The Fitness for Purpose of Analytical Methods

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Eurachem Guide,The Fitness for Purpose of Analytical Methods. A Laboratory Guide to Method Validation and Related Topics. Second edition,Acknowledgements, This document has been produced by members of the Eurachem Method Validation Working Group and others. co opted for this task Those who have contributed to this edition are listed below. Project group,Vicki Barwick LGC UK, Pedro P Morillas Bravo Canal de Isabel II Gesti n ES. Stephen L R Ellison LGC UK,Joakim Engman National Food Agency SE. Elin L F Gjengedal Norwegian University of Life Sciences NO. Ulla Oxenb ll Lund Eurofins Milj A S DK, Bertil Magnusson editor SP Technical Research Institute of Sweden SE.
Hans Thomas M ller Mersin TR,Marina Patriarca Istituto Superiore di Sanit IT. Barbara Pohl Merck KGaA DE,Piotr Robouch European Commission EU. Lorens P Sibbesen chairman Labquality International DK. Elvar Theodorsson University Hospital in Link ping SE. Florent Vanstapel University Hospital Leuven Leuven BE. Isabelle Vercruysse BELAB BE, Aysun Yilmaz Cevre Food and Industrial Analysis Laboratory TR. Perihan Yolci meroglu Okan University TR,Ulf rnemark editor Emendo Dokumentgranskning SE. Copyright of this document is held by the contributing authors All enquiries regarding reproduction in any. medium including translation should be directed to the Eurachem secretariat The text may not be copied for. Recommended citation, This publication should be cited as B Magnusson and U rnemark eds Eurachem Guide The Fitness for.
Purpose of Analytical Methods A Laboratory Guide to Method Validation and Related Topics 2nd ed 2014. ISBN 978 91 87461 59 0 Available from www eurachem org. Subject to journal requirements, The Fitness for Purpose of Analytical Methods Eurachem Guide. Foreword to the second edition 1,Foreword to the first edition 2. Abbreviations and symbols 3,1 Introduction 5,1 1 Rationale and scope for this Guide 5. 1 2 Notes on the use of this Guide 5,1 2 1 Terminology 5. 1 2 2 Quick References 6,2 What is method validation 7.
2 1 Definitions 7, 2 2 What is the difference between validation and verification 7. 3 Why is method validation necessary 9,3 1 Importance of analytical measurement 9. 3 2 The professional duty of the analytical chemist 9. 3 3 Method development 9,4 When should methods be validated or verified 11. 4 1 Method validation 11,4 2 Method verification 11. 5 How should methods be validated 13,5 1 Who carries out method validation 13.
5 1 1 Approaches to method validation 13,5 1 2 Interlaboratory approach 13. 5 1 3 Single laboratory approach 13,5 2 Extent of validation studies 13. 5 3 Validation plan and report 14,5 4 Validation tools 15. 5 4 1 Blanks 15,5 4 2 Routine test samples 15,5 4 3 Spiked materials solutions 15. 5 4 4 Incurred materials 15,5 4 5 Measurement standards 15.
5 4 6 Statistics 16,5 5 Validation requirements 16. 5 6 Method validation process 16,6 Method performance characteristics 19. 6 1 Selectivity 19,6 1 1 Terms and definitions 19,6 1 2 Effects of interferences 19. 6 1 3 Assessment of selectivity 19, The Fitness for Purpose of Analytical Methods Eurachem Guide. 6 2 Limit of detection and limit of quantification 20. 6 2 1 Terms and definitions 20, 6 2 2 Determination of the standard deviation at low levels 21.
6 2 3 Estimating LOD 24,6 2 4 Estimating LOQ 24,6 2 5 Alternative procedures 25. 6 2 6 Capability of detection for qualitative analysis 25. 6 3 Working range 27,6 3 1 Definition 27,6 3 2 Considerations for the validation study 27. 6 3 3 Method and instrument working range 27,6 3 4 Assessing instrument working range 27. 6 3 5 Assessing method working range 28,6 4 Analytical sensitivity 30. 6 4 1 Definition 30,6 4 2 Applications 30,6 5 Trueness 30.
