Overview

Leading the way for analytical chemists developing new techniques. This new comprehensive 5 volume set on separation science provides a much needed research-level text for both academic users and researchers who are working with and developing the most current methods, as well as serving as a valuable resource for graduate and post-graduate students. Comprising of five topical volumes it provides a comprehensive overview of the subject, highlighting aspects that will drive research in this field in the years to come. Volume 1: Liquid Chromatography Volume 2: Special Liquid Chromatography Modes and Capillary Electromigration Techniques Volume 3: Gas, Supercritical and Chiral Chromatography Volume 4: Chromatographic and Related Techniques Volume 5: Sample Treatment, Method Validation, and Applications Key Features: - Comprises over 2,100 pages in 5 volumes – available in print and online - Edited by an international editorial team which has both prominent and experienced senior researchers as well as young and dynamic rising stars - Individual chapters are labeled as either introductory or advanced, in order to guide readers in finding the content at the appropriate level - Fully indexed with cross referencing within and between all 5 volumes

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Author:   Jared Anderson (Iowa State University, Ames, IA) ,  Alain Berthod (University Claude Bernard of Lyon, Villeurbanne, France) ,  Veronica Pino (University of La Laguna (ULL), Canary Islands) ,  Apryll M. Stalcup (Dublin City University's School of Chemical Sciences in Dublin, Ireland)
Publisher:   Wiley-VCH Verlag GmbH
Imprint:   Blackwell Verlag GmbH
Dimensions:   Width: 19.60cm , Height: 21.30cm , Length: 27.90cm
Weight:   5.897kg
ISBN:  

9783527333745

ISBN 10:   3527333746
Pages:   2220
Publication Date:   20 January 2016
Audience:   College/higher education ,  Postgraduate, Research & Scholarly
Format:   Hardback
Publisher's Status:   Active
Availability:   To order  
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Table of Contents

About the Editors XVII Preface XIX List of Contributors XXI Volume 1 1 Basic HPLC Theory and Definitions: Retention, Thermodynamics, Selectivity, Zone Spreading, Kinetics, and Resolution 1 Torgny Fornstedt, Patrik Forssén, and Douglas Westerlund 1.1 Basic Definitions 2 1.1.1 Basic Retention Models and Kinetics 6 1.1.2 Band Broadening and the Plate Height Concept 7 1.1.3 Sources of Zone Broadening 9 1.1.3.1 Eddy Diffusion 10 1.1.3.2 Molecular Diffusion 10 1.1.3.3 Slow Equilibration 10 1.1.4 Dependence of Zone Broadening on Flow Rate 11 1.2 Resolution 12 1.3 Modern Trends in Liquid Chromatography 14 1.3.1 Efficiency Trend 15 1.3.2 Permeability Trend 17 1.3.3 Selectivity and New Material Trend 19 1.4 Conclusions 21 References 22 2 Basic LC Method Development and Optimization 25 Victoria F. Samanidou 2.1 Introduction 25 2.2 Theoretical Aspects 26 2.2.1 Retention Factork 27 2.2.2 Selectivity α 27 2.2.3 Peak Asymmetry 27 2.2.4 Efficiency of Chromatographic Column and Theoretical Plates 27 2.2.5 Resolution Rs 28 2.2.6 The Fundamental vanDeemter Equation 29 2.3 Controlling Resolution 30 2.3.1 How to Improve N 32 2.3.1.1 Physical Characteristics of Packing Material 32 2.3.2 Increase ofk 33 2.3.3 Factors Influencing Selectivity or How to Improve α? 33 2.3.3.1 Optimization of Mobile-Phase Composition 34 2.3.3.2 pH Control, Ion-Pair Reagents, and Other Additives 35 2.3.3.3 Temperature 35 2.3.3.4 Stationary Phase and Column Selection 35 2.3.3.5 Stationary Phase