United States Prevention, Pesticides EPA712-C-96-184
Environmental Protection and Toxic Substances August 1996
Agency (7101)
&EPA Residue Chemistry
Test Guidelines
OPPTS 860.1520
Processed Food/Feed
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INTRODUCTION
This guideline is one of a series of test guidelines that have been
developed by the Office of Prevention, Pesticides and Toxic Substances,
United States Environmental Protection Agency for use in the testing of
pesticides and toxic substances, and the development of test data that must
be submitted to the Agency for review under Federal regulations.
The Office of Prevention, Pesticides and Toxic Substances (OPPTS)
has developed this guideline through a process of harmonization that
blended the testing guidance and requirements that existed in the Office
of Pollution Prevention and Toxics (OPPT) and appeared in Title 40,
Chapter I, Subchapter R of the Code of Federal Regulations (CFR), the
Office of Pesticide Programs (OPP) which appeared in publications of the
National Technical Information Service (NTIS) and the guidelines pub-
lished by the Organization for Economic Cooperation and Development
(OECD).
The purpose of harmonizing these guidelines into a single set of
OPPTS guidelines is to minimize variations among the testing procedures
that must be performed to meet the data requirements of the U. S. Environ-
mental Protection Agency under the Toxic Substances Control Act (15
U.S.C. 2601) and the Federal Insecticide, Fungicide and Rodenticide Act
(7U.S.C. I36,etseq.).
Final Guideline Release: This guideline is available from the U.S.
Government Printing Office, Washington, DC 20402 on The Federal Bul-
letin Board. By modem dial 202-512-1387, telnet and ftp:
fedbbs.access.gpo.gov (IP 162.140.64.19), internet: http://
fedbbs.access.gpo.gov, or call 202-512-0132 for disks or paper copies.
This guideline is also available electronically in ASCII and PDF (portable
document format) from the EPA Public Access Gopher (gopher.epa.gov)
under the heading "Environmental Test Methods and Guidelines."
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OPPTS 860.1520 Processed food/feed.
(a) Scope. (1) Applicability. This guideline is intended to meet test-
ing requirements of both the Federal Insecticide, Fungicide, and
Rodenticide Act (FIFRA) (7 U.S.C. 136, et seq.) and the Federal Food,
Drug, and Cosmetic Act (FFDCA) (21 U.S.C. 301, et seq.).
(2) Background. The source material used in developing this har-
monized OPPTS test guideline is OPP 171-4, Results of Tests on the
Amount of Residue Remaining, Including a Description of the Analytical
Methods Used (Pesticide Assessment Guidelines, Subdivision O: Residue
Chemistry., EPA Report 540/9-82-023, October 1982). This guideline
should be used in conjunction with OPPTS 860.1000, Background.
(b) Purpose. Processing studies are required to determine whether
residues in raw commodities may be expected to degrade or concentrate
during food processing. If residues do concentrate in a processed commod-
ity, a food or feed additive tolerance must be established under section
409 of the FFDCA (or a section 701 Maximum Residue Limit (MRL)
in some cases). However, if residues do not concentrate in processed com-
modities, the tolerance for the raw agricultural commodity (RAC) itself
applies to all processed food or feed derived from it.
(c) Concentration of residues on processing. (1) Whenever there
is a possibility of residue levels in processed foods/feeds exceeding the
level in a RAC, processing data are required. Examples of processed foods/
feeds in which residues may concentrate are apple juice and apple pomace,
the hulls, meal, and refined oil from cottonseed, or the sugar, dried pulp
and molasses from sugar beet roots. A list of processed byproducts is con-
tained in Table 1 of OPPTS 860.1000, Background.
(2) Processing studies should simulate commercial practices as closely
as possible. RAC samples used in processing studies should contain field-
treated quantifiable residues, preferably at or near the proposed tolerance
level, so that concentration factors for the various byproducts can be deter-
mined. As discussed in paragraph (f)(3) of this guideline, this may require
field treatment at exaggerated application rates to obtain sufficient residue
levels for processing studies. Processing studies utilizing spiked samples
are not acceptable, unless it can be demonstrated that the RAC residue
consists entirely of a surface residue.
(3) Only one processing study is required for each crop in Table 1
of OPPTS 860.1000 having a processed commodity. However, it is advis-
able to have multiple samples of the RAC and processed commodities
in the study. As stated in paragraph (f)(2) of this guideline, if multiple
processing studies are available for a given crop, the Agency will use the
average concentration factor obtained across these studies. In some cases
the requirement for a processing study may be waived based on field trial
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data for the RAC reflecting exaggerated application rates. This is discussed
in more detail in paragraph (f)(3) of this guideline.
