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  • LIQUID CHROMATOGRAPHY - MASS SPECTROMETRY

    • PREFACE TO THE THIRD EDITION

    • PREFACE TO THE SECOND EDITION

    • PREFACE TO THE FIRST EDITION

    • CONTENTS

    • ABBREVIATIONS

  • INTRODUCTION

    • Chapter 1 LIQUID CHROMATOGRAPHY AND SAMPLE PRETREATMENT

      • 1. Introduction

      • 2. Instrumentation for liquid chromatography

        • 2.1 The column

        • 2.2 General detector characteristics

        • 2.3 Detectors for LC

      • 3. Separation mechanisms

        • 3.1 Intra- and intermolecular interactions

        • 3.2 Reversed- phase chromatography

        • 3.3 Chromatography of ionic compounds

      • 4. Other modes of liquid chromatography

        • 4.1 Perfusion chromatography

        • 4.2 Immunoaffinity chromatography

        • 4.3 Chiral separation

        • 4.4 Monolithic columns

        • 4.5 Hydrophilic interaction chromatography

        • 4.6 Coupled- column chromatography

      • 5. Sample pretreatment strategies

        • 5.1 Protein precipitation

        • 5.2 Liquid extraction and liquid- liquid extraction

        • 5.3 Solid- phase extraction

        • 5.4 On- line SPE – LC

        • 5.5 Turbulent- flow chromatography

        • 5.6 Restricted- access stationary phases

      • 6. References

    • Chapter 2 MASS SPECTROMETRY

      • 1. Introduction

      • 2. Analyte ionization

        • 2.1 Electron ionization

        • 2.2 Chemical ionization

        • 2.3 Electron- capture negative ionization

        • 2.4 Energy- sudden or desorption ionization

        • 2.5 Nebulization ionization

      • 3. Information from mass spectrometry

        • 3.1 m/z Axis calibration

        • 3.2 Full- spectrum analysis and selected- ion monitoring

      • 4. Mass analysis

        • 4.1 Linear quadrupole MS and MS – MS instruments

          • Tandem mass spectrometry

          • Triple-quadrupole instrument for MS•MS

          • Analysis modes in MS•MS

        • 4.2 Quadrupole ion trap MS and MS – MSn instruments

          • MS•MS and MS•MSn in an ion trap

          • Data-dependent operation in MS•MS

          • Developments in ion-trap MS and MS•MSn

          • Quadrupole•linear ion-trap hybrid instruments

        • 4.3 Time- of- flight instruments

          • MS•MS in a time-of-flight instrument

        • 4.4 Quadrupole – time- of- flight hybrid instruments

        • 4.5 Ion- trap – time- of- flight hybrid instruments

        • 4.6 Fourier- transform ion- cyclotron resonance instruments

          • MS•MSn in an FT-ICR-MS instrument

        • 4.7 Sector and related hybrid instruments

      • 5. References

  • TECHNOLOGY

    • Chapter 3 STRATEGIES IN LC•MS INTERFACING

      • 1. Introduction

      • 2. History of LC – MS

        • Objectives in LC – MS research

        • Off- line or on- line LC – MS

        • General problems in LC – MS coupling

        • 2.1 The start

        • 2.2 Exploration of other strategies

        • 2.3 The breakthrough: commercial LC – MS interfaces

        • 2.4 Further explorations

      • 3. Strategies in LC – MS interfacing

        • 3.1 Introduction of 1 ml/ min of an aqueous solvent

        • 3.2 Analyte enrichment in interfacing

        • 3.3 Solvent- based ionization strategies

      • 4. Conclusion

      • 5. References

    • Chapter 4 HISTORY OF LC•MS INTERFACES

      • 1. Introduction

