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A concise yet comprehensive reference guide on HPLC/UHPLC that focuses on its fundamentals, latest developments, and best practices in the pharmaceutical and biotechnology industries
Written for practitioners by an expert practitioner, this new edition of HPLC and UHPLC for Practicing Scientists 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, the modern standard platform. In addition to introducing readers to HPLC's fundamentals, applications, and developments, the book describes basic theory and terminology for the novice, and reviews relevant concepts, best practices, and modern trends for the experienced practitioner.
HPLC and UHPLC for Practicing Scientists, Second Edition offers three new chapters. One is a standalone chapter on UHPLC, covering concepts, benefits, practices, and potential issues. Another examines liquid chromatography/mass spectrometry (LC/MS). The third reviews at the analysis of recombinant biologics, particularly monoclonal antibodies (mAbs), used as therapeutics. While all chapters are revised in the new edition, five chapters are essentially rewritten (HPLC columns, instrumentation, pharmaceutical analysis, method development, and regulatory aspects). The book also includes problem and answer sections at the end of each chapter.
* Overviews fundamentals of HPLC to UHPLC, including theories, columns, and instruments with an abundance of tables, figures, and key references
* Features brand new chapters on UHPLC, LC/MS, and analysis of recombinant biologics
* Presents updated information on the best practices in method development, validation, operation, troubleshooting, and maintaining regulatory compliance for both HPLC and UHPLC
* Contains major revisions to all chapters of the first edition and substantial rewrites of chapters on HPLC columns, instrumentation, pharmaceutical analysis, method development, and regulatory aspects
* Includes end-of-chapter quizzes as assessment and learning aids
* Offers a reference guide to graduate students and practicing scientists in pharmaceutical, biotechnology, and other industries
Filled with intuitive explanations, case studies, and clear figures, HPLC and UHPLC for Practicing Scientists, Second Edition is an essential resource for practitioners of all levels who need to understand and utilize this versatile analytical technology. It will be a great benefit to every busy laboratory analyst and researcher.
Written for practitioners by an expert practitioner, this new edition of HPLC and UHPLC for Practicing Scientists 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, the modern standard platform. In addition to introducing readers to HPLC's fundamentals, applications, and developments, the book describes basic theory and terminology for the novice, and reviews relevant concepts, best practices, and modern trends for the experienced practitioner.
HPLC and UHPLC for Practicing Scientists, Second Edition offers three new chapters. One is a standalone chapter on UHPLC, covering concepts, benefits, practices, and potential issues. Another examines liquid chromatography/mass spectrometry (LC/MS). The third reviews at the analysis of recombinant biologics, particularly monoclonal antibodies (mAbs), used as therapeutics. While all chapters are revised in the new edition, five chapters are essentially rewritten (HPLC columns, instrumentation, pharmaceutical analysis, method development, and regulatory aspects). The book also includes problem and answer sections at the end of each chapter.
* Overviews fundamentals of HPLC to UHPLC, including theories, columns, and instruments with an abundance of tables, figures, and key references
* Features brand new chapters on UHPLC, LC/MS, and analysis of recombinant biologics
* Presents updated information on the best practices in method development, validation, operation, troubleshooting, and maintaining regulatory compliance for both HPLC and UHPLC
* Contains major revisions to all chapters of the first edition and substantial rewrites of chapters on HPLC columns, instrumentation, pharmaceutical analysis, method development, and regulatory aspects
* Includes end-of-chapter quizzes as assessment and learning aids
* Offers a reference guide to graduate students and practicing scientists in pharmaceutical, biotechnology, and other industries
Filled with intuitive explanations, case studies, and clear figures, HPLC and UHPLC for Practicing Scientists, Second Edition is an essential resource for practitioners of all levels who need to understand and utilize this versatile analytical technology. It will be a great benefit to every busy laboratory analyst and researcher.
A concise yet comprehensive reference guide on HPLC/UHPLC that focuses on its fundamentals, latest developments, and best practices in the pharmaceutical and biotechnology industries
Written for practitioners by an expert practitioner, this new edition of HPLC and UHPLC for Practicing Scientists 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, the modern standard platform. In addition to introducing readers to HPLC's fundamentals, applications, and developments, the book describes basic theory and terminology for the novice, and reviews relevant concepts, best practices, and modern trends for the experienced practitioner.
HPLC and UHPLC for Practicing Scientists, Second Edition offers three new chapters. One is a standalone chapter on UHPLC, covering concepts, benefits, practices, and potential issues. Another examines liquid chromatography/mass spectrometry (LC/MS). The third reviews at the analysis of recombinant biologics, particularly monoclonal antibodies (mAbs), used as therapeutics. While all chapters are revised in the new edition, five chapters are essentially rewritten (HPLC columns, instrumentation, pharmaceutical analysis, method development, and regulatory aspects). The book also includes problem and answer sections at the end of each chapter.
