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Beschreibung

This book provides a detailed description of various multidimensional chromatographic separation techniques. The editor first provides an introduction to the area and then dives right into the various complex separation techniques. While still not used routinely comprehensive chromatography techniques will help acquaint the readers with the fundamentals and possible benefits of multi-dimensional separations coupled with mass spectrometry.

The topics include a wide range of material that will appease all interested in either entering the field of multidimensional chromatography and those looking to gain a better understanding of the topic.

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Seitenzahl: 832

Veröffentlichungsjahr: 2011

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Table of Contents

Series Page

Title Page

Copyright

Contributors

Preface

Chapter 1: Introduction

1.1 Two-dimensional chromatography–mass spectrometry: a 50-year-old combination

1.2 Shortcomings of one-dimensional chromatography

1.3 Benefits of two-dimensional chromatography

1.4 Book content

1.5 Final considerations

References

Chapter 2: Multidimensional Gas Chromatography: Theoretical Considerations

2.1 Symbols

2.2 One-Dimensional GC

2.3 Comprehensive GC × GC

References

Chapter 3: Multidimensional Liquid Chromatography: theoretical considerations

3.1 Two-dimensional LC techniques

3.2 Peak capacity in HPLC: one- and multidimensional separations

3.3 Orthogonality in two-dimensional LC–LC systems

3.4 Sample dimensionality and structural correlations

3.5 Separation selectivity and selection of phase systems in two-dimensional LC–LC

3.6 Programmed elution in two-dimensional HPLC

3.7 Fraction transfer modulation in comprehensive LC × LC: additional band broadening

3.8 Future perspectives

Chapter 4: History, Evolution, and Optimization Aspects of Comprehensive Two-Dimensional Gas Chromatography

4.1 Fundamentals of GC × GC

4.2 Modulation

4.3 GC × GC Data Interpretation

4.4 GC × GC Instrumentation

4.5 Thermal modulators

4.6 Comprehensive Two-Dimensional GC Method Optimization

4.7 Final Remarks

References

Chapter 5: Flow-Modulated Comprehensive Two-Dimensional Gas Chromatography

5.1 Timing Requirements of GC × GC Modulators

5.2 Criteria for Evaluating Modulators

5.3 Forms of Modulation

5.4 Single-Stage Flow Modulation

5.5 Two-Stage Flow Modulation

5.6 Summary of Flow Modulators

5.7 Brief Comparison to Thermal Modulation

5.8 Concluding Remarks

References

Chapter 6: Comprehensive two-dimensional gas chromatography combined with mass spectrometry

6.1 Instrument requirements for GC × GC–MS

6.2 Data processing of GC × GC–TOF MS results

6.3 Method translation in GC × GC–MS

6.4 GC × MS

6.5 Conventional and alternative modulation techniques for GC × GC–MS

6.6 GC × GC–MS APPLICATIONS

6.7 Concluding remarks

References and Further Reading

Chapter 7: Detector Technologies and Applications in Comprehensive Two-dimensional Gas Chromatography

7.1 Detection in GC × GC

7.2 Comments on GC × GC with Mass Spectrometry

7.3 Flame Ionization Detection in GC × GC

7.4 Electron Capture Detection in GC × GC

7.5 Sulfur Chemiluminescence Detection in GC × GC

7.6 Nitrogen Chemiluminescence Detection in GC × GC

7.7 Atomic Emission Detection in GC × GC

7.8 Thermionic Detection in GC × GC

7.9 Flame Photometric Detection in GC × GC

7.10 Case Study of GC × GC with selective detection

7.11 Dual Detection with GC × GC

7.12 Conclusions

References

Chapter 8: History, Evolution, and Optimization Aspects of Comprehensive Two-Dimensional Liquid Chromatography

8.1 Method development and instrumentation

8.2 Technical Problems in Comprehensive Liquid Chromatography

8.3 Detection

8.4 Data representation

8.5 Instrumentation

8.6 Milestones in comprehensive liquid chromatography

8.7 Applications

8.8 Beyond two-dimensional chromatography

8.9 Comparison of LC × LC and off-line 2D LC

8.10 Conclusions

References

Chapter 9: Comprehensive Two-Dimensional Liquid Chromatography Combined with Mass Spectrometry

9.1 HPLC–MS

9.2 LC × LC–MS Instrumentation and Method Development

9.3 LC × LC–MS Applications

References

Chapter 10: Comprehensive two-dimensional liquid chromatography applications

10.1 Comprehensive 2D LC separation of synthetic and natural polymers

10.2 Comprehensive 2D LC separation of Natural products and antioxidants

10.3 Comprehensive 2D LC separation of Pharmaceutical and environmental compounds

10.4 Comprehensive 2D LC separation of Proteins and Peptides

References

Chapter 11: Other Comprehensive Chromatography Methods

11.1 Online two-dimensional liquid chromatography–gas chromatography

11.2 Online two-dimensional supercritical fluid chromatography–gas chromatography

11.3 Online two-dimensional supercritical fluid chromatography–supercritical fluid chromatography

11.4 Online two-dimensional supercritical fluid chromatography-liquid chromatography

References

Chapter 12: Comprehensive Chromatography Data Interpretation Technologies

12.1 Higher-Order Data Structure

12.2 Modifications of First-Order Data-Handling Approaches

12.3 Visualization

12.4 Mass Spectral Detection

12.5 Chemometrics

12.6 Summary of Data Interpretation Technologies

References

Wiley Series

Index

Copyright © 2010 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) 750-4744. 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.

