ALINORM 04/27/23

INTRODUCTION
1) The Codex Committee on Methods of Analysis and Sampling held its Twenty-fifth Session in Budapest, Hungary, from 8 to 12 March 2004, by courtesy of the Government of Hungary. The Session was chaired by Professor Peter Biacs, Director-General of the Hungarian Food Safety Office and by the Vice-Chairperson, Prof. Pal Molnár, Head of Food Quality Department of the Central Food Research Institute (KEKI). The Session was attended by 123 delegates and observers representing 38 Member Countries, one Member Organization (EC) and 14 international organizations. A complete list of participants is given in Appendix I of this report.
OPENING OF THE SESSION
2) The Session was welcomed by Dr Ferenc Nyújtó, Deputy State Secretary of Ministry of Agriculture and Regional Development. Dr Nyújtó welcomed the participants and expressed that it was a great honour for Hungary to host the Codex Committee on Methods of Analysis and Sampling, as it had been doing for many years. He emphasised the increasing interest of members for this Committee whose work is of great importance to other Codex Committees. Dr Nyújtó stressed the adoption of a new Food Law by the Hungarian Parliament last year that dedicates a special chapter to Codex Alimentarius and establishes the National Codex Committee. Emphasizing the role of the Codex Alimentarius standards in assuring food safety and their importance for harmonization and international food trade, Dr Nyújtó wished the delegates all success in their work.
ADOPTION OF THE AGENDA (Agenda Item 1)
3) The delegation of the European Community presented CRD 5 on the division of competence between the European Community and its Member States according to Rule of Procedure II Paragraph 5 of the Codex Alimentarius Commission.
4) The Committee adopted the Provisional Agenda as presented in CX/MAS 04/1. It agreed to consider Agenda Item 5 and Agenda Item 6b) one after the other taking into account that both items related to the evaluation of methods of analysis.
MATTERS REFERRED BY THE CODEX ALIMENTARIUS COMMISSION AND OTHER CODEX COMMITTEES (Agenda Item 2)¹
5) The Committee noted that a number of matters referred by the 26^th Session of the Codex Alimentarius Commission (CAC), and other Codex Committees were for information purposes or would be discussed in more detail under relevant Agenda items. It also noted that some issues such as the follow-up to the evaluation of Codex were still being considered by other Codex Committees. In addition the Committee considered matters referred as follows:
The use of analytical results: sampling, relationship between the analytical results, the measurement uncertainty, recovery factors and provisions in Codex standards
6) The Committee recalled that the paper on the above matters had been considered at its 24^th session and with the aim to make recommendations regarding enforcement of Codex commodity standards especially when making decisions as to whether a lot is in compliance with Codex specifications. It was also recalled that this matter had been referred to the Codex Committee on Food Import and Export Inspection and Certification Systems (CCFICS) and Commodity Committees for their consideration and comments and that these comments were presented in document CX/MAS 04/2-Add.1.
7) The Delegation of the United Kingdom introduced the document and indicated that there was no common understanding between the member states on the use of uncertainty and recovery value when deciding whether the sample is in compliance or not. The Delegation pointed out that the guideline document on “The Use of Analytical results: Sampling, Relationship between the Analytical Results, the Measurement

