Comparative Testing Report on the Detection and Quantification of Maize Events GA21, TC1507 and MIR604

In the frame of Regulation (EC) No 882/2004, the European Union Reference Laboratory for Genetically Modified Food and Feed has the duty to organise comparative testing rounds and to ensure an appropriate follow-up of these activities. This preliminary report describes the outcome of the fourth comparative testing round ILC-EURL-GMFF-CT-02/11. Participants were required to screen two test items denoted maize powder levels 1 and 2, for the presence of maize events 3272, Bt11, Bt176, 59122, GA21, MIR604, MON 810, MON 863, NK603 and TC1507. Any events detected were then to be quantified. This comparative testing round was organised in collaboration with the Food Safety and Quality Unit of the Institute for Reference Materials and Measurements (Geel, BE). The maize test items were produced in-house. The Food Safety and Quality Unit managed the on-line registration and submission of results. A total of 159 laboratories were invited to participate in ILC-EURL-GMFF-CT-02/11. Participants could report the results of the exercise either in mass/mass % or in copy/copy %. In this fourth comparative testing round greater than 86 % of participants gained a satisfactory z-score in the range of -2 to +2 for the results expressed in mass/mass % for both maize powder levels 1 and 2 regardless of the GM event. However, a lower percentage (43–86 %) of z-scores within the working range of -2 to +2 was calculated for those participants that expressed the results in copy/copy %.JRC.I.3-Molecular Biology and Genomic

Comparative Testing Report on the Quantification of Maize Line DAS-59122-7 and Oilseed rape Line GT73 (RT73) - Comparative testing round: ILC-EURL-GMFF-CT-01/12

In the frame of Regulation (EC) No 882/2004, the European Union Reference Laboratory for Genetically Modified Food and Feed has the duty to organise comparative testing rounds and to ensure an appropriate follow-up of these activities. This report describes the outcome of the fifth comparative testing round ILC-EURL-GMFF-CT-01/12. Participants had to determine the content of oilseed rape event GT73 and maize event 59122 in two test items denoted genomic DNA levels 1 and 2, containing different GM percentages of both GM events. This comparative testing round was organised in collaboration with the Food Safety and Quality Unit of the Institute for Reference Materials and Measurements (Geel, BE). The test items were produced in-house. The Food Safety and Quality Unit managed the on-line registration and submission of results. A total of 160 laboratories were invited to participate in ILC-EURL-GMFF-CT-01/12. Eighty laboratories from 36 countries returned results, of which 59 were National Reference Laboratories, six were only members of the European Network of GMO Laboratories, three were only Official control laboratories and 12 were laboratories from third countries. Five laboratories including one National Reference Laboratory and four laboratories from third countries did not submit results. In this fifth comparative testing round 92 % to 98 % of participants gained a satisfactory z-score in the range of -2 to +2 for the results expressed in mass/mass % depending on the GM content and the GM event. However, a lower percentage (38 – 93 %) of z-scores within the working range of -2 to +2 was calculated for those participants that expressed the results in copy/copy %.JRC.I.3-Molecular Biology and Genomic

IMEP-26: Determination of Brominated Flame Retardants in Plastic

This report presents the results of an interlaboratory comparison (ILC) which focussed on the determination of total bromine, total sum of polybrominated biphenyls (PBB), total sum of polybrominated diphenylethers (PBDE), brominated diphenylethers (BDE-47, BDE-99, BDE-183 and BDE-209) and decabrominated biphenyl (BB-209) in plastic. The test material used in this exercise was the Quality Control material (IRMM-310) from the Institute for Reference Materials and Measurements (IRMM) a poly(ethyleneterephthalate) (PET) granulated that has been fortified with commercially available technical mixtures of polybrominated diphenylethers and polybrominated biphenyls. The material was relabelled to avoid its recognition. Twenty-five laboratories from 15 countries registered to the exercise, from which 23 reported results. The informative values provided by the IRMM-310 material information sheet were taken as the assigned values and their associated uncertainties for all measurands. Studies to asses the adequacy of the selected test material regarding its homogeneity for all the selected measurands were undertaken Participants were invited to report the uncertainty of their measurements. Laboratory results were rated with z- and ζ-scores (zeta-scores) in accordance with ISO 13528. The standard deviation for proficiency assessment was fixed to 25 % of the respective assigned value by the advisory board of this ILC. The outcome of the exercise was illustrating quite well the difficulties laboratories do have to provide consistent values for the investigated measurands; the share of satisfactory z-scores ranged between 61 and 88 %. There was a clear tendency to underestimate most of the measurands. The most influencing variables, leading to the observed variability and lack of trueness, were investigated.JRC.DG.D.6-Food Safety and Qualit

