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E-grāmata: HPLC and UHPLC for Practicing Scientists

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  • Formāts: PDF+DRM
  • Izdošanas datums: 10-Jul-2019
  • Izdevniecība: John Wiley & Sons Inc
  • Valoda: eng
  • ISBN-13: 9781119313793
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HPLC and UHPLC for Practicing ScientistsPalielināt
  • Formāts: PDF+DRM
  • Izdošanas datums: 10-Jul-2019
  • Izdevniecība: John Wiley & Sons Inc
  • Valoda: eng
  • ISBN-13: 9781119313793
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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.

Author's Biography xvii
Biographies of Contributors xix
Preface xxi
Foreword xxiii
Acknowledgments xxv
1 Introduction 1(14)
1.1 Introduction
1(3)
1.1.1 Scope
1(1)
1.1.2 What Is HPLC?
2(1)
1.1.3 A Brief History
3(1)
1.1.4 Advantages and Limitations
4(1)
1.1.5 Ultra-High-Pressure Liquid Chromatography (UHPLC)
4(1)
1.2 Primary Modes of HPLC
4(6)
1.2.1 Normal-Phase Chromatography (NPC)
5(1)
1.2.2 Reversed-Phase Chromatography (RPC)
5(1)
1.2.3 Ion-Exchange Chromatography (IEC)
6(2)
1.2.4 Size-Exclusion Chromatography (SEC)
8(1)
1.2.5 Other Separation Modes
8(2)
1.3 Some Common-Sense Corollaries
10(1)
1.4 How to Get More Information
11(1)
1.5 Summary
11(1)
1.6 Quizzes
11(1)
1.6.1 Bonus Quiz
12(1)
References
12(3)
2 Basic Terms and Concepts 15(30)
2.1 Scope
15(1)
2.2 Basic Terms and Concepts
16(8)
2.2.1 Retention Time (tR), Void Time (tM), Peak Height (h), and Peak Width (wb)
16(1)
2.2.2 Retention Volume (VR), Void Volume (VM), and Peak Volume
16(2)
2.2.3 Retention Factor (k)
18(1)
2.2.4 Separation Factor (α)
19(1)
2.2.5 Column Efficiency and Plate Number (N)
20(1)
2.2.6 Peak Volume
20(1)
2.2.7 Height Equivalent to a Theoretical Plate or Plate Height (HETP or H)
21(1)
2.2.8 Resolution (Rs)
21(2)
2.2.9 Peak Symmetry: Asymmetry Factor (As) and Tailing Factor (Tf)
23(1)
2.3 Mobile Phase
24(7)
2.3.1 General Requirements
24(1)
2.3.2 Solvent Strength and Selectivity
25(2)
2.3.3 pH Modifiers and Buffers
27(1)
2.3.4 Acidic Mobile Phases
28(1)
2.3.5 Ion-Pairing Reagents and Chaotropic Agents
29(1)
2.3.6 High-pH Mobile Phases
29(1)
2.3.7 Other Operating Parameters: Flow Rate (F) and Column Temperature (T)
30(1)
2.4 The Resolution Equation
31(2)
2.5 The Van Deemter Equation
33(2)
2.6 Isocratic vs. Gradient Analysis
35(3)
2.6.1 Peak Capacity (n)
35(1)
2.6.2 Gradient Parameters (Initial and Final Solvent Strength, Gradient Time (tG), and Flow Rate)
36(1)
