Mass Spectrometry for the Analysis of Pesticide Residues and their Metabolites (eBook, PDF)
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Mass Spectrometry for the Analysis of Pesticide Residues and their Metabolites (eBook, PDF)
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Provides an overview of the use of mass spectrometry (MS) for the analysis of pesticide residues and their metabolites. * Presents state of the-art MS techniques for the identification of pesticides and their transformation products in food and environment * Covers important advances in MS techniques including MS instrumentation and chromatographic separations (e.g. UPLC, HILIC, comprehensive GCxGC) and applications * Illustrates the main sample preparation techniques (SPE, QuEChERS, microextraction) used in combination with MS for the analysis of pesticides * Describes various established and…mehr
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- Produktdetails
- Verlag: John Wiley & Sons
- Seitenzahl: 288
- Erscheinungstermin: 11. Mai 2015
- Englisch
- ISBN-13: 9781119069980
- Artikelnr.: 42886695
- Verlag: John Wiley & Sons
- Seitenzahl: 288
- Erscheinungstermin: 11. Mai 2015
- Englisch
- ISBN-13: 9781119069980
- Artikelnr.: 42886695
Risk Assessment 1 Despina Tsipi, Helen Botitsi, and Anastasios Economou 1.1
Introduction 1 1.2 Pesticide Chemistry 2 1.2.1 Historical Perspective 2
1.2.2 Identity and Physicochemical Properties of Pesticides 2 1.2.3
Pesticide Classification 4 1.2.4 Modes of Action (MoA) 5 1.3 Pesticide
Metabolites and Transformation Products 8 1.3.1 Biotransformation 9 1.3.2
Environmental Fate 13 1.4 Risk Assessment 14 1.4.1 Safety Factors 14 1.4.2
Ecological Risk Assessment for Pesticides 15 1.5 Dietary Exposure to
Pesticides 17 1.5.1 Acute Exposure or Short-Term Intake 18 1.5.2 Chronic
Exposure or Long-Term Intake 18 1.5.3 Cumulative Exposure to Multiple
Substances 18 1.6 Pesticide Residues in Food 19 1.6.1 Maximum Residue
Limits 19 1.6.2 Residue Definition 20 1.6.3 Reporting of Results 28 1.6.4
Residue Analysis 28 References 29 2 Legislation, Monitoring, and Analytical
Quality Control for Pesticide Residues 35 Despina Tsipi, Helen Botitsi, and
Anastasios Economou 2.1 Introduction 35 2.2 Food Safety 36 2.2.1 CAC of
Food and Agriculture Organization/World Health Organization 36 2.2.2 EU
Legislation 36 2.2.3 US Food Regulations 40 2.3 Water Quality 44 2.3.1 WHO
44 2.3.2 EU Water Framework Directive 44 2.3.3 US EPA Legislation 46 2.4
Method Validation and Quality Control Procedures for Pesticide Residues
Analysis 46 2.4.1 CAC Guidelines 46 2.4.2 EU Guidelines: SANCO Document 47
2.4.3 FDA and EPA Guidelines 48 References 50 3 Advanced Sample Preparation
Techniques for MS Analysis 53 Yolanda Picó 3.1 Introduction 53 3.2
Conventional Extraction and Cleanup Procedures 54 3.2.1 LLE 54 3.2.2 SPE 61
3.2.3 MSPD 63 3.2.4 QuEChERS 63 3.3 Microextraction Techniques 65 3.3.1
Sorbent-Based Microextraction Techniques 65 3.3.2 Liquid-Based
Microextraction Techniques 71 3.4 Alternative Extraction and Cleanup
Procedures 73 3.4.1 Alternative Energy Sources to Enhance the Extraction 73
3.4.2 Coupled-Column Liquid Chromatography (LC/PC, LC/LC Techniques) 79
3.4.3 Direct Analysis in Real Time 80 3.5 Conclusions 81 References 82 4
Recent Developments in Gas Chromatography-Mass Spectrometry 91 Kaushik
Banerjee and Sagar Utture 4.1 Introduction 91 4.2 Advances in GC
