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Ultra-High Performance Liquid Chromatography and Its Applications.

This is the first resource to fully cover the instrumentation, method development, and applications of Ultra-High Performance Liquid Chromatography (U-HPLC). It details both the benefits and limitations of this method in the pharmaceutical industry, clinical research, the food industry, and environm...

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Detalles Bibliográficos
Clasificación:Libro Electrónico
Autor principal: Xu, Q. Alan
Formato: Electrónico eBook
Idioma:Inglés
Publicado: Chicester : Wiley, 2013.
Temas:
Acceso en línea:Texto completo
Tabla de Contenidos:
  • Ultra-High Performance Liquid Chromatography and Its Applications
  • Contents
  • Preface
  • Contributors
  • Chapter 1 UHPLC Method Development
  • 1.1 INTRODUCTION
  • 1.2 METHOD DEVELOPMENT
  • 1.2.1 Gather Sample Information and Define Method Goals
  • 1.2.2 Scout Columns and Mobile Phases
  • 1.2.3 Analyze Scouting Results and Select Separation Conditions
  • 1.2.4 Optimize the Method
  • 1.2.5 Validate the Method
  • 1.2.6 Phase-Appropriate Method Development
  • 1.2.7 Very High Pressure and Frictional Heating in UHPLC
  • 1.2.8 Relevance of Various Instrumentation to Method Development
  • 1.2.9 Method Resolution and Speed Requirements
  • 1.2.10 Example 1.1
  • 1.2.11 Example 1.2
  • 1.3 CONVERSION OF AN HPLC METHOD TO UHPLC
  • 1.3.1 Select a UHPLC Column with the Same Chemistry
  • 1.3.2 Measure Dwell Volumes of HPLC and UHPLC Systems
  • 1.3.3 Calculate Injection Volume, Flow Rate, Holding Time, and Gradient Segment Time
  • 1.3.4 Perform Verification Experiment
  • 1.3.5 Validate the Method
  • 1.3.6 Example 1.3
  • 1.3.7 Example 1.4
  • 1.4 CONVERSION OF A UHPLC METHOD TO HPLC
  • 1.5 SUMMARY
  • REFERENCES
  • Chapter 2 Method Transfer Between HPLC and UHPLC Platforms
  • 2.1 INTRODUCTION
  • 2.2 TRANSFERRING HPLC METHODS TO UHPLC
  • 2.2.1 Fundamental Physical Relationships
  • 2.2.2 Types of UHPLC Applications
  • 2.2.3 Additional Fundamental Considerations
  • 2.2.4 Transfer of Isocratic Methods from HPLC to UHPLC
  • 2.2.5 Cautions on Transferring Isocratic Methods from HPLC to UHPLC
  • 2.2.6 Transfer of Gradient Methods from HPLC to UHPLC
  • 2.2.7 Cautions on the Scaling of Gradient Methods from HPLC to UHPLC
  • 2.2.8 Case Studies and Recommendations
  • 2.2.9 Final Discussion of Practical Challenges
  • 2.2.10 Conclusions on the Transfer of Methods from HPLC to UHPLC
  • 2.3 TRANSFERRING UHPLC METHODS TO HPLC PLATFORMS
  • 2.3.1 UHPLC to Traditional HPLC Columns.