2.6.3 The 0.25 ΔtG Rule: When Is Isocratic Analysis More Appropriate?
37(1)
2.7 The Concept of Orthogonality and Selectivity Tuning
38(3)
2.8 Sample Capacity
41(1)
2.9 Glossary of HPLC Terms
41(1)
2.10 Summary and Conclusion
42(1)
2.11 Quizzes
42(2)
2.11.1 Bonus Quiz
44(1)
References
44(1)
3 HPLC Columns and Trends 45(36)
3.1 Scope
45(1)
3.1.1 Glossary and Abbreviations
45(1)
3.2 General Column Description and Characteristics
46(1)
3.2.1 Column Hardware - Standard vs. Cartridge Format
47(1)
3.3 Column Type
47(3)
3.3.1 Types Based on Chromatographic Mode
48(1)
3.3.2 Column Types Based on Dimension
48(1)
3.3.3 Column Length (L)
48(2)
3.4 Column Packing Characteristics
50(4)
3.4.1 Support Type
50(1)
3.4.2 Particle Size (dp)
51(1)
3.4.3 Surface Area and Pore Size (dpore)
51(1)
3.4.4 Bonding Chemistries
52(2)
3.5 Modern HPLC Column Trends
54(15)
3.5.1 Silica Support Material
54(1)
3.5.2 Hybrid Particles
55(3)
3.5.3 Novel Bonding Chemistries
58(3)
3.5.3.1 Bonded Phases for Retention of Polar Analytes
59(2)
3.5.3.2 Charged Surface Hybrid (CSH)
61(1)
3.5.4 Shorter and Narrower Columns Packed with Small Particles
61(1)
3.5.4.1 Fast LC
61(1)
3.5.4.2 UHPLC
62(1)
3.5.5 Micro-LC and Nano-LC
62(2)
3.5.6 Monoliths
64(1)
3.5.7 Superficially Porous Particles (SPP)
65(2)
3.5.7.1 Kinetic Plots Demonstrating the Superiority of SPP
66(1)
3.5.8 Micropillar Array Chromatography (µPAC)
67(2)
3.6 Guard Columns
69(1)
3.7 Specialty Columns
69(4)
3.7.1 Bioseparations Columns
69(1)
3.7.2 Chiral Columns
69(2)
3.7.3 Supercritical Fluid Chromatography (SFC) Columns
71(1)
3.7.4 Hydrophilic Interaction Liquid Chromatography (HILIC) Columns
72(1)
3.7.5 Mixed-Mode Chromatography (MMC) Columns
72(1)
3.7.6 Application-Specific Columns
73(1)
3.8 RPC Column Selection Guides
73(3)
3.8.1 Some General Guidelines for Bonded Phase Selection
75(1)
3.9 Summary
76(1)
3.10 Quizzes
76(2)
3.10.1 Bonus Quiz
78(1)
References
78(3)
4 HPLC/UHPLC Instrumentation and Trends 81(36)
4.1 Introduction
81(2)
4.1.1 Scope
81(1)
4.1.2 HPLC Systems and Modules
81(2)
4.1.3 Ultra-High-Pressure Liquid Chromatography (UHPLC)
83(1)
4.2 HPLC and UHPLC Solvent Delivery Systems
83(5)
4.2.1 High-Pressure and Low-Pressure Mixing Designs in Multisolvent Pumps
85(1)
4.2.2 System Dwell Volume
86(2)
4.2.2.1 Dwell Volumes of UHPLC Systems
87(1)
4.2.3 Trends
88(1)
4.3 Injectors and Autosamplers
88(3)
4.3.1 Operating Principles of Autosamplers
88(1)
4.3.2 Performance Characteristics and Trends
89(2)
4.4 Detectors
91(1)
4.5 UV/VIS Absorbance Detectors
92(2)
4.5.1 Operating Principles
92(2)
4.5.2 Performance Characteristics
94(1)
4.5.3 Trends in UV/Vis Absorbance Detectors
94(1)
4.6 Photodiode Array Detectors
94(1)
4.6.1 Operating Principles
94(1)
4.6.2 Trends in PDA Detectors
95(1)
4.7 Other Detectors
95(4)
4.7.1 Refractive Index Detector (RID)
96(1)
4.7.2 Evaporative Light Scattering Detector (ELSD)
96(1)
4.7.3 Charged Aerosol Detector (CAD)
97(1)
4.7.4 Conductivity Detector (CD)
97(1)
4.7.5 Fluorescence Detector (FLD)
97(1)
4.7.5.1 Postcolumn Reaction Technique
98(1)