Separations 91 4.2.1 Multidimensional and Comprehensive Two-Dimensional Gas
Chromatography 92 4.2.2 Fast GC 94 4.2.3 LPGC 95 4.3 Mass Spectrometric
Ionization Techniques 96 4.3.1 Electron Impact Ionization (EI) 97 4.3.2 CI
(Positive/Negative Modes) 97 4.3.3 Atmospheric Pressure GC-MS 98 4.4 Mass
Analyzers Interfaced to GC 99 4.4.1 Quadrupole Mass Analyzer 100 4.4.2 Ion
Trap Mass Analyzer 100 4.4.3 QqQ 100 4.4.4 TOF 102 4.5 Mass Spectral
Libraries and Software Approaches in GC-MS Analysis 103 4.6 Matrix Effects
in GC-MS Analysis 106 4.7 Conclusions and Perspectives 108 References 108 5
Recent Developments in Liquid Chromatography-Mass Spectrometry: Advances in
Liquid Chromatographic Separations and Ionization Techniques/Interfaces 113
Alexandros G. Asimakopoulos, Anna Bletsou, Kurunthachalam Kannan, and
Nikolaos S. Thomaidis 5.1 Introduction 113 5.2 Advances in Liquid
Chromatographic Separations 114 5.2.1 Ultraperformance Liquid
Chromatography 116 5.2.2 Hydrophilic Interaction Liquid Chromatography 117
5.3 Ionization Techniques/Interfaces 117 5.3.1 Atmospheric Pressure
Ionization Techniques 118 5.3.2 Direct Electron Ionization 121 5.4 Ambient
Ionization Techniques 122 5.4.1 DESI, Paper Spray, and Low-Temperature
Plasma Ambient Ionization 122 5.4.2 Direct Analysis in Real Time 124 5.4.3
Atmospheric Pressure Glow-Discharge Ionization 125 5.5 Summary 125
References 125 6 Recent Developments in Liquid Chromatography-Mass
Spectrometry: Mass Detectors 131 Silvia Lacorte, Ana Agüera, Montserrat
Cortina-Puig, and Cristian Gómez-Canela 6.1 Introduction: Mass
Spectrometers 131 6.1.1 Triple Quadrupole Mass Analyzer 132 6.1.2
Quadrupole Ion Trap and Triple Quadrupole Linear Ion Trap 135 6.1.3 TOF
Mass Analyzer 138 6.1.4 Hybrid TOF 140 6.1.5 Orbitrap Mass Analyzer 142 6.2
Comparison and Complementarities of Different Mass Analyzers in the LC-MS
Analysis of Pesticide Residues and their Metabolites 147 6.2.1 Dynamic
Range 147 6.2.2 Scan Rate 147 6.2.3 LODs 148 6.2.4 Mass Accuracy 148 6.2.5
Resolution 149 6.2.6 Selectivity 149 6.2.7 Mass Range 150 6.2.8
Fragmentation 150 6.2.9 Identification Capabilities 150 6.2.10
Quantification 151 6.3 Use of Software Techniques and Spectral Libraries in
LC-MS 152 References 154 7 Matrix Effects in Liquid
Chromatography-Electrospray Ionization-Mass Spectrometry 161 Helen Stahnke
and Lutz Alder 7.1 Introduction 161 7.1.1 Some Definitions 161 7.1.2
Differences between Matrix Effects in GC and LC Methods 162 7.1.3
Differences between ESI and Other API Methods 162 7.1.4 A Typical Alarming
Situation 163 7.2 Detection of Matrix Effects 164 7.2.1 Calibration in
Solvent versus Matrix-Matched Calibration 164 7.2.2 Postcolumn Infusion 165
7.2.3 Stable Isotope-Labeled Standards 166 7.3 Reduction of Matrix Effects
166 7.3.1 Change of LC Conditions 166 7.3.2 Change of MS Conditions 166
7.3.3 Better Cleanup 169 7.3.4 Backflush of LC Columns 170 7.3.5
Dilute-and-Shoot 171 7.4 Compensation of Matrix Effects 172 7.4.1 Internal
standards (IS) 172 7.4.2 Matrix-Matched Standards 174 7.4.3 Postcolumn
Infusion 174 7.4.4 Standard Addition 175 7.5 An Attempt to Explain Matrix
Effects 176 7.5.1 Substance Classes Causing Matrix Effects 176 7.5.2
Tentative Mechanisms of Matrix Effects 176 7.5.3 A Recent View on the
Mechanism of Ion Suppression 178 References 180 8 Liquid
Chromatography-Mass Spectrometry Analysis of Pesticide Residues and Their
