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for residues for which no tolerance has been established for lettuce (chlorpyrifos-3,
chlorothalonil-1), and 1 for residues exceeding the tolerance level (endosulfan).

Oranges

Out of 569 samples analyzed, 329 (57.8 percent) were found to contain at least 1 detectable
residue. Eleven different pesticides were detected. Thiabendazole and imazalil, both post-
harvest fungicides, were the most frequently detected. The total number of residues found
was 482. This total includes multiple residues found in single samples, which ranged from 3
samples containing 4 different residues to 118 containing 2 residues. No tolerance violations

were reported.
Peaches

Out of 360 samples analyzed, 307 (85.3 percent) were found to contain at least 1 detectable
residue. Twenty-two different pesticides were detected. Most frequently found were
iprodione, dicloran, captan, and phosmet. The total number of residues found was 677.
This total includes multiple residues detected in single samples, which ranged from 1 sample
containing 7 different residues to 105 samples containing 2 residues. Violations were
reported for 6 domestic samples, all for residues for which no tolerance has been established
for peaches (acephate-2, dimethoate-1, methamidophos-2, thiabendazole-1).

Potatoes

Out of 568 samples analyzed, 404 (71.1 percent) had at least 1 detectable residue. Sixteen
different pesticides were detected. Chlorpropham, a pre- and post-emergence herbicide also
used to inhibit potato sprouting, and thiabendazole were the most frequently detected. The
total number of residues found was 530. This total includes multiple residues found which
ranged from 1 sample containing 4 different residues to 89 containing 2 residues. No
tolerance violations were reported.

4.2 Post-Harvest Fungicides

Benomyl

This fungicide, which has pre- and post-harvest use in fruits and vegetables, was added to
PDP’s testing profile in May 1992. All benomy] analyses were performed at USDA’s
Animal and Plant Health Inspection Service (APHIS) laboratory in Gulfport, Mississippi.
Benomyi was determined as carbendazim (a benomy! degradation product) using reverse-
phase high performance liquid chromatography. A total of 1,327 samples were analyzed for
benomyl. Commodities tested were apples (406 samples), bananas (406), broccoli (139), and
green beans (376). Benomyl residues were detected in 49 of the apple samples tested, 3 of
the bananas, and 34 of the green beans. Residues found were in concentrations ranging from
50 ppb to 0.89 ppm. No tolerance violations were reported. Broccoli samples tested for
benomyl did not have detectable residues of this compound.

28


United States Agricultural P.O. Box 96456

Department of Marketing Washington, DC
Agriculture Service 20090-6456
April 1994
To the Reader:

The Pesticide Data Program (PDP) was implemented in May 1991 by the Agricultural
Marketing Service of the United States Department of Agriculture to collect comprehensive
data on pesticide residues in selected fresh fruits and vegetables. PDP was designed to
provide government agencies with an improved data base to respond more effectively to food
safety issues. The main recipient of the program’s data is the Environmental Protection
Agency, which uses this information to support its risk assessment process.

PDP is funded by Congress and operated through agreements with participating States, which
have the responsibility for sample collection and analysis. Through the end of 1992, there
were six participating States: California, Florida, Michigan, New York, Texas, and
Washington.

PDP operations were expanded in January 1993 to include three new participating States.
The addition of these States--Colorado, North Carolina, and Ohio--increased the segment of
the Nation’s population represented by PDP sampling to approximately 50 percent and
provided for greater regional diversity.

If you have any questions or comments regarding this summary, please contact William J.
Franks, Jr., Director, or Robert L. Epstein, Deputy Director, of the Science Division at
(202) 720-5231.

Sincerely,

Rm Hota

LON HATAMIYA
Administrator

The Agricultural Marketing Service

@ is an agency of the
ECD! / united States Department of Agriculture


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APPENDIX 5
DISTRIBUTION OF RESIDUES DETECTED BY COMMODITY

NUMBER.OF ” NUMBER OF “PERCENT OF
(COMMODITY/PESTICIDE: | SAMPLES. SAMPLES WITH. |. SAMPLES WITH
: ANALYZED" {| RESIDUES DETECTED: RESIDUES DETECTED)
POTATOES
2,4-D 216 6 28
Azinphos—Methyl 568 1 0.2
Chlorpropham 568 337 59.3
DDE 568 56 9.9
DDT 568 8 B 1.4
Diazinon 568 1 0.2
Dicloran 568 5 0.9
Dimethoate 568 1 0.2
Endosulfans 568 45 79
Methamidophos 568 6 1
Methidathion 568 1 02
Methoxychlor 568 2 0.4
Pentachlorobenzene 465 5 1.4
Phorate Sulfone (NY only) 99 3 3.0
Quintozene 568 3 0.5
Thiabendazole* 363 50 13.8
Total Residues Detected: $30

Total number of samples analyzed: 568

Total number of samples with positive findings: 404
Percent of samples with residues detected: 71.1
Number of different pesticides detected: 16

GRAND TOTALS

SAMPLES ce
“NUMBER WITH | PERCENT WITH
ESIDUES DETECTED, RESIDUES DETECTED

"NUMBER OF DIFFERENT | NUMBER

PESTICIDES DETECTED ANALYZED **, ***
is ~49 5592. 3423 612
= + 158 (benomyl & thiabendazole results only) = 5750

{V) Residue was found where no tolerance was established by EPA. Page 7 of 7

(X) Residue was found which exceeds EPA tolerance.

* Implementation of Thiabendazole analysis was delayed in California.

** Number shown as total excludes August samples for which only Benomyl analysis was performed.
*** Some samples were discarded due to poor condition upon arrival at one of the testing facilities.


came from Chile; and (4) the majority of celery, green beans, grapefruit, and oranges
originated from either California or Florida. Figure 2.0 shows the percentage of imported
versus domestic samples per commodity. Figure 2.1 gives the geographic origin of domestic

samples.

Appendix 3 gives the number of samples collected each month by commodity, and the
breakdown of number and percentage of imported versus domestic. As Appendix 3
indicates, 1,114 (19.4 percent) of the samples were imported, and 4,636 (80.6 percent) were
domestic. Celery, green beans, and peaches were not included in the program until
February; therefore, their sample totals are lower. The same applies to broccoli and carrots,
which were added to the program in October. Additionally, a great degree of seasonal
variability was noted in the number of import versus domestic samples for both grapes and

peaches.

13


APPENDIX 5
DISTRIBUTION OF RESIDUES DETECTED BY COMMODITY

= NUMBER OE
"SAMPLES WITH

oe RESIDUES DETECTED |

BROCCOLI
Chiorothalonil 153 2 1.3
Chlorpyrifos 153, 8 5.2
DCPA 153 36 23.5
DDE 153 1 07
Endosulfans 153 10 e 65
Methamidophos 153 4 26
Permethrins 153 2 1.3

Total Residues Detected: 63

Total number of samples analyzed: 153

‘Total number of samples with positive findings: 54

Percent of samples with residues detected: 35.3

Number of different pesticides detected: 7

CARROTS
DDE 153 41 26.8
Diazinon 153 19 12.4
Dimethoate (V-1) 153 1 O7
Endosulfans 153 4 26
Iprodione 153 44 28.8
Parathion 153 3 2.0
Parathion—Methyl 153 2 1.3
TDE 153 1 07
Thiabendazole 153 1 07
Trifluralin (CA only) 42 29 69.0

Total Residues Detected: 145

Total number of samples analyzed: 153

Total number of samples with positive findings: 88
Percent of samples with residues detected: 57.5
Number of different pesticides detected: 10

Page 2 of 7


TABLE 4.1 CONCENTRATION DETECTED vs. ESTABLISHED TOLERANCES
(Pesticides detected in less than ten percent of the samples are not included)

Commodity/ Tolerance Percentage of Mean of Percent of
Pesticide (ppm) Samples with Residues Found Tolerance
Detected Residues (ppm)
POTATOES
Chlorpropham 50 59.3 1.44 2.9
DDE* 1 9.9 0.012 1.2
Thiabendazole 10 13.8 0.61

AL Action Levels (ALs) are established by FDA and are not considered to be the same as
Tolerances. Although there is no registered use for DDT in the U.S., ALs were established for
DDT and its metabolites due to their persistence in the environment.
NT Under 40CFR 180.315 there is no tolerance for methamidophos in green beans. However,
40CEFR 180.108 specifies that for a mixture of acephate and its metabolite methamidophos there
is a tolerance of 3 ppm of which not more than 1 ppm can be methamidophos, only if acephate

is present.

37


518 samples tested
194 detections (37.5%)

fein SO pe oS pe Bananas/Thiabendazole

100

3.8 8

3

Number of Occurrences
8

10-25B 26-50B “51-99 B . 0.10-0.5M 0,51-1.0M
Concentration

153 camples tested
36 detections (23.5%)

min 2 ppb max 34 ppb Broccoli/DCPA

30 = — aH

Number of Occurrences

19B 10-25B _ 26-50 B
ppb - parte per billion Concentration
ppm - parte per million
min - minimum concentration detected
max - Maximum concentration detected 46


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Commodity/Pesticide Pair

Lettuce/Endosulfans
Lettuce/Permethrins
Oranges/Imazalil
Oranges/Thiabendazole
Peaches/Azinphos-Methyl
Peaches/Captan
Peaches/Dicloran
Peaches/Iprodione
Peaches/Parathion-Methyl
Peaches/Phosmet
Potatoes/Chiorpropham
Potatoes/DDE*”
Potatoes/Thiabendazole

Tolerance (ppm)
2.0

20.0

10

10

2.0

50

20

20.0

10
50

10

Page No.
56
57
57
58
58
59
59

60
61
61
62
62

Action Levels (ALs) are established by FDA and are not considered to be the same as
Tolerances. Although there is no registered use for DDT in the U.S., ALs were
established for DDT and its metabolites due to their persistence in the environment.
Under 40CFR 180.315 there is no tolerance for methamidophos in green beans.

However, 40 CFR 180.108 specifies that for a mixture of acephate and its metabolite

methamidophos there is a tolerance of 3 ppm of which not more than 1 ppm can be

methamidophos, only if acephate is present.

42


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589 samples tested Grapefruit/Thiabendazole

210 detections (54.0%)
min 10 ppb - max 1.6 ppm

Number of Occurrences
8 8 8 $ 8 38s g

Ss

°

10258  2650B  51-99B 0.1005M O.SI-10M 119.9M
Concentration

‘552 samples tested

184 detections (27.9%) G rapes/Captan

min 5 ppb - max 3.4 ppm.

7

Number of Occurrences
3

pb = bill 19B 10-25 B 26-50B 51-99B — 0.10-0.5M 0.51-10M 1.1-9.9M
ppb - parts per billion .

ppm - parte per million Concentration

min - minimum concentration detected
max - maximum concentration detected

52


DISTRIBUTION OF RESIDUES DETECTED BY PESTICIDE

APPENDIX 7

[ pee ie SUMMARY OF RESULTS =
& : STATES WHERE "(SAMPLES WITH RESIDUES DETECTED
_ COMMODITIES . SAMPLES WERE NUMBER | Wee Minimum. ' Maximum
ne és ae USAMPLES a “Value | Value:
C. OTHER PESTICIDES
ANILAZINE
CELERY _[CA, WA I 46] 70] 21.7 |.83M [22M
Total # of samples with residues detected = 10
CAPTAN
APPLES CA, FL, MI, NY, TX, WA. 567 45 7.9|10B 19M
GREEN BEANS CA 466 1 0.2258 25B
GRAPES CA, FL, MI, NY, TX, WA 552 154 27.9|5B 3.4M
PEACHES CA, FL, MI, NY, TX, WA 360 51 14.2|5B 2.2M
Total # of samples with residues detected = 251
CARBARYL
APPLES FL, WA 567 3 0.5 [80B 27M
GREEN BEANS NY 466 2 0.4|.29M 69M.
GRAPES CA 552 1 0.2|.13M 13M.
PEACHES FL, NY 360 3 0.8 [33B 2.3M
Total # of samples with residues detected = 9
CHLORPROPHAM
APPLES NY 567 1 0.2|28B 288
POTATOES CA, FL, MI, NY, TX, WA 568 337 §9.3/13B 9.6M
Total # of samples with residues detected = 338
CYPERMETHRIN
LETTUCE [MI, TX 565 | 2] 0.4].18M [34M
Total # of samples with residues detected = 2
DCPA
BROCCOLI CA, FL, MI, TX, WA 153 36 23.5 2B 34B
CELERY CA, FL, TX, WA 508 WW 2.2|5B 41B
GREEN BEANS CA, FL, TX, WA 466 24 5.2|2B 13M
LETTUCE CA, MI, TX, WA. 565 25 4.4[2B 12M
Total # of samples with residues detected = 96
DDE * (Degradation product of DDT)
APPLES FL 567 4 0.2|21B 21B
BROCCOLI FL 153 i) 0.748 4B
CELERY CA, FL, MI, NY, TX 508 28 5.5/4B 31B
CARROTS CA, FL, MI, NY, TX, WA 153 41 26.8 | 2B 13M
GREEN BEANS CA, TX, WA 466 10 2.1128 13B
LETTUCE CA, Mi, NY, WA. 565 12 2.1/2B 17B
POTATOES CA, FL, MI, NY, TX, WA 568 56 9.9|2B 53B
Total # of samples with residues detected = 149