IMEP-40: Determintion of trace elements in seawater

Fifty-three participants from twenty-nine countries registered to the exercise. Seven participants did not report results. The test item used was a seawater sample containing the trace elements As, Cd, Co, Cr, Cu, Fe, Mn, Mo, Ni, Pb, Se and Zn. Laboratories with demonstrated experience in the field provided results to establish the assigned values (Xref). The standard uncertainties associated to the assigned values (uref) were calculated according to ISO Guide 35. Laboratory results were rated with z- and zeta (ζ-) scores in accordance with ISO 13528. The standard deviation for the proficiency assessment, , for all elements was based on the experience in the Water Framework Directive and was set at 25 %. The trace elements were present in very low concentration levels (low μg L-1 range equal to natural contamination levels) and therefore many laboratories reported "lower than" values. The percentage of satisfactory z-scores ranged from 41 % (Cr, Fe) to 86 % (Mo). The low concentration levels of the trace elements in a difficult matrix (high saline content) need to be taken into consideration to understand the general low rate of satisfactory scores. Laboratories that score systematically too high should examine the cause of this positive bias.JRC.D.5-Standards for Food Bioscienc

IMEP-42: Determination of PFASs in fish

The Institute for Reference Materials and Measurements of the Joint Research Centre, a Directorate General of the European Commission (EC-JRC-IRMM) operates the International Measurement Evaluation Programme (IMEP). It organises interlaboratory comparisons (ILC's) in support to European Union (EU) policies. This report presents the results of a proficiency test (PT), IMEP-42, on the determination of perfluoroalkyl substances (PFASs) in fish tissue. The exercise was organised in support to the Commission Recommendation 2010/161/EU on the monitoring of perfluoroalkylated substances in food and the Water Framework Directive 2000/60/EC. Seventeen participants from thirteen countries registered to the exercise and all of them reported results. The test item was fish tissue (pike-perch) containing perfluoroalkyl carboxylates as perfluorononanoic acid (PFNA), perfluorodecanoic acid (PFDA), perfluoroundecanoic acid (PFUnDA), perfluorododecanoic acid (PFDoDA), perfluorotridecanoic acid (PFTrDA) or perfluorotetradecanoic acid (PFTeDA); perfluoroalkyl sulfonates as perfluorohexanesulfonate (PFHxS), linear perfluorooctane sulfonate (L-PFOS) or branched perfluorooctane sulfonate (br-PFOS); and, perfluoroalkyl sulphonamides as perfluorooctane sulphonamide (FOSA). The test item was a candidate certified reference material (CRM) produced by IRMM under ISO Guide 34 accreditation and in line with ISO Guide 35. Laboratories with demonstrated experience in the field provided results to establish the assigned values (Xref). The standard uncertainties associated to the assigned values (uref) were calculated according to the ISO Guide 35 by combining the uncertainty of the characterisation (uchar) with a contribution for homogeneity (ubb) and for stability (ust). Laboratory results were rated with z- and zeta (ζ-) scores in accordance with ISO 13528. The standard deviation for the proficiency assessment, σ ̂, for all elements was set at 25 % of the respective assigned value. The overall performance in this PT was good even though analyte dependent. High rates (78% - 100%) of satisfactory performances expressed as z-scores ≤ 2 were obtained for L-PFOS, PFDA, PFUnDA, PFDoDA, tot-PFOS and FOSA while the lowest rates of satisfactory performances (50%) were obtained for br-PFOS and PFTrDA. Many "less than X" values were reported for the three PFASs that could not be scored due to the high uncertainty on the assigned value (PFNA, PFTeDA and PFHxS). The results in this PT showed that the sensitivities of the methods used by the participants were fit for the purpose of measuring the legal limits set in legislation.JRC.D.5-Standards for Food Bioscienc

IMEP-37: Determination of pesticides in grapes - Interlaboratory Comparison Report

This report presents the results of a proficiency test exercise (PT) which focussed on the determination of pesticides in grapes in support of Regulation 396/2005/EC of the European Parliament and of the Council on maximum residue levels of pesticides in or on food and feed of plant and animal origin. Eighty-seven participants from thirty-three different countries registered to the exercise, of which eighty-one reported results. From these eighty-one participants, forty were from EU countries while forty-one were from outside the EU. The test item was a grapes sample spiked with 20 selected pesticides. The assigned values were obtained as the average of results reported by five expert laboratories having demonstrated experience in the analysis of pesticides in vegetable and fruit matrices. The standard uncertainties related to the assigned values (Uref) were calculated by combining the uncertainty of the characterisation (Uchar) with a contribution for homogeneity (Ubb) and for stability (Ust). Uchar was calculated following the ISO guide 35. Laboratory results were rated with z- and zeta (ζ-) scores in accordance with ISO 13528 and ISO 17043. The z-score compares the participant's deviation from the reference value with the standard deviation for proficiency assessment (σp) used as common quality criterion, the ζ-score states if the laboratory result agrees with the assigned value within the respective uncertainty. The standard deviation for the proficiency assessment, σp, was set by the advisory board of this PT at 25% for the 20 measured pesticides based on previous experience with similar measurands. Participants were not scored for triadimenol due to the large Uref associated to the assigned value. According to the results obtained in the frame of the IMEP-37 study, the participants performed satisfactorily for the 19 scored pesticides ranging from 81 % (carbendazim) to 97 % (azoxystrobin, penconazole, pyrimethanil) of satisfactory z-scores. When analysing the results of the group of non-EU countries separately, similar results were obtained. It can be concluded that the performance in this PT is satisfactory for the laboratories world-wide.JRC.D.5-Standards for Food Bioscienc