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Library of Congress Cataloging-in-Publication Data:

Comprehensive chromatography in combination with mass spectrometry / edited by Luigi Mondello

p. cm.

Includes index.

ISBN 978-0-470-43407-9 (cloth)

1. Chromatographic analysis. 2. Multidimensional chromatography. I. Mondello, Luigi.

QD79.C4C66 2011

543'.8–dc22

2010036838

Contributors

Keith D. Bartle, University of Leeds, Leeds, UK

Leonid Blumberg, Fast GC Consulting, Hockessin, Delaware

Francesco Cacciola, Chromaleont s.r.l., A spin-off of the University of Messina, Messina, Italy and University of Messina, Messina, Italy

Paola Donato, University Campus Bio-Medico, Rome, Italy and University of Messina, Messina, Italy

Paola Dugo, University of Messina, Messina, Italy

Isabelle François, University of Gent, Gent, Belgium; currently at Waters NV/SA, Zellik, Belgium, Division of Waters Corporation, Milford, Massachusetts

Tadeusz Górecki, University of Waterloo, Waterloo, Ontario, Canada

Elizabeth M. Humston, University of Washington, Seattle, Washington

Pavel Jandera, University of Pardubice, Pardubice, Czech Republic

Philip J. Marriott, Monash University, Clayton, Victoria, Australia

Luigi Mondello, University of Messina, Messina, Italy

Ahmed Mostafa, University of Waterloo, Waterloo, Ontario, Canada

Samuel D. H. Poynter, University of Tasmania, Hobart, Tasmania, Australia

Koen Sandra, Metablys, Research Institute for Chromatography, Kortrijk, Belgium

Pat Sandra, University of Gent, Gent, Belgium

Danilo Sciarrone, University of Messina, Messina, Italy

John V. Seeley, Oakland University, Rochester, Michigan

Robert A. Shellie, University of Tasmania, Hobart, Tasmania, Australia

Robert E. Synovec, University of Washington, Seattle, Washington

Peter Q. Tranchida, University of Messina, Messina, Italy

Preface

Over the last half-century, single-column chromatography processes have been widely exploited for untangling constituents forming real-world samples. Many separation scientists are still acquainted with a single chromatography view, that is, the alignment of a series of peaks along a single, rather restricted separation axis. In many cases, one-dimensional separation spaces are enough for the isolation and detection of all the compounds of interest; however, in others, analysts must surrender themselves to an overwhelming antagonist: sample complexity.

In recent years, the great advances made in the field of instrumental analytical chemistry have made it increasingly apparent that natural or synthetic samples, characterized by hundreds, thousands, or even tens of thousands of constituents, are a common occurrence. In one-dimensional chromatography applications, the presence of tangled analytes at the column outlet is a frequent and undesired phenomenon. The most effective way to circumvent such an obstacle is to expand the separation space by using multiple analytical dimensions of a chromatographic and mass spectrometric (MS) nature.

The great analytical benefits provided by comprehensive chromatographic (CC) techniques have been exploited and emphasized by a constantly increasing part of the separation-science community during the last two decades. The term well-known has been stripped from a multitude of real-world samples, the true composition of which has been revealed through CC methodologies. The amount of separation space generated by current-day CC processes is unprecedented, making theses methods best suited for the unraveling of highly complex samples. The addition of a third mass spectrometric dimension to a comprehensive chromatography system generates a very powerful analytical tool: two selectively distinct chromatographic dimensions and a third mass-differentiating dimension.

A series of factors stimulated me to edit the present contribution, devoted to comprehensive two-dimensional chromatography in combination with mass spectrometry: first, and foremost, my personal excitement and passion for CC–MS technology, my main field of research; second, recent instrumental advances and the expanding popularity of CC–MS methods; and finally, and simply, the fact that there is still an immense wealth of information to be revealed on the composition of samples in all scientific fields of research.

Finally, I hope that this book will contribute to the promotion and development of CC–MS methods, which are still far from well established. Although I have been operating in the chromatographic world for quite some time, it is still very exciting for me to “play” with a CC–MS system, run a sample, and reveal its unsuspected complexity. In a way, CC–MS methodologies give us the pleasure to discover things for the first time.

12.0.1 Acknowledgments

As editor of the book, I would like to thank the many people who provided support; read, wrote, offered comments, and gave precious suggestions; and assisted in the editing and proof reading.

I am grateful to the authors for the considerable amount of work devoted to the preparation of the chapters, covering a variety of CC–MS aspects, ranging from historical aspects, to theoretical and optimization considerations, to pure applications, and on to hardware and software evolution.

Special thanks to Dr. Paola Donato and Prof. Peter Quinto Tranchida, for helping in the process of selection and editing, and to Prof. Giovanni Dugo, my father-in-law and mentor, who initiated me into this wonderful world of separation sciences.

Above all, I want to thank my wife, Paola, and my daughters, Alice and Viola, who supported and encouraged me in spite of all the time I was away from them.

Luigi Mondello