Mass Spectrometry Handbook E-Book

• Herausgeber: John Wiley & Sons
• Kategorie: Wissenschaft und neue Technologien
• Serie: Wiley Series on Pharmaceutical Science
• Sprache: Englisch

Seitenzahl: 3527

Veröffentlichungsjahr: 2012

Beschreibung

Due to its enormous sensitivity and ease of use, mass spectrometry has grown into the analytical tool of choice in most industries and areas of research. This unique reference provides an extensive library of methods used in mass spectrometry, covering applications of mass spectrometry in fields as diverse as drug discovery, environmental science, forensic science, clinical analysis, polymers, oil composition, doping, cellular research, semiconductor, ceramics, metals and alloys, and homeland security. The book provides the reader with a protocol for the technique described (including sampling methods) and explains why to use a particular method and not others. Essential for MS specialists working in industrial, environmental, and clinical fields.

Leseprobe

Table of Contents

Cover

WILEY SERIES ON PHARMACEUTICAL SCIENCE AND BIOTECHNOLOGY: PRACTICES, APPLICATIONS AND METHODS

Title page

Copyright page

FOREWORD

PREFACE

CONTRIBUTORS

SECTION I: BIOTECHNOLOGY/PROTEINS

1 TARGETED PROTEOMICS USING IMMUNOAFFINITY PURIFICATION

1.1 INTRODUCTION

1.2 EXPERIMENTAL PROTOCOLS

1.3 APPLICATIONS OF THE PROTOCOLS

1.4 CONCLUSION

ACKNOWLEDGMENTS

2 MASS SPECTROMETRY-BASED METHODS TO INVESTIGATE POSTTRANSLATIONAL PROTEIN MODIFICATIONS BY LIPID PEROXIDATION PRODUCTS

2.1 PROCEDURE CONTROL

2.2 IDENTIFICATION OF HNE-MODIFIED PEPTIDES IN BIOLOGICAL SAMPLES BY SOLID-PHASE ENRICHMENT AND NANO-LC–ESI-MS/MS

2.3 REAGENTS AND STANDARDS

2.4 COMMENTARY

ACKNOWLEDGMENTS

3 IMAGING MASS SPECTROMETRY (IMS) FOR BIOLOGICAL APPLICATION

3.1 INTRODUCTION

3.2 APPLICATIONS OF MALDI-IMS

3.3 EXPERIMENTAL PROCEDURES

3.4 STATISTICAL PROCEDURES FOR IMS DATA ANALYSIS

4 METHODOLOGIES FOR IDENTIFYING MICROORGANISMS AND VIRUSES BY MASS CATALOGING OF RNAs

4.1 INTRODUCTION: THE IMPORTANCE OF MICROBIAL GENOTYPING

4.2 INFORMATICS: ENABLING ASPECTS OF 16S RRNA AND DATABASE CONSTRUCTION

4.3 EXPERIMENTAL METHODS: PCR, TRANSCRIPTION, AND ENZYMATIC FRAGMENTATION

4.4 DATABASE COMPARISON AND RESULTS: TYPICAL RESULTS OF BACTERIAL AND VIRAL GENOTYPING

4.5 DISCUSSION

ACKNOWLEDGMENTS

SECTION II: PHARMACEUTICAL

5 PRECLINICAL PHARMACOKINETICS: INDUSTRIAL PERSPECTIVE

5.1 INTRODUCTION

5.2 A PHARMACOKINETICS PRIMER

5.3 PARAMETERS THAT DEFINE PHARMACOKINETIC PROFILE

5.4 MODELING TO PREDICT SINGLE- AND MULTIPLE-DOSE PHARMACOKINETIC PROFILES

5.5 ROLE OF LC/MS/MS IN PHARMACOKINETIC ASSESSMENT IN DRUG DISCOVERY

6 LC-MS IN DRUG METABOLISM AND PHARMACOKINETICS: A PHARMACEUTICAL INDUSTRY PERSPECTIVE

6.1 INTRODUCTION

6.2 INSTRUMENTATION UTILIZED FOR DMPK STUDIES

6.3 LC-MS FOR IN VITRO ADME SCREENING

6.4 LC-MS FOR IN VIVO BIOANALYSIS IN SUPPORT OF DMPK

6.5 LC-MS IN DRUG METABOLITE PROFILING AND IDENTIFICATION

6.6 SUMMARY AND PERSPECTIVE

ACKNOWLEDGMENTS

7 QUANTITATIVE MASS SPECTROMETRY IN SUPPORT OF PHARMACOKINETIC STUDIES

7.1 INTRODUCTION

7.2 METHODOLOGY

7.3 CURRENT PROTOCOL

7.4 DEFINITIONS

8 DETERMINATION OF PHARMACOKINETIC PARAMETERS BY HPLC-MS/MS AND UPLC-MS/MS

8.1 INTRODUCTION

8.2 LC-MS/MS ASSAYS FOR PK DETERMINATION IN DRUG DISCOVERY

8.3 PK EVALUATION OF LEAD CANDIDATE AND METABOLITES IN PRECLINICAL DEVELOPMENT

8.4 PK ASSAYS FOR DRUG CANDIDATE DURING CLINICAL DEVELOPMENT

8.5 CONCLUSION

9 METHODS FOR SCREENING ENANTIOSELECTIVE INTERACTIONS IN THE SOLUTION PHASE USING ESI-MS

9.1 INTRODUCTION

9.2 ENANTIOSELECTIVE DISCRIMINATION BY MS

9.3 MEASURING ENANTIOSELECTIVE DISCRIMINATION IN SOLUTION WITH ESI-MS

9.4 EMERGING METHODS AND OUTLOOK

10 HYDROGEN/DEUTERIUM EXCHANGE MASS SPECTROMETRY (HDX MS) IN THE STUDIES OF ARCHITECTURE, DYNAMICS, AND INTERACTIONS OF BIOPHARMACEUTICAL PRODUCTS

