HPLC and UHPLC for Practicing Scientists (2nd Edition)
Written for practitioners by an expert practitioner, this new edition of this book adds numerous updates to its coverage of high-performance liquid chromatography, including comprehensive information on UHPLC (ultra-high-pressure liquid chromatography) and the continuing migration of HPLC to UHPLC,...
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| Hlavní autor: | |
|---|---|
| Médium: | E-kniha Kniha |
| Jazyk: | angličtina |
| Vydáno: |
Hoboken, N.J
John Wiley & Sons
2019
Wiley John Wiley & Sons, Incorporated Wiley-Blackwell |
| Vydání: | 2 |
| Témata: | |
| ISBN: | 9781119313762, 1119313767 |
| On-line přístup: | Získat plný text |
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- Title Page Preface Table of Contents 1. Introduction 2. Basic Terms and Concepts 3. HPLC Columns and Trends 4. HPLC/UHPLC Instrumentation and Trends 5. UHPLC: Perspectives, Performance, Practices, and Potential Issues 6. LC/MS: Fundamentals, Perspectives, and Applications 7. HPLC/UHPLC Operation Guide 8. HPLC/UHPLC Maintenance and Troubleshooting 9. Pharmaceutical Analysis 10. HPLC Method Development 11. Regulations, HPLC System Qualification, Method Validation, and Transfer 12. HPLC and UHPLC for Biopharmaceutical Analysis 13. HPLC Applications in Food, Environmental, Chemical, and Life Sciences Analysis Appendix: Keys to Quizzes Index
- 7.7 Guides on Performing Trace Analysis
- 4.2 HPLC and UHPLC Solvent Delivery Systems -- 4.2.1 High‐Pressure and Low‐Pressure Mixing Designs in Multisolvent Pumps -- 4.2.2 System Dwell Volume -- 4.2.2.1 Dwell Volumes of UHPLC Systems -- 4.2.3 Trends -- 4.3 Injectors and Autosamplers -- 4.3.1 Operating Principles of Autosamplers -- 4.3.2 Performance Characteristics and Trends -- 4.4 Detectors -- 4.5 UV/VIS Absorbance Detectors -- 4.5.1 Operating Principles -- 4.5.2 Performance Characteristics -- 4.5.3 Trends in UV/Vis Absorbance Detectors -- 4.6 Photodiode Array Detectors -- 4.6.1 Operating Principles -- 4.6.2 Trends in PDA Detectors -- 4.7 Other Detectors -- 4.7.1 Refractive Index Detector (RID) -- 4.7.2 Evaporative Light Scattering Detector (ELSD) -- 4.7.3 Charged Aerosol Detector (CAD) -- 4.7.4 Conductivity Detector (CD) -- 4.7.5 Fluorescence Detector (FLD) -- 4.7.5.1 Postcolumn Reaction Technique -- 4.7.6 Chemiluminescence Nitrogen Detector (CLND) -- 4.7.7 Electrochemical Detector (ECD) -- 4.7.8 Radiometric Detector -- 4.8 Hyphenated and Specialized Systems -- 4.8.1 LC/MS and LC/MS/MS -- 4.8.2 LC/NMR -- 4.8.3 Other Hyphenated Systems -- 4.8.4 Supercritical Fluid Chromatography (SFC) -- 4.8.5 Preparative LC and SFC -- 4.8.6 Micro‐ and Nano‐LC (Capillary LC) -- 4.8.7 Multidimensional LC -- 4.8.8 Lab‐on‐a‐Chip -- 4.8.9 Specialized Applications Systems -- 4.8.9.1 Gel‐Permeation Chromatography (GPC) -- 4.8.9.2 Ion Chromatography (IC) -- 4.8.9.3 Application‐Specific Systems -- 4.9 HPLC Accessories -- 4.9.1 Solvent Degasser -- 4.9.2 Column Oven -- 4.9.3 Valves for Column and Mobile Phase Selection -- 4.10 Chromatography Data Systems (CDS) -- 4.10.1 User Interface and CDS Workflow -- 4.11 Instrumental Bandwidth (IBW) -- 4.11.1 How to Measure IBW -- 4.11.2 IBW of UHPLC Systems -- 4.12 Manufacturers and Equipment Selection -- 4.13 Trends in HPLC and UHPLC Equipment -- 4.14 Summary -- 4.15 Quizzes
