Index 1 Residual Pesticides 3 Food Additives 4 Others 2 Veterinary Drugs (Antibiotics and Synthetic Antibacterials) 5 Reference Materials

Transcription

1 C9-E7A

2 Index Residual Pesticides. Analysis of 4 Pesticides With Capillary GC-FTD and GC-ECD () - GC Analysis of 4 Pesticides With Capillary GC-FTD and GC-ECD () - GC Analysis of 4 Pesticides With Capillary GC-FTD and GC-ECD (3) - GC 3 Analysis of 4 Pesticides With Capillary GC-FTD and GC-ECD (4) - GC 4 Analysis of 4 Pesticides With Capillary GC-FTD and GC-ECD (5) - GC 5 Analysis of 4 Pesticides With Capillary GC-FTD and GC-ECD (6) - GC 6 Analysis of 4 Pesticides With Capillary GC-FTD and GC-ECD (7) - GC 7 Analysis of 4 Pesticides With Capillary GC-FTD and GC-ECD (8) - GC 8. Analysis of rganophosphorus Pesticide Residue in Agricultural Products () - GC 9 Analysis of rganophosphorus Pesticide Residue in Agricultural Products () - GC. 3 Analysis of rganophosphorus Pesticide Residue in Agricultural Products () - GC Analysis of rganophosphorus Pesticide Residue in Agricultural Products () - GC. 4 Analysis of rganonitrogen and Pyrethroid Pesticide Residue in Agricultural Products () - GC 3 Analysis of rganonitrogen and Pyrethroid Pesticide Residue in Agricultural Products () - GC 4. 5 Analysis of Phoxim in Agricultural Products Using Short Capillary Column - GC 5. 6 Simultaneous Analysis of Pesticides () - GC/MS 6 Simultaneous Analysis of Pesticides () - GC/MS 7. 7 Analysis of Pesticides Using NCI () - GC/MS 8 Analysis of Pesticides Using NCI () - GC/MS 9. 8 Analysis of Residual Pesticides in Food Products Using GC/MS (part ) () - GC/MS Analysis of Residual Pesticides in Food Products Using GC/MS (part ) () - GC/MS. 9 Analysis of Residual Pesticides in Food Products Using GC/MS (part ) () - GC/MS Analysis of Residual Pesticides in Food Products Using GC/MS (part ) () - GC/MS 3. Analysis of Pesticide Residue in Vegetable Juice Using GC/MS () - GC/MS 4 Analysis of Pesticide Residue in Vegetable Juice Using GC/MS () - GC/MS 5. Analysis of Residual rganophosphorus Pesticides in Agricultural Products () - GC/MS 6 Analysis of Residual rganophosphorus Pesticides in Agricultural Products () - GC/MS 7. Analysis of Residual Pesticides in Foods Using nline GPC-GC/MS (Prep-Q) () - GC/MS 8 Analysis of Residual Pesticides in Foods Using nline GPC-GC/MS (Prep-Q) () - GC/MS 9. 3 Analysis of Regulated Pesticides in Foods () - LC 3 Analysis of Regulated Pesticides in Foods () - LC 3. 4 GPC Clean-up Method Used in the Analysis of Pesticide Residue in Foods () - LC 3 GPC Clean-up Method Used in the Analysis of Pesticide Residue in Foods () - LC Analysis of Carbamate Pesticides - LC Analysis of Imazalil in ranges - LC Analysis of Pesticide Residue in Agricultural Products Using LC/MS () - LC/MS 36 Analysis of Pesticide Residue in Agricultural Products Using LC/MS () - LC/MS Analysis of N-methylcarbamate Pesticides Using LC/MS () - LC/MS 38 Analysis of N-methylcarbamate Pesticides Using LC/MS () - LC/MS Analysis of Metribuzin Using Positive and Negative Ion Atmospheric Pressure Chemical Ionization () - LC/MS 4 Analysis of Metribuzin Using Positive and Negative Ion Atmospheric Pressure Chemical Ionization () - LC/MS 4. Analysis of Phenoxypropionic-acid Herbicides Using LC/MS () - LC/MS 4 Analysis of Phenoxypropionic-acid Herbicides Using LC/MS () - LC/MS 43 Veterinary Drugs (Antibiotics and Synthetic Antibacterials). Analysis of Antibiotics and Synthetic Antibacterial Agents in Livestock and Farm-raised Fish () - LC 44 Analysis of Antibiotics and Synthetic Antibacterial Agents in Livestock and Farm-raised Fish () - LC 45. Analysis of xytetracycline - LC Analysis of laguindox in Mixed Feed - LC Analysis of Lasalocid in Mixed Feed - LC Analysis of Polyether Antibiotics in Animal Feeds () - LC 49 Analysis of Polyether Antibiotics in Animal Feeds () - LC 5. 6 Analysis of Spiramycin - LC 5. 7 Simultaneous Analysis of Synthetic Antibacterial Agents () - LC 5 Simultaneous Analysis of Synthetic Antibacterial Agents () - LC 5. 8 Analysis of Sulfamethazine in Pork - LC Analysis of New Quinolone Antibacterial Agents in Poultry - LC 54. Analysis of Synthetic Antibacterial Agents () - LC/MS 55 Analysis of Synthetic Antibacterial Agents () - LC/MS 56. Analysis of New Quinolone Antibacterial Agents in Poultry - LC/MS 57. Analysis of Aminoglycoside Antibiotics () - LC/MS 58 Analysis of Aminoglycoside Antibiotics () - LC/MS Analysis of Flubendazole - LC 6. 4 Analysis of Closantel - LC 6. 5 Analysis of Isometamidium - LC 6. 6 Analysis of Triclabendazole - LC 6. 7 Analysis of Ivermectin and Moxidectin - LC 6. 8 Analysis of Ivermectin like Compounds (antiparasitic agents) () - LC/MS 63 Analysis of Ivermectin like Compounds (antiparasitic agents) () - LC/MS Analysis of Antiparasitic Agents () - LC/MS 65 Analysis of Antiparasitic Agents () - LC/MS 66. Analysis of Zeranol - LC 67. Analysis of Hormone Agents () - LC/MS 68 Analysis of Hormone Agents () - LC/MS 69 3 Food Additives 3. Analysis of p-hydroxybenzoates in Soy Sauce - LC 7 3. Analysis of Sorbic Acid in Ham - LC Propionic Acid in Cookies and Bread - GC Sorbic Acid, Dehydroacetic Acid and Benzoic Acid - GC Analysis of Preservatives in Food Products with Absorption Photometry () - UV 74 Analysis of Preservatives in Food Products with Absorption Photometry () - UV Analysis of Imazalil Contained in ranges - LC Analysis of Thiabendazole - GC Analysis of EDTA in Mayonnaise - LC Analysis of Cooking ils - LC Analysis of Antioxidant - GC Analysis of FDA-Regulated Antioxidants - GC Analysis of Tocopherol - GC Analysis of Phenol Antioxidant in Foods - LC Analysis of Sweetener in Soft Drink - LC Analysis of Saccharin in Pickles - LC Analysis of Acesulfame K - LC Saccharine and Sodium Saccharine - GC Simultaneous Analysis of Water-soluble Tar Pigments - LC Analysis of synthetic coloring agents in Japanese Fukushinzuke pickles, pickled radish and candy - LC Analysis of Blue # in candy - LC Analysis of curcumin - LC Analysis of Flavonoid Pigments - LC Analysis of Betanin - LC Analysis of Food Fragrances - GC Analysis of Standard Fragrance Sample () - GC 9 Analysis of Standard Fragrance Sample () - GC Essential il (Headspace Analysis) - GC Essential il (Direct Analysis) - GC Analysis of Fragrant Material () - GC/MS 94 Analysis of Fragrant Material () - GC/MS 95 Analysis of Fragrant Material (3) - GC/MS Analysis of Potassium Bromate Contained in Bread - LC Ethylene Glycols in Wine - GC Analysis of Propylene Glycol and ther Substances - GC 99 4 thers 4. Analysis of Shellfish Toxins () - LC Analysis of Shellfish Toxins () - LC 4. Analysis of Fumonisin in Sweet Corn () - LC Analysis of Fumonisin in Sweet Corn () - LC Analysis of Aflatoxins () - LC 4 Analysis of Aflatoxins () - LC 5 Analysis of Aflatoxins (3) - LC Analysis of Aflatoxins Using LC/MS () - LC/MS 7 Analysis of Aflatoxins Using LC/MS () - LC/MS Analysis of Patulin Using LC/MS - LC/MS Analysis of rganotin Compounds Using Capillary GC-FPD - GC 4. 7 Analysis of Carbon Tetrachloride Contained in Margarine - GC 4. 8 Analysis of Nitrosamines - GC 4. 9 Analysis of Alkyl Mercury Compounds () - GC Analysis of Alkyl Mercury Compounds () - GC 3 4. Analysis of rganotin in Fish () - GC/MS 4 Analysis of rganotin in Fish () - GC/MS 5 4. Analysis of 3-MCPD in Soy Sauce () - GC/MS 6 Analysis of 3-MCPD in Soy Sauce () - GC/MS 7 4. Analysis of Pb in Milk Using Atomic Absorption Spectrophotometry - AA Analysis of Pb in White Sugar Using Atomic Absorption Spectrophotometry () - AA 9 Analysis of Pb in White Sugar Using Atomic Absorption Spectrophotometry () - AA 4. 4 Measurement of Metals Contained in Food Additives () - AA Measurement of Metals Contained in Food Additives () - AA 4. 5 Analysis of Inorganic Components in Canned Drink (Green Tea) () - ICP-AES 3 Analysis of Inorganic Components in Canned Drink (Green Tea) () - ICP-AES Analysis of Inorganic Components in Processed Food Products - ICP-AES Analysis of Inorganic Components in Powdered Milk () - ICP-AES 6 Analysis of Inorganic Components in Powdered Milk () - ICP-AES 7 Analysis of Inorganic Components in Powdered Milk (3) - ICP-AES Analysis of Powdered Milk Using ICPM-85 - ICP/MS Analysis of Plants Using ICPM-85 () - ICP/MS 3 Analysis of Plants Using ICPM-85 () - ICP/MS 3 Analysis of Plants Using ICPM-85 (3) - ICP/MS 3 5 Reference Materials 5. Individual and Rapid (Simultaneous) Analysis Methods for Residual Pesticides List of Analysis Methods for Regulated Residual Pesticides in Agricultural Products (fficial Methods) () 34 List of Analysis Methods for Regulated Residual Pesticides in Agricultural Products (fficial Methods) () 35 List of Analysis Methods for Regulated Residual Pesticides in Agricultural Products (fficial Methods) (3) 36 List of Analysis Methods for Regulated Residual Pesticides in Agricultural Products (fficial Methods) (4) 37 List of Analysis Methods for Regulated Residual Pesticides in Agricultural Products (fficial Methods) (5) Sample Pretreatment Example for Residual Pesticide Analysis () 39 Sample Pretreatment Example for Residual Pesticide Analysis () 4 Sample Pretreatment Example for Residual Pesticide Analysis (3) Residual Veterinary Drug Regulation Values and Analytical Methods 4

