validation of chromatography data systems...rsc chromatography monographs series editor: professor...

Validation of Chromatography Data SystemsEnsuring Data Integrity, Meeting Business and Regulatory Requirements2nd Edition

RSC Chromatography Monographs

Series Editor:Professor R. M. Smith, Loughborough University of Technology, UK

Titles in this Series:0: Supercritical Fluid Chromatography1: Chromatographic Integration Methods2: Packed Column SFC3: Chromatographic Integration Methods, Second Edition4: Separation of Fullerenes by Liquid Chromatography5: Applications of Solid Phase Microextraction6: HPLC: A Practical Guide7: Capillary Electrochromatography8: Hyphenated Techniques in Speciation Analysis9: Cyclodextrins in Chromatography

10: Electrochemical Detection in the HPLC of Drugs and Poisons11: Validation of Chromatography Data Systems: Meeting Business and

Regulatory Requirements12: Thin-layer Chromatography: A Modern Practical Approach13: High Temperature Liquid Chromatography: A User's Guide for Method

Development14: High Performance Chelation Ion Chromatography15: Protein and Peptide Analysis by LC-MS: Experimental Strategies16: UHPLC in Life Sciences17: Chromatography of Medicinal Plants18: Chromatographic Methods in Metabolomics19: Quantitative In Silico Chromatography: Computational Modelling of

Molecular Interactions20: Validation of Chromatography Data Systems: Ensuring Data Integrity,

Meeting Business and Regulatory Requirements

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Validation of Chromatography Data SystemsEnsuring Data Integrity, Meeting Business and Regulatory Requirements2nd Edition

R. D. McDowallR.D.McDowall Ltd, Bromley, UKEmail: [email protected]

RSC Chromatography Monographs No. 20

Print ISBN: 978-1-84973-662-6PDF eISBN: 978-1-78262-407-3EPUB eISBN: 978-1-78262-980-1ISSN: 1757-7055

A catalogue record for this book is available from the British Library

© R.D.McDowall, 2017

All rights reserved

Apart from fair dealing for the purposes of research for non-commercial purposes or for private study, criticism or review, as permitted under the Copyright, Designs and Patents Act 1988 and the Copyright and Related Rights Regulations 2003, this publication may not be reproduced, stored or transmitted, in any form or by any means, without the prior permission in writing of The Royal Society of Chemistry or the copyright owner, or in the case of reproduction in accordance with the terms of licences issued by the Copyright Licensing Agency in the UK, or in accordance with the terms of the licences issued by the appropriate Reproduction Rights Organization outside the UK. Enquiries concerning reproduction outside the terms stated here should be sent to The Royal Society of Chemistry at the address printed on this page.

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v

RSC Chromatography Monographs No. 20Validation of Chromatography Data Systems: Ensuring Data Integrity, Meeting Business and Regulatory Requirements, 2nd EditionBy R. D. McDowall© R.D.McDowall, 2017Published by the Royal Society of Chemistry, www.rsc.org

Preface to the First Edition

Why read or even buy this book?If you are using a chromatography data system (CDS) in the regulated areas

of the pharmaceutical, medical device, active pharmaceutical ingredient and contract research organisations, you will need to validate the system.

This book will be your guide through the regulations and jargon. It provides practical advice that can be used directly by you to meet regulatory requirements and allow a sustainable validation effort for your chromatogra-phy data system throughout its operational life.

However, computer validation is more than just a means of meeting regu-latory requirements. It is a strategic business tool.

● How much money has your organisation wasted on computer systems that fail to meet initial expectations or do not work? If used correctly, validation is a means of implementing the right system for the right job. Computer validation is quite simply good business practice that, if followed, provides regulatory compliance for no additional cost.

● In addition, implementing electronic signatures with electronic ways of working will allow a laboratory to exploit tangible business benefits from regulatory compliance. This requires more time spent mapping and analysing the current working process and practices but the pay-back is reduction of tedious tasks such as checking for transcription errors in the laboratory and tangible time and resource savings.

