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Cấu trúc
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
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
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
Chapter 4 HISTORY OF LC•MS INTERFACES
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
Food safety analysis
Vitamin analysis
Perspectives
9. References
Chapter 5 INTERFACES FOR ATMOSPHERIC-PRESSURE IONIZATION
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
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
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
Chapter 8 ENVIRONMENTAL APPLICATIONS OF LC•MS
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
Chapter 9 LC•MS IN DRUG DISCOVERYAND DEVELOPMENT
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
Chapter 10 LC•MS IN DRUG METABOLISM STUDIES
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
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
Chapter 12 CLINICAL APPLICATIONS OF LC•MS
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
Chapter 13 LC•MS ANALYSIS OF STEROIDS
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
Chapter 14 LC•MS IN FOOD SAFETY ANALYSIS
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
Chapter 15 LC•MS ANALYSIS OF PLANT PHENOLS
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
APPLICATIONS: BIOMOLECULES
Chapter 16 LC•MS ANALYSIS OF PROTEINS
2. Electrospray ionization of peptides and proteins
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
Chapter 17 LC•MS ANALYSIS OF PEPTIDES ENABLING TECHNOLOGIES
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
Chapter 18 LC•MS IN PROTEOMICS
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
Chapter 19 LC•MS FOR IDENTIFICATION OF POST-TRANSLATIONAL MODIFICATIONS
3. Protein phosphorylation
3.1 MS screening for phosphopeptides
3.2 Liquid- phase selection of phosphopeptides
3.3 Derivatization and labelling of phosphopeptides
4. Protein glycosylation
4.1 Glycoprotein detection using diagnostic oxonium ions
4.2 Glycoprotein characterization
4.3 Towards glycomics
Chapter 20 LC•MS ANALYSIS OF OLIGOSACCHARIDES
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
Chapter 21 LC•MS ANALYSIS OF LIPIDS AND PHOSPHOLIPIDS
2. Fatty acid analysis
3. Triacylglycerols
3.1 Chromatographic separation
3.2 Characterization by MS – MS
3.3 Quantitative analysis
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
Chapter 22 LC•MS ANALYSIS OF NUCLEIC ACIDS
1.1 Nucleosides and nucleotides
1.2 Oligonucleotides
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
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