and Packing Material Composition 36 2.4 Method Development Strategy 37 2.4.1 Gradient Elution versus Isocratic 38 2.4.2 Other Parameters in LC Method Development 38 2.5 Current and Future Trends 39 2.5.1 Two-Dimensional Chromatography 39 2.6 Conclusions 40 References 40 3 Recent Advances in Column Technology 43 Ross Andrew Shalliker and Danijela Kocic 3.1 Introduction 43 3.2 Column Packing: Downward Slurry Packing 45 3.3 Column Bed Heterogeneity 46 3.3.1 Axial Heterogeneity 46 3.3.2 Radial Heterogeneity and the Wall Effect 49 3.4 Active Flow Technology: A New Design Concept in Chromatography Columns 51 3.4.1 AFT Columns: Parallel Segmented Flow 51 3.4.2 AFT Columns: Curtain Flow 52 3.4.3 Performance of AFT Columns 53 3.4.3.1 Sensitivity 53 3.4.3.2 Efficiency 54 3.4.3.3 Speed 58 3.5 Summary 60 References 61 4 Hydrophilic Interaction Liquid Chromatography 63 Xinmiao Liang, Aijin Shen, and Zhimou Guo 4.1 Introduction 63 4.2 Separation Mechanism in HILIC 64 4.3 Stationary Phases for HILIC 67 4.3.1 Conventional NPLC Stationary Phases for HILIC 67 4.3.2 Stationary Phases Developed for HILIC 75 4.3.2.1 Polyaspartamide-Based Stationary Phases 75 4.3.2.2 Amide-Based Stationary Phases 75 4.3.2.3 Saccharides-Based Stationary Phases 76 4.3.2.4 Zwitterionic Stationary Phases 76 4.4 Application of HILIC 77 4.4.1 Application in the Pharmaceutical Field 77 4.4.2 Application in the Separation of Carbohydrates 78 4.4.3 Application in Proteome, Glycoproteome, and Phosphoproteome 78 4.4.4 Application in Metabolomics/Metabonomics 80 4.5 Conclusions and Outlook 81 References 81 5 LC–MS Interfaces 87 Pierangela Palma, Elisabetta Pierini, and Achille Cappiello 5.1 Introduction 87 5.2 API Sources 88 5.2.1 Electrospray Interface (ESI) 89 5.2.1.1 Principles of Operation and Ion Formation 90 5.2.1.2 Factors Influencing ESI Response 92 5.2.1.3 Modes of Operation 92 5.2.2 Atmospheric Pressure Chemical Ionization 93 5.2.2.1 Principles of Operation and Ion Formation 94 5.2.3 Atmospheric Pressure Photoionization 95 5.2.3.1 Principle of Operation 96 5.2.4 Atmospheric Pressure Laser Ionization 98 5.2.4.1 Principle of Operation and Ion Formation 98 5.3 Non-API Sources 99 5.3.1 Direct-EI 100 5.3.2 EI of Cold Molecules in Supersonic Molecular Beam (SMB) 103 5.3.3 Combined Single-Photon Low-Pressure Photoionization and EI Ionization 104 5.3.4 LC/DESI–MS Interface 106 References 107 6 LC–MS Applications in Environmental and Food Analysis 111 Alessandra Gentili, Fulvia Caretti, and Virginia Pérez Fernández 6.1 Introduction 111 6.2 Environmental Applications 112 6.2.1 Last Trends in Sample Preparation for LC–MS Analysis 112 6.2.2 Advances and Trends in Liquid Chromatography 113 6.2.3 Advances and Trends in Mass Spectrometry 113 6.3 Food Toxicant Applications 117 6.3.1 Recent Trends in Sample Preparation for LC–MS Analysis 117 6.3.2 Recent Trends in LC–MS Screening Analysis 118 6.3.3 Recent Trends in LC–MS Confirmatory Analysis 120 6.4 Foodomics as a Recent Approach Embracing Metabolomics, Proteomics, and Lipidomics 121 6.4.1 Food Proteomics 121 6.4.2 Food Metabolomics 124 6.4.3 Food Lipidomics 125 6.5 Trends and Future Developments 127 References 128 7 Solvents in Chromatography and Electrophoresis 135 Alain Berthod and Karine Faure 7.1 Introduction 135 7.2 Physicochemical Properties of Solvents 135 7.2.1 Melting and Boiling Points, and Vapor Pressure 135 7.2.2 Molecular Weight, Density, and Molar Volume 136 7.2.3 Viscosity, Surface Tension, UV Cutoff, and Refractive Index 136 7.2.4 Solvent Polarity Scales 137 7.2.5 New Solvents 142 7.3 