4.7.6 Chemiluminescence Nitrogen Detector (CLND)
98(1)
4.7.7 Electrochemical Detector (ECD)
99(1)
4.7.8 Radiometric Detector
99(1)
4.8 Hyphenated and Specialized Systems
99(6)
4.8.1 LC/MS and LC/MS/MS
99(1)
4.8.2 LC/NMR
100(2)
4.8.3 Other Hyphenated Systems
102(1)
4.8.4 Supercritical Fluid Chromatography (SFC)
102(1)
4.8.5 Preparative LC and SFC
102(1)
4.8.6 Micro- and Nano-LC (Capillary LC)
102(1)
4.8.7 Multidimensional LC
102(2)
4.8.8 Lab-on-a-Chip
104(1)
4.8.9 Specialized Applications Systems
104(1)
4.8.9.1 Gel-Permeation Chromatography (GPC)
104(1)
4.8.9.2 Ion Chromatography (IC)
105(1)
4.8.9.3 Application-Specific Systems
105(1)
4.9 HPLC Accessories
105(1)
4.9.1 Solvent Degasser
105(1)
4.9.2 Column Oven
105(1)
4.9.3 Valves for Column and Mobile Phase Selection
106(1)
4.10 Chromatography Data Systems (CDS)
106(2)
4.10.1 User Interface and CDS Workflow
107(1)
4.11 Instrumental Bandwidth (IBW)
108(3)
4.11.1 How to Measure IBW
109(1)
4.11.2 IBW of UHPLC Systems
110(1)
4.12 Manufacturers and Equipment Selection
111(1)
4.13 Trends in HPLC and UHPLC Equipment
111(1)
4.14 Summary
112(1)
4.15 Quizzes
112(2)
4.15.1 Bonus Quiz
114(1)
References
114(3)
5 UHPLC: Perspectives, Performance, Practices, and Potential Issues 117(30)
5.1 Introduction
117(3)
5.1.1 Scope
117(1)
5.1.2 Glossary and Abbreviations
117(1)
5.1.3 Historical Perspectives: What is UHPLC?
118(2)
5.2 Practical Concepts in UHPLC
120(2)
5.2.1 Rationale for Higher System Pressure
120(1)
5.2.2 Rationale for Low-Dispersion Systems
121(1)
5.2.3 Rationale for Low Dwell Volumes
121(1)
5.2.4 Other UHPLC Instrumental Characteristics
122(1)
5.3 Benefits Of UHPLC and Case Studies
122(10)
5.3.1 Benefit #1: Fast Separations with Good Resolution
122(2)
5.3.2 Benefit #2: High-Resolution Analysis of Complex Samples
124(1)
5.3.3 Benefit #3: Rapid HPLC Method Development
124(5)
5.3.4 Flexibility for Customizing Resolution
129(1)
5.3.5 Other Benefits of UHPLC
130(2)
5.3.5.1 Solvent Saving
130(1)
5.3.5.2 Higher Mass Sensitivity in UV Detection
130(1)
5.3.5.3 Higher Precision Performance for Retention Time and Peak Area
130(1)
5.3.5.4 UHPLC are Compatible with Other Approaches
131(1)
5.4 Potential Issues and How to Mitigate
132(7)
5.4.1 Safety Issues
132(1)
5.4.2 Viscous Heating
133(1)
5.4.3 Instrumental and Operating Nuances
133(2)
5.4.4 Injector Precision
135(1)
5.4.5 UV Detection Noise vs. Mixer Volumes
135(3)
5.4.6 Method Translation (Conversion)
138(1)
5.4.6.1 Running the Same HPLC Methods on HPLC and UHPLC
138(1)
5.4.6.2 Back Conversion of UHPLC Methods to HPLC Method Conditions
139(1)
5.4.6.3 Conversion of Existing HPLC Methods to Faster UHPLC Methods
139(1)
5.4.6.4 Method Validation Requirements After Method Translation
139(1)
5.5 How to Implement UHPLC and Practical Aspects
139(3)
5.5.1 How to Transition from HPLC to UHPLC
139(1)
5.5.2 End-Fittings
140(1)
5.5.3 A Summary of UHPLC System Performance Tradeoffs
140(2)
5.6 Myths in UHPLC
142(1)
5.7 Summary and Conclusions
142(1)
5.8 Quizzes
142(2)
5.8.1 Bonus Quiz
144(1)
References
144(3)
6 LC/MS: Fundamentals, Perspectives, and Applications 147(30)