* Overviews fundamentals of HPLC to UHPLC, including theories, columns, and instruments with an abundance of tables, figures, and key references
* Features brand new chapters on UHPLC, LC/MS, and analysis of recombinant biologics
* Presents updated information on the best practices in method development, validation, operation, troubleshooting, and maintaining regulatory compliance for both HPLC and UHPLC
* Contains major revisions to all chapters of the first edition and substantial rewrites of chapters on HPLC columns, instrumentation, pharmaceutical analysis, method development, and regulatory aspects
* Includes end-of-chapter quizzes as assessment and learning aids
* Offers a reference guide to graduate students and practicing scientists in pharmaceutical, biotechnology, and other industries
Filled with intuitive explanations, case studies, and clear figures, HPLC and UHPLC for Practicing Scientists, Second Edition is an essential resource for practitioners of all levels who need to understand and utilize this versatile analytical technology. It will be a great benefit to every busy laboratory analyst and researcher.
Written for practitioners by an expert practitioner, this new edition of HPLC and UHPLC for Practicing Scientists 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, the modern standard platform. In addition to introducing readers to HPLC's fundamentals, applications, and developments, the book describes basic theory and terminology for the novice, and reviews relevant concepts, best practices, and modern trends for the experienced practitioner.
HPLC and UHPLC for Practicing Scientists, Second Edition offers three new chapters. One is a standalone chapter on UHPLC, covering concepts, benefits, practices, and potential issues. Another examines liquid chromatography/mass spectrometry (LC/MS). The third reviews at the analysis of recombinant biologics, particularly monoclonal antibodies (mAbs), used as therapeutics. While all chapters are revised in the new edition, five chapters are essentially rewritten (HPLC columns, instrumentation, pharmaceutical analysis, method development, and regulatory aspects). The book also includes problem and answer sections at the end of each chapter.
* Overviews fundamentals of HPLC to UHPLC, including theories, columns, and instruments with an abundance of tables, figures, and key references
* Features brand new chapters on UHPLC, LC/MS, and analysis of recombinant biologics
* Presents updated information on the best practices in method development, validation, operation, troubleshooting, and maintaining regulatory compliance for both HPLC and UHPLC
* Contains major revisions to all chapters of the first edition and substantial rewrites of chapters on HPLC columns, instrumentation, pharmaceutical analysis, method development, and regulatory aspects
* Includes end-of-chapter quizzes as assessment and learning aids
* Offers a reference guide to graduate students and practicing scientists in pharmaceutical, biotechnology, and other industries
Filled with intuitive explanations, case studies, and clear figures, HPLC and UHPLC for Practicing Scientists, Second Edition is an essential resource for practitioners of all levels who need to understand and utilize this versatile analytical technology. It will be a great benefit to every busy laboratory analyst and researcher.
Über den Autor
MICHAEL W. DONG, PHD, is the Principal of MWD Consulting, providing expert training and consulting service in HPLC/UHPLC, and pharmaceutical analysis. He is a former senior scientist, for GENENTECH, INC, small molecule analytical chemistry and quality control department. Dr. Dong conducts short courses on HPLC/UHPLC, drug development process, and drug quality at national meetings such as Pittcon, ACS, HPLC, and EAS. He also provides consulting services on CMC, HPLC method development, and solving drug quality issues. He holds a Ph.D. degree in analytical chemistry and has authored 120+ journal articles and three books.