IMEP-38: Determination of total As, Cd, Pb, and Hg in compound feed - Interlaboratory Comparison Report

The Institute for Reference Materials and Measurements (IRMM) of the Joint Research Centre, a Directorate General of the European Commission, operates the International Measurement Evaluation Programme (IMEP). IMEP organizes interlaboratory comparisons (ILCs) in support to EU policies. This report presents the results of the proficiency test (PT) which focused on the determination of total As, Cd, Pb and Hg in compound feed according to Directive 2002/32/EC of the European Parliament and of the Council on undesirable substances in animal feed. The IMEP-38 exercise was organized aiming to assess the performance of food and feed control laboratories and official control laboratories. The test material used in this exercise was commercially available compound feed for cats which after the appropriate processing was spiked, bottled, labelled, numbered accordingly and dispatched to the participants on the 27th of June 2013. Forty-seven laboratories from 24 countries registered to the exercise of which 44 reported results and answered the respective questionnaire. The percentage of satisfactory z-scores ranged from 58 % (total arsenic) to 74 % (total cadmium) and the ζ-scores obtained were lower by 10 to 21%.JRC.D.5-Standards for Food Bioscienc

Determination of total As, Cd, Pb and Hg in vegetable feed: IMEP-119 Proficiency Test Report

This report presents the results of a PT (IMEP-119) of the EURL-HM focussing on the determination of total As, Cd, Pb and Hg in vegetable feed in support to Directive 2002/32/EC of the European Parliament and of the Council on undesirable substances in animal feed. IMEP-119 was also opened to all laboratories who wish to take part in the exercise as a way to benchmark their performance against NRLs and other laboratories. One hundred and two participants from 45 countries registered to the exercise. Only eight participants did not report their results. Laboratory results were rated using z- and zeta (ζ-) scores in accordance with ISO 13528. The relative standard deviation for proficiency assessment was set to 15 % for the total As, Cd and Pb mass fractions, and to 22 % for the total Hg mass fraction, respectively. An overall adequate performance for NRLs and feed control laboratories is shown by the percentage of satisfactory performance (expressed as z-scores). These percentages were ranging from 93 to 74 % for NRLs and from 92 to 69 %, for feed control laboratories, respectively.JRC.D.5-Standards for Food Bioscienc

IMEP-34: Heavy Metals in Toys according to EN 71-3:1994

The Institute for Reference Materials and Measurements (IRMM) of the Joint Research Centre (JRC), a Directorate-General of the European Commission, operates the International Measurement Evaluation Programme (IMEP). It organises interlaboratory comparisons (ILC's) in support to EU policies. This report presents the results of an ILC which focussed on the determination of soluble antimony (Sb), arsenic (As), barium (Ba), cadmium (Cd), chromium (Cr), lead (Pb), mercury (Hg), and selenium (Se) according to European Standard EN 71-3:1994. The principle of the procedure in EN 71-3:1994 [1] consists in the extraction of soluble elements from toy material under the conditions simulating the material remaining in contact with stomach acid for a period of time after swallowing. Fifty eight participants from twenty six countries registered to the exercise, of which 54 reported results for As, Sb, Ba, Se and Hg and 58 for Cr, Pb, and Cd, respectively. The test item used was a certified reference material (CRM 623, comminuted paint flakes from alkyd resin paint), certified in 1998, which is not included anymore in the CRM catalogue. The validity of the certified values was assessed using some expert laboratories in the field. In most of the cases the results reported by the certifiers were not in agreement with the CRM reference values. The mean of the means reported by the expert laboratories was used as assigned value for the different measurands. The results reported by the expert laboratories for mercury were very scattered (RSD = 37.6 %). No assigned value could be attributed for mercury and therefore no scores were provided to the participants for this measurand. The associated uncertainties of the assigned values were obtained following the ISO GUM. Furthermore, participants were invited to report their measurement uncertainties. This was done by all laboratories having submitted results in this exercise. Laboratory results were rated with z- and zeta (ζ-) scores in accordance with ISO 13528. The standard deviations for proficiency assessment were based on the analytical correction laid down in EN 71-3:1994. The outcome of the exercise shows an improvement on the overall performance of the participants when compared to IMEP-24 (a proficiency test for heavy metals in toys run in 2009 in which, the same European standard was followed), particularly for cadmium, lead and to a lesser extent, for selenium and chromium. The share of satisfactory z-scores ranged from 65 to 79 %.JRC.D.5-Food Safety and Qualit

IMEP-35: Determination of Total Lead in Lipsticks (Interlaboratory Comparison Report)

The Institute for Reference Materials and Measurements (IRMM) of the Joint Research Centre (JRC), a Directorate-General of the European Commission, operates the International Measurement Evaluation Programme (IMEP). It organises interlaboratory comparisons (ILCs) in support to EU policies. This report presents the results of a proficiency test exercise (PT) focussed on the determination of total lead in lipsticks which was organised in support of the European Council Directive 79/768/EEC (1976).JRC.D.5-Standards for Food Bioscienc