0081
ppm for TFNG.  The limit of detection (LOD) was calculated to be 0.0056,
0.0031, 0.0036 and 0.0027 ppm for flonicamid, TFNA, TFNA-AM and TFNG,
respectively. The LLMV for cucumber was determined to be 0.020 ppm for
flonicamid and each of the metabolites.  Based on acceptable method
validation and concurrent recoveries within the range of 70-120%, the
method is adequate for data gathering purposes in cucumber fruit
matrices in this study.

  SEQ CHAPTER \h \r 1 The maximum storage interval for treated cucumber
samples was 329 days from harvest to extraction.  All extracted samples
were analyzed within 14 days.  Concurrent freezer storage stability
tests conducted as part of the trial study demonstrated that residues of
flonicamid, TFNA, TFNA-AM and TFNG are stable in cucumbers for up to 336
days of frozen storage, which adequately covers the frozen storage
interval for treated cucumber samples in this study.  

In cucumbers harvested at a 0-day PHI, total residues of flonicamid and
the TFNA, TFNA-AM and TFNG metabolites were <0.203-<0.208 ppm following
two foliar spray applications at total rates of 0.264 lb a.i./A (0.296
kg a.i./ha) without an adjuvant in the spray mixture and <0.106-<0.775
ppm following two foliar applications at rates totaling 0.262-0.291 lb
a.i./A (0.294-0.326 kg a.i./ha) including an adjuvant in one or both of
the spray mixtures.  In cucumbers harvested at a 0-day PHI following two
simulated chemigation applications to the growth medium at total rates
of 0.264-0.269 lb a.i./A (0.296-0.302 kg a.i./ha), total residues were
<0.079-<0.341 ppm.  

Residue decline data indicated that following foliar applications,
residues in cucumber fruit 

decreased with increasing PHIs from 0-7 days;  the residues increased
slightly with increasing PHIs from 0-7 days in cucumber fruit following
simulated chemigation applications to the growth medium.  

A summary of residue data from the cucumber greenhouse trials is
presented in Table 7.

TABLE 7.	Summary of Residue Data from GreenhouseTrials with Flonicamid.

Commodity	Analyte	Total Rate  lb ai/A 

[kg ai/ha]	PHI (days)	Residue Levels

 (ppm)

n	Min.	Max.	LAFT*	HAFT*

	Median

(STMdR)	Mean

(STMR)	Std. Dev.

Foliar

Cucumber fruit	Flonicamid	0.262-0.291 [0.294-326]	0	4	<0.046	0.69	0.054
0.54	0.101	0.2	0.23-

	TFNA

<0.02	0.034	<0.02	0.031	0.02	0.23	0.005

	TFNA-AM

<0.02	<0.02	<0.02	<0.02	0.02	0.02	0

	TFNG

<0.02	0.03	<0.02	0.028	0.02	0.23	0.004

Chemigation

Cucumber fruit	Flonicamid	0.264-0.269 [0.296-0.302]	0	4	0.012	0.2	0.013
0.2	0.112	0.11	0.073

	TFNA

<0.02	0.023	0.02	0.023	0.02	0.021	0.001

	TFNA-AM

<0.02	<0.02	<0.02	<0.02	0.02	0.02	0

	TFNG

<0.02	0.11	<0.02	0.11	0.02	0.043	0.04

*LAFT = Lowest average field trial; HAFT = Highest average field trial. 

Conclusion.   SEQ CHAPTER \h \r 1 The cucumber greenhouse trials are
considered scientifically acceptable.  In cucumbers harvested at a 0-day
PHI, total residues of flonicamid and the TFNA, TFNA-AM and TFNG
metabolites were <0.203-<0.208 ppm following two foliar spray with
adjuvant added in both first and second spray mixtures,  <0.106-<0.775
ppm following two foliar applications with adjuvant added in the first
spray mixtures.  Total residues in cucumbers harvested at a 0-day PHI
following two simulated chemigation applications were <0.079-<0.341 ppm.
 

Residue decline was observed with increasing PHI in cucumber treated by
foliar spray.  The residues in the chemigation treatment increased with
increasing PHI from 0 to 7 days. 

