Study of Pesticide Residues in Agricultural Products towards the Positive List System

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1 December , Study of Pesticide Residues in Agricultural Products towards the Positive List System Yumi A@>N6B6,Naoki YDH=>D@6 and Keiko I8=>=6H=> (Hyogo Prefectural Institute of Public Health and Environmental Sciences: , Arata-cho, Hyogo-ku, Kobe , Japan; Corresponding author) During a 3-year monitoring survey (April 2002 March 2005) of pesticide residues in agricultural products, 592 samples (324 domestic; 268 imported) collected in Hyogo prefecture, Japan were analyzed. The number of tested increased from 232 in FY 2002 to 323 in FY The purpose of the study was to clarify the residue status by accumulating information about detected frequently, to allow e#ective and e$cient regulation under the new Positive List legislation to be implemented in FY Overall, 47 of domestic and 61 of imported samples contained detectable residues and ca. 60 of positive samples contained multiple residues. The limit of quantitation was set at 0.01 mg/g and the limit of detection was mg/ g. Most of the residues were present at low concentrations: 80 of the detections in samples excluding imported citrus fruits were 0.05 mg/g. More than 5 di#erent ( 0.01 mg/g) were detected simultaneously in 13 samples. The sum of the ratios of residues to MRLs was calculated as one of the indexes to represent the risk of multiple residues, and they exceeded 100 in 3 imported frozen vegetables; baby kidney bean, spinach, Welsh onion. Samples in violation of the Food Sanitation Law were not found in our survey, but 1.9 of the samples might be in conflict with the new Positive List legislation. (Received July 8, 2005) Key words: pesticide residue agricultural product the Positive List System simultaneous determination GC/MS LC/MS 1) GC/MS 2) 4) 5) 10) p ( ), LC/MS GC/MS , 119

2 Table GC/MS LC/MS 4. Agilent 6890N 5973inert Agilent 1100 MSD (SL) 5. 9) ODS PSA GC/MS SCAN LC/MS SCAN mg/g (S/N 3) mg/g (Trace) Table ), 10) Fig Table 4 5 Vol. 46, No. 6 (1) mg/g mg/g 0.01 mg/g mg/g 0.05 mg/g mg/g 0.05 mg/g (2) mg/g mg/g 0.01 mg/g 0.05 mg/g mg/g mg/g

3 Organophosphorus pesticide Organochlorine pesticide N-Mmethylcarbamate Table 1. Llist of Pesticides Tested FYs FYs FY 2004 No. GC/MS main LC/MS main GC/MS main LC/MS main GC/MS main LC/MS main thiometon, tolclofosmethyl, triazophos quinalphos, terbufos, tetrachlorvinphos, profenofos, prothiofos, pyraclofos, phosphamidon, pirimiphosmethyl, phorate, phosalone, phosmet, parathion, parathionmethyl, phenthoate, monocrotophos, naled, omethoate, methacrifos, methidathion, isofenphos, isoxathion, malathion, fenthion, fonofos, fosthiazate, iprobenfos, etrimfos, fenitrothion, fensulfothion, -Z), edifenphos, ethion, ethoprophos, dichlorvos, dimethoate, dimethylvinphos(-e, cyanophos, demeton-s-methyl, diazinon, chlorpyrifosmethyl, cyanofenphos, chlorfenvinphos(-e, -Z), chlorpyrifos, cadusafos, carbophenothion, EPN, azinphosmethyl, butamifos, vamidothion phoxim, trichlorfon, methamidophos, Acephate, Anilofos, dichlofenthion, disulfoton, fenamiphos, isocarbophos, mecarbam, mevinphos, piperophos, propaphos, pyridaphenthion, sulprofos Dioxathion, isazofos Bensulide 69 BHC(a-, b-, g-, d-), DDT(p,p -, o,p -), aldrin, captafol, captan, chlordane, chlorobenzilate, dicofol, dieldrin, endosulfan(a-, b-), endrin, folpet, heptachlor, heptachlor epoxide (endo, exo), hexachlorobenzene, indanofan, methoxychlor, mirex, nonachlor, phthalide, quintozene Dichlobenil, dicloran, tecnazene, tetradifon 25 XMC, aldicarb, bendiocarb, carbaryl, carbofuran, ethiofencarb, fenobucarb, isoprocarb, methiocarb, methomyl, metolcarb, oxamyl, propoxur, terbucarb, xylylcarb Furathiocarb Thiodicarb December 2005