10.1 INTRODUCTION

10.2 TECHNIQUE CONSIDERATION

10.3 CONFORMATIONAL PROPERTIES OF PROTEIN DRUGS PROBED BY HDX MS: INTERFERON-Β1A (HDX MS AS A REPORTER OF PROTEIN MISFOLDING AND/OR CONFORMATIONAL INSTABILITY)

10.4 PROTEIN INTERACTION WITH PHYSIOLOGICAL PARTNERS AND THERAPEUTIC TARGETS PROBED BY HDX MS: MECHANISTIC ASPECTS OF TRANSFERRIN-RECEPTOR INTERACTION REVEALED BY HDX MS

10.5 CHALLENGES AND FUTURE DIRECTIONS

ACKNOWLEDGMENTS

11 TOF-SIMS APPLICATIONS TO BIOIMAGING AND BIOMOLECULE EVALUATION METHODS

11.1 INTRODUCTION

11.2 DATA ANALYSIS TECHNIQUES

11.3 SAMPLE PREPARATION

11.4 CHARACTERIZATION OF BIOMOLECULES, BIODEVICES, AND BIOMATERIALS

11.5 IMAGING

11.6 FUTURE DIRECTIONS

11.7 SUMMARY

12 ACCELERATOR MASS SPECTROMETRY IN PHARMACEUTICAL DEVELOPMENT

12.1 INTRODUCTION TO BIOLOGICAL ACCELERATOR MASS SPECTROMETRY

12.2 APPLICATIONS OF AMS IN DRUG DEVELOPMENT

12.3 EXAMPLE CALCULATION OF DOSED TISSUE CONCENTRATION

12.4 SUMMARY

SECTION III: CLINICAL ANALYSIS

13 MASS SPECTROMETRY IN CLINICAL ANALYSIS: SCREENING FOR INBORN ERRORS IN METABOLISM

13.1 INTRODUCTION

13.2 FURTHER PREPARATION FOR ANALYSIS

13.3 DATA PROCESSING

13.4 SUMMARY

14 MASS SPECTROMETRY FOR STEROID ANALYSIS

14.1 INTRODUCTION

14.2 SAMPLE PREPARATION

14.3 GAS CHROMATOGRAPHY–MASS SPECTROMETRY

14.4 ESI-MS AND ELECTROSPRAY IONIZATION TANDEM MASS SPECTROMETRY (ESI-MS/MS)

14.5 APPLICATION OF MS TO STEROID ANALYSIS

14.6 NEW APPLICATIONS

14.7 PROTOCOLS

14.8 CONCLUSIONS

ACKNOWLEDGMENT

APPENDIX 14.1

APPENDIX 14.2

APPENDIX 14.3

APPENDIX 14.4

SECTION IV: FORENSICS

15 FORENSIC APPLICATIONS OF ISOTOPE RATIO MASS SPECTROMETRY

15.1 INTRODUCTION

15.2 FUNDAMENTAL PRINCIPLES

15.3 THEORY OF OPERATION

15.4 APPLICATIONS OF IRMS

15.5 GUIDELINES FOR THE INSTALLATION AND IMPLEMENTATION OF IRMS INTO AN OPERATIONAL FORENSIC LABORATORY

15.6 SUMMARY

16 ANALYSIS OF TRIACETONE TRIPEROXIDE EXPLOSIVE BY MASS SPECTROMETRY

16.1 INTRODUCTION

16.2 BACKGROUND

16.3 ANALYTICAL METHODS

16.4 SAMPLING METHODOLOGY

16.5 CONCLUSION

ACKNOWLEDGMENTS

SECTION V: SPACE EXPLORATION

17 MASS SPECTROMETRY IN SOLAR SYSTEM EXPLORATION

17.1 INTRODUCTION

17.2 COMPONENTS OF A MASS SPECTROMETER: CONSIDERATIONS FOR SPACE APPLICATIONS

17.3 CHROMATOGRAPHIC INSTRUMENTATION IN THE SPACE PROGRAM