Page 5 of 8



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EXECUTIVE SUMMARY

In May 1991, the U.S. Department of Agriculture (USDA) implemented the Pesticide Data
Program (PDP) to collect comprehensive data on pesticide residues in selected fresh fruits
and vegetables. PDP is a multi-agency program with planning, policy, and procedural
efforts coordinated among USDA, the Environmental Protection Agency (EPA), and the
Food and Drug Administration (FDA). Day-to-day program operations are managed by the
Science Division of USDA’s Agricultural Marketing Service (AMS). Data produced by PDP
is collected as close to the consumer as possible, with samples prepared as if for human
consumption (washed, peeled, cored, etc.). PDP data is available to EPA to determine
dietary exposure to pesticide residues, and thus better estimate risk to the consumer.
Commodities were chosen for inclusion in the program based on their level of consumption
by the American public. Pesticides targeted for data collection were selected by EPA in
consultation with USDA and were chosen based on dietary exposure considerations. The
EPA list of pesticides consists of compounds with acute and chronic endpoints, including
suspected carcinogens. PDP data is also available for use by EPA to address pesticide
reregistration and special review needs. An overview of program management and
operations is shown in Figure A. Pesticides in PDP are shown in Figure B.

Agreements were established with agencies in six States (California, Florida, Michigan, New
York, Texas, and Washington) to collect and analyze PDP samples. These States were
selected because they represent diverse geographic areas of the country, approximately 40
percent of the Nation’s population, and a large percentage of the fresh fruits and vegetables
grown in the United States. Participating States were assigned a number of samples to
collect per commodity each month, which was based on the State’s population. This number
was the same for all commodities and remained constant throughout the year. To allow for
collection as close to the consumer level as possible, samples were gathered at sites such as
terminal markets and large distribution centers. Sampling at these locations also provided
information on the origin of the sample, the use of post-harvest fungicides, and pesticide
degradation that occurred during transit and storage.

Sampling guidelines, written by AMS and provided to all participating States, required that
sampling dates and sites be selected at random. Also included in the guidelines were specific
sampling techniques to be utilized by the sample collectors. Strict adherence to the
guidelines and uniformity of sampling techniques were emphasized. Participating States were
responsible for providing AMS with quarterly sampling plans indicating the dates and sites to
be sampled for each month of the quarter. Quality assurance/quality control (QA/QC)
criteria, which are based on EPA’s Good Laboratory Practices (GLPs), were established by
AMS for the participating laboratories. To facilitate meeting these criteria, each laboratory
was provided with similar instrumentation and training on instrument use.

Presented in this summary are the PDP findings for calendar year 1992. The number of
commodities included in the program increased from 7 to 10 in February, and once again

vii


84 dotectone (92.35) Celery/Chlorothalonil

min 2 ppb - max 5.9 ppm

60

30

Number of Occurrences

10 |-

19B 10-25B 26-50 B 51-99B | 0.10-0.5M 0.51-1.0M  1.1-9.9M
Concentration

508 samples tested
67 detections (13.2%)
min 5 ppb - max 0.27 ppm

Celery/Diazinon

25
20
$
E 15
Ge
3
3 10
a
5
0
ppb - parte per billion Led 10.258 26-508 51-99 B 0.10-0.5 M
ppm - parte per million 4 4 Concentration
pm - part 7 ot
max - maximum concentration detected 49


APPENDIX 5

DISTRIBUTION OF RESIDUES DETECTED BY COMMODITY

ae 2 ES ‘NUMBER OF = [°° NUMBEROF PERCENT OF
* COMMODITY/PESIICIDE - SAMPLES SAMPLES WITH ~ SAMPLES WITH .
i : ANALYZED RESIDUES DETECTED} RESIDUES DETECTED

APPLES
Azinphos—Methyl 567 178 31.4
Benomyl 406 49 12.1
Captan 567 45 79
Carbaryl 567 3 0.5
Chlorothalonil (V-1) 567 1 02
Chlorpropham (V-1) 567 1 0.2
Chlorpyrifos 567 400 17.6
DDE 567 1 o2
Diazinon 567 14 25
Dicofol 567 9 1.6
Dimethoate 567 29 51
Diphenylamine 567 173 30.5
Endosulfans 567 75 13.2
Ethion 567 19 3.4
Iprodione (V-1) 567 1 02
Methoxychlor 567 3 05
Myclobutanil 567 1 0.2
O-Phenylphenol (CA only) 154 7 45
Omethoate 567 17 3.0
Parathion 567 WW 19
Parathion—Methyl 567 46 8.41
Phosalone 567 2 0.4
Phosmet 567 7 3.0
Thiabendazole* 519 293 56.5
Vinctozolin (V-1) 567 1 0.2

Total Residues Detected: 1096

Total number of samples analyzed: 567 ** + 51 (benomyl/thiabendazole results only)=618

Total number of samples with positive findings: 502

Percent of samples with residues detected: 88.5

Number of different pesticides detected: 25

BANANAS
Benomyl 406 3 07
Ethoprop (NY only) 99 1 1.0
Imazalil K~-1) 564 23 41
Thiabendazole (X—4)* 518 194 37.5

Total Residues Detected: 221

Total number of samples analyzed: 564 ** + 51 (benomyl/thiabendazole results only) =615.

Total number of samples with po:

sitive findings: 209

Percent of samples with residues detected: 37.1
Number of different pesticides detected: 4

Page 1 of 7



APPENDIX 6 PESTICIDES DETECTED BY PDP AND THEIR CHEMICAL ACTIONS

—==
PESTICIDE CHEMICAL ACTIONS
| Permethrins Insecticide, repellent
o-Phenylphenol Fungicide, Used for Post-Harvest Applications
Phorate Sulfone Insecticide/Acaricide
Cholinesterase Inhibitor
Phosalone Insecticide/Acaricide
Cholinesterase Inhibitor
Phosmet Insecticide/Acaricide
Cholinesterase Inhibitor
Propargite Acaricide, residual killing action

Quintozene (PCNB)

Soil Fungicide, seed dressing agent

TDE

Degradation Product of DDT
Also known as DDD

Thiabendazole

Pre- and Post-Harvest Fungicide

Trifluralin

Selective Pre-emergence Herbicide

Vinclozolin

Fungicide, contact action

Page 3 of 3


Pesticide Data Program (PDP)
Summary of 1992 Data

U.S. Department of Agriculture ¢ Agricultural Marketing Service


LIST OF FIGURES, TABLES, AND APPENDICES

FIGURES/TABLES

Figure A.
Figure B.
Figure 1.0
Table 1.0
Table 2.0
Figure 2.0
Figure 2.1
Table 4.0
Table 4.1
Table 4.2

Figure 4.0

Overview of PDP Management and Operations

Pesticides in PDP

Participating States and Their Geographical Distribution Areas

Frequency of Occurrence of EPA-Targeted Pesticides in PDP Commodities
Samples Collected Per Commodity by Each Participating State

Commodity Distribution Percentages (Imported vs. Domestic)

Origin of Domestic Samples

Summary of Residue Detections Per Commodity

Concentration Detected vs. Established Tolerances

Distribution of Pesticide Residue Concentrations by Commodity

Distribution of Residue Concentrations for Selected Commodities

APPENDICES

Appendix 1
Appendix 2
Appendix 3
Appendix 4

Appendix 5
Appendix 6
Appendix 7
Appendix 8

Appendix 9

Sampling Regions by State
Sample Profile by Origin (Domestic/Import)
Sampling Period and Distribution by Commodity

Average LODs and LOQs Reported by PDP Testing Facilities for Samples
Analyzed in 1992

Distribution of Residues Detected by Commodity
Pesticides Detected by PDP and Their Chemical Actions
Distribution of Residues Detected by Pesticide

Multiple Pesticide Residues Detected

Tolerance Violations Reported to FDA

Vv


TABLE 4.1 CONCENTRATION DETECTED vs. ESTABLISHED TOLERANCES
(Pesticides detected in less than ten percent of the samples are not included)

ee
Commodity/ Tolerance Percentage of Mean of Percent of
Pesticide (ppm) Samples with Residues Found Tolerance
Detected Residues (ppm)
APPLES
Azinphos-Methyl 2.0 31.4 0.083 4.2
Benomyl 7.0 12.1 0.11 1.6
Chlorpyrifos 15 17.6 0.043 2.9
Diphenylamine 10 30.5 0.67 6.7
Endosulfans 2.0 13.2 0.022 11
Thiabendazole 10 56.5 0.62 6.2
BANANAS
Thiabendazole 0.4 37.5 0.090 22.5
BROCCOLI
DCPA (acthal) 5 23.5 0.37 1A
CARROTS
DDE“ 3 26.8 0.018 0.60
Diazinon 0.75 12.4 0.010 1.3
= 5.0 28.8 0.083 17
CELERY
Acephate 10 26.8 0.12 1.2 |
Chlorothalonil 15 32.3 0.24 16 |
Diazinon 0.7 13.2 0.040 |
Dicloran 15 27.6 0.25 1.7 |
Methamidophos 1 114 0.024 24 |
Permethrins 20.0 38.6 0.087 0.44 |
GRAPEFRUIT
Imazalil 10 15.3 1.06 10.6
Thiabendazole 10 54.0 0.14 1.4

35


APPENDIX 7

DISTRIBUTION OF RESIDUES DETECTED BY PESTICIDE

SUMMARY: OF RESULTS: :
Z SAMPLES WITH RESIDUES DETECTED ce
NUMBER’ = % “Minimim “| Maximum
i Value | Value.
C. OTHER PESTICIDES
MYCLOBUTANIL
APPLES NY 567 1 0.2[25B 25B
GRAPES CA, FL, MI, NY, TX, WA 552 94 17.0[12B 53M
Total # of samples with residues detected = 95
O-PHENYLPHENOL
APPLES CA 154 ai 4.5/15B 12M.
GRAPEFRUIT CA 154 1 0.6 | 15B 15B
ORANGES CA 154 5 3.2/15B 58B
Total # of samples with residues detected = 13
OMETHOATE
APPLES FL, Ml, NY 567 17 3.0/8B 38M
CELERY NY 508 1 0,2| 228 228
GREEN BEANS FL, MI, NY 466 18 3.9|8B 49M.
GRAPES FL, MI, NY. 552 24 4.3/8B 52M
LETTUCE CA, Mi, NY 565 4 0.7 | 16B 88B
ORANGES NY 569 1 0.2|75B 758
Total # of samples with residues detected = 65
PARATHION
APPLES CA, NY. 567 1 1.9/5B 75B
CELERY NY 508 3 0.6 |3B 68B
CARROTS NY 153 3 2.0|3B 123
GREEN BEANS NY, TX 466 2 0.4/36B 11M
GRAPES CA, FL, MI, NY. 552 4 0.7 (27B 2.7M.
PEACHES FL, MI, NY. 360 1 3.1/6B 10M
Total # of samples with residues detected = 34
PHORATE SULFONE
POTATOES [NY | 99] 3] 3.0[13B [12M
Total # of samples with residues detected = 3
PHOSALONE
APPLES [FL NY I 567 | 2] 0.4[.43M [54M
Total # of samples with residues detected = 2
PHOSMET
APPLES CA, MI, NY, TX 567 17 3.0/11B 26M
GRAPEFRUIT TX 567 2 0.4 |40B 40B
GRAPES CA, MI, NY, TX 552 5 0.9 |58B 25M
PEACHES CA, FL, MI, NY, TX, WA. 360 51 14.2/15B 2.9M
Total # of samples with residues detected = 75

