analytical method validation and instrument performance verification

304 Pages·2006·2.5 MB·English

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ANALYTICAL METHOD VALIDATION
AND INSTRUMENT PERFORMANCE
VERIFICATION
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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
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Copyright2004byJohnWiley&Sons,Inc.Allrightsreserved.
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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
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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
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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 [e-mail] 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 Copyright2004JohnWiley&Sons,Inc.
1