Uncertainty, Recovery Factors and Provisions in Codex standards” (Annex I to CX/MAS 04/2-Add.1) had been prepared to ensure that the interpretation of sampling, measurement of uncertainty and recovery is harmonized across Codex and to facilitate the uniform interpretation of Codex standards.
8) Several delegations supported further development of this document as it addressed essential issues. However they noted that it had been distributed quite late, therefore there was not enough time to consider it with national experts, which was important to provide a scientific basis for the document.
9) Some delegations drew the attention of the Committee to the fact that it was necessary to clarify to whom the Guidelines were targeted: to Codex Committees or to governments as this was important for further development of the text. In this regard it was indicated that Codex had adopted the IUPAC Guidelines on recovery where much guidance for governments on recovery was already provided.
10) The Delegation of New Zealand indicated that the document should be improved especially on the description of sampling procedures and the basis for the sampling plan; and that the proposal for the handling of uncertainty was not the only way to proceed. Further clarification was also needed on the interpretation of the results, therefore additional work during the session was necessary to improve the text.
11) It was suggested to split this document into two parts: one dealing with sampling, and the other with uncertainty and recovery.
12) Some delegations indicated that the concept of recovery was quite complex, as it is estimated in chemical quantitative analysis, except for Type I methods and that the definition of recovery should be discussed very thoroughly in order to avoid future problems. It was suggested to clarify the use of significant figures and better separate the uncertainty arising from sampling from that arising from analysis, in order to avoid possible confusion.
13) The Committee agreed that an Ad Hoc Working Group should be convened under the Chairmanship of the United Kingdom² to redraft the Guidelines with the understanding that it would be used by Codex Commodity Committees. It also agreed to consider the redrafted Guidelines under Agenda Item 12 “Other Business and Future Work” (see also paras ‎128) to ‎0 .
Single laboratory validated methods of analysis
14) The Committee recalled that following the request of its 24th session, the Codex Committee on Pesticide Residues (CCPR) had proposed criteria of a general nature for the selection of single-laboratory validated methods of analysis, to be included in the Procedural Manual after the General Criteria in order to recognize that inter-laboratory validation of methods of analysis was not always available and applicable for multi-residue analysis purposes.
15) After some discussion regarding the applicability of criteria, the Committee concluded that the proposed criteria should be of a general nature and should be incorporated into the Procedural Manual. It therefore amended the first bullet (i) by deleting the specific reference to the CCPR Guideline on Good Laboratory Practice.
16) In bullet (ii), the Committee deleted the reference to “assurance” in quality system in order to be consistent with the decision of the 24^th Session and clarified that the use of the method was embedded in a quality system in compliance with the ISO/IEC 17025 document. It also clarified that the principles of Good Laboratory Practice were those established by OECD.
17) The Committee amended the last bullet to indicate that the verification of results with other validated methods was applicable “where available”.
18) The Committee agreed to forward the proposed General Criteria for Selection of Single-Laboratory Validated Methods of Analysis to the Committee on General Principles for endorsement and subsequent adoption by the 27^th Session of the Commission and inclusion in the Codex Procedural Manual after the section on General Criteria (see Appendix II).
DRAFT GENERAL GUIDELINES ON SAMPLING (Agenda Item 3)³
19) The Committee recalled that the Draft Guidelines had been adopted by the Commission at Step 5 and circulated for comments at Step 6. The Committee had also agreed at its last session that an Ad hoc Working Group would meet prior to the session in order to consider the comments and facilitate discussion in the Plenary Session.
20) The Delegation of France presented the revised version of the Draft Guidelines prepared by the Working Group (CRD 6) taking into account all the written comments submitted to the meeting. Most comments were of an editorial nature and some substantial amendments had been made to the text as follows.
21) Section 2.3.2 Employment of Authorized Sampling Officers had been amended in the light of the comments received. As regards Section 2.4 Estimation Error it had been agreed that the case where the analytical error is larger than one third of the sampling error would not be covered by the Guidelines. The Working Group had also revised section 4.4 Single Sampling Plans for Average Control.
22) The Committee agreed to delete the reference to “authorized” persons in section 2.3.2 as it was not clear who would authorize them to carry out sampling and this may create confusion. The Committee also agreed to clarify that Lot Size was defined by the number of items in Tables 10, 14 and 17.
23) Many delegations supported the advancement of the Draft Guidelines to Step 8 in order to provide guidance to governments. Some delegations, while supporting the adoption of the document, pointed out that further guidance was needed concerning the application of the sampling plan to specific commodities, in order to facilitate its use by governments. The Committee agreed that Commodity Committees should be encouraged to develop sampling plans for specific commodities, where necessary, on the basis of the general Guidelines.
24) The Committee expressed its appreciation to the Delegation of France and to the Working Group for their excellent work in the development and finalization of these Guidelines addressing complex issues that would provide important guidance to governments.
Status of the Draft General Guidelines on Sampling
25) The Committee agreed to advance the Draft Guidelines to Step 8 for adoption by the 27th Session of the Codex Alimentarius Commission (see Appendix III). It was agreed that the General Guidelines, when adopted, would replace the current Sampling Plans for Prepackaged Foods (AQL 6.5) (CODEX 233-1969).
DRAFT GUIDELINES ON MEASUREMENT UNCERTAINTY⁴
26) The Committee recalled that the draft Guidelines had been adopted by the Commission at Step 5 and circulated for comments at Step 6.
27) The Committee considered the Guidelines section by section and in addition to some editorial amendments made the following changes.
General comments
28) The Delegation of New Zealand drew the attention of the Committee to the fact that the draft Guidelines did not provide enough information on how measurement of uncertainty was to be used, especially in assessing compliance. It indicated that both Measurement Uncertainty and Sampling Plans were used to assess conformance to product specifications, therefore their roles had to be clarified. The Delegation therefore proposed areas where the Guidelines should be expanded.
Introduction
29) The Committee deleted the reference to footnote two as the text of this footnote was already covered by the relevant ISO document.

30) The Committee had a long discussion regarding the content and where to place an amendment proposed by the Delegation of the United Kingdom as to how the quantitative analytical results are to be expressed and reported by analysts. The Committee agreed that the range of “a ± 2u” represented a 95% level of confidence, to be consistent with the recommendation referring to the level of confidence.
31) Some delegations were of the view that the amendment was formulated like a recommendation and therefore better fit to the recommendation section while others argued that it clarified the expression of analytical results and suggested to place it in the Introduction. The Committee agreed to put the proposed wording as second paragraph of the Introduction.
32) The Committee clarified that the Guidelines were applied only to quantitative analysis therefore added a third sentence in the Introduction to this effect.
Terminology
33) It was indicated that the intent of the third note was not clear therefore it could be deleted, however the Delegation of Ireland drew the attention of the Committee to the fact that the use of international definitions such as those presented in ISO documents should not be altered as it was very important for accreditation of laboratories.
34) It was clarified that the definition for Measurement Uncertainty referred to “international” instead of “accepted” and that notes were part of this definition therefore a quotation mark was placed at the end of the last note.
Recommendations
35) The Committee deleted the first recommendation regarding the applicability of the Guidelines as it was already clear from the Introduction that they are to be used by Governments. Recommendations were also rearranged in order to put them in a more logical sequence.
36) It was proposed to hold the decision on the Guidelines until the item on the Use of Analytical Results had been discussed, as it contained recommendations on how measurement of uncertainty is to be used. However the Committee noted that significant progress had been made on the development of the draft Guidelines on Measurement Uncertainty and that it provided valuable guidance to governments. The Committee noted that the other document was at a very early stage of development and that it was not clear enough what the outcome of these discussions might be at this moment (see paras ‎128) to ‎0‎135).
Status of the Draft Guidelines on Measurement Uncertainty
37) The Committee agreed to forward the above Guidelines as amended during the session to the 27^th Session of the Commission to Step 8 for final adoption (see Appendix IV).
38) The Delegation of New Zealand expressed their reservation on this decision.
PROPOSED DRAFT GUIDELINES FOR EVALUATING ACCEPTABLE METHODS OF ANALYSIS (Agenda Item 5)⁵
39) The Committee recalled that the last session had considered Proposed Draft Guidelines intended for governments that proposed two possible approaches: the traditional approach assigning numerical values to specific parameters and the ”fitness-for-purpose” approach. The Committee had agreed to circulate for comments at Step 3 the Proposed Draft Guidelines reflecting the traditional approach and to redraft the document on ”fitness-for-purpose”, for consideration under Agenda Item 6b). The Committee recalled that both documents were discussed separately as they were not at the same stage of development but that they had been initially intended to be part of the same Guidelines for Evaluating Acceptable Methods of Analysis. The Committee therefore agreed to discuss Agenda Item 6b) after Item 5 (see paras. ‎59) to ‎65).
40) The Committee discussed the text section by section and made the following amendments.