Inhaltsverzeichnis
Author's Biography xvii Biographies of Contributors xix Preface xxi Foreword xxiii Acknowledgments xxv 1 Introduction 1 1.1 Introduction 1 1.1.1 Scope 1 1.1.2 What Is HPLC? 2 1.1.3 A Brief History 3 1.1.4 Advantages and Limitations 4 1.1.5 Ultra-High-Pressure Liquid Chromatography (UHPLC) 4 1.2 Primary Modes of HPLC 4 1.2.1 Normal-Phase Chromatography (NPC) 5 1.2.2 Reversed-Phase Chromatography (RPC) 5 1.2.3 Ion-Exchange Chromatography (IEC) 6 1.2.4 Size-Exclusion Chromatography (SEC) 8 1.2.5 Other Separation Modes 8 1.3 Some Common-Sense Corollaries 10 1.4 How to Get More Information 11 1.5 Summary 11 1.6 Quizzes 11 1.6.1 Bonus Quiz 12 References 12 2 Basic Terms and Concepts 15 2.1 Scope 15 2.2 Basic Terms and Concepts 16 2.2.1 Retention Time (tR), Void Time (tM), Peak Height (h), and Peak Width (wb) 16 2.2.2 Retention Volume (VR), Void Volume (VM), and Peak Volume 16 2.2.3 Retention Factor (k) 18 2.2.4 Separation Factor (¿) 19 2.2.5 Column Efficiency and Plate Number (N) 20 2.2.6 Peak Volume 20 2.2.7 Height Equivalent to a Theoretical Plate or Plate Height (HETP or H) 21 2.2.8 Resolution (Rs) 21 2.2.9 Peak Symmetry:Asymmetry Factor (As) and Tailing Factor (Tf) 23 2.3 Mobile Phase 24 2.3.1 General Requirements 24 2.3.2 Solvent Strength and Selectivity 25 2.3.3 pH Modifiers and Buffers 27 2.3.4 Acidic Mobile Phases 28 2.3.5 Ion-Pairing Reagents and Chaotropic Agents 29 2.3.6 High-pH Mobile Phases 29 2.3.7 Other Operating Parameters: Flow Rate (F) and Column Temperature (T) 30 2.4 The Resolution Equation 31 2.5 The Van Deemter Equation 33 2.6 Isocratic vs. Gradient Analysis 35 2.6.1 Peak Capacity (n) 35 2.6.2 Gradient Parameters (Initial and Final Solvent Strength, Gradient Time (tG), and Flow Rate) 36 2.6.3 The 0.25 ¿tG Rule: When Is Isocratic Analysis More Appropriate? 37 2.7 The Concept of Orthogonality and Selectivity Tuning 38 2.8 Sample Capacity 41 2.9 Glossary of HPLC Terms 41 2.10 Summary and Conclusion 42 2.11 Quizzes 42 2.11.1 Bonus Quiz 44 References 44 3 HPLC Columns and Trends 45 3.1 Scope 45 3.1.1 Glossary and Abbreviations 45 3.2 General Column Description and Characteristics 46 3.2.1 Column Hardware - Standard vs. Cartridge Format 47 3.3 Column Type 47 3.3.1 Types Based on Chromatographic Mode 48 3.3.2 Column Types Based on Dimension 48 3.3.3 Column Length (L) 48 3.4 Column Packing Characteristics 50 3.4.1 Support Type 50 3.4.2 Particle Size (dp) 51 3.4.3 Surface Area and Pore Size (dpore) 51 3.4.4 Bonding Chemistries 52 3.5 Modern HPLC Column Trends 54 3.5.1 Silica Support Material 54 3.5.2 Hybrid Particles 55 3.5.3 Novel Bonding Chemistries 58 3.5.4 Shorter and Narrower Columns Packed with Small Particles 61 3.5.5 Micro-LC and Nano-LC 62 3.5.6 Monoliths 64 3.5.7 Superficially Porous Particles (SPP) 65 3.5.8 Micropillar Array Chromatography (¿PAC) 67 3.6 Guard Columns 69 3.7 Specialty Columns 69 3.7.1 Bioseparations Columns 69 3.7.2 Chiral Columns 69 3.7.3 Supercritical Fluid Chromatography (SFC) Columns 71 3.7.4 Hydrophilic Interaction Liquid Chromatography (HILIC) Columns 72 3.7.5 Mixed-Mode Chromatography (MMC) Columns 72 3.7.6 Application-Specific Columns 73 3.8 RPC Column Selection Guides 73 3.8.1 Some General Guidelines for Bonded Phase Selection 75 3.9 Summary 76 3.10 Quizzes 76 3.10.1 Bonus Quiz 78 References 78 4 HPLC/UHPLC Instrumentation and Trends 81 4.1 Introduction 81 4.1.1 Scope 81 4.1.2 HPLC Systems and Modules 81 4.1.3 Ultra-High-Pressure Liquid Chromatography (UHPLC) 83 4.2 HPLC and UHPLC Solvent Delivery Systems 83 4.2.1 High-Pressure and Low-Pressure Mixing Designs in Multisolvent Pumps 85 4.2.2 System Dwell Volume 86 4.2.3 Trends 88 4.3 Injectors and Autosamplers 88 4.3.1 Operating Principles of Autosamplers 88 