3 Residual Pesticides. Analysis of 4 Pesticides With Capillary GC-FTD and GC-ECD () - GC Explanation Gas chromatography (GC) is often employed for analyzing residues of regulated pesticides and, in particular, capillary columns are being used with increased frequency due to their high separation efficiency. This section shows examples of the separation of 4 pesticides, including pesticides with regulated residue levels using four types of capillary columns. The FTD and ECD detectors were used. The pesticides (organochlorinated, organophosphorus and nitrogen-containing) were dissolved in acetone, the mixture concentrations were adjusted to.5 to. mg/l and µl samples were injected into the GC. The analysis results from the two detectors were combined and the relative retention times with EPN as reference were tabulated (the retention time of EPN was assumed to be 3 minutes). It is difficult to simultaneously separate all 4 pesticides with one type of column. However, this relative retention time data can be utilized for screening pesticides before conducting individual analysis. DB- Separation mv 4 mv min Fig... Chromatogram for 4 Pesticides Using DB- (Full Chromatogram, FTD) mv 4 38,39, , 5 6, min Fig... Chromatogram for 4 Pesticides Using DB- (Enlarged Section, FTD) mv 4 3 4, , ,37 4 4,43 44,45 47,48, , ,6 6 65, , , , , , , min Fig...3 Chromatogram for 4 Pesticides Using DB- (Enlarged Section, FTD) min Fig...4 Chromatogram for 4 Pesticides Using DB- (Enlarged Section, FTD) Table.. Analytical Conditions Instrument Column Column temperature Carrier Gas GC-7AAFwFtE ver.3, AC-i DB- 3m.5mm I.D. df=.5µm 5 C(min)- C/min- C -5 C/min-3 C(min) He, 5kPa Detector Detector temperature Injection inlet temperature Injection method Injection volume FTD-7, ECD-7 3 C 8 C High pressure splitless (3kPa min) µl

