Handbook of Modern Pharmaceutical Analysis PDF
Preview Handbook of Modern Pharmaceutical Analysis
HANDBOOK OF MODERN PHARMACEUTICAL ANALYSIS This Is Volume III of SEPARATION SCIENCE AND TECHNOLOGY A reference series edited by Satinder Ahuja HANDBOOK OF MODERN PHARMACEUTICAL ANALYSIS Edited by Satinder Ahuja Ahuja Consulting Calabash, North Carolina Stephen Scypinski RW Johnson Pharmaceutical Research Institute Raritan, New Jersey San Diego San Francisco New York Boston London Sydney Tokyo This book is printed on acid-free paper. Copyright © 2001 by Academic Press All rights reserved. No part of this publication may be reproduced or transmitted in any form or by any means, electronic or mechanical, including photocopy, recording, or any information storage and retrieval system, without permission in writing from the publisher. The appearance of the code at the bottom of the first page of a chapter in this book indicates the Publisher’s consent that copies of the chapter may be made for personal or internal use of specific clients. This consent is given on the condition, however, that the copier pay the stated per-copy fee through the Copyright Clearance Center, Inc. (222 Rosewood Drive, Danvers, Massachusetts 01923), for copying beyond that permitted by Sections 107 or 108 of the U.S. Copyright Law. This consent does not extend to other kinds of copying, such as copying for general distribution, for advertising or promotional purposes, for creating new collective works, or for resale. Copy fees for pre-2001 chapters are as shown on the title pages; if no fee code appears on the title page, the copy fee is the same as for current chapters. 01 $35.00. The information provided in this handbook is compiled from reliable sources but the authors, editor, and the publisher cannot assume any responsibility whatsoever for the validity of all statements, illustrations, data, procedures, and other related materials contained herein or for the consequence of their use. ACADEMIC PRESS A Harcourt Science and Technology Company 525 B Street, Suite 1900, San Diego, CA 92101-4495, USA http://www.academicpress.com Academic Press Harcourt Place, 32 Jamestown Road, London, NW1 7BY, UK Library of Congress Catalog Number: 2001088201 International Standard Book Number: 0-12-045555-2 Printed in the United States of America 00 01 02 03 HP 9 8 7 6 5 4 3 2 1 CONTENTS CONTRIBUTORS xiii PREFACE xvii 1 Modern Pharmaceutical Analysis: An Overview SATINDER AHUJA I. Identity and Purity Requirements 2 II. Bioavailability/Dissolution Requirements 4 III. Regulatory Considerations 5 IV. Regulatory Compliance 8 V. International Conference on Harmonization 9 VI. Global CMC NDA 9 VII. Highlights of Modern Pharmaceutical Analysis 10 References 22 2 Combinatorial Chemistry and High-Throughput Screening in Drug Discovery and Development KEN APPELL, JOHN J. BALDWIN, AND WILLIAM J. EGAN I. Introduction 24 II. Combinatorial Methods 25 v vi CONTENTS III. Methods for Structural Assignment 26 IV. Diversity 28 V. Druglikeness 28 VI. Designing Combinatorial Libraries with Optimal ADME Properties 28 VII. Existing Computational Methods for ADME Properties 30 VIII. Optimization Philosophy 35 IX. Applying Existing ADME Models to Combinatorial Library Design 37 X. The Future of ADME Modeling 38 XI. High-Throughput Screening and Combinatorial Chemistry 39 XII. Assay Plate Formats: Move to Miniaturization 40 XIII. Nonseparation or Homogeneous Assays 43 XIV. Identification of Receptor Antagonists for Chemokine Receptor and Bradykinin-1 by Screening a 150,000-Member Combinatorial Library 44 XV. Structure-based Design of Somatostatin Agonists 47 XVI. Conclusions 48 References 49 3 Solid-State Analysis HARRY G. BRITTAIN I. Introduction 57 II. Properties Associated with the Molecular Level 58 III. Properties Associated with the Particulate Level 65 IV. Properties Associated with the Bulk Level 73 V. Summary 81 References 81 4 Degradation and Impurity Analysis for Pharmaceutical Drug Candidates KAREN M. ALSANTE, ROBERT C. FRIEDMANN, TODD D. HATAJIK, LINDA L. LOHR, THOMAS R. SHARP, KIMBERLY D. SNYDER, AND EDWARD J. SZCZESNY I. Residual Solvents and Water 86 II. Purposeful Degradation Studies 95 III. Isolation and Identification of Impurities/Degradants 119 IV. Mass Spectrometry in Identification of Impurities 127 V. Role of NMR 147 VI. Reference