Physicochemical Properties of Mixtures of Solvents 143 7.3.1 Fully Miscible Solvents 143 7.3.2 Nonfully Miscible Solvents and Phase Diagrams 144 7.3.3 Solvent Mixtures and Chromatographic Retention Times: Elution Strength 146 7.4 Mobile-Phase pH and Buffers 147 7.4.1 pH Definition 147 7.4.2 pH in Hydro-organic Mobile Phases 147 7.4.3 pKa Shifts in Hydro-organic Mobile Phases 148 7.5 Conclusions 151 Acknowledgments 157 References 157 8 Reversed Phase Liquid Chromatography 159 Maria C. García-Alvarez-Coque, Juan J. Baeza-Baeza, and Guillermo Ramis-Ramos 8.1 Introduction 159 8.2 The Stationary Phase 160 8.2.1 Silica Support and Chemical Bonding 161 8.2.2 Types of Phases 163 8.2.3 Silanol Effects 164 8.2.4 Silanol Deactivation 166 8.3 The Mobile Phase 167 8.3.1 Mobile Phase Components 167 8.3.2 Snyder’s Solvent Selectivity Triangle 168 8.3.3 Control of the Mobile-Phase pH 170 8.4 Temperature as Chromatographic Factor 172 8.5 Gradient versus Isocratic Elution 174 8.5.1 Solute Retention and Peak Width 174 8.5.2 Isocratic Elution 175 8.5.3 Gradients of Modifier: The Usual Solution for the General Elution Problem 175 8.5.4 Development of Gradients of Modifier 176 8.5.5 Strengths and Weaknesses of Gradients of Modifier 179 8.5.6 Other Types of Gradients 181 8.6 Attempts to Explain the Retention Mechanisms in RPLC 181 8.6.1 Solvent Adsorption and Partitioning in RPLC 181 8.6.2 The Solvophobic Theory 182 8.6.3 Solute Adsorption or Partitioning? 183 8.6.4 Investigating How RPLC Really Works 184 8.6.5 Going Down to the Molecular Detail 186 8.6.5.1 Chain Conformation 186 8.6.5.2 Adsorption and Partitioning of Common Solvents 186 8.6.5.3 Adsorption and Partitioning of Solutes 188 8.6.5.4 Anomalous Behavior with Highly Aqueous Mobile Phases 189 8.7 Development and Trends in RPLC 190 References 192 9 Modeling of Retention in Reversed Phase Liquid Chromatography 199 Maria C. García-Alvarez-Coque, Guillermo Ramis-Ramos, José R. Torres-Lapasió, and C. Ortiz-Bolsico 9.1 Introduction 199 9.2 Isocratic Elution 199 9.2.1 Polynomial Models to Describe Retention Using Modifier Content as a Factor 199 9.2.2 Polarity Models 201 9.2.3 pH as an Experimental Factor 202 9.3 Dead Time Estimation 206 9.3.1 Static Methods 207 9.3.2 Dynamic Methods 207 9.4 Effect of Temperature 209 9.4.1 Van’t Hoff Equation 209 9.4.2 Combined Effect of Modifier Content, pH, and Temperature 210 9.5 Effect of Pressure 211 9.5.1 Deviations of Retention Factors 211 9.5.2 Correction of Pressure Effects 212 9.6 Enhancing the Prediction of Retention 214 9.6.1 Practical Considerations 214 9.6.2 Influence of the Model Regression Process on the Quality of Predictions 215 9.7 Gradient Elution 216 9.7.1 Integration of the Fundamental Equation for Gradient Elution 216 9.7.2 Nonintegrable Retention Models 217 9.8 Computer-Assisted Interpretive Optimization 218 9.9 Stationary-Phase Characterization 220 9.9.1 Linear Solvation Energy Relationships 220 9.9.2 Local Models for Characterizing RPLC Columns 221 References 223 10 Normal-Phase and Polar Organic Solvents Chromatography 227 Ahmed A. Younes, Charlene Galea, Debby Mangelings, and Y. Vander Heyden 10.1 Introduction 227 10.2 HPLC Retention and Separation Mechanisms 228 10.2.1 Polarity-Based Separations 228 10.2.2 Charge-Based Separations 232 10.2.3 Size-Based Separations 232 10.2.4 Other Separation Mechanisms 232 10.3 Normal-Phase and Polar Organic Solvents Chromatography 233 10.3.1 Retention Mechanism 234 10.3.2 Stationary Phases 234 10.3.2.1 Nonbonded Phases 234 10.3.2.2 Bonded Phases 235 10.3.2.3 Stationary