Page 7 of 8



APPENDIX 7

DISTRIBUTION OF RESIDUES DETECTED BY PESTICIDE

= < SUMMARY OF RESULTS © |
STATES WHERE. : “NUMBER | Ve CEED
SAMPLES WERE. (OF | NUMBE Minimam
COLLECTED Valuc. Value. |
A. EPA — TARGETED PESTICIDES
IPRODIONE
APPLES NY 567 4 0.2|25B 258
CELERY CA, NY, TX, WA 508 13 2.6|25B .29M
CARROTS CA, FL, MI, NY, TX, WA. 153 44 28.8|25B .35M
GREEN BEANS NY, TX 466 2 0.4|25B .88M.
GRAPES CA, FL, Mi, NY, TX, WA 552 161 29.2|14B 3.0M
LETTUCE CA, NY, WA 565 3 0.5|25B 1.2M
PEACHES CA, FL, Ml, NY, TX, WA 360 196 54.4] 14B 16M
Total # of samples with residues detected = 420
LINDANE
CELERY [CA, NY, WA’ I 508 | 3] 0.6[10B. [34M
Total # of samples with residues detected = 3
METHAMIDOPHOS
BROCCOLI TM 153 4 2.6|20B 10M
CELERY CA, FL, MI, NY, TX, WA 508 58 11.4/4B .27M
GREEN BEANS CA, FL, MI, NY, TX, WA 466 129 27.7|48 1.8M
GRAPES NY 552 1 0.2|8B 8B
[LETTUCE CA, Ml, NY, TX 565 15 2.7|4B 45B
PEACHES NY 360 2 0.6|4B 4B
POTATOES CA, TX 568 6 1.41/58 18B
Total # of samples with residues detected = 215
METHOXYCHLOR
APPLES CA, FL, NY 567 3 0.5|49B 58M
GRAPES CA, TX 552 3 0.5|25B 4.0M.
LETTUCE CA 565 5 0.9|25B 58B
PEACHES CA 360 3 0.8|22B 25B
POTATOES CA 568 2 0.4{25B 258
Total # of samples with residues detected = 16
PENTACHLOROBENZENE
POTATOES [CA, WA I 465] Al 1.1[5B [148
Total # of samples with residues detected = 5
PERMETHRINS:
BROCCOLI NY 153 2 1.3/8B 47B
CELERY CA, FL, MI, NY, TX, WA. 508 196 38.6|8B 59M
GREEN BEANS CA, MI 466 3 0.6|23B 85M
LETTUCE CA, FL, Mi, NY, TX, WA 565 62 11,0|5B 1.9M
PEACHES CA, FL, MI, NY 360 10 2.8/8B .24M
Total # of samples with residues detected = 273
QUINTOZENE
CELERY TX WA 508 3 0.6|5B 14B
GREEN BEANS CA, FL, Ml, TX, WA 466 7 15/58 8B
POTATOES CA, FL 568 3 0.5 /5B 19B

Total # of samples with residues detected =

13

Page 2 of 8



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min 15 ppb - max 2.9 ppm

25 —

Ss

Number of Occurrences
aR

0 3] &
10-25B 26-50B 51-99B . 0.10-0.5M 0.51-10M 1.1-9.9M
Concentration

337 datootone (89.3%) Potatoes/Chlorpropham

min 13 ppb - max 9.6 ppm
—

200

Number of Occurrences

19B B 0.10-0.5M 0.51-1.0M  1.1-9.9M

ppb - parts per billion

per million
min - minimum concentration detected
max - maximum concentration detected 61



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APPENDIX 5

DISTRIBUTION OF RESIDUES DETECTED BY COMMODITY

Se NUMBER OF NUMBER OF PERCENT OF ~
COMMODITY/PESTICIDE SAMPLES. | SAMPLES WITH SAMPLES WITH
Brena See: ANALYZED RESIDUES DETECTED! RESIDUES DETECTED

CELERY
Acephate 508 136 26.8
Anilazine (WA & CA only) 46 10 21.7
Azinphos— Methyl 508 2 0.4
Chiorothalonil 508 164 32.3
Chlorpyrifos (V-2) 508 2 0.4
DCPA (V-11) 508 ant 22
DDE 508 28 55
DDT 508 1 o2
Diazinon 508 67 13.2
Dicloran 508 140 27.6
Dimethoate 508 2 0.4
Endosulfans 508 9 1.8
Iprodione (V—2) 508 13 2.6
Lindane 508 3 06
Methamidophos 508 58 11.4
Mevinphos 508 2 0.4
Omethoate 508 1 02
Parathion 508 3 0.6
Parathion—Methyl 508 3 06
Permethrins 508 196 38.6
Quintozene (V—3) 508 3 0.6

Total Residues Detected: 854

Total number of samples analyzed: 508

Total number of samples with positive findings: 409

Percent of samples with residues detected: 80.5

Number of different pesticides detected: 21

GRAPEFRUIT
24-D 252 5 2.0
Chlorpyrifos 567 1 02
Diazinon 567 10 1.8
Dicofol 567 1 0.2
Ethion 567 15 26
Imazalil 567 87 15.3
O-Phenylphenol (CA only) 154 1 06
Phosmet 567 2 0.4
Thiabendazole* 389 210 54.0

Total Residues Detected: 332

Total number of samples analyzed: 567

Total number of samples with positive findings: 260
Percent of samples with residues detected: 45.9
Number of different pesticides detected: 9

Page 3 of 7



FS eae a
min 9 ppb - max 0.62 ppm Apples/Azinphos-Methyl

90

80

Number of Occurrences

° 1-9B 10-25B 26-50 B 51-99 B 0.10-0.5M 0.51-1.0M
Concentration
406 samples tested
49 detections (12.1%)
min 50 ppb - max 0.42 ppm Apples/Benomyl

30 —=

15 /-

10 |-

Number of Occurrences

‘ Ee
19B 10-25B 51-99 B 0.10-0.5 M
ppb - parts per billion CF
ppm - parts per million Concentration
min - minimum concentration detected 43

max - maximum concentration detected


486 sample tested Green Beans/Acephate

118 detections (25.3%)
min 5 ppb - max 3.3 ppm

50
3
3
i
°
%
H
E
Zz
1-9B 10-25B 26-50B 51-99B 0.100.5M 0.51-1.0M  1.1-9.9M
Concentration
466 samples tested
128 detections (27.0%) Green Beans/Endosulfans

50

Number of Occurrences

1-9B 26-50 B 51-99 B 0.10-0.5 M 0.51-1.0M
Concentration

ppb - parts per billion
ppm - parte per million
min - minimum concentration detected
max - maximum concentration detected

55


360 samples tested

Trin 14 ppb max 16 ppm Peaches/Iprodione

90

Number of Occurrences
$ 8

40
30
20
10
° 10-258 26-50B S199B 0,10-0.5M 0.51-10M 1.1-9.9M ; 10-99M
Concentration
360 samples tested.
in 4 ppb max 6-12
in = . rf

mt a Peaches/Parathion-Methyl

20 Ses

°

Number of Occurrences

7 1-98 10-25B 26-50B 51-99 B 0.10-0.5 M
ppb - parte per billion Concentration
ppm - parts per million

min - minimum concentration detected
max - maximum concentration detected

60


466 samples tested
129 detections (27.7%)
min 4 ppb - max 1.8 ppm

Green Beans/Methamidophos

60

Number of Occurrences

S1-99B | 0.100.5M 0.51-10M 1.1-9.9M

Concentration

10-25B 26-50 B

565 samples tested
63 detections (11.2%)
min 2 ppb - max 4.2 ppm.

Lettuce/Endosulfans

25

Py 8

3

Number of Occurrences

ppb - parts per billion
ppm - parts per million

inimum concentration
mine ninkpom eoneneceon

1-9B 1025B 26-50 B 51-99B 0.10-0.5M O.51-1.0M 1.1-9.9M
Concentration
Stettea

56



APPENDIX 5
DISTRIBUTION OF RESIDUES DETECTED BY COMMODITY

ee : e “NUMBER OF =i PERCENTOF.
(COMMODITY /PESTICIDE | | SAMPLES WITH =) SAMPLES WITH: -
Se 2s RESIDUES DETECTED) RESIDUES DETECTED:
PEACHES
Acephate (V-2) 360 2 0.6
Azinphos~ Methyl! 360 45 12.5
Captan 360 51 14.2
Carbaryl 360 3 08
Chlorpyrifos 360 31 8.6
DDT 360 1 0.3
Diazinon 360 27 7.5
Dichlorvos (CA only) 110 1 0.9
Dicloran 360 168 46.7
Dimethoate (V-1) 360 1 03
Endosulfans 360 20 5.6
Iprodione 360 196 54.4
Methamidophos (V-2) 360 2 0.6
Methoxychior 360 3 0.8
Mevinphos 360 3 0.8
Parathion 360 an 3.4
Parathion—Methy! 360 42 117
Permethrins 360 10 28
Phosmet 360 51 14.2
Propargite (FL only) 41 3 7.3
Thiabendazole (V—1)* 230 1 0.4
Vinclozolin 360 5 1.4
Total Residues Detected: 677,

Total number of samples analyzed: 360

Total number of samples with positive findin:

307,

Percent of samples with residues detected: 85.3
Number of different pesticides detected: 22

Page 6 of 7



DISTRIBUTION OF RESIDUES DETECTED BY PESTICIDE

APPENDIX 7

DDT

CELERY NY 508 1 0,2|10B 10B
LETTUCE NY 565 1 0.2/27B 27B
PEACHES NY 360 1 0.3[10B 10B
POTATOES CA, NY. 568 8 1.4/5B 38B

Total # of samples with residues detected = il

DEMETON

GREEN BEANS [NY I 89] 1] 1.4[87B [87B

Total # of samples with residues detected = 1

DEMETON—SULFONE

GREEN BEANS [NY [ 89] ai 22/118 [13B

Total # of samples with residues detected = 2

DIMETHOATE

APPLES CA, FL, Ml, NY, TX 567 29 5.1/10B 27M
CELERY NY, TX 508 2 0.4/14B 44B
CARROTS TMX 153 1 0.7 [708 10B
GREEN BEANS CA, FL, Ml, NY, TX 466 30 6.4|5B 1.2M
GRAPES CA, FL, MI, NY, TX, WA 552 55. 10.0/4B 1.5M.
LETTUCE CA, MI, NY, TX 565 44 78/48 21M
ORANGES FL, Mi, NY, TX 569 4 0.7 | 108 18B
PEACHES ML 360 1 0.3768 10B
POTATOES TM% 568 1 0.2/10B 10B

Total # of samples with residues detected = 167,

DIPHENYLAMINE

APPLES CA, FL, MI, NY, WA 567, 173 30.5 [13B 3.7M
GRAPES CA 552 1 0.2|15B 153

Total # of samples with residues detected = 174

ETHOPROP

BANANAS [NY 99] i 1.0[3B [3B

Total # of samples with residues detected = 1

IMAZALIL.

BANANAS CA, MI, NY, 1X 564 23 4.1|15B 24M
GRAPEFRUIT. CA, FL, MI, NY, TX 567 87 15.3 |15B 33M
ORANGES CA, FL, MI, NY, TX, WA 569 167 29.3 |10B 94M

‘Total # of samples with residues detected = a7

Page 6 of 8



508 samples tested Celery/Dicloran

140 detections (27.6%)
min 5 ppb - max 4.1 ppm

70 —

Number of Occurrences

19B 10-258 26-50 B 51-99B 0.10-0.5M 0,51-10M  1.1-9.9 M
Concentration

58 detectio
in 4 ppb - max O.:

08 gampln texted Celery/Methamidophos

Number of Occurrences

19B 10258 26-50 B 51-99B 0.10-0.5 M
centration

pain concentration detected 50


2.0

C ENTS

List of Figures, Tables, and Appendices

Executive Summary

INTRODUCTION

1,1 1992 Program Operations
1.2 1993 Preview

SAMPLING OVERVIEW

2.1 Sampling Procedures

2.2 — Statistics on Samples Collected
LABORATORY OVERVIEW
3.1 Quality Assurance Program
3.2 Sample Preparation

3.3. Sample Analysis

SAMPLE RESULTS

4.1 Discussion of Results

4.2 Post-Harvest Fungicides

4.3 Environmental Contaminants
4.4 Acid Herbicides

4.5 Multiple Residues Detected
4.6 Non-Detected Residues

4.7 Tolerance Violations

iti


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360 samples tested
51 detections (14.2%)
min 5 ppb - max 2.2 ppm

Peaches/Captan

20

a

Ss

Number of Occurrences

w

360 samples tested
168 detections (46.7%)
min 5 ppb - max 0.23 ppm.