4 . Analysis of 4 Pesticides With Capillary GC-FTD and GC-ECD () - GC mv min Fig...5 Chromatogram for 4 Pesticides Using DB- (Full Chromatogram, ECD) mv min Fig...6 Chromatogram for 4 Pesticides Using DB- (Enlarged Section, ECD) mv , ,47,49,5 4, ,55 56, ,63 65, min 7 74,75 8 8, Fig...7 Chromatogram for 4 Pesticides Using DB- (Enlarged Section, ECD) 9, mv , ,34 35, min Fig...8 Chromatogram for 4 Pesticides Using DB- (Enlarged Section, ECD) ,4 4 Peak No Table.. Relative Retention Times for 4 Pesticides Using DB- (with EPN assumed to be 3 minutes) Compound DCIP methamidophos dichlorvos EPTC propamocarb acephate butylate isoprocarb fenobucarb ethoprophos chlorpropham bendiocarb dimethipin BHC(a) cadusafos trifluralin dimethoate thiometon BHC(b) BHC(g) BHC(s) terbufos diazinon etrimfos ethiofencarb pirimicarb tefluthrin metribuzin bentazone parathion-methyl dimethenamid carbaryl tolclophos-methyl alachrol heptachlor fenitrothion Relative Retention Time Peak No. Compound Relative methiocarb dichlofluanid pirimifos-methyl dimethylvinphos(e) esprocarb thiobencarb malathion dimethylvinphos(z) fenthion aldrin parathion diethofencarb metolachlor chlorpyrifos fosthiazate- fosthiazate- captan pendimethalin chlorfenvinphos(a) heptachlor epoxide pyrifenox- chlorfenvinphos(b) phenthoate quinalphos isofenphos triadimenol chinomethionat vamidothion pyrifenox- paclobutrazol tricyclazole trichlamide fludioxonil butamifos flutolanil prothiofos Retention Time Peak No. Compound Relative Retention Time Peak No. Compound Relative Retention Time 73 myclobutanil cyhalothrin dieldrin DDE(p,p, 5.47 pyraclofos ) 5.47 acrinathrin difenzoquat methyl sulfate pretilachlor flusilazole cyproconazole endrin chlorphenapyr fensulfothion bitertanol- bitertanol- permethrin- pyridaben permethrin- inabenfide cafenstrole chlorobenzilate DDD(p,p, cyfluthrin ) DDT(o,p, cyfluthrin ) 7.4 cyfluthrin mepronil lenacil edifenphos propiconazole cyfluthrin-4 cypermethrin- cypermethrin- halfenprox propiconazole- DDT(p,p, cypermethrin ) cypermethrin captafol thenylchlor acetamiprid tebuconazole pyributicarb dicofol EPN bifenthrin tebufenpyrad furametpyr phosalone mefenacet pyriproxyfen cyhalofop-butyl cyhalothrin- amitraz fenarimol flucythrinate- flucythrinate- pyrimidifen fenvalerate- fenvalerate- fluvalinate- difenoconazole- fluvalinate- difenoconazole- pyrazoxyfen deltamethrin- deltamethrin- tralomethrin imibenconazole

5 Residual Pesticides. Analysis of 4 Pesticides With Capillary GC-FTD and GC-ECD (3) - GC DB-5 Separation Table..3 Analytical Conditions Instrument Column Column temperature Carrier Gas GC-7AAFwFtE ver.3, AC-i DB-5(3 m.5 mm I.D. df=.5µm) 5 C(min)- C/min- C -5 C/min-3 C(min) He, 5kPa Detector Detector temperature Injection inlet temperature Injection method Injection volume FTD-7, ECD-7 3 C 8 C High Pressure Splitless(3kPa, min) µl mv 5 mv ,9 3, min 5 5 min Fig...9 Chromatogram for 4 Pesticides Using DB-5 (Full Chromatogram, FTD) Fig... Chromatogram for 4 Pesticides Using DB-5 (Enlarged Section, FTD) mv 5 36,37 38,39 4, ,46 47,48 49, , ,59 6,6, ,66, , , ,94 95 mv , , , , min min Fig... Chromatogram for 4 Pesticides Using DB-5 (Enlarged Section, FTD) Fig... Chromatogram for 4 Pesticides Using DB-5 (Enlarged Section, FTD) 3

6 . Analysis of 4 Pesticides With Capillary GC-FTD and GC-ECD (4) - GC mv 4 mv , ,3 4,5 3 8, min Fig...3 Chromatogram for 4 Pesticides Using DB-5 (Full Chromatogram, ECD) 5 min Fig...4 Chromatogram for 4 Pesticides Using DB-5 (Enlarged Section, ECD) mv 4 4 4,4 43, , ,54,55 56, ,6, ,74, , mv , , , ,39 4,4 4 Peak No min Fig...5 Chromatogram for 4 Pesticides Using DB-5 (Enlarged Section, ECD) Compound DCIP methamidophos dichlorvos EPTC propamocarb butylate acephate isoprocarb fenobucarb ethoprophos chlorpropham bendiocarb trifluralin cadusafos BHC(a) thiometon dimethoate dimethipin BHC(b) BHC(g) terbufos diazinon BHC(d) tefluthrin etrimfos ethiofencarb pirimicarb dimethenamid metribuzin bentazone parathion-methyl tolclophos-methyl carbaryl heptachlor alachrol fenitrothion Relative Retention Time Peak No. Compound Relative methiocarb esprocarb pirimifos-methyl dimethylvinphos(e) dichlofluanid thiobencarb malathion aldrin metolachlor diethofencarb dimethylvinphos(z) fenthion parathion chlorpyrifos fosthiazate- fosthiazate- chlorfenvinphos(a) heptachlor epoxide pendimethalin pyrifenox- captan isofenphos chlorfenvinphos(b) phenthoate triadimenol quinalphos chinomethionat paclobutrazol pyrifenox- vamidothion trichlamide butamifos flutolanil tricyclazole prothiofos fludioxonil Fig...6 Chromatogram for 4 Pesticides Using DB-5 (Enlarged Section, ECD) Table..4 Relative Retention Times for 4 Pesticides Using DB-5 (with EPN assumed to be 3 minutes) 3 Retention Time Peak No. Compound Relative 73 pretilachlor 74 dieldrin 75 DDE(p,p') 76 difenzoquat methyl sulfate 77 myclobutanil 78 flusilazole 79 cyproconazole- 8 cyproconazole- 8 endrin 8 chlorphenapyr 83 chlorobenzilate 84 fensulfothion 85 DDD(p,p') 86 DDT(o,p') 87 mepronil 88 lenacil 89 edifenphos 9 propiconazole- 9 DDT(p,p') 9 propiconazole- 93 tebuconazole 94 thenylchlor 95 captafol 96 pyributicarb 97 acetamiprid 98 EPN 99 bifenthrin dicofol tebufenpyrad furametpyr 3 phosalone 4 pyriproxyfen 5 mefenacet 6 cyhalofop-butyl 7 cyhalothrin- 35 Retention Time Peak No. Compound Relative Retention Time amitraz cyhalothrin- fenarimol acrinathrin pyraclofos bitertanol- bitertanol- permethrin- permethrin- pyridaben inabenfide cafenstrole cyfluthrin- cyfluthrin- cyfluthrin-3 cyfluthrin-4 cypermethrin- halfenprox cypermethrin- cypermethrin-3 cypermethrin-4 flucythrinate- flucythrinate- pyrimidifen fenvalerate- fenvalerate- fluvalinate- fluvalinate- difenoconazole- difenoconazole- deltamethrin- pyrazoxyfen deltamethrin- tralomethrin imibenconazole min 4