- 2.7 The Concept of Orthogonality and Selectivity Tuning -- 2.8 Sample Capacity -- 2.9 Glossary of HPLC Terms -- 2.10 Summary and Conclusion -- 2.11 Quizzes -- 2.11.1 Bonus Quiz -- 2.12 References -- Chapter 3 HPLC Columns and Trends -- 3.1 Scope -- 3.1.1 Glossary and Abbreviations -- 3.2 General Column Description and Characteristics -- 3.2.1 Column Hardware - Standard vs. Cartridge Format -- 3.3 Column Type -- 3.3.1 Types Based on Chromatographic Mode -- 3.3.2 Column Types Based on Dimension -- 3.3.3 Column Length (L) -- 3.4 Column Packing Characteristics -- 3.4.1 Support Type -- 3.4.2 Particle Size (dp) -- 3.4.3 Surface Area and Pore Size (dpore) -- 3.4.4 Bonding Chemistries -- 3.5 Modern HPLC Column Trends -- 3.5.1 Silica Support Material -- 3.5.2 Hybrid Particles -- 3.5.3 Novel Bonding Chemistries -- 3.5.3.1 Bonded Phases for Retention of Polar Analytes -- 3.5.3.2 Charged Surface Hybrid (CSH) -- 3.5.4 Shorter and Narrower Columns Packed with Small Particles -- 3.5.4.1 Fast LC -- 3.5.4.2 UHPLC -- 3.5.5 Micro‐LC and Nano‐LC -- 3.5.6 Monoliths -- 3.5.7 Superficially Porous Particles (SPP) -- 3.5.7.1 Kinetic Plots Demonstrating the Superiority of SPP -- 3.5.8 Micropillar Array Chromatography (μPAC) -- 3.6 Guard Columns -- 3.7 Specialty Columns -- 3.7.1 Bioseparations Columns -- 3.7.2 Chiral Columns -- 3.7.3 Supercritical Fluid Chromatography (SFC) Columns -- 3.7.4 Hydrophilic Interaction Liquid Chromatography (HILIC) Columns -- 3.7.5 Mixed‐Mode Chromatography (MMC) Columns -- 3.7.6 Application‐Specific Columns -- 3.8 RPC Column Selection Guides -- 3.8.1 Some General Guidelines for Bonded Phase Selection -- 3.9 Summary -- 3.10 Quizzes -- 3.10.1 Bonus Quiz -- 3.11 References -- Chapter 4 HPLC/UHPLC Instrumentation and Trends -- 4.1 Introduction -- 4.1.1 Scope -- 4.1.2 HPLC Systems and Modules -- 4.1.3 Ultra‐High‐Pressure Liquid Chromatography (UHPLC)
- 4.15.1 Bonus Quiz -- 4.16 References -- Chapter 5 UHPLC: Perspectives, Performance, Practices, and Potential Issues -- 5.1 Introduction -- 5.1.1 Scope -- 5.1.2 Glossary and Abbreviations -- 5.1.3 Historical Perspectives: What is UHPLC? -- 5.2 Practical Concepts in UHPLC -- 5.2.1 Rationale for Higher System Pressure -- 5.2.2 Rationale for Low‐Dispersion Systems -- 5.2.3 Rationale for Low Dwell Volumes -- 5.2.4 Other UHPLC Instrumental Characteristics -- 5.3 Benefits Of UHPLC and Case Studies -- 5.3.1 Benefit #1: Fast Separations with Good Resolution -- 5.3.2 Benefit #2: High‐Resolution Analysis of Complex Samples -- 5.3.3 Benefit #3: Rapid HPLC Method Development -- 5.3.4 Flexibility for Customizing Resolution -- 5.3.5 Other Benefits of UHPLC -- 5.3.5.1 Solvent Saving -- 5.3.5.2 Higher Mass Sensitivity in UV Detection -- 5.3.5.3 Higher Precision Performance for Retention Time and Peak Area -- 5.3.5.4 UHPLC are Compatible with Other Approaches -- 5.4 Potential Issues and How to Mitigate -- 5.4.1 Safety Issues -- 5.4.2 Viscous Heating -- 5.4.3 Instrumental and Operating Nuances -- 5.4.4 Injector Precision -- 5.4.5 UV Detection Noise vs. Mixer Volumes -- 5.4.6 Method Translation (Conversion) -- 5.4.6.1 Running the Same HPLC Methods on HPLC and UHPLC -- 5.4.6.2 Back Conversion of UHPLC Methods to HPLC Method Conditions -- 5.4.6.3 Conversion of Existing HPLC Methods to Faster UHPLC Methods -- 5.4.6.4 Method Validation Requirements After Method Translation -- 5.5 How to Implement UHPLC and Practical Aspects -- 5.5.1 How to Transition from HPLC to UHPLC -- 5.5.2 End‐Fittings -- 5.5.3 A Summary of UHPLC System Performance Tradeoffs -- 5.6 Myths in UHPLC -- 5.7 Summary and Conclusions -- 5.8 Quizzes -- 5.8.1 Bonus Quiz -- 5.9 References -- Chapter 6 LC/MS: Fundamentals, Perspectives, and Applications -- 6.1 Introduction -- 6.1.1 Scope