      • 2. Capillary inlet

      • 3. Pneumatic nebulizer interfaces

      • 4. Moving- belt interface

      • 5. Direct liquid introduction

      • 6. Continuous- flow fast- atom bombardment

      • 7. Thermospray interface

        • Instrumentation

        • Analyte ionization

        • Operation and optimization

        • Selected applications

        • Environmental applications

        • Pharmaceutical applications

        • Biochemical applications

      • 8. Particle- beam interface

        • Instrumentation

        • Analyte ionization

        • Operation and optimization

        • Selected applications

        • Environmental applications

        • Food safety analysis

        • Vitamin analysis

        • Perspectives

      • 9. References

    • Chapter 5 INTERFACES FOR ATMOSPHERIC-PRESSURE IONIZATION

      • 1. Introduction

      • 2. Vacuum systems for mass spectrometry

      • 3. History of atmospheric- pressure ion sources

        • 3.1 Fenn electrospray molecular- beam source

        • 3.2 Bruins- Sciex ionspray source

        • 3.3 Smith electrospray CE – MS source

        • 3.4 Chait electrospray source

        • 3.5 Hewlett- Packard orthogonal- sprayer source

      • 4. Commercial atmospheric- pressure ion sources

        • 4.1 Sample introduction devices

        • 4.2 Application of heat in the API source

        • 4.3 Ion- sampling apertures

        • 4.4 Transition- region fragmentation: In- source CID

        • 4.5 Ion optical devices

      • 5. Electrospray liquid introduction devices

        • 5.1 History

        • 5.2 High flow- rate interfaces

        • 5.3 Multichannel electrospray inlets

        • 5.4 Low flow- rate interfaces

        • 5.5 Nano- electrospray needles

        • 5.6 Microfabricated microfluidic and chip- based electrospray devices

      • 6. APCI liquid introduction devices

        • 6.1 History

        • 6.2 Nebulizers for APCI

      • 7. Other atmospheric- pressure introduction devices

        • 7.1 Sonic- spray interface

        • 7.2 Laser spray interface

        • 7.3 Atmospheric- pressure photoionization

        • 7.4 Combined electrospray – APCI source

        • 7.5 Surface- enhanced APCI

      • 8. API sources for other types of mass analysers

        • 8.1 Quadrupole ion- trap instruments

        • 8.2 Time- of- flight instruments

        • 8.3 Fourier- transform ion- cyclotron resonance instruments

          • FT- ICR- MS with an external electrospray ion source

          • FT- ICR- MS with an in- field electrospray ion source

        • 8.4 Magnetic sector instruments

      • 9. Laser- induced ionization in LC – MS

        • Pulsed sample introduction to time- of- flight MS

        • Continuous- flow MALDI for LC – MS

        • Aerosol MALDI for LC – MS

        • Off- line LC – MALDI – MS

        • Atmospheric- pressure matrix- assisted laser desorption ionization

        • Atmospheric- pressure laser ionization

      • 10. References

    • Chapter 6 ATMOSPHERIC-PRESSURE IONIZATION

      • 1. Introduction

      • 2. History of electrospray ionization

        • 2.1 First experiments of Dole

        • 2.2 Electrohydrodynamic ionization

        • 2.3 Ion evaporation experiments of Iribarne and Thomson

        • 2.4 Thermospray ionization

        • 2.5 Soft desolvation or charge residue model

      • 3. Electrospray ionization

        • 3.1 Overview

