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A comprehensive guide to validating analytical methods for. pharmaceutical analysis Validation, Methods which are used for the analysis of pharmaceuticals generate critical data. and it is essential that the quality of this data is assured Validation is required to. demonstrate that these analytical methods are fit for their intended purpose of. Validation data is also required by legislation it is included in submissions to. regulatory authorities all around the world for clinical trial and marketing. applications This book provides guidance on how to carry out a validation. study for analytical methods,Key features include,Analytical. Full review of the available regulatory guidelines on validation and in. particular those from the International Conference on Harmonisation. ICH Sections of the guideline Q2 R1 have been reproduced in this. book with the kind permission of the ICH Secretariat. Thorough discussion of each of the validation characteristics Specificity. Linearity Range Accuracy Precision Detection Limit Quantitation Limit. Robustness System Suitability plus practical tips on how they may be. What to include in a validation protocol with advice on the experimental for. procedure to follow and selection of appropriate acceptance criteria. Validation of Analytical Methods for Pharmaceutical Analysis. How to interpret and calculate the results of a validation study including. the use of suitable statistical calculations Pharmaceutical. A fully explained case study demonstrating how to plan a validation study. what to include in the protocol experiments to perform setting acceptance. criteria interpretation of the results and reporting the study. Oona McPolin BSc MSc CSci CChem MRSC is the training services manager. of Mourne Training Services a training consultancy which provides training. solutions for pharmaceutical analysis She is also a part time college lecturer. This book is based on experience gained from working in the pharmaceutical. industry for over 10 years and from the design and delivery of effective training. courses relating to analytical chemistry and the validation of analytical methods. OONA McPOLIN,OONA McPOLIN,Copyright 2009 Mourne Training Services. The right of Oona McPolin to be identified as the author of this work has been asserted by. her in accordance with the Copyright Designs and Patents act 1988. 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. Mourne Training Services, 14 Burren Road Warrenpoint Co Down Northern Ireland BT34 3SA United Kingdom. Tel 44 0 28 30268236,Email info mournetrainingservices co uk.
Web www mournetrainingservices co uk,ISBN 978 0 9561528 1 7. This book provides guidance on how to perform validation for the analytical methods. which are used in pharmaceutical analysis Validation of the analytical methods which. are used during drug development and drug manufacturing is required to demonstrate. that the methods are fit for their intended purpose Additionally the pharmaceutical. industry around the world is subject to extensive regulations due to the nature of its. products Validation is a regulatory requirement and the data generated during an. analytical method validation study is included in submissions to regulatory authorities. for clinical trial and marketing applications, The definitive reference for this topic is the guideline produced by the International. Conference on Harmonisation of Technical Requirements for Registration of. Pharmaceuticals for Human Use ICH Q2 R1 Validation of Analytical Procedures. Text and Methodology Sections of the guideline have been reproduced in this book. with the kind permission of the ICH Secretariat All ICH guidelines are available via. the website www ich org and thus the validation guideline may be easily checked for. The guidance in this book is primarily aimed at analytical methods for small molecules. Reference is made to validation of methods for pharmaceuticals of biological origin. such as proteins and peptides In principle the ICH guidelines should be applied to. these types of compounds however it is acknowledged they present particular. challenges during validation in particular relating to biological assays The references. provided in Chapter 1 provide more information on the validation of analytical. methods for biopharmaceuticals biotechnology derived products. At the back of the book there is a glossary to help the reader become familiar with the. terminology used in analytical method validation When a new term is introduced it is. shown in bold to indicate to the reader that a definition is available in the glossary In. the appendix there is a list of abbreviations and also a question section so that the. reader can test their understanding of the content. Oona McPolin,INTRODUCTION 1,Validation in the Pharmaceutical Industry 1. Data Quality 1,Analytical Instrument Qualification AIQ 2. The Purpose of an Analytical Method 3,The life cycle of an analytical method 4.
Validation Guidelines 5,Types of Analytical Methods 6. Universal tests 6, Analytical methods not included in the ICH guidelines 8. Analytical techniques 9,Validation Characteristics 10. Specificity 10,Accuracy 10,Precision 10,Detection Limit 11. Quantitation Limit 11,Linearity 11,Robustness 11,References 12.
Further reading 14,VALIDATION CHARACTERISTICS 17,Validation during Method Development 17. Statistics in Analytical Method Validation 18,Standard deviation 18. Confidence intervals 19,Specificity 22,Specificity and selectivity 23. Identification methods 23,Assay and impurity methods 24. Bioanalytical methods 26,Other methods 26,Linearity 27.
Verification of the calibration model 27,Regression analysis 29. Assay and impurity methods 34,Bioanalytical methods 34. Accuracy 37,Impurities 40,Other methods 41,Precision 42. Precision levels 43,System precision 43,Measurement of precision 43. Repeatability 44,Intermediate precision 46,Reproducibility 47.
Accuracy trueness and precision 49,Detection Limit 50. Quantitation Limit 53,Robustness 55,Robustness during method development 59. Robustness during the validation study 60,Solution stability evaluation 64. System Suitability 65,References 67,Further Reading 70. THE VALIDATION PROTOCOL 73,Contents of the Validation Protocol 73.
