Fast Liquid Chromatography-mass Spectrometry Methods In Food And Environmental Analysis

by Oscar Nunez, Hector Gallart-ayala, Claudia P B Martins, Paolo Lucci

Overview

There is a growing need for high-throughput separations in food and environmental research that are able to cope with the analysis of a large number of compounds in very complex matrices. Whereas the most common approach for solving many analytical problems has often been high-performance liquid chromatography (HPLC), the recent use of fast or ultra-fast chromatographic methods for environmental and food analysis has increased the overall sample throughput and laboratory efficiency without loss (and even with an improvement) in the resolution obtained by conventional HPLC systems.This book brings together researchers at the top of their field from across the world to discuss and analyze recent advances in fast liquid chromatography-mass spectrometry (LC-MS) methods in food and environmental analysis. First, the most novel approaches to achieve fast and ultra-fast methods as well as the use of alternative and complementary stationary phases are described. Then, recent advances in fast LC-MS methods are addressed, focusing on novel treatment procedures coupled with LC-MS, new ionization sources, high-resolution mass spectrometry, and the problematic confirmation and quantification aspects in mass spectrometry. Finally, relevant LC-MS applications in food and environmental analysis such as the analysis of pesticides, mycotoxins, food packaging contaminants, perfluorinated compounds and polyphenolic compounds are described.The scope of the book is intentionally broad and is aimed at worldwide analytical laboratories working in food and environmental applications as well as researchers in universities worldwide.

Product Details

ISBN-13:	9781783264933
Publisher:	Imperial College Press
Publication date:	04/27/2015
Pages:	624
Product dimensions:	5.90(w) x 9.10(h) x 1.30(d)

Table of Contents

Preface xvii

Part 1 Fast Liquid Chromatography Advances 1

Chapter 1 UHPLC Separations Using Sub-2pm Particle Size Columns Julie Schappler Jean-Luc Veuthey Davy Guillarme 3

1.1 General Introduction to Ultrahigh Performance Liquid Chromatography (UHPLC) 3

1.2 Proof-of-Concept of Ultrahigh-Pressure Liquid Chromatography (UHPLC) During the 1990s 5

1.3 Benefits of UHPLC Technique: Speed, Resolution, Solvent Consumption and Sensitivity 7

1.4 Method Transfer between HPLC and UHPLC 10

1.4.1 Rules and examples in the isocratic mode 10

1.4.2 Rules and examples in the gradient mode 12

1.5 The Importance of Instrumentation in UHPLC 14

1.5.1 Extra-column band broadening 14

1.5.2 System dwell volume 18

1.5.3 System upper pressure limit 19

1.5.4 Detector data acquisition rate for UHPLC operation 21

1.5.5 Overview of UHPLC instruments and columns on the market 21

1.6 The Importance of Frictional Heating under Very High Pressure Conditions 23

1.7 Comparison of UHPLC Performance with Other Modern LC Strategies 25

1.8 Conclusions and Perspectives 26

References 28

Chapter 2 Core-Shell Column Technology in Fast Liquid Chromatography Oscar Núñez Héctor Gallart-Ayala 33

2.1 Introduction 33

2.2 Fused-Core Technology: Benefits and New Possibilities 34

2.3 Overview of Columns on the Market 39

2.4 Core-Shell Column Technology in Food and Environmental Analysis 45

2.5 Concluding Remarks 51

References 52

Chapter 3 Monolithic Columns in Fast Liquid Chromatography Takeshi Hara Oscar Núñez Tohru Ikegami Nobuo Tanaka 57

3.1 Features of Monolithic Silica Columns: Rapid Separation Using Monolithic Silica Columns in Rod and Capillary Formats 57