10-25B 26-50 B 51-99 B . 0.10-0.5M 0.51-10M 1.1-9.9M
Concentration

Peaches/Dicloran

Number of Occurrences

ppb - parte per billion
ppm - parts per million

inimum concentration detected
max - maximum eoncentration detected

10-25B 26-50B 51-99B 0.10-0.5M 0.51-1.0M 1.1-9.9M 10-99M
Concentration

59


Dicloran

Dicloran, a fungicide with pre- and post-harvest use on fruits and vegetables, was analyzed
for in all 5,592 samples. Residues were found in 355 (6.3 percent) of the samples

tested, although most of the occurrences were in celery and peaches. Concentrations
detected ranged from 5 ppb to 4.1 ppm. None of the residues found exceeded the tolerance

level.

Diphenylamine

Analysis of this fungicide was performed in 4,762 samples and residues were found in 174
(3.7 percent) of the samples. Almost all residues were detected in apples, in concentrations
ranging from 13 ppb to 3.7 ppm. A violation was found in 1 grape sample for residues
where no tolerance was established.

Thiabendazole

Thiabendazole is a fungicide with registered uses on fruits and vegetables. Although this
compound is not an EPA-targeted pesticide, PDP added thiabendazole to its testing profile
because it was being detected frequently in the organonitrogen screen. A total of 4,812
samples were tested for this fungicide in 1992, with residues detected in 1,000 (20.8 percent)
of the samples. The rate of occurrence, however, was mainly localized to four commodities,
with residues detected in 293 of the apple samples tested, 194 of the bananas, 210 of the
grapefruit, and 250 of the oranges. Since most thiabendazole applications are done post-
harvest, these results appear to indicate that this compound penetrates the peelings of
bananas, grapefruit, and oranges because they were removed prior to analysis. Detected
residues ranged from a low of 4 ppb to a high of 4.8 ppm. Violative residues were found in
five samples, four of which were for residues exceeding the tolerance level, and one for
residues where no tolerance was established.

4.3 Environmental Contaminants

DDT, DDE, and TDE

A total of 5,592 samples were screened for DDT and its metabolites DDE and TDE. Use of
DDT has been prohibited in the United States since 1972. However, due to the persistence
of this chemical in the environment, residues of this insecticide, and/or its metabolites, were
found in apples, broccoli, celery, carrots, green beans, lettuce, peaches, and potatoes. DDT
residues were found in 11 samples, 8 of which were potatoes. DDT residues were detected
in concentrations ranging from 5 ppb to 38 ppb. DDE residues were found in 149 samples,
with most positives detected in potatoes (56 positives), carrots (41), and celery (28). DDE
residues were detected in concentrations ranging from 2 ppb to 0.13 ppm. TDE residues
were found in one carrot sample at 2 ppb.

29


SECTION 4.0 - SAMPLE RESULTS

All commodities were screened for selected organochlorine, organophosphate, and
organonitrogen compounds. The advanced analytical technology utilized by PDP laboratories
allows for the detection of residues present at very low concentrations. As a result, a
significant number of samples tested were found to contain residues--albeit, at low levels,

and substantially below tolerances.

Table 4.0 provides a summary of all residue detections per commodity. These results are
explained in further detail in Tables 4.1 and 4.2, and shown graphically in Figure 4.0.

Table 4.1 compares the mean residue concentration of selected pesticides to established
tolerances (pesticides detected in less than ten percent of the samples are not included). Of
the 40 pesticide/commodity pairs listed in Table 4.1, only 5 pairs resulted in a mean
concentration which exceeded 10 percent of the tolerance: thiabendazole/bananas,
imazalil/grapefruit, dimethoate/grapes, myclobutanil/grapes, and acephate/green beans. Five
pairs (DDE/carrots, permethrins/celery, captan/grapes, iprodione/grapes, and captan/peaches)
had mean concentrations below 1 percent of the established tolerance. Table 4.2 shows the
number of residues found in different concentration ranges, from 1-9 parts per billion (ppb)
to greater than 1 part per million (ppm). As seen in this table, approximately 56 percent of
the residues found in all commodities were below 0.1 ppm, and 8.5 percent of the detections
were below 10 ppb. Figure 4.0 shows in more detail the distribution of residues for
commodity-pesticide pairs with at least 10 percent detections.

4.1 Discussion of Results

As Appendix 5 shows, 5,592 samples were analyzed for all PDP compounds except benomyl
and 2,4-D which were tested only in selected commodities. Of these, 61.2 percent were
found to contain detectable residues. The percentage of samples with residues varied from
88.5 percent for apples to 35.3 percent for broccoli. The number of different pesticides
detected per commodity ranged from 4 in bananas to 25 in apples. Additional samples of
apples (51 samples), bananas (51), and'green beans (56) were collected for benomyl and
thiabendazole analyses only, bringing the total to 5,750. Benomyl and thiabendazole results,
including these additional samples, are discussed in section 4.2. Pesticides detected included
insecticides, herbicides, fungicides, and growth regulators (see Appendix 6), Also detected
were DDT and its metabolites, although their presence is due to environmental
contamination, not the result of crop application.

Appendix 7 gives the distribution of residue occurrences by pesticide. The appendix shows
all pesticides detected by PDP divided into three parts as follows: (A) EPA-targeted
pesticides; (B) additional EPA-targeted pesticides; and (C) other pesticides. The EPA-
targeted pesticides, listed in section A, are those included in the program from its inception
through May 1992. Pesticides in section B, although already monitored by PDP, were added
to EPA’s targeted pesticide list in November 1992. Section C lists other pesticides included
in the program. Listed below each pesticide are these commodities in which the pesticide
was detected and the States where the samples were collected. Appendix 7 also gives a

25


Figure 4.0 Index
Distribution of Residue Concentrations for Selected Commodities

Commodity/Pesticide Pair Tolerance (ppm) Page No.

Apples/Azinphos-Methyl 2.0 43
Apples/Benomyl 7.0 43
Apples/Chlorpyrifos 1.5 44
Apples/Diphenylamine 10 44
Apples/Endosulfans 2.0 45
Apples/Thiabendazole 10 45
Bananas/Thiabendazole 0.4 46
Broccoli/DCPA (Dacthal) 5 46
Carrots/DDE*” 3 47
Carrots/Diazinon 0.75 47
Carrots/Iprodione 5.0 48
Celery/Acephate 10 48
Celery/Chlorothalonil 15 49
Celery/Diazinon 0.7 49
Celery/Dicloran 15 50
Celery/Methamidophos 1 50
Celery/Permethrins 20.0 51
Grapefruit/Imazalil 10 51
Grapefruit/Thiabendazole 10 52
Grapes/Captan 50 52
Grapes/Dimethoate 1 53
Grapes/Iprodione 60.0 53
Grapes/Myclobutanil 1.0 54
Grapes/Vinclozolin 6.0 34
Green Beans/Acephate 3 55
Green Beans/Endosulfans 2.0 55

Green Beans/Methamidophos NT 56


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APPENDIX 5
DISTRIBUTION OF RESIDUES DETECTED BY COMMODITY

Be Ons ees NUMBER OF | NUMBER OF | PERCENT OF
| COMMODITY /PESTICIDE SAMPLES. : SAMPLES WITH | “SAMPLES WITH
ee Ee | UANALYZED | .| RESIDUES DETECTED! RESIDUES DETECTED
GRAPES:
Azinphos— Methyl 552 4 07
Captan 552 154 27.9
Carbaryl 552 1 02
Chlorpyrifos (X—1) 552 24 43
Diazinon 552 an) 2.0
Dicloran 552 35 6.3
Dicofol 552 23 42
Dimethoate (X-1) 552 55 10.0
Diphenylamine (V—-1) 552 1 0.2
Endosulfans 552 22 4.0
iprodione 552 161 29.2
Methamidophos (V—1) 552 1 0.2
Methoxychlor 552 3 05
Mevinphos 552 1 02
Myclobutanil 552 94 17.0
Omethoate 552 24 43
Parathion (X-1) 552 4 0.7
Parathion—Methyl 552 2 0.4
Phosmet 552 5 og
Thiabendazole* 388 1 03
Vinelozolin 552 130 23.6
Total Residues Detected: 756
Total number of samples analyzed: 552
Total number of samples with positive findings: 381
Percent of samples with residues detected: 69.0
Number of different pesticides detected: 21
GREEN BEANS.
Acephate (X—1) 466 118 25.3
Azinphos—Methy! 466 16 3.4
Benomyl 376 34 9.0
Captan 466 1 02
Carbaryl 466 2 0.4
Chlorothalonil 466 33 7
Chlorpyrifos 466 1 0.2
DCPA 466 24 5.2
DDE 466 10 24
Demeton (NY only) 89 1 14
Demeton-S (NY only) 89 2 22
Diazinon 466 4 0.9
Dicloran 466 5 Ww
Dimethoate 466 30 64
Endosulfans 466 126 27.0
Ethion 466 1 02
Iprodione 466 2 0.4
Methamidophos (V—~18) 466 129 27.7
Omethoate 466 18 3.9
Parathion 466 2 0.4
Parathion—Methyl 466 2 0.4
Permethrins (V-3) 466 3 0.6
Quintozene 466 7 15
Vinelozolin 466 5 11
Total Residues Detected: 576

Total number of samples analyzed: 466 **, *** + 56 (benomyl/thiabendazole results only) =522
Total number of samples with positive findings: 279
Percent of samples with residues detected: 59.9
Number of different pesticides detected: 24

Page 4 of 7



4.7 Tolerance Violations

Tolerances, which are the maximum amount of residue that is allowed in or on a food crop,
are established by EPA. A violation occurs when a residue is found which exceeds tolerance
levels, or when a residue is found for which there is no tolerance for that particular crop.
With the exception of meat, poultry, and egg products, for which USDA is responsible,
tolerances for all other foods are enforced by FDA. In order to take prompt corrective
action, samples collected under enforcement programs have to be analyzed within hours of
collection. Since PDP samples are not collected for this purpose, emphasis is placed on
searching for residues at the lowest detectable levels rather than on quick sample turnaround.
In fact, because of the complexity of the sample analysis requirements and the data review
process, it may take 1 month or longer to complete a sample set.

During 1992, 63 samples were found to contain 66 violative residues (double violations were
found in 3 of the samples), 15 of which were detected in imported commodities. As
Appendix 9 indicates, 53 samples found in violation had residues where no tolerance was
established by EPA for that pesticide/commodity pair, and 10 had residues which exceeded
the tolerance. Under the Memorandum of Understanding signed by USDA, EPA, and FDA,
the Pesticide Data Program is required to inform FDA of any violative residues found. PDP
data may assist FDA by pinpointing areas where closer surveillance may be required.

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APPENDIX 5

DISTRIBUTION OF RESIDUES DETECTED BY COMMODITY

Total number of samples analyzed: 569

Total number of samples with positive findings: 329
Percent of samples with residues detected: 57.8
Number of different pesticides detected: 11

Bee oo : “NUMBER OF NUMBER OF PERCENT OF
‘COMMODITY /PESTICIDE: oo SAMPLES: SAMPLES WITH = SAMPLES WITH.

