High-Throughput Analysis for Food Safety

PERRY G. WANG, PHD, is a research chemist in the Office of Regulatory Science, CFSAN, US FDA. Prior to joining the FDA, Dr. Wang worked in the pharmaceutical and medical device industries. His expertise in the pharmaceutical field focuses on high-throughput drug analysis by LC-MS/MS. His current research at the FDA includes developing analytical methods for chemical ingredients in cosmetics and personal care products by GC-MS/MS and LC-MS/MS. This book is edited in his private capacity but not as an employee of the FDA.MARK F. VITHA, PHD, is a professor at Drake University. He is the editor of The Chemical Analysis Series (Wiley) and the co-editor of Interfaces and Interphases in Analytical Chemistry. In 2011, he was awarded the Windsor Professor of Science and the Ronald D. Troyer Research Fellowship. JOHN F. KAY, PHD, is a chemist and recently retired as the R&D manager at the UK Veterinary Medicines Directorate. For almost 20 years he actively participated in the Codex Alimentarius Committee on Residues of Veterinary Drugs in Food and remains on the JECFA expert roster 2012-2016 for veterinary drug residues. He has held an Honorary Senior Research Fellowship in the Department of Mathematics and Statistics at the University of Strathclyde, Scotland since 2005.

• Preface xiContributors xiiiChapter 1 Introduction: Basic Principles of Assays to be Covered, Sample Handling, And Sample Processing 1Wanlong Zhou, Eugene Y. Chang, and Perry G. Wang1.1 Introduction 11.1.1 Current Situation and Challenges of Food Safety and Regulations 11.1.2 Residues and Matrices of Food Analysis and High-Throughput Analysis 21.1.3 Food Safety Classifications 31.1.4 “High Throughput” Definition 31.1.5 Scope of the Book 41.2 Advanced Sample Preparation Techniques 51.2.1 Automation of Weighing and Preparing Standard Solutions 51.2.2 QuEChERS 61.2.3 Swedish Extraction Technique (SweEt) and Other Fast Sample Preparation Methods 61.2.4 Turbulent Flow Chromatography 71.2.5 Pressurized Liquid Extraction 71.2.6 Automated 96- and 384-Well Formatted Sample Preparation as well as Automated SPE Workstations 81.2.7 Solid-Phase Microextraction 81.2.8 Microextraction by Packed Sorbent 91.2.9 Liquid Extraction Surface Analysis 91.2.10 Headspace GC 101.2.11 Summary 101.3 Future Perspectives 10Acknowledgment 11References 11Chapter 2 Survey Of Mass Spectrometry-Based High-Throughput Methods In Food Analysis 15Lukas Vaclavik, Tomas Cajka, Wanlong Zhou, and Perry G. Wang2.1 Introduction 152.2 Techniques Employing Chromatographic Separation 152.2.1 Gas Chromatography–Mass Spectrometry 152.2.2 Liquid Chromatography–Mass Spectrometry 212.3 Direct Techniques 302.3.1 Matrix-Assisted Laser Desorption/Ionization-Mass Spectrometry 302.3.2 Headspace (Solid-Phase Microextraction)-Mass Spectrometry E-Nose 372.3.3 Ambient Desorption/Ionization-Mass Spectrometry 382.4 Concluding Remarks 62Acknowledgments 62References 63Chapter 3 Quality Systems, Quality Control Guidelines and Standards, Method Validation, and Ongoing Analytical Quality Control 73David Galsworthy and Stewart Reynolds3.1 Introduction 733.1.1 Quality System Design 733.1.2 Procedures 743.1.3 Roles and Responsibilities 743.1.4 Quality Manual 743.1.5 Document Control 743.1.6 Control of Records 753.1.7 Audits 753.1.8 Validation of Methodology 753.1.9 Staff Competency 753.1.10 Internal Quality Control 763.1.11 Method Performance Criteria 763.2 Qualitative Screening Methods 763.2.1 Selectivity of Mass Spectrometry-Based Methods 783.2.2 Confirmatory Methods 783.2.3 Validation of Qualitative Screening Multiresidue Methods for Pesticide Residues in Foods 793.3 Elements of the Analytical Workflow 803.3.1 Sample Preparation 803.3.2 Effects of Sample Processing 813.3.3 Extraction Efficiency 813.4 Initial Method Validation 813.5 Ongoing Analytical Quality Control 863.5.1 Internal Quality