Christine Gu
6.1 Introduction
147(3)
6.1.1 Scope
147(1)
6.1.2 LC/MS Technology and Instrumentation
147(1)
6.1.3 Basic Terminologies and Concepts for MS
148(2)
6.1.4 Interfacing HPLC and MS
150(1)
6.2 LC/MS Instrumentation
150(7)
6.2.1 Ion Sources
150(2)
6.2.2 Fragmentation
152(1)
6.2.3 Mass Analyzers
153(2)
6.2.4 Detectors
155(2)
6.3 Small-Molecules Drug Research and Development
157(7)
6.3.1 Mass Measurement and Elemental Composition Determination
157(2)
6.3.2 Structural Elucidation
159(3)
6.3.3 Trace Quantitation
162(2)
6.4 Emerging Biopharmaceutical Applications
164(7)
6.4.1 Intact Mass Measurement of Proteins
166(1)
6.4.2 Structural Characterization of Proteins (Bottom-Up and Top-Down Approaches)
166(4)
6.4.3 Peptide Quantitation
170(1)
6.5 Environmental, Food Safety, Clinical, Toxicology, and "Omics" Applications
171(1)
6.6 Future Perspectives
171(1)
6.7 Quizzes
172(5)
6.7.1 Bonus Quiz
174(1)
References
174(3)
7 HPLC/UHPLC Operation Guide 177(22)
7.1 Scope
177(1)
7.2 Safety and Environmental Concerns
177(3)
7.2.1 Safety Concerns
177(2)
7.2.2 Environmental Concerns
179(1)
7.3 Mobile Phase and Sample Preparation
180(2)
7.3.1 Mobile Phase Premixing
180(1)
7.3.2 Mobile Phase Additives and Buffers
180(1)
7.3.3 Filtration
180(1)
7.3.4 Degassing
181(1)
7.3.5 Samples, Diluents, and Sample Preparation
181(1)
7.4 Best Practices in HPLC/UHPLC System Operation
182(7)
7.4.1 Pump Operation
182(1)
7.4.2 HPLC Column Use, Precaution, Connection, and Maintenance
183(1)
7.4.2.1 Column Use
183(1)
7.4.2.2 Column Precautions
183(1)
7.4.2.3 Column Connections
183(1)
7.4.2.4 Column Maintenance and Regeneration
184(1)
7.4.3 Autosampler Operation
184(2)
7.4.4 Column Oven and Switching Valve
186(1)
7.4.5 UV/Vis Detector Operation
186(1)
7.4.6 HPLC System Shutdown
187(1)
7.4.7 Guidelines for Increasing HPLC Precision
187(2)
7.4.7.1 Guidelines for Improving Retention Time Precision
187(1)
7.4.7.2 Guidelines for Improving Peak Area Precision
188(1)
7.5 From Chromatograms to Reports
189(4)
7.5.1 Qualitative Analysis Strategies
192(1)
7.5.2 Quantitation Analysis Strategies
192(1)
7.6 Summary of HPLC Operation
193(1)
7.7 Guides on Performing Trace Analysis
193(2)
7.8 Summary
195(1)
7.9 Quizzes
195(1)
7.9.1 Bonus Quiz
196(1)
References
196(3)
8 HPLC/UHPLC Maintenance and Troubleshooting 199(22)
8.1 Scope
199(1)
8.2 HPLC System Maintenance
199(5)
8.2.1 HPLC Pump
200(2)
8.2.2 UV/Vis Absorbance or Photodiode Array Detectors (PDA)
202(2)
8.2.3 Injector and Autosampler
204(1)
8.3 HPLC Troubleshooting
204(9)
8.3.1 General Problem Diagnostic and Troubleshooting Guide
205(1)
8.3.2 Common HPLC Problems
206(7)
8.3.2.1 Pressure Problems and Causes
207(1)
8.3.2.2 Baseline Problems (Chromatogram)
207(3)
8.3.2.3 Peak Problems (Chromatogram)
210(3)
8.3.2.4 Data Performance Problems
213(1)
8.4 Troubleshooting Case Studies
213(4)
8.4.1 Case Study 1: Reducing Baseline Shift and Noise for Gradient Analysis
213(1)
8.4.2 Case Study 2: Poor Peak Area Precision
214(1)
8.4.3 Case Study 3: Poor Assay Accuracy Data
215(1)