4 Organonitrogen Pyrethroid Table 1. Continued FYs FYs FY 2004 No. GC/MS main LC/MS main GC/MS main LC/MS main GC/MS main LC/MS main EPTC, acibenzolar-s-methyl, alachlor, Acetamiprid, Ametryn, Bifenazate, atrazine, bifenox, bitertanol, bromacil, azoxystrobin, benalaxyl, chloridazon, buprofezin, butachlor, butylate, carpropamid, bromobutide, cumyluron, cafenstrole, chlomethoxyfen, clethodim, butafenacil, dymron, chlorfenapyr, chlornitrofen, clofentezine, carbetamide, fenpyroximate, chlorpropham, cyanazine, desmedipham, clomeprop, fentrazamide, cyhalofopbutyl, cyproconazole, ethoxyquin, dimepiperate, ferimzone (-E,-Z), cyprodinil, dichlofluanid, imazalil, dimethametryn, inabenfide, diclocymet, diethofencarb, imibenconazole, dithiopyr, nitenpyram, diethyltoluamide, difenoconazole, iprodione, etridiazole, oxadixyl, diflufenican, dimethenamid, mepanipyrim, fenbuconazole, oxaziclomefone, dimethomorph, diphenamid, methabenzthiazuron, fenothiocarb, oxpoconazole diphenylamine, esprocarb, ethychlozate, pencycuron, fenoxanil, fumarate, etobenzanid, etoxazole, famoxadone, prochloraz, fenpropimorph, phenmedipham, fenarimol, fenoxapropethyl, fipronil, propamocarb, fluacrypyrim, tepraloxydim, fludioxonil, flumioxazin, flusilazole, pymetrozine, indoxacarb-mp, thiacloprid flutolanil, furametpyr, hexaconazole, pyrazoxyfen, metalaxyl, kresoximmethyl, lenacil, mefenacet, tebufenozide, metominostrobin(-e, -Z), mepronil, metolachlor, metribuzin, thiabendazole, naproanilide, myclobutanil, nitrofen, paclobutrazol, tricyclazole oxabetrinil, penconazole, pendimethalin, pentoxazone, prometryn, pirimicarb, pretilachlor, procymidone, pyroquilon, propanil, propiconazole,propyzamide, quinoclamine, pyraflufenethyl, pyributicarb, pyridaben, thiamethoxam, pyrifenox(-e,-z), pyrimethanil, thiocyclam, pyrimidifen, pyriminobacmethyl(-e,-z), tolfenpyrad, pyriproxyfen, quizalofopethyl, simazine, trifloxystrobin simetryn, swep, tebuconazole, tebufenpyrad, terbacil, tetraconazole, thenylchlor, thifluzamide, thiobencarb, tolylfluanid, triadimefon, triadimenol, trichlamide, triflumizole, trifluralin, uniconazole P, vinclozolin Carfentrazone-ethyl, oxadiazon Amitraz, benzofenap, chlorfluazuron, chromafenozide, clothianidin, cyazofamid, cycloxydim, cymoxanil, diflubenzuron, dimethirimol, diuron, flufenoxuron, hexaflumuron, hexythiazox, imidacloprid, isouron, linuron, lufenuron, methoxyfenozide, probenazole, pyrazolate, teflubenzuron, triforine 175 Acrinathrin, allethrin, bifenthrin, bioresmethrin, cyfluthrin, cyhalothrin, cypermethrin, deltamethrin, ethofenprox, fenpropathrin, fenvalerate, flucythrinate, fluvalinate, halfenprox, imiprothrin, permethrin, phenothrin, pyrethrins, silafluofen, tefluthrin, tetramethrin, tralomethrin Cycloprothrin Vol. 46, No. 6

5 Table 1. Continued FYs FYs FY 2004 No. GC/MS main LC/MS main GC/MS main LC/MS main GC/MS main LC/MS main Other Benfuresate, bromopropylate, cinmethylin, dimethipin, diphenyl, isoprothiolane, methoprene, phenothiol, piperonyl butoxide o-phenylphenol, propargite MCPB-ethyl MCPA-methyl Benzobicyclon 14 Total No Table 2. Llist of Pesticide Metabolites Tested FYs FYs FY 2004 No. GC/MS main LC/MS main GC/MS main LC/MS main GC/MS main LC/MS main Organophosphorus EPN oxon, demeton-s-methyl sulfone, diazinon oxon, fenitrothion oxon, isofenphos oxon, isoxathion oxon, malathion oxon, parathion oxon, parathionmethyl oxon, prothiofos oxon Vamidothion sulfone Disulfoton sulfone Demeton-S-methyl sulfoxide 13 Organochlorine p,p -DDE, p,p -DDD, endosulfan sulfate, dichlorobenzophenone (dicofol metabolite), oxychlordane, phthalimide (folpet methabolite), tetrahydrophthalimide (captan, captafol metabolite) 7 N-Methylcarbamate Aldicarb sulfone, aldicarb sulfoxide, ethiofencarb sulfone, ethiofencarb sulfoxide, methiocarb sulfone, methiocarb sulfoxide 7 3-Hydroxycarbofuran Organonitrogen Dichlofluanid metabolite, 2,4-dichloroaniline (imibenconazole metabolite), furametpyr metabolite, tolylfluanid metabolite, triflumizole metabolite Imazalil metabolite, imibenconazole desbenzyl, iprodione metabolite, mepanipyrim metabolite Oxpoconazole metabolite, thiacloprid-amide Amitraz metabolite, carbendazim, oxpoconazole formyl 14 Total No December 2005

