《仪器与方法验证专著》（英文版） Analytical Method Validation and Instrument Performance veriticatig

Analvtical Mether Instrument Perfomance eriticatio RELIABLE DATA Edited b RTI

ANALYTICAL METHOD VALIDATION AND INSTRUMENT PERFORMANCE Ⅴ ERIFICATION Edited by CHUNG CHOW CHAN Eli Lilly canada, Inc HERMAN LAM GlaxoSmithKline Canada, Inc Y.C. LEE Patheon YM. Inc. XUE-MING ZHANG Novex pharma WILEY- INTERSCIENCE A JOHN WILEY sons. INc.. publication

ANALYTICAL METHOD VALIDATION AND INSTRUMENT PERFORMANCE VERIFICATION Edited by CHUNG CHOW CHAN Eli Lilly Canada, Inc. HERMAN LAM GlaxoSmithKline Canada, Inc. Y. C. LEE Patheon YM, Inc. XUE-MING ZHANG Novex Pharma A JOHN WILEY & SONS, INC., PUBLICATION

ANALYTICAL METHOD VALIDATION AND INSTRUMENT PERFORMANCE VERIFICATION

ANALYTICAL METHOD VALIDATION AND INSTRUMENT PERFORMANCE VERIFICATION

ANALYTICAL METHOD VALIDATION AND INSTRUMENT PERFORMANCE Ⅴ ERIFICATION Edited by CHUNG CHOW CHAN Eli Lilly canada, Inc HERMAN LAM GlaxoSmithKline Canada, Inc Y.C. LEE Patheon YM. Inc. XUE-MING ZHANG Novex pharma WILEY- INTERSCIENCE A JOHN WILEY sons. INc.. publication

ANALYTICAL METHOD VALIDATION AND INSTRUMENT PERFORMANCE VERIFICATION Edited by CHUNG CHOW CHAN Eli Lilly Canada, Inc. HERMAN LAM GlaxoSmithKline Canada, Inc. Y. C. LEE Patheon YM, Inc. XUE-MING ZHANG Novex Pharma A JOHN WILEY & SONS, INC., PUBLICATION

Copyright o 2004 by John Wiley Sons, Inc. All rights reserve Published by John Wiley Sons, Inc, Hoboken, New Jersey Published simultaneously in Canada. No part of this publication may be reproduced, stored in a retrieval system, or transmitted in any form or by any means, electronic, mechanical, photocopying, recording, scanning, or otherwise, cept as permitted under Section 107 or 108 of the 1976 United States Copyright Act, without either the prior written permission of the Publisher, or authorization through payment of the appropriate per-copy fee to the Copyright Clearance Center, Inc, 222 Rosewood Drive, Danvers, Ma01923,978-750-8400,fax978-646-8600,oronthewebatwww.copyright.com.Requeststo the Publisher for permission should be addressed to the Permissions Department, John Wiley Sons, Inc, 111 River Street, Hoboken, NJ 07030,(201)748-6011, fax(201)748-6008. Limit of Liability/Disclaimer of Warranty: While the publisher and author have used their best efforts in preparing this book, they make no representations or warranties with respect to the accuracy or completeness of the contents of this book and specifically disclaim any implied warranties of merchantability or fitness for a particular purpose. No warranty may be created or extended by sales repres presentatives or written sales materials. The advice and strategies contained herein may not be suitable for your situation. You should consult with a professional where appropriate. Neither the publisher nor author shall be liable for any loss of profit or any other commercial damages, including but not limited to special, incidental, consequential, or other damages. For general information on our other products and services please contact our Customer Care Department within the U.S. at 877-762-2974, outside the U.S. at 317-572-3993 or fax317-572-4002 wiley also publishes its books in a variety of electronic formats. Some content that appears in print, however, may not be available in electronic format. Library of Congress Cataloging-in-Publication Data: Analytical method validation and instrument performance verification Chung Chow Chan... et al. J Includes bibliographical references and index. ISBN 0-471-259535(cloth: alk. 1. Drugs-Analysis-Methodology-Evaluation. 2. Laboratories-Equipment and supplies-Evaluation. 3. Laboratories-Inst ts-Evaluation DNLM: 1. Chemistry, Pharmaceutical-instrumentation. 2. Chemistry, Pharmaceutical-methods. 3. Clinical Laboratory Techniques-standards 4. Technology, Pharmaceutical-methods QV 744 A532 2004]I Chan, RS189A5682004 61028-dc21 2003014141 Printed in the United States of America