(4) The total toxic residue should be measured in the raw agricultural
commodity at the time processing is initiated and in all processed com-
modities of the crop listed in Table 1 of OPPTS guideline 860.1000. With
the exception of the small grains, the Agency will not normally translate
data between crops. In the case of small grains, a processing study on
wheat satisfies the requirement for studies on barley, buckwheat, millet,
oats and rye if the pesticide is applied to all these crops in a similar manner
and comparable residue levels occur in the grains.
(5) Unless the processed commodities are analyzed within thirty days
of their production, data demonstrating the stability of residues in rep-
resentative processed commodities during storage are required as described
in OPPTS guideline 860.1380.
(6) If the processing studies indicate that residues concentrate on
processing, then a food additive petition, including a food additive regula-
tion proposal, is normally required as specified by section 409 of the
FFDCA. However, for a processed food or feed that is not ready-to-eat,
an MRL may need to be proposed under section 701 of the FFDCA. This
is explained in more detail in paragraph (f)(5) of this guideline.
(d) Reduction of the residue level on processing. In those cases
where the assumption of tolerance level residues occurring in commodities
results in unacceptable exposure, then the petitioner has the option of sub-
mitting data on food prepared for consumption. The Agency will take into
account data on washing, trimming, cooking, peeling or processing to the
extent that these procedures are used on specific commodities. Although
the lower levels of residues resulting from such processes may be used
in the risk assessment, the tolerance will still be set on the commodity
as it travels in interstate commerce. Of course, if these data indicate that
residues concentrate in some fractions while decreasing in others, both the
higher and lower residue levels will be used in the risk assessment. The
Agency will also take into account the wide variation in techniques used
to prepare food. For example, if cooking completely destroys the residue
on a vegetable, the Agency will use, at a maximum, the limit of quantita-
tion (LOQ) in the cooking study as the residue level for cooked vegetables.
The Agency will also use the consumption of uncooked vegetables and
the tolerance level to estimate the exposure from uncooked vegetables.
(e) Maximum theoretical concentration factors. (1) This paragraph
addresses maximum theoretical concentration factors for use in determina-
tion of the exaggerated application rate needed for field trials on commod-
ities which can be processed. The use of exaggerated rate studies is dis-
cussed in more detail in paragraph (f)(3) of this guideline. The following
Table 1 provides a listing of maximum theoretical concentration factors.
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A secondary use of this list could be for worst case dietary exposure as-
sessment, when experimental processing data are unavailable.
Table 1.—Maximum Theoretical Concentration Factors by Crop
Crop
Maximum Concentration Factor
Apples
Barley
Beets, sugar
Canola
Citrus
Coconut
Coffee
Corn
Cottonseed
Figs
Grapes
Mint (peppermint, spearmint)
Oats
Olive
Peanuts
Pineapple
Potatoes
Plums (prunes)
Rapeseed
Rice
Rye
Safflower
Soybeans
Sugarcane
Sunflower
Tomatoes
Wheat
>14x*
8x
>20x*
3x
1000x
3x
4.5x
25x
6x
3.5x
5x*
330x
8x**
10x
3x
4x
5x
3.5x
2x
8x
10x
9x
12x
>20x*
4.5x
5.5x*
8x
*Experimental factor
**Based on factor for wheat
(2) The list is not all inclusive as factors are not available for all
processed commodities listed in Table 1 of OPPTS 860.1000. In addition,
some processed commodities may have greater potential for concentration
than those processed commodities for which factors were calculated. For
those commodities for which higher concentrations are expected, the
Agency has tabulated some experimental concentration factors, by compar-
ing proposed and established food/feed additive tolerances to the proposed
and established tolerances for the RAC. Additional factors may be added
or updated in the future as further information becomes available.
(3) There are two types of processes for which maximum theoretical
concentration factors can easily be calculated. The first type is where the
concentration is based on the loss of water during processing. In this case,
the theoretical concentration factor is the ratio of the percent of dry matter
in the processed commodity to the percent of dry matter in the RAC. For
example, grapes contain 18 percent dry matter while raisins contain 85
percent dry matter. The theoretical concentration factor for the processing
of grapes into raisins is 85/18 or 4.7x. The second type of process is that
in which a RAC is separated into components, such as the processing of
corn grain into corn oil. In this case, the theoretical concentration factor
is 100 percent divided by the percentage of the processed commodity in
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the RAC. Corn grain may contain as little as 4 percent corn oil. The theo-
retical concentration factor for processing of corn into oil then is
100/4, or 25x.
