本書是《農(nóng)藥獸藥多組分殘留質(zhì)譜分析技術(shù)》的第1卷農(nóng)藥篇,介紹了農(nóng)藥多殘留分析技術(shù)和千余種農(nóng)藥不同色譜-質(zhì)譜條件下的質(zhì)譜參數(shù),實(shí)現(xiàn)了一次樣品制備,GC-MS和LC-MS/MS同時測定,擴(kuò)大了檢測目標(biāo)的范圍。書中包括20項(xiàng)適用于10余類農(nóng)產(chǎn)品(包括水果、蔬菜、糧谷、茶葉、中草藥、食用菌、果蔬汁、蜂蜜、動物組織、水產(chǎn)品、牛奶、奶粉及飲用水)中800多種農(nóng)藥化學(xué)污染物殘留的色譜-質(zhì)譜分析方法。
本書可供從事食品安全、農(nóng)業(yè)環(huán)境保護(hù)及農(nóng)藥開發(fā)利用等技術(shù)研究與應(yīng)用的技術(shù)人員參考,也可作為大學(xué)教學(xué)參考用書。
龐國芳,中國檢驗(yàn)檢疫科學(xué)研究院,研究員,中國工程院院士,國家質(zhì)檢總局首席研究員、國際公職化學(xué)家聯(lián)合會(AOAC)專家,國際AOAC 2014年度 Harvey W. Wiley 獎獲得者。近30年一直工作在食品檢驗(yàn)檢疫一線,致力于食品科學(xué)檢測技術(shù)理論與實(shí)踐的研究,解決了我國相關(guān)出口食品、農(nóng)產(chǎn)品等遭遇的技術(shù)瓶頸,為推動我國對外貿(mào)易發(fā)展做出了杰出貢獻(xiàn)。研究制定了141項(xiàng)國際、國家檢測技術(shù)標(biāo)準(zhǔn)。在國內(nèi)、國際出版食品安全檢測技術(shù)論著10部。發(fā)表論文100余篇,35篇被SCI收錄。3次榮獲國家科學(xué)技術(shù)進(jìn)步二等獎,6次榮獲國際AOAC組織頒發(fā)的科學(xué)技術(shù)獎勵。
Main Researchers/Editors xiii
Preface xv
Brief Introduction xvii
1. Introduction 1
1.1 Insecticides 1
1.1.1 Organophosphate Insecticides 1
1.1.2 Carbamate Insecticides 2
1.1.3 Organochlorine Insecticides 2
1.1.4 Pyrethroid Insecticides 2
1.1.5 Neonicotinoid Insecticides 2
1.2 Herbicides 3
1.2.1 Phenolic Herbicides 3
1.2.2 Phenoxy Acid Herbicides 3
1.2.3 Benzoic Acid Herbicides 4
1.2.4 Diphenyl Ether Herbicides 4
1.2.5 Dinitroaniline Herbicides 4
1.2.6 Amide Herbicides 4
1.2.7 Carbamate Herbicides 5
1.2.8 Thiocarbamate Herbicides 5
1.2.9 Urea Herbicides 5
1.2.10 Sulfonylurea Herbicides 5
1.2.11 S-Triazine Herbicides 5
1.2.12 Quaternary Ammoniums Herbicides 6
1.2.13 Organophosphate Herbicides 6
1.2.14 Other Herbicides 6
1.3 Bactericides 6
1.3.1 Triazole Bactericides 7
1.3.2 Amide Bactericides 7
1.3.3 Pyridinamine Bactericides 7
1.3.4 Strobin Bactericides 7
1.3.5 Oxazo Bactericides 8
1.3.6 Pyrrole Bactericides 8
1.3.7 Amino Acid Bactericides 8
1.3.8 Derivants of Cinnamic Acid 8
1.3.9 Others 8
1.4 Pesticides Banned in the World 8
1.4.1 Pesticides Banned in China 8
1.4.2 Pesticides Banned in Japan 9
1.4.3 Pesticides Banned in European Union 9
2. Analytical Methods for 793 Pesticides and Related
Chemical Residues in Products of Plant Origin 11
2.1 Determination of 512 Pesticides and Related Chemical Residues
in Fruit Juice and Wine: LC-MS-MS Method (GB/T 23206-2008) 11
2.1.1 Scope 11
2.1.2 Principle 11
2.1.3 Reagents and Materials 11
2.1.4 Apparatus 21
2.1.5 Sample Pretreatment 21
2.1.6 Determination 22
2.1.7 Precision 24
Researchers 24
2.2 Determination of 500 Pesticides and Related Chemical Residues
in Fruits and Vegetables: GC-MS Method (GB/T 19648-2006) 25
2.2.1 Scope 25
2.2.2 Principle 25
2.2.3 Reagents and Materials 25
2.2.4 Apparatus 35
2.2.5 Sample Pretreatment 35
2.2.6 GC-MS Determination 36
2.2.7 Precision 37
Researchers 37
2.3 Determination of 450 Pesticides and Related Chemical Residues
in Fruits and Vegetables: LC-MS-MS Method(GB/T 20769-2008) 37
2.3.1 Scope 37