6 310 Table 3. Number of Samples Tested and Containing Detectable Pesticide Residues during FYs Sample group Tested No. Positive 1 Multi residues 2 No. No. Total Domestic Cereals Beans Vegetables Fruits Nuts & seeds Imported Cereals Vegetables Frozen vegetables Citrus fruits Other fruits Samples containing 1 or more pesticide residues mg/g 2 Samples containing multipesticide residues mg/g 0.01 mg/g 0.05 mg/g mg/g 0.5 mg/g mg/g Table 6 7 (1) 0.01 mg/g Vol. 46, No (2) 0.01 mg/g Table 8 1 8) 11) 10 (ADI) 0.2 mg/kg/day 50 kg 40 g ADI Fig. 1. Detection rates of positive samples during FYs

7 December Table 4. Pesticide Residues Found in Domestic Agricultural Products (FYs ) Pesticide Tested samples Residue ( mg/g) Total detections Commodity Cereals Ferimzone Unpolished rice Dichlorvos Unpolished rice Isoprothiolane Unpolished rice Phthalide Unpolished rice Silafluofen Unpolished rice Vegetables Procymidone Cucumber, eggplant etc. Carbendazim Lettuce, cucumber etc. Acetamiprid Shirona, sweet pepper etc. Azoxystrobin Tomato, cucumber etc. Methomyl Babykidney bean etc. Ethofenprox Green soybean, cucumber etc. Permethrin Shirona, sweet pepper etc. Iprodione Chinese cabbage, cucumber etc. Chlorfenapyr Chinese cabbage, sweet pepper etc. Fenvalerate Chinese cabbage, lettuce etc. Acephate Carrot, lettuce etc. Oxadixyl Cucumber, Chinese cabbage etc. Chlorotalonil Asparagus, tomato etc. Methamidophos Chinese cabbage, carrot etc. Metalaxyl Cucumber, Chinese cabbage etc. Imidacloprid Sweet pepper etc. Cypermethrin Lettuce, Welsh onion Fruits Acetamiprid Grape, apple etc. Kresoximmethyl Grape, apple etc. Captan Apple, Japanese pear etc. Cyprodinil Grape, apple Carbendazim Japanese persimmon, melon etc. Chlorpyrifos Apple Fenpropathrin Apple etc. Bromopropylate Japanese pear, apple Iprodione Grape, peach etc. Cyhalothrin Apple Mepanipyrim Grape etc. Carbaryl Apple etc. Permethrin Plum, Japanese persimmon etc. Fludioxonil Grape Propargite Apple Cypermethrin Japanese persimmon Tebufenpyrad Strawberry etc. Fenitrothion Grape etc. Triflumizole Grape etc. Azoxystrobin Grape etc. Chlorfenapyr Apple etc. Diazinon Apple etc. Methamidophos Fig etc.

