Chemical Residue Analysis, FY Florida Dept. of Agriculture

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1 Chemical Residue Analysis, FY Florida Dept. of Agriculture Jo Marie Cook Bureau of Chemical Residue Laboratories Florida Department of Agriculture and Consumer Services

2 Bureau of Chemical Residue Labs Pesticide Regulatory Surveillance Pesticide Data Program Food Emergency Response Network BP Memorandum of Agreement New LIMS

3 Custom LIMS Standard Mixes Screening Plans Excel Results Data Entry Web-based Oracle State regulatory Field Sampling application Link to PDP field application

4 Food Emergency Response Network (FERN) New Employees Exactive Plus Orbi-trap large screens Arsenic Speciation in Rice EPA / FERN exercise Two Proficiencies Select Agent by LC/MS/MS method review

5 Seafood Safety (Program Ends October 2013)

6 Samples Analyzed in FY July 1, 2012 to June 30, 2013 Pesticide Data Program 1,569 F & V for pesticides # pesticides 655 applesauce baby food broccoli cantaloupe tangerines 169

7 LIMITS OF DETECTION (mg/kg) PDP BROCCOLI LODs 183 pesticides

8 LOWER LIMITS OF DETECTION (mg/kg) PDP BABYFOOD APPLESAUCE LODs 201 pesticides

9 Samples Analyzed in FY July 1, 2012 to June 30, 2013 State Regulatory 930 fresh F & V for pesticides 204 pesticides 1,696 seafood, PAHs & dispersant 15 PAHs, DOSS 1 consumer complaint oyster Introduced Orbitrap and added 114 LC/MS analytes

10 LIMITS OF DETECTION (mg/kg) STATE REGULATORY LODs pesticides

11 Expanded Qualitative Screen State Regulatory Screen expanded LC/MS 226 compounds (qualitative 0.01LOD 0.05 LOQ) GC/MS 91 compounds (quantitative 0.01 LOD 0.02 LOQ)

12 LOWER LIMITS OF DETECTION (mg/kg) State Regulatory Mega Screen 317 pesticides

13 3 rd party Standard Mixes Standards prepared, verified, certificate of analysis 256 compounds in 13 mixes Most at 100 ng/ul = 40 LOQ Add together to make LC/MS mega mix

14 Origin of Samples, FY , % Florida 376 Florida Fruits &Vegetables 1,696 Seafood 1 Complaint - oyster % Other U.S. States % Other Countries 2,627 TOTAL

15 FY 12-13: 90 Pesticides Detected out of 204 Screened FY 07-13: 138 Pesticides Detected. OXAMYL OXIME IMIDACLOPRID PROPAMOCARB HCL PERMETHRIN TOTAL MYCLOBUTANIL BOSCALID FENPROPATHRIN CAPTAN CYPERMETHRIN ENDOSULFAN SULFATE CYPRODINIL PYRIMETHANIL BIFENTHRIN FLUDIOXONIL CHLORPYRIFOS PYRACLOSTROBIN IMAZALIL AZOXYSTROBIN THIABENDAZOLE CHLOROTHALONIL

16 Commodities with pesticides LETTUCE-LEAF CILANTRO BLUEBERRIES BLACKBERRIES PEARS MANGOES PEACHES PAPAYAS CELERY CANTALOUPE AVOCADOS SQUASH-YELLOW POTATOES-SWEET EGGPLANTS ZUCCHINI CARROTS-ROOTS BEANS-GREEN BANANAS POTATOES PINEAPPLES GRAPES APPLES TANGERINES PEPPERS-BELL ORANGES CUCUMBERS GRAPEFRUIT STRAWBERRIES TOMATO 536 of 930 samples = 58%

17 Pesticides Detected and Violations in Fresh Fruits and Vegetables Fiscal Year Samples Analyzed % with Hits % Violations 52% 60% 55% 54% 56% 57% 58% 1.94% 2.11% 0.99% 1.07% 1.56% 4.16% 3.12% % U.S. 0.6% 0.9% 0.7% 0.42% 0.38% 2.63% 2.41% Violations % Import Violations 6.3% 6.5% 2.4% 2.4% 5.51% 1.53% 4.91%

18 18 Commodities with Violations 23 violative pesticides Commodity Pesticide Tolerance (ppm) ASPARAGUS METHAMIDOPHOS NONE BEET-ROOTS CHLOROTHALONIL 0 BEET-TOPS x 2 CYPERMTHRIN 0.05 ATRAZINE, FLONICAMID, CHLOROTHALONIL 0 CABBAGE x 2 DIMETHOATE, OMETHOATE 0 CILANTRO x 5 CHLOROTHALONIL, ENDOSULFANS, PCA, PCNB, METHAMIDOPHOS 0 CYFLUTHRIN, PROPAMOCARB HCL 0 CULANTRO CYPERMETHRIN 0.05 METHIOCARB 0 CUCUMBERS x2 CHLORFENAPYR 0.01 IPRODIONE 0 EGGPLANT THIACLOPRID 0 GRAPES METHOXYFENOZIDE 1.0 MANGOES CARBENDAZIM 0 MUSHROOMS x 2 CARBENDAZIM 0 ORANGES x2 DIPHENYLAMINE, CARBENDAZIM 0 SNOW PEAS IPRODIONE, CARBENDAZIM 0 HOT PEPPERS PERMETHRIN 0 SUMMER SQUASH ENDOSULFANS 0 STRAWBERRIES x2 PERMETHRIN 0 CARBARYL 4.0 TANGARINES x2 CARBENDAZIM 0 TOMATOES TRIDIMEFON, TRIADIMENOL 0

