Pharmaceutical analysis for small molecules. (2017)

• Record Type: Book
• Further Information: Note: Edited by Behnam Davani.
• Editors: Davani, Behnam
• Contents: About the Editor xvi List of Contributors xviii Preface xxi Acknowledgment xxv 1 Drug Approval Process and Regulatory Requirements 1 1.1 Introduction 1 1.2 The Regulatory Process for New Drug Entity 2 1.2.1 Preclinical Studies 2 1.2.2 Investigational New Drug Application (INDA) 2 1.2.2.1 Phase 1 Clinical 2 1.2.2.2 Phase 2 Clinical 3 1.2.2.3 Phase 3 Clinical 3 1.2.3 New Drug Application (NDA) 3 1.2.3.1 NDA Review by FDA 3 1.2.3.2 NDA Review Process 4 1.3 Good Laboratory Practice for Nonclinical Laboratory Studies 5 1.4 Validation of Analytical Procedures: Methodology 6 1.5 FDA Role in the Discovery and Development of New Drug Entities 7 1.5.1 INDA Analytical Requirements 7 1.5.2 NDA Analytical Requirements 8 1.5.3 Biotechnology?]Derived Products – Small Molecules 8 1.6 FDA Inspectors’ Role in Analytics Relative to Products in the Marketplace 9 1.6.1 FDA Compliance Program Guidance Manual (Implemented on 09/11/2015 with a Completion Date of 09/11/2016 – Program 7356.002) 9 1.6.2 Guide for Inspection of Microbiological Pharmaceutical Quality Control Laboratories 10 1.6.3 Biotechnology Inspection Guide 11 1.7 Conclusions 12 References 12 2 Pharmacopeias and Compendial Approval Process 14 2.1 Introduction 14 2.2USP History 14 2.3 Evolution of the Mission of the USP 15 2.4 The USP Organization 16 2.4.1 The USP Convention 16 2.4.2 The Board of Trustees 16 2.4.3 The Council of Experts 16 2.4.4 Expert Panels to the Council of Experts 16 2.4.5 Stakeholder Forums and Project Teams 17 2.4.6 USP Staff 17 2.5 The USP-NF Revision Process 17 2.6 Publications of USP 18 2.6.1 USP?]NF 18 2.6.2 Pharmacopeial Forum 18 2.6.3 Supplements 18 2.6.4 USP Spanish Edition 18 2.6.5 USP Reference Standards 18 2.6.6 Chromatographic Columns 18 2.6.7 USP Dictionary 18 2.6.8 USP Dietary Supplements Compendium 19 2.6.9 Food Chemical Codex 19 2.6.10 USP Medicines Compendium 19 2.7 Relationship between USP and FDA 19 2.8 USP and the Pharmacopoeias of Europe and Japan 20 2.8.1 The European Pharmacopoeia 20 2.8.2 The Pharmacopeia of Japan 21 2.9 Harmonization of Pharmacopeial Monographs and General Chapters 21 2.9.1 PDG Working Procedures 22 2.9.2 Status of the Pharmacopeial Harmonization Initiative 25 2.9.3 Roles and Responsibilities of Major Stakeholders in Pharmacopeial Harmonization 28 2.9.4 The Roles and Responsibilities of Industry in Pharmacopeial Harmonization 29 2.9.5 The Roles and Responsibilities of the Regulatory Agencies in Pharmacopeial Harmonization 30 2.9.6 The Roles and Responsibilities of the International Conference on Harmonization (ICH) in Pharmacopeial Harmonization 30 2.9.7 Advantages of Pharmacopeial Harmonization 31 2.9.8 Disadvantages of Pharmacopeial Harmonization 31 2.10 Comparisons between the PDG Process and the ICH Process in Harmonization 32 2.11 The Special Case of Pharmacopeial Harmonization of Excipients 33 2.12 Retrospective versus Forward Pharmacopeial Harmonization 33 2.13 Conclusions and Recommendations 34 2.14 Final Thoughts 35 List of Abbreviations 35 References 36 3 Common Methods in Pharmaceutical Analysis 37 3.1 Scope 37 3.2 Analytical Methods 37 3.2.1 Separation Methods 37 3.2.1.1 High?]Performance Liquid Chromatography 37 3.2.1.2 Gas Chromatography 39 3.2.1.3 Thin?]Layer Chromatography 39 3.2.1.4 Supercritical Fluid Chromatography 39 3.2.1.5 Capillary Electrophoresis 40 3.3 Spectroscopy Methods 40 3.3.1 Ultraviolet 40 3.3.2 Infrared 