8 312 Vol. 46, No. 6 Table 5. Pesticide Residues Found in Imported Agricultural Products (FYs ) Pesticide Tested samples Residue ( mg/g) Total detections Commodity Cereals Isoprothiolane Polished rice Dichlorvos Polished rice Vegetables Permethrin Celery etc. Dicloran Celery Omethoate Okra, baby pea Carbendazim Welsh onion, garlic sprout etc. Cypermethrin Okra Propiconazole Celery Frozen vegetables Cypermethrin Spinach, komatsuna etc. Carbendazim Baby kidney bean, komatsuna etc. Omethoate Baby kidney bean, baby pea etc. Methamidophos Broccoli, baby kidney bean etc. DDT Baby kidney bean etc. Triadimenol Baby pea, baby kidney bean etc. Chlorpyrifos Komatsuna, baby kidney bean etc. Fenvalerate Green soybean, Welsh onion etc. Methomyl Baby kidney bean Dimethoate Baby kidney bean, Welsh onion Cyproconazole Baby kidney bean Endosulfan Baby kidney bean, spinach etc. Chlorfenapyr Green soybean etc. Fenpropathrin Welsh onion, baby kidney bean Procymidone Leek, spinach Dicofol Baby kidney bean, green soybean Monocrotophos Welsh onion, baby kidney bean Triazophos Baby kidney bean, green soybean Citrus fruits Imazalil Orange, grapefruit, lemon Thiabendazole Orange, grapefruit, lemon Chlorpyrifos Orange, grapefruit, lemon o-phenylphenol Orange, grapefruit, lemon Methidathion Orange, grapefruit, lemon Diphenylamine Lemon Prothiofos Grapefruit Diazinon Orange, lemon Bromopropylate Orange etc. Carbendazim Lemon etc. Carbaryl Lemon, orange Ethion Grapefruit Azoxystrobin Grapefruit Other fruits Chlorpyrifos Banana etc. Triflumizole Pineapple Iprodione Banana, grape etc. Carbendazim Banana etc. Myclobutanil Cherry etc. Captan Avocado, strawberry

9 December Table 6. Distribution of Multiple Pesticide Residues ( 0.01 mg/g) Detected on Domestic Samples Sample No. of detected residues Total positive samples Tested Group Commodity No. samples Cereals Unpolished rice Polished rice Corn Buckwheat Wheat flour Subtotal Beans Soybean Vegetables Green soybean Cucumber Lettuce Tomato Chinese cabbage Sweet pepper Welch onion Eggplant Cabbage Carrot Potato Onion Garden radish Spinach Komatsuna Sweet potato Broccoli Garland chrysanthemum Pumpkin Taro Baby kidney bean Lotus root Chingensai Small green pepper Broad bean Burdock Cauliflower Celery Nigauri Asparagus Ginger Shirona Aouri Japanese mushroom Santousai Turnip Subtotal Fruits Grape Japanese pear Apple Japanese persimmon Fig Peach Watermelon Melon Mandarin orange Strawberry Loquat Japanese plum Summer orange Subtotal Nuts & seeds Chestnut Total

10 314 Vol. 46, No. 6 Table 7. Distribution of Multiple Pesticide Residues ( 0.01 mg/g) Detected on Imported Samples Sample No. of detected residues Total positive samples Tested Group Commodity No. samples Cereals Polished rice Wheat flour Subtotal Vegetables Okra Broccoli Pumpkin Burdock Celery Welsh onion Sweet pepper Asparagus Japanese mushroom Garlic Garlic sprout Baby pea Guava tea Baby snack pea Onion Subtotal Frozen Green soybean vegetables Baby pea Baby kidney bean Komatsuna Spinach Welsh onion Okra Chingensai Broccoli Taro Pea Asparagus Broad bean Sweet pepper Pumpkin Japanese mushroom Lotus root Leek Corn Garlic sprout Mushroom Subtotal Citrus fruits Lemon Orange Grapefruit Subtotal Other fruits Banana Pineapple Avocado Kiwi fruit Grape Cherry Strawberry (frozen) Melon Subtotal Total

11 December Table 8. Multiple Pesticide Residues in Agricultural Products Cucumber (domestic) (2004.6) 1 Chinese cabbage (domestic) ( ) Pesticide Residue MRL 2 ( ) 3 Pesticide Residue MRL ( ) Chlorfenapyr Acephate Metalaxyl Methamidophos 0.07 Mepanipyrim Chlorfenapyr Procymidone Fenvalerate Oxadixyl Famoxadone Cabendazim Imidacloprid Tr. 4 1 Total (Residue/MRL 14.1 Total (Residue/MRL 7.5 Grape (domestic) (2002.7) Apple (domestic) ( ) Pesticide Residue MRL ( ) Pesticide Residue MRL ( ) Acetamiprid Chlorpyrifos Fenitrothion Prothiofos Tr. 0.3 Permethrin Fenpropathrin Cyprodinil Cyhalothrin Folpet Acetamiprid Fludioxonil Cyprodinil Mepanipyrim Kresoximmethyl Triflumizole Pyrimethanil Tr. 10 Total (Residue/MRL 21.3 Total (Residue/MRL 9.3 Celery (America) (2005.1) Paprika (sweet pepper) (Korea) (2004.7) Pesticide Residue MRL ( ) Pesticide Residue MRL ( ) Acephate Chlorfenapyr Methamidophos Tr. Pyridaben Tr. 3.0 Permethrin Oxadixyl DDT Tr. 0.2 Imidacloprid Oxamyl Tr. 5 Azoxystrobin 0.01 Dicloran Procymidone Tr. 5 Propiconazole Azoxystrobin Tr. 5 Linuron Tr. 0.2 Total (Residue/MRL 9.7 Total (Residue/MRL 11.4 Spinach, frozen (China) (2002.9) Komatsuna, frozen (China) ( ) Pesticide Residue MRL ( ) Pesticide Residue MRL ( ) Chlorpyrifos Chlorpyrifos Methamidophos 0.01 Fipronil 0.27 Parathionmethyl Tr. 1.0 Acetamiprid DDT Tr. 0.2 DDT Tr. 0.2 Cypermethrin Cyhalothrin Fenvalerate Cabendazim Tr. 3 Total (Residue/MRL Total (Residue/MRL 6.6