        • 3.2 Electrospray nebulization

        • 3.3 Electrochemical processes

        • 3.4 Analyte concentration and properties

        • 3.5 Wrong- way- around electrospray

      • 4. Atmospheric- pressure chemical ionization

        • 4.1 Ionization by a corona discharge

        • 4.2 Solvent- mediated ( atmospheric- pressure) chemical ionization

          • Positive- ion mode

          • Some general considerations

          • Negative- ion mode

        • 4.3 Electron- capture negative ionization APCI

      • 5. Atmospheric- pressure photoionization

      • 6. LC – MS by means of ESI and APCI

        • 6.1 Hardware issues

        • 6.2 Flow- rate

        • 6.3 Mobile- phase composition

          • Solvent selection

          • Buffers

          • Ion- pairing agents

          • Other additives

          • Solving mobile- phase incompatibilities

      • 7. Matrix effects in LC – MS

        • 7.1 Remove matrix constituents

        • 7.2 Eliminate effects on accuracy and/ or precision

      • 8. References

  • APPLICATIONS: SMALL MOLECULES

    • Chapter 7 LC•MS ANALYSIS OF PESTICIDES

      • 1. Introduction

      • 2. Mass spectrometry of pesticides and herbicides

        • 2.1 Carbamates

        • 2.2 Organophosphorous pesticides

        • 2.3 Triazines

        • 2.4 Phenylureas

        • 2.5 Halogenated phenoxy acids

        • 2.6 Sulfonylureas

        • 2.7 Quaternary ammonium herbicides

        • 2.8 Miscellaneous pesticide classes

      • 3. Strategies in environmental analysis

        • 3.1 General considerations

        • 3.2 Sample pretreatment strategies

          • Liquid- liquid extraction

          • Off- line solid- phase extraction

          • On- line solid- phase extraction

          • Immunoaffinity- based pretreatment

      • 4. Environmental target compound analysis

        • 4.1 Quaternary ammonium herbicides as target compounds

        • 4.2 Confirmation of identity

      • 5. Environmental multiresidue screening

        • 5.1 Multiresidue target analysis

        • 5.2 General contaminant screening

      • 6. Pesticide degradation and metabolism

        • 6.1 Chlorophenols and nitrophenols

        • 6.2 Pesticide degradation products

        • 6.3 Ionic chloracetanilide metabolites

      • 7. Pesticide residues in fruit and vegetables

      • 8. Biological monitoring of pesticide exposure

      • 9. References

    • Chapter 8 ENVIRONMENTAL APPLICATIONS OF LC•MS

      • 1. Introduction

      • 2. Natural organic matter

      • 3. Endocrine disrupting compounds

        • 3.1 Steroids

      • 4. Surfactants

        • 4.1 Anionic surfactants

        • 4.2 Nonionic surfactants

      • 5. Pharmaceuticals

      • 6. Haloacetic acids

      • 7. Aromatic sulfonates

      • 8. References

    • Chapter 9 LC•MS IN DRUG DISCOVERYAND DEVELOPMENT

      • 1. Introduction

      • 2. Open- access LC – MS for synthetic chemists

      • 3. Characterization of combinatorial libraries

      • 4. LC – MS in high- throughput bioactivity screening

      • 5. Screening and identification of drug impurities

        • 5.1 General issues in impurity profiling

        • 5.2 Identification of reaction byproducts

        • 5.3 Degradation products in drug substances

        • 5.4 MS- directed fractionation in preparative LC

      • 6. References

    • Chapter 10 LC•MS IN DRUG METABOLISM STUDIES

      • 1. Introduction