7 Residual Pesticides. Analysis of 4 Pesticides With Capillary GC-FTD and GC-ECD (5) - GC DB-3 Separation Table..5 Analytical Conditions Instrument Column Column temperature Carrier Gas GC-7AAFwFtE ver.3, AC-i DB-3 (3m.5mm I.D. df=.5µm) 5 C(min)- C/min- C -5 C/min-8 C(5min) He, 5kPa Detector Detector temperature Injection inlet temperature Injection method Injection volume FTD-7, ECD-7 3 C 8 C High Pressure Splitless (3kPa, min) µl mv mv , , 3 4 min Fig...7 Chromatogram for 4 Pesticides Using DB-3 (Full Chromatogram, FTD) 5 5 min Fig...8 Chromatogram for 4 Pesticides Using DB-3 (Enlarged Section, FTD) mv mv , , ,39 4,4, ,45,46 47, , , ,6 6 64, , , , , ,4 5, , 3 4, ,36 37,38 39, min Fig...9 Chromatogram for 4 Pesticides Using DB-3 (Enlarged Section, FTD) min Fig... Chromatogram for 4 Pesticides Using DB-3 (Enlarged Section, FTD) 5

8 . Analysis of 4 Pesticides With Capillary GC-FTD and GC-ECD (6) - GC mv 5 mv min 5 5 min Fig... Chromatogram for 4 Pesticides Using DB-3 (Full Chromatogram, ECD) Fig... Chromatogram for 4 Pesticides Using DB-3 (Enlarged Section, ECD) mv ,35, ,4 44, ,54 55,56 57,58,59 6, ,65 66, , , ,8, mv mv 5 5 3, , 3 4, ,36 37,38 39, min min Fig...3 Chromatogram for 4 Pesticides Using DB-3 (Enlarged Section, ECD) Peak No. Compound DCIP dichlorvos methamidophos EPTC propamocarb butylate acephate isoprocarb ethoprophos fenobucarb chlorpropham cadusafos trifluralin bendiocarb BHC(a) thiometon terbufos BHC(g) diazinon dimethoate tefluthrin etrimfos dimethipin pirimicarb heptachlor BHC(b) dimethenamid ethiofencarb tolclophos-methyl metribuzin bentazone alachrol esprocarb BHC(d) aldrin parathion-methyl Relative Retention Time Peak No. Compound Relative pirimifos-methyl thiobencarb carbaryl chlorpyrifos methiocarb dimethylvinphos(e) fenitrothion dichlofluanid malathion fenthion metolachlor diethofencarb dimethylvinphos(z) parathion heptachlor epoxide pyrifenox- chlorfenvinphos(a) pendimethalin fosthiazate fosthiazate quinalphos chinomethionat isofenphos chlorfenvinphos(b) phenthoate pyrifenox- captan triadimenol trichlamide prothiofos DDE(p,p') dieldrin paclobutrazol butamifos pretilachlor.575 Fig...4 Chromatogram for 4 Pesticides Using DB-3 (Enlarged Section, ECD) Table..6 Relative Retention Times for 4 Pesticides Using DB-3 (with EPN assumed to be 3 minutes) Retention Time Peak No. Compound Relative difenzoquat methyl sulfate vamidothion endrin flutolanil DDT(o,p') flusilazole chlorobenzilate myclobutanil DDD(p,p') dicofol tricyclazole cyproconazole chlorfenapyr fensulfothion DDT(p,p') edifenphos mepronil fludioxonil propiconazole- propiconazole- thenylchlor pyributicarb lenacil captafol bifenthrin tebuconazole tebufenpyrad EPN pyriproxyfen furametpyr amitraz phosalone cyhalothrin- mefenacet cyhalofop-butyl Retention Time Peak No. Compound Relative 7 cyhalothrin- 8 acrinathrin 9 fenarimol permethrin- pyraclofos permethrin- 3 acetamiprid 4 pyridaben 5 bitertanol- 6 inabenfide 7 bitertanol- 8 halfenprox 9 cyfluthrin- cyfluthrin- cyfluthrin-3 cypermethrin- 3 cyfluthrin-4 4 cafenstrole 5 cypermethrin- 6 cypermethrin-3 7 cypermethrin-4 8 flucythrinate- 9 pyrimidifen 3 flucythrinate- 3 fenvalerate- 3 fenvalerate- 33 fluvalinate- 34 difenoconazole- 35 difenoconazole- 36 fluvalinate- 37 deltamethrin- 38 pyrazoxyfen 39 deltamethrin- 4 tralomethrin 4 imibenconazole Retention Time

9 Residual Pesticides. Analysis of 4 Pesticides With Capillary GC-FTD and GC-ECD (7) - GC DB-7 Separation Instrument Column Column temperature Carrier Gas GC-7AAFwFtE ver.3, AC-i DB-7(3m.5mm I.D. df=.5µm) 5 C(min)- C/min - C - 5 C/min-8 C(5min) He, 5kPa-5kPa/min-35kPa Table..7 Analytical Conditions Detector Detector temperature Injection inlet temperature Injection method Injection volume FTD-7, ECD-7 3 C 8 C High Pressure Splitless (3kPa, min) µl mv mv min Fig...5 Chromatogram for 4 Pesticides Using DB-7 (Full Chromatogram, FTD) 5 5 min Fig...6 Chromatogram for 4 Pesticides Using DB-7 (Enlarged Section, FTD) mv 9 34,36,37,38 6,63,64,65 74,, mv, ,3, ,43, , , , , , ,89 9,9 93,94 95,96 97, , , , , min Fig...7 Chromatogram for 4 Pesticides Using DB-7 (Enlarged Section, FTD) min Fig...8 Chromatogram for 4 Pesticides Using DB-7 (Enlarged Section, FTD) 7