17.4 OVERVIEW OF PAST AND PRESENT PLANETARY MASS SPECTROMETER EXPERIMENTS

17.5 CONCLUSION

ACKNOWLEDGMENT

18 APPLICATION OF GC × GC–TOFMS TO THE CHARACTERIZATION OF EXTRATERRESTRIAL ORGANIC MATTER

18.1 INTRODUCTION

18.2 EXPERIMENTAL

18.3 RESULTS AND DISCUSSION

18.4 CONCLUSIONS

ACKNOWLEDGMENTS

SECTION VI: HOMELAND SECURITY

19 METHODS OF MASS SPECTROMETRY IN HOMELAND SECURITY APPLICATIONS

19.1 INTRODUCTION

19.2 PROTEOMICS-BASED DETECTION METHODS

19.3 POLYMERASE CHAIN REACTION–MASS SPECTROMETRY

19.4 SMALL MOLECULE-BASED MASS SPECTROMETRY METHODS

19.5 CONCLUSIONS

ACKNOWLEDGMENTS

20 HOMELAND SECURITY

20.1 INTRODUCTION

20.2 CHEMICAL THREATS

20.3 BIOLOGICAL THREATS

20.4 NUCLEAR AND RADIOLOGICAL THREATS

20.5 EXPLOSIVE THREATS

20.6 CONCLUSION

ACKNOWLEDGMENT

21 MASS SPECTROMETRY IN HOMELAND SECURITY

21.1 INTRODUCTION

21.2 DETECTION METHODOLOGY: BULK DETECTION AND TRACE DETECTION

21.3 INSTRUMENTATION

21.4 DETECTION OF EXPLOSIVES BY MS

21.5 SYSTEM INTEGRATION

21.6 CONCLUSION

ACKNOWLEDGMENTS

22 MEASUREMENTS OF SURFACE CONTAMINANTS AND SORBED ORGANICS USING AN ION TRAP SECONDARY ION MASS SPECTROMETER

22.1 INTRODUCTION

22.2 INSTRUMENTAL DESCRIPTION

22.3 ANALYSIS OF ALKYL METHYLPHOSPHONIC ACIDS (AMPAS)

22.4 ANALYSIS OF BLISTER AGENTS

22.5 ANALYSIS OF NERVE AGENTS

22.6 DIRECT SAMPLE INTRODUCTION MASS SPECTROMETRY (DSIMS) ANALYSIS OF SURROGATES IN CONTACT WITH PERMEABLE MATERIALS

22.7 CONCLUSIONS AND PROSPECTS

ACKNOWLEDGMENT

23 DETERMINATION OF ACTINIDES: DETERMINATION OF LOW-CONCENTRATION URINE URANIUM 235/238 ISOTOPE RATIOS

23.1 INTRODUCTION

23.2 APPROACHES

23.3 COMMENTARY

23.4 SUMMARY

SECTION VII: FOOD ANALYSIS

24 MASS SPECTROMETRY IN AGRICULTURE, FOOD, AND FLAVORS: SELECTED APPLICATIONS

24.1 INTRODUCTION

24.2 EXAMPLES OF GC/MS AND LC/MS APPLICATIONS FOR PROFILING PLANT METABOLITES AND DETERMINATION OF SELECTED CONTAMINANTS IN GRAIN AND FLAVOR COMPOUNDS IN FOODS

25 TOP-DOWN PROTEOMIC IDENTIFICATION OF PROTEIN BIOMARKERS OF FOOD-BORNE PATHOGENS USING MALDI-TOF-TOF-MS/MS

25.1 INTRODUCTION

25.2 BASIC PROTOCOL

25.3 COMMENTARY

SECTION VIII: ENVIRONMENTAL

26 DETERMINATION OF DITHIOCARBAMATE FUNGICIDES IN FOOD BY HYDROPHILIC INTERACTION LIQUID CHROMATOGRAPHY/MASS SPECTROMETRY