(4) In cases where a crop had multiple processed fractions, only the
fraction having the highest maximum theoretical concentration factor is
listed in Table 1 (see paragraph (e)(l) of this guideline). In some cases,
only typical yields were available for a particular RAC, particularly for
grains. A factor was still calculated, but may not actually be the maximum
theoretical concentration factor. The following Table 2 shows calculations
for those commodities where concentration is based on loss of water, Table
3 shows calculations for those commodities where concentration is based
on separation into components, and Table 4 is a tabulation of experi-
mentally determined factors obtained by comparing proposed and estab-
lished food/feed additive tolerances to the proposed and established toler-
ances for the RAC. A bibliography for the tables is given in paragraph
(e)(5) of this guideline.
Table 2.—Theoretical Concentration Factors Based on Loss of Water
Crop
Figs
dry fiqs
Grapes
raisins
Potatoes
dried (flakes granules)
Plums
prunes
Tomatoes
puree
paste
percent dry
matter
22
76
18
85
20
93
21
72
6
8.5
33
Factor
3.5
4.7
47
34
1.4
5.5
Reference
PAM I sec 202 12
PAM I sec., 202.12
Harris Guide
Harris Guide
USDA
USDA
PAM I, sec. 202.12
PAM I sec 202 12
p 311 Commercial Vegetable
ing, 2nd Ed.
p. 272, Commercial Vegetable
ing, 2nd Ed.
p. 277, Commercial Vegetable
ing, 2nd Ed.
Process-
Process-
Process-
Table 3.—Theoretical Concentration Factors Based on Separation into Components
Crop
Barley grain
bran
pearled
Beets sugar
sugar
molasses
dried pulp
Canola
meal
oil
Mini-
mum
percent
of whole
13
82
8
52
33
Factor
7.7
1.2
12.5
1.9
3.0
Reference
based on wheat bran
p. 426, Principles of Field Crop Production
Advances in Sugar Beet Production
p. 259, by difference, CRC Handbook of Process-
ing and Utilization in Agriculture
p. 259, CRC Handbook of Processing and Utiliza-
tion in Agriculture
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Table 3.—Theoretical Concentration Factors Based on Separation into Components—Continued
Crop
Citrus
peel
oil
pulp dehydrated
juice
Coconut
oil
copra (dried meal)
Coffee
roasted bean
instant
Corn grain
oil
Cottonseed
hulls
meal
oil
Grapes
juice
Mint
oil
Oats
flour
rolled oats
Olive oil
oil
Peanuts
meal
oil
Pineapple
process residue
juice
Potatoes
processed waste
Rapeseed
meal
Rice grain (rough rice) ...
hulls
bran
Rye grain
bran
flour
Safflower
meal
Mini-
mum
percent
of whole
30
0.1
50
35
1.2
4
26
45
16
82
03
70
10
46
36
26
25
52
20
13
10
11
Factor
33
1000
2
29
2.1
18 percent
loss in
weight in
roasting
4.4
25.0
38
22
6.3
1.2
333
1 4
108
2.2
28
3.8
40
1.9
50
7.7
100
9.1
Reference
p 1391 Considine Foods and Food Production
Encyclopedia
PAM I, sec. 202.12
p. 1387, Considine Foods and Food Production
Encyclopedia
PAM I sec 202 1 5
ORES (from USDA Handbook No. 102)
p. 459 Considine
PP no. OE3875-based on weights in processing
study
p. 243, Corn, Culture, Processing, Products
p 187 CRC Handbook of Processing and Utiliza-
tion in Agriculture
p 187 CRC Handbook of Processing and Utiliza-
tion in Agriculture
p. 187, CRC Handbook of Processing and Utiliza-
tion in Agriculture
Harris Guide
15 ml_ oil from 10 Ib hay
p 577-8 Cereal Crops
p. 1372, Considine Foods and Food Production
Encyclopedia
p. 139, by difference, see p 293, Peanuts:....