8.4.4 Case Study 4: Equipment Malfunctioning and Problems with Blank
216(1)
8.5 Summary and Conclusion
217(1)
8.6 Quizzes
218(1)
8.6.1 Bonus Quiz
219(1)
References
219(2)
9 Pharmaceutical Analysis 221(24)
9.1 Introduction
221(1)
9.1.1 Scope
221(1)
9.1.2 Glossary and Abbreviations
221(1)
9.2 Overview of Drug Development Process
222(2)
9.3 Sample Preparation Perspectives
224(1)
9.4 HPLC, SFC, and HPLC/MS in Drug Discovery
224(1)
9.5 HPLC Testing Methodologies for DS and DP
225(14)
9.5.1 Identification Test (DS, DP)
227(1)
9.5.2 ASSAY (Rough Potency and Performance Testing, DP)
227(3)
9.5.2.1 Testing for Uniformity of Dosage Units
227(1)
9.5.2.2 Dissolution Testing
228(2)
9.5.3 Stability-Indicating Assay (Potency and Purity Testing of DS and DP)
230(8)
9.5.3.1 Trends in Stability-Indicating Methods
230(1)
9.5.3.2 Potency Determination (DS, DP)
231(1)
9.5.3.3 Qualification of Reference Standard for the API
232(1)
9.5.3.4 Quantitation of Impurities and Degradation Products (DS, DP)
233(1)
9.5.3.5 Case Study of an HPLC Method of an API with Multiple Chiral Centers
234(2)
9.5.3.6 Control of Chemical and Chiral Purities of Starting Materials for Multichiral APIs
236(1)
9.5.3.7 DP with Multiple APIs or Natural Products
237(1)
9.5.3.8 Stability Studies
237(1)
9.5.4 Assay of Preservatives
238(1)
9.5.5 Assay of Pharmaceutical Counterions
238(1)
9.5.6 Assay of Potential Genotoxic Impurities (PGI)
239(1)
9.6 Cleaning Verification
239(1)
9.7 Bioanalytical Testing
240(2)
9.8 Summary
242(1)
9.9 Quizzes
242(1)
9.9.1 Bonus Quiz
243(1)
References
243(2)
10 HPLC Method Development 245(36)
10.1 Introduction
245(1)
10.1.1 Scope
245(1)
10.1.2 Considerations Before Method Development
245(1)
10.1.3 HPLC Method Development Trends in Pharmaceutical Analysis
246(1)
10.2 A Five-Step Strategy for Traditional HPLC Method Development
246(12)
10.2.1 Step 1: Defining Method Types and Goals
246(2)
10.2.1.1 Method Goals and Acceptance Criteria for Quantitative Assays
247(1)
10.2.2 Step 2: Gathering Sample and Analyte Information
248(1)
10.2.3 Step 3: Initial HPLC Method Development
248(5)
10.2.3.1 Initial Detector Selection
249(1)
10.2.3.2 Selection of Chromatographic Mode
250(1)
10.2.3.3 Selecting Samples
250(1)
10.2.3.4 Initial Selection of HPLC Column and Mobile Phase
251(1)
10.2.3.5 Generating the First Chromatogram
251(1)
10.2.3.6 Case Study: Initial Purity Method Development of an NCE Using a Broad Gradient
251(2)
10.2.4 Step 4: Method Fine-Tuning and Optimization
253(3)
10.2.4.1 Mobile Phase Parameters (%B, pH, Buffer, Solvent Type)
255(1)
10.2.4.2 Operating Parameters (F, T, ΔΦ, tG, Gradient Segment)
255(1)
10.2.4.3 Column Parameters (Bonded Phase Type, L, dp, dc)
255(1)
10.2.4.4 Detector Setting and Sample Amount
256(1)
10.2.5 Step 5: Method Prequalification
256(1)
10.2.6 Summary of Method Development Steps
257(1)
10.2.7 Phase-Appropriate Method Development and Validation
257(1)
10.2.8 Method Development Software Tools
258(1)
10.3 Case Studies
258(10)
10.3.1 A Phase-0 Drug Substance Method for an NCE
259(1)