3.1.1 Fabrication of columns 57

3.1.2 The support structure regarding through-pores, skeletons, and amount of silica in a column 60

3.1.3 Column permeability, column efficiency, and improvement of preparation method 62

3.1.4 Current performance of monolithic silica columns 68

3.1.5 Kinetic performance 71

3.1.6 Functionalization of monolithic silica columns 73

3.1.7 Advantages and disadvantages: roles of monolithic silica columns 74

3.2 Features of Organic Polymer Monolithic Columns 79

3.3 Food and Environmental Applications 84

3.4 Summary and Conclusions 93

References 95

Chapter 4 High-Temperature Liquid Chromatography Thorsten Teutenberg 109

4.1 A Brief Definition of High-Temperature Liquid Chromatography 109

4.1.1 Using high eluent temperatures for increasing the separation speed 110

4.1.2 Using high eluent temperatures for modulation of solvent strength 112

4.2 Instrumental Requirements 115

4.3 Suitable Stationary Phases 119

4.3.1 Silica-based stationary phases 119

4.3.2 Porous graphitic carbon 121

4.3.3 Metal oxide stationary phases 121

4.3.4 Polymeric stationary phases 122

4.4 Retention Time Modeling 122

4.4.1 Van't Hoff equation 122

4.4.2 Isothermal separations 123

4.4.3 Temperature programmed separations 125

4.4.4 Multi-gradient separations 127

4.5 Special Hyphenation Techniques 127

4.5.1 Isotope ratio mass spectrometry 127

4.5.2 LC Taste® 130

4.6 Applications Relevant to Environmental Analysis 131

4.7 Applications Relevant to Food Analysis 132

4.8 General Conclusions and Outlook 133

References 134

Chapter 5 Hydrophilic Interaction Liquid Chromatography (HILIC) and Perfluorinated Stationary Phases Cristina C. Jacob Héctor Gallart-Ayala Gonçalo Gamboa da Costa 149

5.1 Introduction 149

5.2 Hydrophilic Interaction Liquid Chromatography (HILIC) 150

5.2.1 HILIC stationary phases 151

5.2.2 Retention mechanism 156

5.2.3 Practical aspects 157

5.3 Fluorinated Stationary Phases 171

5.4 Summary 178

Disclaimer 179

References 179

Part 2 Advances in Fast Liquid Chromatography-Mass Spectrometry Methods 185

Chapter 6 On-Line Sample Pre-Treatment Procedures Applied to LC-MS Tony Edge Joseph Herman 187

6.1 Introduction 187

6.2 Off-Line Approaches to Sample Preparation 188

6.2.1 QuEChERS 188

6.2.2 Protein precipitation 189

6.2.3 Liquid-liquid extraction 190

6.3 How a Mass Spectrometer Works and Ion Suppression 191

6.3.1 Measuring matrix effects 192

6.4 Other Matrix Effects 193

6.4.1 Method robustness 193

6.4.2 System robustness 194

6.4.3 Carryover 195

6.5 On-Line Approaches 205

6.5.1 Use of switching valves 206

6.5.2 Discussion of different configurations available 207

6.6 On-Line SPE 212

6.6.1 Theory of SPE 212

6.6.2 Some general considerations 212

6.6.3 Mechanisms 212

6.6.4 Practical considerations with on-line SPE 215

6.7 Turbulent Flow Chromatography 221

6.7.1 Theory of TFC 221

6.7.2 Practical considerations with TFC 223

6.8 MIPs 228

6.8.1 Theory and manufacture of MIPs 229

6.8.2 Practical considerations with MIPs 232

6.9 Restricted-Access Media (RAM) 239

6.9.1 Theory of RAM 239

6.9.2 Practical considerations with RAM 241

6.10 Discussion on Future and Other Technologies 244

6.11 Conclusion 245

References 247

Chapter 7 Ambient Mass Spectrometry: Food and Environmental Applications Tiina J. Kauppila Anu Vaikkinen 271

7.1 Ambient Mass Spectrometry Techniques 271

7.1.1 Desorption electrospray ionization (DESI) 271

7.1.2 Direct analysis in real time (DART) 273

7.1.3 Desorption atmospheric pressure photoionization (DAPPI) 275

7.2 Food Analysis 276

7.2.1 Pesticides and fungicides 276

7.2.2 Food chemistry 282

7.2.3 Authenticity assessment 289

7.2.4 Quality control 291

7.2.5 Food packaging/tableware 293

7.2.6 Food safety 294

7.3 Environmental Analysis 296

7.3.1 Analysis of toxic compounds from contaminated surfaces 296

7.3.2 Water 305

7.3.3 Volatile organic compounds and atmospheric aerosols 308

7.3.4 Species identification by chemotyping 311

7.4 Conclusions 312

References 313

Chapter 8 Liquid Chromatography-High-Resolution Mass Spectrometry in Environmental and Food Analysis Paolo Lucci Claudia P. B. Martins 325

8.1 Introduction 325

8.2 The Use and Applicability of LC-HRMS 327

8.3 Is LC-HRMS Overtaking LC-MS/MS? 332

8.4 Confirmatory Strategies 334

8.5 The Identification of Unknowns 340

8.6 Conclusions and Future Perspectives 341

References 341

Chapter 9 Liquid Chromatography-Mass Spectrometry: Quantification and Confirmation Aspects Jaume Aceña Daniel Rivas Bozo Zonja Sandra Pérez Damià Barceló 347