4.3.2 Performance Characteristics and Trends 89 4.4 Detectors 91 4.5 UV/VIS Absorbance Detectors 92 4.5.1 Operating Principles 92 4.5.2 Performance Characteristics 94 4.5.3 Trends in UV/Vis Absorbance Detectors 94 4.6 Photodiode Array Detectors 94 4.6.1 Operating Principles 94 4.6.2 Trends in PDA Detectors 95 4.7 Other Detectors 95 4.7.1 Refractive Index Detector (RID) 96 4.7.2 Evaporative Light Scattering Detector (ELSD) 96 4.7.3 Charged Aerosol Detector (CAD) 97 4.7.4 Conductivity Detector (CD) 97 4.7.5 Fluorescence Detector (FLD) 97 4.7.6 Chemiluminescence Nitrogen Detector (CLND) 98 4.7.7 Electrochemical Detector (ECD) 99 4.7.8 Radiometric Detector 99 4.8 Hyphenated and Specialized Systems 99 4.8.1 LC/MS and LC/MS/MS 99 4.8.2 LC/NMR 100 4.8.3 Other Hyphenated Systems 102 4.8.4 Supercritical Fluid Chromatography (SFC) 102 4.8.5 Preparative LC and SFC 102 4.8.6 Micro- and Nano-LC (Capillary LC) 102 4.8.7 Multidimensional LC 102 4.8.8 Lab-on-a-Chip 104 4.8.9 Specialized Applications Systems 104 4.9 HPLC Accessories 105 4.9.1 Solvent Degasser 105 4.9.2 Column Oven 105 4.9.3 Valves for Column and Mobile Phase Selection 106 4.10 Chromatography Data Systems (CDS) 106 4.10.1 User Interface and CDSWorkflow 107 4.11 Instrumental Bandwidth (IBW) 108 4.11.1 How to Measure IBW 109 4.11.2 IBW of UHPLC Systems 110 4.12 Manufacturers and Equipment Selection 111 4.13 Trends in HPLC and UHPLC Equipment 111 4.14 Summary 112 4.15 Quizzes 112 4.15.1 Bonus Quiz 114 References 114 5 UHPLC: Perspectives, Performance, Practices, and Potential Issues 117 5.1 Introduction 117 5.1.1 Scope 117 5.1.2 Glossary and Abbreviations 117 5.1.3 Historical Perspectives: What Is UHPLC? 118 5.2 Practical Concepts in UHPLC 120 5.2.1 Rationale for Higher System Pressure 120 5.2.2 Rationale for Low-Dispersion Systems 121 5.2.3 Rationale for Low Dwell Volumes 121 5.2.4 Other UHPLC Instrumental Characteristics 122 5.3 Benefits Of UHPLC and Case Studies 122 5.3.1 Benefit #1: Fast Separations with Good Resolution 122 5.3.2 Benefit #2: High-Resolution Analysis of Complex Samples 124 5.3.3 Benefit #3: Rapid HPLC Method Development 124 5.3.4 Flexibility for Customizing Resolution 129 5.3.5 Other Benefits of UHPLC 130 5.4 Potential Issues and How to Mitigate 132 5.4.1 Safety Issues 132 5.4.2 Viscous Heating 133 5.4.3 Instrumental and Operating Nuances 133 5.4.4 Injector Precision 135 5.4.5 UV Detection Noise vs. Mixer Volumes 135 5.4.6 Method Translation (Conversion) 138 5.5 How to Implement UHPLC and Practical Aspects 139 5.5.1 How to Transition from HPLC to UHPLC 139 5.5.2 End-Fittings 140 5.5.3 A Summary of UHPLC System Performance Tradeoffs 140 5.6 Myths in UHPLC 142 5.7 Summary and Conclusions 142 5.8 Quizzes 142 5.8.1 Bonus Quiz 144 References 144 6 LC/MS: Fundamentals, Perspectives, and Applications 147Christine Gu 6.1 Introduction 147 6.1.1 Scope 147 6.1.2 LC/MS Technology and Instrumentation 147 6.1.3 Basic Terminologies and Concepts for MS 148 6.1.4 Interfacing HPLC and MS 150 6.2 LC/MS Instrumentation 150 6.2.1 Ion Sources 150 6.2.2 Fragmentation 152 6.2.3 Mass Analyzers 153 6.2.4 Detectors 155 6.3 Small-Molecules Drug Research and Development 157 6.3.1 Mass Measurement and Elemental Composition Determination 157 6.3.2 Structural Elucidation 159 6.3.3 Trace Quantitation 162 6.4 Emerging Biopharmaceutical Applications 164 6.4.1 Intact Mass Measurement of Proteins 166 6.4.2 Structural Characterization of Proteins (Bottom-Up and Top-Down Approaches) 166 6.4.3 Peptide Quantitation 170 6.5 Environmental, Food Safety, Clinical, Toxicology, and "Omics" Applications 171 6.6 Future Perspectives 171 6.7 Quizzes 172 6.7.1 Bonus Quiz 174 References 174 7 HPLC/UHPLC Operation Guide 177 7.1 Scope 177 7.2 Safety and