Analytical Separation Science, 5 Volume Set

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.

• About the Editors XVIIPreface XIXList of Contributors XXIVolume 11 Basic HPLC Theory and Definitions: Retention, Thermodynamics, Selectivity, Zone Spreading, Kinetics, and Resolution 1Torgny Fornstedt, Patrik Forssén, and Douglas Westerlund1.1 Basic Definitions 21.1.1 Basic Retention Models and Kinetics 61.1.2 Band Broadening and the Plate Height Concept 71.1.3 Sources of Zone Broadening 91.1.3.1 Eddy Diffusion 101.1.3.2 Molecular Diffusion 101.1.3.3 Slow Equilibration 101.1.4 Dependence of Zone Broadening on Flow Rate 111.2 Resolution 121.3 Modern Trends in Liquid Chromatography 141.3.1 Efficiency Trend 151.3.2 Permeability Trend 171.3.3 Selectivity and New Material Trend 191.4 Conclusions 21References 222 Basic LC Method Development and Optimization 25Victoria F. Samanidou2.1 Introduction 252.2 Theoretical Aspects 262.2.1 Retention Factork 272.2.2 Selectivity α 272.2.3 Peak Asymmetry 272.2.4 Efficiency of Chromatographic Column and Theoretical Plates 272.2.5 Resolution Rs 282.2.6 The Fundamental vanDeemter Equation 292.3 Controlling Resolution 302.3.1 How to Improve N 322.3.1.1 Physical Characteristics of Packing Material 322.3.2 Increase ofk 332.3.3 Factors Influencing Selectivity or How to Improve α? 332.3.3.1 Optimization of Mobile-Phase Composition 342.3.3.2 pH Control, Ion-Pair Reagents, and Other Additives 352.3.3.3 Temperature 352.3.3.4 Stationary Phase and Column Selection 352.3.3.5 Stationary Phase and Packing Material Composition 362.4 Method Development Strategy 372.4.1 Gradient Elution versus Isocratic 382.4.2 Other Parameters in LC Method Development 382.5 Current and Future Trends 392.5.1 Two-Dimensional Chromatography 392.6 Conclusions 40References 403 Recent Advances in Column Technology 43Ross Andrew Shalliker and Danijela Kocic3.1 Introduction 433.2 Column Packing: Downward Slurry Packing 453.3 Column Bed Heterogeneity 463.3.1 Axial Heterogeneity 463.3.2 Radial Heterogeneity and the Wall Effect 493.4 Active Flow Technology: A New Design Concept in Chromatography Columns 513.4.1 AFT Columns: Parallel Segmented Flow 513.4.2 AFT Columns: Curtain Flow 523.4.3 Performance of AFT Columns 533.4.3.1 Sensitivity 533.4.3.2 Efficiency 543.4.3.3 Speed 583.5 Summary 60References 614 Hydrophilic Interaction Liquid Chromatography 63Xinmiao Liang, Aijin Shen, and Zhimou Guo4.1 Introduction 634.2 Separation Mechanism in HILIC 644.3 Stationary Phases for HILIC 674.3.1 Conventional NPLC Stationary Phases for HILIC 674.3.2 Stationary Phases Developed for HILIC 754.3.2.1 Polyaspartamide-Based Stationary Phases 754.3.2.2 Amide-Based Stationary Phases 754.3.2.3 Saccharides-Based Stationary Phases 764.3.2.4 Zwitterionic Stationary Phases 764.4 Application of HILIC 774.4.1 Application in the Pharmaceutical Field 774.4.2 Application in the Separation of Carbohydrates 784.4.3 Application in Proteome, Glycoproteome, and Phosphoproteome 784.4.4 Application in Metabolomics/Metabonomics 804.5 Conclusions and Outlook 81References 815 LC–MS Interfaces 87Pierangela Palma, Elisabetta Pierini, and Achille Cappiello5.1 Introduction 875.2 API Sources 885.2.1 Electrospray Interface (ESI) 895.2.1.1 Principles of Operation and Ion Formation 905.2.1.2 