Canola

DER Reference:	48657103.de.1

The IR-4 has submitted field trial data for flonicamid on canola.  Nine
field trials were conducted in the United States during the 2007-2008
growing seasons in the North American Free Trade Agreement (NAFTA)
Growing Zones 2 (NJ; 1 trial), 5 (SD; 3 trials), 7 (ND; 2 trials), and
11 (ID and WA; 3 trials).

Two WA trials (WA05 and WA10) were conducted by different Principal
Field Investigators (PFIs) at the same trial location; examination of
the field trial records indicates that there are sufficient differences
between the trials, including a 372- to 373-day offset in application
dates, for the trials to constitute separate trials for purposes of
OCSPP 860.1500 data requirements.  Three of the SD trials (SD02, SD03,
and SD05) were conducted by the same PFI.  Careful examination of the
field trial records indicates that the only differences between trials
SD02/SD03 were:  use of different tank mixes for all applications, a
~7-mile separation between the two trial locations, and a 1-day off-set
in application dates (application 1 only).  HED has concluded that the
differences between the trials (SD02 and SD03) are insufficient to
classify them as separate trials; therefore, these trials constitute a
single trial with replicate samples for purposes of OCSPP 860.1500 data
requirements.  Examination of the field trial records indicates that
there are sufficient differences between trials SD05 and SD02/SD03,
including a 377 to 380-day offset in application dates for this trial to
constitute a separate trial.  The adjustment in trial numbers results in
a total of eight field trials, with two trials conducted in NAFTA Zone
5.

Each trial consisted of one untreated plot and one treated plot.  At
each trial location, the treated plot received three foliar broadcast
applications of a 50% water soluble granule (SG) formulation of
flonicamid (Beleaf 50 SG) at 0.085-0.092 lb ai/A/application, for a
total seasonal rate of 0.261-0.272 lb ai/A.  Applications were made at
6- to 8-day RTIs using ground equipment in spray volumes of 10-20 gal/A.
 No adjuvants were added to the spray mixtures at any trial site. 
Samples of canola seed were harvested from all trials at a 6- to 8-day
PHI) seed samples from four trial sites were dried in the field or
greenhouse for 1-10 days prior to collection.  

Samples were analyzed for residues of flonicamid and its metabolites
(TFNA, TFNA-AM, and TFNG) using the high performance liquid
chromatography with tandem mass spectrometric detection (LC/MS/MS)
adapted from FMC No. P-3561M.  The limit of quantitation (LOQ;
determined as the lowest level of method validation, LLMV) was 0.02 ppm
for each analyte.  Variable recoveries were obtained in method
validation and concurrent method validation reflecting fortification
with each analyte at 0.020, 0.20, and 2.0 ppm.  Method validation
recoveries were generally slightly low (flonicamid, TFNA, and TFNA-AM)
to very low (TFNG) for all analytes at all fortification levels except
flonicamid at 2.0 ppm and TFNA-AM at 0.20 and 2.0 ppm, for which
recoveries were acceptable (mean 78-84%).  Concurrent recoveries for all
analytes were generally acceptable at the 0.20 and 2.0 ppm fortification
levels:  mean recoveries were 72-85% with standard deviations of 4-12%. 
However, low concurrent recoveries were obtained at 0.020 ppm:  53% for
flonicamid, 68% for TFNA, 62% for TFNA-AM, and 41% for TFNG.  The
petitioner noted that the lower than expected recoveries were caused by
ion suppression due to matrix interference.  Several approaches were
taken to reduce the ion suppression, including additional cleanups and
different elution programs, but the problem could not be eliminated. 
The ChemSAC reviewed the situation and concluded that the LOQ is 0.2 ppm
for each analyte in canola matrices (03/14/2012).  The fortification
levels used in method validation and concurrent method recovery were
adequate to bracket expected residue levels.  Concurrent recoveries were
corrected for residues in the controls; residues in the treated samples
were not corrected for residues in controls. Quantifiable residues of
TFNA, TFNA-AM, and TFNG were converted to parent equivalents by the
study reviewer using molecular weight conversion factors of 1.20, 1.21,
and 0.92, respectively (MW of flonicamid 229.17 ÷ MW of TFNA 191.11, MW
of TFNA-AM 190.12, or the MW of TFNG 248.2).

Samples were stored frozen (< -15 °C) from collection to analysis for
311-748 days (10.2-24.6 months).  Samples were analyzed within 0-3 days
of extraction.  Storage stability data generated concurrently with the
field trial study demonstrate that residues of flonicamid, TFNA,
TFNA-AM, and TFNG were stable in/on samples of canola stored frozen for
up to 735 days (24.2 months).  

