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77.19 €
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HPLC: A practical user's guide (2nd Ed.)
Auteur(s) : MCMASTER Marvin C. Date de parution: 01-2007 Langue : ANGLAIS 238p. 16x24 Hardback
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| Résumé | | A common method of chemical analysis, modern high-performance (or high-pressure) liquid chromatography (HPLC) has many applications, most notably in the pharmaceutical industry, where it is often coupled with mass spectrometry for definitive identification of compounds. HPLC: A Practical User's Guide, Second Edition is the perfect companion for the novice chromatographer who needs to keep an HPLC system up and running, and to get the most out of the bewildering variety of column types available for making separations. This new edition brings the guide up to date with information on important advances, while maintaining the proven techniques and writing that made the first edition a useful teaching tool and reference. |
| Sommaire | | PREFACE. I HPLC PRIMER. 1 Advantages and Disadvantages of HPLC. 1.1 How It Works. 1.1.1 A Separation Model of the Column. 1.1.2 Basic Hardware: A Quick, First Look. 1.1.3 Use of Solvent Gradients. 1.1.4 Ranges of Compounds. 1.2 Other Ways to Make My Separation. 1.2.1 FPLCFast Protein Liquid Chromatography. 1.2.2 LCTraditional Liquid Chromatography. 1.2.3 GLCGas Liquid Chromatography. 1.2.4 SFCSupercritical Fluid Chromatography. 1.2.5 TLCThin Layer Chromatography. 1.2.6 EPElectrophoresis. 1.2.7 CZECapillary Zone Electrophoresis. 2 Selecting an HPLC System. 2.1 Characteristic Systems. 2.1.1 Finding a Fit: Detectors and Data Processing. 2.1.2 System Models: Gradient Versus Isocratic. 2.1.3 Vendor Selection. 2.1.4 Brand Names and Clones. 2.1.5 HardwareSupport. 2.2 System Cost Estimates. 2.2.1 Type I System15,000). 2.2.2 Type II System25,000). 2.2.3 Type III System35,000). 2.2.4 Type IV System50,000). 2.3 Columns. 2.3.1 Sizes: Analytical and Preparative. 2.3.2 Separating Modes: Selecting Only What You Need. 2.3.3 Tips on Column Use. 3 Running Your Chromatograph. 3.1 Set-up and Start-up. 3.1.1 Hardware Plumbing 101: Tubing and Fittings. 3.1.2 Connecting Components. 3.1.3 Solvent Clean-up. 3.1.4 Water Purity Test. 3.1.5 Start-up System Flushing. 3.1.6 Column Preparation and Equilibration. 3.2 Sample Preparation and Column Calibration. 3.2.1 Sample Clean-up. 3.2.2 Plate Counts. 3.3 Your First Chromatogram. 3.3.1 Reproducible Injection Techniques. 3.3.2 Simple Scouting for a Mobile Phase. 3.3.3 Examining the Chromatogram. 3.3.4 Basic Calculations of Results. II HPLC OPTIMIZATION. 4 Separation Models. 4.1 Partition. 4.1.1 Separation Parameters. 4.1.2 Efficiency Factor. 4.1.3 Separation (Chemistry) Factor. 4.2 Ion Exchange Chromatography. 4.3 Size Exclusion Chromatography. 4.4 Affinity Chromatography. 5 Column Preparation. 5.1 Column Variations. 5.2 Packing Materials and Hardware. 5.3 Column Selection. 6 Column Aging, Diagnosis, and Healing. 6.1 Packing DegradingBonded-Phase Loss. 6.2 Dissolved Packing MaterialEnd Voids. 6.3 Bound Material. 6.4 Pressure Increases. 6.5 Column ChannelingCenter-Voids. 6.6 Normal Phase, Ion Exchange, and Size Columns. 6.7 Zirconium and Polymer Columns. 7 Partition Chromatography Modifications. 7.1 Reverse-Phase and Hybrid Silica. 7.1.1 Ionization Suppression. 7.1.2 Ion Pairing. 7.1.3 Organic Modifiers. 7.1.4 Chelation. 7.2 Acidic Phase Silica. 7.3 Reverse-Phase Zirconium. 7.4 Partition Mode Selection. 8 Chromatography. 8.1 Ion Exchange. 8.1.1 Cationic:Weak and Strong. 