1、BS ISO8196-3:2009ICS 67.100.10NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDMilk Definitionand evaluation of theoverall accuracy ofalternative methods ofmilk analysisPart 3: Protocol for the evaluation andvalidation of alternative quantitativemethods of milk a
2、nalysisThis British Standardwas published underthe authority of theStandards Policy andStrategy Committee on 30November 2009. BSI 2009ISBN 978 0 580 58451 0Amendments/corrigenda issued since publicationDate CommentsBS ISO 8196-3:2009National forewordThis British Standard is the UK implementation of
3、ISO 8196-3:2009.The UK participation in its preparation was entrusted to TechnicalCommittee AW/5, Chemical analysis of milk and milk products.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessar
4、y provisionsof a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.BS ISO 8196-3:2009Reference numbersISO 8196-3:2009(E)IDF 128-3:2009(E)ISO and IDF 2009INTERNATIONAL STANDARD ISO8196-3IDF128-3First edition2009
5、-10-01Milk Definition and evaluation of the overall accuracy of alternative methods of milk analysis Part 3: Protocol for the evaluation and validation of alternative quantitative methods of milk analysis Lait Dfinition et valuation de la prcision globale des mthodes alternatives danalyse du lait Pa
6、rtie 3: Protocole pour lvaluation et la validation des mthodes quantitatives alternatives danalyse du lait BS ISO 8196-3:2009ISO 8196-3:2009(E) IDF 128-3:2009(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewe
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9、e file is suitable for use by ISO member bodies and IDF national committees. In the unlikely event that a problem relating to it is found, please inform the ISO Central Secretariat at the address given below. COPYRIGHT PROTECTED DOCUMENT ISO and IDF 2009 All rights reserved. Unless otherwise specifi
10、ed, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO or IDF at the respective address below. ISO copyright office International Dairy Federation Case po
11、stale 56 CH-1211 Geneva 20 Diamant Building Boulevard Auguste Reyers 80 B-1030 Brussels Tel. + 41 22 749 01 11 Tel. + 32 2 733 98 88 Fax + 41 22 749 09 47 Fax + 32 2 733 04 13 E-mail copyrightiso.org E-mail infofil-idf.org Web www.iso.org Web www.fil-idf.org Published in Switzerland ii ISO and IDF 2
12、009 All rights reservedBS ISO 8196-3:2009ISO 8196-3:2009(E) IDF 128-3:2009(E) ISO and IDF 2009 All rights reserved iiiContents Page Foreword iv Foreword .v Introductionvi 1 Scope1 2 Normative references1 3 Terms and definitions .2 4 General principles for the validation of alternative methods .3 4.1
13、 Validation protocol 3 4.2 Field of validity of the approval .3 5 Technical protocol for the validation 4 5.1 Course of operations 4 5.2 Method comparison study4 5.3 Report and approval delivery.16 Annex A (informative) Measurement process and overall accuracy.18 Annex B (informative) Limits for the
14、 performance characteristics with raw milk19 Annex C (informative) Calculation examples.22 Annex D (informative) Summary of statistical formulas for method evaluations 37 Annex E (informative) Procedure for sample set preparation in linearity evaluation41 Bibliography45 BS ISO 8196-3:2009ISO 8196-3:
15、2009(E) IDF 128-3:2009(E) iv ISO and IDF 2009 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical c
16、ommittees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with t
17、he International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft Internat
18、ional Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be
19、 the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 8196-3|IDF 128-3 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 5, Milk and milk products, and the International Dairy Federation (IDF). It is being publ
20、ished jointly by ISO and IDF. ISO 8196|IDF 128 consists of the following parts, under the general title Milk Definition and evaluation of the overall accuracy of alternative methods of milk analysis: Part 1: Analytical attributes of alternative methods Part 2: Calibration and quality control in the
21、dairy laboratory Part 3: Protocol for the evaluation and validation of alternative quantitative methods of milk analysis BS ISO 8196-3:2009ISO 8196-3:2009(E) IDF 128-3:2009(E) ISO and IDF 2009 All rights reserved vForeword IDF (the International Dairy Federation) is a non-profit organization represe
22、nting the dairy sector worldwide. IDF membership comprises National Committees in every member country as well as regional dairy associations having signed a formal agreement on cooperation with IDF. All members of IDF have the right to be represented at the IDF Standing Committees carrying out the
23、technical work. IDF collaborates with ISO in the development of standard methods of analysis and sampling for milk and milk products. The main task of Standing Committees is to prepare International Standards. Draft International Standards adopted by the Action Teams and Standing Committees are circ
24、ulated to the National Committees for voting. Publication as an International Standard requires approval by at least 50 % of IDF National Committees casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. IDF shall not be
25、held responsible for identifying any or all such patent rights. ISO 8196-3|IDF 128-3 was prepared by the International Dairy Federation (IDF) and Technical Committee ISO/TC 34, Food products, Subcommittee SC 5, Milk and milk products. It is being published jointly by ISO and IDF. All work was carrie
26、d out by the Joint ISO-IDF Action Team on Automated methods of the Standing Committee on Quality assurance, statistics of analytical data and sampling under the aegis of its project leader, Mr. O. Leray (FR). This edition of ISO 8196-3|IDF 128-3, together with ISO 8196-1|IDF 128-1 and ISO 8196-2|IDF
27、 128-2, cancels and replaces IDF 128:1985, which has been technically revised. ISO 8196|IDF 128 consists of the following parts, under the general title Milk Definition and evaluation of the overall accuracy of alternative methods of milk analysis: Part 1: Analytical attributes of alternative method
28、s Part 2: Calibration and quality control in the dairy laboratory Part 3: Protocol for the evaluation and validation of alternative quantitative methods of milk analysis BS ISO 8196-3:2009ISO 8196-3:2009(E) IDF 128-3:2009(E) vi ISO and IDF 2009 All rights reservedIntroduction This part of ISO 8196|I