Residue decline data on canola were not submitted.  Since sufficient
data have been reported on residue decline of residues in a variety of
crops, further study on canola is necessary (See D290386, 4/22/2005).  

A summary of the residue data is presented in Table 8.  The combined
residues of flonicamid and metabolites TFNA, TFNA-AM, TFNG following
three foliar broadcast applications of the 50% SG formulation of
flonicamid at 0.261-0.272 lb ai/A, residues (per trial averages,
calculated as flonicamid equivalents) are:  <0.2-0.333 and  <0.18-0.287
ppm for flonicamid and metabolite TFNG, respectively; residues of TFNA
and TFNA-AM are below the LOQ (<0.24 ppm).  The combined residues of
flonicamid and the three metabolites are <086-1.10 ppm.

TABLE 8.  Summary of Residue Data from Canola Field Trials with
Flonicamid.

Commodity	Analyte	Total

Rate

(lb ai/A)	PHI (days)	Residue Levels (ppm flonicamid equivalents)1,2

n	Sample Min.	Sample Max.	LAFT2	HAFT2	Median	Mean	Std.  Dev.

Canola seed	Flonicamid	0.261-0.272	6-8	8	<0.2	0.333	<0.2	0.333	0.2	0.215
0.048

	TFNA 

<0.24	<0.24	<0.24	<0.24	0.24	0.24	0

	TFNA-AM

<0.24	<0.24	<0.24	<0.24	0.24	0.24	0

	TFNG

<0.18	0.287	<0.18	0.287	0.18	0.195	0.039

	Combined3

<0.86	1.10	<0.86	1.1	0.86	0.650	0.245

1 The LOQ was 0.2 ppm for all analytes.  Values reflect per trial
averages; n = no. of field trials.  Data reflect conversion of
quantifiable residues of TFNA, TFNA-AM, and TFNG to parent equivalents
by the study reviewer.

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

3 Combined residues of flonicamid, TFNA, TFNA-AM, and TFNG calculated
using molecular weight conversion factors of 1.20, 1.21, and 0.92,
respectively.

Conclusion. The submitted canola field trial data are acceptable. The
residues of flonicamid, TFNA, TFNA-AM and TFNG in/on canola seed
harvested at a 6- to 8-day PHI following three foliar broadcast
applications of the 50% SG formulation of flonicamid at 0.261-0.272 lb
ai/A were  <0.2-0.333 ppm and  <0.2-0.287 ppm for flonicamid and TFNG,
respectively.  The residues were <LOQ (<0.2 ppm) for TFNA and TFNA-AM in
all trials.  The combined residues of flonicamid and the three
metabolites are <086-1.10 ppm.

Processed Food and Feed. 860.1520

Canola

DER Reference:	48657103.de.2

A processing study was carried out to determine the magnitude of
flonicamid, TFNA, TFNA-AM and TFNG residues in canola seed (RAC) and
processed canola commodities.  In one field trial, Beleaf 50SG was
applied as three foliar broadcast applications in/on  canola at an
exaggerated rate  ( ~3x ) of 0.272-0.276 lb ai/A/application for a total
rate of 0.821 lb ai/A.  Applications were made at 6-day RTIs using
ground equipment in spray volumes of 15-20 gal/A.  No adjuvants were
added to the spray mixture.  

Canola seed was harvested at an 8-day PHI and stored frozen within 29
minutes of collection and were shipped frozen within 28 days of harvest
via ACDS truck to the processing facility.  Processing was completed
within 195 days of harvest, and the samples were placed in frozen
storage (~-18 °C) for up to 6 days prior to shipment via overnight air
express to the analytical laboratory, the Food and Environmental Quality
Laboratory at Washington State University (FEQL; Richland, WA) for
analysis.  At the analytical laboratory, samples were stored frozen
(<-15 °C) until analysis.

The processing procedures simulated commercial operations to generate
the required fractions of canola seed (RAC) into meal and oil. 

Samples were analyzed for residues of flonicamid and metabolites TFNA,
TFNA-AM, and TFNG using the LC/MS/MS method FMC No. P-3561M as described
under analytical methods.  A number of minor modifications to the method
were specified, including changes in clean-up procedures, reagents, and
sample sizes.  Conversion to parent equivalents was not necessary
because residues of the metabolites in canola meal and oil were below
the LOQ in/on all samples.  