Scope
41) The Committee agreed that in paragraph 3 laboratories “should comply with Codex Guidelines CAC/GL 27” (instead of “must”) as guidelines should not be too prescriptive.
Requirements
42) The Committee agreed that methods should be assessed “as appropriate” against the criteria listed, since all methods might not need to be assessed according to all criteria, and the third bullet point on detection/determination limits was amended accordingly.
43) As regards precision (fifth bullet point), the Committee had an exchange of views on the need to clarify the text and agreed to retain only the reference to repeatability intra-laboratory and reproducibility inter-laboratory as the purpose of the section was to describe requirements for methods, not to establish definitions.
44) The Committee also noted that the initial text corresponded to the definition of “precision” in the Procedural Manual and agreed that the definition should be amended to delete the reference to measurement uncertainty considerations at it created confusion. The Committee agreed to consider the amendment to the definition under Agenda Item 7 that would address the review of terminology.
Accuracy
Estimation
45) The Committee agreed with the proposal of the Delegation of Ireland that reference material should be matrix matched and with a similar level of analyte and the first sentence was amended accordingly.
46) The Committee agreed to refer to z-value rather than z-score in order to avoid confusion with the terminology used by IUPAC and inserted a reference to NMKL Procedure No. 9 (2001) that had developed the calculation of z-value presented in the working document. An additional sentence was added to clarify the relation between the z-value, the reference value and the confidence interval in the second equation.
47) The Delegation of New Zealand expressed the view that the section should cover estimation only and that bias should not be used as a criterion to accept or reject a method since bias could be corrected. After some discussion, the Committee added a sentence to the effect that a z-value outside the range |z|≤2 indicates a significant bias and a bias correction should be made in this case.
Detection/Determination Limits
48) The Delegation of the Republic of Korea expressed the view that the reference to the acronym “LoQ” for Determination Limit created confusion, as this should refer to limit of quantification and that these two limits were not equivalent in its national regulations. Other delegations pointed out that “determination limit” was equivalent to “limit of quantification” in their national regulations. In order to avoid confusion, the Committee agreed to avoid the use of acronyms and to specify which limit was applied throughout the section.
Linearity
49) The Committee agreed that results should be proportionate to the quantity of the analyte, as the current text erroneously referred to “quality”. As it was noted that the text reflected the current definition of “linearity” in the Procedural Manual, the Committee agreed to make the relevant correction when discussing terminology under Agenda Item 7.
Precision Characteristics
Estimation
50) The Delegation of New Zealand expressed its objection to the use of an acceptance criterion based on precision and proposed to delete the current text and to specify only that repeatability and reproducibility should be estimated by standard procedures, such as IUPAC 1987 Protocol. The Delegation of the United Kingdom indicated that the concept of comparison should be retained especially as one element of the criteria approach was the assessment of precision and even methods that had been collaboratively tested might have a large precision characteristic.
51) The Delegation of the Netherlands proposed to remove the second sentence of the paragraph indicating in which case the method could be used as a validated method in order to make the text less prescriptive.

