CRD 16 Codex Committee on Methods of Analysis and Sampling (29th Session) Budapest, Hungary (10-14 March 2008) European Community Comments on items 2, 3a, 4 and 5b 1
European Community comments on the Matters referred by the Codex Alimentarius Commission and other Codex Committees (Agenda item 2, CX/MAS 08/29/2) Mixed Competence Member States Vote The European Community and its Member States are pleased to offer the following comments on Agenda item 2. A. GENERAL DECISIONS OF THE COMMISSION 1. Strategic Plan 2008-2013 of the Codex Alimentarius Commission EC comment on activity 1.4: The ECMS fully support the importance of the development and maintenance of Codex standards listing available methods of analysis and sampling with a global overview under the responsibility of a dedicated committee ensuring that scientific and technological developments are taken into account while keeping in mind the limited resources of developing countries. EC comment on activity 2.5: The ECMS note that some concerns were recently raised as regards the financial resources devoted by FAO and WHO to the provision of scientific advice and 2
therefore welcome a rationalisation of the process in order to make the best use of the limited resources available. In that regard, the ECMS welcome the Global Initiative for Food-related Scientific Advice as an initiative being taken to ensure sustainable funding of the programmes of FAO and WHO on the provision of scientific advice to the Codex Alimentarius Commission and member countries. EC comment on activity 3.3: The ECMS would favour the development of priority-setting criteria and the recourse to an efficient mechanism to prioritise the list of proposals for new work, although it is recognised that part of CCMAS activities are depending on the work of other committees. EC comment on activity 4.1: The ECMS note that CCMAS has established a high level of cooperation with other international organisations involved in methods of analysis and sampling such as ISO and AOAC. EC comment on activity 5.5: The ECMS are in favour of an enhanced participation of nongovernmental organizations in the Codex work. 3
EC comment on activity 5.6: The ECMS are of the opinion that an important effort should be made to develop new communication approaches about Codex work. B. DECISIONS OF THE COMMISSION RELATED TO THE WORK OF THE COMMITTEE 1. Committee on Fresh Fruits and Vegetables Draft Guidelines for the Inspection and Certification of Fresh Fruits and Vegetables for Conformity to Quality Standards The proposed draft Codex Guidelines for the Inspection and Certification of Fresh Fruits and Vegetables for Conformity to Quality Standards were progressed to step 5 by the 30 th Session of the CAC and transmitted to CCFICS and CCMAS for observations on consistency within Codex. A Working Group led by Canada works electronically on the revision of the document in order to provide a revised version that will be circulated again for further comments at Step 6 and consideration by the next session of CCFFV. It was noted that there might be a need for a physical meeting of the Working Group. At last session of CCFFV, the ECMS suggested that the Committee cross references to the new OECD "Scheme" rather than continuing to work on the Guidelines. However this approach was not supported by the other members, who, recognizing the good work and progress that had been made on the revision, were in favour of progressing the document. The ECMS believe that the language of the draft guidelines is sometimes overly prescriptive and stringent and would suggest the Committee to recommend CCFFV to fully consider the OECD Scheme in order to avoid contradictions and duplication of work. 2. Committee on Sugars Standard for Sugars: Method for Determination of Colour in Plantation and Mill White Sugar The ECMS support the CCS recommendation that Method GS9/1/2/3-8 (2005) should be applied to the determination of colour for all sugars covered by the Standard including plantation or mill white sugar (PMWS). [EC comments in response to CL 2006/32 CS (12/12/06)] The recommendation concerning the possibility to continue to apply method GS2/3-10 (2005) for colour determination of white sugars with a maximum colour of 50 IU as a simpler and more environmentally friendly alternative method at national or regional level can also be supported. 4
C. MATTERS REFERRED BY OTHER COMMITTEES AND TASK FORCES 1. Committee on Contaminants in Foods The European Community submitted to CCCF the data contained in Annex 2 of CX/MAS 08/29/2 and would welcome progress from CCMAS on methods for the determination of dioxins and PCBs. 2. Ad hoc Intergovernmental Task Force on Foods Derived from Biotechnology The ECMS fully support the need for urgent completion of the work on the detection and identification of foods derived from biotechnology. 3. Committee on Milk and Milk Products Discussion Paper on sampling plans for milk products in presence of significant measurement error The ECMS would favour an horizontal approach by CCMAS of this issue. This could take the form of an amendment of the General Guidelines on Sampling. 5
European Community comments on the Draft Guidelines for Evaluating Acceptable Methods of Analysis (Agenda item 3a, CX/MAS 08/29/3) Mixed Competence Member States Vote The European Community and its Member States (ECMS) note that the Delegation of New Zealand is currently in the process of preparing 3 scientific papers to be published in scientific publications as agreed during the 28 th Session of CCMAS. The ECMS therefore believe that this agenda item should still be held at step 7 until publication of the scientific papers. 6