Factors Influencing ESI Response 925.2.1.3 Modes of Operation 925.2.2 Atmospheric Pressure Chemical Ionization 935.2.2.1 Principles of Operation and Ion Formation 945.2.3 Atmospheric Pressure Photoionization 955.2.3.1 Principle of Operation 965.2.4 Atmospheric Pressure Laser Ionization 985.2.4.1 Principle of Operation and Ion Formation 985.3 Non-API Sources 995.3.1 Direct-EI 1005.3.2 EI of Cold Molecules in Supersonic Molecular Beam (SMB) 1035.3.3 Combined Single-Photon Low-Pressure Photoionization and EI Ionization 1045.3.4 LC/DESI–MS Interface 106References 1076 LC–MS Applications in Environmental and Food Analysis 111Alessandra Gentili, Fulvia Caretti, and Virginia Pérez Fernández6.1 Introduction 1116.2 Environmental Applications 1126.2.1 Last Trends in Sample Preparation for LC–MS Analysis 1126.2.2 Advances and Trends in Liquid Chromatography 1136.2.3 Advances and Trends in Mass Spectrometry 1136.3 Food Toxicant Applications 1176.3.1 Recent Trends in Sample Preparation for LC–MS Analysis 1176.3.2 Recent Trends in LC–MS Screening Analysis 1186.3.3 Recent Trends in LC–MS Confirmatory Analysis 1206.4 Foodomics as a Recent Approach Embracing Metabolomics, Proteomics, and Lipidomics 1216.4.1 Food Proteomics 1216.4.2 Food Metabolomics 1246.4.3 Food Lipidomics 1256.5 Trends and Future Developments 127References 1287 Solvents in Chromatography and Electrophoresis 135Alain Berthod and Karine Faure7.1 Introduction 1357.2 Physicochemical Properties of Solvents 1357.2.1 Melting and Boiling Points, and Vapor Pressure 1357.2.2 Molecular Weight, Density, and Molar Volume 1367.2.3 Viscosity, Surface Tension, UV Cutoff, and Refractive Index 1367.2.4 Solvent Polarity Scales 1377.2.5 New Solvents 1427.3 Physicochemical Properties of Mixtures of Solvents 1437.3.1 Fully Miscible Solvents 1437.3.2 Nonfully Miscible Solvents and Phase Diagrams 1447.3.3 Solvent Mixtures and Chromatographic Retention Times: Elution Strength 1467.4 Mobile-Phase pH and Buffers 1477.4.1 pH Definition 1477.4.2 pH in Hydro-organic Mobile Phases 1477.4.3 pKa Shifts in Hydro-organic Mobile Phases 1487.5 Conclusions 151Acknowledgments 157References 1578 Reversed Phase Liquid Chromatography 159Maria C. García-Alvarez-Coque, Juan J. Baeza-Baeza, and Guillermo Ramis-Ramos8.1 Introduction 1598.2 The Stationary Phase 1608.2.1 Silica Support and Chemical Bonding 1618.2.2 Types of Phases 1638.2.3 Silanol Effects 1648.2.4 Silanol Deactivation 1668.3 The Mobile Phase 1678.3.1 Mobile Phase Components 1678.3.2 Snyder’s Solvent Selectivity Triangle 1688.3.3 Control of the Mobile-Phase pH 1708.4 Temperature as Chromatographic Factor 1728.5 Gradient versus Isocratic Elution 1748.5.1 Solute Retention and Peak Width 1748.5.2 Isocratic Elution 1758.5.3 Gradients of Modifier: The Usual Solution for the General Elution Problem 1758.5.4 Development of Gradients of Modifier 1768.5.5 Strengths and Weaknesses of Gradients of Modifier 1798.5.6 Other Types of Gradients 1818.6 Attempts to Explain the Retention Mechanisms in RPLC 1818.6.1 Solvent Adsorption and Partitioning in RPLC 1818.6.2 The Solvophobic Theory 1828.6.3 Solute Adsorption or Partitioning? 