  • 2.3.2 UHPLC to Superficially Porous Particle HPLC Columns
  • 2.3.3 UHPLC to HPLC Method Transfer
  • 2.4 TRANSFERRING LC METHODS TO OTHER LABS
  • 2.4.1 UHPLC Instrument Issues Encountered During Method Transfers
  • 2.4.2 Back to LC Basics
  • REFERENCES
  • Chapter 3 Practical Aspects of Ultrahigh Performance Liquid Chromatography
  • 3.1 INTRODUCTION
  • 3.2 EFFECT OF EXTRA-COLUMN VOLUME ON PERFORMANCE OF SUB-2 lM PARTICLE-PACKED COLUMNS IN UHPLC
  • 3.2.1 Theoretical Considerations
  • 3.2.2 Extra-Column Volumes and Column Volumes
  • 3.2.3 Effect of Extra-Column Volume on Performance
  • 3.3 COLUMN PRESSURE AND FRICTIONAL HEATING
  • 3.3.1 Column Pressure vs. Particle Size
  • 3.3.2 Phenomenon of Frictional Heating
  • 3.3.3 Effect of Frictional Heating on Retention Factor
  • 3.3.4 Factors Leading to Frictional Heating
  • 3.3.5 How to Resolve Thermal Gradient Issues
  • 3.3.6 Effect of Pressure on Mobile Phase Characteristics
  • 3.3.7 Effect of Pressure on Retention Factor with Minimal Frictional Heating
  • 3.4 METHOD TRANSFER BETWEEN UHPLC AND HPLC AND OTHER TIPS
  • 3.4.1 Column Dimension and Particle Size
  • 3.4.2 Column Chemistry and Mobile Phase
  • 3.4.3 Flow Rate and Gradient Profile
  • 3.4.4 Injection Volume
  • 3.4.5 Dwell Volume
  • 3.4.6 UV Detection
  • 3.4.7 Other Tips
  • 3.5 CONCLUDING REMARKS
  • REFERENCES
  • Chapter 4 Coupling UHPLC with MS: The Needs, Challenges, and Applications
  • 4.1 INTRODUCTION
  • 4.2 TECHNICAL REQUIREMENTS FOR THE COUPLING OF UHPLC WITH MS
  • 4.2.1 Mobile Phase Flow Rate Compatibility
  • 4.2.2 Acquisition Rate and Data Quality
  • 4.2.3 Band-Broadening in UHPLC-MS Conditions
  • 4.3 UHPLC-MS FOR BIOANALYTICAL ASSAYS
  • 4.3.1 Selectivity Issues and Matrix Effects
  • 4.3.2 Time Delivery Constraints
  • 4.4 DRUG METABOLISM STUDIES USING UHPLC-MS
  • 4.4.1 High-Throughput Metabolite Assays.
  • 4.4.2 High-Resolution Metabolite Identification
  • 4.5 MULTI-ANALYTE SCREENING WITH UHPLC-MS
  • 4.5.1 Sample Preparation Procedures
  • 4.5.2 UHPLC Conditions
  • 4.5.3 Triple Quadrupole vs. Time-of-Flight Analyzers
  • 4.6 UHPLC-MS IN METABOLOMICS
  • 4.6.1 UHPLC-MS for Metabolomics in Human and Animal Tissues
  • 4.6.2 UHPLC-MS for Metabolomics in Plant Extracts
  • 4.7 ANALYSIS OF PROTEINS WITH UHPLC-MS
  • 4.7.1 Issues and Solutions in Intact Protein Analysis
  • 4.7.2 UHPLC-MS for Intact Protein Analysis
  • 4.8 CONCLUSIONS
  • REFERENCES
  • Chapter 5 The Potential of Shell Particles in Fast Liquid Chromatography
  • 5.1 INTRODUCTION
  • 5.2 COLUMN EFFICIENCY
  • 5.3 FAST LIQUID CHROMATOGRAPHY
  • 5.3.1 Trends in Fast Liquid Chromatography
  • 5.3.2 Adjusting Conventional Methods to Fast Separations (Geometrical Method Transfer
  • 5.4 THE IMPACT OF EXTRA-COLUMN BAND-BROADENING IN FAST LIQUID CHROMATOGRAPHY
  • 5.5 SHELL PARTICLES, THE INFLUENCE OF SHELL THICKNESS
  • 5.6 THE EFFICIENCY OF COLUMNS PACKED WITH SHELL PARTICLES
  • 5.6.1 The Mass Transfer Kinetics of Shell Particles
  • 5.6.2 The Longitudinal Diffusion in Columns Packed with Shell Particles
  • 5.6.3 The Eddy Dispersion in Columns Packed with Shell Particles
  • 5.6.4 The Frictional Heating in Columns Packed with Shell Particles
  • 5.6.5 Limited Efficiency When Shell Particles Packedin Narrow-Bore Columns
  • 5.6.6 The Success of the New Generation Shell Particles
  • 5.7 FAST SEPARATIONS BY APPLYING THE NEW GENERATION OF SHELL PARTICLES
  • 5.8 APPLICATIONS OF COLUMNS PACKED WITH THE LATEST GENERATION OF SHELL PARTICLES
  • 5.8.1 Pharmaceutical and Bioanalytical Applications
  • 5.8.2 Food Analytical Applications
  • 5.8.3 Environmental Analytical Applications
  • 5.8.4 Multidimensional Separations
  • 5.9 CONCLUSION
  • REFERENCES
  • Chapter 6 UHPLC Determination of Drugs of Abuse in Human Biological Matrices.