8.1.2 Anionic:Weak and Strong. 8.2 Size Exclusion. 8.2.1 Organic Soluble Samples. 8.2.2 Hydrophilic Protein Separation. 8.3 Affinity Chromatography. 8.3.1 Column Packing Modification. 8.3.2 Chelation and Optically Active Columns. 9 Hardware Specifics. 9.1 System Protection. 9.1.1 Filters, Guard Columns, and Saturation Columns. 9.1.2 Inert Surfaces and Connections. 9.2 Pumping. 9.2.1 High- and Low-Pressure Mixing Controllers. 9.2.2 Checking Gradient Performance. 9.3 Injectors and Autosamplers. 9.4 Detectors. 9.4.1 Mass Dependent Detectors. 9.4.2 Absorptive Detectors. 9.4.3 Specific Detectors. 9.5 Fraction Collectors. 9.6 Data Collection and Processing. 10 Troubleshooting and Optimization. 10.1 Hardware and ToolsSystem Pacification. 10.2 Reverse Order Diagnosis. 10.3 Introduction to Data Acquisition. 10.4 Solvent Conservation. III HPLC UTILIZATION. 11 Preparative Chromatography. 11.1 Analytical Preparative. 11.2 Semipreparative. 11.3 Preparative. 12 Sample Preparation and Methods Development. 12.1 Sample Preparation. 12.1.1 Deproteination. 12.1.2 Extraction and Concentration. 12.1.3 SFE (Cartridge Column) Preparations. 12.1.4 Extracting Encapsulated Compounds. 12.1.5 SFE Trace Enrichment and Windowing. 12.1.6 Derivatives. 12.2 Methods Development. 12.2.1 Standards Development. 12.2.2 Samples Development. 12.3 Gradient Development. 13 Application Logics: Separations Overview. 13.1 Fat-Soluble Vitamins, Steroid, and Lipids. 13.2 Water-Soluble Vitamins, Carbohydrates, and Acids. 13.3 Nucleomics. 13.4 Proteomics. 13.5 Clinical and Forensic Drug Monitoring. 13.6 Pharmaceutical Drug Development. 13.7 Environmental and Reaction Monitoring. 13.8 Application Trends. 14 Automation. 14.1 Analog-to-Digital Interfacing. 14.2 Digital Information Exchange. 14.3 HPLC System Control and Automation. 14.4 Data Collection and Interpretation. 14.4.1 Preinjection Baseline Setting. 14.4.2 Peak Detection and Integration. 14.4.3 Quantitation: Internal/External Standards. 14.5 Automated Methods Development. 14.5.1 Automated Isocratic Development. 14.5.2 Hinge Point Gradient Development. 14.6 Data Exportation to the Real World. 14.6.1 Word Processors: .ASC, .DOC, .RTF, .WS, .WP Formats. 14.6.2 Spread Sheets: .DIF, .WK, .XLS Formats. 14.6.3 Databases: .DB2 Format. 14.6.4 Graphics: .PCX, .TIFF, .JPG Formats. 14.6.5 Chromatographic Files: Metafiles and NetCDF. 15 Recent Advances in LC/MS Separations. 15.1 A LC/MS Primer. 15.1.1 Quadrupole MS and Mass Selection. 15.1.2 Other Types of MS Analyzers for LC/MS. 15.1.3 LC/MS Interfaces. 15.1.4 LC/MS Computer Control and Data Processing. 15.2 Microflow Chromatography. 15.3 Ultrafast HPLC Systems. 15.4 Chip HPLC Systems. 15.5 Standardized LC/MS in Drug Design. 16 New Directions in HPLC. 16.1 Temperature-Controlled Chromatography. 16.2 Ultrafast Chromatography. 16.3 Monolith Capillary Columns. 16.4 Micro-Parallel HPLC Systems. 16.5 Two-Dimensional HPLC Systems. 16.6 The Portable LC/MS. APPENDICES. APPENDIX A Personal Separations Guide. APPENDIX B FAQs for HPLC Systems and Columns. APPENDIX C Tables of Solvents and Volatile Buffers. APPENDIX D Glossary of HPLC Terms. APPENDIX E HPLC Troubleshooting Quick Reference. APPENDIX F HPLC Laboratory Experiments. Laboratory 1System Start-up and Column Quality Control. Laboratory 2Sample Preparation and Methods Development. Laboratory 3Column and Solvent Switching and Pacification. Appendix G Selected Reference List. INDEX. |
Thèmes :
- Chimie - industries chimiques / Chimie analytique / Chromatographie
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