LIQUID CHROMATOGRAPHY: FUNDAMENTALS AND INSTRUMENTATION

Size: px

Start display at page:

Download "LIQUID CHROMATOGRAPHY: FUNDAMENTALS AND INSTRUMENTATION"

Lorin Smith
5 years ago
Views:

1 .. LIQUID CHROMATOGRAPHY: FUNDAMENTALS AND INSTRUMENTATION SALVATORE FANALI PAUL R. HADDAD CouN F. PooLE PETER SCHOENMAKERS DAVID LLOYD ELSEVIER AMSTERDAM BOSTON HEIDELBERG LONDON NEW YORK OXFORD PARIS SAN DIEGO SAN FRANCISCO SINGAPORE SYDNEY TOKYO

2 Contents Co~tributors xi 1. Milestones in the Development of Liquid Chromatography 1 L.R. SNYDER AND J.W. DOLAN 1.1. Introduction HPLC Theory and Practice Columns Equipment Detectors 12 Apologies and Acknowledgements 13 References Kinetic Theories of Liquid Chromatography 19 A. FELINGER AND A. CA VAZZINI 2.1. Introduction Macroscopic Kinetic Theories Microscopic Kinetic Theories Comparison of the Microscopic and Macroscopic Models 38 References Column Technology in Liquid Chromatography 41 K.K. UNGER, S. LAMOTIE AND E. MACHTEJEVAS 3.1. Introduction Column Design and Hardware Column Packing Materials and Stationary Phases Column Systems and Operations Chromatographic Column Testing and Evaluation Column Maintenance and Troubleshooting Today's Column Market-an Evaluation, Comparison, and Critical Appraisal 74 References 83

3 vi CONTENTS 4. Secondary Chemical Equilibria in Reversed-Phase Liquid Chromatography 87 M.C. GARCIA-ALVAREZ-COQUE AND ].R. TORRES-LAPASIO 4.1. Introduction Acid-Base Equilibria Ion-Interaction Chromatography Micellar Liquid Chromatography Metal Complexation 100 Further Reading Hydrophilic Interaction Liquid Chromatography 105 A. CAVAZZINI AND A. FELINGER 5.1. Introduction Principles of HILIC Mobile and Stationary Phases Commonly Employed in HILIC Application Examples 114 References Hydrophobic Interaction Chromatography 121 C.T. TOMAZ AND ].A. QUEIROZ 6.1. Introduction Principles of Hydrophobic Interaction Chromatography Main Factors that Affect Hydrophobic Interaction Chromatography Purification Strategies Practical Aspects of Hydrophobic Interaction Chromatography Purification Selected A1 plications Future Trends 135 References _ Liquid-Solid Chromatography 143 L.R. SNYDER AND ].W. DOLAN 7.1. Introduction Retention and Separation Method Development Problems in the Use of Normal-Phase Chromatography 154 References Ion Chromatography 157 B. PAULL AND P.N. NESTERENKO 8.1. Introduction Basic Principles and Separation Modes 158

4 CONTENTS vii 8.3. Instrumentation Applications 185 References Size-Exclusion Chromatography 193 A.M. STRIEGEL 9.1. Introduction Historical Background Retention In Size-Exclusion Chromatography Band Broadening in Size-Exclusion Chromatography Resolution in Size-Exclusion Chromatography Size-Exclusion Chromatography Enters the Modem Era: The Determination of Absolute Molar Mass Size-Exclusion Chromatography Today: Multidetector Measurements, Physicochemical Characterization, Two-Dimensional Techniques Conclusions 219 Acknowledgement and Disclaimer 220 References Solvent Selection in Liquid Chromatography 225 G. RAMIS-RAMOS AND M.C. GARclA-ALVAREZ-COQUE Elution Strength Columns and Solvents in RPLC, NPLC, and HILIC Assessment of the Elution Strength Schoenmakers's Rule Isoeluotropic Mixtures Solvent-Selectivity Triangles Practical Guidelines for Optimization of Mobile Phase Composition Additional Considerations for Solvent Selection 246 References Method Development in Liquid Chromatography 251 J.W. DOLAN AND L.R. SNYDER Introduction Goals A Structured Approach to Method Development Method Development in Practice Prevalidation Validation Documentation Summary 266 References 267