Standards 166 VII. Summary 168 References 168 CONTENTS vii 5 Preformulation Studies EDWARD LAU (deceased) I. Introduction 173 II. Preformulation Studies 180 III. Analytical Techniques and Instruments for Preformulation Studies 214 IV. Regulatory Requirements for Preformulation 224 V. Summary and Conclusions 226 Appendix 1 227 Appendix 2 229 Appendix 3 232 References 232 6 Solid Dosage-Form Analysis PHILIP J. PALERMO I. Introduction 235 II. Physicochemical Characterization Techniques 241 III. Near-Infrared Analysis 252 IV. Automation 257 V. Future Directions 262 VI. Summary 263 VII.Acknowledgments 263 References 263 7 Parenteral Dosage Forms GREGORY A. BIRRER, SATYA S. MURTHY, AND JIE LIU I. Characteristics of Parenteral Dosage Forms 270 II. Pharmaceutical Analysis During Formulation and Process Develop- ment 271 III. Analytical Testing for Finished Parenteral Products 272 IV. Packaging Components Testing 273 V. Process Development Support 274 VI. In-Process Testing 275 VII. Release Testing 276 VIII. Raw Material Testing 278 IX. Validation of Analytical Procedure 279 X. Stability-Indicating Methods 281 XI. Method Transfer 281 XII. Cleaning Method Validation 282 XIII. Admixture Studies 282 XIV. Microbiological Testing of Parenteral Formulations 283 XV. Sterility Testing 284 viii CONTENTS XVI. Bacterial Endotoxin Testing 290 XVII. Particulate Matter Testing 292 XVIII. Bioburden Testing of Parenteral Product Solution 294 XIX. Introduction to Cleaning Validation 298 XX. Swab Selection (Recovery and Compatability Studies) 298 XXI. Technician Qualification 298 XXII. Sampling 299 XXIII. Acceptance Criteria 300 XXIV. Methods of Analysis 301 XXV. Grouping/Matrix Approach 301 XXVI. Validation Protocol 302 XXVII. Validation Report 302 XXVIII. Summary 302 References 303 8 New Drug Delivery Systems DAVID C. PANG I. Introduction 307 II. Oral Drug Delivery 308 III. Direct Drug Delivery 310 IV. Dermatological Delivery System 311 V. Tumor-Targeted Drug Delivery Systems 311 VI. Biodegradable Drug Delivery System 313 VII. Protein Drug Delivery System 315 VIII. Devices 319 IX. Summary 323 References 323 9 Compendial Testing CHRISTINE F. RICHARDSON I. Introduction 325 II. A Brief History of the United States Pharmacopeia 326 III. Compendial Testing for Formulated Products and Active Ingredients 327 IV. Which Compendium to Use and When to Use It 340 V. Validation 340 VI. Harmonization of Testing Methods for Multicountry Submission 342 VII. Conclusions 343 VIII. Acknowledgments 344 References 344 CONTENTS ix 10 Method Development HENRIK T. RASMUSSEN I. Introduction 345 II. Overview of Separation Methods 346 III. High-Performance Liquid Chromatography 349 IV. Thin-Layer Chromatography 374 V. Gas Chromatography 375 VI. Supercritical-Fluid Chromatography 376 VII. Capillary Electrophoresis 379 VIII. Conclusions 383 IX. Summary 383 References 384 11 Setting Up Specifications IAN E. DAVIDSON I. Introduction 387 II. Setting Specifications at Different Stages of Drug Development 389 III. International Conference on Harmonization Guidelines 393 IV. Pharmacopeias and Specifications 410 V. Statistical Considerations in Setting Specifications 411 VI. Summary 412 References 412 12 Validation of Pharmaceutical Test Methods JONATHAN B. CROWTHER I. Background and Chapter Overview 415 II. Validation Terminology and Definitions 418 III. Method Development and Its Influence on Method Validation 419 IV. Validation Requirements of The Method 428 V. Validation Documentation 428 VI. Validation Experimentation 429 VII. Method Transfer 436 VIII. Revalidation 438 IX. Reference Standards 438 X. Summary 441 Acknowledgments 442 References 442 x CONTENTS 13 Stability Studies JESSICA CHA, JOSEPH S. RANWEILER, PHILIP A. LANE I. Introduction 445 II. Operational Issues 446 III. Excipients 461 IV. Drug Substance 463 V. Drug Product 471 VI. Summary 480 Glossary 480 Appendix 482 References 483 14 Analytical Methodology Transfer STEPHEN SCYPINSKI I. Introduction 485 II. The Drug Development Process 486 III. Types of Method Transfer 487 IV. Requirements and Elements of Analytical Technology Transfer 489 V. Technical Transfer Time Line/Project Plan 492 VI. Analysis of Results/Statistical Packages 493 VII. Analyst Certification and Training 494 VIII. Transfer of Technical Ownership 494 IX. Chapter Summary 497 References 497 15 Pharmaceutical