6 5 1 Terminology to describe measurement quality 30. 6 5 2 Determination of bias 31,6 5 3 Interpreting bias measurements 34. 6 6 Precision 35,6 6 1 Replication 35,6 6 2 Precision conditions 35. 6 6 3 Precision limits 36, 6 6 4 Simultaneous determination of repeatability and intermediate precision 36. 6 7 Measurement uncertainty 38,6 8 Ruggedness 38,6 8 1 Definition 38. 6 8 2 Ruggedness test 38,7 Using validated methods 41.
8 Using validation data to design quality control 43. 8 1 Introduction 43,8 2 Internal quality control 43. 8 3 External quality control 44,9 Documentation of validated methods 45. 9 1 From draft to final version 45,9 2 Recommendations 45. 9 2 1 Checking the instructions 45,9 2 2 Recommendations in standards 45. 9 2 3 Document control 45, 10 Implications of validation data for calculating and reporting results 47.
Annex A Method documentation protocol 49, Annex B Statistical basis of limit of detection calculations 53. Annex C Analysis of variance ANOVA 54,Annex D Notes on qualitative analysis 56. Bibliography 59, The Fitness for Purpose of Analytical Methods Eurachem Guide. Foreword to the second edition, Since the first edition of this Guide in 1998 a number of important developments in analytical quality. have taken place Firstly the ISO 9000 series of standards which is widely used to provide a basis for. a quality management system has been revised Its philosophy forms an integral part of international. conformity assessment standards and guides which underpins competence requirements for. laboratories proficiency testing PT providers and reference material RM producers These. documents all stress the importance of using validated methods. Secondly several general or sector specific guides on method validation have been revised or. developed EU legislation contains mandatory requirements for analytical measurements in many. Thirdly much effort has been invested by the analytical community in implementing the uncertainty. concept For example in its Harmonized guidelines for single laboratory validation of methods of. analysis 2002 IUPAC predicted that with an increasing reliance on measurement uncertainty as a. key indicator of both fitness for purpose and reliability of results analytical chemists will increasingly. undertake measurement validation to support uncertainty estimation In the following years. accreditation bodies issued policies and guidance documents clearly recognising the use of method. validation data in the measurement uncertainty estimation process. Furthermore the International vocabulary of metrology Basic and general concepts and associated. terms VIM has been substantially revised taking into account chemical and biological. measurements Although terminology related to method validation is far from harmonised the. situation has improved VIM is also a normative document for laboratories accredited to e g ISO IEC. 17025 and ISO 15189, The second edition of this Guide aims to reflect changes in international standards and guidance.
documents and puts less emphasis on terms and definitions Instead the Guide refers to the VIM and. other readily available sources As a consequence the list of terms and definitions has been omitted. from the Annex Literature cited in this edition of this Guide are listed in the Bibliography at the end. Additional sources and literature related to method development and validation is available as a. Reading list under the menu item Publications on the Eurachem website at www eurachem org. Annex A is revised as a consequence of changes to ISO 78 2 This edition has also been extended to. include information on the statistical basis of limit of detection calculations Annex B analysis of. variance Annex C and qualitative analysis Annex D, It is becoming increasingly common among routine laboratories especially in the clinical sector to. use commercially available measuring systems This means that the responsibility for validation. mainly lies with the manufacturer The laboratory s work will focus on verifying the manufacturer s. published performance data and demonstrate that the method works on the end user s premises. However looking back to the foreword to the first edition we conclude that the six principles stated. there are still relevant and are consistent with the requirements of international standards such as. ISO IEC 17025, The Fitness for Purpose of Analytical Methods Eurachem Guide. Foreword to the first edition, An initiative in the UK to promote good practice in analytical measurement has identified six. principles of analytical practice which taken together are considered to constitute best practice The. six principles which are described in more detail in a separate guide are. 1 Analytical measurements should be made to satisfy an agreed requirement i e to a defined. 2 Analytical measurements should be made using methods and equipment which have been. tested to ensure they are fit for purpose, 3 Staff making analytical measurements should be both qualified and competent to undertake. the task and demonstrate that they can perform the analysis properly. 4 There should be a regular independent assessment of the technical performance of a. laboratory, 5 Analytical measurements made in one location should be consistent with those made.