52) The Delegation of the European Community supported the current text as it was important to retain the notion of comparison of repeatability and reproducibility values to decide whether methods could be used as validated methods.
53) The Committee could not come to a conclusion on this question and agreed that it would require further consideration at the next session.
Status of the Proposed Draft Guidelines for Evaluating Acceptable Methods of Analysis
54) The Committee agreed to advance the Proposed Draft Guidelines, as amended at the current session, for adoption at Step 5 by the 27^th Session of the Codex Alimentarius Commission (see Appendix V).
CRITERIA FOR EVALUATING ACCEPTABLE METHODS OF ANALYSIS (Agenda Item 6)
PROPOSED DRAFT GUIDELINES FOR SETTLING DISPUTES OVER ANALYTICAL (TEST) RESULTS (Agenda Item 6a)
55) The Committee recalled that its last session had agreed that the delegation of France would develop Proposed Draft Guidelines to address disputes arising from differences in laboratory results, and that this new work had subsequently been approved by the Commission.
56) The Delegation of France informed the Committee that it had not been able to prepare the document as several related issues were still under discussion in the Committee and had not yet been resolved, such as sampling, measurement uncertainty and the use of recovery factors, the use of significant figures, the application of specifications to the lot or the unit. The Delegation recalled that it had prepared a document at the last session based on ISO 4529:2000 including a procedure for the declaration of conformity and that it had been considered too complex for practical use, but that guidelines in this area should follow a scientific approach.
57) Several delegations supported the development of guidance for governments in order to facilitate dispute settlements and pointed out that the document should be practical enough to be used by governments. The Committee agreed that the document should address only disputes related to analytical methodology and should not consider sampling issues.
Status of the Proposed Draft Guidelines for Settling Disputes over Analytical (Test) Results
58) The Committee agreed that the Delegation of France would prepare a new version of the Proposed Draft Guidelines for consideration by the next session.
CONSIDERATION OF THE FITNESS-FOR-PURPOSE APPROACH TO EVALUATING METHODS OF ANALYSIS (Agenda Item 6b)⁶
59) The Committee recalled that the last session had considered Proposed Draft Guidelines for Evaluating Acceptable Methods of Analysis proposing two possible approaches: the traditional approach and the ”fitness-for-purpose” approach. The Committee had agreed that the Proposed Draft Guidelines applying the traditional approach would be circulated at Step 3 (see Agenda Item 5) and that the Delegation of the United Kingdom would redraft the document on “fitness for purpose” with the assistance of a drafting group for further consideration. The Committee recalled that these documents were not at the same stage of development but that they had been initially intended to be part of the Guidelines for Evaluating Acceptable Methods of Analysis. The Committee therefore discussed Agenda Item 6b) after Item 5 (see paras ‎39) to ‎54).
60) The Delegation of the United Kingdom, while introducing the revised document, indicated that the fitness for purpose approach took all values into account by defining a fitness function as a single parameter. The document also defined the related uncertainty function, explained how the estimated characteristic function could be constructed from precision, and presented some examples of the application of this new procedure. The Delegation stressed the importance of considering this issue at the international level as it would affect regulations and was already applied or under development in some areas of EC food legislation.
61) The Committee expressed its appreciation to the Delegation of the United Kingdom for developing this comprehensive document that addressed complex issues of importance for the future work of the Committee.
62) The Delegation of the United States expressed the view that this was an interesting approach and that it had no objection in principle to the elaboration of the document but that it was premature to apply it for regulatory purposes, and that further discussion would be needed in this respect.
63) The Delegation of New Zealand expressed its reservations to the approach proposed and referred to its earlier objections to the application of acceptance criteria to bias and precision. The Delegation pointed out that the fitness function was quite arbitrary and that it would require a solid scientific basis, especially as it was likely to affect regulatory decisions. In particular, fitness for purpose should examine the effect of bias and measurement uncertainty on decisions made using results generated by the test method. The Delegation indicated that it had carried out studies in this area and was prepared to provide the results to the Committee for further consideration.
64) The Delegation of Germany expressed its reservations on this approach as all characteristics were subsumed into one function and questioned whether it adequately reflected the characteristics of the method. The Delegation of the Netherlands highlighted the relation between the issues under consideration and the recommendations in the Draft Guidelines on Measurement Uncertainty and supported further consideration of the fitness-for-purpose approach in view of its importance.
65) The Committee agreed that the delegation of the United Kingdom, in cooperation with interested delegations, would revise the document for further consideration at the next session.
REVIEW OF THE ANALYTICAL TERMINOLOGY FOR CODEX USE IN PROCEDURAL MANUAL (Agenda item 7)⁷
66) The Committee recalled that at its last session it was agreed to initiate the revision of the Definitions contained in the Codex Procedural Manual and that this was approved by the 26th Session of the Commission as new work. It also recalled that a Circular Letter has been distributed requesting comments on the Analytical Terminology for Codex Use.
General comments
67) Some delegations stressed the need to have only one set of harmonized definitions in Codex and to establish different definitions only in case of necessity. Analytical terminology should be clearly defined and justified otherwise there was a possibility to get different data and results. It was indicated that international definitions contained in ISO or IUPAC documents were being revised therefore it was necessary to have cross references in order to ensure consistency. The Delegation of the Republic of Korea proposed to define and describe terminology that is not yet defined and which is used for describing the meaning of a certain term.
Result
68) The Delegation of New Zealand suggested defining the “Test method” or “Method” as it could simplify further definition of “Result”. However the Committee noted that the proposed definition was already consistent with the definition in other international documents therefore left it unchanged.
Specificity
69) The Delegation of Austria noted that the definition of “specificity “ was quite similar to “selectivity” and that its use created some confusion especially as “specificity” defined in Codex did not include the words “of similar behaviour” which were necessary for gaining and quenching effects of matrix substances. The Committee was informed about recently published statistical approaches for estimation of selectivity, based on the IUPAC definition⁸. As “selectivity” was well defined in IUPAC, the Committee agreed to delete the definition of “specificity” and in future to refer only to “selectivity” as defined in IUPAC.
Accuracy (as a concept) and accuracy (as statistic)
70) The Committee noted that the section on accuracy was quite confusing as it contained two definitions: one used as a concept and the other as a statistic and that the definition on a statistic contained a second note which was not quite correct. It was also noted that this definition needed harmonization with other Codex Committees such as the Committee on Pesticide Residues and the Committee on Residues of Veterinary Drugs in Foods. The Committee agreed that there should be only one definition of “accuracy” and this definition should be the one defined by ISO 3534-1.
Trueness
71) The Committee noted that there was some inconsistency between the definitions of trueness in Codex and ISO and decided to include the second sentence of the note in the ISO definition.
72) The amended definitions are presented in Appendix II.
Approach to the Review of Terminology
73) The Committee had a discussion on the approach to the revision of terminology.
74) In order to simplify work, it was proposed to use only references and sources from international definitions; however the Committee noted that it would be difficult to accept this as definitions were so important that they should be fully spelt out in the Procedural Manual.
75) The Delegation of Finland drew the attention of the Committee to the fact that it was difficult to proceed with the revision of further definitions without having the opinion of international organizations working in the area of terminology. It noted that this matter was considered at the Inter-Agency Meeting (IAM) before the CCMAS and suggested that a paper containing the comparison of definitions should be prepared for consideration by the next session of the Committee. Many delegations supported this proposal especially as ongoing work on the revision of definitions was carried out by relevant international organizations and this would facilitate harmonization of definitions for Codex purposes.
76) The Committee agreed that a Circular Letter would be prepared asking member governments and interested international organizations their suggestions as to which definitions should be necessary for Codex purposes and which current Codex definitions should be amended. The Committee agreed that this Circular Letter should include the compendium prepared in 2002 by IAM and including all current appropriate definitions developed or being revised by relevant international organizations. It also agreed that the Delegation of the United States with the assistance of AOAC and other interested members and observers⁹ should prepare a paper in the light of comments received, addressing the above issues and providing an analysis and recommendations/rationale for appropriate definitions to be used for Codex purposes, for consideration by the next session of the Committee.
ENDORSEMENT OF METHODS OF ANALYSIS PROVISIONS IN CODEX STANDARDS (Agenda Item 8)¹⁰
77) The report of the Ad hoc Working Group on Endorsement of Methods of Analysis (CRD 1) was presented by its Chair, Dr Roger Wood (United Kingdom). The Committee endorsed the methods proposed with the following amendments and comments.
Committee on Fats and Oils
78) The Observer from AOCS drew the attention of the Committee to the proposal from the Committee on Fats and Oils to delete the year of publication in the reference as this would simplify the updating and endorsement process. It was also noted that under ISO/IEC 17025: 1999, analysts were required to use the most updated version of methods of analysis. This proposal was supported by other observers, who indicated that when significant changes were made to a method, a new number was given to the method and this avoided any confusion.
79) Several delegations supported the inclusion of the year of publication in the method as this was an important reference for laboratories, especially for regulatory purposes. They expressed the view that it was not possible to endorse all future changes that might occur in a method without being informed of those changes, and that the list of methods should be reviewed regularly to ensure that all updates were taken into account. The Committee agreed to retain the year of publication at this stage and to consider this question further at its next session.
Fat Spreads and Blended Fat Spreads
80) The Committee noted that the level of 3% milk fat was the essential composition factor used to differentiate fat spreads from blended spreads. The Committee recalled that the CCFO had recommended to convert the butyric acid concentration into milk fat concentration and to report the range in which the milk fat concentration of a sample would lie, in the absence of a single agreed factor. Some delegations pointed out that the question of the factor should be clarified by the CCFO and that the method could not be fully endorsed until this was resolved. It was suggested that reference be made to the figure used by the World Customs Organization for fat spreads, but some delegations noted that an average figure established for customs purposes would not solve a problem of interpretation of analytical results.
81) The Committee agreed to endorse temporarily the methods proposed as Type I pending the definition of a conversion factor by the Committee on Fats and Oils.
Olive Oils and Olive-Pomace Oils
82) The Delegations of Italy and Morocco expressed their reservations on the inclusion of the ISO 15788-2: 2003 method for stigmastadienes as it had not been considered by the Committee on Fats and Oils and was not used in the framework of the International Olive Oil Council. The Committee agreed to endorse temporarily this method and to forward it to the CCFO for consideration. All other methods were endorsed as proposed, with the editorial corrections proposed by the Delegation of Spain.
Named Vegetable Oils
83) The Committee endorsed the revised list of methods proposed by the CCFO, including the deletion of several IUPAC methods that are not any longer available.
Committee on Fish and Fishery Products
Determination of Fish Content in Quick Frozen Fish Sticks
84) The Delegation of Indonesia pointed out that the Interim Nitrogen Factors used for white fish to calculate fish content originated from temperate regions and the Committee noted that additional factors for other species could be put forward for consideration by the Committee on Fish and Fishery Products in order to refine further the methodology. The method was endorsed as proposed.
Ad hoc Intergovernmental Task Force on Fruit and Vegetable Juices
Fruit Juices and Nectars
85) The Committee noted that the Working Group on endorsement had agreed to consider for endorsement the methods corresponding to permitted ingredients and additives or processing aids, as listed in the Draft Standard (Annex – Section C.1), and that the other methods listed by the Task Force as quality methods or authenticity methods would not be considered for endorsement but listed separately.
86) The Delegation of Canada (Mrs Carla Barry, Chair of the WG on methods of analysis in the Task Force) recalled that the Task Force had agreed to define a complete set of methods as they were necessary as references at the international level but that it had not been possible at that stage to define values for the parameters related to authenticity and quality. These values might be established in the future and that would be facilitated by the harmonisation of methods of analysis. The Delegation therefore proposed that the Committee endorse the methods for authenticity and quality (section C.2 of CRD 1). This position was supported by the Delegation of Brazil, referring to its written comments, and several other delegations.
87) The Secretariat recalled that methods should correspond to specific provisions in standards and that so far the Committee had endorsed only methods for analytes or properties that were identified in Codex standards. If this approach was changed for fruit juices, this might also affect the overall endorsement process.
88) Some delegations pointed out that the provision in the General Criteria of the Selection of Methods of Analysis on “direct pertinence to the Codex standard” did not mean that a numerical value should be specified in the standard. The Secretariat referred to the “Recommendations for a Checklist of Information Required to Evaluate Methods of Analysis Submitted to the CCMAS for Endorsement” especially point 1.1.3 Analyte or Property and 1.1.4 Codex Specification or Limit requiring “the specification, limit, tolerance or guideline which is given in the standard and which provides the boundary between acceptable and unacceptable material” and noted that this boundary should be defined in the standard, whether it was numerical or not. Some delegations expressed the view that the Recommendations were not relevant as they