1838.6.4 Investigating How RPLC Really Works 1848.6.5 Going Down to the Molecular Detail 1868.6.5.1 Chain Conformation 1868.6.5.2 Adsorption and Partitioning of Common Solvents 1868.6.5.3 Adsorption and Partitioning of Solutes 1888.6.5.4 Anomalous Behavior with Highly Aqueous Mobile Phases 1898.7 Development and Trends in RPLC 190References 1929 Modeling of Retention in Reversed Phase Liquid Chromatography 199Maria C. García-Alvarez-Coque, Guillermo Ramis-Ramos, José R. Torres-Lapasió, and C. Ortiz-Bolsico9.1 Introduction 1999.2 Isocratic Elution 1999.2.1 Polynomial Models to Describe Retention Using Modifier Content as a Factor 1999.2.2 Polarity Models 2019.2.3 pH as an Experimental Factor 2029.3 Dead Time Estimation 2069.3.1 Static Methods 2079.3.2 Dynamic Methods 2079.4 Effect of Temperature 2099.4.1 Van’t Hoff Equation 2099.4.2 Combined Effect of Modifier Content, pH, and Temperature 2109.5 Effect of Pressure 2119.5.1 Deviations of Retention Factors 2119.5.2 Correction of Pressure Effects 2129.6 Enhancing the Prediction of Retention 2149.6.1 Practical Considerations 2149.6.2 Influence of the Model Regression Process on the Quality of Predictions 2159.7 Gradient Elution 2169.7.1 Integration of the Fundamental Equation for Gradient Elution 2169.7.2 Nonintegrable Retention Models 2179.8 Computer-Assisted Interpretive Optimization 2189.9 Stationary-Phase Characterization 2209.9.1 Linear Solvation Energy Relationships 2209.9.2 Local Models for Characterizing RPLC Columns 221References 22310 Normal-Phase and Polar Organic Solvents Chromatography 227Ahmed A. Younes, Charlene Galea, Debby Mangelings, and Y. Vander Heyden10.1 Introduction 22710.2 HPLC Retention and Separation Mechanisms 22810.2.1 Polarity-Based Separations 22810.2.2 Charge-Based Separations 23210.2.3 Size-Based Separations 23210.2.4 Other Separation Mechanisms 23210.3 Normal-Phase and Polar Organic Solvents Chromatography 23310.3.1 Retention Mechanism 23410.3.2 Stationary Phases 23410.3.2.1 Nonbonded Phases 23410.3.2.2 Bonded Phases 23510.3.2.3 Stationary Phases and Selectivity 23610.3.3 Mobile Phases 23810.3.3.1 Mobile-Phase Selection 23810.3.3.2 Solvent Strength and Selectivity 23910.3.3.3 Isocratic and Gradient Elution 24110.4 Conclusions 242References 24311 Inline Detectors 245Ramisetti Nageswara Rao and Pothuraju Nageswara Rao11.1 Introduction 24511.2 Detector Characteristics 24611.2.1 Sensitivity 24611.2.2 Selectivity 24611.2.3 Linearity 24711.2.4 Dynamic Range 24711.2.5 Detector Cell Volume 24711.3 UV-Visible Absorbance Detector 24711.3.1 Fixed Wavelength Detector 24911.3.2 Variable Wavelength Detector 25011.4 Photodiode Array Detector (PDA) 25111.5 Fluorescence Detector 25211.6 Refractive Index Detector (RID) 25511.7 Evaporative Light-Scattering Detector 25611.8 Electrochemical Detector 25711.9 Charged Aerosol Detection 25811.10 Conductivity Detector 25911.11 Coupling Detectors 26011.12 Comparison of HPLC Detectors 260References 26112 pH Effects on Chromatographic Retention Modes 263Paweł Wiczling, Łukasz Kubik, and Roman Kaliszan12.1 Introduction 26312.2 pH Measurements of Mobile Phase 26412.3 Effect of pH on Isocratic Retention 26612.4 pH Effect on Organic Modifier Gradients 26812.5 pH Gradient 26912.6 Determination of pKa, log kw (Hydrophobicity), and S 27412.7 Effect of pH in Normal-Phase Mode 27512.8 Summary 277References 27713 Chemometrics in Data Analysis and Liquid Chromatographic Method