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Solution MANUAL OF METHODS OF ANALYSIS OF PESTICIDE RESIDUE IN FOODS 100% Complete and Verified

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Codex Guidelines on Good Practice in Pesticide Residue Analysis 5 2 Sample Collection 17 3 Reporting Analytical Results 23 4 Pesticide Standards 30 5 Purification of Solvents and Reagents 32 6 Extraction and Clean-Up Methods in Pesticide Residue Analysis 35 7 Multi Residue Method for Determination of Chlorinated Pesticide 43 i) Dichlorodiphenyltrichloroethane 43 ii) HCH 43 iii) Endosulphan 43 iv) Aldrin 43 v) Dieldrin 43 vi) Chlordane 43 vii) Heptachlor 43 8 Multi Residue Method for Determination of Organo-Phosphorus Pesticides 56 i) Acephate 57 ii) Chlorpyriphos 57 iii) Chlorpyriphos-methyl 57 iv) Demeton-O 57 v) Diazinon 57 vi) Dimethoate 57 vii) Ethion 57 viii) Fenitrothion 57 ix) Malaoxan 57 x) Malathion 57 xi) Mathamidophos 57 xii) Monocrotophos 57 xiii) Omethoate 57 xiv) Paraoxon 57 xv) Paraoxon-Methyl 57 xvi) Parathion 57 xvii) Parathion-Methyl 57 xviii) Phosalone 57 xix) Pirimiphos-Methyl 57 9 Multiresidue Gas Chromatography Method for Synthetic Pyrethroids 62 i) Bifenthrin 63 ii) Fenopropathrin 63 iii) Cyhalothrin 63 iv) Permethrin 63PESTICIDE RESIDUES 2016 2 v) Cypermethrin 63 vi) Fluvalinate 63 vii) Fenvalerate 63 viii) Deltamethrin 63 10 Multiresidue Method of N-Methylcarbamate Insecticides 66 i) Carbaryl 69 ii) Carbofuron 69 11 Multiple Residue Method for Fumigants 70 i) Ethylene Dibromide 70 ii) Carbon Tetrachloride 70 iii) Methyl Bromide 70 iv) Phosphine 72 12 Thiamethoxam 77 13 Thiodicarb/Methomyl 83 14 Cymoxanil 87 15 Multiresidue Gas Chromatographic Method for Determination of Organochlorine and Pyrethroid pesticides in Milk, Fish and Eggs 91 16 Acetamiprid 96 17 Imidacloprid 99 18 Pretilachlor 106 19 Isoprothiolane 110 20 Fosetyl 115 21 Propiconazole 122 22 Dithiocarbamates 126 (i) Ferbam 126 (ii) Ziram 126 (iii) Thiram 126 (iv) Maneb 126 (v)Zineb 126 (vi)Mancozab 126 (vii) Nabam 126 23 Ethylene Thiourea and Ethylene Urea 134 24 Tricyclazole 136 25 Triadimefon and Triadimenol 140 26 Metalaxyl 146 27 Triazole Fungicides 149 i) Hexaconazole 150 ii) Propiconazole 150 iii) Penconazole 150 iv) Myclobutanil 150 v) Triademifon 150 vi) Bitertanol 150 28 Chlorsulfuron and Metasulfuron 156 29 Anilophos 162 30 Diclofop-Methyl 165 31 Glufosinate 170 32 Linuron 181 33 Diquat and Paraquat 185PESTICIDE RESIDUES 2016 3 34 Atrazine and Simazine 188 35 Metribuzin 192 36 2, 4-D 196 37 Pendimethalin Analytical Methods of Pesticide Residues in Water 201 38 Organochlorine Pesticides in Water by Gas Chromatographic Method 204 i) Aldrin 204 ii) α- BHC 204 iii) β- BHC 204 iv) γ - BHC 204 v) δ - BHC 204 vi) α- chlordane 204 vii) γ - chlordane 204 viii) 4,4'- ODD 204 ix) 4,4'- DDE 204 x) 4,4'- Dichlorodiphenyltrichloroethane 204 xi) Dieldrin 204 xii) Endosulfan I 204 xiii) Endosulfan II 204 xiv) Endosulfan Sulphate 204 xv) Heptachlor 204 xvi) Heptachlor Expoxide 204 39 N-Methylcarbamoylomimes and N-Methlycarbamates in Finished Drinking Water 211 i) Aldicrab 211 ii) Aldicarb Sulfone 211 iii) Aldicarb Sulfoxide 211 iv) Baygon 211 v) Carbaryl 211 vi) Carboftiron 211 vii) 3-hydroxycarboruron 211 viii) Methiocarb 211 ix) Methomyl 211 x) Oxamyl 211 40 Determinatin of Alachlor, Atrazine and Butachlor in Water 216 41 Determination of 2,4-D in Drinking Water by Liquid-Liquid Microextraction, Derivatization, and Fast Gas Chromatography With Electron Capture Detection 226 42 Determination of Isoproturon in Water by Solid-Phase Extraction and Liquid Chromatography 233 43 Nitrogen and Phosphorus Containing Pesticides in Finished Drinking Water 234 (i) Dichlorvos 234 (ii) Phorate 234 (iii) Chlorpyrifos. Methyl 234 (iv) Chlopyrifos 234 (v) Monocrotophos 234 (vi) Dimethoate 234PESTICIDE RESIDUES 2016 4 (vii) Malathion 234 (viii) Parathion, Methyl 234 (ix) Parathion, Ethyl 234 (x) Ethion 234 (xi) Phosphamidon 234 (xii) Atrazine 234 (xiii) Simazine 234 44 Laboratory Safety 242 Note: The test methods given in the manuals are validated/ standardized test methods. However, it would be the responsibility of the respective testing laboratory to confirm that the above methods are validated in its laboratory and gives proper result in their laboratory.PESTICIDE RESIDUES 2016 5 MANUAL FOR ANALYSIS OF PESTICIDE RESIDUES 1. CODEX GUIDELINES ON GOOD PRACTICE IN PESTICIDE RESIDUE ANALYSIS 1.1 Introduction: The Codex document ALINORM 76/24 Appendix IV (Report of the ad hoc Working Group on Methods of Analysis) contained the following statement: "It was considered that the ultimate goal in fair practice in international trade depended, among other things, on the reliability of analytical results. This in turn, particularly in pesticide residue analysis, depended not only on the availability of reliable analytical methods, but also on the experience of the analyst and on the maintenance of good practice in the analysis of pesticides.