Briefly, samples of seed were extracted twice with acetonitrile
(ACN):water (1:1, v:v), then centrifuged and filtered.  The combined
extract was acidified with concentrated HCl and cleaned up using C18
solid phase extraction (SPE), then evaporated to remove ACN.  The sample
was partitioned with ethyl acetate four times; and the ethyl acetate
fractions were combined, reduced by evaporation, and applied to a
Carbograph SPE cartridge.  The resulting eluate was evaporated to
dryness and re-suspended in 1% formic acid for LC/MS/MS analysis. 

Samples of meal were extracted with ACN/water as above.  The combined
aqueous extract was adjusted to volume with water and evaporated to
remove ACN, then partitioned with hexane and evaporated to remove
hexane.  The resulting extract was acidified with concentrated HCl and
subjected to partitioning with ethyl acetate followed by Carbograph SPE
cleanup as above.  The resulting eluate was evaporated to dryness and
re-suspended in 1% formic acid for LC/MS/MS analysis. 

Samples of oil were extracted with ACN/water, partitioned with hexane,
and acidified as for meal, then subjected to C18 SPE clean-up as for
seed.  The eluate was partitioned with ethyl acetate four times, and the
ethyl acetate fractions were combined, reduced by evaporation and
adjusted to volume with 1% formic acid for LC/MS/MS analysis.

The LOQ (determined as the LLMV) was 0.02 ppm for each analyte.  The
LODs were calculated as 1/3 the LOQs. 

Residue data from the canola processing study are reported in Table 9. 
Residues of flonicamid were 0.232 ppm in/on canola seed (RAC) and below
the LOQ (<0.02 ppm) in meal and oil.  Residues of TFNA, TFNA-AM, and
TFNG were each below the LOQ (<0.02 ppm) in/on canola seed, meal, and
oil.  Combined residues of flonicamid, TFNA, TFNA-AM, and TFNG were
<0.292 ppm in/on seed and <0.08 ppm in meal and oil.  The processing
data indicate that combined residues of flonicamid, TFNA, TFNA-AM, and
TFNG do not concentrate in meal or oil (processing factor <0.27x).

The processing factors calculated in this study were less than the
maximum theoretical concentration factors for canola of 1.9x for meal
and 3.0x for oil (based on separation into components; OCSPP 860.1520,
Table 3).

TABLE 9.	Residue Data from Canola Processing Study with Flonicamid.

RAC	Processed Commodity	Total Rate

(lb ai/A)	PHI	Residues (ppm)1 [Average]	Processing Factor2

Flonic-amid	TFNA	TFNA-AM 	TFNG	Com-bined3	Flonic-amid	TFNA	TFNA-AM	TFNG
Com-bined3

Canola	Seed

(RAC)	0.821	8	--4,

0.232

[0.232]	<0.02,

<0.02

[<0.02]	<0.02,

<0.02

[<0.02]	<0.02,

<0.02

[<0.02]	<0.292

[<0.292]	NA5-	NA	--	--	--

	Meal

	<0.02,

<0.02

[<0.02]	<0.02,

<0.02

[<0.02]	<0.02,

<0.02

[<0.02]	<0.02,

<0.02

[<0.02]	<0.08,

<0.08

[<0.08]	<0.09x	NC5	NC	NC	<0.27x

	Oil

	<0.02	<0.02	<0.02	<0.02	<0.08	<0.09x	NC	NC	NC	<0.27x

1 The LOQ was 0.02 ppm for all analytes.  Averages and combined residues
were calculated by the study reviewer using the LOQ for values reported
as <LOQ.  The second value for seed and meal reflects the results of
redilution (seed) or reinjection (meal).  Residues of the metabolites
were <LOQ in/on all samples and therefore were not converted to parent
equivalents.

2 Processing Factor = [Measured residue for analyte in the processed
fraction] / [Measured residue for analyte in the RAC]. 

3 Combined residues of flonicamid, TFNA, TFNA-AM, and TFNG.

4 The first value obtained for seed (0.143 ppm) was rejected by the
study director because it was outside the linearity range.