Validation Characteristics to be Studied 74,Experimental Procedure and Acceptance Criteria 75. Specificity 75,Linearity 76,Accuracy 77,Precision 78. Detection Limit and Quantitation Limit 79,Robustness 80. Stability 80,Validation Protocol by Type of Method 81. Identification 81,Impurities 83,Bioanalytical methods 86.
Other methods 87,Validation of methods in Pharmacopoeias 87. Automated methods 87,Validation by Phase of Development 88. Validation Software 90,Planning and Execution of the Validation Study 90. Review the timing and resources required 90, Determine the most efficient order of experiments 91. Execute the study 92,Documentation 92,Case Study 93.
Planning and execution of the study 99,References 102. Further reading 104,THE VALIDATION REPORT 107,Contents of the Validation Report 107. Statistics in Analytical Method Validation 108,Statistical significance 108. Comparative studies 108,Outliers 110,Results for Each Validation Characteristic 112. Specificity 112,Linearity 113,Accuracy 113,Precision 113.
Detection Limit and Quantitation Limit 114,Robustness 114. Stability 114,Results to include in the validation report 115. Non compliance with acceptance criteria 117,Documentation 117. Revalidation 117,Case Study 119,References 125,Further reading 125. GLOSSARY 129,LIST OF ABBREVIATIONS 137,Introduction.
alidation is defined as finding or testing the truth of something When. analytical methods are used to generate results about the characteristics of. drug related samples it is vital that the results are trustworthy they may be. used as the basis for decisions relating to administering the drug to patients A. validation study is performed on an analytical method to ensure that reliable results are. always obtained,Validation in the Pharmaceutical Industry. Analytical method validation is just one type of validation required during drug. development and manufacturing To comply with the requirements of current Good. Manufacturing Practices GMP 1 3 pharmaceutical companies should have an overall. validation policy which documents how validation will be performed This will. include the validation of production processes cleaning procedures analytical. methods in process control test procedures and computerised systems The purpose. of this validation is to show that processes involved in the development and. manufacture of drugs such as production cleaning and analytical testing can be. performed in an effective and reproducible manner, The reason that validation is included in cGMP in this way is to ensure that quality is. built in at every step and not just tested for at the end Validation is intended to. provide assurance of the quality of a system or process through a quality methodology. for the design manufacture and use of that system or process that cannot be found. by simple testing alone 4,Data Quality, The quality of analytical data is assured by the combination of a number of critical. components as shown in Figure 1 In the data quality triangle5 the components are. layered each layer adds to the overall quality of the data The base of the triangle is. Analytical Instrument Qualification AIQ this is documented evidence that an. instrument performs suitably for its intended purpose and that it is properly. maintained and calibrated The next layer is analytical method validation the subject. of this book This is documented evidence that demonstrates that the analytical. method is suitable for its intended use The top layers of the triangle are system. 2009 Mourne Training Services 1, T H E V A L I D A T I O N O F A N A L Y T I C A L M E T H O D S. suitability tests and quality control checks these are used to demonstrate that the. combination of system and method performed as expected at the time of the analysis. System suitability tests are commonly used for chemical analyses which are usually. subject to GMP regulations and quality control checks are commonly used for. bioanalytical analyses which are usually subject to GLP regulations Overall AIQ and. analytical method validation assure the quality before the analysis is performed and. system suitability tests and quality control checks assure the quality immediately before. or during the analysis, Figure 1 Data quality triangle from Basal et al in AAPS PharmSciTech5.
Control Checks,System Suitability Tests,Analytical Method Validation. Analytical Instrument Qualification,Analytical Instrument Qualification AIQ. The equipment which is used for all types of validation related to drug development. and manufacture needs to be qualified In the case of analytical methods this refers to. the analytical instrumentation required to perform the test Analytical method. validation must be performed on appropriately qualified instruments. The qualification procedure is usually carried out in four stages during which all. actions are documented5 6 These are,Design Qualification DQ. This covers all procedures prior to the installation of the system in the selected. environment The DQ defines the functional and operational specifications of the. instrument and details the conscious decisions in the selection of the supplier For. commercial off the shelf COTS analytical instrumentation users generally have very. little input into the design of the instrument and thus the DQ will detail the user. requirements and the rationale for the selection of a particular supplier For custom. designed analytical instrumentation the DQ details the key features of the design and. how they address the user requirements,2009 Mourne Training Services 2. I N T R O D U C T I O N,Installation Qualification IQ.
This covers all the procedures relating to the installation of the instrument in the. selected environment The IQ establishes that the instrument is received as designed. and specified that it is properly installed in the selected environment and that this. environment is suitable for the operation and use of the instrument The IQ may be. carried out by the supplier and or the user For some complex instrumentation it may. have to be performed by the supplier,Operational Qualification OQ. This is the process of demonstrating that an instrument will function according to its. operational specification in the selected environment The OQ usually takes place. after the IQ of a new instrument or after a change to the instrument such as repair or. change of location As with the IQ the OQ may be carried out by the supplier. and or the user IQ OQ is now offered by most suppliers of analytical. instrumentation when a new instrument is purchased. Performance Qualification PQ, This is defined as the process of demonstrating that an instrument consistently. analytical methods are used to generate results about the characteristics of drug related samples it is vital that the results are trustworthy they may be used as the basis for decisions relating to administering the drug to patients

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