Residue Analysis in Food-Principles and Applications

326 Pages·2000·54.422 MB·\326

by  Michael O`Keefe (Editor)

Residue Analysis in Food

Residue Analysis in Food
Principles and Applications
Edited by
Michael O'Keeffe
Teagasc, The National Food Centre, Dublin, Ireland
Boca Raton London New York
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CONTENTS
Preface XV
Contributors xvii
1 Introduction 1
Michael O'Keeffe
1.1 Chemical Contamination of Food 1
1.2 Residue Analysis 2
1.3 Advances in Residue Analysis Methodologies 3
1.4 TheSampleistheKey 5
1.5 Analytical Methods 6
1.6 SpecialIssuesinResidueAnalysis 9
1.7 Future 11
1.8 References 11
2 Primary Extraction Technologies 17
Marie-Louise Scippo and Guy Maghuin-Rogister
2.1 Introduction 17
2.1.1 Typesofresidues 17
2.1.2 Justification for primary extraction 18
2.1.3 Difficulties intheanalysis ofresidues 18
2.2 Stages intheAnalysis ofResidues inFood 19
2.2.1 Sampling 19
2.2.2 Transfer tothelaboratory and storage 19
2.2.3 Thawing 20
2.2.4 Internal standard 20
2.2.5 Homogenisation 21
2.2.5.1 Milk 21
2.2.5.2 Eggs 21
2.2.5.3 Tissues 22
2.2.6 Enzyme/acid hydrolysis and digestion 22
2.2.7 (Primary)Extraction 23
2.2.8 Clean-up 25
2.2.8.1 Elimination of water 25
2.2.8.2 Elimination of fat 25
V
vi CONTENTS
2.2.8.3 Elimination of proteins 25
2.2.8.4 Elimination of co-extractives 26
2.2.9 Solvent removal 26
2.2.10 End point determination 26
2.3 Liquid-Liquid Partitioning 26
2.3.1 Theory 26
2.3.1.1 Multiple extraction 27
2.3.1.2 Influence of pH 28
2.3.1.3 Influence of temperature 28
2.3.1.4 Ion-pairing 28
2.3.1.5 Salting-out 28
2.4 Recovery Estimation in Quantitative Analysis 29
2.5 Examples 29
2.5.1 Pesticides 29
2.5.2 p-Agonists 30
2.5.3 Steroid hormones 31
2.5.3.1 Androgens 32
2.5.3.2 O estrogens 32
2.5.3.3 Progestagens 32
2.5.4 Antibiotics 32
2.5.4.1 Poly ethers 32
2.5.4.2 Macrolides 33
2.5.4.3 Chloramphenicol 33
2.5.5 Mycotoxins 33
2.5.6 Further reading 33
2.6 References 34
3 Sorbent Technologies : Principles and Applications 37
Steven A. Barker
3.1 Introduction 37
3.2 Solid Phase Extraction 38
3.2.1 Adsorption mode 38
3.2.2 Sizeexclusion orpermeation mode 39
3.2.3 Bonded phase partition mode 40
3.3 SorbentTechnologies: Columns, Cartridges andDiscs 43
3.4 Solid Phase Microextraction 45
3.5 Matrix SolidPhaseDispersion 45
3.6 CharacteristicsoftheMSPDProcess 49
3.6.1 Unique sample interactions 49
3.6.2 The nature ofthe solid support andbonded phase 49
CONTENTS vii
3.6.3 Matrix modification 50
3.6.4 Solvent elution 51
3.6.5 Thematrixeffect 51
3.7 Applications 52
3.8 References 58
4 Automated Extraction/Clean-Up Technologies 73
Alida A.M. Stolker, Saskia S. Sterk and LeendertA. van Ginkel
4.1 Introduction 73
4.2 Automated Solid-Phase Extraction Techniques 74
4.2.1 Principle 74
4.2.2 Applications of automated solid-phase extraction techniques 76
4.3 Column Switching Techniques 77
4.3.1 Principle 77
4.3.2 Applications of column-switching techniques 78
4.3.2.1 Sample clean-up 78
4.3.2.2 Sample enrichment 83
4.4. Supercritical FluidExtraction (SFE) 84
4.4.1 Principle 84
4.4.2 Applications ofSFE 88
4.4.2.1 Introduction 88
4.4.2.2 SFE of residues of analytes from'non-fatty'matrices 89
4.4.2.3 SFE of residues of analytes from fatty matrices 92
4.4.2.4 SFE of residues of analytes from samples of fat 98
4.5 Conclusions 100
4.6 References 101