2.3.2 Principle 45
2.3.3 Reagents and Materials 45
2.3.4 Apparatus 46
2.3.5 Sample Pretreatment 46
2.3.6 Determination 47
2.3.7 Precision 49
Researchers 50
2.4 Determination of 475 Pesticides and Related Chemical Residues
in Grains: GC-MS Method (GB/T 19649-2006) 50
2.4.1 Scope 50
2.4.2 Principle 50
2.4.3 Reagents and Materials 50
2.4.4 Apparatus 59
2.4.5 Sample Pretreatment 59
2.4.6 GC-MS Method Determination 60
2.4.7 Precision 61
Researchers 61
2.5 Determination of 486 Pesticides and Related Chemical Residues
in Grains: LC-MS-MS Method (GB/T 20770-2008) 61
2.5.1 Scope 61
2.5.2 Principle 69
2.5.3 Reagents and Materials 69
2.5.4 Apparatus 71
2.5.5 Sample Pretreatment 71
2.5.6 Determination 72
2.5.7 Precision 73
Researchers 73
2.6 Determination of 519 Pesticides and Related Chemical
Residues in Tea Leaves: GC-MS Method (GB/T 23204-2008) 74
2.6.1 Scope 74
2.6.2 Determination of 490 Pesticides and Related Chemical Residues in Tea: GC-MS Method 74
2.6.3 Determination of 29 Acidic Herbicides in Tea:GC-MS Method 85
Researchers 91
2.7 Determination of 448 Pesticides and Related Chemical
Residues in Tea Leaves: LC-MS-MS Method (GB/T23205-2008) 92
2.7.1 Scope 92
2.7.2 Principle 92
2.7.3 Reagents and Materials 92
2.7.4 Apparatus 101
2.7.5 Sample Pretreatment 101
2.7.6 Determination 102
2.7.7 Precision 103
Researchers 103
2.8 Determination of 488 Pesticides and Related Chemical
Residues in Mulberry Twig, Honeysuckle, Barbary Wolfberry
Fruit, and Lotus Leaf: GC-MS Method (GB/T 23200-2008) 103
2.8.1 Scope 103
2.8.2 Principle 104
2.8.3 Reagents and Materials 104
2.8.4 Apparatus 113
2.8.5 Sample Pretreatment 113
2.8.6 Determination 114
2.8.7 Precision 115
Researchers 115
2.9 Determination of 413 Pesticides and Related Chemical
Residues in Mulberry Twig, Honeysuckle, Barbary Wolfberry
Fruit, and Lotus Leaf: LC-MS-MS Method (GB/T 23201-2008) 115
2.9.1 Scope 115
2.9.2 Principle 115
2.9.3 Reagents and Materials 116
2.9.4 Apparatus 123
2.9.5 Sample Pretreatment 123
2.9.6 Determination 124
2.9.7 Precision 126
Researchers 126
2.10 Determination of 503 Pesticides and Related Chemical
Residues in Mushrooms: GC-MS Method (GB/T 23216-2008) 126
2.10.1 Scope 126
2.10.2 Principle 126
2.10.3 Reagents and Materials 127
2.10.4 Apparatus 136
2.10.5 Sample Pretreatment 136
2.10.6 Determination 137
2.10.7 Precision 138
Researchers 138
2.11 Determination of 440 Pesticides and Related Chemical
Residues in Edible Fungus: LC-MS-MS Method(GB/T 23202-2008) 138
2.11.1 Scope 138
2.11.2 Principle 138
2.11.3 Reagents and Materials 146
2.11.4 Apparatus 147
2.11.5 Sample Pretreatment 147
2.11.6 Determination 148
2.11.7 Precision 149
Researchers 149
3. Analytical Methods for 790 Pesticides and Related
Chemical Residues in Products of Animal Origin 151
3.1 Determination of 511 Pesticides and Related Chemical
Residues in Milk and Milk Powder: GC-MS Method(GB/T 23210-2008) 151
