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...
Clasificación: | Libro Electrónico |
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Autor principal: | |
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.