- Cover -- Title Page -- Copyright -- Contents -- Author's Biography -- Biographies of Contributors -- Preface -- Foreword -- Acknowledgments -- Chapter 1 Introduction -- 1.1 Introduction -- 1.1.1 Scope -- 1.1.2 What Is HPLC? -- 1.1.3 A Brief History -- 1.1.4 Advantages and Limitations -- 1.1.5 Ultra‐High‐Pressure Liquid Chromatography (UHPLC) -- 1.2 Primary Modes of HPLC -- 1.2.1 Normal‐Phase Chromatography (NPC) -- 1.2.2 Reversed‐Phase Chromatography (RPC) -- 1.2.3 Ion‐Exchange Chromatography (IEC) -- 1.2.4 Size‐Exclusion Chromatography (SEC) -- 1.2.5 Other Separation Modes -- 1.3 Some Common‐Sense Corollaries -- 1.4 How to Get More Information -- 1.5 Summary -- 1.6 Quizzes -- 1.6.1 Bonus Quiz -- 1.7 References -- Chapter 2 Basic Terms and Concepts -- 2.1 Scope -- 2.2 Basic Terms and Concepts -- 2.2.1 Retention Time (tR), Void Time (tM), Peak Height (h), and Peak Width (wb) -- 2.2.2 Retention Volume (VR), Void Volume (VM), and Peak Volume -- 2.2.3 Retention Factor (k) -- 2.2.4 Separation Factor (α) -- 2.2.5 Column Efficiency and Plate Number (N) -- 2.2.6 Peak Volume -- 2.2.7 Height Equivalent to a Theoretical Plate or Plate Height (HETP or H) -- 2.2.8 Resolution (Rs) -- 2.2.9 Peak Symmetry: Asymmetry Factor (As) and Tailing Factor (Tf) -- 2.3 Mobile Phase -- 2.3.1 General Requirements -- 2.3.2 Solvent Strength and Selectivity -- 2.3.3 pH Modifiers and Buffers -- 2.3.4 Acidic Mobile Phases -- 2.3.5 Ion‐Pairing Reagents and Chaotropic Agents -- 2.3.6 High‐pH Mobile Phases -- 2.3.7 Other Operating Parameters: Flow Rate (F) and Column Temperature (T) -- 2.4 The Resolution Equation -- 2.5 The Van Deemter Equation -- 2.6 Isocratic vs. Gradient Analysis -- 2.6.1 Peak Capacity (n) -- 2.6.2 Gradient Parameters (Initial and Final Solvent Strength, Gradient Time (tG), and Flow Rate) -- 2.6.3 The 0.25 ΔtG Rule: When Is Isocratic Analysis More Appropriate?
- 6.1.2 LC/MS Technology and Instrumentation -- 6.1.3 Basic Terminologies and Concepts for MS -- 6.1.4 Interfacing HPLC and MS -- 6.2 LC/MS Instrumentation -- 6.2.1 Ion Sources -- 6.2.2 Fragmentation -- 6.2.3 Mass Analyzers -- 6.2.4 Detectors -- 6.3 Small‐Molecules Drug Research and Development -- 6.3.1 Mass Measurement and Elemental Composition Determination -- 6.3.2 Structural Elucidation -- 6.3.3 Trace Quantitation -- 6.4 Emerging Biopharmaceutical Applications -- 6.4.1 Intact Mass Measurement of Proteins -- 6.4.2 Structural Characterization of Proteins (Bottom‐Up and Top‐Down Approaches) -- 6.4.3 Peptide Quantitation -- 6.5 Environmental, Food Safety, Clinical, Toxicology, and "OMICS" Applications -- 6.6 Future Perspectives -- 6.7 Quizzes -- 6.7.1 Bonus Quiz -- 6.8 References -- Chapter 7 HPLC/UHPLC Operation Guide -- 7.1 Scope -- 7.2 Safety and Environmental Concerns -- 7.2.1 Safety Concerns -- 7.2.2 Environmental Concerns -- 7.3 Mobile Phase and Sample Preparation -- 7.3.1 Mobile Phase Premixing -- 7.3.2 Mobile Phase Additives and Buffers -- 7.3.3 Filtration -- 7.3.4 Degassing -- 7.3.5 Samples, Diluents, and Sample Preparation -- 7.4 Best Practices in HPLC/UHPLC System Operation -- 7.4.1 Pump Operation -- 7.4.2 HPLC Column Use, Precaution, Connection, and Maintenance -- 7.4.2.1 Column Use -- 7.4.2.2 Column Precautions -- 7.4.2.3 Column Connections -- 7.4.2.4 Column Maintenance and Regeneration -- 7.4.3 Autosampler Operation -- 7.4.4 Column Oven and Switching Valve -- 7.4.5 UV/Vis Detector Operation -- 7.4.6 HPLC System Shutdown -- 7.4.7 Guidelines for Increasing HPLC Precision -- 7.4.7.1 Guidelines for Improving Retention Time Precision -- 7.4.7.2 Guidelines for Improving Peak Area Precision -- 7.5 From Chromatograms to Reports -- 7.5.1 Qualitative Analysis Strategies -- 7.5.2 Quantitation Analysis Strategies -- 7.6 Summary of HPLC Operation