3.1.1 Scope 151
3.1.2 Principle 151
3.1.3 Reagents and Materials 151
3.1.4 Apparatus 162
3.1.5 Sample Pretreatment 162
3.1.6 Determination 163
3.1.7 Precision 164
Researchers 164
3.2 Determination of 493 Pesticides and Related Chemical
Residues in Milk and Milk Powder: LC-MS-MS Method(GB/T 23211-2008) 165
3.2.1 Scope 165
3.2.2 Principle 165
3.2.3 Reagents and Materials 165
3.2.4 Apparatus 175
3.2.5 Sample Pretreatment 175
3.2.6 Determination 176
3.2.7 Precision 178
Researchers 178
3.3 Determination of 485 Pesticides and Related Chemical
Residues in Fugu, Eel, and Prawn: GC-MS Method(GB/T 23207-2008) 179
3.3.1 Scope 179
3.3.2 Principle 187
3.3.3 Reagents and Materials 187
3.3.4 Apparatus 188
3.3.5 Sample Pretreatment 189
3.3.6 Determination 190
3.3.7 Precision 191
Researchers 191
3.4 Determination of 450 Pesticides and Related Chemical
Residues in Fugu, Eel, and Prawn: LC-MS-MS Method(GB/T 23208-2008) 192
3.4.1 Scope 192
3.4.2 Principle 200
3.4.3 Reagents and Materials 200
3.4.4 Apparatus 201
3.4.5 Sample Pretreatment 201
3.4.6 Determination 203
3.4.7 Precision 204
Researchers 204
3.5 Determination of 497 Pesticides and Related Chemical
Residues in Honey, Fruit Juice, and Wine: GC-MS Method(GB/T 19426-2006) 204
3.5.1 Scope 204
3.5.2 Principle 204
3.5.3 Reagents and Materials 213
3.5.4 Apparatus 214
3.5.5 Sample Pretreatment 214
3.5.6 Determination 215
3.5.7 Precision 216
Researchers 217
3.6 Determination of 486 Pesticides and Related Chemical
Residues in Honey: LC-MS-MS Method (GB/T 20771-2008) 217
3.6.1 Scope 217
3.6.2 Principle 217
3.6.3 Reagents and Materials 217
3.6.4 Apparatus 227
3.6.5 Sample Pretreatment 227
3.6.6 Determination 228
3.6.7 Precision 232
Researchers 232
3.7 Determination of 478 Pesticides and Related Chemical
Residues in Animal Muscles: GC-MS Method(GB/T 19650-2006) 232
3.7.1 Scope 232
3.7.2 Principle 232
3.7.3 Reagents and Materials 232
3.7.4 Apparatus 242
3.7.5 Sample Pretreatment 242
3.7.6 Determination 243
3.7.7 Precision 244
Researchers 244
3.8 Determination of 461 Pesticides and Related Chemical
Residues in Animal Muscles: LC-MS-MS Method(GB/T 20772-2008) 245
3.8.1 Scope 245
3.8.2 Principle 253
3.8.3 Reagents and Materials 253
3.8.4 Apparatus 254
3.8.5 Sample Pretreatment 254
3.8.6 Determination 256
3.8.7 Precision 257
Researchers 257
4. Determination of 450 Pesticides and Related
Chemical Residues in Drinking Water: LC-MS-MS Method (GB/T 23214-2008) 259
4.1 Scope 259
4.2 Principle 259
4.3 Reagents and Materials 259
4.4 Apparatus 268
4.5 Sample Pretreatment 269
4.5.1 Preparation of Test Sample 269
4.5.2 Extraction 269
4.5.3 Clean-up 269
4.6 Determination 269
4.6.1 LC-MS-MS Operating Condition 269
4.6.2 Qualitative Determination 271
4.6.3 Quantitative Determination 271
4.7 Precision 272
Researchers 272
5. Basic Research on Chromatography-Mass Spectroscopy