10.3.2 Stability-Indicating Method Development for an NCE Using DryLab
260(2)
10.3.3 Stability-Indicating Method for a Combination Drug Product with Two APIs
262(3)
10.3.4 Automated Method Development System Employing Fusion QbD Software
265(3)
10.4 A Three-Pronged Template Approach for Rapid HPLC Method Development
268(4)
10.4.1 Template #1: Fast LC Isocratic Potency or Performance Methods
269(1)
10.4.2 Template #2: Generic Broad Gradient Methods
270(1)
10.4.3 Template #3: Multisegment Gradient Methods for NCEs
271(1)
10.4.4 Summary of the Three-Pronged Approach
272(1)
10.5 A Universal Generic Method for Pharmaceutical Analysis
272(4)
10.5.1 Rationales for the Generic Method Parameters
272(1)
10.5.2 Adjustment of the Generic Method for Stability-Indicating Assays
273(2)
10.5.3 Summary of the Universal Generic Method Approach
275(1)
10.6 Comments on Other HPLC Modes
276(1)
10.7 Summary and Conclusions
276(1)
10.8 Quizzes
277(1)
10.8.1 Bonus Quiz
278(1)
References
278(3)
11 Regulations, HPLC System Qualification, Method Validation, and Transfer 281(24)
11.1 Introduction
281(1)
11.1.1 Scope
281(1)
11.1.2 Glossary and Abbreviations
281(1)
11.2 Regulatory Environment in the Pharmaceutical Industry
281(4)
11.2.1 Regulations
283(1)
11.2.1.1 Good Manufacturing Practice (GMP)
283(1)
11.2.1.2 International Council for Harmonization (ICH) Guidelines
283(1)
11.2.1.3 Good Laboratory Practice (GLP)
284(1)
11.2.2 The Role of the United States Food and Drug Administration (U.S. FDA)
284(1)
11.2.3 The United States Pharmacopeia (USP)
284(1)
11.3 HPLC System Qualification
285(5)
11.3.1 Design Qualification (DQ)
285(1)
11.3.2 Installation Qualification (IQ)
285(2)
11.3.3 Operational Qualification (OQ)
287(1)
11.3.4 Performance Qualification (PQ)
287(1)
11.3.5 System Qualification Documentation
287(1)
11.3.6 System Calibration
287(2)
11.3.7 System Suitability Testing (SST)
289(1)
11.4 Method Validation
290(8)
11.4.1 Data Required for Method Validation
291(5)
11.4.1.1 Specificity
291(1)
11.4.1.2 Linearity and Range
292(2)
11.4.1.3 Accuracy
294(1)
11.4.1.4 Precision: Repeatability, Reproducibility
294(1)
11.4.1.5 Sensitivity: Detection Limit and Quantitation Limit
295(1)
11.4.1.6 Robustness
296(1)
11.4.2 Case Studies and Summary Data on Method Validation
296(2)
11.5 Method Transfer
298(1)
11.6 Regulatory Filings
298(1)
11.7 Cost-Effective Regulatory Compliance Strategies
298(4)
11.7.1 Regulatory Compliance in Other Industries
301(1)
11.8 Summary and Conclusions
302(1)
11.9 Quizzes
302(1)
11.9.1 Bonus Quiz
303(1)
References
303(2)
12 HPLC and UHPLC for Biopharmaceutical Analysis 305(30)
Jennifer Rea
Taylor Zhang
12.1 Introduction
305(3)
12.2 Size-Exclusion Chromatography (SEC)
308(4)
12.2.1 SEC Introduction
308(1)
12.2.2 SEC Theory and Fundamentals
308(1)
12.2.3 SEC Method Conditions
309(2)
12.2.4 SEC Applications
311(1)
12.3 Ion-Exchange Chromatography (IEC)
312(2)
12.3.1 IEC Introduction
312(1)
12.3.2 IEC Theory and Fundamentals
313(1)
12.3.3 IEC Method Conditions
313(1)
12.3.4 IEC Applications
314(1)
12.4 Affinity Chromatography
314(3)