10 . Analysis of 4 Pesticides With Capillary GC-FTD and GC-ECD (8) - GC mv min Fig...9 Chromatogram for 4 Pesticides Using DB-7 (Full Chromatogram, ECD) mv 68,69 3 mv min Fig...3 Chromatogram for 4 Pesticides Using DB-7 (Enlarged Section, ECD) 9, 5 8 mv 5 6,7 3, ,35,37, , , , , ,63,64 65,66, ,77, , , ,99,, ,, 3, ,3, , , Peak No Fig...3 Chromatogram for 4 Pesticides Using DB-7 (Enlarged Section, ECD) Compound DCIP dichlorvos EPTC methamidophos butylate propamocarb acephate trifluralin isoprocarb fenobucarb chlorpropham ethoprophos cadusafos tefluthrin BHC(a) thiometon terbufos bendiocarb diazinon BHC(g) BHC(b) etrimfos dimethoate heptachlor BHC(s) dimethenamid tolclophos-methyl aldrin pirimicarb ethiofencarb parathion-methyl esprocarb alachrol metribuzin dimethipin min Relative Retention Time Peak No. Compound Relative pirimifos-methyl metolachlor bentazone diethofencarb chlorpyrifos thiobencarb parathion fenitrothion dimethylvinphos(e) malathion carbaryl dichlofluanid methiocarb pendimethalin heptachlor epoxide fenthion dimethylvinphos(z) chlorfenvinphos(a) triadimenol trichlamide isofenphos chlorfenvinphos(b) paclobutrazol pyrifenox- quinalphos pretilachlor prothiofos pyrifenox- chinomethionat fosthiazate phenthoate fosthiazate DDE(p,p ) dieldrin butamifos Fig...3 Chromatogram for 4 Pesticides Using DB-7 (Enlarged Section, ECD) Table..8 Relative Retention Times for 4 Pesticides Using DB-7 (with EPN assumed to be 3 minutes) Retention Time Peak No. Compound Relative 7 flutoluanil 7 captan 73 chlorphenapyr 74 flusilazole 75 chlorobenzilate 76 myclobutanil 77 endrin 78 cyproconazole 79 cyproconazole 8 difenzoquat methyl sulfate 8 vamidothion 8 DDT(o,p ) 83 DDD(p,p ) 84 fludioxonil 85 DDT(p,p ) 86 mepronil 87 propiconazole- 88 propiconazole- 89 fensulfothion 9 tricyclazole 9 tebuconazole 9 bifenthrin 93 tebufenpyrad 94 edifenphos 95 acrinathrin 96 thenylchlor 97 pyributicarb 98 lenacil 99 cyhalothrin- cyhalothrin- captafol EPN 3 amitraz 4 cyhalofop-butyl min Retention Time Peak No. Compound Relative Retention Time furametpyr phosalone pyriproxyfen fenarimol bitertanol- permethrin- acetamiprid pyraclofos permethrin- pyridaben bitertanol- mefenacet cyfluthrin- cyfluthrin- cyfluthrin-3 halfenprox cypermethrin- cypermethrin- inabenfide flucythrinate- cypermethrin-3 flucythrinate- cafenstrole fluvalinate- fluvalinate- pyrimidifen fenvalerate- fenvalerate- deltamethrin- deltamethrin- tralomethrin difenoconazole pyrazoxyfen imibenconazole

11 Residual Pesticides. Analysis of rganophosphorus Pesticide Residue in Agricultural Products () - GC Analysis Based on Standards for Foods and Additives Specified in Japan's Food Sanitation Law (Notice 37 Issued by Japan's Ministry of Health,Labour and Welfare) Explanation As a result of the diversification of foods and improvements in the ways foods are transported and stored, a wide variety of food products are imported from all over the world and eaten as part of our daily diet. There are, however, many reported cases of excessive levels of pesticide residue being found in imported foods, particularly imported vegetables, and the safety of imported vegetables has become an issue of some concern. The analysis of organophosphorus pesticide based on the standards for foods and additives specified in Japan's Food Sanitation Law (Japan's Ministry of Health,Labour and Welfare Notice 37, D, item (6)) is described here as an example. The analysis method varies with the sample; samples are categorized into three groups that each have different analysis methods fruits, vegetables, green powdered tea, and hops; grain, beans, nuts, and seeds; and teas other than green powdered tea. The sample processing methods for the first two groups are described below. Pretreatment (Fruits, vegetables, green powdered tea, and hops) (Grain, beans, nuts, and seeds) Sample Extraction Purification Quantitative analysis (Fruits, vegetables, green powdered tea, or hops) Approx. kg of sample homogenized g of sample weighed out Addition of ml of acetone; homogenization for 3min; suction filtration through layer of diatomaceous earth Homogenization of residue and 5mL of acetone; suction filtration; vacuum concentration at 4 C max. 3mL separating funnel; ml of saturated NaCl solution Extracted twice with 4-mixture of ethyl acetate and n-hexane solution (first time ml; second time 5mL) Dehydration of organic solvent layer; vacuum concentration at 4 C max. Residue dissolved with mixture of acetone and n-hexane (approx. 5mL) Column tube of inner diameter 5mm and length 3mm filled with 5g of silica gel and 5g of NaS4 Extract injected Elution with ml mixture of acetone and n-hexane () Vacuum concentration of eluate at 4ºC max.; acetone added to residue to make 5mL solution GC-FTD, FPD Sample Extraction Degreasing Purification Quantitative analysis (Grain, beans, nuts, or seeds) Pulverization; 4µm standard sieve g; ml of water; left for hours Addition of ml of acetone; homogenization for 3min; suction filtration through layer of diatomaceous earth Homogenization of residue and 5mL of acetone; suction filtration; vacuum concentration at 4 C max. 3mL separating funnel; ml of saturated NaCl solution Extracted twice with 4 mixture of ethyl acetate and n-hexane solution (first time ml; second time 5mL) Dehydration of organic solvent layer; removal of organic solvent at 4 C max. ml of n-hexane added to residue ml separating funnel; 3mL of n-hexane saturated with acetonitrile; shaken for 5min; extracted another times (3 times in total) Vacuum concentration of acetonitrile layer at 4 C max. Residue dissolved with a -mixture of acetone and n-hexane (approx. 5mL) Column tube of inner diameter 5mm and length 3mm filled with 5g of silica gel and 5g of NaS4 Extract injected Elution with ml mixture of acetone and n-hexane () Vacuum concentration of eluate at 4 C max.; acetone added to residue to make 5mL solution GC-FTD, FPD 9