This book is intended to help the reader to validate their CDS in the

current risk based regulatory climate and is written by a chromatographer

Preface to the First Editionvi

with extensive experience of validating many different computerised systems in many different organisations since 1986.

The principles and practices of validation outlined in this book are also applicable to other types of computerised systems used in laboratories.

Bob McDowallBromley, UK

vii


Preface to the Second Edition

The importance of validation of laboratory computerised systems operat-ing in regulated laboratories has not changed and is indeed become more important since the publication of the first edition of this book. Since 2005, there has been detection of increased fraud and falsification involving chro-matography data systems, as evidenced in FDA warning letters and citations by other regulatory authorities. Coupled with this, are poor data manage-ment practices that have also resulted in increased regulatory scrutiny of these systems as often chromatographic analysis can constitute up to 100% of a GXP regulated laboratory’s workload. This results in the detailed exam-ination of the system: the validation, change control as well as the integrity of the electronic records/raw data generated.

In addition, there have been many regulatory changes since the first edition:

● A United States Pharmacopeia general chapter <1058> in 2008 on ana-lytical instrument qualification (AIQ) and a new version published in USP XXXX 1st Supplement.

● The Food and Drug Administration (FDA) has produced guidance including an updated compliance program guide for pre-approval inspections where one of the three objectives is a detailed examination of the laboratory data contained in a regulatory submission as well as data integrity guidance.

● In Europe, EU GMP 8 of the 9 main chapters of Part 1 have been revised plus Annex 11 on computerised systems and Annex 15 on qualification and validation.

● Data integrity guidance has been published by the UK regulatory agency (Medicines and Healthcare Products Regulatory Agency), the World Health Organisation, the FDA, PIC/S and EMA.

Preface to the Second Editionviii

● GAMP Forum have published the second edition of the good practice guide on risk based validation of laboratory computerised systems and an updated electronic records and data integrity guidance.

All of these documents have resulted in changes to validating and operat-ing computerised systems in general and chromatography data systems in particular as well as the way of managing the electronic records that these systems generate and process.

As a result of regulatory changes, the second edition of this book has grown from 25 to 37 chapters, (about three times the size of the first edition) and the content of each chapter is greatly expanded with more practical detail to help the reader in their task of validation and operational control of a chromatog-raphy data system. Moreover, the sub-title of the book has been amended to reflect the current regulatory interest in data integrity.

As with the first edition of this book, the principles and practical approaches described here are applicable to other computerised systems in regulated laboratories.

Bob McDowallBromley, UK

ix


Biography

Bob McDowall is an analytical chemist with over 45 years of experience. After graduating from the University of Newcastle-upon-Tyne in 1972 he completed his PhD at the Department of Forensic Medicine, London Hospital Medical College, University of London in 1977. Then, he worked for two major inter-national pharmaceutical companies working in bioanalysis for 15 years. In 1990 he was a co-chair of the first Bioanalytical Methods Validation meeting that was co-organised by the American Association of Pharmaceutical Scientists and the Food and Drug Administration. He was a co-author of the subsequent publication that was a major input into the FDA’s Guidance for Industry on the subject issued a few years later.

In 1993 he set up his consultancy practice. Initially, this was McDowall Consulting but this entity was replaced by R. D. McDowall Limited, founded in 1998.

Bob’s interests are process improvement, laboratory informatics, com-puterised system validation including Part 11 and data integrity, quality software development, interpretation of GXP regulations and laboratory automation. He is also a trained auditor working in the GLP, GMP and GCP areas.

He has published widely for over 40 years including editing the first book on LIMS in 1987 and for his work in training and advancement of the sub-ject he was presented with the 1997 LIMS Award by the LIMS Institute. Bob has written the Questions on Quality column in LC-GC Europe since 1993 and the Focus on Quality column in Spectroscopy since 2000. He is also a presenter and trainer giving many presentations and short courses in his subject areas.