5 NC = Not calculated; residues were below the LOQ (<0.02 ppm for all in
analytes) in the RAC and processed fraction; NA= not available

Conclusions.  The processing study is acceptable to satisfy data
requirements.  Adequate processing studies on canola are available.  The
observed processing factors for canola meal and canola oil were each
<0.27x.  Therefore, tolerances for residues on meal and oil are not
needed. 

Submittal of Analytical Reference Standards (860.1650)

As of April 26, 2012, the analytical reference standards for flonicamid
and the metabolites TFNA, TFNA-AM and TFNG including TFNA-OH and TFNG-AM
are available at the EPA National Pesticide Standards Repository with
expiration dates ranging from 2014 – 2016 (personal communication,
Dallas Wright and Theresa Cole, ACB, 05/26/2012).

Confined Accumulation in Rotational Crops (860.1850)

No new study was conducted under this guideline and none is required. 

Field Accumulation in Rotational Crops (860.1900)

No new data was submitted for this guideline and none is required in
support of the current petition.

Proposed Tolerances (860.1550)

The IR-4 has proposed the establishment of permanent tolerances for
berry low growing subgroup 13-07G, cucumber for greenhouse use, and
rapeseed, subgroup 20A.

According to HED’s Interim Guidance on Tolerance Expressions (5/27/09,
S. Knizer), the tolerance expression should be stated as follows:

Tolerances are established for the residues of the insecticide
flonicamid, including its metabolites and degradates, in or on the
commodities in the table below.  Compliance with the tolerance levels
specified below is to be determined by measuring only the sum of
flonicamid [N-(cyanomethyl)-4-(trifluoromethyl)-3-pyridinecarboxamide]
and its metabolites TFNA (4-trifluoromethylnicotinic acid), TFNA-AM
(4-trifluoromethylnicotinamide), and TFNG
[N-(4-trifluoromethylnicotinoyl)glycine], calculated as the
stoichiometric equivalent of flonicamid, in or on the following
commodities.

 

The submitted magnitude of the residue data for the RACs of the
representative crops (strawberry, cucumber, and canola) are adequate to
support the tolerance and registration requests for berry, low growing,
subgroup13-07G,  cucumber for greenhouse use, and rapeseed subgroup 20A.
  The OECD spreadsheet calculation procedure was used to determine
appropriate tolerance levels; see Appendix II.

HED recommends for establishment of tolerances using the same tolerance
expression and at the tolerance levels listed in Table 10 below.  The
petitioner should submit a revised section F reflecting the tolerances
and commodity definitions as recommended.

Table 10.  Tolerance Summary for Flonicamid

Commodity	Established/Proposed Tolerance 

(ppm)	Recommended Tolerance (ppm)	Comments (correct commodity
definition)

Berry, low growing, subgroup 13-07G	1.4	1.51

	Cucumber for greenhouse use only	1.3	1.52	Vegetable, cucurbit, group 92

Rapeseed subgroup 20A	1.5	1.53

	1 The representative commodity for the berry, low growing, subgroup
13-07G is strawberry.  The OECD spreadsheet calculation procedure gave
values of 1.5 ppm for strawberry.

2 A tolerance was currently established on cucumber at 0.4 ppm, as a
member of the cucurbit vegetable group.  The current petition is to
increase the tolerance to 1.3 ppm for cucumber grown in greenhouse only.
 The OECD spreadsheet calculation procedure gave values of 1.5 ppm for
cucumber grown in the greenhouse treated at the proposed label rate by
foliar spray.  The OECD spreadsheet calculation procedure gave a value
of 0.7 ppm for cucumber treated by chemigation in the greenhouse. This
tolerance value and the existing tolerance of 0.40 ppm in 40 CFR
§180.613 will be covered under the foliar spray treatment in
greenhouse.  

3 The representative commodity for the rapeseed, subgroup 20A is canola.
 The OECD spreadsheet calculation procedure gave values of 1.5 ppm for
canola. 

 

No tolerances are required for the processed commodities of canola based
on the demonstrated processing factor of <0.27x for each canola meal and
canola oil.  The maximum theoretical concentration factors for canola
meal and canola oil are 1.9x and 3.0x, respectively (OCSPP §860.1520,
Table 3). 