LE: ce | 2 ANALYZED |" | RESIDUES DETECTED! RESIDUES DETECTED

LETTUCE
Acephate 565 36 6.4
Chiorothatonil (V-1) 565 1 0.2
Chlorpyrifos (V-3) 565 3 05
Cypermethrin 565 2 0.4
DCPA 565 25 44
DDE 565 12 24
DDT 565 1 0.2
Diazinon 565 10 1.8
Dicloran 565 2 0.4
Dimethoate 565 44 78
Disulfoton Sulfone (CA only) 184 3 1.9
Endosulfans (X—1) 565 63 11.2
Iprodione 565 3 0.5
Methamidophos 565 15 27
Methoxychlor 565 5 0.9
Mevinphos 565 5 0g
Omethoate 565 4 07
Parathion—Methyl 565 1 0.2
Permethrins 565 62 11.0

Total Residues Detected: 297

Total number of samples analyzed: 565

Total number of samples with positive findings: 201

Percent of samples with residues detected: 35.6

Number of different pesticides detected: 19

ORANGES:
2,4-D 215 2 09
Chlorpyrifos 569 18 3.2
Diazinon 569 3 0.5
Dicofol 569 2 0.4
Dimethoate 569 4 0.7
Ethion 569 14 25
Imazalil 569 167 29.3
Methidathion 569 16 28
O-Phenyiphenol (CA only) 154 5 3.2
Omethoate 569 1 0.2
Thiabendazole* 392 250 63.8

Total Residues Detected: 482

Page 5 of 7



APPENDIX 7

DISTRIBUTION OF RESIDUES DETECTED BY PESTICIDE

es cea : SUMMARY: OF RESULTS
ee "STATES WHERE | NUMBER SAMPLES: SAITH RESIDUES DETECTED
‘COMMODITIES | SAMPLES WERE : :
S Sf COLLECTED.
A. EPA — TARGETED PESTICIDES
2,4-D
GRAPEFRUIT. FL, MI, TX 252 5 2.0/10B 10B
ORANGES NY 215 2 0.9/10B 10B
POTATOES CA, FL, MI, NY, TX 216 6 28/358 70B
Total # of samples with residues detected = 13
ACEPHATE
CELERY CA, FL, MI, NY, TX, WA 508 136 26.8 [5B 1.7M
GREEN BEANS. CA, FL, MI, NY, TX, WA 466 118 25.3|5B 3.3M
LETTUCE CA, FL, MI, NY, TX 565 36 6.4/6B 7M
PEACHES NY 360 2 0.6 |6B 248
Total # of samples with residues detected = 292
BENOMYL
APPLES CA, FL, MI, NY, TX, WA 406 49 12.1 |50B 42M
BANANAS CA, FL, MI 406 3 0.7|50B 12M
GREEN BEANS CA, FL, MI, NY, TX, WA 376 34 9.0 |50B 89M
Total # of samples with residues detected = 86
CHLORPYRIFOS
APPLES CA, FL, Mi, NY, TX, WA 567 100 17.6 |4B 64M
BROCCOLI TX 153 8 §.2/10B 14M
CELERY FL, NY 508 2 0.4|5B 5B
GREEN BEANS WA 466 1 0.2/13B 13B
GRAPEFRUIT. TX 567 1 0.2/10B 10B
GRAPES CA, FL, MI, NY, TX, WA 552 24 4.3|5B 77M
LETTUCE NY, TX 565 3 0.5/10B 9B
ORANGES CA, MI, NY, TX, WA 569 18 3.2|5B 13B
PEACHES CA, FL, Mi, NY, TX WA 360 31 8.6/4B 66B
Total # of samples with residues detected = 188
DICLORAN
CELERY CA, FL, Mi, NY, TX, WA 508 140. 27.6|5B 4.1M
GREEN BEANS CA, FL, TX, WA 466 5 1.1 /5B 55M
GRAPES CA, FL, MI, NY, TX, WA. 552 35 6.3|8B 1.1M
LETTUCE CA, WA 565 2 0.4|5B 53B
PEACHES CA, FL, MI, NY, TX, WA’ 360 168 46.7 |5B .23M
POTATOES CA, FL, Mi, NY, WA 568 5 0.9/5B 20M
Total # of samples with residues detected = 355
DICOFOL
APPLES FL, Ml, NY, TX 567 9 1.6] 11B 19M
GRAPEFRUIT. NY 567 1 0.2/30B 30B
GRAPES CA, FL, MI, NY, TX, WA 552 23 4.2|8B 4.0M
ORANGES NY, TX 569 2 0.4/30B 36B
‘Total # of samples with residues detected = 35

Page 1 of 8



SECTION 1.0 - INTRODUCTION

The U.S. Department of Agriculture (USDA) implemented the Pesticide Data Program
(PDP) in May 1991 to collect data on pesticide residues in selected fresh fruits and
vegetables. Overall program planning and policy procedures are coordinated among USDA,
the Environmental Protection Agency (EPA), and the Food and Drug Administration (FDA).
PDP residue data, which is collected as close to the consumer as possible, is available to
EPA to determine dietary exposure to pesticide residues, and thus better estimate risk to the
consumer, PDP also assists EPA in addressing pesticide reregistration and special review
needs by providing residue data needed to complete these processes.

USDA’s Agricultural Marketing Service (AMS) was charged with the implementation and
day-to-day management of PDP activities with the cooperating state agencies. This includes
all residue sampling and testing procedures, development and maintenance of the automated
information management system, and reporting of residue data. AMS also consults with
EPA and FDA to determine data needs and program planning.

Additionally, three other USDA agencies participate in PDP operations: National
Agricultural Statistics Service (NASS), Economic Research Service (ERS), and Human
Nutrition Information Service (HNIS). NASS provides agricultural chemical usage data and
support of the PDP sampling protocol; ERS analyzes NASS and AMS data and assesses the
economic implications of alternative pest control; and, HNIS conducts surveys of food intake
to provide information for EPA’s risk assessment studies.

To implement the Pesticide Data Program, AMS established agreements with Departments of
Agriculture in six States: California, Florida, Michigan, New York, Texas, and
Washington. These States were selected because they represent diverse geographic areas of
the country, approximately 40 percent of the Nation’s population, and a large percentage of
the fresh fruits and vegetables grown in the United States. Participating States were assigned
a number of samples to collect per commodity each month, which was based on the State’s
population. This number was the same for all commodities and remained constant

throughout the year.

There are other States to which a significant amount of produce is distributed through the
participating States. They are: Alaska, Connecticut, Hawaii, Massachusetts, Nevada, New
Jersey, and Vermont. Although these States are not participating in the program, PDP data
will apply to a significant portion of their population as well. Figure 1.0 shows the location
of the participating States and their geographical distribution areas.

AMS works with EPA to develop the list of pesticides and commodities targeted for data
collection by PDP. Commodities chosen for inclusion in the program are among those most
prevalently consumed by the American public. The EPA list consists of pesticides whose
toxicity is under evaluation by this Agency (i.e., pesticides with acute and chronic endpoints
including suspected carcinogens). The list is revised periodically to address current EPA
data needs. Program operations were designed so these revisions in the testing profile can be


APPENDIX 6 PESTICIDES DETECTED BY PDP AND THEIR CHEMICAL ACTIONS

PESTICIDE CHEMICAL ACTIONS
Dimethoate Insecticide/Acaricide
Cholinesterase Inhibitor
Diphenylamine Pre- and Post-Harvest Fungicide
Disulfoton Sulfone Insecticide/Acaricide
Cholinesterase Inhibitor
(Oxidized to Sulfone in plants)
Endosulfans Insecticide/Acaricide, contact action
Ethion Insecticide/Acaricide, contact action
Cholinesterase Inhibitor
Ethoprop Nematocide/Insecticide (soil insecticide)
Imazalil Post-Harvest Fungicide
Tprodione Fungicide
Lindane Herbicide, Gamma isomer of BHC
Malathion Insecticide, Cholinesterase Inhibitor
Methamidophos Insecticide/Acaricide
Cholinesterase Inhibitor
|| Methidathion Fungicide, contact action
Methoxychlor Insecticide/Acaricide
food storage control spray
Mevinphos Insecticide/Acaricide
Cholinesterase Inhibitor
Myclobutanil Fungicide
Omethoate Insecticide/Acaricide
Cholinesterase Inhibitor
Parathion Insecticide/Acaricide
Cholinesterase Inhibitor
Parathion-Methyl Insecticide/Acaricide
Cholinesterase Inhibitor

Page 2 of 3


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APPENDIX 14

SAMPLING REGIONS BY STATE

Ss OS “NUMBER PERCENT NUMBER PERCENT
= REGION «.. OF SITES. SITES OE SAMPLES: = -SAMPLES |
CALIFORNIA
AVENAL 1 0.4 5 0.3
BAKERSFIELD 3 1 18 W
BYRON 1 0.4 0 0.0
CHICO 1 0.4 5 03
COLTON 1 0.4 3 0.2
DELANO 1 0.4 0 0.0
EAST BAY (OAKLAND) 31 10.9 293 18.7
FAIRFIELD 2 0.7 3 0.2
FRESNO 10 35 57 3.6
LAKE TAHOE 1 0.4 3 0.2
LOS ANGELES BASIN 119 419 632 40.3
MADERA 1 0.4 9 0.6
MERCED 1 04 1 0.7
MONTEREY BAY AREA 4 14 12 08
OXNARD AREA 2 07 0 0.0
REDDING 2 0.7 8 05
SACRAMENTO. 28 9.9 92 5.9
SAN DIEGO AREA an 39 23 15
SAN JOSE 1 0.4 13 08
SAN LUIS OBISPO AREA 2 07 6 0.4
STOCKTON AREA 6 24 20 13
UKIAH 1 0.4 2 0.1
VISALIA 1 0.4 4 03
WEST BAY (SAN FRAN) 52 18.3 347 22.4
YUBA CITY AREA 1 0.4 2 0.1
TOTAL 284 100.0). A568 100:0%
FLORIDA
GREEN COVE SPRINGS 1 4.2 38 44
JACKSONVILLE 5 20.8 226 26.0
LAKELAND 1 42 51 5.9
MIAMI 3 12.5 43 5.0
ORLANDO 2 8.3 a1 10.5
PLANT CITY 2 8.3 45 5.2
POMPANO BEACH 5 20.8 181 20.9
TAMPA/ST. PETERSBURG 5 20.8 193 22.2
TOTALS 2 24 100.0 B68). 100.0%:
MICHIGAN
ANN ARBOR AREA 4 8.3 59 75
BATTLE CREEK 1 24 20 25
BAY CITY AREA 1 24 17 2.2
BRIGHTON 1 24 25 3.2
CADILLAC 1 24 29 37
DECATUR 1 21 21 27
DETROIT AREA 18 37.5 275 34.9
FLINT 2 4.2 21 27
GRAND RAPIDS 7 14.6 130 16.5
KALAMAZOO 1 24 14 18
LANSING 6 12.5 98 12.4
NILES 1 21 25 3.2
SAGINAW 1 241 35 44
STANDISH 1 241 19 24
TRAVERSE CITY 2 4.2 0 0.0
TOTAL: 48 100.0 ABB 100:0:

Page 1 of 2



3d.

sejdwes onsewog jo ulbO

2 eunB1y

19


552 samples tested
94 detections (17.0%)
min 12 ppb - mex 0.53 ppm

Grapes/Myclobutanil

8

8

Number of Occurrences

5

552 samples tested
130 detections (23.6%)
min 3 ppb - max 2.3 ppm

26-50 B 51-99B 0.10-0.5 M 0.51-1.0M
Concentration

Grapes/Vinclozolin

Number of Occurrences

ppb - parte per billion
ppm rts per million
i um concentration detected
imum concentration detected

10-25B 26-50B

54


392 samples tested
250 detections (63.8%)
min 6 ppb - max 1.6 ppm

Oranges/Thiabendazole

200

3 3

Number of Occurrences

$

360 samples tested
45 detections (12.5%)
min 4 ppb - max 0.74 ppm

Concentration

Peaches/Azinphos-Methyl

2

Number of Occurrences

ppb - parts per billion

ppm - parts per million
min - minimum concentration d
max - maximum concentration

0.10-0.5 M.

0.51-1.0M

198 10-25B 26-50 B 51-99B

Concentration

cted

letected 58



APPENDIX 6 PESTICIDES DETECTED BY PDP AND THEIR CHEMICAL ACTIONS

| PESTICIDE CHEMICAL ACTIONS

Mixture of Demeton-O isomer and Demeton-S isomer

2,4-D Pre- and Post-Harvest Herbicide
Acephate Insecticide, weak Cholinesterase Inhibitor
(the metabolite is Methamidophos) -
Anilazine Fungicide, leaf action
Azinphos-Methyl Insecticide, Cholinesterase Inhibitor
| Benomyl Pre- and Post-Harvest Fungicide
Captan Protectant Pre- and Post-Harvest Fungicide
Carbaryl Insecticide, weak Cholinesterase Inhibitor
Chlorothalonil Fungicide, leaf action
Chloropropham Herbicide/Growth Regulator
Pre- and Post-Emergence
Chlorpyrifos Insecticide, Cholinesterase Inhibitor
| Cypermethrin Insecticide
(cis/trans isomers 1:1 curative action)
DDE Degradation Product of DDT
DDT Insecticide
(All uses canceled, degrades to DDE and TDE)
Dacthal (DCPA) Herbicide
Demeton Systemic Insecticide/Acaricide

Demeton-S Sulfone

Metabolite of Demeton-S

Diazinon

Insecticide, Cholinesterase Inhibitor

Dichlorvos (DDVP)

Insecticide/Acaricide
Post-Harvest Fumigant and Penetrant Action

Dicloran

Pre-Harvest Fungicide

Dicofol

Acaricide
(the metabolite is dichlorobenzophenone) |

Page 1 of 3


SECTION 2.0 - SAMPLING OVERVIEW

PDP’s sampling protocol was designed to be objective and random. This was accomplished
by requiring that: (1) the number of samples collected each month be proportional to State
population; (2) sampling dates and sites be selected at random; and (3) no predetermination
be made regarding product variety or origin. The procedures used for sample collection also
effectively removed the impact of many sources of systemic bias. As a result, PDP data
generated during 1992 should produce reasonably good estimates of the prevalence of
pesticide residues in the food supply. Nevertheless, because PDP data will ultimately be
used to make national inferences for dietary risk assessment, AMS enlisted the services of
USDA’s National Agricultural Statistics Service (NASS) to increase the statistical
defensibility of PDP’s sampling protocol.