12 316 Vol. 46, No. 6 Table 8. Continued Baby kidney bean, frozen (China) (2002.7) Welsh onion, frozen (China) (2004.2) Pesticide Residue MRL ( ) Pesticide Residue MRL ( ) Chlorpyrifos Monocrotophos Dimethoate Dimethoate Omethoate 0.11 Omethoate Tr. Methamidophos 0.06 Isocarbophos 0.01 Monocrotophos Endosulfan DDT Cypermethrin Dicofol Fenvalerate Buprofezin Tr. Fenpropathrin 0.15 Pyridaben Tr. 2.0 Carbofuran Tr. Methomyl Triadimenol Tr. Isoprocarb Tr. Paclobutrazol 0.19 Cypermethrin Fenvalerate Fenpropathrin 0.02 Propargite 0.01 Triadimenol Total (Residue/MRL Total (Residue/MRL Green soybean, frozen (China) Grape (Chile) Pesticide Residue MRL ( ) Pesticide Residue MRL ( ) Cypermethrin Methomyl Fenvalerate Iprodione Dicofol Cyprodinil Chlorfenapyr 0.01 Fludioxonil DDT Tr. 2.0 Dichlorvos Tr. 0.5 Total (Residue/MRL 24.3 Total (Residue/MRL 20.4 Grapefruit (America) Lemon (Chile) Pesticide Residue MRL ( ) Pesticide Residue MRL ( ) Imazalil Imazalil Imazalil met Imazalil met Thiabendazole Thiabendazole o-phenylphenol Diphenylamine 0.02 Azoxystrobin 0.05 Metalaxyl Chlorpyrifos Chlorpyrifos Ethion Total (Residue/MRL 81.5 Total (Residue/MRL 35.3 Date of test year, month Standards for Withholding Registration of Pesticides on Crop Residues are represented in Italic letter, and others are Pesticide Residues Standards ( mg/g). Residue (mg/g) / MRL (mg/g) ( ) Tr. indicates trace level residue ( mg/g) was detected.

13 December Table 9. Pesticide Residues Suggestive of Unregistered Application Commodity (Date of test year, month) Pesticide Residue (mg/g) MRL 1 Carrot (domestic) ( ) Acephate 0.15 Methamidophos 0.06 Corn (domestic) ( ) Acephate Tr Methamidophos 0.02 Fig (domestic) ( ) Acephate Tr. 1.0 Methamidophos Chingensai (domestic) ( ) Oxadixyl 0.02 Garland chrysanthemum (domestic) ( ) Carbendazim 0.02 Baby kidney bean (domestic) ( ) Methomyl 1.0 Tomato (domestic) ( ) Methomyl Pesticide Residues Standards (mg/g) in Food Sanitation Law 2 Tr. indicates trace level residue ( mg/g) was detected. Table 10. Pesticide Residues PotentiallyViolating the New Positive List Legislation Commodity (Date of test year, month) Pesticide Residue (mg/g) MRL 1 Carrot (domestic) ( ) Acephate Methamidophos Orange (New Zealand) ( ) Diazinon Lemon (Chile) ( ) Diphenylamine Broccoli (America) ( ) Oxaziclomefon Okra (Thailand) ( ) EPN Baby kidney bean, frozen (Thailand) ( ) Cyproconazole Baby kidney bean, frozen (China) ( ) Fenpropathrin Breen Soybean, frozen (Taiwan) ( ) Chlorfenapyr Breen Soybean, frozen (China) ( ) Chlorfenapyr Komatsuna, frozen (China) ( ) Fipronil Welsh onion, frozen (China) ( ) Paclobutrazol Fenpropathrin The Final Draft of Provisional Maximum Residue Limits (mg/g) in Food Sanitation Law The uniform level set as the level having no potential to cause damage to human health mg/g ADI 0.6 mg/kg/day 0.05 mg/g mg/g 1.0 mg/g Table Table 9 6. (0.01 mg/g) Table )

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