Phases and Selectivity 236 10.3.3 Mobile Phases 238 10.3.3.1 Mobile-Phase Selection 238 10.3.3.2 Solvent Strength and Selectivity 239 10.3.3.3 Isocratic and Gradient Elution 241 10.4 Conclusions 242 References 243 11 Inline Detectors 245 Ramisetti Nageswara Rao and Pothuraju Nageswara Rao 11.1 Introduction 245 11.2 Detector Characteristics 246 11.2.1 Sensitivity 246 11.2.2 Selectivity 246 11.2.3 Linearity 247 11.2.4 Dynamic Range 247 11.2.5 Detector Cell Volume 247 11.3 UV-Visible Absorbance Detector 247 11.3.1 Fixed Wavelength Detector 249 11.3.2 Variable Wavelength Detector 250 11.4 Photodiode Array Detector (PDA) 251 11.5 Fluorescence Detector 252 11.6 Refractive Index Detector (RID) 255 11.7 Evaporative Light-Scattering Detector 256 11.8 Electrochemical Detector 257 11.9 Charged Aerosol Detection 258 11.10 Conductivity Detector 259 11.11 Coupling Detectors 260 11.12 Comparison of HPLC Detectors 260 References 261 12 pH Effects on Chromatographic Retention Modes 263 Paweł Wiczling, Łukasz Kubik, and Roman Kaliszan 12.1 Introduction 263 12.2 pH Measurements of Mobile Phase 264 12.3 Effect of pH on Isocratic Retention 266 12.4 pH Effect on Organic Modifier Gradients 268 12.5 pH Gradient 269 12.6 Determination of pKa, log kw (Hydrophobicity), and S 274 12.7 Effect of pH in Normal-Phase Mode 275 12.8 Summary 277 References 277 13 Chemometrics in Data Analysis and Liquid Chromatographic Method Development 279 Biljana Jančic ́-Stojanovic ́and Tijana Rakic ́ 13.1 Introduction 279 13.2 Chemometrics in Data Analysis 280 13.2.1 Data Preprocessing 280 13.2.2 Data Analysis 284 13.3 Chemometrics in LC Method Development 285 13.3.1 Analytical Target Profile and Critical Quality Attributes (Definition of the Objectives of the Method) 286 13.3.2 Quality Risk Assessment and Critical Process Parameters (Definition of Investigated Factors and Their Levels) 287 13.3.3 Investigation of the Knowledge Space (Selection of an Appropriate Experimental Design) 288 13.3.3.1 Screening Designs 289 13.3.3.2 Optimization Designs 291 13.3.4 Critical Quality Attributes Modeling (Creation of Mathematical Models) 293 13.3.5 Design Space 294 13.3.6 Selection of the Working Points 295 13.3.7 Robustness Testing 295 13.4 Conclusions 296 References 296 Index to Volume 1 I1-I18 Volume 2 Part One Special Liquid Chromatography Modes 299 1 Chiral Liquid Chromatography: Recent Applications with Special Emphasis on the Enantioseparation of Amino Compounds 301 István Ilisz 2 Chiral Separation of Some Classes of Pesticides by HPLC Method 321 Imran Ali, Iqbal Hussain, Mohd Marsin Sanagi, and Hassan Y. Aboul-Enein 3 Micellar Liquid Chromatography: Fundamentals 371 Maria C. García-Alvarez-Coque, Maria J. Ruiz-Angel, and Samuel Carda-Broch 4 Micellar Liquid Chromatography: Method Development and Applications 407 Maria C. García-Alvarez-Coque, Maria J. Ruiz-Angel, and Samuel Carda-Broch 5 Affinity Chromatography 461 Erika L. Pfaunmiller, Jesbaniris Bas, Marissa Brooks, Mitchell Milanuk, Elliott Rodriguez, John Vargas, Ryan Matsuda, and David S. Hage 6 Immunoaffinity Chromatography: Advantages and Limitations 483 Nancy E. Thompson and Richard R. Burgess Part Two Capillary Electromigration Techniques 503 7 Capillary Electromigration Techniques: Capillary Electrophoresis 505 Václav Kašička 8 Modern Injection Modes (Stacking) for CE 531 Joselito P. Quirino 9 Capillary Gel Electrophoresis 555 Márta Kerékgyártó and András Guttman 10 Nonaqueous Capillary Electrophoresis 581 Julie Schappler and Serge Rudaz 11 Detectors in Capillary Electrophoresis 607 Petr