26.1 CHEMISTRY AND USES OF DITHIOCARBAMATES (DTCs)

26.2 CHALLENGES OF RESIDUE ANALYSIS OF DTC FUNGICIDES

26.3 PRECAUTIONS CONCERNING INSTABILITY OF DTCs

26.4 HYDROPHILIC INTERACTION LIQUID CHROMATOGRAPHY (HILIC)

26.5 MASS SPECTRA OF DTCs

26.6 SAMPLE EXTRACTION

26.7 DETERMINATION OF DTC FUNGICIDES BY LC/MS AND LIQUID CHROMATOGRAPHY/TRIPLE QUADRUPOLE MASS SPECTROMETRY (LC/MS-MS)

26.8 METHOD COMPARISON

26.9 TROUBLESHOOTING

27 DISINFECTANT AND BY-PRODUCT ANALYSIS IN WATER TREATMENT BY MEMBRANE INTRODUCTION MASS SPECTROMETRY

27.1 METHODS

27.2 APPLICATIONS

28 PROTON TRANSFER REACTION MASS SPECTROMETRY (PTR-MS)

28.1 INTRODUCTION

28.2 HOW TO IDENTIFY ISOMERIC/ISOBARIC COMPOUNDS

28.3 APPLICATIONS

28.4 CONCLUSIONS AND PROSPECT

ACKNOWLEDGMENTS

29 DETERMINATION OF CHLORINATED COMPOUNDS IN DIALYSIS WATER AND IN BIOLOGICAL FLUIDS/MATRICES

29.1 QUALITY CONTROL

29.2 DETERMINATION OF CHLORINATED COMPOUNDS IN DIALYSIS WATER AND BIOLOGICAL FLUIDS BY SPME-GC/MS

29.3 COMMENTARY

SECTION IX: GEOLOGICAL

30 MASS SPECTROMETRY TECHNIQUES FOR ANALYSIS OF OIL AND GAS TRAPPED IN FLUID INCLUSIONS

30.1 INTRODUCTION: WHAT ARE FLUID INCLUSIONS?

30.2 SCREENING OF SAMPLES PRIOR TO DETAILED GC-MS ANALYSIS

30.3 METHODS FOR GEOCHEMICAL ANALYSIS BY GC-MS OF GROUPS OF OIL INCLUSIONS

30.4 TOWARD ANALYSIS OF THE CHEMISTRY OF SINGLE PETROLEUM INCLUSIONS

30.5 GEOLOGICAL APPLICATIONS OF OIL INCLUSION ANALYSIS BY GC-MS

30.6 RELIABILITY AND CONSTRAINTS ON FLUID INCLUSION OIL ANALYSIS BY GC-MS

30.7 SUMMARY

31 LA-MC-ICP-MS APPLIED TO U-PB ZIRCON GEOCHRONOLOGY

31.1 INTRODUCTION

31.2 PRELIMINARY REMARKS

31.3 MATERIALS AND METHODS

31.4 DIRECT PB/PB ISOTOPE RATIO MEASUREMENTS ON NATURAL SOLUTIONS AT VERY LOW CONCENTRATION (WITHOUT LASER)

31.5 PB/PB AND U/PB ISOTOPE RATIO MEASUREMENTS TO DATE ZIRCON USING A LASER COUPLED WITH MC-ICP-MS

31.6 FRONTIER IN U-PB DATING: AGE DETERMINATION IN QUATERNARY ZIRCON USING LA-MC-ICP-MS

31.7 CONCLUDING REMARKS

ACKNOWLEDGMENTS

32 HYDROCARBON PROCESSING

32.1 INTRODUCTION

32.2 APPLICATIONS OF MS IN UNCONVENTIONAL OIL REFINING

32.3 APPLICATIONS OF MS IN COAL-TO-LIQUIDS (CTL) PROCESSES

32.4 SUMMARY

33 HYDROCARBON PROCESSING: MALDI-MS OF POLYDISPERSE HYDROCARBON SAMPLES

33.1 DESCRIPTION OF PROBLEM

33.2 SUMMARY OF RELEVANT WORK IN THIS FIELD BY OTHERS

33.3 CURRENT STATUS OF TECHNIQUE WITH BRUKER DALTONICS REFLEX IV MALDI-TOF-MS

33.4 RESULTS

33.5 SUPPORTING INFORMATION FROM OTHER TECHNIQUES

33.6 CONCLUSIONS

34 RENEWABLE ENERGY: MASS SPECTROMETRY IN BIOFUEL RESEARCH

34.1 INTRODUCTION

34.2 GENERAL PROCEDURE FOR SINGLE QUADRUPOLE ESI-MS AND CHEMOMETRICS IN BIOFUEL RESEARCH

34.3 APPLICATIONS USING SINGLE QUADRUPOLE ESI-MS AND CHEMOMETRICS IN BIOFUEL RESEARCH

34.4 CONCLUSIONS AND FUTURE PERSPECTIVES

SECTION X: ARCHAEOLOGY

35 MASS SPECTROMETRY IN ARCHAEOLOGY

35.1 INTRODUCTION

35.2 ORDER OF TOPICS

35.3 ISOTOPE RATIO MEASUREMENTS

35.4 COMPOSITIONAL ANALYSIS BY MS IN ARCHAEOLOGY

35.5 PROTEOMICS IN ARCHAEOLOGY

36 ARCHAEOMETRIC DATA FROM MASS SPECTROMETRIC ANALYSIS OF ORGANIC MATERIALS: PROTEINS, LIPIDS, TERPENOID RESINS, LIGNOCELLULOSIC POLYMERS, AND DYESTUFF

36.1 INTRODUCTION

36.2 GC/MS

36.3 PY-GC/MS

36.4 HPLC/MS

36.5 DIRECT MS TECHNIQUES: DE-MS, DTMS, DI-MS, ESI-MS AND ESI-MS/MS, MALDI-MS, AND LDI-MS

37 LASER ABLATION ICP-MS IN ARCHAEOLOGY

37.1 BACKGROUND AND CONTEXT

37.2 LA-ICP-MS ELEMENTAL ANALYSIS

37.3 ELEMENTAL ANALYSIS WITH LA-TOF-ICP-MS

37.4 ISOTOPE RATIO ANALYSIS WITH LA-ICP-MS

37.5 DATING APPLICATIONS OF LA-ICP-MS AND LA-MC-ICP-MS

37.6 CONCLUSION

ACKNOWLEDGMENTS

38 SPATIALLY RESOLVED MS IN THE STUDY OF ART AND ARCHAEOLOGICAL OBJECTS

38.1 INTRODUCTION

38.2 ROLE OF MASS SPECTROMETRY (MS) IN STUDYING WORKS OF ART AND ARCHAEOLOGICAL REMAINS

38.3 SIMS

38.4 LDI-BASED MS METHODS

38.5 PROTOCOLS

39 LASER ABLATION–INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY FOR THE INVESTIGATION OF ARCHAEOLOGICAL SAMPLES

