MULTIDIMENSIONAL LIQUID CHROMATOGRAPHY MULTIDIMENSIONAL LIQUID CHROMATOGRAPHY Theory and...

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  • MULTIDIMENSIONAL LIQUID CHROMATOGRAPHY

    Theory and Applications in Industrial Chemistry and the Life Sciences

    Edited by

    STEVEN A. COHEN Life Sciences R&D, Waters Corporation Milford, MA 01757, USA

    MARK R. SCHURE Theoretical Separation Science Laboratory Rohm and Haas Company Springhouse, PA 19477-0904, USA

    A JOHN WILEY & SONS, INC., PUBLICATION

    Innodata File Attachment 9780470276259.jpg

  • MULTIDIMENSIONAL LIQUID CHROMATOGRAPHY

  • MULTIDIMENSIONAL LIQUID CHROMATOGRAPHY

    Theory and Applications in Industrial Chemistry and the Life Sciences

    Edited by

    STEVEN A. COHEN Life Sciences R&D, Waters Corporation Milford, MA 01757, USA

    MARK R. SCHURE Theoretical Separation Science Laboratory Rohm and Haas Company Springhouse, PA 19477-0904, USA

    A JOHN WILEY & SONS, INC., PUBLICATION

  • Copyright � 2008 by John Wiley & Sons, Inc. All rights reserved.

    Published by John Wiley & Sons, Inc., Hoboken, New Jersey Published simultaneously in Canada

    No part of this publication may be reproduced, stored in a retrieval system, or transmitted in any form or by any means, electronic, mechanical, photocopying, recording, scanning, or otherwise, except as permitted under Section 107 or 108 of the 1976 United States Copyright Act, without either the prior written permission of the Publisher, or authorization through payment of the appropriate per-copy fee to the Copyright Clearance Center, Inc., 222 Rosewood Drive, Danvers, MA 01923, 978-750-8400, fax 978-750-4470, or on theweb at www.copyright.com.Requests to the Publisher for permission should be addressed to the Permissions Department, John Wiley & Sons, Inc., 111 River Street, Hoboken, NJ 07030, 201-748-6011, fax 201-748-6008, or online at http://www.wiley.com/go/permission.

    Limit of Liability/Disclaimer of Warranty: While the publisher and author have used their best efforts in preparing this book, they make no representations or warranties with respect to the accuracy or completeness of the contents of this book and specifically disclaim any implied warranties of merchantability or fitness for a particular purpose. No warranty may be created or extended by sales representatives or written sales materials. The advice and strategies contained herein may not be suitable for your situation. You should consult with a professional where appropriate. Neither the publisher nor author shall be liable for any loss of profit or any other commercial damages, including but not limited to special, incidental, consequential, or other damages.

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    Library of Congress Cataloging-in-Publication Data:

    Multidimensional liquid chromatography: theory and applications in industrial chemistry and the life sciences / edited By Steven A. Cohen, Mark R. Schure.

    p. cm. Includes index. ISBN 978-0-471-73847-3 (cloth)

    1. Liquid chromatography. 2. Chemical engineering. 3. Chemistry, Technical. 4. Biochemistry. I. Cohen, Steven A., 1953- II. Schure, Mark R.; 1952- QD79.C454M85 2007 543’.84–dc22 2007041576

    Printed in the United States of America 10 9 8 7 6 5 4 3 2 1

    http://www.copyright.com http://www.wiley.com/go/permission http://www.wiley.com http://www.wiley.com

  • CONTENTS

    Foreword xiii

    Preface xv

    Contributors xvii

    1 Introduction 1

    1.1 Previous Literature Which Covers MDLC 4 1.2 How this Book is Organized 5 References 6

    PART I THEORY 9

    2 Elements of the Theory of Multidimensional Liquid Chromatography 11

    2.1 Introduction 11 2.2 Peak Capacity 13 2.3 Resolution 17 2.4 Orthogonality 19 2.5 Two-Dimensional Theory of Peak Overlap 21 2.6 Dimensionality, Peak Ordering, and Clustering 23 2.7 Theory of Zone Sampling 24 2.8 Dilution and Limit of Detection 26 2.9 Chemometric Analysis 27

    v

  • 2.10 Future Directions 28 References 30

    3 Peak Capacity in Two-Dimensional Liquid Chromatography 35

    3.1 Introduction 35 3.2 Theory 37 3.3 Procedures 41 3.4 Results and Discussion 42 3.5 Conclusions 49 Appendix 3A Generation of Random Correlated Coordinates 50 Appendix 3B Derivation of Limiting Correlation Coefficient r 54 References 56

    4 Decoding Complex 2D Separations 59

    4.1 Introduction 59 4.2 Fundamentals: The Statistical Description of Complex

    Multicomponent Separations 62 4.3 Decoding 1D and 2D Multicomponent Separations

    by Using the SMO Poisson Statistics 68 4.4 Decoding Multicomponent Separations by the