5 viii CONTENTS 12. Theory and Practice of Gradient Elution Liquid Chromatography 269 J.W. DOLAN AND L.R. SNYDER Introduction The Effects of Experimental Conditions on Separation Method Development Problems Associated with Gradient Elution 281 References General Instrumentation 283 ].G. SHACKMAN Introduction Solvent Source Pumping Systems Gradient-Elution Mixing Systems Sample Injection Column Compartment Tubings and Fittings Detector Overview Ultraviolet-Visible Absorbance Detectors Refractive Index Detectors Evaporative Light-Scattering Detectors Charged Aerosol Detectors Conductivity Detectors Fluorescence Detectors Electrochemical Detectors Other Detection Methods 303 References Advanced Spectroscopic Detectors for Identification and Quantification: Mass Spectrometry 307 S. CROTTI, I. ISAK AND P. TRALDI Introduction Ionization Methods Suitable for LC Coupling How to Increase Specificity of MS Data Micro- and Nano-LC-MS Capillary Electrochromatography 325 References Advanced Spectroscopic Detectors for Identification and Quantification: FTIR and Raman 333 ]. KULIGOWSKI, B. LENDL, AND G. QUINT AS Introduction Off-Line Hyphenation 337

6 CONTENTS ix On-Line Hyphenation Conclusions 345 References Advanced Spectroscopic Detectors for Identification and Quantification: Nuclear Magnetic Resonance 349 J.-L. WOLFENDER, N. BOHNI, K. NDJOKO-IOSET AND A.S. EDISON Introduction Hyphenation ofnmr with HPLC Advances in NMR Sensitivity Strategies for Obtaining NMR Information from a Given LC Peak Integration with a Multiple Detection System (LC-NMR-MS) Quantification Capabilities Fields of Application Conclusions 379 Acknowledgments 380 References Quantitative Structure Property (Retention) Relationships in Liquid Chromatography 385 R. KALISZAN Introduction Methodology and Goals of QSRR Studies Applications of QSRR in Proteomics Characterization of Stationary Phases QSRR and Assessment of Lipophilicity of Xenobiotics QSRR Analysis of Retention Data Determined on lmmobilized-biomacromolecule Stationary Phases Quantitative Retention-(Biological) Activity Relationships Chemometrically Processed Multivariate Chromatographic Data in Relation to Pharmacological Properties of Drugs and "Drug Candidates" Concluding Remarks 401 Acknowledgment 402 References Modeling of Preparative Liquid Chromatography 407 T. FORNSTEDT, P. FORSSEN AND). SAMUELSSON Introduction Column Model Adsorption Model Process Optimization of Preparative Chromatography Case Example 422 References 422

7 X CONTENTS 19. Process Concepts in Preparative Chromatography 427 M. KASPERE!T AND A. SEIDEL-MORGENSTERN Introduction Classical!socratic Discontinuous Elution Chromatography Other Discontinuous Operating Concepts Continuous Concepts of Preparative Chromatography Optimization and Concept Comparison Conclusions 448 Acknowledgments 448 References 449 Index Miniaturization and Microfluidics 453 F. FORET, P. SMEJKAL AND M. MACKA Introduction, Definitions, and Scope Microfluidic Systems for Separations Commercial Instrumentation Conclusion 465 Acknowledgment 465 References Capillary Electrochromatography 469 A. ROCCO, G. D'ORAZIO, Z. A TURK! AND S. FANAU Introduction Principles of Capillary Electrochromatography Instrumentation Method Optimization in CEC Examples of Some Recent Applications Conclusions and Future Trends 486 References 487

Introduction to Pharmaceutical Chemical Analysis

Introduction to Pharmaceutical Chemical Analysis Hansen, Steen ISBN-13: 9780470661222 Table of Contents Preface xv 1 Introduction to Pharmaceutical Analysis 1 1.1 Applications and Definitions 1 1.2 The