1、BS ISO 8196-3:2009 ICS 67.100.10 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BRITISH STANDARD Milk Definition and evaluation of the overall accuracy of alternative methods of milk analysis Part 3: Protocol for the evaluation and validation of alternative quantitative metho
2、ds of milk analysisThis British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 November 2009. BSI 2009 ISBN 978 0 580 58451 0 Amendments/corrigenda issued since publication Date Comments BS ISO 8196-3:2009 National foreword This British Standard is th
3、e UK implementation of ISO 8196-3:2009. The UK participation in its preparation was entrusted to Technical Committee AW/5, Chemical analysis of milk and milk products. A list of organizations represented on this committee can be obtained on request to its secretary. This publication does not purport
4、 to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations.BS ISO 8196-3:2009Reference numbers ISO 8196-3:2009(E) IDF 128-3:2009(E) ISO and IDF 2009INTERNATIONAL STANDARD
5、ISO 8196-3 IDF 128-3 First edition 2009-10-01 Milk 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
6、mthodes alternatives danalyse du lait Partie 3: Protocole pour lvaluation et la validation des mthodes quantitatives alternatives danalyse du lait BS ISO 8196-3:2009 ISO 8196-3:2009(E) IDF 128-3:2009(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing
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11、ce International Dairy Federation Case postale 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
12、Published in Switzerland ii ISO and IDF 2009 All rights reservedBS ISO 8196-3:2009 ISO 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 th
13、e validation of alternative methods .3 4.1 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 accura
14、cy.18 Annex B (informative) Limits for the 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 Bi
15、bliography45 BS ISO 8196-3:2009 ISO 8196-3:2009(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 n
16、ormally carried out through ISO technical committees. 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 i
17、n the work. ISO collaborates closely with the 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 prep
18、are International Standards. Draft International 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 s
19、ome of the elements of this document may be 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 Internation
20、al Dairy Federation (IDF). It is being published 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
21、 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 8196-3:2009 ISO 8196-3:2009(E) IDF 128-3:2009(E) ISO and IDF 2009 All rights reserved vForeword IDF (the International Dairy Fede
22、ration) is a non-profit organization representing 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 t
23、he IDF Standing Committees carrying out the 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 A
24、ction Teams and Standing Committees are circulated 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
25、 subject of patent rights. IDF shall not be 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
26、 jointly by ISO and IDF. All work was carried 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
27、with ISO 8196-1|IDF 128-1 and ISO 8196-2|IDF 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:
28、 Analytical attributes of alternative methods 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 8196-3:2009 ISO 8196-3:2009(E) IDF 128-3:2009(E) vi ISO and IDF 2009 All rights
29、 reservedIntroduction This part of ISO 8196|IDF 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
30、new instruments available for study. The latter 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 o
31、ne or more assessments of the relevant performance 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 characterist
32、ics, including guidance for checking statistical 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
33、 their area. An example is given for the evaluation of a method for the determination of fat, protein, lactose, urea and somatic cell count in milk. BS ISO 8196-3:2009 INTERNATIONAL STANDARD ISO 8196-3:2009(E) IDF 128-3:2009(E) ISO and IDF 2009 All rights reserved 1Milk Definition and evaluation of
34、the overall accuracy of alternative methods of 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 mil
35、k analysis. The protocol is applicable to all milk components including somatic cells. For microbiological parameters other standards, such as ISO 16140 5 , 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 no
36、t allow the organization of an interlaboratory study 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 p
37、rotocol defined in this part of ISO 8196|IDF 128. 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 a
38、ny amendments) applies. ISO 3534-1, Statistics Vocabulary 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
39、evaluation of the overall accuracy of alternative 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 la
40、boratory ISO 9622, Whole milk Determination of milkfat, protein and lactose content Guidance on the operation of mid-infrared instruments 1)ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories 1) Equivalent to IDF 141. BS ISO 8196-3:2009 ISO 8196-3:2009(E) I
41、DF 128-3:2009(E) 2 ISO and IDF 2009 All rights reserved3 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 demons
42、tration that results obtained with an alternative method 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 mea
43、surement EXAMPLES A measurand may be a milk component, a physical characteristic or a biological element. NOTE Adapted from ISO/IEC Guide 99:2007 8 , 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) determi
44、ned either directly or on a test portion 3.4 methods 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 confir
45、m results of a previous methods comparison study (3.4) 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 lab
46、oratory (3.7) 3.7 organizing laboratory laboratory having 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 characte
47、r delivered by an official body 3.9 international approval 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 I
48、SO 8196-3:2009 ISO 8196-3:2009(E) IDF 128-3:2009(E) ISO 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 me
49、thods comparison study includes the assessment of the 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 und