were not part of the Procedural Manual and the Committee agreed that they should not be taken into account in the case of fruit juices.
89) Some delegations proposed to endorse the methods only temporarily as Type IV in order to retain the valuable information resulting from the work of the Task Force, with the understanding that they would be endorsed when the relevant provisions were completed. The Delegation of Brazil pointed out that all the methods proposed had been validated and therefore should not be listed as Type IV. The Committee therefore agreed that the methods would be listed without a type as “temporarily endorsed” pending the establishment of numerical values by the Task Force.
90) The Committee made some corrections to the methods proposed for endorsement by the Working Group (section C.1 of CRD 1) and agreed to include methods for total nitrogen and for cellobiose to the list. The Committee noted that the ISO method for the determination of ascorbic acid was not validated and agreed that it should be retained as Type IV. The Delegation of Switzerland proposed to include method EN 14130 for the determination of Vitamin C but this was not accepted as this method had not been collaboratively tested.
91) The Delegation of Japan proposed that the applicability of methods for food additives that are also intrinsic constituents of fruit juices and nectars should be clarified. The Committee agreed that the Task Force should provide clarification in this respect.
Committee on Nutrition and Foods for Special Dietary Uses
Gluten Free Foods
92) The Committee had an extensive discussion on the proposed Enzyme-Linked Immunoassay R5 Mendez (ELISA) Method forwarded by the CCNFSDU for the determination of gluten. The Observer of the WGPAT (Prolamin Working Group) pointed out that method AOAC 991.19 was inadequate, especially as regards specificity and sensitivity and that the new method proposed was the only one that could determine all gliadin fractions, and the toxic gliadin peptide. The method had been collaboratively tested, the results had been published in scientific literature and all relevant information was available to analysts. In addition, only the extraction cocktail was patented but its composition was described in literature and could be used by laboratories. The Observer referred to the documents on the characteristics of the methods that had been presented to the Working Group and proposed to endorse the method as it represented a significant progress in order to address an important health problem.
93) The Observer of AOAC indicated that the colorimetric AOAC 991.19 method had been approved for final action in 2001, was collaboratively tested and publicly available and routinely used by laboratories.
94) The Delegation of Sweden expressed its concern with the fact that the proposed method was not publicly available to analysts and proposed to endorse the AOAC method for the determination of gluten as it was currently used in several countries for the analysis and control of gluten-free foods.
95) The Delegation of France pointed out that the ELISA method was not applicable to certain foods and questioned its relevance in a standard covering all gluten free foods, and drew the attention of the Committee to the comments of AAC in CRD 3, especially as regards the applicability to wheat starch hydrolysates.
96) Some delegations pointed out that the standard did not define clearly what should be measured since section 6.2 referred to a detection limit of 10 ppm without specifying whether this applied to gluten or gliadins. The Committee agreed to ask the CCNFSDU to clarify the applicability of the method and how it related to the provisions for “gluten free” in the standard.
97) The Delegation of the EC (Institute for Reference Material and Measurements) informed the Committee about its work to develop the European gliadin reference material, that was in the process of certification and indicated that the IRMM would initiate a comparison of methods at the end of 2004.
98) The Observer form AOECS expressed the view that it was essential to have a reference method to determine gluten in order to address the health problem faced by coeliac patients, and pointed out that a wide variability existed in the results obtained with the AOAC method. The Observer recalled that no method had been established in present Standard for Gluten Foods, and that the revision of the standard had been underway for several years, since there was no agreement at the moment on the levels or the method of determination.
99) The Observer from AOCS proposed that the R5 ELISA method should be considered by one of the IAM organizations that developed methods of analysis in order to present it according to an internationally recognized format as this would facilitate its consideration for endorsement by the CCMAS.
100) Some delegations expressed the view that the method was acceptable from a scientific point of view and supported its endorsement and inclusion in the standard for gluten free foods as this would be a significant progress to address the health problems of coeliac patients.
101) The Committee agreed to inform the Committee on Nutrition and Foods for Dietary Uses of the issues raised concerning the method and to endorse temporarily the Enzyme-Linked Immunoassay R5 Mendez (ELISA) as Type IV, with the understanding that the method would be considered by the next session.
Methods for Additives and Contaminants
102) The Delegation of the Netherlands proposed to amend the type of the two adopted general methods for the determination of heavy metals, using the second method as Type II since microwave digestion provides better results than dry ashing. However the Committee noted that the equipment necessary for this method was not available in all laboratories and the Committee agreed to retain the current types of the methods at this stage. The Committee agreed to clarify that these general methods apply to all foods except fats and oils.
103) The Delegation of the Netherlands informed the Committee that the CEN method for nitrates and nitrites had been published as final CEN methods and the Committee agreed to endorse them as Type III methods. It as noted that the second CEN method was identical to the NMKL method. The Delegation of Morocco pointed out that when spectrometric methods were used for the determination of nitrites interferences with ascorbic acid may occur and it would be preferable to select electrochemical methods that were more selective.
104) The Committee endorsed the other amendments proposed to the methods for additives and contaminants in order to ensure consistency between the methods.
105) The Committee agreed with the proposal of the Delegation of the United Kingdom to initiate the conversion of the methods for trace elements into criteria, for consideration at the next session in the framework of the Agenda Item on Endorsement. The Committee welcomed the proposal of the Observer from NMKL to work in this area with interested delegations and international organisations.
106) The Committee expressed its appreciation to Dr Wood and to the Working Group for their constructive work in order to facilitate the discussions in the Plenary Session and agreed that it would be reconvened prior to the next session. The status of the endorsement of methods of analysis and sampling is presented in Appendix VI.
CRITERIA FOR THE METHODS FOR THE DETECTION AND IDENTIFICATION OF FOODS DERIVED FROM BIOTECHNOLOGY – GENERAL APPROACH AND CRITERIA FOR THE METHODS (Agenda Item 9)¹¹
107) The Committee recalled that the last session had agreed that the Delegations of Germany and the United Kingdom in cooperation with a drafting group would prepare a revised document that would include recommendations for quality control measures in laboratories and criteria for methods of analysis.
108) The Delegation of the United Kingdom introduced the document and indicated that it included recommendations on the criteria for methods of analysis and quality control measures that should be introduced in laboratories performing GM analysis, with specific focus the detection of DNA markers based on PCR that were more commonly used.
109) The Delegation of Germany referred to the list of methods developed by the Task Force on Foods Derived from Biotechnology and highlighted the importance of further work on guidelines that would provide guidance to governments to select methods for the detection of foods derived from biotechnology.