The tolerance expression under §180.613(a)(2) for  livestock
commodities should be stated as:

	Tolerances are established for the residues of the insecticide
flonicamid, including 	its metabolites and degradates, in or on the
commodities in the table below.  	Compliance with the tolerance levels
specified below is to be determined by 	measuring only the sum of
flonicamid [N-(cyanomethyl)-4-(trifluoromethyl)-3-	pyridinecarboxamide]
and its metabolites TFNA (4-trifluoromethylnicotinic acid), 	and TFNA-AM
(4-trifluoromethylnicotinamide), calculated as the stoichiometric 
equivalent of flonicamid, in or on the following commodities.

The existing livestock commodity tolerances are adequate.

There are currently no Codex or Canadian maximum residue limits (MRLs)
established for residues of flonicamid in crop or livestock commodities.
 An International Residue Limit Status sheet (IRL) is attached to this
Summary Document (APPENDIX  I).

  SEQ CHAPTER \h \r 1 Attachments:  

Appendix I - International Residue Limit Status sheet

Appendix II - Tolerance Assessment Calculations

Template Version September 2005

Appendix I

International Residue Limits

Flonicamid (PC Code 128016; 04/26/2012) 

Summary of US and International Tolerances and Maximum Residue Limits 

Residue Definition:

US	Canada	Mexico2	Codex3

40 CFR 180.613:

Plant :  flonicamid [N
-(cyanomethyl)-4-(trifluoromethyl)-3-pyridinecarboxamide] and its
metabolites TFNA [4-trifluoromethylnicotinic acid], TFNA-AM
[4-trifluoromethylnicotinamide], and TFNG [N
-(4-trifluoromethylnicotinoyl)glycine]

 Livestock: residues of flonicamid [N
-(cyanomethyl)-4-(trifluoromethyl)-3-pyridinecarboxamide], and its
metabolites TFNA [4-trifluoromethylnicotinic acid] and TFNA-AM
[4-trifluoromethylnicotinamide] 	None

None

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

	US	Canada	Mexico2	Codex3

Berry, low growing, subgroup 13-07G	1.5

	Vegetable, cucurbit, group 9 	1.5

	Rapeseed Subgroup 20A	1.5

	Completed: M. Negussie; 05/01/2012

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.

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

Appendix II

Tolerance Assessment Calculations

For each of the crops listed below, the OECD calculator was used for
calculating recommended tolerances.  As specified in the OECD document,
the average residue value was used 

The rounding procedures specified in the OECD guideline were also used.

For each of the crops listed below, the field trials reflect the
proposed application rates and samples were collected at the proposed
pre-harvest intervals.  

Berry, Low Growing, Subgroup 13-07G

The dataset used to establish a tolerance for residues of flonicamid
in/on berry, low growing consisted of field trial data representing
total application rate of 0.263-0.280 lb ai/A (3 applications at
0.086-0.094 lb ai/A/application) with a 0-day PHI.  The representative
crop of the low growing berry is strawberry.  The average residue values
for strawberry crop field trial used to calculate the tolerances are
provided in Table II-1 and these values were entered in the OECD
calculator.  Using the OECD calculator, the recommended tolerance is 1.5
ppm.  A crop group tolerance is appropriate for berry low growing
subgroup 13-07G.  The recommended tolerance is slightly higher than the
proposed (1.4 ppm).

Cucumber (Greenhouse)

The dataset used to establish a tolerance for residues of flonicamid
in/on greenhouse grown cucumber consisted of greenhouse trial data
representing two methods of application: (a) foliar application rates of
0.262-0.291lb ai/A (2 foliar applications at  0.129-0.147  lb
ai/A/application) with a 6-7-days RTI and 0-days PHI) and (b)
application by simulated chemigation to the rock wool substrate in which
the cucumber plants were grown using syringe) at rates of 0.264-0.269 lb
ai/A (2 chemigation application at 0.130-0.134 lb ai/A/application) with
 a 6- to 7-day RTI and 0-days PHI.    

The average residue values for cucumber greenhouse trial (a) and (b)
used to calculate the tolerances are provided in Table II-1 and these
values were entered in the OECD calculator.  Using the OECD calculator,
the recommended tolerance is 1.5 ppm.  The recommended tolerance for
cucurbit vegetables, group 9, is higher than the proposed (1.3 ppm) for
greenhouse cucumbers.