Copyright  2004 by John Wiley & Sons, Inc. All rights reserved. Published by John Wiley & Sons, Inc., Hoboken, New Jersey. Published simultaneously in Canada. No part of this publication may be reproduced, stored in a retrieval system, or transmitted in any form or by any means, electronic, mechanical, photocopying, recording, scanning, or otherwise, except as permitted under Section 107 or 108 of the 1976 United States Copyright Act, without either the prior written permission of the Publisher, or authorization through payment of the appropriate per-copy fee to the Copyright Clearance Center, Inc., 222 Rosewood Drive, Danvers, MA 01923, 978-750-8400, fax 978-646-8600, or on the web at www.copyright.com. Requests to the Publisher for permission should be addressed to the Permissions Department, John Wiley & Sons, Inc., 111 River Street, Hoboken, NJ 07030, (201) 748-6011, fax (201) 748-6008. Limit of Liability/Disclaimer of Warranty: While the publisher and author have used their best efforts in preparing this book, they make no representations or warranties with respect to the accuracy or completeness of the contents of this book and specifically disclaim any implied warranties of merchantability or fitness for a particular purpose. No warranty may be created or extended by sales representatives or written sales materials. The advice and strategies contained herein may not be suitable for your situation. You should consult with a professional where appropriate. Neither the publisher nor author shall be liable for any loss of profit or any other commercial damages, including but not limited to special, incidental, consequential, or other damages. For general information on our other products and services please contact our Customer Care Department within the U.S. at 877-762-2974, outside the U.S. at 317-572-3993 or fax 317-572-4002. Wiley also publishes its books in a variety of electronic formats. Some content that appears in print, however, may not be available in electronic format. Library of Congress Cataloging-in-Publication Data: Analytical method validation and instrument performance verification / Chung Chow Chan ...[et al.]. p. ; cm. Includes bibliographical references and index. ISBN 0-471-25953-5 (cloth : alk. paper) 1. Drugs—Analysis—Methodology—Evaluation. 2. Laboratories—Equipment and supplies—Evaluation. 3. Laboratories— Instruments—Evaluation. [DNLM: 1. Chemistry, Pharmaceutical—instrumentation. 2. Chemistry, Pharmaceutical—methods. 3. Clinical Laboratory Techniques—standards. 4. Technology, Pharmaceutical—methods. QV 744 A532 2004] I. Chan, Chung Chow. RS189.A568 2004 610
.28—dc21 2003014141 Printed in the United States of America. 10 9 8 7 6 5 4 3 2 1

CONTENTS Contributors 1 Overview of Pharmaceutical Product Development and Its Associated Quality System Chung Chow Chan and Eric Jensen 2 Potency Method validation Chung Chow Chan 3 Method Validation for HPLC Analysis of Related Substances in Pharmaceutical drug products Y. C. Lee 4 Dissolution Method validation Chung Chow Chan, Neil Pearson, Anna Rebelo-Cameirao, and Y. C. Lee 5 Development and Validation of Automated Methods Chantal incledon and herman lam 6 Analysis of Pharmaceutical Inactive Ingredients Xue-Ming Zhang 7 Validation Study of JP Heavy Metal limit Test Yoshiki Nishino

CONTENTS Contributors vii Preface ix 1 Overview of Pharmaceutical Product Development and Its Associated Quality System 1 Chung Chow Chan and Eric Jensen 2 Potency Method Validation 11 Chung Chow Chan 3 Method Validation for HPLC Analysis of Related Substances in Pharmaceutical Drug Products 27 Y. C. Lee 4 Dissolution Method Validation 51 Chung Chow Chan, Neil Pearson, Anna Rebelo-Cameirao, and Y. C. Lee 5 Development and Validation of Automated Methods 67 Chantal Incledon and Herman Lam 6 Analysis of Pharmaceutical Inactive Ingredients 85 Xue-Ming Zhang 7 Validation Study of JP Heavy Metal Limit Test 95 Yoshiki Nishiyama v