PAM I sec 202 25
PP no 6F0482
NorthWest Food Processors Association
p. 259, by difference, CRC Handbook of Process-
ing and Utilization in Agriculture
pp 649 652 Cereal Crops
p. 649, 652, Cereal Crops
p 244-5 CRC Handbook of Processing and Utili-
zation in Agriculture
p. 114, CRC Handbook of Processing and Utiliza-
tion in Agriculture
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Table 3.—Theoretical Concentration Factors Based on Separation into Components—Continued
Crop
oil (safflower)
Soybeans
hulls
meal
oil
Sugarcane
molasses
sugar
Sunflower
meal
oil
Tomatoes
juice
Wheat grain
bran
flour
shorts
Mini-
mum
percent
of whole
30
9
46
8
8.5
22
40
70
13
72
12
Factor
3.3
11.3
2.2
12.0
11.8
4.5
2.5
1.4
7.7
1.4
8.3
Reference
p. 114, CRC Handbook of Processing and Utiliza-
tion in Agriculture
MRID No. 424482-03, Appendix B, p67
CBRS No. 10541, D. Miller, 1/29/93
CBRS No. 10541, D. Miller, 1/29/93
p. 426, Principles of Field Crop Production
p. 146, by difference, CRC Hand book of Process-
ing and Utilization in Agriculture
p. 146, CRC Hand book of Processing and Utiliza-
tion in Agriculture
p. 303, Commercial Vegetable Processing, 2nd.
Ed.
p. 2125, Considine
pp. 295-6, Cereal Crops
DD. 295-6. Cereal Croos
Table 4.—Maximum Observed (Experimental) Concentration Factors
Crop
apple pomace
sugar beet pulp, dry
suaarcane molasses
Maximum Concentration Factor 1
14x
20x
20x
1 These factors are based on a comparison of proposed and established food additive tolerances to the proposed
and established tolerances on raw agricultural commodities.
(5) The following is a bibliography for Tables 1 through 4.
Pesticide Analytical Manual, Volume I (PAM I), 1994, Food and Drug Adminis-
tration.
Agriculture Handbook No. 8, Composition of Foods: Raw, Processed, prepared,
U. S. Department of Agriculture, Agricultural Research Service, B. K. Watt,
and A. L. Merrill, December, 1963.
CRC Handbook of Processing and Utilization in Agriculture, Volume II, Part
2 Plant Products, I. A. Wolff, ed., CRC Press, Boca Raton, FL 1983.
Foods and Food Production Encyclopedia, D. M. Considine, and G. D.
Considine, eds., Van Nostrand Reinhold, New York, 1982.
Commercial Vegetable Processing, 2nd Edition, ed. B. S. Luk, and J. G.
Woodroof, Avi/Van Nostrand Reinhold, New York, 1988.
Peanuts: Production, Processing, Products, 2nd Edition, J. G. Woodroof, Avi
Publishing, Westport, CT, 1973.
Corn: Culture, Processing, Products, Ed. G. E. Inglett, Avi Publishing, Westport,
CT, 1970.
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Oats: Chemistry and Technology, ed. F. H. Webster, American Association of
Cereal Chemists, Inc., St. Paul, MN 1986.
Advances in Sugar Beet Production: Principles and Practices, eds., R. T. John-
son, et. al., Iowa State University Press, Ames, IA 1971.
Harris Guide.
Feeds & Nutrition—Complete, First Edition, Ensminger, M. E., and C. G.
Olentine, Jr., Ensminger Publishing Co., Clovis, CA 1978.
Cereal Crops, Leonard, W. H., and J. H. Martin, Macmillan Co., New York,
1963.
Principles of Field Crop Production. 3rd. Edition, Martin, J. H., W. H. Leonard,
and D. L. Stamp, Macmillan, New York, 1976.
(f) Determining the need for food/feed additive tolerances—(1)
RAC residue value, (i) The Agency will consider using some average
residue value from field trials if it can be determined that there is sufficient
mixing during processing such that variation among individual samples
from a field will be substantially evened out. It has been stated that "*
* * * the most relevant 'average' residue value from crop field trials is
the highest average residue value from the series of individual field trials
* * * *." This value is sometimes referred to as the HAFT (highest aver-
age field trial). Other average values (e.g. average of all field trials) may
be considered if the circumstances involved in processing of the crop war-
rant. Such an example would be where processing is likely to involve
blending of crop from across a regional or national market.