Analysis Documentation HITESH CHOKSHI AND KATHLEEN SCHOSTACK I. Scope 499 II. Introduction 500 III. Pharmaceutical Analysis During Product Life Cycle 500 IV. Regulatory Documents 510 V. Compliance Documents 516 VI. Research Documents 520 VII. Summary 521 VIII. Conclusions 522 Appendix I: References for CMC Guidances 522 Appendix II: U.S. NDA Table of Contents—Analytical Documentation 525 CONTENTS xi 16 An Innovative Separation Platform: Electrophoretic Microchip Technology LIAN JI JIN, JEROME FERRANCE, ZHILI HUANG, AND JAMES P. LANDERS I. Introduction 529 II. Microchip Fabrication 531 III. Detection Techniques 535 IV. Pharmaceutical Potential 545 V. Concluding Remarks 549 VI. Summary 549 References 549 INDEX 555 This Page Intentionally Left Blank CONTRIBUTORS Numbers in parentheses indicate the pages on which the authors’ contributions begin. Satinder Ahuja (1) Ahuja Consulting, 330 Middleton Drive, Suite 803, Calabash, North Carolina 28467 Karen M. Alsante (85) Pfizer Global Research and Development Division, Ana- lytical Research and Development, P.O. Box 4077, Pfizer Inc., Eastern Point Road, Groton, Connecticut 06340 Ken Appell (23) Pharmacopeia, Inc., P.O. Box 5350, Princeton, New Jersey 08543-5350 John J. Baldwin (23) Pharmacopeia, Inc., P.O. Box 5350, Princeton, New Jersey 08543-5350 Gregory A. Birrer (269) Baxter Anesthesia Critical Care, Baxter Healthcare Medication Delivery, 95 Spring Street, New Providence, New Jersey 07974 Harry G. Brittain (57) Center for Pharmaceutical Physics, 10 Charles Road, Milford, New Jersey 08848 Jessica Cha (445) The R. W. Johnson Pharmaceutical Research Institute, P.O. Box 300, Route 202, Raritan, New Jersey, 08869 Hitesh Chokshi (499) Hoffmann-La Roche, Inc. 340, Kingsland Street, Nutley, New Jersey 07110 xiii xiv CONTRIBUTORS Jonathan B. Crowther (415) Ortho-Clinical Diagnostics, 1001 U.S. Highway 202, Raritan, New Jersey, 08869-0606 Jan E. Davidson (387) Aventis Pharmaceuticals, P.O. Box 6800, Route 202- 206, Bridgewater, New Jersey 08560 William J. Eagan (23) Pharmacopeia, Inc., P.O. Box 5350, Princeton, New Jersey 08543-5350 Judy Estrada (269) Gensia-Sicor Pharmaceuticals, 19 Hughes Street, Irvine, California 92618-1902 Jerome Ferrance (ch. 16) Department of Chemistry, University of Virginia, McCormick Road, Charlottesville, Virginia 22901 Robert C. Friedmann (85) Pfizer Global Research and Development Division, Process Research and Development, P.O. Box 4077, Pfizer Inc., Eastern Point Road, Groton, Connecticut 06340 Todd D. Hatajik (85) Pfizer Global Research and Development Division, Ana- lytical Research and Development, P.O. Box 4077, Pfizer Inc., Eastern Point Road, Groton, Connecticut 06340 Zhili Huang (529) Department of Chemistry, University of Virginia, McCormick Road, Charlottesville, Virginia 22901 Lian Ji Jin (ch. 16) Department of Chemistry, University of Virginia, McCormick Road, Charlottesville, Virginia 22901 James P. Landers (529) Department of Chemistry, University of Virginia, and Department of Pathology, University of Virginia Health Science Center, Charlottesville, Virginia 22901 Philip A. Lane (445) The R. W. Johnson Pharmaceutical Research Institute, P.O. Box 300, Route 202, Raritan, New Jersey 08869 Edward P. Lau (173) (deceased) E. L. Associates, 102 Lanark Road, Wilmington, Delaware 19807 Jie Liu (269) Baxter Anesthesia Critical Care, Baxter Healthcare Medication Delivery, 95 Spring Street, New Providence, New Jersey 07974 Linda L. Lohr (85) Pfizer Global Research and Development Division, Analyt- ical Research and Development, P.O. Box 4077, Pfizer Inc., Eastern Point Road, Groton, Connecticut 06340 Satya S. Murthy (269) Baxter Anesthesia Critical Care, Baxter Healthcare Medication Delivery, 95 Spring Street, New Providence, New Jersey 07974 Philip J. Palermo (235) Purdue Pharma L. P., 444 Saw Mill River Road, Ardsley, New York 10502 David C. Pang (307) American Association of Pharmaceutical Scientists, 2107 Wilson Boulevard, #700, Arlington, Virginia 22201-3046 Joseph S. Ranweiler (445) The R. W. Johnson Pharmaceutical Research Institute, P.O. Box 300, Route 202, Raritan, New Jersey 08869 Henrik T. Rasmussen (345) Analytical Chemistry Research and Development, The R. W. Johnson Pharmaceutical Research Institute, 1000 Route 202, Raritan, New Jersey 08869
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