110) The Delegation of the United States welcomed the paper that provided a good scientific basis for further discussion and drew the attention of the Committee to its comments in CRD 9. It noted in particular that the document developed criteria mostly for DNA-based methods but that alternative methods based on the detection of protein should also be addressed.
111) The Delegation of Brazil expressed the view that the validation of immunoassay methods should be considered, and that in Annex 1 more information should be included on the description of the method, such as: complete description of the primer, number of cycles, composition of cycles, equipment, amplicon length, type of polymerase and reference material.
112) The Delegation of Japan questioned the application of those criteria contained in the document to the detection of GMOs although they are applicable to chemical analysis.
113) The Delegation of Norway proposed to amend the section on the modular approach to reflect that it should not be used ”unless independence between the modules can be documented”, since it should not be systematically avoided.
114) The Delegation of Cuba drew the attention of the Committee to the issues related to consumer protection, that might need to be addressed by the Task Force in the future and in particular the level of transgenicity of the material.
115) The Committee discussed whether new work should be initiated in the Step Procedure in order to circulate for comments as soon as possible the document in Appendix I: Guidelines for the Validation and Quality Control Requirements for GMO Analyses.
116) Some delegations stressed the need to proceed rapidly as governments needed guidance on this very important and complex issue. Other delegations indicated that they had been part of the original Working Group but there had not been enough time to provide detailed comments and that it would be preferable to consider the text carefully before initiating the elaboration of specific guidelines.
117) The Committee agreed that the document would be revised by the Delegations of the United Kingdom and Germany with the assistance of a Drafting Group¹² for consideration at the next session, with a view to the elaboration of Guidelines.
METHODS OF ANALYSIS FOR THE DETERMINATION OF DIOXINS AND PCBS (Agenda Item 10)¹³
118) The Delegation of Germany expressed its deep regret that due to the lack of input it had not been possible to prepare a list of methods for determination of dioxins and PCBs for consideration at this session. The Delegation drew the attention of the Committee to the fact that the WHO and EC had started a joint project related to rapid assays for dioxins and related compounds (see CX/MAS 04/INF1) which would provide an additional input in preparing a more comprehensive list of methods for determination of the above compounds.
119) The Committee agreed that a Circular Letter would be prepared to seek information on the current methods used for determination of dioxins and related compounds. This information should be forwarded to Germany who would prepare a paper for consideration at the next session of the Committee.
REPORT OF AN INTER-AGENCY MEETING ON METHODS OF ANALYSIS AND SAMPLING (Agenda Item 11)¹⁴
120) The Chairman of the Inter-Agency Meeting (IAM) Dr Roger Wood introduced the draft report of the 16^th IAM and informed the Committee that CRD 2 was being presented mainly for information purposes and highlighted the following important issues discussed at the IAM.
121) It was indicated that the criteria approach had been adopted by the Commission and that the validation data would have to be made available to customers to ensure a successful application of this approach.
122) Dr Wood drew the attention of the Committee to the problem related to the application by laboratories of proficiency testing and noted that high level laboratories could provide reference values for particular difficult analyses.
123) The Committee was informed about the progress of the electronic compendium of analytical methods and that validated methods of analysis should be made generally available.
124) As regards the question of incorporation of changes to methods/method corrections in the Codex Alimentarius, it was indicated that the current system was retained.
125) The Committee was informed that the paper on harmonization of analytical terminology would be updated and available from the website.
126) Finally Dr Wood informed the Committee about the discussions on the Terms of Reference of the IAM and future changes in the Secretariat.
127) The Committee expressed its appreciation to the IAM and Dr Wood for their constructive work and contribution to the work of the Committee and noted that the final report would be made available from the website of AOAC.
OTHER BUSINESS AND FUTURE WORK (Agenda Item 12)
The Use of Analytical Results: Sampling Plans, Relationship Between the Analytical Results, the Measurement Uncertainty, Recovery Factors and Provisions in Codex Standards
128) The Committee recalled that it had agreed to consider the Guidelines redrafted by the Ad Hoc Working Group under Agenda Item 12 “Other Business and Future Work” (see also paras ‎6) to ‎13).
129) The Chairperson of the Ad Hoc Working Group presented the document and indicated that the text was substantively revised and it should give simple instructions to Commodity Committees regarding sampling, relationship between the analytical results, the measurement uncertainty, recovery factors and provisions in the Codex standards.
130) The Committee amended the title to reflect the view that the use of analytical results related not to sampling as such but rather to sampling plans.
131) The Delegation of New Zealand was of the view that there was a contradiction between the first and last paragraphs of the section on Issues Involved and this required further rewording for clarification purposes. It proposed several substantial amendments as follows. The section on Measurement Uncertainty was not sufficiently general, as this was not the only way to proceed, and should be addressed in a separate paper. The sampling plan should specify whether the specification applied to the average in a lot or the proportion of non-conforming; significant figures should not be addressed in the document as this question relates to reporting not to the use in conformity assessment.
132) The Committee amended the first paragraph in the Recommendations section to clarify that when Commodity Committees discuss and agree on a specification, the concerned analytical methods should also be stated.
133) Different views were expressed regarding the section on Recovery. The Delegation of Ireland drew the attention of the Committee to the fact that recovery was relevant to organic analysis especially when low levels were analysed and proposed to amend the sentence so that the analytical results are to be reported on recovery ”where relevant and appropriate”.
134) Some delegations proposed to delete this section while other delegations were of the view that the two first sentences from the earlier version of the document better reflected recommendations regarding recovery. The Committee agreed to amend this section as proposed by the Delegation of Ireland and retained it in square brackets for further discussion.

