ISO/TS TECHNICAL SPECIFICATION 22176 First edition 2020-01 Cosmetics Analytical methods - Development of a global approach for validation of quantitative analytical methods Cosmetiques - Méthodes analytiques - Développement d'une approche globale pour la validation des methodesanalytiques quantitatives Reference number IS0/TS22176:2020(E) ISO ISO2020 IS0/TS22176:2020(E) COPYRIGHTPROTECTEDDOCUMENT IS02020 All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting below or Iso's member body in the country of the requester. ISO copyright office CP 401 : Ch. de Blandonnet 8 CH-1214 Vernier, Geneva Phone:+4122749 0111 Fax: +41 22 749 09 47 Email: copyright@iso.org Website: www.iso.org Published in Switzerland ii @ IS0 2020 - All rights reserved IS0/TS22176:2020(E) Contents Page Foreword ..V Introduction. ..vi 1 Scope. ..1 2 Normative references 3 Terms, definitions and symbols 3.1 Terms and definitions .1 3.2 Symbols.... General principles ..6 4 4.1 Reminder .6 4.2 Variousconditionsfortheestimationofprecision .6 4.3 Accuracyprofile 7 5 Procedure .9 5.1 Definition of the measured quantity .9 5.2 Definition of objectives. 9 5.2.1 Choiceofthe scopeofvalidation .9 5.2.2 Choice ofacceptancelimits. .9 5.3 Selectionof validation samples .10 5.3.1 Choice of the type of matrix or types of matrices .10 5.3.2 Methodsforestablishingreferencevalues .10 5.4 Characterization plan for validation... ..10 5.4.1 Organization ..10 5.4.2 Choiceofthenumberofseries,repetitionsand concentrationsforthe characterizationplanforvalidation ..11 5.5 Calibration plan for the indirect methods ..1 5.5.1 Organization ..11 5.5.2 Choiceofthenumberofseries,repetitionsandconcentrationsforthe calibrationplan .12 5.6 Testing ..13 5.7 Calculation ofpredicted inverse concentrations forindirect methods .14 5.7.1 General. .14 5.7.2 Calculation of the calibration models .14 5.7.3 Calculation ofback-calculated concentrations by inverse prediction .15 5.8 Calculation ofthevalidation criteriaby concentration level .15 5.8.1 General. .15 5.8.2 Trueness criteria by series .15 5.8.3 Trueness and precision criteria by concentration ..16 Calculation ofthetolerance intervals ..17 5.8.4 5.9 Construction of the accuracy profile .18 5.10 Interpretation of the accuracy profilefor validation .19 5.10.1 General. .19 5.10.2 Decision rules. 20 5.10.3 Definition ofthe scope of validity 21 5.10.4 Choice of a calibration procedure for the routine 21 5.10.5 Influenceand significance oftheβproportion 21 5.10.6 Identification of outliers. .22 Managementoftheoutcomes duringroutineuse ..22 6 AnnexA (normative)Calculation ofrepeatability,intermediateprecisionand reproducibility standard deviations. ..23 AnnexB(normative)Contentsofthevalidationfile ..25 Annex C (informative) Setting-up an assayfor determining the accuracy profile in the case ofNDELAincosmeticsamples .27 iii IS0 2020-All rights reserved