Development 279Biljana Jančic ́-Stojanovic ́and Tijana Rakic ́13.1 Introduction 27913.2 Chemometrics in Data Analysis 28013.2.1 Data Preprocessing 28013.2.2 Data Analysis 28413.3 Chemometrics in LC Method Development 28513.3.1 Analytical Target Profile and Critical Quality Attributes (Definition of the Objectives of the Method) 28613.3.2 Quality Risk Assessment and Critical Process Parameters (Definition of Investigated Factors and Their Levels) 28713.3.3 Investigation of the Knowledge Space (Selection of an Appropriate Experimental Design) 28813.3.3.1 Screening Designs 28913.3.3.2 Optimization Designs 29113.3.4 Critical Quality Attributes Modeling (Creation of Mathematical Models) 29313.3.5 Design Space 29413.3.6 Selection of the Working Points 29513.3.7 Robustness Testing 29513.4 Conclusions 296References 296Index to Volume 1 I1-I18Volume 2Part One Special Liquid Chromatography Modes 2991 Chiral Liquid Chromatography: Recent Applications with Special Emphasis on the Enantioseparation of Amino Compounds 301István Ilisz2 Chiral Separation of Some Classes of Pesticides by HPLC Method 321Imran Ali, Iqbal Hussain, Mohd Marsin Sanagi, and Hassan Y. Aboul-Enein3 Micellar Liquid Chromatography: Fundamentals 371Maria C. García-Alvarez-Coque, Maria J. Ruiz-Angel, and Samuel Carda-Broch4 Micellar Liquid Chromatography: Method Development and Applications 407Maria C. García-Alvarez-Coque, Maria J. Ruiz-Angel, and Samuel Carda-Broch5 Affinity Chromatography 461Erika L. Pfaunmiller, Jesbaniris Bas, Marissa Brooks, Mitchell Milanuk, Elliott Rodriguez, John Vargas, Ryan Matsuda, and David S. Hage6 Immunoaffinity Chromatography: Advantages and Limitations 483Nancy E. Thompson and Richard R. BurgessPart Two Capillary Electromigration Techniques 5037 Capillary Electromigration Techniques: Capillary Electrophoresis 505Václav Kašička8 Modern Injection Modes (Stacking) for CE 531Joselito P. Quirino9 Capillary Gel Electrophoresis 555Márta Kerékgyártó and András Guttman10 Nonaqueous Capillary Electrophoresis 581Julie Schappler and Serge Rudaz11 Detectors in Capillary Electrophoresis 607Petr Tůma and František Opekar12 Trends in CE-MS and Applications 629Anna Tycova and Frantisek Foret13 Capillary Electrochromatography 653Kai Zhang and Ruyu Gao14 Micellar Electrokinetic Chromatography 675Paolo Iadarola, Marco Fumagalli, and Simona Viglio15 Chip-Based Capillary Electrophoresis 707Yuanhong Xu, Jizhen Zhang and Jingquan Liu16 Chiral Separations by Capillary Electrophoresis 731E. Sánchez-López, M. Castro-Puyana, M.L. Marina, and A.L. CregoIndex to Volume 2 I1-I24Volume 31 Gas Chromatography: Theory and Definitions, Retention and Thermodynamics, and Selectivity 775Glenn E. Spangler2 Basic Overview on Gas Chromatography Injectors 807Md. Musfiqur Rahman, A.M. Abd El-Aty, and Jae-Han Shim3 Basic Overview on Gas Chromatography Columns 823Md. Musfiqur Rahman, A.M. Abd El-Aty, Jeong-Heui Choi, Ho-Chul Shin, Sung Chul Shin, and Jae-Han Shim4 Overview of Detectors in Gas Chromatography 835Md. Musfiqur Rahman, A.M. Abd El-Aty, and Jae-Han Shim5 Current Use of Gas Chromatography and Applications 849Walter Vetter6 Gas Chromatography with Mass Spectrometry (GC-MS) 883Walter Vetter7 Chiral GC 927Volker Schurig8 New Essential Events in Modern Applications of Inverse Gas