Characteristic Parameters of Pesticide and Chemical Pollutants 273
5.1 Mass Spectrometry Data of 1200 Pesticides and Chemical
Pollutants Determined by GC-MS, GC-MS-MS, and LC-MS-MS 277
5.1.1 Retention Times, Quantifier and Qualifier Ions of
567 Pesticides and Chemical Pollutants Determined by GC-MS 277
5.1.2 Monitoring of Selected Ions for 567 Pesticides
and Chemical Pollutants Determined by GC-MS 311
5.1.3 Retention Time, Quantifier and Qualifier Ions, and
Collision Energies of 454 Pesticides and Chemical Pollutants Determined by GC-MS-MS 321
5.1.4 Monitoring of Selected Ions for 454 Pesticides
and Chemical Pollutants Determined by GC-MS-MS 349
5.1.5 Retention Time, Quantifier and Qualifier Ions,
and Collision Energies of 284 Environmental Pollutants by GC-MS-MS 356
5.1.6 Retention Times, Selective Ions, and Relative Abundances
of Endosulfans Determined by GC-NCI-MS 374
5.1.7 Retention Times, Quantifying and Qualifying Ions,
Declustering Potentials, and Collision Energies of 9 Environmental Pollutants Determined by LC-MS-MS 375
5.1.8 Retention Times, Quantifying and Qualifying Ions,Fragmentor, and Collision Energies of 569 Pesticides
and Chemical Pollutants Determined by LC-MS-MS 376
5.1.9 Accurate Masses, Retention Times, Parent Ions,and Collision Energies of 492 Pesticides and Chemical
Pollutants Determined by LC-TOF-MS 410
5.2 Linear Equation Parameters of 1200 Pesticides and
Chemical Pollutants Determined by GC-MS, GC-MS-MS,and LC-MS-MS 457
5.2.1 Linear Equations, Linear Ranges, and Correlation
Coefficients of 567 Pesticides and Chemical Pollutants Determined by GC-MS 457
5.2.2 Linear Equations, Linear Ranges, and Correlation
Coefficients of 466 Pesticides and Chemical Pollutants Determined by GC-MS-MS 491
5.2.3 Linear Equations, Linear Ranges, and Correlation
Coefficients of 284 Environmental Pollutants Determined by GC-MS-MS 519
5.2.4 Linear Equations, Linear Ranges, and Correlation
Coefficients of Endosulfans Determined by GC-MS(NCI) 536
5.2.5 Linear Equations, Linear Ranges, and Correlation
Coefficients of 9 Environmental Pollutants Determined by LC-MS-MS 537
5.2.6 Linear Equations, Linear Ranges, and Correlation
Coefficients of 569 Pesticides and Chemical Pollutants Determined by LC-MS-MS 538
5.3 GPC Analytical Parameters of Pesticides and Chemical Pollutants 572
5.3.1 GPC Analytical Parameters of 744 Pesticides and Chemical Pollutants 572
5.3.2 GPC Analytical Parameters of 107 Pesticides and Chemical Pollutants 599
Appendix A: Index of 1039 Pesticides and Chemical Pollutants Determined
by GC-MS, GC-MS-MS and LC-MS-MS 603
Appendix B: Solvent Selected and Concentration of Mixed Standard
Solution of Pesticides and Chemical Pollutants 661
Appendix C: Physicochemical Properties of 900 Pesticides
and Chemical Pollutants 707
Appendix D: MRM Chromatograms of 493 Pesticides
and Related Chemicals 791
Index 857