Mass Spectrometry: Clinical and Biomedical Applications

360 Pages·1992·11.037 MB·English

by  Matthias Mann, John B. Fenn (auth.), Dominic M. Desiderio (eds.)

Mass Spectrometry
Clinical and Biomedical Applications
Volume 1
MODERN ANALYTICAL CHEMISTRY
Series Editor: David M. Hercules
University of Pittsburgh
ADVANCES IN COAL SPECTROSCOPY
Edited by Henk L. C. Meuzelaar
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
Volume 3: Edited by Peter C. Jurs
ION CHROMATOGRAPHY
Hamish Small
ION-SELECTIVE ELECTRODES IN ANALYTICAL CHEMISTRY
Volumes 1 and 2
Edited by Henry Freiser
LIQUID CHROMATOGRAPHY IMASS SPECTROMETRY
Techniques and Applications
Alfred L. Yergey, Charles G. Edmonds, Ivor A. S. Lewis, and Marvin L. Vestal
MASS SPECTROMETRY
Clinical and Biomedical Applications
Volume 1
Edited by Dominic M. Desiderio
MODERN FLUORESCENCE SPECTROSCOPY
Volumes 1-4
Edited by E. L. Wehry
PRINCIPLES OF CHEMICAL SENSORS
Jifi 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.
Mass Spectrometry
Clinical and Biomedical Applications
Volume 1
Edited by
Dominic M. Desiderio
Departments 0/ Neurology and Biochemistry
The University o/Tennessee, Memphis
Memphis, Tennessee
SPRINGER SCIENCE+BUSINESS MEDIA, LLC
Library of Congress Cataloglng-ln-Publ1cation Data
Mass spectrometry / edited by Dominic M. Des1der1o.
p. cm. — (Modern analytical chemistry)
Includes bibliographical references and Index.
Contents: v. 1. Clinical and biomedical applications.
1. Mass spectrometry. 2. Blomolecules—Analysis. I. Des1der1o,
Dominic M. II. Series.
[DNLM: 1. Chemistry, Clinical — Instrumentation. 2. Chemistry,
Clinical—methods. 3. Spectrum Analysis, Mass. QC 454.M3 M41421]
QP519.9.M3M352 1992
616. 07'56—dc20
DWLM/DLC
for Library of Congress 92-49302
CIP
Grateful acknowledgmeht is made to Henry Holt & Company for permission to reprint an excerpt
from "The Road Not Taken," in The Poetry of Robert Frost, New York: Holt, Rinehart and
Winston, 1979.
ISBN 978-1-4899-1175-9 ISBN 978-1-4899-1173-5 (eBook)
DOI 10.1007/978-1-4899-1173-5
© Springer Science+Business Media New York 1992
Originally published by Plenum Press, New York in 1992
Softcover reprint of the hardcover 1st edition 1992
All 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 permission from the Publisher
Contributors
Donald H. Chace, Division of Genetics and Metabolism and Department of
Pediatrics, Duke University Medical Center, Durham, North Carolina 27710
Dominic M. Desiderio, Departments of Neurology and Biochemistry, Charles B.
Stout Neuroscience Mass Spectrometry Laboratory, University of Tennessee
Memphis, Tennessee 38163
Charles G. Edmonds, Chemical Methods and Separations Group, Chemical Sci
ences Department, Pacific Northwest Laboratory, Richland, Washington 99352
Kym F. Faull, The Neuropsychiatric Institute and Department of Psychiatry and
Biobehavioral Sciences, UCLA School of Medicine, Los Angeles, California
90024
John B. Fenn, Department of Chemical Engineering, Yale University, New
Haven, Connecticut 06520
David J. Harvey, Department of Pharmacology, University of Oxford, Oxford
OXl 3QT, England
Tomiko Kuhara, Division of Human Genetics, Medical Research Institute, Kan
azawa Medical University, Uchinada, Ishikawa 920-02, Japan
Joseph A. Loo, Chemical Methods and Separations Group, Chemical Sciences
Department, Pacific Northwest Laboratory, Richland, Washington 99352
Matthias Mann, European Molecular Biology Laboratory, 6900 Heidelberg, Ger
many.
Isamu Matsumoto, Division of Human Genetics, Medical Research Institute,
Kanazawa Medical University, Uchinada, Ishikawa 920-02, Japan
David S. Millington, Division of Genetics and Metabolism and Department of
Pediatrics, Duke University Medical Center, Durham, North Carolina 27710
Diane Rindgen, Department of Chemistry and The Barnett Institute of Chemical
Analysis and Materials Science, Northeastern University, Boston, Massachu
setts 02115
v
vi Contributors
Kunihiko Saito, Department of Medical Chemistry, Kansai Medical University,
Moriguchi, Osaka 570, Japan
Richard D. Smith, Chemical Methods and Separations Group, Chemical Sci
ences Department, Pacific Northwest Laboratory, Richland, Washington
99352
Paul Vouros, Department of Chemistry and The Barnett Institute of Chemical
Analysis and Materials Science, Northeastern University, Boston, Massachu
setts 02115
Preface
Two roads diverged in a wood, and I
I took the one less traveled by,
And that has made all the difference.
Robert Frost
The purpose of this book is to collect recent developments in the use of mass
spectrometry in the field of clinical and biomedical research. Several broad areas
of research are described, including electrospray ionization, metabolism, phys
iology, neuronal systems, and structural modifications of proteins. More specifi
cally, the principles and applications of electrospray ionization are described, and
the use of mass spectrometry in the study of amino acids, platelet-activating
factor, muscle relaxants, acylcarnitines, neurotransmitters and neuropeptides,
cannabinoids, and glycoproteins is described.
This volume was prompted by the continuing use of mass spectrometry in
an expanding variety of research areas in the clinical and biomedical sciences