135) It was proposed to forward the document to the Committee on General Principles for their endorsement and subsequent adoption by the Commission and inclusion in the Procedural Manual as guidance to the Codex Commodity Committees. However the Committee noted that although the document was substantively improved, several issues remained to be addressed and there was a need for further consideration therefore decided to request comments on the current version and consider it at the next session of the Committee (see Appendix VII). It also agreed that the advice of Commodity Committee would be sought on this document.
FUTURE WORK
136) The Committee noted that, as a result of the discussions at the current session, the next session would consider the following items:
• Proposed Draft Guidelines for Evaluating Acceptable Methods of Analysis
• Consideration of the Fitness-For Purpose Approach to Evaluating Methods of Analysis
• The Use of Analytical Results: Sampling Plans, Relationship between the Analytical Results, the Measurement Uncertainty, Recovery Factors and Provisions in Codex Standards
• Proposed Draft Guidelines for Settling Disputes Over Analytical (Tests) Results
• Review of Analytical Terminology for Codex Use in the Procedural Manual
• Endorsement of Methods of Analysis Provisions in Codex Standards, including Conversion of Methods for Trace Elements into Criteria
• Criteria for the Methods for the Detection and Identification of Foods derived from Biotechnology
• Methods of Analysis for Determination of Dioxins and Related Compounds
• Report of an Inter-Agency Meeting on Methods of Analysis
DATE AND PLACE OF THE NEXT SESSION (Agenda Item 13)
137) The Committee was informed that the 26^th Session of the Committee would be held in Budapest from 4 to 8 April 2005. The exact venue would be determined by the host country and the Codex Secretariat.

