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For more, Visit http://www.77169.uni.cc ANALYTICAL METHOD VALIDATION AND INSTRUMENT PERFORMANCE VERIFICATION For more, Visit http://www.77169.uni.cc 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 For more, Visit http://www.77169.uni.cc Copyright2004byJohnWiley&Sons,Inc.Allrightsreserved. PublishedbyJohnWiley&Sons,Inc.,Hoboken,NewJersey. PublishedsimultaneouslyinCanada. 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LibraryofCongressCataloging-in-PublicationData: Analyticalmethodvalidationandinstrumentperformanceverification/ ChungChowChan...[etal.]. p. ;cm. Includesbibliographicalreferencesandindex. ISBN0-471-25953-5(cloth:alk.paper) 1. Drugs—Analysis—Methodology—Evaluation. 2. Laboratories—Equipmentandsupplies—Evaluation.3. Laboratories—Instruments—Evaluation. [DNLM:1.Chemistry,Pharmaceutical—instrumentation.2. Chemistry, Pharmaceutical—methods.3. ClinicalLaboratoryTechniques—standards. 4. Technology,Pharmaceutical—methods.QV744A5322004]I.Chan, ChungChow. RS189.A5682004 610(cid:1).28—dc21 2003014141 PrintedintheUnitedStatesofAmerica. 10987654321 For more, Visit http://www.77169.uni.cc CONTENTS Contributors vii Preface ix 1 Overview of Pharmaceutical Product Development and Its Associated Quality System 1 ChungChowChanandEricJensen 2 Potency Method Validation 11 ChungChowChan 3 Method Validation for HPLC Analysis of Related Substances in Pharmaceutical Drug Products 27 Y.C.Lee 4 Dissolution Method Validation 51 ChungChowChan,NeilPearson,AnnaRebelo-Cameirao,andY.C.Lee 5 Development and Validation of Automated Methods 67 ChantalIncledonandHermanLam 6 Analysis of Pharmaceutical Inactive Ingredients 85 Xue-MingZhang 7 Validation Study of JP Heavy Metal Limit Test 95 YoshikiNishiyama v For more, Visit http://www.77169.uni.cc vi CONTENTS 8 Bioanalytical Method Validation 105 FabioGarofolo 9 Procurement, Qualification, and Calibration of Laboratory Instruments: An Overview 139 HermanLam 10 Performance Verification of UV–Vis Spectrophotometers 153 HermanLam 11 Performance Verification of HPLC 173 HermanLam 12 Operational Qualification of a Capillary Electrophoresis Instrument 187 NicoleE.Baryla 13 LC-MS Instrument Calibration 197 FabioGarofolo 14 Karl Fisher Apparatus and Its Performance Verification 221 RickJairam,RobertMetcalfe,andYu-HongTse 15 The pH Meter and Its Performance Verification 229 Yu-HongTse,RickJairam,andRobertMetcalfe 16 Qualification of Environmental Chambers 243 GilmanWongandHermanLam 17 Equipment Qualification and Computer System Validation 255 LudwigHuber 18 Validation of Excel Spreadsheet 277 HeikoBrunner Index 299 CONTRIBUTORS NicoleE. Baryla, Ph.D.,EliLillyCanada,Inc.,3650DanforthAvenue,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 LudwigHuber, Ph.D.,Agilent Technologies, Hewlett-PackardStrasse 8, 76337 Waldbronn, Germany ChantalIncledon, GlaxoSmithKlineCanada,Inc.,7333MississaugaRoad 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 viii CONTRIBUTORS Yoshiki Nishiyama, Eli Lilly Japan KK, 4-3-3 Takatsukadai, Nishi-ku, Kobe 651-2271, Japan Neil Pearson, Eli Lilly Canada, Inc., 3650 Danforth Avenue, Toronto, Ontario M1N 2E8, Canada Anna Rebelo-Cameirao, Eli Lilly Canada, Inc., 3650 Danforth Avenue, Toronto, Ontario M1N 2E8, Canada Yu-Hong Tse, Ph.D., GlaxoSmithKline Canada, Inc., 7333 Mississauga Road North, Mississauga, Ontario L5N 6L4, Canada Gilman Wong, GlaxoSmithKline Canada, Inc., 7333 Mississauga Road North, Mississauga, Ontario L5N 6L4, Canada Xue-MingZhang, Ph.D.,NovexPharma,380ElginMillsRoadEast,Richmond Hill, Ontario L4C 5H2, Canada PREFACE For pharmaceutical manufacturers to achieve commercial production of safe and effective medications requires the generation of a vast amount of reliable data duringthedevelopmentofeachproduct.Toensurethatreliabledataaregenerated in compliance with current Good Manufacturing Practices (cGMPs), all analyt- ical activities involved in the process need to follow Good Analytical Practices (GAPs).GAPscanbeconsideredastheculminationofathree-prongedapproach todatagenerationandmanagement:methodvalidation,calibratedinstrument,and training.Therequirementforthegenerationofreliabledataisveryclearlyrepre- sented in the front cover design, where the three strong pillars represent method validation, calibrated instrument, and training, respectively. Thisbookisdesignedtocovertwoofthethreepillarsofdatageneration.The chapters are written with a unique practical approach to method validation and instrument performance verification. Each chapter begins with general require- mentsandisfollowedbythestrategiesandstepstakentoperformtheseactivities. The chapter ends with the author sharing important practical problems and their solutions with the reader. I encourage you to share your experience