To accomplish this objective, NASS introduced a "site weighting" method by which the
probability of a site being selected is proportional to the volume of produce it distributes.
Implemented in January 1993, this method will allow users of PDP data to make virtually
unbiased estimates of the prevalence of pesticide residues in commodities collected in the
nine participating States. In addition, this procedure makes it possible to quantify the
accuracy of these estimates for both the nine States and the Nation as a whole. NASS will
continue to provide long-term maintenance for PDP’s sampling and estimation systems.

PDP samples were collected by the six participating States at sites such as terminal markets
and large distribution centers. These sites were chosen for sample collection because they
are the last stopover before produce reaches retailers (and subsequently consumers), and
because grower and packer information is still available at these locations. Data collected
closer to the time of consumption provides a better picture of exposure to pesticide residues.
This is because residues measured at these sites take into account pesticide degradation that
occurs during transit and storage, as well as residues resulting from the application of post-

harvest fungicides. ’

The volume of produce distributed by the State sampling sites varies greatly depending on
their geographic location and the area they serve. In the larger States, such as Texas, as
many as 161,500 tons of produce may be distributed by one site in a given year. Each
participating State was responsible for researching and compiling its list of appropriate
sampling sites, which varied in number from 18 in Washington to 284 in California.

As discussed in the Introduction (section 1.0), the States were assigned a number of samples
to collect per commodity each month, based on population. This number was the same for
all commodities and remained constant throughout the year. Sample assignments were as
follows: California-14, Florida-8, Michigan-7, New York-9, Texas-9, and Washington-5S.

Representatives of each participating State were trained in PDP sampling procedures, and

were responsible for training the sample collectors in their respective States. Uniformity of
sampling technique and strict adherence to PDP sampling procedures were emphasized.

di!


58 dotoctione (2.9%) Potatoes/DDE

min 2 ppb - max 53 ppb

30

Number of Occurrences

1-9B 10-25B 26-50 B 51-99 B
Concentration
min 4 ppb. mex 2.7 ppm Potatoes/Thiabendazole
30
ot

Number of Occurrences
a

19B 1025 B 26-50B 51-99B _ 0.100.5M 0.51-10M 1.19.9M
Concentration

ppb - parts per billion
ppm - parts per million

tie ~ minimum concentration detected
> maximum concentration detected 62


from 10 to 12 in October. The number of participating States remained at six throughout all
of 1992. However, agreements were established with three additional States (Colorado,
North Carolina, and Ohio) in August to begin sample collection in January 1993.

The addition of these three States increased the segment of the Nation’s population
represented by PDP sampling to approximately 50 percent and provided a greater degree of
regional diversity. The number of testing facilities, located in the participating States,
remained at eight through April. A USDA regional laboratory, needed to perform selective
multiresidue analyses, became PDP’s ninth testing facility in May.

During 1992, a total of 5,750 samples were collected, of which 158 were analyzed for
benomyl and thiabendazole only. The remaining 5,592 were analyzed for all other PDP
compounds with the exception of 2,4-D and benomyl, which were tested only in selected
commodities. Residues of 49 different pesticides were detected in approximately 60 percent
of all the samples. Many samples contained multiple residues, with as many as eight found
in one sample.

The number of samples collected by each State was as follows: California-1,568, Florida-
868, Michigan-788, New York-1,018, Texas-988, and Washington-520. These produce
samples originated from the 6 participating States, 31 other States, and 16 foreign countries.

Although, in general, the levels of pesticide residues detected were substantially below
tolerances, violative residues were detected in 63 of the samples, 15 of which were in
imported commodities. Of the 63 violative samples, 10 exceeded the tolerance level and the
other 53 had residues where no tolerance was established. AMS and the States notified FDA
of these violations. These data may assist FDA by pinpointing areas where closer
surveillance may be required.

The data collection protocols and advanced analytical technology utilized by PDP have
resulted in a significant number of residue detections, albeit at very low levels, in some
commodities. For example, at least one detectable residue was found in 88.5 percent of the
apples tested, 80.5 percent of the celery, in 85.3 percent of the peaches, and in 71.1 percent
of the potatoes. More than 55 percent of all residues found were below 0.10 parts per
million (100 ppb), with 8.5 percent of the detections less than 0.01 parts per million (10
ppb). These data should provide a strong basis for EPA to determine the dietary exposure to
pesticide residues.

PDP’s sampling protocol was enhanced in January 1993 by the implementation of a more
statistically defensible method of site weighting that reflected both an improved site selection
routine and the incorporation of commodity volume data from sampling sites. This method
will allow users of PDP data to not only make virtually unbiased estimates of the prevalence
of pesticides for commodities collected in the nine participating States, but also to quantify
the accuracy of those estimates both for the nine States and the Nation as a whole. The
enhanced sampling protocol was developed with the support of the USDA National
Agricultural Statistics Service, who will continue to provide long-term maintenance for
PDP’s sampling and estimation systems.

viii


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4.4 Acid Herbicides

2,4-D and Bromoxynil

Analyses for these herbicides were conducted at the APHIS and New York laboratories. The
method used involved a gel permeation chromatography cleanup step followed by a
methylation step. A total of 1,108 samples were tested for 2,4-D and 1,041 were tested for
bromoxynil. Commodities tested were apples, grapefruit, grapes, oranges, and potatoes.
Residues of 2,4-D were detected in five of the grapefruit samples, two of the oranges, and
six of the potatoes. Concentrations reported for 2,4-D ranged from 10 ppb to 70 ppb. No
bromoxynil residues were detected. No violative residues were found in any of the
commodities tested.

4.5 Multiple Residues Detected

PDP’s capability to detect residue concentrations much lower than tolerance levels has
resulted in the detection of multiple residues in individual samples, These multiple residues
may have resulted from the application of different pesticides to the crop during a growing
season, from spray drift, or from environmental contamination. In some instances, pesticides
which have similar chemical action (e.g., cholinesterase inhibitors) have been detected in
individual samples. Such is the case for one sample which contained residues of captan,
endosulfans, omethoate, dimethoate, diphenylamine, thiabendazole, azinphos-methyl, and
vinclozolin. Of these, omethoate, dimethoate, and azinphos-methyl are cholinesterase
inhibitors.

Appendix 8 summarizes the information on commodities containing multiple residues.
Column A shows, in descending order, the number of residues that were detected in a single
sample. Columns B and C give the number and percentage of samples found to contain the
number of residues listed in Column A. Column D lists the three most frequently detected
pesticides. In parentheses next to each pesticide is the number of residue findings for that
pesticide. For example, row 2 under celery shows that 14 samples, representing 2.8 percent
of the samples analyzed, contained 5 different residues each. In this case, the 3 most
frequently detected pesticides were: acephate with 13 positives, permethrins with 11, and
dicloran with 10.

4.6 Non-Detected Residues

Of the 16 EPA-targeted pesticides, atrazine, bromoxynil, and HCB were not detected in any
of the 5,592 samples. It should be noted, however, that atrazine and HCB have no
registered uses for any of the PDP commodities. Bromoxynil testing, which was performed
in selected commodities, is discussed in section 4.2 above. Results for the EPA-targeted
pesticides are summarized in Table 1.0.

30


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4. Process Control Spike: A compound of physical and chemical characteristics
similar to those of the pesticides being tested is used to evaluate the analytical process
on a sample-by-sample basis. Each of the analytical set components, except for the
reagent and matrix blanks, is spiked with process controls.

5. Storage Spikes: Ifa sample set is going to be frozen as a homogenate for more
than 72 hours prior to analysis, analysts are required to prepare storage spikes.
Storage spikes provide information on whether degradation has occurred while the
sample was frozen, and are prepared in the same manner as matrix spikes. However,
they do not replace the requirement to run a fresh matrix spike at the time of analysis.

e Method Performance and Confirmation - Laboratories are required to determine the
limits of detection (LOD) and limits of quantitation (LOQ) for each
commodity/pesticide pair. Confirmation by mass spectrometry, or a suitable alternate
detection system, is required for all initial findings. If a finding is violative, the
sample is reanalyzed in duplicate from the frozen homogenate, along with the
appropriate blanks and a spike of the violative residue at the suspected level.

e Standard Operating Procedures (SOPs) - Standard Operating Procedures were
developed to provide uniform administrative, sampling, and laboratory procedures.

After submission, all data generated by the laboratories are reviewed for completeness
and adherence to PDP requirements.

e On-Site Reviews - On-site reviews were performed to determine compliance with
SOPs. Improvements in sampling and laboratory procedures were made as a result of
the on-site reviews.

3.2 Sample Preparation

Upon arrival at the testing facility, samples were visually examined for acceptability-and
discarded if determined to be inedible (decayed, extensively bruised). Accepted samples
were then prepared emulating the practices of the average consumer, to more closely
represent actual exposure to residues. For example, where applicable, commodities were
washed, peeled, cored, etc., as if for human consumption.

Samples were homogenized using choppers and/or blenders and separated into analytical
portions (aliquots) for analysis. If testing could not be performed immediately, the entire
analytical set (sample set plus all quality control samples) was frozen at -40° C, or lower,
according to PDP’s QA/QC requirements. Surplus aliquots, not used for the initial testing,
were retained frozen in the event that replication of analysis or verification testing was
needed.

22


109 detection (17-6%) Apples/Chlorpyrifos

min 4 ppb - max 0.64 ppm

i ——

Number of Occurrences

26-50 B 51-99 B 0.10-0.5M 0.51-1.0M
Concentration

Apples/Diphenylamine

min 13 ppb - max 3.7 ppm

60 ratanstinatie Faas aa eae ee a

Number of Occurrences

19B

ppb - parte per billion
ppm - parts per million

min - minimurn concentration detected
max ~fmaxmum coneentrason ‘detected 44



APPENDIX 1
SAMPLING REGIONS BY STATE

oe NUMBER PERCENT: (= NUMBER =
REGION OF SITES SITES © OF SAMPLES:
NEW YORK
ALBANY 13 6.9 123 124
ALBION 1 05 0 0.0
BUFFALO 28 14.8 142 13.9
BYRON 1 05 0 0.0
CANASTOTA 3 16 3 0.3
CASTILE 1 Os 0 0.0
CHITTENANGO 2 1 0 0.0
HORSEHEADS 4 05 12 12
ITHACA 1 05 13 13
JAMESTOWN 4 241 32 31
LOCKPORT/BATAVIA 1 05 1 0.4
LONG ISLAND 13 69 66 65
MARION 2 11 1 0.4
NEW YORK CITY 80 42.3 395 38.8
NORWICH 1 05 14 14
ONTARIO 1 05 0 0.0
OSWEGO 3 1.6 0 0.0
PLATTSBURG AREA 1 05 0 0.0
ROCHESTER 9 48 78 77
SCHOHARIE 1 05 1 0.1
SOUTHEAST NEW YORK 13 69 54 53
SYRACUSE 8 4.2 73 7.2
WILLSBORO. 1 0.5 10 1.0
TOTALS = = 189, = 100.00 OI 700.0:
TEXAS
AMARILLO 1 34 37 37
BRENHAM 1 34 42 43
DALLAS/FORT WORTH 8 25.0 289 29.3
EL PASO 1 3.1 44 45
HOUSTON 8 25.0 290 29.4
LUBBOCK 2 63 61 6.2
LUFKIN 3 9.4 37 37
SAN ANTONIO 7 21.9 153 15.5
TYLER 1 3.1 35 35
TOTAL” 72 an) oe ©9000
WASHINGTON
SEATTLE/TACOMA 14 778 414 79.6
SPOKANE 3 16.7 65 125
YAKIMA 1 5.6 44 79
TOTAL ee Tae ry ee ea
TOTAL: a 595 ae 850

Page 2 of2



summary of results which shows total number of samples, the number and percent of
positives in those samples, and minimum and maximum detected concentration values.

These are reported in either parts per billion (B) for concentrations between 1-99 B or parts
per million (M) for higher concentrations. The following is an overview of findings for each
commodity.

Apples

Out of 567 samples analyzed, 502 (88.5 percent) were found to contain detectable residues of
at least 1 pesticide. Twenty five different pesticides were detected, with thiabendazole,
azinphos-methyl, and diphenylamine found most frequently. The total number of

residues found was 1,096. This total includes multiple residues detected in single samples,
which, as seen in Appendix 8, ranged from 1 sample containing 8 residues to 161 samples
containing 2 residues. Violations were reported for four domestic samples containing
residues of chlorothalonil, chlorpropham, iprodione, and vinclozolin, for which no tolerance
has been established for apples.