that require the combination of the efficient ionization of large and polar bio
molecules with the high level of detection sensitivity and molecular specificity
that mass spectrometry and tandem mass spectrometry offer to those areas of
research. The chapters in this book continue to define the concepts of clinical and
biomedical mass spectrometry, and the data reported by the authors in this
volume reflect the very careful attention to experimental detail, the interaction of
mass spectroscopists with biological and clinical scientists, and the continued
development of mass spectrometric methodologies.
It has been a pleasure to work with this group of contributors, and I wish to
express my appreciation to them for writing their chapters and describing the
research done in their laboratories.
This book collects the state-of-the-art mass spectrometry research in the
areas of clinical and biomedical sciences into one volume, and it is hoped that a
newcomer to these fields of research will find this volume helpful to his or her
research.
Dominic M. Desiderio
Memphis, Tennessee
vii
Contents
Chapter 1
Electrospray Mass Spectrometry: Principles and Methods
Matthias Mann and John B. Fenn
1. Introduction .............................................. 1
1.1. History ............................................. 1
1.2. Electrospray vis-a-vis Other Ionization Methods . . . . . . . . . . . . 3
1.3. How ESMS Is Perfonned .............................. 6
2. The Component Processes of ESMS .......................... 7
2.1. Charged "Droplets by Electrospray Dispersion .............. 8
2.2. Ion Fonnation from Charged Droplets .................... l3
2.3. Ion Transport ......................................... 22
2.4. Analysis of ES Ions ................................... 24
3. Some Practical Considerations ............................... 30
3.1. Sample Preparation and Introduction . . . . . . . . . . . . . . . . . . . . . . 30
3.2. Fouling Problems ..................................... 30
3.3. Perfonnance Diagnosis ................................. 31
3.4. Data Systems and Software ............................. 31
4. Summary and Conclusions .................................. 32
References ............................................... 33
Chapter 2
The Analysis of Biomolecules by Electrospray Ionization-Mass
Spectrometry and Tandem Mass Spectrometry
Richard D. Smith, Joseph A. Loo, and Charles G. Edmonds
1. Introduction .............................................. 37
2. Experimental Methods and Considerations ..................... 39
2.1. The Electrospray Source . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
2.2. l?e Atmosphere-Vacuum Interface ...................... 41
ix
x Contents
3. ESI-MS of Large Biomolecules . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . 43
3.1. Molecular Weight Determination ......................... 43
3.2. Positive-Ion Spectra of Large Polypeptides and Proteins. . . . . . 45
3.3. Higher-Order Protein Structure Effects .................... 52
3.4. Negative-Ion Spectra of Large Polypeptides and Proteins ..... 58
4. ESI-Tandem Mass Spectrometry of Polypeptides and Proteins ..... 64
4.1. General Considerations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 64
4.2. Melittin ............................................. 64
4.3. Ribonuclease A ....................................... 73
4.4. Serum Albumins ...................................... 76
5. Combined Separations and ESI-MS of Polypeptides and Proteins .. 84
6. Conclusions .............................................. 91
Summary ................................................ 91
References ............................................... 92
Chapter 3
The Analysis of Muscle Relaxants by Mass Spectrometric Methods
Diane Rindgen and Paul Vouros
1. Introduction ............................................. . 99
2. Chemical Analysis ........................................ . 102
2.1. Other Analytical Techniques ........................... . 102
2.2. Mass Spectrometric Techniques ......................... . 103
3. Conclusions ............................................. . 127
References 129
Chapter 4
Quantitative Analytical Mass Spectrometry of Endogenous Neuropeptides
in Human Pituitaries
Dominic M. Desiderio
1. Introductory Comments and Overview . . . . . . . . . . . . . . . . . . . . . . . . . 133
2. Qualitative Analytical Mass Spectrometry ...................... 135
3. Quantitative Analytical Mass Spectrometry ..................... 136
4. Basic Principles of the Analytical Method .. . . . . . . . . . . . . . . . . . . . . 138
4.1. Tissue Acquisition .................................... 139
4.2. Extraction ........................................... 140
4.3. Reversed-Phase High-Performance Liquid Chromatography. .. 140
4.4. Fast Atom Bombardment Ionization ...................... 141
4.5. Scan Modes .......................................... 142
4.6. Internal Standard . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 148
4.7. Calibration Curves .................................... 148
4.8. Electrospray Ionization ................................. 151