European Community comments on the Proposed Draft Guidelines on Analytical Terminology for Codex Use (Agenda item 4, CX/MAS 08/29/5) Mixed Competence Member States Vote The European Community and its Member States (ECMS) wish to commend the Delegation of the United States for leading the electronic Working Group which produced the new version of the Proposed Draft Guidelines on Analytical terminology for Codex Use. The ECMS globally support the proposed definitions but would however like to propose the following comments: - Page 3, Appendix I, SPECIFIC ANALYTICAL TERMS, 1 st sentence of the para. There is stated, that The following analytical terms are used in the Procedural Manual (PM) and are defined below:. Nevertheless, some of these terms are not mentioned in the PM (e.g. Empirical method of analysis ). Moreover the definition of Empirical method of analysis is close to the definition of Defining method (Type I) in the PM. This might be confusing. The ECMS propose to delete the term and definition of Empirical method of analysis from Appendix I. - Page 6: The ECMS wish to propose an amended definition for the limit of detection as follows. The present definition is "The detection limit is conventionally defined as field blank + 3σ, where σ is the standard deviation of the field blank value signal (IUPAC definition)". This definition creates problems when the blank value is giving a significant contribution to the limit of detection, which is fairly common in e.g. trace element analysis. In such cases the mean blank level is deducted from the analytical reading, before the result is calculated, and not included in the limit of detection. The ECMS therefore propose to complement or replace the present definition with the following: "Limit of detection: smallest measured content, from which it is possible to deduce the presence of the analyte with reasonable statistical certainty. The limit of detection is numerically equal to three times the standard deviation of the mean of blank determinations (n > 20)." - Page 12, Appendix II, 1 st sentence of the para. + List of terms below - There is stated, that These terms were not included in CL 2007/10-MAS, but should be further evaluated by the Committee for inclusion in the guideline. Nevertheless, some of these terms were included in CL 2007/10-MAS (e.g. Bias, Applicability, Limit of Quantification) and they are even already included in Appendix I. Moreover some of the terms in the Appendix II are very similar or almost the same like terms in the Appendix I (Limit of detection/detection limit, Limit of Quantification/Quantification limit...). The ECMS support the terms and definitions in the Appendix I and propose to delete the terms Bias, Applicability (and practicability), Detection limit and Quantification limit from Appendix II. 7
European Community comments on the Conversion of Methods for Trace Elements into Criteria/Guidelines on establishing Methods Criteria for the Identification of Relevant Analytical Methods (Agenda item 5b, CX/MAS 08/29/7) Mixed Competence Member States Vote The European Community and its Member States (ECMS) wish to commend the working group for the result achieved. The guidelines have now a clearer structure; the scope has been widened to other fields of analysis than element analysis and specific criteria (values) have been established to make it possible to evaluate the acceptability of existing methods on one hand and to develop methods that will be accepted as suitable if the criteria are fulfilled, on the other hand. The ECMS fully support the initiation of new work in that field. General Remarks The limits or ranges chosen for the criteria Recovery and Precision are quite wide. The possibility of a real and effective evaluation of the proficiency of the method might be very limited or not be possible any more. EC Commission Decision 2002/657/EC laying down criteria for performance of analytical methods in residue control in food of animal origin might also contain some useful information in this context. We would like to suggest not prescribing specific concentration dependent ranges for recovery rates. Otherwise, if it stands as in the current version one has to be aware of some inconsistencies with EU legislation. Nevertheless it should be requested that the recovery rate is given since not the recovery rate itself but its reproducibility is of importance. Within the criteria it should be taken care that the recovery rate is not bigger than 100% plus the relative reproducibility of the method. We would like to advise to thoroughly check whether the suggested values/limits for the criteria can be transferred without any adaptations to other fields of analysis or other substance groups. As mentioned above, using the criteria as currently given in the tables in some cases this might lead to values that are not consistent with EU legislation. For example this is the case with the maximum limit given for benzoapyrene in Regulation (EC) No. 1881/2006. The maximum limits vary from 1 to10 μg/kg. According to the Codex-criteria a method suitable for processed cereal based food should have a LOD of less than 0.2 μg/kg; for a method suitable for molluscs a LOD of 2 μg/kg would be sufficient. To the contrary, according to Regulation (EC) No. 333/2007 the LOD for all methods for benzoapyrene regardless of the matrix to be analysed have to be lower than 0.3 μg/kg. According to the EC regulation the recovery rate may vary between 50 and 120 %. The Codexcriteria allow for only 80 to 110 % in this concentration range. Similar deviations have to be noted with inorganic tin. Maximum levels for tin in canned foods are set to 200 mg/kg, for canned beverages to 100 mg/kg (Regulation (EC) No. 1881/2006). Following the Codex-criteria methods 8