Bananas

Out of 564 samples analyzed, 209 (37.1 percent) had residues of at least 1 pesticide. Four
different pesticides were found. Of these, thiabendazole, a post-harvest fungicide, was the
most frequently found (194 samples). The total number of residues, including multiple
residues, was 221. Violations were reported for 5 samples, (imazalil-1, thiabendazole-4), all
of which were for residues exceeding the tolerance.

Broccoli

Of 153 samples analyzed, 54 (35.3 percent) had at least 1 detectable residue. Seven different
pesticides were found. DCPA (dacthal) was detected in 36 samples and was the most
frequently found pesticide. The total number of residues found, including multiple residues,
was 63. No violations were reported.

Carrots

Of 153 samples analyzed, 88 (57.5 percent) had at least 1 detectable residue. Ten different
pesticides were detected. Iprodione, DDE, and diazinon were the residues found most
frequently (trifluralin, detected in 69 percent of the samples tested, was analyzed in 42 of the
samples only). The total number of residues found, including multiple residues, was 145. A
violation was reported for one sample containing residues of dimethoate, for which there is
no tolerance established for carrots.

Celery
Of 508 samples analyzed, 409 (80.5 percent) had at least 1 detectable residue. Twenty-one

different pesticides were found. Permethrins, chlorothalonil, dicloran, and acephate were the
most frequently detected (anilazine, detected in 21.7 percent of the samples tested, was

26


APPENDIX 7

DISTRIBUTION OF RESIDUES DETECTED BY PESTICIDE

eee re SUMMARY OF RESULIS
CATES WHERE NUMBER ‘SAMPLES WITH RESIDUES DETECTED
OF | NUMBER % ‘Minimum Mada
COLLECTED. ea SAMPLES: s 2 Value oj Malue |
C. OTHER PESTICIDES
PROPARGITE
PEACHES [FL [ ai] 3] 73 ].74M [3M
Total # of samples with residues detected = 3
TDE * (Degradation product of DDT)
CARROTS [FL [ 153] 1] 0.7 [2B ae}
Total # of samples with residues detected = 1
THIABENDAZOLE
APPLES CA, FL, MI, NY, TX, WA 519 293 56.5|15B 4.8M.
BANANAS CA, FL, MI, NY, TX, WA 518 194 37.5 |10B 1,5M
CARROTS MI 153. 1 0.7 |12B 128
GRAPEFRUIT CA, FL, MI, NY, TX, WA 389 210 54.0|10B 1,6M
GRAPES FL 388 1 0.3 |.22M 22M
ORANGES CA, FL, Mi, NY, TX, WA 392 250 63.8 |6B 1.6M.
PEACHES Mi 230 1 0.4/95B. 95B
POTATOES CA, FL, MI, NY, TX, WA 363 50 13.8 [4B 2.7M.
Total # of samples with residues detected = 1000
TRIFLURALIN
CARROTS ICA I 42] 29] 69.0[25B [12M
Total # of samples with residues detected = 29
VINCLOZOLIN
APPLES NY 567 1 0.2/30B 30B
GREEN BEANS NY 466 5 1.1/ 298 25M
GRAPES CA, FL, Mi, NY, TX, WA 552 130 23.6 [3B 2.3M.
PEACHES FL, Ml, NY. 360 5 1.4/18B 41M

Total # of samples with residues detected =

141

TOTAL NUMBER OF DIFFERENT RESIDUES DETECTED:

‘TAL NUMBER OF SAMPLES ANALYZED: —



196 dotaotone (28.6%) Celery/Permethrins

min 8 ppb - max 0.59 ppm

70

:

fo)

S

by

E

Zz

26-50 B 51-99 B 0.10-0.5 M 0.51-1.0M
Concentration

567 samples tested = .
eee ee Grapefruit/Imazalil

35

Number of Occurrences

e 19B 10-25B 26-50 B 51-99 B 0.10-0.5 M
OO Pee Pet aa Concentration

ppm - parts per million

min - imum concentration detected
max - maximum concentration detected

51


APPENDIX 7

DISTRIBUTION OF RESIDUES DETECTED BY PESTICIDE

Saree

SSUMMARY OF RESULTS:

"NUMBER Te SAMBLES WITHRESIDUESD! DETECTED

‘COMMODITIES | SAMPLES WERE NUMBER Minimum | Maxiium
8 ee COLLECTED: “SAMPLES | _ Value Value
B. ADDITIONAL EPA - TARGETED PESTICIDES
AZINPHOS—METHYL
APPLES CA, FL, Ml, NY, TX, WA 567 178 37.4/9B 62M
CELERY MI 508 2 0.4/48B .11M
GREEN BEANS FL, Mi, NY, TX 466 16 3.4/408 38M
GRAPES NY, TX 552 4 0.7408 57M
PEACHES CA, Ml, NY, TX 360 45 72.5/4B -74M
POTATOES TM 568 1 0.2/40B 40B
‘Total # of samples with residues detected = 246
CHLOROTHALONIL
APPLES FL 567 7 0.2/23B 238
BROCCOLI TM 153 2 1.3/12B 37B
CELERY CA, FL, Ml, NY, TX, WA 508 164 32.3/2B 5.9M
GREEN BEANS CA, FL, NY, TX, WA 466 33 7.1|5B 1.6M
LETTUCE FL 565 1 0.2|.23M 23M
‘Total # of samples with residues detected = 201
DIAZINON
(APPLES CA, NY, 1X 567, 4 2.5[58 73B
CELERY CA, FL, Mi, NY, 1X, WA 508 67 13.2|5B 27M
CARROTS CA, FL, Ml, NY, WA 153 19 72.4(5B 2738
GREEN BEANS 1X, WA 466 4 09/68 998
GRAPEFRUIT TMx 567 70 1.8 [3B 288
GRAPES NY, TX 552 1 2.0|6B 143
LETTUCE CA, Ml, TX 565 10 18/58 63B
ORANGES TM 569 3 0.5[6B 6B
PEACHES CA, FL, MI, NY, TX 360 27 7.5|58 40M
POTATOES CA 568 1 0.2418 118
‘otal # of samples with residues detected = 166
DICHLORVOS
PEACHES [CA [ 110] 1] 0.9|59B _[59B
‘Total # of samples with residues detected = 1
DISULFOTON SULFONE
LETTUCE [cA [ 154] 3] 4.9[42B [16M
Total # of samples with residues detected = 3
ENDOSULFANS
APPLES CA, FL, MI, NY, TX, WA 567 75 73.2|3B 28M
BROCCOLI CA, NY, TX, WA 153 10 6.5 |2B 12M
CELERY MI_NY, 1X, WA 508 9 1.8/4B 1.0M
CARROTS MI, WA 153 4 2.6|2B 438
GREEN BEANS CA, FL, MI, NY, 1X, WA 466 126 27.0|3B 7.0M
GRAPES CA, FL, MI, NY, 1X 552 22 4.0|3B “11M
LETIUCE CA, FL, MI, NY, 1X, WA 565, 63 11.2/28 4.2M
PEACHES CA, FL, MI, NY, TX, WA 360 20 5.6|3B 97B
POTATOES CA, FL, MI, NY, TX WA 568 45 7.9/4B 97M
374

‘Total # of samples with residues detected =

Page 3 of 8


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DISTRIBUTION OF RESIDUES DETECTED BY PESTICIDE

APPENDIX

7

e eee (SUMMARY OF RESULTS: co
oo _ STATES WHERE NUMBER | SAMPLES WITH RESIDUES DETECTED
COMMODITIES SAMPLES WERE. OF | NUMBER| = @ = Minimum | Maximum
Le sa COLLECTED _ SAMPLES [00 eg Value. {Value
B. ADDITIONAL EPA — TARGETED PESTICIDES
ETHION
APPLES CA, FL, Mi, NY, TX, WA 567 19 3.4/6B 1.7M
GREEN BEANS MI 466 1 0.2(5B 5B
GRAPEFRUIT. CA, FL, Mi, NY, TX 567 15 2.6|2B 27B
ORANGES FL, MI, NY, TX 569 14 25/48 258
‘Total # of samples with residues detected = 49
METHIDATHION
ORANGES CA, MI, NY, TX 569 16 2.8/4B 43B
POTATOES TM 568 1 0.2|16B 16B
Total # of samples with residues detected = 17
MEVINPHOS
CELERY CA 508 2 0.4(5B 208
GRAPES NY 552 4 0.2/15B 15B
LETTUCE CA, WA 565, 5 0.9|5B 13M.
PEACHES NY 360 3 0.8 |.10M 18M.
Total # of samples with residues detected = YW
PARATHION—METHYL
APPLES CA, Ml, NY, TX 567 46 8.1/1B 81B
CELERY FL, MI 508 3 0.6|31B 628
CARROTS Mi 153 2 1.3/8B 8B
GREEN BEANS MI, NY 466 2 0.4/8B 16M
GRAPES CA, NY 552 2 0.4/15B 328
LETTUCE WA 565, 1 0.2|.21M 21M
PEACHES CA, FL, Ml, NY, TX 360 42 11.7(4B 12M
Total # of samples with residues detected = 98

Page 4 0f8



TABLE 4.1 CONCENTRATION DETECTED vs. ESTABLISHED TOLERANCES
(Pesticides detected in less than ten percent of the samples are not included)

Commodity/ Tolerance Percentage of Mean of Percent of
Pesticide (ppm) Samples with Residues Found Tolerance
Detected Residues (ppm)
eames
Captan 50 27.9 0.29 0.58
Dimethoate 1 10.0 0.13 13.0
Iprodione 60.0 29.2 0.27 0.45
Myclobutanil 1.0 17.0 0.11 11.0
Vinclozolin 6.0 23.6 0.35 3.8
GREEN BEANS
Acephate 3 25.3 0.52 17.3
Endosulfans 2.0 27.0 0.13 6.5
Methamidophos 27.7 0.15 Sod
LETTUCE
Endosulfans 2.0 11.2 0.11 5.5
Permethrins 20.0 11.0 0.31 1.6
ORANGES
Imazalil 10 29.3 0.15 1.5
Thiabendazole 10 63.8 0.28 2.8
PEACHES
Azinphos-Methyl 2.0 12.5 0.15 75
Captan 50 14.2 0.26 0.52
Dicloran 20 46.7 1.05 5.3
Iprodione 20.0 54.4 0.85 4.3
Parathion-Methyl 1 11.7 0.035 3.5
Phosmet 10 14.2 0.15 1.5

36


In January 1993, AMS established agreements with Colorado, North Carolina, and Ohio to
begin collecting samples for PDP. Under these agreements, all samples collected by these
three States would be sent to one or more of the other participating laboratories for analysis.
With the addition of these States, the segment of the Nation’s population represented by PDP
sampling was increased to approximately 50 percent, including produce directly distributed to
nearby States such as New Mexico and Wyoming.

Testing for five.N-methyl carbamates began in January. Formetanate analysis for apples and
peaches started in July 1993, and for oranges in October. :


552 samples tested

mint pbs max 1-8 ppm Grapes/Dimethoate

15

3
T

w

Number of Occurrences

10-25B 26-50B 51-99 B , 0:10-0.5M 0.51-1.0M 1.1-9.9M
Concentration

552 samples tested

rnin 18 ppb: max 3.0 ppm Grapes/Iprodione

100

Number of Occurrences
8 8 8 $8 8 & Bg sg

19B 1025B 2%650B  51-99B 0.100.5M 0.51-1.0M 1.19.9M
Concentration

pb - parte per billion
- parts per million

min minimum concentration detected |
max - maximum concentration detected 53


implemented in a timely manner. In addition to the pesticides requested by EPA, other
compounds have been included in the program due to their frequent detection by the
participating laboratories.

PDP’s database uses FDA’s pesticide and methodology codes, which enhance uniform data
reporting among government agencies. However, no comparisons should be made between
PDP and FDA pesticide residue monitoring data because of the basic differences in the two
Agencies’ programs. FDA’s regulatory monitoring is aimed at enforcing EPA tolerances
rather than at providing data for EPA’s use in risk assessment. Because of this, FDA’s
sampling protocol is designed to emphasize infractions of the law and, therefore, the data do
not represent actual exposure to pesticide residues. PDP’s goal, on the other hand, is to
generate data mainly for risk assessment studies; therefore, its sampling protocol is designed
to produce unbiased data from which national inferences can be made on dietary exposure.