Metabolites in Food Samples 187 Ana Lozano, Aukasz Rajski, María del Mar
Gómez-Ramos, Carmen Ferrer, Maria D. Hernando, and Amadeo R. Fernández-Alba
8.1 Introduction 187 8.2 Application of LC-QqQ-MS/MS for the Targeted
Analysis of Pesticide Residues and their Metabolites in Food Samples 189
8.2.1 Sensitivity 192 8.2.2 Linearity 193 8.2.3 Matrix Effects 193 8.3
Application of LC-Hrms to the Analysis of Pesticide Residues and their
Metabolites in Food Samples 195 8.3.1 Detection and Identification 195
8.3.2 Resolution 197 8.3.3 MS/MS Identification 200 8.3.4 Sensitivity 201
8.3.5 Linearity 201 8.3.6 Matrix Effect 202 8.4 Data Processing: Automated
Database Searches 202 8.5 Conclusions and Future Developments 203
References 203 9 Application of LC-MS/MS and LC-TOF -MS for the
Identification of Pesticide Residues and Their Metabolites in Environmental
Samples 207 Imma Ferrer and E. Michael Thurman 9.1 Introduction and
Occurrence of Pesticides in Environmental Samples 207 9.2 State-of-the-Art
Techniques for the Identification of Pesticides and their Degradation
Products 208 9.2.1 LC-MS/MS for the Analysis of Target Compounds 208 9.2.2
LC-TOF-MS and LC-QTOF-MS for the Analysis of Target and Nontarget Compounds
209 9.3 Use of Accurate Mass Tools for the Identification of Pesticide
Residues and their Metabolites in Food and Water Samples 215 9.3.1
Molecular Features 215 9.3.2 Accurate Mass Filters and Isotopic Mass Defect
220 9.3.3 Diagnostic Ion Approach 221 9.3.4 Accurate Mass Databases 223
9.3.5 Accurate Mass Profiling 225 9.4 Conclusions 227 References 227 10
Mass Spectrometric Techniques for the Determination of Pesticide
Transformation Products Formed by Advanced Oxidation Processes 231 Ioannis
K. Konstantinou 10.1 Introduction 231 10.2 Sample Preparation 232 10.3
Hyphenated MS Techniques 237 10.3.1 Low-Resolution Mass Spectrometry:
Single-Stage Quadrupole 238 10.3.2 Identification of Pesticide TPs by GC-MS
238 10.3.3 Identification of Pesticide TPs by LC-MS 240 10.3.4
Identification of Pesticide TPs by the Combination of GC-MS and LC-MS 241
10.4 Tandem MS 241 10.4.1 Identification of Pesticide TPs by QqQ-MS 243
10.4.2 Identification of Pesticide TPs by IT-MS 244 10.5 HRMS 249 10.5.1
Single Mass Analyzer 249 10.5.2 Hybrid HR Mass Spectrometers 255 10.6
Conclusions and Perspectives 256 References 259 Index 263
Risk Assessment 1 Despina Tsipi, Helen Botitsi, and Anastasios Economou 1.1
Introduction 1 1.2 Pesticide Chemistry 2 1.2.1 Historical Perspective 2
1.2.2 Identity and Physicochemical Properties of Pesticides 2 1.2.3
Pesticide Classification 4 1.2.4 Modes of Action (MoA) 5 1.3 Pesticide
Metabolites and Transformation Products 8 1.3.1 Biotransformation 9 1.3.2
Environmental Fate 13 1.4 Risk Assessment 14 1.4.1 Safety Factors 14 1.4.2
Ecological Risk Assessment for Pesticides 15 1.5 Dietary Exposure to
Pesticides 17 1.5.1 Acute Exposure or Short-Term Intake 18 1.5.2 Chronic
Exposure or Long-Term Intake 18 1.5.3 Cumulative Exposure to Multiple
Substances 18 1.6 Pesticide Residues in Food 19 1.6.1 Maximum Residue
Limits 19 1.6.2 Residue Definition 20 1.6.3 Reporting of Results 28 1.6.4
Residue Analysis 28 References 29 2 Legislation, Monitoring, and Analytical
Quality Control for Pesticide Residues 35 Despina Tsipi, Helen Botitsi, and
Anastasios Economou 2.1 Introduction 35 2.2 Food Safety 36 2.2.1 CAC of
Food and Agriculture Organization/World Health Organization 36 2.2.2 EU
