Liquid Chromatography Mass Spectrometry. Techniques and Applications

Transcription

1 Liquid Chromatography Mass Spectrometry Techniques and Applications

2 MODERN ANALYTICAL CHEMISTRY Series Editor: David Hercules University of Pittsburgh ANALYTICAL ATOMIC SPECTROSCOPY William G. Schrenk APPLIED ATOMIC SPECTROSCOPY Volumes 1 and 2 Edited by E. L. Grove CHEMICAL DERIVATIZATION IN ANALYTICAL CHEMISTRY Edited by R. W. Frei and J. F. Lawrence Volume 1: Chromatography Volume 2: Separation and Continuous Flow Techniques COMPUTER-ENHANCED ANALYTICAL SPECTROSCOPY Volume 1: Edited by Henk L. C. Meuzelaar and Thomas L. Isenhour Volume 2: Edited by Henk L. C. Meuzelaar ION CHROMATOGRAPHY Hamish Small ION-SELECTIVE ELECTRODES IN ANALYTICAL CHEMISTRY Volumes 1 and 2 Edited by Henry Freiser LIQUID CHROMATOGRAPHY /MASS SPECTROMETRY Techniques and Applications Alfred L. Yergey, Charles G. Edmonds, Ivor A. S. Lewis, and Marvin L. Vestal MODERN FLUORESCENCE SPECTROSCOPY Volumes 1-4 Edited by E. L. Wehry PHOTOELECTRON AND AUGER SPECTROSCOPY Thomas A. Carlson PRINCIPLES OF CHEMICAL SENSORS Jifl Janata TRANSFORM TECHNIQUES IN CHEMISTRY Edited by Peter R. Griffiths A Continuation Order Plan is available for this series. A continuation order will bring delivery of each new volume immediately upon publication. Volumes are billed only upon actual shipment. For further information please contact the publisher.

3 Liquid Chromatography Mass Techniques and Applications Alfred L. Yergey National Institutes of Health Bethesda, Maryland Charles G. Edmonds Battelle Pacific Northwest Laboratories Richland, Washington lvor A. S. Lewis King's College London, United Kingdom and Marvin L. Vestal Vestee Corporation Houston, Texas Spectrometry Springer Science+Business Media, LLC

4 Library of Congress Cataloging in Publication Data Liquid chromatography/mass spectrometry: techniques and applications / Alfred L. Yergey... [et al.]. p. cm. - (Modern analytical chemistry) Includes bibliographical references. ISBN ISBN (ebook) DOI / Liquid chromatography. 2. Mass spectrometry. 1. Yergey, Alfred L. II. Series. QD79.C454L '.0894-dc20 CIP Springer Science+Business Media New York 1990 Originally published by Plenum Press New York in Softcover reprint of the hardcover I st edition 1990 AII rights reserved No part of this book may be reproduced, stored in a retrieval system, or transmitted in any form or by any means, electronic, mechanical, photocopying, microfilming, recording, or otherwise, without written permis sion from the Publisher

5 Preface This book is intended both to be an introduction to techniques and applications of liquid chromatography/mass spectrometry and to serve as a reference for future workers. When we undertook its writing, we chose not to cover the field, particularly applications, exhaustively. Rather we wished to produce a book that would be of use to people just beginning to use the technique as well as to more advanced practitioners. In this regard, we have sought to highlight techniques and applications that are of current importance, while not neglecting descriptions of approaches that may be of significance in the future. We hope that we have succeeded in this. At the same time we hope that the bibliography, with indexes classified by author and title, will make this book of value to those who may disagree with our emphasis. ACKNOWLEDGMENTS. One of us (C.G.E.) wishes to acknowledge the encouragment of Professor J. A. McCloskey in undertaking this project. All four of us are grateful for the continuous and expert assistance of V. A. Edmonds in the preparation of the Bibliography. Alfred L. Y ergey Bethesda, Maryland Charles G. Edmonds Richland, Washington lvor A.S. Lewis London, England Marvin L. Vestal Houston, Texas v

6 Contents 1. Introduction Direct Liquid Introduction Interfaces Introduction Operating Principles Specific DLI Interfaces Capillary Inlets Diaphragm Interfaces Nebulizing Interfaces Interfaces Using Unusual Fluids Continuous Flow FAB Interfaces SFC Interfaces Additional References Mechanical Transport Devices Introduction Continuous Transport Systems Moving-Wire Interfaces Moving-Belt Interfaces The Heated-Wire Concentrator Mechanized Fraction Collectors Discussion Future Prospects Thermospray Introduction Apparatus for Thermospray vii

7 viii Contents The Vaporizer Probe The Thennospray Ion Source Electron Gun Discharge Electrode Vacuum System Thennospray Control System Ion Optics and Mass Analyzer Mechanisms Involved in Thennospray Vaporization and Ionization Vaporization and Nebulization in the Thennospray Capillary Free Jet Expansion Ionization Mechanisms Production of Molecular Ions Ion Evaporation from Charged Liquid Droplets Ion Production from Charged Liquid Droplets- A Summary Ion Production from Charged Solid Particles Ionic Equilibria in a Vaporizing Droplet Gas Phase Ion-Molecule Reactions Repeller Effects Optimizing Thennospray LC/MS for Particular Applications Selection and Modification of LC Conditions Selection of Ionization Technique Operating Temperatures Vaporizer Tip Temperature Summary Additional References Particle Beam Interfaces LC/MS of Nucleic Acid Constituents Introduction LC/MS of Nucleobases and Related Compounds Nucleobases Methylxanthine Bases LC/MS of Nucleosides Liquid Chromatography of Nucleosides Methods Employed for Nucleosides Performance Comparisons for Nucleosides Application of LC/MS to Nucleoside Analysis LC/MS of Nucleotides

8 Contents ix Methods Employed for Nucleotides and Dinucleotides Applications of LC/MS to Nucleotides and Dinucleotides Future Prospects Additional References LC/MS of Conjugated Molecules Introduction Glucuronides Acy lcarnitines Sulfates Additional References Applications of LC/MS to Amino Acids, Peptides, and Proteins Background Applications Using Immobilized Enzyme Digestions Limitations and Future Work A Bibliography of Combined Liquid Chromatography/Mass Spectrometry Introduction Methods Organization of the Bibliography Additional References Bibliography Author Index Subject Index Index