39.1 INTRODUCTION

39.2 PRINCIPLE OF LA-ICPMS

39.3 KEY ASPECTS FOR DEVELOPING AN LA-ICPMS METHOD IN ARCHAEOMETRIC RESEARCH: MULTIELEMENTAL APPLICATIONS

39.4 LA-ICPMS FOR ISOTOPIC ANALYSIS OF ARCHAEOLOGICAL SAMPLES

39.5 CONCLUSIONS AND FUTURE RESEARCH

ACKNOWLEDGMENTS

SECTION XI: SURFACE ANALYSIS

40 MASS SPECTROMETRY IN SEMICONDUCTOR RESEARCH

40.1 INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY (ICP-MS)

40.2 LA-ICP-MS

40.3 SSMS

40.4 GDMS

40.5 SIMS

40.6 SECONDARY NEUTRAL MASS SPECTROMETRY (SNMS)

40.7 ACCELERATOR MASS SPECTROMETRY (AMS)

40.8 APT

40.9 OUTLOOK

41 ANALYSIS OF THIN AND THICK FILMS

41.1 INTRODUCTION

41.2 THIN AND THICK LAYERS: A TENTATIVE DEFINITION

41.3 WHAT SPECIFIC INFORMATION MS TECHNIQUES COULD BRING TO THIN AND THICK FILMS ANALYSIS COMPARED TO OTHER TECHNIQUES?

41.4 MAIN MS TECHNIQUES APPLIED TO THIN/THICK FILMS

41.5 TIME OF SPUTTERING/SPEED OF ACQUISITION TRADE-OFF

41.6 DIFFERENCES IN SPUTTERING/IONIZATION MECHANISMS BETWEEN SIMS AND GD-MS

41.7 PULSE SHAPES AND HOW TO BEST USE TEMPORAL INFORMATION FOR PULSED GLOW DISCHARGE MASS SPECTROMETRY

41.8 MEASUREMENT AND DATA INTERPRETATION IN GD-TOFMS

41.9 PRACTICAL EXAMPLES

41.10 CONCLUSIONS

42 SIMS FOR ORGANIC FILM ANALYSIS

42.1 INTRODUCTION

42.2 ORGANIC COMPOUNDS ANALYSIS AND IMAGING

42.3 DEPTH PROFILING AND 3D ANALYSIS

42.4 CONCLUSIONS

ACKNOWLEDGMENTS

43 CERAMICS: CONTRIBUTION OF SECONDARY ION MASS SPECTROMETRY (SIMS) TO THE STUDY OF CRYSTAL CHEMISTRY OF MICA MINERALS

43.1 SECONDARY ION MASS SPECTROMETRY TECHNIQUE AS A FUNDAMENTAL TOOL FOR IN SITU ELEMENTAL ANALYSIS

43.2 LIGHT AND VOLATILE ELEMENTS Li, Be, B, H, AND F

43.3 IMPROVEMENTS OF SIMS PROCEDURES FOR LIGHT AND VOLATILE ELEMENTS

43.4 SIMS PROCEDURES FOR THE STUDY OF LIGHT ELEMENTS IN MICAS

43.5 CHEMISTRY AND STRUCTURE OF MICAS: A SYNTHETIC OVERVIEW

43.6 INVESTIGATION OF MICAS

43.7 THE ROLE OF SIMS IN THE CONTEXT OF A MULTIMETHODIC APPROACH: CHARACTERIZATION OF THE IONIC SITE OF MICAS

43.8 THE ROLE OF SIMS IN THE CHARACTERIZATION OF INHOMOGENEITIES AT THE MICROMETER SCALE IN MICAS: SOME EXAMPLES

43.9 CONCLUDING REMARKS

ACKNOWLEDGMENTS

APPENDIX 43.1

APPENDIX 43.2

SECTION XII: POLYMERS

44 ETV-ICPMS FOR ANALYSIS OF POLYMERS

44.1 INTRODUCTION

44.2 BASIC OPERATING PRINCIPLES OF ETV-ICPMS

44.3 METHOD DEVELOPMENT FOR QUANTITATIVE ANALYSIS OF POLYMERS

44.4 OVERVIEW: GENERAL CAPABILITIES OF ETV-ICPMS FOR TRACE ANALYSIS OF POLYMERS

ACKNOWLEDGMENTS

45 POLYMERS

45.1 INTRODUCTION

45.2 ESI

45.3 ESI AND POLYMERS WITH A BROAD MMD

45.4 NANOELECTROSPAY IONIZATION

45.5 ATMOSPHERIC PRESSURE ELECTROSPRAY IONIZATION

45.6 DESORPTION ELECTROSPRAY IONIZATION

45.7 ION MOBILITY SEPARATION

45.8 MALDI

45.9 MALDI MATRICES

45.10 MALDI SAMPLE PREPARATION

45.11 DIFFERENTIATING LINEAR AND CYCLIC CHAINS BY MALDI

45.12 COMPARING MALDI SPECTRA AND SIZE EXCLUSION CHROMATOGRAMS

45.13 MALDI AND POLYMERS WITH A BROAD MMD

45.14 THE OFFLINE COMBINATION OF MALDI AND SEC

45.15 OPTIMIZATION OF THE SEC-MALDI METHOD

45.16 MALDI AND OTHER CHROMATOGRAPHIC TECHNIQUES

45.17 MALDI OF COPOLYMERS AND OTHER COMPLEX POLYMERS

45.18 TANDEM MASS SPECTROMETRY

46 MASS SPECTROSCOPY IN POLYMER RESEARCH

46.1 INTRODUCTION

46.2 STRUCTURAL ANALYSIS

46.3 ABSOLUTE MOLECULAR WEIGHTS AND MOLECULAR WEIGHT DISTRIBUTIONS

46.4 POLYMER DEGRADATION

46.5 POLYMER SURFACE AND INTERFACE

47 LASER MASS SPECTROMETRY APPLIED TO THE ANALYSIS OF POLYMERS

47.1 INTRODUCTION

47.2 METHODS

47.3 RESULTS

47.4 CONCLUSION

SECTION XIII: ANALYTICAL TECHNIQUES

48 MEASURING THERMODYNAMIC PROPERTIES OF METALS AND ALLOYS

48.1 INTRODUCTION

48.2 KNUDSEN CELL VAPOR SOURCES AND MOLECULAR BEAMS

48.3 MASS SPECTROMETRIC ANALYSIS OF THE MOLECULAR BEAM

48.4 MEASUREMENT OF THERMODYNAMIC PROPERTIES OF METALS AND ALLOYS

48.5 CHECKS FOR CORRECT OPERATION AND CONSISTENCY IN MEASUREMENTS

48.6 FUTURE DIRECTIONS

48.7 SUMMARY AND CONCLUSIONS

ACKNOWLEDGMENTS

APPENDIX 48.1

49 HIGH-PERFORMANCE THIN-LAYER CHROMATOGRAPHY–MASS SPECTROMETRY FOR ANALYSIS OF SMALL MOLECULES

49.1 HIGH-PERFORMANCE THIN-LAYER CHROMATOGRAPHY

49.2 COUPLING TO MASS SPECTROMETRY

49.3 COMMERCIALLY AVAILABLE HPTLC-MS SYSTEMS

49.4 COMPARISON OF THE APPROACHES AND OUTLOOK