Environmental Concerns 177 7.2.1 Safety Concerns 177 7.2.2 Environmental Concerns 179 7.3 Mobile Phase and Sample Preparation 180 7.3.1 Mobile Phase Premixing 180 7.3.2 Mobile Phase Additives and Buffers 180 7.3.3 Filtration 180 7.3.4 Degassing 181 7.3.5 Samples, Diluents, and Sample Preparation 181 7.4 Best Practices in HPLC/UHPLC System Operation 182 7.4.1 Pump Operation 182 7.4.2 HPLC Column Use, Precaution, Connection, and Maintenance 183 7.4.3 Autosampler Operation 184 7.4.4 Column Oven and Switching Valve 186 7.4.5 UV/Vis Detector Operation 186 7.4.6 HPLC System Shutdown 187 7.4.7 Guidelines for Increasing HPLC Precision 187 7.5 From Chromatograms to Reports 189 7.5.1 Qualitative Analysis Strategies 192 7.5.2 Quantitation Analysis Strategies 192 7.6 Summary of HPLC Operation 193 7.7 Guides on Performing Trace Analysis 193 7.8 Summary 195 7.9 Quizzes 195 7.9.1 Bonus Quiz 196 References 196 8 HPLC/UHPLC Maintenance and Troubleshooting 199 8.1 Scope 199 8.2 HPLC System Maintenance 199 8.2.1 HPLC Pump 200 8.2.2 UV/Vis Absorbance or Photodiode Array Detectors (PDA) 202 8.2.3 Injector and Autosampler 204 8.3 HPLC Troubleshooting 204 8.3.1 General Problem Diagnostic and Troubleshooting Guide 205 8.3.2 Common HPLC Problems 206 8.4 Troubleshooting Case Studies 213 8.4.1 Case Study 1: Reducing Baseline Shift and Noise for Gradient Analysis 213 8.4.2 Case Study 2: Poor Peak Area Precision 214 8.4.3 Case Study 3: Poor Assay Accuracy Data 215 8.4.4 Case Study 4: Equipment Malfunctioning and Problems with Blank 216 8.5 Summary and Conclusion 217 8.6 Quizzes 218 8.6.1 Bonus Quiz 219 References 219 9 Pharmaceutical Analysis 221 9.1 Introduction 221 9.1.1 Scope 221 9.1.2 Glossary and Abbreviations 221 9.2 Overview of Drug Development Process 222 9.3 Sample Preparation Perspectives 224 9.4 HPLC, SFC, and HPLC/MS in Drug Discovery 224 9.5 HPLC Testing Methodologies for DS and DP 225 9.5.1 Identification Test (DS, DP) 227 9.5.2 ASSAY (Rough Potency and Performance Testing, DP) 227 9.5.3 Stability-Indicating Assay (Potency and Purity Testing of DS and DP) 230 9.5.4 Assay of Preservatives 238 9.5.5 Assay of Pharmaceutical Counterions 238 9.5.6 Assay of Potential Genotoxic Impurities (PGI) 239 9.6 Cleaning Verification 239 9.7 Bioanalytical Testing 240 9.8 Summary 242 9.9 Quizzes 242 9.9.1 Bonus Quiz 243 References 243 10 HPLC Method Development 245 10.1 Introduction 245 10.1.1 Scope 245 10.1.2 Considerations Before Method Development 245 10.1.3 HPLC Method Development Trends in Pharmaceutical Analysis 246 10.2 A...
Details
| Erscheinungsjahr: | 2019 |
|---|---|
| Fachbereich: | Theoretische Chemie |
| Genre: | Chemie |
| Rubrik: | Naturwissenschaften & Technik |
| Medium: | Taschenbuch |
| Inhalt: | 416 S. |
| ISBN-13: | 9781119313762 |
| ISBN-10: | 1119313767 |
| Sprache: | Englisch |
| Herstellernummer: | 1W119313760 |
| Einband: | Kartoniert / Broschiert |
| Autor: | Dong, Michael W |
| Auflage: | 2nd edition |
| Hersteller: | Wiley |
| Maße: | 254 x 177 x 30 mm |
| Von/Mit: | Michael W Dong |
| Erscheinungsdatum: | 23.07.2019 |
| Gewicht: | 0,862 kg |
Über den Autor
MICHAEL W. DONG, PHD, is the Principal of MWD Consulting, providing expert training and consulting service in HPLC/UHPLC, and pharmaceutical analysis. He is a former senior scientist, for GENENTECH, INC, small molecule analytical chemistry and quality control department. Dr. Dong conducts short courses on HPLC/UHPLC, drug development process, and drug quality at national meetings such as Pittcon, ACS, HPLC, and EAS. He also provides consulting services on CMC, HPLC method development, and solving drug quality issues. He holds a Ph.D. degree in analytical chemistry and has authored 120+ journal articles and three books.