5 Immunochemical and Receptor Technologies 107
Willem Haasnoot and Robert Schilt
5.1 Introduction 107
5.2 Specific Reagents 108
5.2.1 Antibodies 108
5.2.1.1 Antibody-antigen interaction 109
5.2.1.2 Poly-or monoclonal recombinant or anti-anti-idiotype 110
antibodies
5.2.1.3 Antibodies towards haptens 112
5.2.2 Receptors 112
5.2.2.1 Receptor binding 112
5.2.2.2 Hormonal receptors 113
5.2.2.3 Steroid hormone receptors 113
viii CONTENTS
5.3 AssayFormats andApplications 114
5.3.1 Radioimmunoassay (RIA) 116
5.3.2 Receptor assays 117
5.3.2.1 Radio receptor assay (RRA ) 111
5.3.2.2 Microbial receptor assay 118
5.3.2.3 Functional tests 119
5.3.3 Enzyme-linked immunosorbent assay(ELISA) 119
5.3.4 Solparticleimmunoassay (SPIA) 121
5.3.5 Enhanced enzyme immunoassays 123
5.3.5.1 Avidin-biotin systems 123
5.3.5.2 Chemiluminescence enzyme immunoassays (cEIA) 124
5.3.5.3 Electro-chemiluminescence immunoassays 125
5.3.6 Fluorescence immunoassays 125
5.3.6.1 Fluorescence polarisation immunoassay (FPIA) 126
5.3.6.2 Time-resolved fluoroimmunoassay (TR-FIA) or dissociation 126
enhanced lanthanide fluoroimmunoassay (DELFIA)
5.3.6.3 Solid phase fluorescence immunoassay (SPFIA) 127
5.3.7 Biosensors 127
5.3.7.1 Biosensor applications 128
5.4 SamplePreparation andScreeningAssays 129
5.5 Immunoaffinity Chromatography 132
5.5.1 IACcolumns 133
5.5.1.1 Commercially available columns 133
5.5.1.2 Column preparation 134
5.5.1.3 Column characteristics 134
5.5.2 IACprocedures 134
5.5.3 IACapplications 135
5.5.3.1 Mycotoxins 135
5.5.3.2 Growth promoters 136
5.5.3.3 Veterinary drugs and other analytes 136
5.5.3.4 Pesticides and contaminants 137
5.6 References 137
6 High Performance Thin Layer Chromatography for Residue Analysis 145
Hubert F De Brabander and Katia De Wasch
6.1 Introduction 145
6.2 TheFourStepsofTLC 146
6.2.1 Application 146
6.2.2 Development 147
6.2.2A The stationary phase 148
6.2.2.2 The solvents 148
6.2.2.3 Automated multiple development (AMD) 149
CONTENTS ix
6.2.3 Detection 149
6.2.3.1 The visualisation 150
6.23.2 The documentation 151
6.2 A Quantification 151
6.3 SomeSpecialFeaturesofTLC 153
6.3.1 Two-dimensional TLC 153
6.3.2 "4x4"-TLC 154
6.3.3 Anti-diagonal development 155
6.3.4 Coupled layers 156
6.3.5 Reaction TLC 157
6.3.5.1 Derivatisation at the application site 157
6.3.5.2 Other reactions at the application site 158
6.3.6 Some additional advantages ofTLC 158
6.4 Quality CriteriafortheUseofTLCinResidueAnalysis 158
6.4.1 Introduction 158
6.4.2 Discussion ofthe quality criteria 159
6.5 Comparison ofTLCwithotherMethods for ResidueAnalysis 161
6.6 Examples ofTLCMethods inResidueAnalysis 162
6.6.1 TLCmethodsforillegalgrowth promoters 162
6.6.1.1 Thyreostatic drugs 162
6.6.1.2 Anabolic steroids 163
6.6.1.3 Beta-agonists 164
6.6.1.4 Corticosteroids 165
6.6.2 TLC methods for antibacterials 164
6.6.2.1 Sulphonamides 165
6.6.2.2 Tetracyclines 165
6.6.2.3 Polyether antibiotics 165
6.6.2.4 Macrolide antibiotics 166
6.6.3 TLCmethodsforother residues 166
6.7 IsThereaFutureforTLCinResidueAnalysis? 166
6.7.1 Automation inTLC 167
6.7.2 Enhancing specificity in TLC 167
6.7.3 TLC/MS 168
6.7.3.1 Direct TLC/MS 168
6.7.3.2 TLC with additional hyphenated MS techniqu 168
6.8 Conclusion 169
6.9 References 171
7 Gas Chromatography 177
Bruno Le Bizec, Marie-Pierre Montrade and François André