    Autocovariance Function 74 4.5 Application to 2D Separations 78

    4.5.1 Results from SMO Method 81 4.5.2 Results from 2D Autocovariance

    Function Method 84 4.6 Concluding Remarks 88 Acknowledgments 88 References 88

    PART II COLUMNS, INSTRUMENTATION AND METHODS DEVELOPMENT 91

    5 Instrumentation for Comprehensive Multidimensional Liquid Chromatography 93

    5.1 Introduction 93 5.2 Heart-Cutting Versus Comprehensive Mode 95 5.3 Chromatographic Hardware 97

    5.3.1 Valves 97 5.4 CE Interfaces 104

    5.4.1 Gated Interface for HPLC–CE 104 5.4.2 Microfluidic Valves for On-Chip

    Multidimensional Analysis 105

    vi CONTENTS

  • 5.5 Columns and Combinations 106 5.5.1 Column Systems, Dilution, and Splitting 108

    5.6 Detection 109 5.7 Computer Hardware and Software 109

    5.7.1 Software Development 110 5.7.2 Valve Sequencing 111 5.7.3 Data Format and Storage 113

    5.8 Zone Visualization 115 5.8.1 Contour Visualization 115 5.8.2 2D Peak Presentation 117 5.8.3 Zone Visualization in Specific Chemical (pI) Regions 117 5.8.4 External Plotting Programs 117 5.8.5 Difference Plots 118 5.8.6 Multi-channel Data 118

    5.9 Data Analysis and Signal Processing 119 5.10 Future Prospects 120

    References 121

    6 Method Development in Comprehensive Multidimensional Liquid Chromatography 127

    6.1 Introduction 127 6.2 Previous Work 128 6.3 Column Variables 130 6.4 Method Development 130

    6.4.1 The Cardinal Rules of 2DLC Method Development 132 6.5 Planning the Experiment 143 6.6 General Comments on Optimizing the 2DLC Experiment:

    Speed–Resolution Trade-off 143 Acknowledgment 144 References 144

    7 Monolithic Columns and Their 2D-HPLC Applications 147

    7.1 Introduction 147 7.2 Monolithic Polymer Columns 148

    7.2.1 Structural Properties of Polymer Monoliths 148 7.2.2 Chromatographic Properties of

    Polymer Monolithic Columns 150 7.2.3 Two-Dimensional HPLC Using Polymer Monoliths 152

    7.3 Monolithic Silica Columns 153 7.3.1 Preparation 154 7.3.2 Structural Properties of Monolithic Silica Columns 154 7.3.3 Chromatographic Properties of

    Monolithic Silica Columns 156

    CONTENTS vii

  • 7.4 Peak Capacity Increase by Using Monolithic Silica Columns in Gradient Elution 158

    7.5 2D HPLC Using Monolithic Silica Columns 159 7.5.1 RP-RP 2D HPLC Using Two Different Columns 161 7.5.2 RP–RP 2D HPLC Using Two Similar Columns 164 7.5.3 Ion Exchange–Reversed-Phase 2D HPLC

    Using a Monolithic Column for the 2nd-D 166 7.5.4 IEX-RP 2D HPLC Using a Monolithic RP

    Capillary Column for the 2nd-D 168 7.6 Summary and Future Improvement of 2D HPLC 171 References 171

    8 Ultrahigh Pressure Multidimensional Liquid Chromatography 177

    8.1 Background: MDLC in the Jorgenson Lab 177 8.1.1 Cation Exchange–Size Exclusion 178 8.1.2 Anion Exchange–Reversed Phase 180 8.1.3 Cation Exchange–Reversed Phase 181 8.1.4 Size Exclusion–Reversed Phase 183

    8.2 Online Versus Off-Line MDLC 188 8.3 MDLC Using Ultrahigh Pressure Liquid Chromatography:

    Benefits and Challenges 189 8.3.1 An Introduction to UHPLC 190 8.3.2 UHPLC for LC�LC: High Speed

    Versus High Peak Capacity 191 8.3.3 LC�UHPLC for Separations of Intact Proteins 191

    8.4 Experimental Details 193 8.4.1 Instrumentation 193 8.4.2 Data Analysis 194 8.4.3 Chromatographic Conditions 195 8.4.4 Samples 196

    8.5 Results and Discussion 196 8.6 Future Directions for UHP-MDLC 202 References 203

    PART III LIFE SCIENCE APPLICATIONS 205

    9 Peptidomics 207

    9.1 State of the Art—Why Peptidomics? 207 9.2 Strategies and Solutions 208 9.3 Summary and Conclusions 218 References 218

    viii CONTENTS

  • 10 ATwo-Dimensional Liquid Mass Mapping Technique for Biomarker Discovery 221

    10.1 Introduction 221 10.2 Methods for Separating and Identifying Proteins 223

    10.2.1 pI-Based Methods of Separation 223 10.2.2 Chromatofocusing-A Column Based pH Separation 225 10.2.3 Nonporous Separation of Proteins 226 10.2.4 Electrospray-Time of Flight-Mass Spectrometry 228 10.2.5 MALDI Peptide Mass Fingerprinting 229 10.2.6 Data Analysis and Recombination 230

    10.3 Applications 230 10.3.1 Proteomic Mapping and Clustering

    of Multiple Samples—Application to Ovarian Cancer Cell Lines 230

    10.3.2 2D Liquid Mass Mapping of Tumor Cell Line Secreted Samples, Application to Metastasis-Associated Protein Profiles 233

    10.3.3 Identification Annotation and Data Correlation in MCF10 Human Breast Cancer Cell Lines 235

    10.4 Summary and Conclusions 237 Acknowledgments 238 References 238

    11 Coupled Mult