Inhaltsverzeichnis
Author's Biography xvii Biographies of Contributors xix Preface xxi Foreword xxiii Acknowledgments xxv 1 Introduction 1 1.1 Introduction 1 1.1.1 Scope 1 1.1.2 What Is HPLC? 2 1.1.3 A Brief History 3 1.1.4 Advantages and Limitations 4 1.1.5 Ultra-High-Pressure Liquid Chromatography (UHPLC) 4 1.2 Primary Modes of HPLC 4 1.2.1 Normal-Phase Chromatography (NPC) 5 1.2.2 Reversed-Phase Chromatography (RPC) 5 1.2.3 Ion-Exchange Chromatography (IEC) 6 1.2.4 Size-Exclusion Chromatography (SEC) 8 1.2.5 Other Separation Modes 8 1.3 Some Common-Sense Corollaries 10 1.4 How to Get More Information 11 1.5 Summary 11 1.6 Quizzes 11 1.6.1 Bonus Quiz 12 References 12 2 Basic Terms and Concepts 15 2.1 Scope 15 2.2 Basic Terms and Concepts 16 2.2.1 Retention Time (tR), Void Time (tM), Peak Height (h), and Peak Width (wb) 16 2.2.2 Retention Volume (VR), Void Volume (VM), and Peak Volume 16 2.2.3 Retention Factor (k) 18 2.2.4 Separation Factor (¿) 19 2.2.5 Column Efficiency and Plate Number (N) 20 2.2.6 Peak Volume 20 2.2.7 Height Equivalent to a Theoretical Plate or Plate Height (HETP or H) 21 2.2.8 Resolution (Rs) 21 2.2.9 Peak Symmetry:Asymmetry Factor (As) and Tailing Factor (Tf) 23 2.3 Mobile Phase 24 2.3.1 General Requirements 24 2.3.2 Solvent Strength and Selectivity 25 2.3.3 pH Modifiers and Buffers 27 2.3.4 Acidic Mobile Phases 28 2.3.5 Ion-Pairing Reagents and Chaotropic Agents 29 2.3.6 High-pH Mobile Phases 29 2.3.7 Other Operating Parameters: Flow Rate (F) and Column Temperature (T) 30 2.4 The Resolution Equation 31 2.5 The Van Deemter Equation 33 2.6 Isocratic vs. Gradient Analysis 35 2.6.1 Peak Capacity (n) 35 2.6.2 Gradient Parameters (Initial and Final Solvent Strength, Gradient Time (tG), and Flow Rate) 36 2.6.3 The 0.25 ¿tG Rule: When Is Isocratic Analysis More Appropriate? 37 2.7 The Concept of Orthogonality and Selectivity Tuning 38 2.8 Sample Capacity 41 2.9 Glossary of HPLC Terms 41 2.10 Summary and Conclusion 42 2.11 Quizzes 42 2.11.1 Bonus Quiz 44 References 44 3 HPLC Columns and Trends 45 3.1 Scope 45 3.1.1 Glossary and Abbreviations 45 3.2 General Column Description and Characteristics 46 3.2.1 Column Hardware - Standard vs. Cartridge Format 47 3.3 Column Type 47 3.3.1 Types Based on Chromatographic Mode 48 3.3.2 Column Types Based on Dimension 48 3.3.3 Column Length (L) 48 3.4 Column Packing Characteristics 50 3.4.1 Support Type 50 3.4.2 Particle Size (dp) 51 3.4.3 Surface Area and Pore Size (dpore) 51 3.4.4 Bonding Chemistries 52 3.5 Modern HPLC Column Trends 54 3.5.1 Silica Support Material 54 3.5.2 Hybrid Particles 55 3.5.3 Novel Bonding Chemistries 58 3.5.4 Shorter and Narrower Columns Packed with Small Particles 61 3.5.5 Micro-LC and Nano-LC 62 3.5.6 Monoliths 64 3.5.7 Superficially Porous Particles (SPP) 65 3.5.8 Micropillar Array Chromatography (¿PAC) 67 3.6 Guard Columns 69 3.7 Specialty Columns 69 3.7.1 Bioseparations Columns 69 3.7.2 Chiral Columns 69 3.7.3 Supercritical Fluid Chromatography (SFC) Columns 71 3.7.4 Hydrophilic Interaction Liquid Chromatography (HILIC) Columns 72 3.7.5 Mixed-Mode Chromatography (MMC) Columns 72 3.7.6 Application-Specific Columns 73 3.8 RPC Column Selection Guides 73 3.8.1 Some General Guidelines for Bonded Phase Selection 75 3.9 Summary 76 3.10 Quizzes 76 3.10.1 Bonus Quiz 78 References 78 4 HPLC/UHPLC Instrumentation and Trends 81 4.1 Introduction 81 4.1.1 Scope 81 4.1.2 HPLC Systems and Modules 81 4.1.3 Ultra-High-Pressure Liquid Chromatography (UHPLC) 83 4.2 HPLC and UHPLC Solvent Delivery Systems 83 4.2.1 