      • 2. General considerations

        • 2.1 Phase- I metabolism

        • 2.2 Phase- II metabolism

        • 2.3 General approach in metabolite identification

      • 3. Identification of Phase- I metabolites

        • 3.1 Prediction of metabolites

        • 3.2 Radioactive labelling and detection

        • 3.3 Metabolite identification from mass shifts

        • 3.4 Importance of LC separation

      • 4. Tools in metabolite identification

        • 4.1 MS – MS instrumentation: Triple quadrupole and ion trap

        • 4.2 Precursor- ion and neutral- loss analysis modes

        • 4.3 MS – MS instrumentation: Quadrupole – time- of- flight hybrid

        • 4.4 Data- dependent acquisition

        • 4.5 MS – MS instrumentation: Quadrupole – linear- ion- trap hybrid

        • 4.6 Multi- instrument strategies in metabolite identification

        • 4.7 Combined LC – MS and LC – NMR

        • 4.8 Hydrogen/ deuterium exchange

        • 4.9 Stable- isotope labelling and isotope cluster technique

        • 4.10 Element- specific metabolite detection by LC – ICP- MS

      • 5. Identification of Phase- II metabolites

        • 5.1 LC – MS( – MS) of conjugated metabolites

        • 5.2 Neutral- loss and precursor- ion analysis

      • 6. Additional topics in metabolism studies

        • 6.1 Metabolic stability screening

        • 6.2 Membrane permeability in Caco- 2 cell monolayers

        • 6.3 Drug- drug interaction via cytochrome P450 inhibition screening

      • 7. References

    • Chapter 11 QUANTITATIVE BIOANALYSIS USING LC•MS

      • 1. Introduction

      • 2. General considerations

      • 3. Method development

        • 3.1 Sample pretreatment

        • 3.2 Chromatography

        • 3.3 Choice between ESI and APCI

        • 3.4 Internal standard

        • 3.5 Mass spectrometry

      • 4. Selected applications

        • 4.1 Reserpine

        • 4.2 Risperidone

        • 4.3 Cholesterol- reducing drugs

        • 4.4 Methylphenidate

        • 4.5 Loratadine

      • 5. Matrix effects

        • 5.1 Understanding matrix effects

        • 5.2 Quantitative description of matrix effects

        • 5.3 Reduction or elimination of matrix effects

        • 5.4 Other issues related to matrix effects

        • 5.5 Matrix effects in other application areas

      • 6. Sample pretreatment

        • 6.1 Sample filtration

        • 6.2 Protein precipitation

        • 6.3 Liquid- liquid extraction

        • 6.4 Solid- phase extraction

        • 6.5 Alternative SPE- related procedures

        • 6.6 Do we need sample pretreatment?

      • 7. Liquid chromatography

        • 7.1 Do we need LC separation?

        • 7.2 Monolithic columns

        • 7.3 Hydrophilic interaction chromatography

        • 7.4 Chiral separations

      • 8. Increasing sample throughput

      • 9. References

    • Chapter 12 CLINICAL APPLICATIONS OF LC•MS

      • 1. Introduction

      • 2. Therapeutic drug monitoring

        • 2.1 Immunosuppressive drugs

        • 2.2 TDM of HIV protease inhibitors

        • 2.3 Nucleoside reverse transcriptase inhibitors

        • 2.4 Non- nucleoside reverse transcriptase inhibitors

      • 3. Neonatal screening for inherited metabolic disorders

        • 3.1 Acylcarnitines

        • 3.2 Amino acids

      • 4. Analysis of drugs of abuse Chapter

        • 4.1 Amphetamines

        • 4.2 Lysergic acid diethylamide ( LSD)