Tůma and František Opekar 12 Trends in CE-MS and Applications 629 Anna Tycova and Frantisek Foret 13 Capillary Electrochromatography 653 Kai Zhang and Ruyu Gao 14 Micellar Electrokinetic Chromatography 675 Paolo Iadarola, Marco Fumagalli, and Simona Viglio 15 Chip-Based Capillary Electrophoresis 707 Yuanhong Xu, Jizhen Zhang and Jingquan Liu 16 Chiral Separations by Capillary Electrophoresis 731 E. Sánchez-López, M. Castro-Puyana, M.L. Marina, and A.L. Crego Index to Volume 2 I1-I24 Volume 3 1 Gas Chromatography: Theory and Definitions, Retention and Thermodynamics, and Selectivity 775 Glenn E. Spangler 2 Basic Overview on Gas Chromatography Injectors 807 Md. Musfiqur Rahman, A.M. Abd El-Aty, and Jae-Han Shim 3 Basic Overview on Gas Chromatography Columns 823 Md. Musfiqur Rahman, A.M. Abd El-Aty, Jeong-Heui Choi, Ho-Chul Shin, Sung Chul Shin, and Jae-Han Shim 4 Overview of Detectors in Gas Chromatography 835 Md. Musfiqur Rahman, A.M. Abd El-Aty, and Jae-Han Shim 5 Current Use of Gas Chromatography and Applications 849 Walter Vetter 6 Gas Chromatography with Mass Spectrometry (GC-MS) 883 Walter Vetter 7 Chiral GC 927 Volker Schurig 8 New Essential Events in Modern Applications of Inverse Gas Chromatography 979 Adam Voelkel, Henryk Grajek, Beata Strzemiecka, and Katarzyna Adamska 9 Chip-Based Gas Chromatography 999 Hamza Shakeel and Masoud Agah 10 Portable Gas Chromatography 1021 Philip A. Smith 11 Packed Column Sub- and Supercritical Fluid Chromatography 1051 Caroline West, Syame Khater, and Eric Lesellier 12 Instrumentation for Sub- and Supercritical Fluid Chromatography 1075 Taghi Khayamian, Ali Daneshfar, and Hassan Ghaziaskar Index to Volume 3 I1-I18 Volume 4 1 High-Performance Thin-Layer Chromatography 1093 Vicente L. Cebolla, Luis Membrado, Carmen Jarne, and Rosa Garriga 2 Field Flow Fractionation 1143 Gaëtane Lespes, Julien Gigault, and Serge Battu 3 Separations with a Liquid Stationary Phase: Countercurrent Chromatography or Centrifugal Partition Chromatography 1177 Alain Berthod and Karine Faure 4 Preparative Chromatography: Batch and Continuous 1207 José P.S. Aniceto and Carlos M. Silva 5 Fast and Miniaturized Chromatography 1315 Bárbara Socas-Rodríguez, Antonio V. Herrera-Herrera, Miguel Ángel González-Curbelo, Javier González-Sálamo, and Javier Hernández-Borges 6 Two-Dimensional Liquid Chromatography 1357 Morgan Sarrut, Nicola Marchetti, and Sabine Heinisch Index to Volume 4 I1-I14 Volume 5 1 Sampling Strategies: Statistics of Sampling 1385 Małgorzata Bodnar, Piotr Konieczka, and Jacek Namieśnik 2 Targeted and Non-Targeted Analysis 1401 Luis E. Rodriguez-Saona, Marçal Plans Pujolras, and M. Monica Giusti 3 Conventional Extraction Techniques: Soxhlet and Liquid–Liquid Extractions and Evaporation 1437 Adegbenro Peter Daso and Okechukwu Jonathan Okonkwo 4 Main uses of Microwaves and Ultrasounds in Analytical Extraction Schemes: an Overview 1469 Idaira Pacheco-Fernández, Providencia González-Hernández, Priscilla Rocío-Bautista, María José Trujillo-Rodríguez, and Verónica Pino 5 Membrane-assisted Separations 1503 Jan Åke Jönsson 6 Dispersive Solid-Phase Extraction 1525 Bárbara Socas-Rodríguez, Antonio V. Herrera-Herrera, María Asensio-Ramos, and Javier Hernández-Borges 7 Solid-Phase Extraction 1571 Nil Ozbek, Asli Baysal, Suleyman Akman, and Mehmet Dogan 8 Solid-Phase Microextraction 1595 Ali Mehdinia and Mohammad Ovais Aziz-Zanjani 9 Liquid-Phase Microextraction 1625 Mohammad Reza Ganjali, Morteza Rezapour, Parviz Norouzi, and Farnoush Faridbod 10 Analytical Supercritical Fluid Extraction 