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MANUAL OF METHODS
OF ANALYSIS OF
FOODS

PESTICIDE RESIDUES




Endosulphan DDT




FOOD SAFETY AND STANDARDS AUTHORITY OF INDIA
MINISTRY OF HEALTH AND FAMILY WELFARE
GOVERNMENT OF INDIA
NEW DELHI
2016

, PESTICIDE RESIDUES 2016

MANUAL FOR ANALYSIS OF PESTICIDE RESIDUE IN FOODS

TABLE OF CONTENTS

S.No. TITLE/METHOD PAGE NO.
1 Codex Guidelines on Good Practice in Pesticide Residue Analysis 5

2 Sample Collection 17
3 Reporting Analytical Results 23
4 Pesticide Standards 30
5 Purification of Solvents and Reagents 32
6 Extraction and Clean-Up Methods in Pesticide Residue Analysis 35
7 Multi Residue Method for Determination of Chlorinated Pesticide 43
i) Dichlorodiphenyltrichloroethane 43
ii) HCH 43
iii) Endosulphan 43
iv) Aldrin 43
v) Dieldrin 43
vi) Chlordane 43
vii) Heptachlor 43
8 Multi Residue Method for Determination of Organo-Phosphorus 56
Pesticides
i) Acephate 57
ii) Chlorpyriphos 57
iii) Chlorpyriphos-methyl 57
iv) Demeton-O 57
v) Diazinon 57
vi) Dimethoate 57
vii) Ethion 57
viii) Fenitrothion 57
ix) Malaoxan 57
x) Malathion 57
xi) Mathamidophos 57
xii) Monocrotophos 57
xiii) Omethoate 57
xiv) Paraoxon 57
xv) Paraoxon-Methyl 57
xvi) Parathion 57
xvii) Parathion-Methyl 57
xviii) Phosalone 57
xix) Pirimiphos-Methyl 57
9 Multiresidue Gas Chromatography Method for Synthetic 62
Pyrethroids
i) Bifenthrin 63
ii) Fenopropathrin 63
iii) Cyhalothrin 63
iv) Permethrin 63