  • 6.1 INTRODUCTION
  • 6.2 CLASSES OF DRUGS AND ILLICIT SUBSTANCES
  • 6.2.1 Amphetamines
  • 6.2.2 Benzodiazepines
  • 6.2.3 Cannabinoids
  • 6.2.4 Cocaine Alkaloids
  • 6.2.5 Designer Drugs
  • 6.2.6 Ketamine
  • 6.2.7 Lysergic Acid Diethylamide
  • 6.2.8 Opiates and Opioids
  • 6.2.9 Diuretics, b -Blockers, and Stimulants
  • 6.3 DRUG METABOLIZATION IN THE HUMAN BODY
  • 6.4 HUMAN MATRICES ANALYZED
  • 6.4.1 Whole Blood, Plasma, and Serum
  • 6.4.2 Fingerprints, Sebum, and Sweat
  • 6.4.3 Hair
  • 6.4.4 Meconium
  • 6.4.5 Oral Fluid
  • 6.4.6 Urine
  • 6.5 PRETREATMENT AND ANALYSIS
  • REFERENCES
  • Chapter 7 UHPLC in the Analyses of Isoflavones and Flavonoids
  • 7.1 INTRODUCTION
  • 7.2 UHPLC IN POLYPHENOLIC COMPOUNDS DETERMINATION
  • 7.2.1 Determination of Polyphenolic Compounds in Biological Fluids
  • 7.2.2 Determination of Polyphenolic Compounds in Foods
  • 7.2.3 Determination of Polyphenolic Compounds in Plant Extract
  • 7.3 SUMMARY
  • REFERENCES
  • Chapter 8 UHPLC for Characterization of Protein Therapeutics
  • 8.1 INTRODUCTION
  • 8.2 PROTEIN CHARACTERIZATION AND LOT RELEASE TESTING
  • 8.3 HPLC AND UHPLC
  • 8.4 REVERSED-PHASE UHPLC FOR PROTEIN ANALYSIS
  • 8.5 REVERSED-PHASE UHPLC FOR PEPTIDE MAP ANALYSIS
  • 8.6 UHPLC FOR LC-MS AND LC-MS/MS APPLICATIONS
  • 8.7 HYDROPHILIC INTERACTION CHROMATOGRAPHY (HILIC) FOR GLYCAN PROFILING
  • 8.8 HYDROPHOBIC INTERACTION CHROMATOGRAPHY FOR HYDROPHOBICITY ANALYSIS
  • 8.9 ION EXCHANGE CHROMATOGRAPHY FOR CHARGE VARIANT ANALYSIS
  • 8.10 SIZE EXCLUSION CHROMATOGRAPHY FOR SIZE HETEROGENEITY ANALYSIS
  • 8.11 CONCLUSION
  • ACKNOWLEDGMENT
  • REFERENCES
  • Chapter 9 UHPLC/MS Analysis of Illicit Drugs
  • 9.1 INTRODUCTION
  • 9.2 APPLICATIONS OF UHPLC/MS IN ILLICIT DRUG ANALYSIS
  • 9.2.1 Development of a UHPLC/MS Method for Simultaneous Identification of Multiple Drugs of Abuse.
  • 9.2.2 Quantitative Analysis of Pseudoephedrine Tablets by UHPLC/MS
  • 9.2.3 Identification of Cannabinoids in Baked Goods by UHPLC/MS
  • 9.2.4 Identification of Psychotropic Substances in Mushrooms and Chocolate by UHPLC/MS
  • 9.2.5 Identification of Lysergic Acid Diethylamide in Candy by UHPLC/MS
  • 9.3 CONCLUSIONS
  • REFERENCES
  • Chapter 10 Ultra-High Performance Liquid Chromatography
  • Mass Spectrometry and Its Application
  • 10.1 INTRODUCTION
  • 10.2 INSTRUMENTATION OF UHPLC-MS
  • 10.2.1 UHPLC System
  • 10.2.2 Mass Spectrometer
  • 10.3 UHPLC-MS APPLICATIONS
  • 10.3.1 UHPLC-MS Applications in Analysis of Traditional Chinese Medicines
  • 10.3.2 UHPLC-MS Applications in Metabonomics
  • 10.3.3 UHPLC-MS Applications in Drug Metabolism
  • 10.3.4 UHPLC-MS Applications in Pharmacokinetics
  • 10.4 CONCLUSIONS
  • REFERENCES
  • Index.