with a LOD of less than 20 and 10 mg/kg, respectively, are suitable. According to Regulation (EC) No. 333/2007 the LOD must be lower than 5 mg/kg in all cases. When suggesting to alternatively calculate a minimum applicable concentration range instead of a numeric value for LOD and LOQ, what are the reasons for discriminating between ML below and above 0.1 mg/kg as concerns the coverage factor? Why not use a coverage factor of 3 for concentration below 0.1 mg/kg as well? Specific comments p 3 Table Recovery The last three lines third column should read 100 μ(micro)g/kg, 10 μ(micro)g/kg, 1μ(micro)g/kg Trueness z-score calculation, using data from proficiency testing (Laboratory-Performance Studies; definition in Procedural Manual 16th ed. p 81) should not be used. For the evaluation of the trueness preferably Certified Reference Material should be used. If this material is unavailable, data from Method-Performance Studies might be used. p 4 CONVERSION OF SPECIFIC METHODS OF ANALYSIS TO METHOD CRITERIA BY THE CCMAS - there is no definition of the term collaborative trial. For more clarity it should be replaced by the term Method-Performance Study. p 5-Note: The paragraph note was already omitted in the Procedural Manual 16th ed. p 7 - second last para - Note- the term Performance Studies is not precise; if Method-Performance Studies is meant this term should be used here. - last para for more clarity instead of the applicable level. It should read The minimum applicable concentration range and the expression expected variation should be described more precisely. p 8 - first para - second last line should read: for concentrations at or above 10-7 ( 0.1 mg/kg ) For concentrations lower than 0.1 mg/kg, a coverage factor of 2 could be recommended. - in Table 1- the figures given for the lower and upper level of the minimum applicable range in column 5, 7, 8 are not understandable. (e.g. calculating the range for a ML of 10mg/kg according to the formula leads to ±3.39, resulting in 6.6 and 13.4 for the lower and upper level, respectively.) - second last para - the recommendation is not in line with Regulation (EC) No. 333/2007 as far as inorganic tin is concerned (see above). p 9 second para et seqq. the formula should read ML k. s R. - third para the expression precision requirement should be described more precisely. In the last line for this para needs to be deleted. 9
p 9 The precision - in the sentence The numeric value for the criteria on precision is based on the concentration range of ML delete range, since MLs are no ranges but specific values. Table 2 for uniformity of the terms used, it would be better to use unity uniformly instead of concentration range. Compare to Table 4 p 10 Table 4 for uniformity give either concentration ranges or only one concentration throughout column 1 as well as column 3. e.g. 10 in column 1 corresponds to 10% in column 3. Table 4 In the headline as well as in column 4 it should read Recovery range. para Trueness delete results from proficiency tests. For reason, see above. In the sentence One way of measuring trueness is by use of z-score (proficiency tests) or zeta-score (collaborative studies) which express the difference between the obtained and true value including the uncertainty thereof. delete z-score (proficiency tests) or. For reason see above. replace (collaborative studies) by (method-performance studies). For reason see above. put true value in quotation marks or replace by the term consensus value p12 HOW TO ELUCIDATE A METHOD S COMPLIANCE WITH THE CRITERIA last sentence: replace have to be applied by have to be evaluated for clarity. p 12 -Table 7 - in method 1 a HorRat-Ratio of 2 is exceeded (2 x RSD TR at a concentration of 2.2 mg/kg < 36 ) - in method 11 an RSDR (up to 47%) is not in conformity with the criteria and therefore is to be categorized as not suitable. p 13 Conclusion method 11 is not suitable. For reason see above. Note solely method 10 fulfils the criterion of showing satisfactory performance around the ML p 13 - CRITERIA FOR METHODS FOR DIOXINS AND DIOXIN-LIKE PCBs Para 3 in the last sentence the maximum level varies between 1.5 and 10.0 pg/g (μg/kg) fat for different foodstuffs. It should read: varies between 1.5 and 12.0 pg/g (ng/kg) fat or wet weight. there are a few inconsistencies comparing the criteria set in Regulation (EC) No. 1883/2006 and the Codex-criteria. E.g. allowable range for the recovery rate is 60-120 % compared to 40-120% and RSD R (ΣTEQ) < 15 % compared to RSD R < 44 %. p 14 RECOMMENDATIONS For the whole section the above mentioned should be logically taken in consideration. p 24 - METHODS ENDORSED BY CODEX; HOWEVER SHOULD BE LOOKED AT AGAIN para 3 instead of the methods are tested o levels all below LOD,.. it should probably read below LOQ. Compare to table p 19. 10