1659 Julian Martínez and Ana Carolina de Aguiar 11 Extraction Methods Facilitated by the use of Magnetic Nanoparticles 1681 Priscilla Rocío-Bautista and Verónica Pino 12 Sample Derivatization in Separation Science 1725 Pascal Cardinael, Hervé Casabianca, Valerie Peulon-Agasse, and Alain Berthod 13 Validation of Analytical Methods Based on Chromatographic Techniques: An Overview 1757 Juan Peris-Vicente, Josep Esteve-Romero, and Samuel Carda-Broch 14 “Omics” and Biomedical Applications 1809 Pasquale Ferranti, Chiara Nitride, and Monica Gallo 15 Food Applications: Using Novel Sample Preparation Modes 1859 Mónica González and Venerando González 16 Forensic Applications 1877 Matías Calcerrada Guerreiro, María López-López, Ma Ángeles Fernández de la Ossa, and Carmen García-Ruiz 17 Environmental Applications of Solid Phase Microextraction Techniques 1897 Sarah Montesdeoca-Esponda, M Esther Torres-Padrón, Zoraida Sosa-Ferrera, and José Juan Santana-Rodríguez Index to Volume 5 I1-I20 Index 1929

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Jared L. Anderson is a Professor of Chemistry in the Department of Chemistry at Iowa State University in Ames, Iowa. He obtained his B.S. degree from South Dakota State University in 2000 and his Ph.D. in analytical chemistry from Iowa State University in 2005. He was an assistant, associate, and full professor of chemistry in the Department of Chemistry and Biochemistry at the University of Toledo (Ohio) before joining the faculty at Iowa State University in August 2015. He was awarded the ""Emerging Leader in Chromatography Award"" in 2010 by LCGC North America and the ""Young Investigator in Separation Science Award"" by the American Chemical Society in 2012. He is also the recipient of the 2016 Pittsburgh Conference Achievement Award given by the Society for Analytical Chemists of Pittsburgh. He has authored over 100 peer-reviewed publications. Alain Berthod graduated in 1979 from University Claude Bernard of Lyon, Villeurbanne, France. He took a research position at the French National Center for Scientific Research (CNRS), where he made his career ending as a Research Director in the Institute of Analytical Sciences. He was granted the ""emeritus"" status in 2015. He is a member of the editorial board of several analytical journals and the editor of Separation & Purification Reviews. He has edited seven symposium volumes and authored three books and over 250 articles, reviews, and book chapters. Veronica Pino is a Professor in the Department of Chemistry, Analytical Division of the University of La Laguna (ULL), Canary Islands. She obtained a Ph.D. degree in Analytical Chemistry in 2002 from ULL, with Doctorate Extraordinary Award and Special Mention for Young Canary Researchers from the Canary Government. She has conducted several research stays during her career, including Wake Forest University, Canary Institute of Agrarian Research, Iowa State University, University of Toledo, and University Claude Bernard. She was awarded with a prestigious ""Ramon y Cajal"" research associate position in 2010 at ULL. She has authored over 70 articles, reviews, and book chapters. Apryll Stalcup is Professor of Analytical Chemistry at Dublin City University's School of Chemical Sciences in Dublin, Ireland, where she heads the Irish Separation Science Cluster. A graduate from Georgetown University, she held professorships at the University of Hawaii and the University of Cincinnati before moving to Dublin in 2012.

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