Biographyx

He has been a contributor to the GAMP Good Practice Guides for IT Compli-ance (2005) and Control and Risk Based Validation of Laboratory Computerised Systems second edition (2012). Bob was a co-author of a stimulus to the revision process of United States Pharmacopoeia general chapter <1058> in January 2012 and the final version will be published in USP XXXX 1st Supplement in 2017.

xi


Acknowledgements

I would like to thank Neil Lander, Heather Longden, Loren Smith and Paul Smith for their help in obtaining figures used in this book. In addition, I appreciate the review and comment by Chris Burgess and Mark Newton during the preparation of the text.

xiii


Contents

Chapter 1 How to Use this Book 1

1.1 PurposeandScope 1 1.2 TheWayItWas… 2 1.3 TheWayItShouldBe… 3 1.4 BookStructure:LifetoDeathofaCDS 3 1.4.1 ChapterStructure 4 1.4.2 Part1:UnderstandingtheBasics 6 1.4.3 Part2:PlanningtheWork 7 1.4.4 Part3:SelectingtheSystem 8 1.4.5 Part4:Risk,Traceability,Configuration,

InstallationandIntegration 9 1.4.6 Part5:UserAcceptanceTesting 10 1.4.7 Part6:SupportingDocumentationand

SystemRelease 10 1.4.8 Part7:MaintainingtheValidationStatus 11 1.4.9 Part8:RecordsRetentionandSystem

Retirement 12 1.4.10 Part9:WhenAllElseFails:Retrospective

ValidationofaCDS 12 1.4.11 EnsuringDataIntegrity 12 1.4.12 ImportanceoftheSecondPersonReviewin

EnsuringDataIntegrity 13 1.5 UseYourOrganisation’sComputerValidation

Procedures 13 1.5.1 TerminologyUsedinthisBook 14 1.6 WhyDoesitTakesoLongtoValidateaCDS? 14 1.6.1 CDSValidation:TheWayItIs 14

Contentsxiv

1.6.2 CDSValidation:TheWayItShouldBe 14 1.6.3 TheCoreSystem 15 1.7 TenCriticalSuccessFactorsforFastCDSValidation 16 1.7.1 ManagementInvolvementandBacking 16 1.7.2 DedicatedKeyProjectTeamMembers 17 1.7.3 UseanAppropriateLifeCycleModel 17 1.7.4 KnowledgeoftheCDSApplication 18 1.7.5 ActiveandFlexibleQualityAssurance

Involvement 18 1.7.6 EffectiveandCompliantITParticipation 18 1.7.7 UsetheSupplierEffectively 19 1.7.8 Planning,PlanningandPlanning 20 1.7.9 FocusontheCoreSystem 20 1.7.10 GetMorefromLessTesting 21 1.8 Assumptions,ExclusionsandLimitations 21

Chapter 2 What is a CDS? The Past, Present and Future 22

2.1 IntroductiontoChromatographyDataSystems 22 2.2 WhatisaChromatographyDataSystem? 22 2.2.1 TypesofChromatographyDataSystem 23 2.2.2 NamingConventions 25 2.2.3 DataAcquisitionFiles 25 2.2.4 InstrumentControlFiles 26 2.2.5 SequenceFile 27 2.2.6 AcquisitionofChromatographicData 27 2.2.7 ManagementofData:DatabaseorFiles? 28 2.2.8 InterpretationofChromatographicData 28 2.2.9 SystemSuitabilityTest(SST)Calculations 30 2.2.10 Calibration 30 2.2.11 UserDefinedAnalyticalRunParameters 31 2.2.12 CollationofResultsandReports 32 2.2.13 ArchitectureofaNetworkedCDS 32 2.3 EvolutionofChromatographyDataSystems 33 2.3.1 CDS:WhereHaveWeComeFrom? 33 2.3.2 TheEvolutionaryAgesofCDS 34 2.4 StoneAge:PaperBasedPeakMeasurement

Techniques 35 2.4.1 CutandWeigh 36 2.4.2 RulerandPencil 36 2.4.3 DiskIntegrator 37 2.4.4 SummaryofStoneAgeCDS 37 2.5 BronzeAge:ElectronicPeakMeasurement 38 2.5.1 CentralDataSystems 38 2.5.2 ComputingIntegrators 38 2.5.3 SummaryofBronzeAgeCDS 39

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