(ii) As a result of this policy, it is necessary to determine the HAFT
for each RAC for which a processing study has shown concentration of
residues. For each field trial reflecting the maximum residue use (i.e. maxi-
mum number and rate of application, minimum preharvest interval) and
considered acceptable for determining the section 408 of FFDCA tolerance
(i.e. values discarded for reasons such as contamination should not be in-
cluded), residue values for all samples at that site reflecting that use should
be averaged. (NOTE: If residues were corrected for low method recoveries
or for losses during storage in order to determine the tolerance, the cor-
rected values should also be used in this exercise.) The highest such aver-
age value is the HAFT and is to be used to calculate the maximum ex-
pected residue in processed commodities. For field trials in which only
one sample per site reflects the maximum residue use no averaging can
be done and the highest individual residue value becomes the HAFT.
(2) Multiple processing studies, (i) Whenever more than one proc-
essing study has been conducted for a particular pesticide on a given RAC,
the average concentration factor should be used for each processed com-
modity when determining the need for section 409 tolerances (or section
701 MRLs under paragraph (c)(6) of this guideline). Similarly, if multiple
samples or subsamples are analyzed within a processing study, the average
residue value should be used for each commodity as opposed to using
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the lowest value from the RAC samples and the highest value for the
processed fraction samples, which would result in the highest concentra-
tion factors. When averaging concentration factors across studies, factors
which exceed the theoretical maximum should be lowered to the latter
for averaging purposes. In no instance should a section 409 tolerance (or
section 701 MRL) be based on a concentration factor greater than the theo-
retical maximum. If only one processing study has been conducted and
the theoretical concentration factor has been exceeded, the section 409 or
section 701 residue level should be based on the factor (if available) listed
in Tables 1 through 4 of this guideline.
(ii) As stated in paragraph (c)(2) of this guideline, processing studies
should reflect actual commercial practices. If several studies are available
and a step (e.g. washing) that is routinely used in the processing of that
RAC is omitted, it may be inappropriate to include that study in the cal-
culation of the average concentration factor.
(3) Use of exaggerated rate studies, (i) The Agency encourages use
of field trials with exaggerated application rates in cases where residues
near or below the analytical method's LOQ are expected in the RAC from
the maximum registered rate (lx). For purposes of this discussion, pes-
ticide uses can be divided into those which result in quantifiable residues
in the RAC and those which do not. The former would have section 408
tolerances set above the LOQ, while the latter would usually have toler-
ances set at the LOQ. In either case, if possible, processing studies should
use RAC samples which contain quantifiable residues.
(ii) For uses which result in quantifiable residues in the RAC from
the registered application rate, exaggerated rate applications are not needed
to generate RAC samples for processing if all field trials lead to residues
well above the LOQ. However, if residues below or near the LOQ are
observed in some field trials, it is advisable for an exaggerated application
rate to be used to generate RAC samples for the processing study. Regard-
less of whether exaggerated application rates are used, if a section 408
tolerance is based on the presence of quantifiable residues and concentra-
tion of residues is observed in a processed commodity, that concentration
factor will be used in conjunction with the HAFT or other applicable aver-
age value and other relevant factors (e.g. variability of the analytical meth-
od) to determine the need for a section 409 tolerance (or section 701
MRL). In other words, the concentration factor will not be adjusted for
the use of exaggerated rates in cases where quantifiable residues are ob-
served in the RAC from the registered use.
(iii) In those cases where all RAC samples from the field trials show
residues below the LOQ and the residue data cover all significant growing
regions for the crop as delineated in OPPTS 860.1500, it may be possible
to waive the processing study and conclude that section 409 tolerances
(or section 701 MRLs) are not needed based on the results of field trials
8
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conducted at exaggerated application rates. With the exception of mint
and citrus, if exaggerated rate data are available and these field trials result
in no quantifiable residues in the RAC, no processing study and section
409 tolerances are required provided that the rate was exaggerated by at
least the highest theoretical concentration factor among all the processed
commodities derived from that crop or 5x, whichever is less. Processing
studies will be needed for citrus and mint in virtually all cases due to
the extremely high potential concentration factors for citrus oil (l,000x)
and mint oil (33Ox).
(iv) If no quantifiable residues are found in the RAC from the maxi-
mum registered rate, but the exaggerated rate does produce quantifiable
residues, the latter samples should be processed and residues measured
in the appropriate commodities. Any residues still above the LOQ in the
processed commodities should be adjusted for the degree of exaggeration.
These adjusted residues should then be compared to the LOQ for the RAC.