CONTENTS 8 Bioanalytical Method validation 9 Procurement, Qualification, and Calibration of Laboratory Instruments: An Overview 139 He 10 Performance Verification of UV-Vis Spectrophotometers Herman lam 11 Performance verification of hIPlc 173 Herman lam 12 Operational Qualification of a Capillary Electrophoresis Instrume Nicole E. Baryla 3 LC-MS Instrument Calibration 197 Fabio garofolo 14 Karl Fisher Apparatus and Its Performance Verification Rick Jairam, Robert Metcalfe, and Yu-Hong Tse 15 The pH Meter and Its Performance verification ll-Hong Tse, Rick Jairam, and robert metcalfe 16 Qualification of Environmental Chambers Gilman Wong and Herman Lam 17 Equipment Qualification and Computer System Validation Ludwig huber 18 Validation of Excel Spreadshe Index

vi CONTENTS 8 Bioanalytical Method Validation 105 Fabio Garofolo 9 Procurement, Qualification, and Calibration of Laboratory Instruments: An Overview 139 Herman Lam 10 Performance Verification of UV–Vis Spectrophotometers 153 Herman Lam 11 Performance Verification of HPLC 173 Herman Lam 12 Operational Qualification of a Capillary Electrophoresis Instrument 187 Nicole E. Baryla 13 LC-MS Instrument Calibration 197 Fabio Garofolo 14 Karl Fisher Apparatus and Its Performance Verification 221 Rick Jairam, Robert Metcalfe, and Yu-Hong Tse 15 The pH Meter and Its Performance Verification 229 Yu-Hong Tse, Rick Jairam, and Robert Metcalfe 16 Qualification of Environmental Chambers 243 Gilman Wong and Herman Lam 17 Equipment Qualification and Computer System Validation 255 Ludwig Huber 18 Validation of Excel Spreadsheet 277 Heiko Brunner Index 299

CONTRIBUTORS Nicole E. Baryla, Ph. D, Eli Lilly Canada, Inc, 3650 Danforth Avenue, Toronto Ontario min 2E8. Canada Heiko Brunner, Ph. D, Lilly Forschung GmbH, Essener Strasse 93, D-22419 Hamburg, Germany Chung Chow Chan, Ph. D, Eli Lilly Canada, Inc, 3650 Danforth Avenue Toronto Ontario min 2E8. Canada Fabio Garofolo, Ph. D, Vicuron Pharmaceuticals, Inc, via R. Lepetit 34 1-21040 Gerenzano, italy Ludwig Huber, Ph. D, Agilent Technologies, Hewlett-Packard Strasse 8, 76337 Waldbronn, Germany Chantal Incledon, GlaxoSmithKline Canada, Inc, 7333 Mississauga Road North Mississauga, Ontario L5n 6L4, Canada Rick Jairam, Glaxo SmithKline Canada, Inc, 7333 Mississauga Road North, Mississauga, Ontario L5n 6L4, Canada Eric Jensen, Ph. D, Eli Lilly Company, Indianapolis, IN Herman Lam, Ph D. GlaxoSmithKline Canada. Inc.. 7333 Mississauga Road North. Mississauga. Ontario lsn 6L4 Canada Y C. Lee, Ph D. Patheon YM, Inc. 865 York Mills Road, toronto, Ontario M3B lY5. Canada Robert Metcalfe, Ph. D, GlaxoSmithKline Canada, Inc, 7333 Mississauga Road North. Mississauga. Ontario Lsn 6L4 Canada

CONTRIBUTORS Nicole E. Baryla, Ph.D., Eli Lilly Canada, Inc., 3650 Danforth Avenue, Toronto, Ontario M1N 2E8, Canada Heiko Brunner, Ph.D., Lilly Forschung GmbH, Essener Strasse 93, D-22419 Hamburg, Germany Chung Chow Chan, Ph.D., Eli Lilly Canada, Inc., 3650 Danforth Avenue, Toronto, Ontario M1N 2E8, Canada Fabio Garofolo, Ph.D., Vicuron Pharmaceuticals, Inc., via R. Lepetit 34, I-21040 Gerenzano, Italy Ludwig Huber, Ph.D., Agilent Technologies, Hewlett-Packard Strasse 8, 76337 Waldbronn, Germany Chantal Incledon, GlaxoSmithKline Canada, Inc., 7333 Mississauga Road North, Mississauga, Ontario L5N 6L4, Canada Rick Jairam, GlaxoSmithKline Canada, Inc., 7333 Mississauga Road North, Mississauga, Ontario L5N 6L4, Canada Eric Jensen, Ph.D., Eli Lilly & Company, Indianapolis, IN Herman Lam, Ph.D., GlaxoSmithKline Canada, Inc., 7333 Mississauga Road North, Mississauga, Ontario L5N 6L4, Canada Y.C. Lee, Ph.D., Patheon YM, Inc., 865 York Mills Road, Toronto, Ontario M3B 1Y5, Canada Robert Metcalfe, Ph.D., GlaxoSmithKline Canada, Inc., 7333 Mississauga Road North, Mississauga, Ontario L5N 6L4, Canada vii