6 Organisations making analytical measurements should have well defined quality control and. quality assurance procedures, These principles are equally relevant to laboratories whether they are working in isolation or. producing results which need to be compared with those from other laboratories. This document is principally intended to assist laboratories in implementing Principle 2 by giving. guidance on the evaluation of testing methods to show that they are fit for purpose. The first edition 1998 of this Guide was developed by a Eurachem Working Group from a draft originally. produced by LGC The following persons were members of the Eurachem group at that time. D Holcombe P De Bi vre D B ttger C Eastwood J Hlavay M Holmgren W Horwitz M Lauwaars B. Lundgren L Massart J Miller J Morkowski B te Nijenhuis B Nyeland R Philipp P Radvila J Smeyers. Verbeke R Stephany M Suchanek C Vandervoorst H Verplaetse H Wallien M Walsh W Wegscheider. D Westwood H J van de Wiel, The manager s guide to VAM UK Department of Trade and Industry Valid Analytical Measurement. Programme Published as VAM Principles M Sargent Anal Proc 1995 32 201 202. The Fitness for Purpose of Analytical Methods Eurachem Guide. Abbreviations and symbols, The following abbreviations acronyms and symbols occur in this Guide. AMC Analytical Methods Committee,ANOVA Analysis of variance. AOAC International a globally recognized standards developing organization. ASTM International a globally recognized standards developing organization. BIPM International Bureau of Weights and Measures, CCQM Consultative Committee for Amount of Substance Metrology in Chemistry.
CEN European Committee for Standardization, CITAC Cooperation on International Traceability in Analytical Chemistry. CLSI Clinical and Laboratory Standards Institute,CRM certified reference material. EA European co operation for Accreditation,EC European Commission. EPA Environmental Protection Agency,EQA external quality assessment. EU European Union, GUM Evaluation of measurement data Guide to the expression of uncertainty in.
measurement, ICH International Conference on Harmonisation of Technical Requirements for. Registration of Pharmaceuticals for Human Use,IEC International Electrotechnical Commission. ISO International Organization for Standardization. IUPAC International Union of Pure and Applied Chemistry. JCGM Joint Committee for Guides in Metrology,LOD limit of detection. LOQ limit of quantification,NATA National Association of Testing Authorities. QA quality assurance,QC quality control,RSC Royal Society of Chemistry.
SANCO European Commission s Directorate General for Health and Consumers. SOP standard operating procedure,PT proficiency testing. RM reference material,RSD relative standard deviation. UV VIS ultraviolet visible, VIM International vocabulary of metrology Basic and general concepts and associated. The Fitness for Purpose of Analytical Methods Eurachem Guide. b absolute bias,b relative bias in, kQ multiplier used in calculating limit of quantification. m number of measurements, n number of replicate observations averaged when reporting results.
nb number of blank observations averaged when calculating the blank correction. r repeatability limit,R reproducibility limit,relative recovery apparent recovery in per cent. relative spike recovery in per cent,s standard deviation. s0 estimated standard deviation of single results at or near zero concentration. standard deviation used for calculating an LOD or LOQ. sI intermediate precision standard deviation,sr repeatability standard deviation. sR reproducibility standard deviation,u standard uncertainty. x mean value arithmetic average,xref reference value.
mean value of measurements with an alternative method e g a reference method. mean value of spiked sample in a recovery experiment. added concentration in a recovery experiment, The Fitness for Purpose of Analytical Methods Eurachem Guide. 1 Introduction, 1 1 Rationale and scope for this qualitative methods for determining the presence. Guide of one or more analytes e g the concepts of, Method validation is an important requirement in selectivity and limit of detection LOD. The Fitness for Purpose of Analytical Methods Eurachem Guide MV 2014 1 Foreword to the second edition Since the first edition of this Guide in 1998 a number of important developments in analytical quality have taken place Firstly the ISO 9000 series of standards which is widely used to provide a basis for a quality management system has been revised Its philosophy forms an integral part

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