<p>Preface xi</p> <p>Contributors xiii</p> <p><b>Chapter 1 Introduction: Basic Principles of Assays to be Covered, Sample Handling, And Sample Processing 1<br /> </b><i>Wanlong Zhou, Eugene Y. Chang, and Perry G. Wang</i></p> <p>1.1 Introduction 1</p> <p>1.1.1 Current Situation and Challenges of Food Safety and Regulations 1</p> <p>1.1.2 Residues and Matrices of Food Analysis and High-Throughput Analysis 2</p> <p>1.1.3 Food Safety Classifications 3</p> <p>1.1.4 “High Throughput” Definition 3</p> <p>1.1.5 Scope of the Book 4</p> <p>1.2 Advanced Sample Preparation Techniques 5</p> <p>1.2.1 Automation of Weighing and Preparing Standard Solutions 5</p> <p>1.2.2 QuEChERS 6</p> <p>1.2.3 Swedish Extraction Technique (SweEt) and Other Fast Sample Preparation Methods 6</p> <p>1.2.4 Turbulent Flow Chromatography 7</p> <p>1.2.5 Pressurized Liquid Extraction 7</p> <p>1.2.6 Automated 96- and 384-Well Formatted Sample Preparation as well as Automated SPE Workstations 8</p> <p>1.2.7 Solid-Phase Microextraction 8</p> <p>1.2.8 Microextraction by Packed Sorbent 9</p> <p>1.2.9 Liquid Extraction Surface Analysis 9</p> <p>1.2.10 Headspace GC 10</p> <p>1.2.11 Summary 10</p> <p>1.3 Future Perspectives 10</p> <p>Acknowledgment 11</p> <p>References 11</p> <p><b>Chapter 2 Survey Of Mass Spectrometry-Based High-Throughput Methods In Food Analysis 15<br /> </b><i>Lukas Vaclavik, Tomas Cajka, Wanlong Zhou, and Perry G. Wang</i></p> <p>2.1 Introduction 15</p> <p>2.2 Techniques Employing Chromatographic Separation 15</p> <p>2.2.1 Gas Chromatography–Mass Spectrometry 15</p> <p>2.2.2 Liquid Chromatography–Mass Spectrometry 21</p> <p>2.3 Direct Techniques 30</p> <p>2.3.1 Matrix-Assisted Laser Desorption/Ionization-Mass Spectrometry 30</p> <p>2.3.2 Headspace (Solid-Phase Microextraction)-Mass Spectrometry E-Nose 37</p> <p>2.3.3 Ambient Desorption/Ionization-Mass Spectrometry 38</p> <p>2.4 Concluding Remarks 62</p> <p>Acknowledgments 62</p> <p>References 63</p> <p><b>Chapter 3 Quality Systems, Quality Control Guidelines and Standards, Method Validation, and Ongoing Analytical Quality Control 73<br /> </b><i>David Galsworthy and Stewart Reynolds</i></p> <p>3.1 Introduction 73</p> <p>3.1.1 Quality System Design 73</p> <p>3.1.2 Procedures 74</p> <p>3.1.3 Roles and Responsibilities 74</p> <p>3.1.4 Quality Manual 74</p> <p>3.1.5 Document Control 74</p> <p>3.1.6 Control of Records 75</p> <p>3.1.7 Audits 75</p> <p>3.1.8 Validation of Methodology 75</p> <p>3.1.9 Staff Competency 75</p> <p>3.1.10 Internal Quality Control 76</p> <p>3.1.11 Method Performance Criteria 76</p> <p>3.2 Qualitative Screening Methods 76</p> <p>3.2.1 Selectivity of Mass Spectrometry-Based Methods 78</p> <p>3.2.2 Confirmatory Methods 78</p> <p>3.2.3 Validation of Qualitative Screening Multiresidue Methods for Pesticide Residues in Foods 79</p> <p>3.3 Elements of the Analytical Workflow 80</p> <p>3.3.1 Sample Preparation 80</p> <p>3.3.2 Effects of Sample Processing 81</p> <p>3.3.3 Extraction Efficiency 81</p> <p>3.4 Initial Method Validation 81</p> <p>3.5 Ongoing Analytical Quality Control 86</p> <p>3.5.1 Internal Quality Control 86</p> <p>3.5.2 Proficiency Testing 86</p> <p>3.6 Validation of Qualitative Screening Multiresidue Methods for Veterinary Drug Residues in Foods 87</p> <p>3.6.1 EU Legislation Covering Method Validation for Veterinary Drug Screening 87</p> <p>3.6.2 Determination of Specificity/Selectivity and Detection Capability (CC<i>β</i>) Using the Classical Approach 88</p> <p>3.6.3 Establishment of a Cutoff Level and Calculation of CC<i>β </i>88</p> <p>3.6.4 Determination of the Applicability 89</p> <p>3.7 Conclusions 90</p> <p>References 90</p> <p><b>Chapter 4 Deliberate Chemical Contamination and Processing Contamination 93<br /> </b><i>Stephen Lock</i></p> <p>4.1 Introduction 93</p> <p>4.2 Heat-Induced Food Processing Contaminants 97</p> <p>4.3 Packaging Migrants 101</p> <p>4.4 Malicious Contamination of Food 105</p> <p>References 111</p> <p><b>Chapter 5 Multiresidual Determination Of 295 Pesticides And Chemical Pollutants In Animal Fat By Gel Permeation