50 LASER IONIZATION MASS SPECTROMETRY OF INORGANIC IONS

50.1 INTRODUCTION

50.2 SAMPLE PREPARATION

50.3 MASS AXIS CALIBRATION

50.4 LIMITS OF DETECTION

50.5 DETERMINING OXIDATION STATES

50.6 FOLLOWING THE COURSE OF REACTIONS

50.7 VARIOUS APPLICATIONS

50.8 DESORPTION/IONIZATION ON SILICON (DIOS) AND OTHER MATRIX-FREE APPROACHES

50.9 COMPARISON OF LDI WITH OTHER MASS SPECTROMETRIC IONIZATION TECHNIQUES

50.10 CONCLUSION

51 MASS SPECTROMETRY IN THE SSITKA STUDIES

51.1 INTRODUCTION

51.2 SSITKA EXPERIMENTAL

51.3 THEORETICAL BASES OF SSITKA FOR DISCRIMINATION OF REACTION MECHANISMS

51.4 SSITKA APPLICATION FOR THE IDENTIFICATION OF REACTION MECHANISMS

51.5 ISOTOPE TRANSIENT KINETICS APPLICATION FOR THE STUDY OF MASS TRANSFER PROCESSES

51.6 SSITKA APPLICATION FOR THE STUDY OF OXYGEN TRANSPORT IN SOLIDS

51.7 BRØNSTED ACIDITY STUDY OF FIBERGLASS MATERIALS BY H/D EXCHANGE

51.8 CONCLUSION

52 PROTON TRANSFER REACTION MASS SPECTROMETRY: APPLICATIONS IN THE LIFE SCIENCES

52.1 INTRODUCTION

52.2 PTR-MS

52.3 PLANT MEASUREMENTS

52.4 BREATH ANALYSIS

52.5 CONCLUSION

Index

WILEY SERIES ON PHARMACEUTICAL SCIENCE AND BIOTECHNOLOGY: PRACTICES, APPLICATIONS AND METHODS

Series Editor:

Mike S. Lee

Milestone Development Services

Mike S. Lee • Integrated Strategies for Drug Discovery Using Mass Spectrometry

Birendra Pramanik, Mike S. Lee, and Guodong Chen • Characterization of Impurities and Degradants Using Mass Spectrometry

Mike S. Lee and Mingshe Zhu • Mass Spectrometry in Drug Metabolism and Disposition: Basic Principles and Applications

Mike S. Lee (editor) • Mass Spectrometry Handbook

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Library of Congress Cataloging-in-Publication Data:

Mass spectrometry handbook / edited by Mike S. Lee.

p. cm.

 Includes index.

 ISBN 978-0-470-53673-5 (cloth)

 1. Mass spectrometry–Handbooks, manuals, etc. I. Lee, Mike S., 1960–

 QD96.M3M36 2012

 543'.65–dc23

2011034171

FOREWORD

It is a pleasure to provide this foreword to the Handbook of Mass Spectrometry, edited by Dr. Mike S. Lee, a PhD graduate of my research group at the University of Florida 25 years ago. Mike is not only an outstanding scientist and a visionary in how mass spectrometry can drive science in a diverse range of disciplines; he is also a master at assembling and leading a team of experts, as he has ably demonstrated with this volume.

Mass spectrometry, although barely a hundred years old, has become the dominant force in modern analytical chemistry. It provides unparalleled levels of sensitivity and selectivity for trace analysis, and an impressive range of capabilities and application. Some of these unique capabilities arise from the unique feature of mass spectrometry (compared to other spectrometric methods) that the sample itself (matter) passes through the spectrometer and is separated and detected. Thus mass spectrometry is both a spectrometric method and a separation method!

Many of the capabilities of modern mass spectrometry arise from the remarkable advances in instrumentation over the past 30 years, many of which are reviewed in this handbook. Advances in ionization techniques have expanded the applicability of mass spectrometry from small, volatile, and thermally stable molecules to large, nonvolatile, and labile molecules, including intact proteins and polymers. The coupling of mass spectrometry with separation techniques (gas chromatography [GC], liquid chromatography [LC], capillary electrophoresis [CE], and even a second stage of mass spectrometry) has established it as the standard for trace mixture analysis. Innovations in mass analyzers continue to bring improved performance in terms of mass resolution, mass range, and sensitivity. And perhaps most impressively, the pace of advances in mass spectrometry instrumentation and methodologies has not slacked off—we continue to see remarkable advances every year.

I often date the “coming of age” of modern analytical mass spectrometry to a 1982 quote from Chemical & Engineering News:

Mass spectrometry has advanced to the point that it’s no longer (as has been said) … “the method of choice – if there’s no other way.”