12 . Analysis of rganophosphorus Pesticide Residue in Agricultural Products () - GC Fig... shows a chromatogram of mg/l standard organophosphorus pesticide solution. Analysis was performed after adding standard organophosphorus pesticide solution. Fig... to..4 show the chromatograms of apples, spinach, and soybeans. µv (x,) Peaks DDVP 6 MEP Dimethoate 7 Malathion 3 Diazinon 8 Chlorpyrifos 4 IBP 9 Prothiofos 5 Parathion-methyl EPN each mg/l µv (,) min min Fig... Chromatogram of standard organophosphorus pesticide solution (mg/l) Fig... Chromatogram of apples (.5µg/g standard pesticide solution added) µv (,) µv (,) min min Fig...3 Chromatogram of spinach (.5µg/g standard pesticide solution added) Fig...4 Chromatogram of soybeans (µg/g standard pesticide solution added) Analytical Conditions Instrument GC-AF, FPD-, AC-i Column Rtx- (5m.53mm I.D., df =.5µm) Column Temp. 8 C(min)-8 C/min-5 C(5min) Carrier Gas He, 46kPa (6.5mL/min, cm/s, constant-velocity mode) Detector FPD- (P Filter) Inj. Temp. 3 C Det. Temp 8 C Injection method Splitless (min) Injection volume µl

13 Residual Pesticides.3 Analysis of rganophosphorus Pesticide Residue in Agricultural Products () - GC Analysis Based on the Rapid Analysis Method Specified in Japan's Food Sanitation Law (Notices 43, 44, and 45 Issued by the Environmental Health Bureau's Food Chemistry Division in 997) Explanation In 997, Japan's Ministry of Health, Labour and Welfare issued notification of a pesticide-residue rapid analysis method as a simple and quick way for screening many pesticide residues. With this method, the same analysis method can be used for many different agricultural products and pesticides and some of the pretreatment operations can be automated using the GPC method. The pesticides are analyzed in groups, such as chlorine, phosphorus, and nitrogen, using GC-ECD, GC-FPD, and GC-FTD. If, however, pesticide residue with a concentration exceeding approximately 5% of the regulated value is detected using the rapid analysis method, quantitative measurement must be carried out as stipulated by the corresponding notification. The analysis of organophosphorus pesticide is described as an example. Pretreatment Extraction with acetone is carried out on the sample and, after redissolving in ethyl acetate with a diatomaceous-earth column, GPC clean-up is performed and the sample is purified with a silica-gel mini-column. rganophosphorus pesticides are analyzed with GC-FPD or GC-FTD after concentration. Carbamate pesticides are analyzed by taking a sample of the solution after performing GPC clean-up and analyzing the sample in this state or after diluting with hydrochloric acid. rganochlorine or pyrethroid pesticides are investigated by performing analysis after refining first with silica gel and then with a Florisil mini-column. Sample Extraction Vegetables, fruits, green powdered tea, hops g Grain, beans, nuts, seeds g of sample passed through 4µm standard sieve; ml of water added; left for hours ml of acetone added; homogenization and extraction for 3min; suction filtration through layer of diatomaceous earth Filtrate residue and 5mL of acetone Concentrated to ml max. at 4 C max.; 6g of NaCl added Total volume injected into diatomaceous-earth column; left for min Container used for concentration washed with 5mL of ethyl acetate; wash liquid injected into column GPC clean-up ml of extract injected into GPC clean-up apparatus Eluted with mixture of ethyl acetate and cyclohexane Separate out fraction corresponding to elution times between fluvalinate and quinomethionate Concentrated at 4 C max.; dissolved into a 4mL () mixture of acetone and hexane (extract A) Mini-column purification ml of extract A injected into silica-gel mini-column Eluted with ml of acetone and hexane () Quantitative analysis Solvent removed; 37 mixture of ether and hexane added to residue to make 4mL solution (extract B) ml of extract A collected; solvent removed; dissolved in ml of methanol; HPLC measurement (pirimicarb) Dilute hydrochloric acid added to.3ml of remaining sample to make solution of 3mL; filtration; HPLC measurement (N-methylcarbamate) HPLC (carbamates) Quantitative analysis ml of extract B collected; solvent removed; residue dissolved in acetone to make ml (ml for grain or beans) solution GC-FTD, FPD (organophosphorus, organonitrogens) Quantitative analysis ml of extract B collected; solvent removed; residue dissolved in ml (37) mixture of ether and hexane ml of extract B injected into Florisil mini-column; eluted with 8mL (37) mixture of ether and hexane; eluted with 5mL (37) mixture of acetone and hexane; each outflow liquid concentrated; residue dissolved in hexane to make ml (ml for grain or beans) solution GC-ECD (organochlorines, pyrethroids)

14 .3 Analysis of rganophosphorus Pesticide Residue in Agricultural Products () - GC µv(x,) Peaks DDVP Dimethoate 3 Diazinon 4 IBP 5 Parathion-methyl 6 MEP 7 Malathion 8 Chloropyrifos 9 Prothiofos EPN each mg/l µv(,) min min Fig..3. Chromatogram of standard organophosphorus pesticides solution (mg/l) Fig..3. Chromatogram of processed spinach liquid with.5µg/g standard pesticide solution added µv(,) µv(,) min min Fig..3.3 Chromatogram of processed soybean liquid with µg/g standard pesticide solution added Fig..3.4 Chromatogram of processed rice liquid with µg/g standard pesticide solution added [References] Handbook for Food Sanitation Laws, 3 Edition, Shinnippon-hoki Publishing Co., Ltd., () Analytical Conditions Instrument GC-AF, FPD-, AC-i Column Rtx- (5m.53mm I.D., df =.5µm) Column Temp. 8 C(min)-8 C/min-5 C(5min) Carrier Gas He, 46kPa (6.5mL/min, cm/s, constant-velocity mode) Detector FPD- (P Filter) Inj. Temp. 3 C Det. Temp. 8 C Injection method Splitless (min) Injection volume µl