with us, too. If you have observations or problem solutions, please do not hesitate to email them to me at chung chow [email protected] the support of the Calibration & Validation Group (CVG) in Canada, I have set up a technical solution-sharing page at the Web site www.cvg.ca. The third pillar, training, is best left to indi- vidualorganizations,asitwillbeindividualizedaccordingtoeachorganization’s strategy and culture. Themethodvalidationsectionofthisbookdiscussesandprovidesguidancefor thevalidationofcommonandnot-so-commonanalyticalmethodsthatareusedto supportdevelopmentandforproductrelease.Chapter 1givesanoverviewofthe activities from the discovery of new molecules to the launch of new products in ix x PREFACE the pharmaceutical industry. It also provides an insight into quality systems that needtobebuiltintothefundamentalactivitiesofthediscoveryanddevelopment processes. Chapters 2 to 5 provide guidance and share practical information for validation of common analytical methods (e.g., potency, related substances, and dissolutiontesting).Methodvalidationforpharmaceuticalexcipients,heavymet- als, and bioanalysis are discussed in Chapters 6 to 8. Theinstrumentperformanceverificationsectionofthebookprovidesunbiased information on the principles involved in verifying the performance of instru- mentsthatareusedforthegenerationofreliabledataincompliancewithcGMPs. The reader is given different approaches to the successful verification of instru- ment performance. The choice of which approach to implement is left to the reader based on the needs of the laboratory. Chapters 9 to 15 provide infor- mation on common analytical instruments used in the development laboratory (e.g., HPLC, UV–Vis spectrophotometers, and pH meters). Chapter 13 provides a detailed discussion of the LC-MS system, which is fast becoming a standard analyticallaboratoryinstrument.Sinceagreatportionofanalyticaldatafromthe drug development process comes from stability studies, Chapter 16 is included to provide guidance to ensure proper environmental chamber qualification. Computers have become a central part of the analytical laboratory. Therefore, wehavededicatedthelasttwochapterstoanintroductiontothisfieldofcomputer system and software validation. Chapter 17 guides quality assurance managers, lab managers, information technology personnel, and users of equipment, hard- ware, and software through the entire qualification and validation process, from writing specifications and vendor qualification to installation and to both initial and ongoing operations. Chapter 18 is an in-depth discussion of the approaches to validation of Excel spreadsheets, one of the most commonly used computer programs for automatic or semiautomatic calculation and visualization of data. Theauthorsofthisbookcomefromabroadculturalandgeographicalbaseof pharmaceuticalcompanies,vendorsandcontractmanufacturersandofferabroad perspective to the topics. I want to thank all the authors, co-editors, reviewers, and the management teams of Eli Lilly & Company, GlaxoSmithKline Canada, Inc., Patheon Canada, Inc., Novex Pharma, and Agilent Technologies who have contributed to the preparation of this book. In addition, I want to acknowledge Herman Lam for the design of the front cover, which clearly depicts the cGMP requirements for data generation. CHUNG CHOW CHAN, PH.D. 1 OVERVIEW OF PHARMACEUTICAL PRODUCT DEVELOPMENT AND ITS ASSOCIATED QUALITY SYSTEM C C C , P .D. HUNG HOW HAN H EliLillyCanada,Inc. E J , P .D. RIC ENSEN H EliLilly&Company,Indianapolis 1.1 INTRODUCTION Pharmaceutical product development consists of a series of logical and system- atic processes. When successful, the final outcome is a commercially available dosage form. However, this process can become a long and complicated pro- cess if any of the steps lose their focus. The industry has undergone many changes over the years to increase focus on efficiency and efficacy of the devel- opment process. The overall cycle of pharmaceutical product development is summarized in Figure 1.1. The clinical study of drug development is the most obvious and best known to laypersons and scientists. However, many associated behind-the-sceneactivitiesarealsoactivelypursuedinaparallelandtimelyman- ner to ensure the success of pharmaceutical product development. Clinical and commercial success cannot be achieved without successful completion of these other activities. It is important to note that the clinical phase boxes in Figure 1.1 may not be aligned exactly chronologically with other development activities. AnalyticalMethodValidationandInstrumentPerformanceVerification,EditedbyChungChow Chan,HermanLam,Y.C.Lee,andXue-MingZhang ISBN0-471-25953-5 Copyright2004JohnWiley&Sons,Inc. 1
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