Indeed, mass spectrometry is the method of choice for an amazing range of applications, from structure determination of proteins to forensic toxicology, from fundamental studies of reaction kinetics to imaging tissues. And that breadth of use and dominance of mass spectrometry is well represented in the chapters assembled here.

The remarkable growth of mass spectrometry is well represented in the growth of attendance at the Annual Meeting on Mass Spectrometry and Allied Topics of the American Society for Mass Spectrometry, from 700 attendees in the mid-1970s to 7000 today. This reflects not only the expanding scope of application of the technique, but also the ease with which modern mass spectrometers can be mastered by users new to the field, without needing to understand the underlying fundamentals. This handbook provides in its 13 sections and 52 chapters an excellent overview of that wide range of applications. The breadth of coverage makes this an excellent resource for practicing mass spectrometrists as well as to those new to the field.

Welcome to a hopefully stimulating journey through modern mass spectrometry and its breadth of applications!

RICHARD A. YOST

University of Florida

October 2011

PREFACE

Mass spectrometry is an integral part of modern research in academic, industrial, and clinical laboratories. The Handbook of Mass Spectrometry represents the current state-of-the-art practices in these laboratory settings. The purpose of the handbook is to provide a unique reference that allows for easy access to a variety of applications that involve mass spectrometry. The intent of the handbook is to provide a resource for beginners, practitioners, and experts to obtain vital background, current approaches, and real-world methodology. Further, the handbook can also be viewed as an interactive time capsule to perhaps delineate “where we are,” “where we came from,” and “where we are headed” with regard to these specific applications—current and emerging. Thus, the handbook is not intended to be comprehensive, but rather to provide unique, in-depth information on specific techniques and experiences.

The evolution of mass spectrometry has been both dramatic and fascinating. Trace analytical measurement, specifically the demand for trace mixture analysis, has created an increased demand for this powerful tool. In many cases, the preference for the trace mixture sample type has transformed the mass spectrometer into a gold standard platform for qualitative and quantitative assays.

In its simplest form, a mass spectrometer can be viewed as a molecular weighing machine. Much like we regularly weigh ourselves in the morning to provide an early, facile benchmark for personal health and well-being, mass spectrometers are being used for a similar function. Specifically, a mass spectrometer is routinely used to monitor the “well-being” of a specific analyte. Moreover, the confirmation each analyte (structure or amount), or ensemble of analytes, often provides a surrogate benchmark into a specific process that relates to a biological or chemical condition.

Regardless of the application, mass spectrometry-based methods can be organized into two areas of analytical focus: qualitative (“What is it?”) and quantitative (“How much is there?”) analysis. Similar to the building of a picture puzzle—starting with the edges (the molecular ion!) to define the size of the puzzle and/or set a defined limit to where all remaining subsequent puzzle pieces (fragment ions!) may fit inside the edges—the use of mass spectrometry provides a powerful way to quickly and confidently “define the edges” by providing molecular weight information.

Molecular weight can then become a surrogate for confirmation or even be used for the identification of a targeted compound, particularly when used in conjunction with an authentic standard or chromatographic technique, for example. Advanced studies that involve two or more dimensions of mass analysis can also be used to obtain specific structural detail (fragment ions that correspond to specific pieces of the picture puzzle!) or more selectivity to enable powerful approaches for high throughput quantitation. Moreover, similar to how high-definition televisions are improving our entertainment experience, the higher resolution mass spectrometry (and chromatography!) technologies are poised to provide a benefit to the scientific community in perhaps a highly routine manner.

Thus, the diverse contributions to the handbook are essentially unified based on the puzzle analogy. Confident and definitive “What is it?” and/or “How much is there?” information is obtained via molecular weight measurements provided by the mass spectrometer. The specific mass spectrometer and, of course, specific chemistries (i.e., sample preparation, chromatography, ionization) help to define the analytical method.

Although the handbook is not necessarily designed to be comprehensive, the contributions represent an impressive array of critical work from diverse areas ranging from biological studies to food analysis to environmental analysis to archaeology. Each chapter in the handbook contains several compulsory elements: (1) essential background and history of the application; (2) detailed analytical methodology; and finally, (3) valuable references for more in-depth study.

Each contributor has provided critical updates in their respective field of expertise. Both current and emerging trends are highlighted. Perhaps a distinguishing feature of the handbook is that nearly all of the chapters provide a detailed description of the actual methodologies used in their respective laboratory—specifically intended so that others may initiate similar work in their respective laboratory. We hope that this unique feature will allow broad base interest and use for all scientists!