15 Residual Pesticides.4 Analysis of rganonitrogen and Pyrethroid Pesticide Residue in Agricultural Products () - GC Explanation The analysis of organonitrogen and pyrethroid pesticides using the rapid analysis method is described here. Fig..4. and.4. show chromatograms of standard organophosphorus and standard organonitrogen pesticide solutions analyzed under the same conditions. Both organophosphorus and organonitrogen pesticides can be detected with GC-FTD. Also, in the pretreatment for the rapid analysis method, both pesticides are eluted into the same fraction. Fig..4.3 shows a chromatogram of processed soy bean liquid with 3 organophosphorus and 4 organonitrogen pesticides added. Fig..4.4 shows a chromatogram of a standard pyrethroid pesticide solution. Separation and quantitative analysis can be difficult for pyrethroid pesticides as there are often many isomers within a standard product. Consideration is also required for substances that convert their forms at the GC injector inlet (for example, deltamethrin changes to tralomethrin). Fig..4.5 shows a chromatogram of processed spinach liquid with a standard pyrethroid pesticide added. Pretreatment (Pretreatment for Pesticide-residue Rapid Analysis Method) Sample Extraction Vegetables, fruits, green powdered tea, hops g Grain, beans, nuts, seeds g of sample passed through 4µm standard sieve; ml of water added; left for hours ml of acetone added; homogenization and extraction for 3min; suction filtration through layer of diatomaceous earth Filtrate residue and 5mL of acetone Concentrated to ml max. at 4 C max.; 6g of NaCl added Total volume injected into diatomaceous-earth column; left for min Container used for concentration washed with 5mL of ethyl acetate; wash liquid injected into column Vacuum concentration at 4 C max.; dissolved in 4mL () mixture of ethyl acetate and cyclohexane GPC clean-up ml of extract injected into GPC clean-up apparatus Eluted with mixture of ethyl acetate and cyclohexane Separate out fraction corresponding to elution times between fluvalinate and quinomethionate Concentrated at 4 C max.; dissolved into a 4mL () mixture of acetone and hexane (extract A) Mini-column purification ml of extract A injected into silica-gel mini-column Eluted with ml of acetone and hexane () Quantitative analysis After removal of solvent; 37 mixture of ether and hexane added to residue to make 4mL solution (extract B) ml of extract A collected; solvent removed; dissolved in ml of methanol; HPLC measurement (pirimicarb) Dilute hydrochloric acid added to.3ml of remaining sample to make solution of 3mL; filtration; HPLC measurement (N-methylcarbamate) HPLC (carbamates) Quantitative analysis ml of extract B collected; solvent removed; residue dissolved in acetone to make ml (ml for grain or beans) solution GC-FTD, FPD (organophosphorus, organonitrogens) Quantitative analysis ml of extract B injected into Florisil mini-column; eluted with 8mL (37) mixture of ether and hexane (first fraction); eluted with 5mL (37) mixture of acetone and hexane (second fraction); each outflow liquid concentrated; residue dissolved in hexane to make ml (ml for grain or beans) solution GC-ECD (organochlorines, pyrethroids) 3

16 .4 Analysis of rganonitrogen and Pyrethroid Pesticide Residue in Agricultural Products () - GC µv (x,) 4. P DDVP P Ethoprophos 3.5 P3 Dimethoate P4 Diazinon P5 IBP 3. P6 Parathion-methyl P7 Pirimiphos-methyl P8 MEP.5 P9 Malathion P Chlorpyrifos P Parathion P. P Prothiofos P3 EPN.5 P P3 P4 P7 P9 P P8 P5 P6 P P P3 µv (x,). N Isoprocarb 9. N Alachrol N3 Diethofencarb N4 Paclobutrazol 8. N5 Flutolanil N6 Pretilachlor 7. N7 Mepronil N8 Lenacil N9 Thenylchlor 6. N Tebufenpyrad N Pyriproxyfen 5. N Mefenacet N3 Fenarimol N4 Bitertanol 4. N5 Bitertanol N N4 N N N3 N5 N6 N8 N9 N7 N N3 N4 N N min min Fig..4. Chromatogram of standard organophosphorus pesticides solution obtained using GC-FTD Fig..4. Chromatogram of standard organonitrogen pesticides solution obtained using GC-FTD µv (x,) P N P P3 P9 P7 P4 P5 N3+P P8 P6 P N6+P N5 N4 N N7 N8 N9 P3 N N N3 N4 N N5 µv (x,,).5 Pyrethrine Pyrethrine 3 Pyrethrine 3 4 Pyrethrine 4. 5 Bifenthrin 6 Pyrethrine 5 7 Cyhalothrin 8 Acrinathrin 9 Cyhalothrin.75 Acrinathrin Acrinathrin 3 Acrinathrin 4 3 Permethrin 4 Permethrin.5 5 Cyfruthrin 6 Cyfruthrin.5. 7 Cypermethrin 8 Cypermethrin 9 Flucythrinate Flucythrinate Fenbalerate Fenbalerate 3 Fluvalinate 4 Tralomethrin 5 Deltamethrin 6 Tralomethrin 7 Deltamethrin (5) 6(7) min Fig..4.3 Chromatogram of processed soy bean solution obtained using GC-FTD (3 organophosphorus and 4 organonitrogen pesticides. to.5µg/g added) µv (x,) min Fig..4.5 Chromatogram of processed spinach liquid obtained using GC-ECD (first fraction, µg/g pesticide added) 8 9 4(5) 3 6(7) min Fig..4.4 Chromatogram of standard pyrethroid pesticides solution obtained using GC-ECD (mg/l) Analytical Conditions Instrument GC-AF, FPD-, AC-i, GCsolution Column BPX5 (3m.5mm I.D., df =.5µm) Column Temp. 8 C(min)- C/min-9 C-5 C/min-8 C(5min) Carrier Gas He, 43kPa (.4mL/min, 45cm/s, constant-velocity mode) Detector FTD- Inj. Temp. 5 C Det. Temp. 8 C Injection method High-pressure, splitless (3kPa, min) Injection volume µl Analytical Conditions Instrument GC-7A, ECD-7, AC-i, GCsolution Column ZB- (3m.5mm I.D., df =.5µm) Column Temp. 5 C(min)-5 C/min-75 C- C/min-3 C(4min) Carrier Gas He, 5kPa (.7mL/min, constant-pressure mode) Detector ECD-7 Inj. Temp. 8 C Det. Temp. 3 C Injection method High-pressure, splitless (3kPa, min) Injection volume µl 4