High-Pressure and Low-Pressure Mixing Designs in Multisolvent Pumps 85 4.2.2 System Dwell Volume 86 4.2.3 Trends 88 4.3 Injectors and Autosamplers 88 4.3.1 Operating Principles of Autosamplers 88 4.3.2 Performance Characteristics and Trends 89 4.4 Detectors 91 4.5 UV/VIS Absorbance Detectors 92 4.5.1 Operating Principles 92 4.5.2 Performance Characteristics 94 4.5.3 Trends in UV/Vis Absorbance Detectors 94 4.6 Photodiode Array Detectors 94 4.6.1 Operating Principles 94 4.6.2 Trends in PDA Detectors 95 4.7 Other Detectors 95 4.7.1 Refractive Index Detector (RID) 96 4.7.2 Evaporative Light Scattering Detector (ELSD) 96 4.7.3 Charged Aerosol Detector (CAD) 97 4.7.4 Conductivity Detector (CD) 97 4.7.5 Fluorescence Detector (FLD) 97 4.7.6 Chemiluminescence Nitrogen Detector (CLND) 98 4.7.7 Electrochemical Detector (ECD) 99 4.7.8 Radiometric Detector 99 4.8 Hyphenated and Specialized Systems 99 4.8.1 LC/MS and LC/MS/MS 99 4.8.2 LC/NMR 100 4.8.3 Other Hyphenated Systems 102 4.8.4 Supercritical Fluid Chromatography (SFC) 102 4.8.5 Preparative LC and SFC 102 4.8.6 Micro- and Nano-LC (Capillary LC) 102 4.8.7 Multidimensional LC 102 4.8.8 Lab-on-a-Chip 104 4.8.9 Specialized Applications Systems 104 4.9 HPLC Accessories 105 4.9.1 Solvent Degasser 105 4.9.2 Column Oven 105 4.9.3 Valves for Column and Mobile Phase Selection 106 4.10 Chromatography Data Systems (CDS) 106 4.10.1 User Interface and CDSWorkflow 107 4.11 Instrumental Bandwidth (IBW) 108 4.11.1 How to Measure IBW 109 4.11.2 IBW of UHPLC Systems 110 4.12 Manufacturers and Equipment Selection 111 4.13 Trends in HPLC and UHPLC Equipment 111 4.14 Summary 112 4.15 Quizzes 112 4.15.1 Bonus Quiz 114 References 114 5 UHPLC: Perspectives, Performance, Practices, and Potential Issues 117 5.1 Introduction 117 5.1.1 Scope 117 5.1.2 Glossary and Abbreviations 117 5.1.3 Historical Perspectives: What Is UHPLC? 118 5.2 Practical Concepts in UHPLC 120 5.2.1 Rationale for Higher System Pressure 120 5.2.2 Rationale for Low-Dispersion Systems 121 5.2.3 Rationale for Low Dwell Volumes 121 5.2.4 Other UHPLC Instrumental Characteristics 122 5.3 Benefits Of UHPLC and Case Studies 122 5.3.1 Benefit #1: Fast Separations with Good Resolution 122 5.3.2 Benefit #2: High-Resolution Analysis of Complex Samples 124 5.3.3 Benefit #3: Rapid HPLC Method Development 124 5.3.4 Flexibility for Customizing Resolution 129 5.3.5 Other Benefits of UHPLC 130 5.4 Potential Issues and How to Mitigate 132 5.4.1 Safety Issues 132 5.4.2 Viscous Heating 133 5.4.3 Instrumental and Operating Nuances 133 5.4.4 Injector Precision 135 5.4.5 UV Detection Noise vs. Mixer Volumes 135 5.4.6 Method Translation (Conversion) 138 5.5 How to Implement UHPLC and Practical Aspects 139 5.5.1 How to Transition from HPLC to UHPLC 139 5.5.2 End-Fittings 140 5.5.3 A Summary of UHPLC System Performance Tradeoffs 140 5.6 Myths in UHPLC 142 5.7 Summary and Conclusions 142 5.8 Quizzes 142 5.8.1 Bonus Quiz 144 References 144 6 LC/MS: Fundamentals, Perspectives, and Applications 147Christine Gu 6.1 Introduction 147 6.1.1 Scope 147 6.1.2 LC/MS Technology and Instrumentation 147 6.1.3 Basic Terminologies and Concepts for MS 148 6.1.4 Interfacing HPLC and MS 150 6.2 LC/MS Instrumentation 150 6.2.1 Ion Sources 150 6.2.2 Fragmentation 152 6.2.3 Mass Analyzers 153 6.2.4 Detectors 155 6.3 Small-Molecules Drug Research and Development 157 6.3.1 Mass Measurement and Elemental Composition Determination 157 6.3.2 Structural Elucidation 159 6.3.3 Trace Quantitation 162 6.4 Emerging Biopharmaceutical Applications 