Chromatography 979Adam Voelkel, Henryk Grajek, Beata Strzemiecka, and Katarzyna Adamska9 Chip-Based Gas Chromatography 999Hamza Shakeel and Masoud Agah10 Portable Gas Chromatography 1021Philip A. Smith11 Packed Column Sub- and Supercritical Fluid Chromatography 1051Caroline West, Syame Khater, and Eric Lesellier12 Instrumentation for Sub- and Supercritical Fluid Chromatography 1075Taghi Khayamian, Ali Daneshfar, and Hassan GhaziaskarIndex to Volume 3 I1-I18Volume 41 High-Performance Thin-Layer Chromatography 1093Vicente L. Cebolla, Luis Membrado, Carmen Jarne, and Rosa Garriga2 Field Flow Fractionation 1143Gaëtane Lespes, Julien Gigault, and Serge Battu3 Separations with a Liquid Stationary Phase: Countercurrent Chromatography or Centrifugal Partition Chromatography 1177Alain Berthod and Karine Faure4 Preparative Chromatography: Batch and Continuous 1207José P.S. Aniceto and Carlos M. Silva5 Fast and Miniaturized Chromatography 1315Bárbara Socas-Rodríguez, Antonio V. Herrera-Herrera, Miguel Ángel González-Curbelo, Javier González-Sálamo, and Javier Hernández-Borges6 Two-Dimensional Liquid Chromatography 1357Morgan Sarrut, Nicola Marchetti, and Sabine HeinischIndex to Volume 4 I1-I14Volume 51 Sampling Strategies: Statistics of Sampling 1385Małgorzata Bodnar, Piotr Konieczka, and Jacek Namieśnik2 Targeted and Non-Targeted Analysis 1401Luis E. Rodriguez-Saona, Marçal Plans Pujolras, and M. Monica Giusti3 Conventional Extraction Techniques: Soxhlet and Liquid–Liquid Extractions and Evaporation 1437Adegbenro Peter Daso and Okechukwu Jonathan Okonkwo4 Main uses of Microwaves and Ultrasounds in Analytical Extraction Schemes: an Overview 1469Idaira Pacheco-Fernández, Providencia González-Hernández, Priscilla Rocío-Bautista, María José Trujillo-Rodríguez, and Verónica Pino5 Membrane-assisted Separations 1503Jan Åke Jönsson6 Dispersive Solid-Phase Extraction 1525Bárbara Socas-Rodríguez, Antonio V. Herrera-Herrera, María Asensio-Ramos, and Javier Hernández-Borges7 Solid-Phase Extraction 1571Nil Ozbek, Asli Baysal, Suleyman Akman, and Mehmet Dogan8 Solid-Phase Microextraction 1595Ali Mehdinia and Mohammad Ovais Aziz-Zanjani9 Liquid-Phase Microextraction 1625Mohammad Reza Ganjali, Morteza Rezapour, Parviz Norouzi, and Farnoush Faridbod10 Analytical Supercritical Fluid Extraction 1659Julian Martínez and Ana Carolina de Aguiar11 Extraction Methods Facilitated by the use of Magnetic Nanoparticles 1681Priscilla Rocío-Bautista and Verónica Pino12 Sample Derivatization in Separation Science 1725Pascal Cardinael, Hervé Casabianca, Valerie Peulon-Agasse, and Alain Berthod13 Validation of Analytical Methods Based on Chromatographic Techniques: An Overview 1757Juan Peris-Vicente, Josep Esteve-Romero, and Samuel Carda-Broch14 “Omics” and Biomedical Applications 1809Pasquale Ferranti, Chiara Nitride, and Monica Gallo15 Food Applications: Using Novel Sample Preparation Modes 1859Mónica González and Venerando González16 Forensic Applications 1877Matías Calcerrada Guerreiro, María López-López, Ma Ángeles Fernández de la Ossa, and Carmen García-Ruiz17 Environmental Applications of Solid Phase Microextraction Techniques 1897Sarah Montesdeoca-Esponda, M Esther Torres-Padrón, Zoraida Sosa-Ferrera, and José Juan Santana-RodríguezIndex to Volume 5 I1-I20Index 1929