17 Residual Pesticides.5 Analysis of Phoxim in Agricultural Products Using Short Capillary Column - GC Explanation Phoxim is an organophosphorus insecticide that has a wide range of effects. It is also known, however, to decompose easily in analysis when exposed to high temperatures in, for example, the injection inlet or column. In the example presented here, a short capillary column of length 5m is used in order to minimize the level of decomposition of phoxim in GC analysis and improve the level of separation from other organophosphorus pesticides. Analysis Using the Notified Method Fig..5. shows the chromatogram obtained for a standard mixture of organophosphorus pesticides under the notified conditions for phoxim (using a wide-bore column of inner diameter.53mm and length m). The separation of pirimifos-methyl, malathion, parathion, chlorpyrifos, and phoxim is insufficient. Analysis Using Short Capillary Column Fig..5. shows the chromatogram obtained for the same standard mixture using a short capillary column of inner diameter.mm and length 5m (high-pressure splitless analysis at 35kPa). It can be seen that there is better separation for phoxim. Also, using a short column makes it possible to elute phoxim at the relatively low temperature of 3ºC and so we can expect a reduction in the level of decomposition of phoxim in the column. Fig..5.3 shows a chromatogram for soybean to which phoxim was added to a concentration of approx..4µg/g. (The concentration for other pesticides was in the range.4 to.6µg/g.) There is no significant interference from other constituents and there is good separation µv (,,) each mg/l o 3 4 mv o DDVP Ethoprophos 3 Dimethoate 4 Diazinon 5 IBP 6 Parathion-methyl 7 MEP 8 Pirimifos-methyl o Phoxim Malathion Parathion Chlorpyrifos 3 Prothiofos 4 EPN each mg/l 5 5 min Fig..5. Chromatogram for standard mixture of organophosphorus pesticides including phoxim (mg/l) 5. Table.5. Conditions for analysis using notified method Instrument Column Col.Temp. Carrier gas Detector Injection-inlet temperature Injection method Injection volume Table.5. Conditions for analysis using short capillary column Instrument Column Col.Temp. Carrier gas Detector Injection-inlet temperature Injection method Injection volume µv (,) GC-7AAF, FPD-7c, AC-i CBP- m.53mm I.D. df =.µm 5 C(min)-3 C/min-5 C(min) -3 C/min-5 C He, ml/min FPD-7c (P Mode), 8ºC 5ºC Splitless (min) µl GC-AF, FPD-, AC-i CBP- 5m.mm I.D. df =.5µm 6ºC (min) - 3ºC/min - 3ºC (min) - 3ºC/min - 5ºC He, 5kPa (.8mL/min) FPD- (P Mode) 8ºC 5ºC High-pressure splitless (35kPa, min) µl min Fig..5. Chromatogram for standard mixture of organophosphorus pesticides including phoxim (mg/l). 8 o min Fig..5.3 Chromatogram for processed soybean solution to which organophosphorus pesticides including phoxim have been added (phoxim.4µg/g; other pesticides.4 to.6µg/g) 5

18 .6 Simultaneous Analysis of Pesticides () - GC/MS Explanation Residual Pesticides on vegetables and fruits are a matter of concern. There are various kinds of pesticides used, among which approximately 4 are subjected to regulations in Japan. A good way of analyzing these pesticides is simultaneous GC/MS measurement. Here, an example of a simultaneous analysis of 86 pesticides using GC/MS is shown. Analytical Conditions Instrument Column Col.Temp. Inj.Temp. I/F Temp. Carrier Gas GCMS-QP5 DB- 3m.5mmI.D. df=.5µm 5 C(min)- C/min-3 C -3 C/min-3 C(7min) 8 C 8 C He kpa(min)-kpa/min-5kpa Table.6. List of pesticides and molecular weights Component Molecular weight Component Molecular weight Methamidophos 4 44 Chinomethionat 34 Dichlorvos 45 β-chlorfenvinphos Propamocarb Quinalphos 98 4 Acephate Phenthoate 3 5 Isoprocarb Triadimenol 95 6 Fenobucarb 7 49 Vamidothion 87 7 Ethoprophos 4 5 Trichlamide Chlorproham 3 5 Methoprene 3 9 Bendaiocarb 3 5 Flutolanil 33 Dimethipin 53 Dieldrin 378 α-bhc Prothiofos 344 Dimethoate 9 55 Myclobutanil 88 3 Thiometon p,p'-dde 36 4 β-bhc Pretilachlor 3 5 γ-bhc Endrin σ-bhc Fensulfothion 38 7 Terbufos 88 6 Chlorobenzilate 34 8 Diazinon 34 6 p,p'-ddd 38 9 Ethiofencarb 5 6 o,p'-ddt 35 Etrimfos 9 63 Mepronil 69 Pirimicarb Lenacil 34 Metribuzin 4 65 Edifenphos 3 3 Bentazone Captafol Parathion-methyl p,p'-ddt 35 5 Carbaryl 68 Propiconazole 34 6 Heptachlor EPN 33 7 Fenitrothion 77 7 Dicofol 37 8 Methiocarb 5 7 Phosalone Dichlofluanid 33 7 Mefenacet 98 3 Esprocarb Amitraz 93 3 Pirimifos-methyl Cyhalothrin Thiobencarb Bitertanol Malathion Pyridaben Aldrin Inabenfide Fenthion Permethrin Parathion 9 79 Cyfluthrin Chlorpyrifos Cypermethrin Diethofencarb 67 8 Flucythrinate Captan 99 8 Fenvalerate 49 4 Heptachlor epoxide Fluvalinate 5 4 Pendimethalin 8 84 Pyrazoxyfen α-chlorfenvinphos Deltamethrin Pyrifenox Tralomethrin 66 6

19 Residual Pesticides.6 Simultaneous Analysis of Pesticides () - GC/MS TIC Fig..6. Analysis of 86 pesticides using DB- 7

20 .7 Analysis of Pesticides Using NCI () - GC/MS Explanation Trace analysis is required for the measurement of residual pesticides in vegetables and fruits, but it is difficult to extract only pesticides, even after a cleanup pretreatment. NCI is an effective method for this analysis. Generally, positive ions are detected in mass spectrometry, but negative-ion analysis may be used depending on the compound. The negative ions of such compounds allow microanalysis with minimal interference from the matrix. Trace amount of pesticides that cannot be detected using the conventional EI method can be detected by this method. Analytical Conditions Instrument Column Col.Temp. Inj.Temp. I/F Temp. Carrier Gas GCMS-QP55A DB- 3m.5mmI.D. df=.5µm 5 C(min)- C/min-3 C -3 C/min-3 C(7min) 8 C 8 C He kpa(min)-kpa/min-5kpa Cl 4,84 Cl Cl 5 Cl Cl Cl Fig..7. α-bhc mass spectrum (upper EI, lower NCI) 8