Control 863.5.2 Proficiency Testing 863.6 Validation of Qualitative Screening Multiresidue Methods for Veterinary Drug Residues in Foods 873.6.1 EU Legislation Covering Method Validation for Veterinary Drug Screening 873.6.2 Determination of Specificity/Selectivity and Detection Capability (CCβ) Using the Classical Approach 883.6.3 Establishment of a Cutoff Level and Calculation of CCβ 883.6.4 Determination of the Applicability 893.7 Conclusions 90References 90Chapter 4 Deliberate Chemical Contamination and Processing Contamination 93Stephen Lock4.1 Introduction 934.2 Heat-Induced Food Processing Contaminants 974.3 Packaging Migrants 1014.4 Malicious Contamination of Food 105References 111Chapter 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 117Yan-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 Pang5.1 Introduction 1175.1.1 Persistent Organic Pollutants 1185.1.2 Polycyclic Aromatic Hydrocarbons 1195.1.3 Polychlorinated Biphenyls 1195.1.4 Phthalate Esters 1205.1.5 Multiclass and Multiresidue Analyses 1205.2 Experiment 1225.2.1 Instruments 1225.2.2 Reagents 1225.2.3 Preparation of Standard Solutions 1225.2.4 Sample Preparation 1235.2.5 Analytical Methods 1245.2.6 Qualitative and Quantitative Determination 1365.3 Results and Discussion 1365.3.1 Selection of GPC Cleanup Conditions 1365.3.2 Selection of Extraction Solvent 1385.3.3 Comparison of Sample Extraction Methods 1505.3.4 Comparison of Sample Cleanup 1515.3.5 Linear Range, LOD, and LOQ 1525.3.6 Recoveries and Precisions 1525.3.7 Actual Sample Analysis 1575.4 Conclusions 161References 162Chapter 6 Ultrahigh-Performance Liquid Chromatography Coupled With High-Resolution Mass Spectrometry: A Reliable Tool For Analysis Of Veterinary Drugs In Food 167María del Mar Aguilera-Luiz, Roberto Romero-González,Patricia Plaza-Bolaños, José Luis Martínez Vidal,and Antonia Garrido Frenich6.1 Introduction 1676.2 Veterinary Drug Legislation 1686.3 Analytical Techniques for VD Residue Analysis 1726.3.1 Chromatographic Separation 1746.3.2 High-Resolution Mass Spectrometers 1756.4 Food Control Applications 1816.4.1 Screening Applications 1816.4.2 Confirmation and Quantification Methods 1916.4.3 Comparison Studies 1956.5 Conclusions and Future Trends 201Acknowledgments 202References 203Chapter 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 213Eric Verdon, Dominique Hurtaud-Pessel,and Jagadeshwar-Reddy Thota7.1 Introduction 2137.2 Issues Associated with Veterinary Drug Residues and European Regulations 2157.3 Choosing a Strategy: Targeted or Nontargeted Analysis? 2167.3.1 Targeted Analysis Using HRMS 2187.3.2 Nontargeted Analysis Using HRMS: Screening for Unknown Compounds 2197.4 Application Number 1: Identification of Brilliant Green and its Metabolites in Fish under High-Resolution Mass Spectral Conditions (Targeted and Nontargeted Approaches) 2207.5 Application Number 2: Targeted and Nontargeted Screening Approaches for the Identification of Antimicrobial Residues in Meat 2237.6 Conclusions 227References 227Chapter 8 High-Throughput Analysis of Mycotoxins 231Marta Vaclavikova, Lukas Vaclavik, and Tomas Cajka8.1 Introduction 2318.1.1 Legislation and Regulatory Limits 2318.1.2 Emerging Mycotoxins 2378.1.3 Analysis of Mycotoxins in the High-Throughput Environment 2388.2 Sample Preparation 2398.2.1 Sampling 2408.2.2 Matrices of Interest 2408.2.3 Extraction of Mycotoxins 2418.2.4 Purification of Sample Extracts 2468.3 Separation and Detection of Mycotoxins 2478.3.1 Liquid Chromatography–Mass Spectrometry-Based Methods 2488.3.2 High-Resolution Mass Spectrometry in Mycotoxins Analysis 2508.4 No-Separation Mass Spectrometry-Based Methods 2528.4.1 Matrix-Assisted Laser Desorption Ionization–Mass Spectrometry 2528.4.2 Ambient Ionization Mass Spectrometry 2538.4.3 Ion Mobility Spectrometry 2548.4.4 Immunochemical Methods 2568.5 Conclusions 259Acknowledgments 259References 259Index 267