40 3.3.3 Raman Spectroscopy 40 3.3.4 Nuclear Magnetic Resonance 41 3.3.5 Mass Spectrometry 41 3.4 Other Spectroscopy Methods 41 3.4.1 Atomic Absorption Spectroscopy and Inductively Coupled Plasma Spectroscopy 41 3.5 Wet Chemistry Methods 42 3.5.1 Titration 42 3.5.2 Loss on Drying (LOD) 42 3.5.3 Loss on Ignition (LOI) 43 3.5.4 Residue on Ignition (ROI) or Sulfated Ash 43 3.5.5 Water Determination 43 3.6 Performance Methods (Contributed by Oscar Liu) 43 3.6.1 Disintegration 43 3.6.2 Dissolution 44 3.6.3 Uniformity of Dosage Units 45 3.6.4 Aerodynamic Particle Size Distribution Analysis 46 3.7 Microbiological Methods (Contributed by Roger Dabbah) 47 3.7.1 Introduction 47 3.7.2 Microbial Limit Tests 48 3.7.2.1 Microbial Limit Tests – Enumeration via a Plate Count 48 3.7.2.2 Membrane Filtration Method 49 3.7.2.3 Most Probable Number (MPN) Procedure 49 3.7.3 Tests for Specified Microorganisms 49 3.7.4 Sterility Test 50 3.8 Critical Factors Involved in Microbial Limit Tests and in Sterility Tests 51 3.9 Harmonization of Pharmacopeial Procedures and Requirement 52 3.10 Bacterial Endotoxins Test 52 3.11 Summary 53 References 54 4 Common Calculations 58 4.1 Scope 58 4.2 Calculations (Quantitative Analysis) 58 4.2.1 Percent Loss on Drying (LOD) 58 4.2.2 Percent Loss on Ignition (LOI) 59 4.2.3 Percent Residue on Ignition (ROI) 59 4.2.4 Assay 59 4.2.4.1 Chromatography (HPLC, GC) 59 4.2.4.2 Spectroscopy (UV, IR, etc.) 61 4.2.4.3 Titration 62 4.2.4.3.1 Direct 62 4.2.4.3.2 Residual or Back Titration 62 4.2.5 Organic Impurities 63 4.2.5.1 Chromatography (HPLC, GC) 63 4.3 Calculations (System Suitability Parameters) 64 4.3.1 Resolution (R) 64 4.3.2 Tailing Factor (T) or Asymmetry Factor (As) 65 4.3.3 Number of Theoretical Plates (N) 66 4.3.4 Capacity Factor (k′) or Retention Factor (k) 67 4.4 Summary 67 References 67 5 Analytical Method Validation, Verification, and Transfer 69 5.1 Introduction 69 5.2 Scope 69 5.3 Typical Validation Characteristics 70 5.4 Definition and Determination of Analytical Characteristics 70 5.4.1 Accuracy 70 5.4.2 Precision 71 5.4.2.1 Repeatability 71 5.4.2.2 Intermediate Precision (Ruggedness) 71 5.4.2.3 Reproducibility 72 5.4.3 Specificity 72 5.4.4 Detection Limit (DL) 73 5.4.5 Quantitation Limit (QL) 74 5.4.6 Linearity 75 5.4.7 Range 75 5.5 Types of Analytical Procedures 76 5.6 Typical Validation Requirement 76 5.7 Revalidation 77 5.8 System Suitability 77 5.9 Forced Degradation (Stressed) Studies 78 5.10 Analytical Method Verification 79 5.11 Analytical Method Transfer 81 5.11.1 Comparative Testing 81 5.11.2 Co?]Validation between Labs 81 5.11.3 Revalidation 81 5.11.4 Transfer Waiver 81 5.12 Summary and Conclusion 82 References 82 6 Specifications 84 6.1 Scope 84 6.2 Introduction 84 6.3 Types of Tests 86 6.4 Types of Specifications 87 6.5 Selection of Tests and Procedures 89 6.5.1 Universal Tests 89 6.5.1.1 Drug Substances 90 6.5.1.2 New Drug Products 92 6.5.2 Specific Tests 94 6.5.2.1 Drug Substances 94 6.5.2.2 Drug Products 95 6.6 Establishing Acceptance Criteria 97 6.6.1 Rounding Rules 97 6.6.2 Statistical Estimation 98 6.6.2.1 Confidence Interval 100 <p&gt
• Edition: 1st
• Publisher Details: Hoboken, New Jersey : John Wiley & Sons, Inc
• Publication Date: 2017
• Extent: 1 online resource
• Subjects: 615.19; Drugs -- Design
• Languages: English
• ISBNs: 9781119425014; 9781119425038
• Related ISBNs: 9781119121114
• Notes: Note: Includes bibliographical references and index.; Note: Description based on CIP data; resource not viewed.
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