Chromatography (Gpc) Cleanup Coupled With Gc–Ms/Ms, Gc–Nci-Ms, And Lc–Ms/Ms 117<br /> </b><i>Yan-Zhong Cao, Yong-Ming Liu, Na Wang, Xin-Xin Ji, Cui-Cui Yao, Xiang Li, Li-Li Shi, Qiao-Ying Chang, Chun-Lin Fan, and Guo-Fang Pang</i></p> <p>5.1 Introduction 117</p> <p>5.1.1 Persistent Organic Pollutants 118</p> <p>5.1.2 Polycyclic Aromatic Hydrocarbons 119</p> <p>5.1.3 Polychlorinated Biphenyls 119</p> <p>5.1.4 Phthalate Esters 120</p> <p>5.1.5 Multiclass and Multiresidue Analyses 120</p> <p>5.2 Experiment 122</p> <p>5.2.1 Instruments 122</p> <p>5.2.2 Reagents 122</p> <p>5.2.3 Preparation of Standard Solutions 122</p> <p>5.2.4 Sample Preparation 123</p> <p>5.2.5 Analytical Methods 124</p> <p>5.2.6 Qualitative and Quantitative Determination 136</p> <p>5.3 Results and Discussion 136</p> <p>5.3.1 Selection of GPC Cleanup Conditions 136</p> <p>5.3.2 Selection of Extraction Solvent 138</p> <p>5.3.3 Comparison of Sample Extraction Methods 150</p> <p>5.3.4 Comparison of Sample Cleanup 151</p> <p>5.3.5 Linear Range, LOD, and LOQ 152</p> <p>5.3.6 Recoveries and Precisions 152</p> <p>5.3.7 Actual Sample Analysis 157</p> <p>5.4 Conclusions 161</p> <p>References 162</p> <p><b>Chapter 6 Ultrahigh-Performance Liquid Chromatography Coupled With High-Resolution Mass Spectrometry: A Reliable Tool For Analysis Of Veterinary Drugs In Food 167<br /> </b><i>María del Mar Aguilera-Luiz, Roberto Romero-González,</i><i>Patricia Plaza-Bolaños, José Luis Martínez Vidal,</i><i>and Antonia Garrido Frenich</i></p> <p>6.1 Introduction 167</p> <p>6.2 Veterinary Drug Legislation 168</p> <p>6.3 Analytical Techniques for VD Residue Analysis 172</p> <p>6.3.1 Chromatographic Separation 174</p> <p>6.3.2 High-Resolution Mass Spectrometers 175</p> <p>6.4 Food Control Applications 181</p> <p>6.4.1 Screening Applications 181</p> <p>6.4.2 Confirmation and Quantification Methods 191</p> <p>6.4.3 Comparison Studies 195</p> <p>6.5 Conclusions and Future Trends 201</p> <p>Acknowledgments 202</p> <p>References 203</p> <p><b>Chapter 7 A Role For High-Resolution Mass Spectrometry In The High-Throughput Analysis And Identification Of Veterinary Medicinal Product Residues And Of Their Metabolites In Foods Of Animal Origin 213<br /> </b><i>Eric Verdon, Dominique Hurtaud-Pessel,</i><i>and Jagadeshwar-Reddy Thota</i></p> <p>7.1 Introduction 213</p> <p>7.2 Issues Associated with Veterinary Drug Residues and European Regulations 215</p> <p>7.3 Choosing a Strategy: Targeted or Nontargeted Analysis? 216</p> <p>7.3.1 Targeted Analysis Using HRMS 218</p> <p>7.3.2 Nontargeted Analysis Using HRMS: Screening for Unknown Compounds 219</p> <p>7.4 Application Number 1: Identification of Brilliant Green and its Metabolites in Fish under High-Resolution Mass Spectral Conditions (Targeted and Nontargeted Approaches) 220</p> <p>7.5 Application Number 2: Targeted and Nontargeted Screening Approaches for the Identification of Antimicrobial Residues in Meat 223</p> <p>7.6 Conclusions 227</p> <p>References 227</p> <p><b>Chapter 8 High-Throughput Analysis of Mycotoxins 231<br /> </b><i>Marta Vaclavikova, Lukas Vaclavik, and Tomas Cajka</i></p> <p>8.1 Introduction 231</p> <p>8.1.1 Legislation and Regulatory Limits 231</p> <p>8.1.2 Emerging Mycotoxins 237</p> <p>8.1.3 Analysis of Mycotoxins in the High-Throughput Environment 238</p> <p>8.2 Sample Preparation 239</p> <p>8.2.1 Sampling 240</p> <p>8.2.2 Matrices of Interest 240</p> <p>8.2.3 Extraction of Mycotoxins 241</p> <p>8.2.4 Purification of Sample Extracts 246</p> <p>8.3 Separation and Detection of Mycotoxins 247</p> <p>8.3.1 Liquid Chromatography–Mass Spectrometry-Based Methods 248</p> <p>8.3.2 High-Resolution Mass Spectrometry in Mycotoxins Analysis 250</p> <p>8.4 No-Separation Mass Spectrometry-Based Methods 252</p> <p>8.4.1 Matrix-Assisted Laser Desorption Ionization–Mass Spectrometry 252</p> <p>8.4.2 Ambient Ionization Mass Spectrometry 253</p> <p>8.4.3 Ion Mobility Spectrometry 254</p> <p>8.4.4 Immunochemical Methods 256</p> <p>8.5 Conclusions 259</p> <p>Acknowledgments 259</p> <p>References 259</p> <p>Index 267</p>