Principles, Methods, and General Applications (eBook)

Front Cover 1
Principles, Methods, and General Applications 4
Copyright Page 5
Table of Contents 10
CONTRIBUTORS TO VOLUME I 6
PREFACE 8
Chapter 1. Introduction 16
I. Regulatory Control 16
II. The Residue Chemist 18
III. The "Zero Tolerance" 19
IV. Conclusions 19
References 20
Chapter 2. Principles of Formulation Analysis 22
I. Introduction 22
II. Philosophy of Formulation Analysis 23
III. Sample Handling and Storage 24
IV. Extraction and Separation Procedures 28
V. Types of Analysis 30
VI. Instrumentation 33
VII. Records and Reports 34
VIII. Future of Formulation Analysis 35
References 38
Chapter 3. Principles of Residue Analysis 40
I. Field Experiment 40
II. Pre-Analysis 43
III. Analytical Measurement 50
IV. Interpretations and Recommendations 57
References 59
Chapter 4. Principles of Food Additive Analysis 62
I. Introduction 62
II. General Considerations 64
III. Analysis of Direct Food Additives 65
IV. Analysis of Indirect Food Additives 68
Appendix I: Food Additives for Which Tolerances Are Established or Proposed 80
Appendix II: Summary of Polymer-Related F.D.A. Regulations 93
Appendix III: Examples of Analyses of Indirect Food Additives 98
References 100
Chapter 5. Extraction and Clean-Up Procedures 102
I. Introduction 102
II. Solvent Extraction 103
III. Evaluation of Clean-Up Procedures 109
IV. Universal Type of Clean-Up 112
V. General Separation Procedures 116
VI. Chromatography 119
References 123
Chapter 6. Principles of Toxicological Testing Methods 124
I. Introduction 124
II. General Principles in Toxicology 125
III. Specific Methodology 125
IV. Selection of Animals for Toxicological Studies 132
V. Interpretation of Results 134
VI. Future Trends in Toxicology 135
References 136
Chapter 7. The Pesticide Residue Laboratory 138
I. The Problem 138
II. The Pesticide Residue Laboratory 139
III. Personnel 145
Chapter 8. Spectrophotometric Methods 146
I. Ultraviolet and Visible 146
II. Infrared 164
III. Fluorescence 182
References 201
Chapter 9. Gas Chromatography 204
I. Introduction 204
II. Basic Principles 205
III. Apparatus 206
IV. Interpretation of Analytical Results 223
V. Analytical Applications to Pesticide Problems 227
VI. Conclusions 237
References 237
Chapter 10. Paper Chromatography 242
I. Insecticides 242
II. Fungicides 264
III. Herbicides 265
IV. Rodenticides 266
References 266
Chapter 11. Total Halide Analysis 268
I. Combustion Techniques 268
II. Schöniger Technique. Oxygen Flask Combustion Method 276
III. Sodium Reduction 283
IV. Total Bromide 288
References 294
Chapter 12. Neutron Activation Analysis 296
I. Introduction 296
II. Theory of Neutron Activation 297
III. Neutron Activation Procedure 303
IV. Sensitivities for Thermal-Neutron Activation 312
V. Application of Neutron Activation Analysis 317
VI. Instrumentation and Neutron Sources 335
ACKNOWLEDGMENTS 337
References 337
Chapter 13. Isotope Methods 340
I. Introduction 340
II. Definition of Terms 341
III. Establishing a Laboratory 342
IV. Selection of Compounds 348
V. Instrumentation 352
VI. Preparation of Samples 371
VII. Counting of Samples 378
VIII. Reporting Radioactive Data 381
IX. Special Techniques 383
Glossary 385
References 386
Chapter 14. Enzymatic Methods 388
I. Introduction 388
II. Kinetics of Cholinesterase Activity 389
III. Kinetics of Cholinesterase Inhibition 390
IV. Action of Cholinesterases 392
V. Methods of Measuring Cholinesterase Activity 396
VI. Activation of Cholinesterase Inhibitors 399
VII. Application of Cholinesterase Inhibition to Residue Analysis 406
VIII. Conclusions 410
References 411
Chapter 15. Bioassay–Insects 414
I. Introduction 414
II. Principle of Bioassay 415
III. Test Insects and Sensitivity 418
IV. Factors Affecting Bioassay 420
V. Qualitative and Semiquantitative Bioassay 422
VI. Macrobioassay 423
VII. Microbioassay 424
VIII. Specific Bioassay 432
IX. Integration between Bioassay and Physicochemical Analysis 433
X. Application and Operation 435
XI. Summary and Discussion 435
References 437
Chapter 16. Bioassay of Microbial Pesticides 440
I. Introduction 440
II. Microbial Pesticide Products and Federal Regulation 442
III. Quantitative Analytical Methods for Spore or Particle Determination 445
IV. Insect Bioassay of Microbial Pesticides 452
References 456
Chapter 17. Bioassay–Plants 458
I. Introduction 458
II. Extraction of Regulating Substances from Plants and Preparation of Extracts for Bioassay 459
III. Responses to Growth-Regulating Substances, Principles Involved, and Suitability of These Responses for Bioassay 466
IV. Identification of Regulating Substances with Plant Assays 479
V. Conclusions 482
References 483
Chapter 18. Screening Methods 486
I. The Selection of Methods 486
II. A Screening System for Insecticides Containing Chlorine and Those That Inhibit Cholinesterase 488
ACKNOWLEDGMENT 505
References 505
Chapter 19. Statistical Evaluation of Results and Sampling Procedures 506
I. Introduction 506
II. Frequency Curves 507
III. Analysis of Variance 514
IV. Linear Regression 534
V. Sampling 536
VI. Concluding Remarks 540
ACKNOWLEDGMENT 541
References 541
Appendix 542
Chapter 20. Residue Analysis in the Food Industry 546
I. Introduction 546
II. Prevention of Over-Tolerance Residues 548
III. Formulation of Sprays and Dusts 551
IV. Analysis of Food Crops 551
V. Pesticide Laboratory for the Food Industry 554
VI. Degradation of Pesticides 555
VII. General Methods of Analysis 556
VIII. Validity of Results 557
IX. Summary 558
References 559
Chapter 21. Residue Analysis in the Dairy Industry 560
I. The Place of Pesticides in Agriculture 560
II. Nature and Effects of Pesticides 563
III. Physical and Chemical Characteristics of Fat in Milk 569
IV. Methods Available for Pesticide Analysis in Dairy Products 573
V. Interpretation of Analytical Results 581
VI. Control of the Pesticide Problem 583
References 584
Chapter 22. Methods for Pesticide Analysis in Meat Products 586
I. Sources of Residues in Meats 586
II. Residue Analysis in Meat and Meat Products— Problems Encountered 589
III. Screening Methods 590
References 595
Chapter 23. Formulation and Residue Analysis in Government Laboratories 598
I. Introduction 598
II. Formulation Analysis 602
III. Residue Analyses 617
Author Index 630
Subject Index 641