If the adjusted residues are greater than or equal to twice the LOQ, a
section 409 tolerance (or section 701 MRL) is needed. Due to the varia-
bility associated with an analytical method near its LOQ, a food additive
tolerance (or section 701 MRL) will not normally be established for resi-
dues less than twice the LOQ. For example, consider a field corn RAC
tolerance set at 0.05 ppm (LOQ) and residues of 0.08 ppm being found
in the RAC and 0.30 ppm in the oil following a 5x application rate. Ad-
justing for the 5x rate, oil residues would be 0.06 ppm, which is less
than twice the LOQ. Therefore, a section 409 tolerance is not necessary.
However, if the oil residues were 1.0 ppm, a section 409 tolerance (or
perhaps section 701 MRL) at 0.20 ppm (1.0 ppm/5) would be necessary.
(v) One additional scenario needs to be discussed regarding use of
exaggerated rates. In some cases no quantifiable residues may be found
in the RAC, but the exaggerated rate is less than the maximum theoretical
concentration factor (or 5x, whichever is less) due to phytotoxicity limita-
tions. In these instances a decision will be made case-by-case as to the
need for a processing study. If a processing study is deemed necessary,
any quantifiable residues in processed fractions would be adjusted for the
degree of exaggeration as explained in the previous paragraph. Some of
the factors to consider when determining if the processing study is needed
include how close the degree of exaggeration comes to the theoretical fac-
tor (or 5x, whichever is less) and whether detectable residues (i.e. greater
than limit of detection but less than LOQ) are found in any RAC samples.
Another consideration would be whether the pesticide is likely to be
present on a specific portion of the RAC based on when it is applied
and/or its ability to translocate. For example, a pesticide applied late in
the growing season would be more likely to be on the surface of a fruit
and have greater potential to concentrate in pomace than one applied only
at the bloom stage or earlier.
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(4) Impact of Ready-to-Eat (RTE). (i) The classification of a proc-
essed food as RTE or not RTE will determine whether or not the possibil-
ity of setting a section 701 MRL needs to be explored as discussed under
paragraph (f)(5) of this guideline. Until recently, the Agency has consid-
ered any food available for sale as being ready-to-eat. The Agency now
holds that RTE food has a common sense meaning of food which is
consumed without further preparation and will apply this interpretation in
future actions. Therefore, food should now be considered "ready-to-eat"
if it consumed "as-is" or is added to other RTE foods (e.g. condiments).
(ii) The Agency also realizes that application of this definition of RTE
may be difficult in many instances. The following processed foods are
examples of not-ready-to-eat: mint oil, citrus oil, guar gum, and dried tea.
Examples of clearly RTE foods are raisins, olives, and potato chips. Vege-
table oils are an example of foods not so easily characterized under this
RTE standard. The Agency is presently analyzing information on food
consumption and mixing of livestock feeds in order to classify processed
commodities with respect to RTE. As such decisions are made, they will
be made available to the public.
(5) Determining the need for section 409 tolerances or section 701
MRL's. (i) The Agency will establish food/feed additive tolerances
(FATs) under section 409 of the FFDCA for processed foods or feeds
that are classified as RTE if residues in those processed commodities are
likely to exceed the corresponding section 408 tolerances. Therefore, for
an RTE food such as raisins, the concentration factor (taking into account
multiple processing studies and exaggerated rates, if applicable) should
be multiplied by the HAFT (or other applicable average value) and that
value compared to the RAC tolerance. If that number is appreciably higher
than the section 408 tolerance, a food/feed additive (section 409) tolerance
will be needed. The judgment as to "appreciably higher" will need to
take into account how close the residue level is to the LOQ of the analyt-
ical method. If residues in the processed food are less than twice the LOQ,
a section 409 tolerance is normally not needed. On the other hand, when
residues in the processed food (i.e. concentration factor times HAFT) are
significantly above the LOQ, a section 409 tolerance will normally be
needed if those residues are approximately 1.5x the section 408 tolerance
(or higher). For situations in which the processed food/feed residues are
close to that level (e.g. 1.3 to 1.7x those in the RAC), all relevant informa-
tion including variability in recovery data will be considered by the Agen-
cy when assessing the need for food/feed additive tolerances.
(ii) The procedure is more complex for processed foods or feeds that
are not RTE (nRTE). If residues in an nRTE processed food exceed the
section 408 tolerance, residues in the RTE forms of those foods/feeds will
need to be determined and then compared to the section 408 tolerance.
If the residues in the RTE (i.e. mixed/diluted) form do not exceed the
RAC tolerance, the Agency will establish an MRL on the nRTE processed
10
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commodity under section 701 of the FFDCA. On the other hand, if resi-
dues in the RTE (mixed/diluted) form still appreciably exceed those in
the RAC, a food/feed additive tolerance will be established for the NRTE
processed commodity under section 409 of the FFDCA.