19 FY Violations 2.41% of U.S. samples 4.91% of imported samples U.S. Violations in: BEETS CABBAGE CILANTRO GRAPES ORANGES HOT PEPPERS SUMMER SQUASH STRAWBERRIES TANGARINES Imported Violations in: ASPARAGUS CILANTRO CULANTRO CUCUMBERS EGGPLANT ORANGES SNOW PEAS TOMATOES Peru Mexico Costa Rica Mexico, Canada Honduras S. Africa Peru Mexico

20 FY Commodities with 6 or more Pesticides Detected in a Single Sample # of Pesticides found Commodity 10 PEACHES 9 TOMATO* 8 GRAPES* 7 CILANTRO* 7 STRAWBERRIES* 6 PEPPERS-BELL 6 BLUEBERRIES 6 PEPPERS-HOT* 6 CITRUS* 6 BLACKBERRIES

21 Fy07-13 Strawberries: 34 Pesticides found 6 Violations PESTICIDE Maximum TOLERANCE PESTICIDE Maximum TOLERANCE ACETAMIPRID FLUDIOXONIL AZOXYSTROBIN MALATHION BIFENTHRIN MALATHION O ANALOG BQL BOSCALID METALAXYL BUPROFEZIN METHOMYL 0.65 NONE CAPTAN METHOMYL CARBARYL METHOXYFENOZIDE CARBARYL MYCLOBUTANIL CHLORANTRANILIPROLE NALED (based on dichlorvos) CHLOROTHALONIL 1.2 NONE NOVALURON CHLORPYRIFOS NOVALURON CYPERMETHRIN BQL PERMETHRIN TOTAL 0.42 NONE CYPRODINIL PROPICONAZOLE DIAZINON BQL PYRACLOSTROBIN DICOFOL pp' BQL PYRACLOSTROBIN DIFENOCONAZOLE PYRIMETHANIL ENDOSULFAN I QUINOXYFEN ENDOSULFAN II SPINOSAD A ENDOSULFAN SULFATE SPINOSAD D ENDOSULFAN TOTAL BQL SPIROMESIFEN ETOXAZOLE TETRAHYDROPHTHALIMIDE FENHEXAMID THIAMETHOXAM FENPROPATHRIN THIOPHANATE ME (based on carbendazim) FENPYROXIMATE TRIFLOXYSTROBIN FLUDIOXONIL TRIFLUMIZOLE

22 2007 to 2013 Strawberries: 34 Pesticides found 6 Violations PESTICIDE MAXIMUM (PPM) TOLERANCE ACETAMIPRID CARBARYL CARBARYL CHLOROTHALONIL 1.2 NONE METHOMYL 0.65 NONE METHOMYL PERMETHRIN TOTAL NONE PYRIMETHANIL

23 Citrus: 30 Pesticides found 7 Violations PESTICIDE MAXIMUM (PPM) TOLERANCE 1 NAPHTHOL ACETAMIPRID ALDICARB SULFOXIDE AZOXYSTROBIN BUPROFEZIN CARBARYL CARBENDAZIM 0.17 NONE THIOPHANATE ME (based on carbendazim) CHLORPYRIFOS CYPERMETHRIN DICOFOL pp' DIMETHOATE DIPHENYLAMINE 0.13 NONE ETHION FENBUCONAZOLE FENPROPATHRIN FLUDIOXONIL IMAZALIL IMIDACLOPRID MALATHION METHIDATHION O PHENYLPHENOL PHOSMET PIPERONYL BUTOXIDE PYRACLOSTROBIN PYRIDABEN PYRIMETHANIL PYRIPROXYFEN SPIRODICLOFEN THIABENDAZOLE

24 Pesticides Commonly Found in Citrus IMAZALIL THIABENDAZOLE CHLORPYRIFOS PYRACLOSTROBIN AZOXYSTROBIN CARBARYL O-PHENYLPHENOL FENPROPATHRIN FENBUCONAZOLE DICOFOL-pp' METHIDATHION PYRIMETHANIL

25 Citrus: 783 Samples Analyzed 645 with Pesticides 82% 30 Pesticides found 7 Violations PESTICIDE MAXIMUM (PPM) TOLERANCE CARBENDAZIM 0.17 NONE THIOPHANATEME (based on carbendazim) DIPHENYLAMINE 0.13 NONE

26 Future Goals Implement / Maintain FSLIMS Pesticides by end of 2015 Antibiotics in Honey and Seafood