1

, PESTICIDE RESIDUES 2016

v) Cypermethrin 63
vi) Fluvalinate 63
vii) Fenvalerate 63
viii) Deltamethrin 63
10 Multiresidue Method of N-Methylcarbamate Insecticides 66
i) Carbaryl 69
ii) Carbofuron 69
11 Multiple Residue Method for Fumigants 70
i) Ethylene Dibromide 70
ii) Carbon Tetrachloride 70
iii) Methyl Bromide 70
iv) Phosphine 72
12 Thiamethoxam 77
13 Thiodicarb/Methomyl 83
14 Cymoxanil 87
15 Multiresidue Gas Chromatographic Method for Determination of 91
Organochlorine and Pyrethroid pesticides in Milk, Fish and Eggs
16 Acetamiprid 96
17 Imidacloprid 99
18 Pretilachlor 106
19 Isoprothiolane 110
20 Fosetyl 115
21 Propiconazole 122
22 Dithiocarbamates 126
(i) Ferbam 126
(ii) Ziram 126
(iii) Thiram 126
(iv) Maneb 126
(v)Zineb 126
(vi)Mancozab 126
(vii) Nabam 126
23 Ethylene Thiourea and Ethylene Urea 134
24 Tricyclazole 136
25 Triadimefon and Triadimenol 140
26 Metalaxyl 146
27 Triazole Fungicides 149
i) Hexaconazole 150
ii) Propiconazole 150
iii) Penconazole 150
iv) Myclobutanil 150
v) Triademifon 150
vi) Bitertanol 150
28 Chlorsulfuron and Metasulfuron 156
29 Anilophos 162
30 Diclofop-Methyl 165
31 Glufosinate 170
32 Linuron 181
33 Diquat and Paraquat 185


2

, PESTICIDE RESIDUES 2016

34 Atrazine and Simazine 188
35 Metribuzin 192
36 2, 4-D 196
37 Pendimethalin Analytical Methods of Pesticide Residues in Water 201
38 Organochlorine Pesticides in Water by Gas Chromatographic 204
Method
i) Aldrin 204
ii) α- BHC 204
iii) β- BHC 204
iv) γ - BHC 204
v) δ - BHC 204
vi) α- chlordane 204
vii) γ - chlordane 204
viii) 4,4'- ODD 204
ix) 4,4'- DDE 204
x) 4,4'- Dichlorodiphenyltrichloroethane 204
xi) Dieldrin 204
xii) Endosulfan I 204
xiii) Endosulfan II 204
xiv) Endosulfan Sulphate 204
xv) Heptachlor 204
xvi) Heptachlor Expoxide 204
39 N-Methylcarbamoylomimes and N-Methlycarbamates in Finished 211
Drinking Water
i) Aldicrab 211
ii) Aldicarb Sulfone 211
iii) Aldicarb Sulfoxide 211
iv) Baygon 211
v) Carbaryl 211
vi) Carboftiron 211
vii) 3-hydroxycarboruron 211
viii) Methiocarb 211
ix) Methomyl 211
x) Oxamyl 211
40 Determinatin of Alachlor, Atrazine and Butachlor in Water 216
41 Determination of 2,4-D in Drinking Water by Liquid-Liquid 226
Microextraction, Derivatization, and Fast Gas Chromatography
With Electron Capture Detection
42 Determination of Isoproturon in Water by Solid-Phase Extraction 233
and Liquid Chromatography
43 Nitrogen and Phosphorus Containing Pesticides in Finished 234
Drinking Water
(i) Dichlorvos 234
(ii) Phorate 234
(iii) Chlorpyrifos. Methyl 234
(iv) Chlopyrifos 234
(v) Monocrotophos 234
(vi) Dimethoate 234



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