9.1 Introduction 347

9.2 Increasing Chromatographic Resolution: from HPLC to UHPLC 348

9.3 From Low- to High-Resolution Mass Spectrometry Instruments 350

9.4 Method Validation 352

9.4.1 Accuracy, precision and recovery 353

9.4.2 Linearity, sensitivity and stability 353

9.4.3 Selectivity of the method 354

9.5 Quantification and Confirmation in LC-MS 359

9.5.1 Quantification with LC/LR-MS/MS 359

9.5.2 Confirmation aspects in LC/LR-MS/MS 360

9.5.3 Quantification with LC-HRMS 364

9.5.4 Confirmation aspects in LC-HRMS 366

9.6 Conclusions and Future Needs 369

Acknowledgements 370

References 371

Part 3 Relevant LC-MS Applications in Food and Environmental Analysis 379

Chapter 10 Multiresidue Analysis of Pesticides: LC-MS/MS versus LC-HRMS Juan V. Sancho María Ibáñez 381

10.1 Introduction 381

10.2 LC-MS/MS (QqQ) 384

10.3 High-Resolution Mass Spectrometry 389

10.3.1 Target screening of pesticides 391

10.3.2 Non-target screening 397

10.3.3 Elucidation of metabolites and degradation products 401

10.4 Conclusions and Future Trends 403

References 404

Chapter 11 Food-Packaging Contaminants Silvia Lacorte Montse Cortina Albert Guart Antonio Borrell 421

11.1 Introduction 421

11.2 Hazardous Compounds in Food-Packaging Materials 428

11.2.1 Alkyiphenols and phenols 433

11.2.2 Phthalates 434

11.2.3 Bisphenol A and related compounds 435

11.2.4 UV filters 436

11.2.5 Perfluorochemicals 437

11.2.6 Primary aromatic amines 437

11.2.7 NIAS 438

11.3 Sample Preparation 438

11.3.1 Solid food matrices 440

11.3.2 Liquid matrices 444

11.4 Analytical Methodologies 450

11.5 Migration: Overall and Specific Migration 454

11.6 Food Packaging Migration Studies 466

11.7 General Legislation 471

11.8 Conclusions 472

Acknowledgements 473

References 473

Chapter 12 Liquid Chromatography-Mass Spectrometry for the Analysis of Perfluorinated Compounds in Water Samples Marianna Rusconi Stefano Polesello Sara Valsecchi 485

12.1 Introduction 485

12.2 Analytical Challenges in the Analysis of Perfluorinated Compounds in Water 486

12.3 Novel Approaches for High-Throughput Sample Extraction Procedures 487

12.3.1 Off-line extraction methods 488

12.3.2 Automation in extraction procedures 492

12.4 Advanced Chromatographic Separation for the Determination of PFAS in Water Samples 502

12.4.1 Advanced stationary phases 502

12.4.2 From conventional HPLC to UHPLC and nano-HPLC 503

12.5 Advances in the Mass Spectrometric Detection of Perfluorinated Compounds 505

12.6 Conclusions 508

References 509

Chapter 13 Determination of Phenolic Compounds in Food Matrices: Application to Characterization and Authentication Javier Saurina Sonia Sentellas 517

13.1 Introduction 517

13.2 Polyphenols 518

13.3 Metabolomic Approach 523

13.3.1 Flowchart of metabolomics 525

13.4 Data Analysis 527

13.5 Determination of Polyphenols by LC-MS 530

13.5.1 Sample treatment 530

13.5.2 Chromatographic methods 533

13.5.3 LC-MS methods 533

13.6 Concluding Remarks 539

References 540

Chapter 14 Liquid Chromatography-Mass Spectrometric Analysis of Mycotoxins in Food Veronica M. T. Lattanzio Angelo Visconti 549

14.1 Introduction 549

14.2 LC-MS Analysis of Multiple Mycotoxins: Sample Preparation Aspects 559

14.3 The Potential of High-Resolution Mass Spectrometry in Mycotoxin Analysis 564

14.4 Matrix Effects in LC-MS Determination of Mycotoxins 566

14.5 Performance Evaluation of LC-MS Methods for Multiple-Mycotoxin Determination 571

14.6 LC-MS Identification and Determination of Masked Mycotoxins 573

14.7 LC-MS-Rased Multi-Class Methods 575

14.8 Conclusions 578

References 579

Index 591