Certainly, the handbook is quite diverse in scope and application. The handbook is organized into 13 sections—starting with life sciences and culminating with specialized analytical techniques. Section I provides an exciting perspective on the recent applications of mass spectrometry for the identification of proteins and peptides. These methods represent the emerging role of mass spectrometry in biology-related fields to assist with the determination of both process and function. The section also provides the recent methodology used for imaging studies on biological systems as well as the profiling of microorganisms and viruses. The current state-of-the-art work performed in the pharmaceutical industry is featured in Section II. A continuum of work that begins with drug discovery activities such as pharmacokinetics (surrogate studies to determine dosing regimen in humans) as well as mass spectrometry methods for screening, characterization, and imaging are featured in Section II. The pharmaceutical section concludes with perspectives into drug development with the use of accelerator mass spectrometry. Exciting growth and, perhaps, a renaissance, is currently experienced in the field of clinical analysis. Section III provides a timely and critical update on the use of mass spectrometry for the screening of inborn errors and steroid analysis in a clinical laboratory setting. The distinct criteria and features necessary for a clinical laboratory—as opposed to a research setting—are powerfully represented and easily understood. Forensics is indeed a challenging area of focus that requires diverse analytical tools as well as a strict protocol of analysis—from sampling to preparation to analysis to reporting. Section IV contains two important applications of mass spectrometry in this field. The use of isotope ratio mass spectrometry is highlighted followed by a specific application that describes the analysis of the explosive triacetone triperoxide. Section V addresses the important role of mass spectrometry in programs involved with space exploration. A fascinating perspective on the use of mass spectrometry for solar system exploration is provided. This chapter is followed by work that features the use of gas chromatography (GC)/gas chromatography–mass spectrometry (GC-MS) for the characterization of extraterrestrial organic matter. Travel and safety has been greatly impacted over the past decade. Section VI contains the recent work that describes the various uses of mass spectrometry for homeland security. Specific methods are detailed along with the requirements and challenges for this specialized application. The safety of our food and subsequent food supply is of critical worldwide importance. The role of mass spectrometry for food analysis is highlighted in Section VII. A perspective on agriculture, food and flavors is provided to give the reader some historical perspectives and background in food analysis. The recent mass spectrometry application of “top-down” proteomic methods for the identification of biomarkers of foodborne pathogens highlights future direction and analysis formats. Perhaps a cornerstone of commercial applications of mass spectrometry is in the field of environmental analysis. Section VIII contains the recent work that details how mass spectrometry is used to monitor targeted analytes such as fungicides, commercial by-products, and targeted carcinogens. Section IX focuses on geology. In this section, the authors provide their unique perspective on mass spectrometry applications that address the analysis of oil and gas, geochronology, and hydrocarbon processing. The section concludes with a chapter on the current status and prospects for renewable energy. Mass spectrometry methods have made significant contributions to archaeology. Section X focuses on recent work to give the reader historical and background information as well as specific studies that require careful field work (collection of the actual samples!) along with trace analysis using mass spectrometry-based methods. Surface analysis is a challenging area of study with very specific criteria for analysis. Section XI provides perspective and recent methods in the area of semiconductor research, organic film analysis, and characterization of ceramic materials. Section XII provides perspective on the role and uses of mass spectrometry in polymer research. Background and methodology are highlighted from three leading laboratories. Specialized analytical techniques are presented in Section XIII. The section begins with a chapter on the approaches used for the measurement of metals and alloys followed by a variety of interesting techniques that involve the use of thin layer chromatography, laser ionization, steady-state isotopic transient kinetic analysis, and proton transfer reaction mass spectrometry.

It is my sincere hope that the handbook provides the information and details to assist scientists with current work as well as inspire future studies. Also, because of the vast content of work, it is hoped that seemingly unrelated applications provide helpful insight into novel uses of mass spectrometry and promote new areas of research.

Finally, I wish to acknowledge the contributions of many—authors, collaborators, editors, and families—who made this handbook possible. Also, along with the terrific editorial staff at John Wiley & Sons, I would like to give a special acknowledgment to Gladys Mok, Managing Editor at John Wiley & Sons, for her significant contributions and premier support during this project.

MIKE S. LEE

Milestone Development Services

August 2011

CONTRIBUTORS

Rinat R. Abzalimov, PhD, Department of Chemistry, University of Massachusetts-Amherst, Amherst, MA

Thomas Andrews, Division of Chemistry and Chemical Engineering, Southwest Research Institute, San Antonio, TX

Satoka Aoyagi, PhD, Department of Regional Development, Faculty of Life and Environmental Science, Shimane University, Matsue-shi, Shimane, Japan

Anthony D. Appelhans, Idaho National Laboratory, Interfacial Chemistry Department, Idaho Falls, ID

Maite Aramendía Marzo, PhD, Centro Universitario de la Defensa, Academia General Militar, Carretera de Huesca, Zaragoza, Spain

Athula B. Attygalle, PhD, Center for Mass Spectrometry, Department of Chemistry, Chemical Biology, and Biomedical Engineering, Stevens Institute of Technology, Hoboken, NJ

B.S. Bal’zhinimaev, PhD, Boreskov Institute of Catalysis, Siberian Branch of the Russian Academy of Sciences, Novosibirsk, Russia

Salvatore Battiato, Institute of Chemistry and Technology of Polymers, National Research Council of Italy, Catania, Italy

Luther W. Beegle, PhD, Jet Propulsion Laboratory, California Institute of Technology, Pasadena, CA

Philippe Belenguer, PhD, University of Toulouse, France

Graham Bench, PhD, Lawrence Livermore National Laboratory, Center for Accelerator Mass Spectrometry, Livermore, CA

Sarah J. Benson, PhD, Australian Federal Police, Forensic & Data Centres, Canberra, ACT, Australia

Cedric E. Bobst, PhD, Department of Chemistry, University of Massachusetts-Amherst, Amherst, MA

Nerea Bordel Garcia, PhD, University of Oviedo, Spain

Jérôme Bour, PhD, Department of Advanced Materials and Structures, Centre de Recherche Public Henri Tudor (CRPHT), Esch sur Alzette, Luxembourg

Gísli Bragason, BSc, MBA, ArcticMass, Sturlugata, Reykjavik, Iceland

Bruce A. Buchholz, PhD, Lawrence Livermore National Laboratory, Center for Accelerator Mass Spectrometry, Livemore, CA

John C. Cambier, PhD, Integrated Department of Immunology, National Jewish Medical and Research Center, Denver, CO