        • 4.3 Morphine and its glucuronides

        • 4.4 Cocaine and its metabolites

        • 4.5 Multiresidue methods

      • 5. Systematic toxicological analysis

      • 6. References

    • Chapter 13 LC•MS ANALYSIS OF STEROIDS

      • 1. Introduction

      • 2. Mass spectrometry of steroids and steroid conjugates

        • 2.1 History

        • 2.2 Electrospray and APCI of steroids

        • 2.3 Steroid derivatization

        • 2.4 ESI and APCI of steroid conjugates

        • 2.5 Fragmentation of steroids in MS – MS

      • 3. Doping analysis in sports

        • 3.1 Racing horses

        • 3.2 Human athletes

      • 4. Clinical studies

        • 4.1 Breast and prostate cancer

        • 4.2 Neurosteroids

      • 5. Development of steroid drugs

      • 6. References

    • Chapter 14 LC•MS IN FOOD SAFETY ANALYSIS

      • 1. Introduction

      • 2. Mass spectrometry of antibiotics

        • 2.1 Sulfonamides

        • 2.2 ( Fluoro) quinolones

        • 2.3 Tetracyclines

        • 2.4 Betalactam antibiotics

        • 2.5 Aminoglycosides

        • 2.6 Macrolide antibiotics

        • 2.7 Chloramphenicol

      • 3. Residue analysis of antibiotics

        • 3.1 Sulfonamides

        • 3.2 ( Fluoro) quinolone antibiotics

        • 3.3 Tetracyclines

        • 3.4 Betalactam antibiotics

        • 3.5 Aminoglycosides

        • 3.6 Macrolides

        • 3.7 Chloramphenicol

      • 4. Residue analysis of steroids

      • 5. Heterocyclic aromatic amines

      • 6. Toxins

        • 6.1 Trichothecene mycotoxins

        • 6.2 Other mycotoxins

        • 6.3 Marine biotoxins

      • 7. References

    • Chapter 15 LC•MS ANALYSIS OF PLANT PHENOLS

      • 1. Introduction

      • 2. Mass spectrometry of flavonoids

        • 2.1 General structure

        • 2.2 LC – MS analysis

        • 2.3 Information in mass spectra

        • 2.4 Aglycone fragmentation in positive- ion MS – MS

        • 2.5 Aglycone fragmentation in negative- ion MS – MS

        • 2.6 Fragmentation of flavonoid glycosides

        • 2.7 Acetylated flavonoid glycosides

        • 2.8 LC – NMR in structure elucidation of flavonoids

      • 3. LC – MS analysis of flavonoids in plant material

        • 3.1 Flavonoids in plant materials

        • 3.2 Flavonoids in medicinal plants

      • 4. LC – MS analysis of flavonoids in food products

        • 4.1 Flavonoid profiling

        • 4.2 Flavonoids and isoflavones in soybean products

        • 4.3 Flavonoids and catechins in tea

      • 5. LC – MS analysis of flavonoids in body fluids

        • 5.1 Flavonoids in human body fluids

        • 5.2 Phytoestrogenic activity of flavonoids

      • 6. Anthocyanidins and related compounds

      • 7. Related plant phenolic compounds

      • 8. References

  • APPLICATIONS: BIOMOLECULES

    • Chapter 16 LC•MS ANALYSIS OF PROTEINS

      • 1. Introduction

      • 2. Electrospray ionization of peptides and proteins

        • 2.1 History

        • 2.2 Molecular- weight determination

        • 2.3 Ionization mechanism and charge- state distribution

      • 3. LC – MS of intact proteins

        • 3.1 Direct infusion experiments

        • 3.2 Reversed- phase LC – MS of proteins

        • 3.3 Other LC modes in LC – MS of proteins

        • 3.4 Selected applications

      • 4. Characterization of proteins

      • 5. Protein conformation

      • 6. Conclusions and perspectives

      • 7. References

    • Chapter 17 LC•MS ANALYSIS OF PEPTIDES ENABLING TECHNOLOGIES

      • 1. Introduction

      • 2. Nanoelectrospray

      • 3. Proteins from gel electrophoresis

      • 4. Sample pretreatment

        • 4.1 Selective enrichment of proteins

        • 4.2 Desalting and solvent switching

        • 4.3 Derivatization

        • 4.4 Enzymatic digestion

      • 5. Liquid- phase separations

        • 5.1 Reversed- phase LC – MS of peptides

        • 5.2 Nano- LC

        • 5.3 Reducing analysis time in LC

        • 5.4 Multidimensional LC

        • 5.5 Microfluidic chips

        • 5.6 Capillary electrophoresis – MS

      • 6. Identification of peptides and proteins

        • 6.1 Fragmentation of peptides