(iii) In order to determine whether residues in the RTE (mixed/di-
luted) forms of nRTE processed foods/feeds exceed those in the RAC,
the Agency will develop dilution factors. These will be based on the least
amount of dilution that may occur for the nRTE food. For example, flour,
assuming it is classified as nRTE, is likely to have a relatively low dilution
factor based on its use in preparation of commodities such as crackers,
bagels, and tortillas. Dried tea, on the other hand, is likely to have a large
dilution factor based on the relative weight of water used to brew tea.
At this time there is no list of dilution factors. As these factors are derived,
the Agency will announce them to the public periodically.
(iv) The procedure for assessing nRTE processed commodities is as
follows. The concentration factor (accounting for multiple processing stud-
ies and exaggerated rates, if necessary) is multiplied by the HAFT (or
other applicable average value) to determine residues in the nRTE proc-
essed food. If the residue in the nRTE food does not appreciably exceed
the section 408 tolerance, neither a section 409 tolerance nor section 701
MRL is needed. If the residue in the nRTE processed food does appre-
ciably exceed the RAC tolerance, that residue should be divided by the
dilution factor to determine the residue level in the RTE form. If the resi-
due in the RTE (mixed/diluted) food is basically equal to or less than
the section 408 tolerance, a section 701 MRL is needed for the nRTE
processed commodity. If the residue in the RTE (mixed/diluted) food still
appreciably exceeds the section 408 tolerance, a section 409 (i.e. food or
feed additive) tolerance is needed for the nRTE processed commodity.
(v) This procedure can be illustrated by some examples using mint
and the nRTE food mint oil. The assumption is made that for three dif-
ferent pesticides that the HAFT value is 8.0 ppm and that the RAC toler-
ance is 10 ppm. The assumption is also made that the dilution factor for
mint oil is 160 for its use in preparation of RTE foods. Pesticide A is
observed to concentrate 1.3x in mint oil. The concentration factor times
the HAFT is equal to 10.4 ppm, which is not appreciably higher than
the RAC tolerance of 10 ppm. Neither a section 409 tolerance nor section
701 MRL is needed for the mint oil. Pesticide B is found to concentrate
40x in mint oil. The concentration factor (40) times the HAFT (8.0 ppm)
is qual to 320 ppm, well above the RAC tolerance of 10 ppm. The residues
in the RTE (mixed/diluted) food are then calculated to be 2 ppm by divid-
ing the mint oil residue of 320 ppm by the dilution factor of 160. The
2 ppm residue in the RTE food is below the 10 ppm RAC tolerance. There-
fore, a section 701 MRL of 320 ppm should be established for the nRTE
mint oil. Pesticide C is found to concentrate 320x in mint oil. The con-
centration factor (320) times the HAFT (8.0 ppm) is 2,560 ppm, which
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is well above the RAC tolerance of 10 ppm. The residues in the RTE
food are then calculated to be 16 ppm by dividing the mint oil residue
of 2,560 ppm by the dilution factor of 160. The 16 ppm in the RTE
(mixed/diluted) food appreciably exceeds the 10 ppm RAC tolerance.
Therefore, a section 409 or food additive tolerance is needed for mint oil
at 2,560 ppm (or more likely at 2,500 ppm considering significant figures).
(g) Data report format. The following describes a suggested format
for a study report, item by item. However, other formats are also accept-
able, provided that the information described this paragraph is included.
(1) Title/cover page. Title page and additional documentation require-
ments (i.e. requirements for data submission and procedures for claims
of confidentiality of data if relevant to the study report) should precede
the content of the study. These requirements are described in PR Notice
86-5 (see paragraph (h)(5) of this guideline).
(2) Table of contents.
(3) Summary/introduction.
(4) Materials—(i) Test substance. (A) Identification of the pesticide
formulated product used in the field trial from which the RAC used in
the processing study was derived, including the active ingredient therein,
or if fortified RAC samples were used in the processing study, identity
of the fortifying substances.
(B) Identification and amount of residues in experimentally treated
RAC samples at the time the processing study is initiated.
(C) Any and all additional information petitioners consider appro-
priate and relevant to provide a complete and thorough description and
identification of the test substances used in the processing study.
(ii) Test commodity. (A) Identification of the RACs (crop/type/vari-
ety) and the specific crop parts used in the processing study.