Legislation 36 2.2.3 US Food Regulations 40 2.3 Water Quality 44 2.3.1 WHO
44 2.3.2 EU Water Framework Directive 44 2.3.3 US EPA Legislation 46 2.4
Method Validation and Quality Control Procedures for Pesticide Residues
Analysis 46 2.4.1 CAC Guidelines 46 2.4.2 EU Guidelines: SANCO Document 47
2.4.3 FDA and EPA Guidelines 48 References 50 3 Advanced Sample Preparation
Techniques for MS Analysis 53 Yolanda Picó 3.1 Introduction 53 3.2
Conventional Extraction and Cleanup Procedures 54 3.2.1 LLE 54 3.2.2 SPE 61
3.2.3 MSPD 63 3.2.4 QuEChERS 63 3.3 Microextraction Techniques 65 3.3.1
Sorbent-Based Microextraction Techniques 65 3.3.2 Liquid-Based
Microextraction Techniques 71 3.4 Alternative Extraction and Cleanup
Procedures 73 3.4.1 Alternative Energy Sources to Enhance the Extraction 73
3.4.2 Coupled-Column Liquid Chromatography (LC/PC, LC/LC Techniques) 79
3.4.3 Direct Analysis in Real Time 80 3.5 Conclusions 81 References 82 4
Recent Developments in Gas Chromatography-Mass Spectrometry 91 Kaushik
Banerjee and Sagar Utture 4.1 Introduction 91 4.2 Advances in GC
Separations 91 4.2.1 Multidimensional and Comprehensive Two-Dimensional Gas
Chromatography 92 4.2.2 Fast GC 94 4.2.3 LPGC 95 4.3 Mass Spectrometric
Ionization Techniques 96 4.3.1 Electron Impact Ionization (EI) 97 4.3.2 CI
(Positive/Negative Modes) 97 4.3.3 Atmospheric Pressure GC-MS 98 4.4 Mass
Analyzers Interfaced to GC 99 4.4.1 Quadrupole Mass Analyzer 100 4.4.2 Ion
Trap Mass Analyzer 100 4.4.3 QqQ 100 4.4.4 TOF 102 4.5 Mass Spectral
Libraries and Software Approaches in GC-MS Analysis 103 4.6 Matrix Effects
in GC-MS Analysis 106 4.7 Conclusions and Perspectives 108 References 108 5
Recent Developments in Liquid Chromatography-Mass Spectrometry: Advances in
Liquid Chromatographic Separations and Ionization Techniques/Interfaces 113
Alexandros G. Asimakopoulos, Anna Bletsou, Kurunthachalam Kannan, and
Nikolaos S. Thomaidis 5.1 Introduction 113 5.2 Advances in Liquid
Chromatographic Separations 114 5.2.1 Ultraperformance Liquid
Chromatography 116 5.2.2 Hydrophilic Interaction Liquid Chromatography 117
5.3 Ionization Techniques/Interfaces 117 5.3.1 Atmospheric Pressure
Ionization Techniques 118 5.3.2 Direct Electron Ionization 121 5.4 Ambient
Ionization Techniques 122 5.4.1 DESI, Paper Spray, and Low-Temperature
Plasma Ambient Ionization 122 5.4.2 Direct Analysis in Real Time 124 5.4.3
Atmospheric Pressure Glow-Discharge Ionization 125 5.5 Summary 125
References 125 6 Recent Developments in Liquid Chromatography-Mass
Spectrometry: Mass Detectors 131 Silvia Lacorte, Ana Agüera, Montserrat
Cortina-Puig, and Cristian Gómez-Canela 6.1 Introduction: Mass
Spectrometers 131 6.1.1 Triple Quadrupole Mass Analyzer 132 6.1.2
Quadrupole Ion Trap and Triple Quadrupole Linear Ion Trap 135 6.1.3 TOF
Mass Analyzer 138 6.1.4 Hybrid TOF 140 6.1.5 Orbitrap Mass Analyzer 142 6.2
Comparison and Complementarities of Different Mass Analyzers in the LC-MS
Analysis of Pesticide Residues and their Metabolites 147 6.2.1 Dynamic
Range 147 6.2.2 Scan Rate 147 6.2.3 LODs 148 6.2.4 Mass Accuracy 148 6.2.5
Resolution 149 6.2.6 Selectivity 149 6.2.7 Mass Range 150 6.2.8
Fragmentation 150 6.2.9 Identification Capabilities 150 6.2.10
Quantification 151 6.3 Use of Software Techniques and Spectral Libraries in
LC-MS 152 References 154 7 Matrix Effects in Liquid
Chromatography-Electrospray Ionization-Mass Spectrometry 161 Helen Stahnke