SUMMARY STATUS OF WORK

(*) For inclusion in the Procedural Manual

¹ CX/MAS 04/2, CX/MAS 04/2-Add.1 (Prepared by the United Kingdom, for consideration in conjunction with Matters Referred from Other Codex Committees on the Use of the Analytical Results), CRD 4 (comments of Phillippines).

² Austria, Brazil, Canada, Czech Republic, Egypt, Finland, Germany, Japan, Netherlands, New Zealand, United States

³ ALINORM 03/23, Appendix IV, CL 2003/29-MAS, CX/MAS 04/3 (comments of European Community, Finland, Hungary, Japan, New Zealand, United States), CRD 4 (comments of the Philippines), CRD 6 (revised version prepared by the Ad Hoc Working Group)

⁴ ALINORM 03/23, Appendix V, CL 2003/29-MAS, CX/MAS 04/4 (comments of Finland, Ireland, Japan and New Zealand), CX/MAS 04/4-Add.1 (comments of Iran), CRD 4 (comments of the Phillippines)

⁵ ALINORM 03/23, Appendix VII, CL 2003/29-MAS, CX/MAS 04/5 (comments of Brazil), CRD 4 (comments of the Philippines)

⁶ CX/MAS 04/7, CRD 4 (comments of the Philippines), CRD 8 (comments of the United States)

⁷ CL 2003/43-MAS; CX/MAS 04/8 (comments of Cuba, France, Iran, United States of America); CX/MAS 04/8-Add.1 (comments of Japan, New Zealand); CRD 7 (comments of Austria); CRD 11 (comments of Brazil).

⁸ Anal. Bioanal. Chem (2003), 377: 1060 - 1060

⁹ Austria, Brazil, the EC, AOCS

¹⁰ CX/MAS 04/9, CX/MAS 04/9-Add.1, CX/MAS 04/9-Add.2 (coments of Canada), CRD 1 (report of the Working group on Endorsement), CRD3 (comments o AAC), CRD 10 (comments of Brazil)

¹¹ CX/MAS 04/10, CRD 9 (comments of the United States)

¹² Argentina, Australia, Brazil, Canada, Egypt, European Community, France, Iran, Ireland, Italy, Japan, Malaysia, Netherlands, Norway, Philippines, United States, AOAC, AOCS, BIO, CROPLIFE International, EUROPABIO and ISO

¹³ CX/MAS 04/INF 1 (Draft report on the Symposium on Rapid Assays for Dioxins and related Compounds)

¹⁴ CRD 2 (Report of the 16^th Meeting of international organizations working in the field of methods of analysis and sampling (Inter-Agency Meeting)