PDP data also assists FDA by providing information on the use of post-harvest fungicides,
and by pinpointing areas where closer surveillance may be required as a follow-up to
apparent violations identified by PDP.

1.1 1992 Program Operations

This summary presents PDP operations and residue detections for calendar year 1992. The
number of commodities included in the program increased from 7 in January, to 10 in
February, and to 12 in October. Commodities added to the program, in order of inclusion,
were celery, green beans, peaches, broccoli, and carrots. The number of EPA-targeted
pesticides in the program also increased from 11 in January to 13 in March, and to 16 in
July. Table 1.0 shows the 16 EPA-targeted pesticides, the 12 PDP commodities, and their
dates of inclusion in the program. Also shown are the number of samples analyzed for these
compounds and the number of positive detections for each pesticide/commodity combination.
In addition, 12 other compounds capable of being detected by PDP were added to EPA’s list
of targeted pesticides in November.

PDP enlisted the services of USDA’s Animal and Plant Health Inspection Service (APHIS)
laboratory in May to begin testing for benomy] in selected commodities. With the addition
of APHIS, the number of testing facilities increased to nine.

1.2 1993 Preview

PDP’s sampling protocol was enhanced in January 1993 by the implementation of a more
statistically defensible method of site weighting that reflected both an improved site selection
routine and the incorporation of commodity volume data from selected sites. The

enhanced protocol was developed with the support of the USDA National Agricultural
Statistics Service, who will continue to provide long-term maintenance for PDP’s sampling
and estimation systems.


ist detections 126.8%) Carrots/DDE

min 2 ppb - max 0.13 ppm

35
8
Fl
3°
:)
5
3
Zz
19B 10-25B 26-50B . 51-99B 0.10-0.5M
Concentration
153 samples tested . .
Eee as Carrots/Diazinon
15
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B
g 7
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a 19B 10-25B 26-50B
ppb - parts per Enea Co tis
- parts centrat
in thinimum concentration detected n on
max - maximum concentration detected 47



SECTION 3.0 - LABORATORY OVERVIEW

During 1992, PDP laboratories performed analyses on 5,750 samples. Most of the pesticides
in the program were analyzed using general multiresidue methods (MRMs), which are
capable of detecting several compounds simultaneously. Benomyl, bromoxynil, and 2,4-D,
which are not detectable by MRMs, were analyzed by USDA’s Animal and Plant Health
Inspection Service (APHIS) laboratory using selective multiresidue methods.

3.1 Quality Assurance Program

To achieve data equivalency among participating laboratories, PDP required adherence to
rigorous quality assurance/quality control (QA/QC) criteria. To demonstrate the suitability
of analytical methods, as well as the proficiency of the technical staff, laboratories were
required to perform method validation studies for each pesticide/commodity pair.

PDP’s quality assurance program encompasses five elements:

e Proficiency Check Samples - All facilities were required to participate in the PDP
Check Sample Program. Periodically (approximately every 4 months), three to four
prepared commodities, containing several pesticides of known quantities, were sent to
the participating laboratories and tested under the same conditions as routine samples.
The resulting data were used to determine performance equivalency among the testing
laboratories, and to evaluate individual laboratory performance.

e Quality Control - Since quality control requirements are the same for one sample as
for several samples, it is more economical and efficient to collect and process the
samples as a set. Laboratories were permitted to refrigerate incoming samples of the
same commodity for up to 72 hours, to allow for different sample arrival times from
the collection sites. PDP quality control guidelines require that samples be tested as
part of an analytical set, which includes the sample set and the following components:

1, Reagent Blank: An amount of distilled water, equivalent to the natural moisture
content of the commodity, is run through the entire analytical process to determine

glassware cleanliness and system integrity.

2. Matrix Blank: A previously analyzed sample of the same commodity, which
contains either very low concentrations of known residues or no detectable residues,
is divided into two portions. The first portion is used to give background information
on naturally occurring chemicals, and the second one is used to prepare a matrix

spike.

3. Matrix Spike(s): A portion(s) of matrix blank is spiked with all pesticides of
interest to PDP prior to extraction. The matrix spike is used to determine the
accuracy of the analyst and instrument performance.

21


2.1 Sampling Procedures

AMS provided the States with quarterly program plans specifying the commodities to be
collected. In turn, each State was required to submit to AMS a quarterly sampling plan
designating the date(s) of collection and sampling sites per commodity. Both the dates and
sites were chosen at random; however, a commodity could not be sampled twice from the
same site in a given month. The States were asked to collect all samples for one commodity
on the same date, or within two consecutive dates, and to ensure that samples would arrive at
the testing facility within 24 hours of collection. :

A sample information form was filled out for each sample collected, which included the State
abbreviation, date, site number, and commodity code. The information provided by these
four items was combined to generate a unique identification number for that sample.
Information requested on the form also included: (1) whether the sample was domestic or
imported; (2) if imported, country of origin; (3) name of sampling site, grower, and packer;
and (4) a listing of potential or known post-harvest fungicides which may have been applied
to the sample.

States were asked to use alternative sampling sites, especially for terminal markets, in the
event that a commodity was not available at the original sampling site. This would better
enable the States to fulfill the objectives of the program plan (number of samples to collect
per commodity each month). The alternate sites were also chosen ‘at random, but a certain
amount of flexibility was provided for logistical purposes.

2.2 Statistics on Samples Collected

A total of 5,750 samples of fresh produce were collected during 1992. Table 2.0 shows the
number of samples collected per commodity by each State. These figures are, in some
cases, less than the total assigned number of samples due to the unavailability of product at
either the original or the alternative sampling site. States collected 5-pound samples for each
applicable testing facility.

The commodity codes utilized by PDP are: apples-AP, bananas-BN, broccoli-BR,
carrots-CR, celery-CE, grapefruit-GF, grapes-GR, green beans-GB, lettuce-LT, oranges-OG,
peaches-PC, and potatoes-PO.

Appendix 1 lists the geographic region of sampling sites in each State, the number of
sampling sites in each region, and the number and percent of samples collected in each
region.

As indicated in Appendix 2, samples collected by PDP in 1992 originated from the 6
participating States, 31 other States, and 16 foreign countries. Appendix 2 also shows that:
(1) 100 percent of the bananas and 46.9 percent of the grapes were imported; (2) all but 2
lettuce samples were domestic, with 86.1 percent grown in California; (3) 65 percent of the
domestically grown peaches came from California, and 91.7 percent of the imported peaches

12


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analyzed in 46 of the samples only). The total number of residues found was 854. This
total includes multiple residues detected in single samples, which ranged from 2 samples
containing 6 different residues to 127 samples containing 2 residues. Violations were
reported for 18 domestic samples containing residues of DCPA (11), quintozene (3),
chlorpyrifos (2), and iprodione (2), for which no tolerance has been established for celery.

Grapefruit

Out of 567 samples analyzed, 260 (45.9 percent) had at least 1 detectable residue. Nine
different pesticides were found. Thiabendazole and imazalil, both post-harvest fungicides,
were the most frequently detected. The total number of residues found, including multiple

residues, was 332. No tolerance violations were reported.

Grapes

Out of 552 samples analyzed, 381 (69.0 percent) were found to contain at least 1 detectable
residue. Twenty-one different pesticides were detected. Most frequently found were
iprodione, captan, vinclozolin, and myclobutanil. The total number of residues found was
756. This total includes multiple residues detected in single samples, which ranged from 1
sample containing 6 different residues to 113 samples containing 2 residues. Violations were
reported for five samples, one domestic and four imported commodities. Two of these
violations were for residues for which no tolerance has been established for grapes
(diphenylamine and methamidophos), and 3 for residues exceeding the tolerance level
(parathion-1, chlorpyrifos-1, dimethoate-1).

Green Beans

Out of 466 samples analyzed, 279 (59.9 percent) were found to contain at least 1 detectable
residue. Twenty four different pesticides were detected. Most frequently found were
methamidophos, endosulfans, and acephate. The total number of residues found was 576.
This total includes multiple residues detected in single samples, which ranged from 7 samples
containing 5 different residues to 84 samples containing 2 residues. Violations were reported
for 22 samples, 15 domestic and 7 imported commodities. Twenty-one of these violations
were for residues for which no tolerance has been established for green beans
(methamidophos-18, permethrins-3), and 1 for residues exceeding the tolerance level

(acephate-methamidophos combined).

Lettuce

Of 565 samples analyzed, 201 (35.6 percent) had at least 1 detectable residue. Nineteen
different pesticides were found. The most frequently found pesticides were permethrins and
endosulfans. The total number of residues found, including multiple residues, was 297.
Multiple residues found in single samples ranged from 1 containing 5 different residues to 42
which had 2 residues. Violations were reported for 5 domestic samples. Of these, 4 were

27


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3.3 Sample Analysis

Variations of the Luke extraction procedures developed by FDA were used by Florida,
Michigan, New York, and Texas. California and Washington used the multiresidue method
developed by the California Department of Food and Agriculture (CDFA). Sample
extraction and cleanup preparation procedures, to achieve the levels of detection required by

the program, were based on organic solvent/partition procedures.

Various types of chromatography were used for the initial identification and quantitation of
pesticides. Confirmation was accomplished by mass spectrometry or by alternate detection
systems when applicable. Confirmation was deemed necessary due to the complexity of
commodity matrices and the low concentration levels of detected residues. The confirmatory
analysis provided an extra measure of confidence in both the identification of the pesticide

residue and its concentration.

Average limits of detection (LODs) and limits of quantitation (LOQs) for testing laboratories
are shown in Appendix 4.

23


565 samples tested

62 detections (11.0%) Lettuce/Permethrins

min 5 ppb - max 1.9 ppm

30

15 -

Number of Occurrences

19B 1025B = 26-50B = S1-99B_ | 0.100.5M O.51-1.0M 1.1-9.9M
centration

167 detections (29.9%) Oranges/Imazalil

min 10 ppb - max 0.94 ppm

90

80

70

6

50

Number of Occurrences

19B 26-50B 51-99 B 0.10-0.5 M 0.51-1.0M
ppb - parts per billion Concentration
ppm

per million

ium concentration detected
imum concentration detected

57


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Figure 2.0
Commodity Distribution Percentages
Percent

imported vs. Domestic J

Apples

Bananas
. 2.0

I
Broccoli 98.0
by
Carrots 94.1
2.0

Cele:

vy 98.0
Grapefruit 0.7)
99.3

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Green

Beans

Lettuce

Oranges

Peaches

Potatoes



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Figure B

Pesticides in PDP

22.0%

HE Original EPA List (16)

2,4-D
Acephate
Atrazine”
Benomyl
Bromoxynil*
Chlorpyrifos
Dicloran
Dicofol

a

Hexachlorobenzene (HCB)*

Iprodione

Lindane
Methamidophos
Methoxychior
Pentachlorobenzene
Permethrins
Quintozene (PCNB)

* Not detected

48.0%

30.0%

Additional EPA List (12) [2244 Other (26)

Azinphos-methyl
Chlorothalonil
Diazinon
Dichlorvos
Disulfoton sulfone
Endosulfans
Ethion
Fenamiphos*
Malathion*
Methidathion
Mevinphos
Parathion-methyl

Anilazine
Captan
Carbaryl
Chlorpropham
Cypermethrin
DCPA
DDE+DDT+TDE
Demeton
Demeton-S Sulfone
Dimethoate
Diphenylamine
Ethoprop
Imazalil
Myclobutanil
O-phenyphenol
Omethoate
Parathion
Phorate Sulfone
Phosalone
Phosmet
Propargite
Thiabendazole
Trifluralin
Vinclozolin

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567 samples teeted

rin’ ppb men Oe Apples/Endosulfans

min 3 ppb - max 0.28 ppm

35 ——=

Number of Occurrences

519 samples tested

293 detections (66.5%) Apples/Thiabendazole

min 15 ppb - max 4.8 ppm

150

Number of Occurrences

1-983 10-258 26-50 B 51-99B . 0.100.5M 0.! OM = 1.1-9.9M
Concentration

ppb - parte per billion

ppm - parte per million
min - minimum concentration detected
max - maximum concentration detected
45


1453 samples tested
44 detections (28.8%)
min 25 ppb - max 0.35 ppm

5

Carrots/Iprodione

Number of Occurrences

1508 samples tested
136 detections (26.8%)
min 5 ppb - max 1.7 ppm.

Celery/Acephate

40

ppb - parts per billion
ppm - parte per million

min - minimum concentration dete:
n teeta

max - imum concentrati

51-99 B 0.10-0.5M 0.51-1.0M  1.1-9.9M

Concentration

19B 26-50 B

10-258

48