164 6.4.1 Intact Mass Measurement of Proteins 166 6.4.2 Structural Characterization of Proteins (Bottom-Up and Top-Down Approaches) 166 6.4.3 Peptide Quantitation 170 6.5 Environmental, Food Safety, Clinical, Toxicology, and "Omics" Applications 171 6.6 Future Perspectives 171 6.7 Quizzes 172 6.7.1 Bonus Quiz 174 References 174 7 HPLC/UHPLC Operation Guide 177 7.1 Scope 177 7.2 Safety and Environmental Concerns 177 7.2.1 Safety Concerns 177 7.2.2 Environmental Concerns 179 7.3 Mobile Phase and Sample Preparation 180 7.3.1 Mobile Phase Premixing 180 7.3.2 Mobile Phase Additives and Buffers 180 7.3.3 Filtration 180 7.3.4 Degassing 181 7.3.5 Samples, Diluents, and Sample Preparation 181 7.4 Best Practices in HPLC/UHPLC System Operation 182 7.4.1 Pump Operation 182 7.4.2 HPLC Column Use, Precaution, Connection, and Maintenance 183 7.4.3 Autosampler Operation 184 7.4.4 Column Oven and Switching Valve 186 7.4.5 UV/Vis Detector Operation 186 7.4.6 HPLC System Shutdown 187 7.4.7 Guidelines for Increasing HPLC Precision 187 7.5 From Chromatograms to Reports 189 7.5.1 Qualitative Analysis Strategies 192 7.5.2 Quantitation Analysis Strategies 192 7.6 Summary of HPLC Operation 193 7.7 Guides on Performing Trace Analysis 193 7.8 Summary 195 7.9 Quizzes 195 7.9.1 Bonus Quiz 196 References 196 8 HPLC/UHPLC Maintenance and Troubleshooting 199 8.1 Scope 199 8.2 HPLC System Maintenance 199 8.2.1 HPLC Pump 200 8.2.2 UV/Vis Absorbance or Photodiode Array Detectors (PDA) 202 8.2.3 Injector and Autosampler 204 8.3 HPLC Troubleshooting 204 8.3.1 General Problem Diagnostic and Troubleshooting Guide 205 8.3.2 Common HPLC Problems 206 8.4 Troubleshooting Case Studies 213 8.4.1 Case Study 1: Reducing Baseline Shift and Noise for Gradient Analysis 213 8.4.2 Case Study 2: Poor Peak Area Precision 214 8.4.3 Case Study 3: Poor Assay Accuracy Data 215 8.4.4 Case Study 4: Equipment Malfunctioning and Problems with Blank 216 8.5 Summary and Conclusion 217 8.6 Quizzes 218 8.6.1 Bonus Quiz 219 References 219 9 Pharmaceutical Analysis 221 9.1 Introduction 221 9.1.1 Scope 221 9.1.2 Glossary and Abbreviations 221 9.2 Overview of Drug Development Process 222 9.3 Sample Preparation Perspectives 224 9.4 HPLC, SFC, and HPLC/MS in Drug Discovery 224 9.5 HPLC Testing Methodologies for DS and DP 225 9.5.1 Identification Test (DS, DP) 227 9.5.2 ASSAY (Rough Potency and Performance Testing, DP) 227 9.5.3 Stability-Indicating Assay (Potency and Purity Testing of DS and DP) 230 9.5.4 Assay of Preservatives 238 9.5.5 Assay of Pharmaceutical Counterions 238 9.5.6 Assay of Potential Genotoxic Impurities (PGI) 239 9.6 Cleaning Verification 239 9.7 Bioanalytical Testing 240 9.8 Summary 242 9.9 Quizzes 242 9.9.1 Bonus Quiz 243 References 243 10 HPLC Method Development 245 10.1 Introduction 245 10.1.1 Scope 245 10.1.2 Considerations Before Method Development 245 10.1.3 HPLC Method Development Trends in Pharmaceutical Analysis 246 10.2 A...
Details
| Erscheinungsjahr: | 2019 |
|---|---|
| Fachbereich: | Theoretische Chemie |
| Genre: | Chemie |
| Rubrik: | Naturwissenschaften & Technik |
| Medium: | Taschenbuch |
| Inhalt: | 416 S. |
| ISBN-13: | 9781119313762 |
| ISBN-10: | 1119313767 |
| Sprache: | Englisch |
| Herstellernummer: | 1W119313760 |
| Einband: | Kartoniert / Broschiert |
| Autor: | Dong, Michael W |
| Auflage: | 2nd edition |
| Hersteller: | Wiley |
| Maße: | 254 x 177 x 30 mm |
| Von/Mit: | Michael W Dong |
| Erscheinungsdatum: | 23.07.2019 |
| Gewicht: | 0,862 kg |
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