12.4.1 Affinity Chromatography Introduction
314(1)
12.4.2 Affinity Chromatography Theory and Fundamentals
315(1)
12.4.3 Affinity Chromatography Method Conditions
315(1)
12.4.4 Affinity Chromatography Applications
316(1)
12.5 Hydrophilic Interaction Liquid Chromatography (HILIC)
317(3)
12.5.1 HILIC Introduction
317(1)
12.5.2 HILIC Theory and Fundamentals
317(1)
12.5.3 HILIC Method Conditions
318(1)
12.5.4 HILIC Applications
318(2)
12.6 Reversed-Phase Chromatography (RPC)
320(2)
12.6.1 RPC Introduction
320(1)
12.6.2 RPC Theory and Fundamentals
320(1)
12.6.3 RPC Method Conditions
321(1)
12.6.4 RPC Applications
321(1)
12.7 Hydrophobic Interaction Chromatography (HIC)
322(2)
12.7.1 HIC Introduction
322(1)
12.7.2 HIC Theory and Fundamentals
322(1)
12.7.3 HIC Method Conditions
323(1)
12.7.4 HIC Applications
324(1)
12.8 Mixed-Mode Chromatography (MMC)
324(2)
12.8.1 MMC Introduction
324(1)
12.8.2 MMC Theory and Fundamentals
325(1)
12.8.3 MMC Method Conditions
325(1)
12.8.4 MMC Applications
325(1)
12.9 Multidimensional Liquid Chromatography
326(2)
12.9.1 Multidimensional LC Introduction
326(1)
12.9.2 Multidimensional LC Theory and Fundamentals
326(1)
12.9.3 Multidimensional LC Method Conditions
327(1)
12.9.4 Multidimensional LC Applications
327(1)
12.10 Summary
328(1)
12.11 Quizzes
328(1)
References
329(6)
13 HPLC Applications in Food, Environmental, Chemical, and Life Sciences Analysis 335(36)
13.1 Introduction
335(1)
13.1.1 Scope
335(1)
13.2 Food Applications
335(14)
13.2.1 Natural Food Components
336(5)
13.2.1.1 Sugars
336(1)
13.2.1.2 Fats, Oils, and Triglycerides
337(1)
13.2.1.3 Free Fatty Acids and Organic Acids
338(2)
13.2.1.4 Proteins and Amino Acids
340(1)
13.2.2 Food Additives
341(5)
13.2.2.1 Flavors: A Case Study on HPLC Analysis of Capsaicins
345(1)
13.2.3 Contaminants
346(3)
13.2.3.1 Mycotoxins
347(1)
13.2.3.2 Antimicrobial Additives
348(1)
13.2.3.3 Pesticide Residues
348(1)
13.3 Environmental Applications
349(3)
13.3.1 Listing of U.S. EPA Test Methods Using HPLC
349(1)
13.3.2 Pesticides Analysis
349(2)
13.3.2.1 Carbamates and Glyphosate
350(1)
13.3.3 Polynuclear Aromatic Hydrocarbons (PAH)
351(1)
13.3.3.1 Case Study: Quick Turnaround Analysis of PAHs in Multimedia Samples
351(1)
13.3.4 HPLC Analysis of Carbonyl Compounds (Aldehydes and Ketone)
352(1)
13.4 Chemical Industry, GPC, and Plastics Applications
352(4)
13.4.1 Gel-Permeation Chromatography (GPC) and Analysis of Plastics Additives
352(4)
13.5 Ion Chromatography (IC)
356(1)
13.6 Life Sciences Applications
356(10)
13.6.1 Proteins, Peptides, and Amino Acids
357(6)
13.6.2 Bases, Nucleosides, Nucleotides, Oligonucleotides, and Nucleic Acids
363(1)
13.6.3 Bioscience Research in Proteomics, Metabolomics, Glycomics and Clinical Diagnostics
363(3)
13.7 Summary
366(1)
13.8 Quizzes
366(2)
13.8.1 Bonus Questions
368(1)
References
368(3)
Keys to Quizzes 371(2)
Index 373
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.
Biežāk uzdotie jautājumi par e-grāmatām Biežāk uzdotie jautājumi par e-grāmatām
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