        • 6.2 Database searching

        • 6.3 De novo sequencing

      • 7. Mass spectrometry

        • 7.1 Mass analysers

        • 7.2 Data- dependent acquisition

        • 7.3 Fourier- transform ion- cyclotron resonance MS

      • 8. Conclusions and perspectives

      • 9. References

    • Chapter 18 LC•MS IN PROTEOMICS

      • 1. Introduction

      • 2. Proteomics, a concise overview

        • 2.1 Peptide mass fingerprinting

        • 2.2 Peptide sequence analysis

        • 2.3 Accurate- mass, affinity, or sequence tags

      • 3. Mining the proteome

        • 3.1 Bottom- up protein identification

        • 3.2 Shotgun protein identification: on- line LC × LC – MS

        • 3.3 Shotgun protein identification: off- line prefractionation

        • 3.4 Shotgun protein identification: FT- ICR- MS

        • 3.5 Top- down protein identification

        • 3.6 Identification of membrane proteins

      • 4. Protein- expression profiling

        • 4.1 Labelling of proteins: ICAT

        • 4.2 Labelling of proteins or peptides: Alternative methods

        • 4.3 Isolation of labelled peptides

        • 4.4 Targeted quantitative analysis

      • 5. Protein- protein interactions

      • 6. Biomarker discovery

      • 7. References

    • Chapter 19 LC•MS FOR IDENTIFICATION OF POST-TRANSLATIONAL MODIFICATIONS

      • 1. Introduction

      • 2. General considerations

      • 3. Protein phosphorylation

        • 3.1 MS screening for phosphopeptides

        • 3.2 Liquid- phase selection of phosphopeptides

        • 3.3 Derivatization and labelling of phosphopeptides

        • 3.4 Selected applications

      • 4. Protein glycosylation

        • 4.1 Glycoprotein detection using diagnostic oxonium ions

        • 4.2 Glycoprotein characterization

        • 4.3 Towards glycomics

      • 5. References

    • Chapter 20 LC•MS ANALYSIS OF OLIGOSACCHARIDES

      • 1. Introduction

      • 2 Structure of oligosaccharides

      • 3. Mass spectrometry of oligosaccharides

        • 3.1 Electrospray ionization of oligosaccharides

        • 3.2 MS – MS of oligosaccharides

        • 3.3 Multistage MS – MS using ion- trap instruments

        • 3.4 Structural characterization of oligosaccharides

        • 3.5 Derivatization of oligosaccharides

      • 4. LC – MS analysis of oligosaccharides

        • 4.1 High- performance anion- exchange chromatography

        • 4.2 Reversed- phase chromatography

        • 4.3 Other modes of chromatography

      • 5. Conclusion and perspectives

      • 6. References

    • Chapter 21 LC•MS ANALYSIS OF LIPIDS AND PHOSPHOLIPIDS

      • 1. Introduction

      • 2. Fatty acid analysis

      • 3. Triacylglycerols

        • 3.1 Chromatographic separation

        • 3.2 Characterization by MS – MS

        • 3.3 Quantitative analysis

        • 3.4 Selected applications

      • 4. Metabolites of arachidonic acid

        • 4.1 Hydroxyeicosatetraenoic acids

        • 4.2 Prostaglandins

      • 5. Phospholipids

        • 5.1 Sphingomyelins

        • 5.2 Chromatography of glycerophospholipids

        • 5.3 Characterization by MS – MS of glycerophospholipids

        • 5.4 Lipidomics

      • 6. References

    • Chapter 22 LC•MS ANALYSIS OF NUCLEIC ACIDS

      • 1. Introduction

        • 1.1 Nucleosides and nucleotides

        • 1.2 Oligonucleotides

      • 2. General considerations

        • 2.1 LC analysis of nucleosides and nucleotides

        • 2.2 ESI- MS of nucleosides and nucleotides

        • 2.3 LC analysis of oligonucleotides

        • 2.4 Desalting sample pretreatment strategies

        • 2.5 ESI- MS of oligonucleotides

        • 2.6 Fragmentation by MS – MS

      • 3. Selected applications on oligonucleotides

        • 3.1 Quality control of synthetic oligonucleotides

        • 3.2 Antisense oligonucleotides

        • 3.3 Polymerase chain reaction products

        • 3.4 Single nucleotide polymorphism

      • 4. LC – MS analysis of modified nucleosides

        • 4.1 Urinary analysis of oxidized nucleobases

      • 5. LC – MS analysis of DNA adducts

      • 6. References

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