The existing tolerance for cucurbit vegetables is 0.4 ppm.  This is
based on the evaluation of  crop field trial data for summer squash,
cantaloupe, and  cucumber (D290386, A. Acierto, 04/22/2005).  The
highest residues were 0.17 ppm on squash, 0.34 ppm on cucumber, and 0.25
ppm on cantaloupe. The recommended tolerance of 1.5 ppm for cucurbit
vegetables is appropriate for the representative commodities.

Rapeseed, Subgroup 20A

The dataset used to establish a tolerance for residues of flonicamid
in/on rapeseed consisted of field trial data representing total
application rate of 0.261-0.272 lb ai/A (3 applications at 0.085-0.092
lb ai/A/application) with 6- to 8-day RTI and 6- to 8-day and 6- to
8-day PHI.  The representative crop is canola.   The average residue
values for the canola field trial used to calculate the tolerances are
provided in Table II-1 and these values were entered in the OECD
calculator.  Using the OECD calculator, the recommended tolerance is 1.5
ppm.  A crop group tolerance is appropriate for rapeseed subgroup 20A. 
The proposed tolerance of 1.5 ppm is appropriate.

Flonicamid

Strawberry

USA

0.258-0.282 lb ai/A

 	 

Total number of data (n)	7

Percentage of censored data	0%

Number of non-censored data	7

Lowest residue	0.200

Highest residue	0.710

Median residue	0.410

Mean	0.446

Standard deviation (SD)	0.193

Correction factor for censoring (CF)	1.000

 	 

Proposed MRL estimate	 

 	 

- Highest residue	0.710

- Mean + 4 SD	1.219

- CF x 3 Mean	1.337

Unrounded MRL	1.337

 	 

Rounded MRL	1.5

 	 

 High uncertainty of MRL estimate.

[Small dataset]

 

 

Residues (mg/kg)	n

0.2	1

0.25	1

0.36	1

0.41	1

0.56	1

0.63	1

0.71	1

Flonicamid

Cucumber (Member of Cucurbit Crop Group)

USA/Canada

Foliar,0.262-0.291lb ai/A, 0-day PHI

 	 

Total number of data (n)	4

Percentage of censored data	0%

Number of non-censored data	4

Lowest residue	0.114

Highest residue	0.619

Median residue	0.164

Mean	0.265

Standard deviation (SD)	0.240

Correction factor for censoring (CF)	1.000

 	 

Proposed MRL estimate	 

 	 

- Highest residue	0.619

- Mean + 4 SD	1.224

- CF x 3 Mean	0.795

Unrounded MRL	1.224

 	 

Rounded MRL	1.5

 	 

 High uncertainty of MRL estimate.

[Small dataset]

Residues (mg/kg)	n

0.114	1

0.121	1

0.206	1

0.619	1

Flonicamid

Cucumber (Member of Cucurbit Crop Group)

USA and Canada

Chemigation  0.264-0.269 lb ai/A (0.296-0.302 kg/ha, 0-day PHI

 	 

Total number of data (n)	4

Percentage of censored data	0%

Number of non-censored data	4

Lowest residue	0.079

Highest residue	0.341

Median residue	0.175

Mean	0.192

Standard deviation (SD)	0.110

Correction factor for censoring (CF)	1.000

 	 

Proposed MRL estimate	 

 	 

- Highest residue	0.341

- Mean + 4 SD	0.633

- CF x 3 Mean	0.577

Unrounded MRL	0.633

 	 

Rounded MRL	0.7

 	 

 High uncertainty of MRL estimate.

[Small dataset]

Residues (mg/kg)	n

0.079	1

0.154	1

0.195	1

0.341	1



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Region / USA

0.261-0.272 lb ai/A PHI = 6-8 days 

 	 

Total number of data (n)	8

Percentage of censored data	75%

Number of non-censored data	2

Lowest residue	0.860

Highest residue	1.100

Median residue	0.860

Mean	0.895

Standard deviation (SD)	0.084

Correction factor for censoring (CF)	0.500

 	 

Proposed MRL estimate	 

 	 

- Highest residue	1.100

- Mean + 4 SD	1.231

- CF x 3 Mean	1.343

Unrounded MRL	1.343

 	 

Rounded MRL	1.5

 	 

 High uncertainty of MRL estimate.

[High level of censoring]

Residues (mg/kg)	n

 < 0.86 	6

0.9	1

1.1	1

	

Flonicamid	Summary of Analytical Chemistry and Residue Data	DP# D396902

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