(B) Sample identification (source of samples, field trial identification
number; control or weathered residue sample, coding and labeling informa-
tion (should be the same as or cross-referenced to the sample coding/label-
ing assigned at harvest)).
(C) Treatment histories (pesticides used, rates, number of applica-
tions, preharvest intervals (PHIs), etc.) of the RAC samples used in the
processing study.
(D) The developmental stages, general condition (immature/mature,
green/ripe, fresh/dry, etc.) and sizes of the RAC samples used in the proc-
essing study.
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(E) Any and all additional information the petitioner considers appro-
priate and relevant to provide a complete and thorough description of the
RACs used in the processing study.
(5) Methods—(i) Experimental design. For example:
(A) Number of test/control samples.
(B) Number of replicates.
(C) Residue levels in the RACs to be used.
(D) Representativeness of test commodities to the matrices of con-
cern, etc.
(ii) Test procedures—(A) Fortification (spiking) procedure, if used
(detail the manner in which the test compounds were introduced to the
RACs).
(B) A description of the processing procedure used and how closely
it simulates commercial practice. Quantities of starting RAC and of result-
ing processed commodities.
(C) A description of the methods of residue analysis (see OPPTS
860.1340, Residue analytical method).
(D) A description of the means of validating the methods of residue
analysis (see OPPTS 860.1340).
(E) A description of any storage stability validation studies that may
have been performed (see OPPTS 860.1380, Storage stability data).
(6) Results/discussion—(i) Residue results. (A) Raw data and correc-
tion factors applied, if any.
(B) Recovery levels.
(C) Storage stability levels, if applicable.
(D) Direct comparison of residues in the RAC with those in each
processed product or processing fraction derived from that sample, etc.
(ii) Statistical treatments. Describe tests applied to the raw data.
(iii) Quality control. Include if not covered elsewhere. Describe con-
trol measures/precautions followed to ensure the fidelity of the processing
study.
(iv) Other. Constituting any and all additional information the peti-
tioner considers appropriate and relevant to provide a complete and thor-
ough description of the processing study or studies.
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(7) Conclusions. Discuss conclusions that may be drawn concerning
the concentration/reduction of the test compounds in the test matrices as
a function of the standard commercial processing procedure, and the need
for food/feed additive tolerances or section 701 MRLs.
(8) Certification. Certification of authenticity by the Study Director
(including signature, typed name, title, affiliation, address, telephone num-
ber, date).
(9) Tables/figures, (i) Tables of raw data from the processing study,
method recovery data, storage stability recovery data (if applicable); etc.
(ii) Graphs, figures, flowcharts, etc. (as relevant—include the process-
ing procedure with weights of RAC and processed fractions).
(10) Appendixes, (i) Representative chromatograms, spectra, etc. (as
applicable).
(ii) Reprints of methods and other studies (unless physically located
elsewhere in the overall data submission, in which case cross-referencing
will suffice) which will support the registrant's conclusions.
(iii) Other, comprising any relevant material not fitting in any of the
other portions of this report.
(h) References. The following references should be consulted for ad-
ditional background material on this test guideline.
(1) Environmental Protection Agency, Pesticide Reregistration Rejec-
tion Rate Analysis—Residue Chemistry; Follow-up Guidance for: Generat-
ing Storage Stability Data; Submission of Raw Data; Maximum Theoreti-
cal Concentration Factors; Flowchart Diagrams. EPA Report No. 737-R-
93-001, February, 1993.
(2) Environmental Protection Agency, Pesticide Reregistration Rejec-
tion Rate Analysis - Residue Chemistry; Follow-up Guidance for: Updated
Livestock Feeds Tables; Aspirated Grain Fractions (Grain Dust); A Toler-
ance Perspective; Calculating Livestock Dietary Exposure; Number and
Location of Domestic Crop Field Trials. EPA Report No. 737-K-94-001,
June, 1994.
(3) Environmental Protection Agency, Pesticide Reregistration Rejec-
tion Rate Analysis—Residue Chemistry; EPA Report No. 738-R-92-001,
June, 1992.
(4) Environmental Protection Agency, FIFRA Accelerated Reregistra-
tion—Phase 3 Technical Guidance. EPA Report No. 540/09-90-078.
(Available from National Technical Information Service, Springfield, VA).
(5) Environmental Protection Agency, Pesticide Registration Notice
PR 86-5, Standard Format for Data Submitted under the FIFRA and Cer-
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tain Provisions of the Federal Food, Drug, and Cosmetic Act (FFDCA),
May 3,1986.
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