29、DF 128 is complementary to ISO 8196-1|IDF 128-1. It describes a protocol for the evaluation of new alternative methods for which ISO 8196-1|IDF 128-1 cannot apply, e.g. when the organization of interlaboratory studies is hampered by too small a number of new instruments available for study. The latt
30、er is generally the case with dedicated instrumental methods (e.g. milk payment analysis, milk recording analysis) of which the commercialization depends on official approvals for use. An application for such an official approval is to be accompanied by one or more assessments of the relevant perfor
31、mance characteristics. This part of ISO 8196|IDF 128 specifies a harmonized protocol for such a method validation by an expert laboratory. It lists the evaluation steps, provides a criteria-based approach for the assessment of the performance characteristics, including guidance for checking statisti
32、cal compliance. On the basis of such a harmonized protocol, only a limited number of evaluations should suffice for a decision on approval either by national bodies or by an international organization for the application of the methods and/or equipment in their area. An example is given for the eval
33、uation of a method for the determination of fat, protein, lactose, urea and somatic cell count in milk. BS ISO 8196-3:2009INTERNATIONAL STANDARD ISO 8196-3:2009(E)IDF 128-3:2009(E) ISO and IDF 2009 All rights reserved 1Milk Definition and evaluation of the overall accuracy of alternative methods of
34、milk analysis Part 3: Protocol for the evaluation and validation of alternative quantitative methods of milk analysis 1 Scope This part of ISO 8196|IDF 128 specifies a protocol for the evaluation and validation of alternative quantitative methods of milk analysis. The protocol is applicable to all m
35、ilk components including somatic cells. For microbiological parameters other standards, such as ISO 161405, apply. This part of ISO 8196|IDF 128 is also applicable to the validation of new alternative methods where a limited number of analysts does not allow the organization of an interlaboratory st
36、udy and ISO 8196-1|IDF 128-1, therefore, does not apply. This part of ISO 8196|IDF 128 also establishes general principles of a procedure for granting international approvals of these alternative methods. These principles are based on the validation protocol defined in this part of ISO 8196|IDF 128.
37、 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 3534-1, Statistics Vo
38、cabulary and symbols Part 1: General statistical terms and terms used in probability ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions ISO 8196-1|IDF 128-1, Milk Definition and evaluation of the overall accuracy of alternative
39、 methods of milk analysis Part 1: Analytical attributes of alternative methods ISO 8196-2|IDF 128-2, Milk Definition and evaluation of the overall accuracy of alternative methods of milk analysis Part 2: Calibration and quality control in the dairy laboratory ISO 9622, Whole milk Determination of mi
40、lkfat, protein and lactose content Guidance on the operation of mid-infrared instruments1)ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories 1) Equivalent to IDF 141. BS ISO 8196-3:2009ISO 8196-3:2009(E) IDF 128-3:2009(E) 2 ISO and IDF 2009 All rights rese
41、rved3 Terms and definitions For the purpose of this document, the terms and definitions given in ISO 8196-1|IDF 128-1, ISO 8196-2|IDF 128-2, ISO 3534-1 and ISO 5725-1 apply, together with the following. 3.1 validation of an alternative method demonstration that results obtained with an alternative m
42、ethod are comparable to those obtained with the reference method, thereby showing compliance of accuracy with defined requirements and fitness for purpose 3.2 measurand component analyte criterion particular quantity or characteristic subject to measurement EXAMPLES A measurand may be a milk compone
43、nt, a physical characteristic or a biological element. NOTE Adapted from ISO/IEC Guide 99:20078, 2.6. 3.3 quantitative method method of analysis whereby the result is an amount of a quantity, a concentration or a value of a measurand (3.2) determined either directly or on a test portion 3.4 methods
44、comparison study study, performed by an organizing laboratory of an alternative method against the reference method under test bed conditions 3.5 method confirmation study study performed in routine laboratories, of an alternative method to confirm results of a previous methods comparison study (3.4
45、) 3.6 interlaboratory study study of performance of an alternative method on one or more “identical” laboratory samples of homogeneous, stable materials under documented conditions in several laboratories and under the control of an organizing laboratory (3.7) 3.7 organizing laboratory laboratory ha
46、ving qualified staff and equipment to perform a methods comparison study (3.4) 3.8 national approval authorization of use of a method for defined purposes in a country generally for reasons of collective interest and/or having an official character delivered by an official body 3.9 international app
47、roval authorization of use of a method for defined purposes at the international level generally for reasons of collective interest and/or having an official character delivered by an international organization for the benefit of stakeholders BS ISO 8196-3:2009ISO 8196-3:2009(E) IDF 128-3:2009(E) IS
48、O and IDF 2009 All rights reserved 34 General principles for the validation of alternative methods 4.1 Validation protocol 4.1.1 General The validation protocol comprises two phases as specified in 4.1.2 and 4.1.3 respectively. 4.1.2 Phase I A methods comparison study includes the assessment of the
49、analytical attributes and a comparison of the alternative method against the reference method under test bed conditions. This part of the evaluation has to be carried out by an organizing laboratory specialized in analytical evaluations as well as being experienced in the application of the relevant reference method. The laboratory shall conform to ISO/IEC 17025 for this activity. 4.1.3 Phase II A method confirmation study under routine testing conditions is initiated after a succ