and Lutz Alder 7.1 Introduction 161 7.1.1 Some Definitions 161 7.1.2
Differences between Matrix Effects in GC and LC Methods 162 7.1.3
Differences between ESI and Other API Methods 162 7.1.4 A Typical Alarming
Situation 163 7.2 Detection of Matrix Effects 164 7.2.1 Calibration in
Solvent versus Matrix-Matched Calibration 164 7.2.2 Postcolumn Infusion 165
7.2.3 Stable Isotope-Labeled Standards 166 7.3 Reduction of Matrix Effects
166 7.3.1 Change of LC Conditions 166 7.3.2 Change of MS Conditions 166
7.3.3 Better Cleanup 169 7.3.4 Backflush of LC Columns 170 7.3.5
Dilute-and-Shoot 171 7.4 Compensation of Matrix Effects 172 7.4.1 Internal
standards (IS) 172 7.4.2 Matrix-Matched Standards 174 7.4.3 Postcolumn
Infusion 174 7.4.4 Standard Addition 175 7.5 An Attempt to Explain Matrix
Effects 176 7.5.1 Substance Classes Causing Matrix Effects 176 7.5.2
Tentative Mechanisms of Matrix Effects 176 7.5.3 A Recent View on the
Mechanism of Ion Suppression 178 References 180 8 Liquid
Chromatography-Mass Spectrometry Analysis of Pesticide Residues and Their
Metabolites in Food Samples 187 Ana Lozano, Aukasz Rajski, María del Mar
Gómez-Ramos, Carmen Ferrer, Maria D. Hernando, and Amadeo R. Fernández-Alba
8.1 Introduction 187 8.2 Application of LC-QqQ-MS/MS for the Targeted
Analysis of Pesticide Residues and their Metabolites in Food Samples 189
8.2.1 Sensitivity 192 8.2.2 Linearity 193 8.2.3 Matrix Effects 193 8.3
Application of LC-Hrms to the Analysis of Pesticide Residues and their
Metabolites in Food Samples 195 8.3.1 Detection and Identification 195
8.3.2 Resolution 197 8.3.3 MS/MS Identification 200 8.3.4 Sensitivity 201
8.3.5 Linearity 201 8.3.6 Matrix Effect 202 8.4 Data Processing: Automated
Database Searches 202 8.5 Conclusions and Future Developments 203
References 203 9 Application of LC-MS/MS and LC-TOF -MS for the
Identification of Pesticide Residues and Their Metabolites in Environmental
Samples 207 Imma Ferrer and E. Michael Thurman 9.1 Introduction and
Occurrence of Pesticides in Environmental Samples 207 9.2 State-of-the-Art
Techniques for the Identification of Pesticides and their Degradation
Products 208 9.2.1 LC-MS/MS for the Analysis of Target Compounds 208 9.2.2
LC-TOF-MS and LC-QTOF-MS for the Analysis of Target and Nontarget Compounds
209 9.3 Use of Accurate Mass Tools for the Identification of Pesticide
Residues and their Metabolites in Food and Water Samples 215 9.3.1
Molecular Features 215 9.3.2 Accurate Mass Filters and Isotopic Mass Defect
220 9.3.3 Diagnostic Ion Approach 221 9.3.4 Accurate Mass Databases 223
9.3.5 Accurate Mass Profiling 225 9.4 Conclusions 227 References 227 10
Mass Spectrometric Techniques for the Determination of Pesticide
Transformation Products Formed by Advanced Oxidation Processes 231 Ioannis
K. Konstantinou 10.1 Introduction 231 10.2 Sample Preparation 232 10.3
Hyphenated MS Techniques 237 10.3.1 Low-Resolution Mass Spectrometry:
Single-Stage Quadrupole 238 10.3.2 Identification of Pesticide TPs by GC-MS
238 10.3.3 Identification of Pesticide TPs by LC-MS 240 10.3.4
Identification of Pesticide TPs by the Combination of GC-MS and LC-MS 241
10.4 Tandem MS 241 10.4.1 Identification of Pesticide TPs by QqQ-MS 243
10.4.2 Identification of Pesticide TPs by IT-MS 244 10.5 HRMS 249 10.5.1
Single Mass Analyzer 249 10.5.2 Hybrid HR Mass Spectrometers 255 10.6
Conclusions and Perspectives 256 References 259 Index 263