TY - JOUR A1 - Bilsel, M. A1 - Goren, A.C. A1 - Gokcen, T. A1 - Gunduz, S. A1 - Koch, Matthias A1 - Kaloulides, E. A1 - Giannikopoulou, P. A1 - Wai-Tong, G.T. A1 - Chan, A. T1 - Report on key comparison CCQM-K138: determination of aflatoxins (AFB(1), AFB(2), AFG(1), AFG(2) and total AFs) in dried fig JF - Metrologia N2 - The presence of any aflatoxin contamination in exported figs needs to be monitored and measured through reliable and traceable methods, which require pure and matrix certified reference materials. On the other hand, certified reference materials (CRM) for determination of aflatoxins in dried fig are not yet available. Moreover, there is a lack of CRMs to be used in routine testing laboratories for method validation and quality control. The routine testing laboratories, participating in commercial proficiency testing (PT) programs, use the results available from consensus values to evaluate the performance of the participating laboratories, rather than metrologically traceable assigned values. This study initially proposed as a key comparison and presented at the EURAMET TC-MC SCOA meeting in Malta in 2015 and subsequently at the CCQM OAWG meeting in April 2015, proposes a CRM candidate for determination of levels of aflatoxins B1, B2, G1, G2 and their total in dried. Evidence of successful participation in formal, relevant international comparisons are needed to document measurement capability claims (CMCs) made by national metrology institutes (NMIs) and designated institutes (DIs). In total nine NMI/DI participated in the Track C Key Comparison CCQM-K138 Determination of aflatoxins (AFB1, AFB2, AFG1, AFG2 and Total AFs) in Dried Fig. Participants were requested to evaluate the mass fractions expressed in ng/g units, of aflatoxins B1, B2, G1, G2 and total aflatoxin in a dried food matrix, dried fig. The CCQM-K138 results for the determination of aflatoxins (AFB1, AFB2, AFG1, AFG2 and total AFs) are ranging from 5.17 to 7.27 ng/g with an %RSD of 10.47 for AFB1, ranging from 0.60 to 0.871 ng/g with an %RSD of 11.69 for AFB2, ranging from 1.98 to 2.6 ng/g with an %RSD of 10.36 for AFG1, ranging from 0.06 to 0.32 ng/g with an %RSD of 35.6 for AFG2, and ranging from 8.29 to 10.31 ng/g with an %RSD of 7.69 for Total AFs. All participants based their analyses on LC-MS/MS, HPLC-FLD, HR-LC/MS, and IDMS. Brief descriptions of the analytical methods used by the participants, including sample preparation, analytical technique, calibrants, and quantification approach are summarized in Appendix F. Linear Pool was used to assign the Key Comparison Reference Values (KCRVs) for B1, B2, G1, G2 and total aflatoxins. Due to the traceability requirements for the calibrants not being met, results of KEBS, INTI, VNIIM and BAM were excluded from KCRV determination. Successful participation in CCQM-K138 demonstrates the following measurement capabilities in determining mass fraction of organic compounds, with molecular mass of 100 g/mol to 500 g/mol, having high polarity (pKow > -2), in mass fraction range from 0.05 ng/g to 500 ng/g in dried food matrices. KW - Aflatoxins KW - Mycotoxins KW - Dried fig KW - Food contaminants PY - 2019 DO - https://doi.org/10.1088/0026-1394/56/1A/08008 SN - 0026-1394 SN - 1681-7575 VL - 56 IS - 1A SP - 08008-1 EP - 08008-106 PB - IOP CY - Bristol AN - OPUS4-50326 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bilsel, M. A1 - Gökçen, T. A1 - Binici, B. A1 - Isleyen, A. A1 - Piechotta, Christian A1 - Kar-wai, A. A1 - Krylov, A. A1 - Miheeva, A. A1 - Beliakov, M. A1 - Palagina, M. A1 - chenko, Irina Tka A1 - Perkola, N. A1 - Lewin, M. A1 - Hua, T. T1 - High polarity analyte(s) in aqueous media: determination of L-PFOA and L-PFOS in ground water JF - Metrologia N2 - The CCQM-K156 comparison was coordinated by TUBITAK UME on behalf of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) for National Measurement Institutes (NMIs) and Designated Institutes (DIs) which provide measurement services in organic analysis under the 'Comité International des Poids et Mesures' Mutual Recognition Arrangement (CIPM MRA). Perfluoro alkyl substances (PFAS) such as PFOS and PFOA have been used in numerous industrial applications and products. Because of their high stability and resistance to biodegradation, atmospheric photooxidation, direct photolysis and hydrolysis, they are extremely persistent in the environment. The European Union (EU) Water Framework Directive lists PFOS as a priority hazardous substance that poses a significant risk to the aquatic environment. The use of PFOS-containing Aqueous Film-Forming Foams (AFFFs) has been banned since June 2011 in the EU. As relatively water-soluble, effectively non-degradable compounds, PFOS and PFOA migrate to ground water. They are not removed in the conventional drinking water treatment, and therefore cause health risks in polluted areas. The EU Drinking Water Directive and the European Commission has proposed a limit value of 100 ng/L for the sum of 20 PFAS, including PFOS and PFOA. This study provides the means for assessing measurement capabilities for determination of high polarity measurands in a procedure that requires extraction, clean-up, analytical separation and detection. Successful participation in CCQM-K156 demonstrates measurement capabilities in determining mass fraction of organic compounds, with a molecular mass of 200 g/mol to 700 g/mol, having high polarity pKow -2, in a mass fraction range from 0.5 ng/kg to 500 ng/kg in aqueous media. Nine NMIs and DIs participated in the CCQM-K156 key comparison. Seven institutes reported their results. SPE was applied in the sample pre-treatment and LC-MS was applied for detection. All participating laboratories applied isotope dilution mass spectrometry (IDMS) techniques for quantification. Participants established the metrological traceability of their results using certified reference materials (CRMs) from NMIs with stated traceability; where commercially available high purity materials were used the purity was determined in-house. The CCQM-K156 results for L-PFOA and L-PFOS range from 2.75 ng/kg to 5.50 ng/kg with a % RSD of 19.5 % for L-PFOA and from 2.04 ng/kg to 4.45 ng/kg with a % RSD of 21.3 % for L-PFOS. The KCRV was assigned using a Hierarchical Bayesian Random Effects Model (HB REM) estimator from the values reported by six of the participants. One participant result of L-PFOS and one result of L-PFOA were excluded from the KCRV for technical reasons. The KCRV was 4.9 ng/kg ± 0.4 ng/kg for L-PFOA and 3.8 ng/kg ± 0.4 ng/kg for L-PFOS. The six institutes that were included in the assignment of consensus KCRV all agreed within their standard uncertainties. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA). KW - PFAS KW - Surface water KW - ILC KW - CCQM PY - 2022 DO - https://doi.org/10.1088/0026-1394/59/1A/08016 VL - 59 IS - 1A SP - 1 EP - 3 PB - IOP Publishing AN - OPUS4-58941 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Westwood, S. A1 - Martos, G. A1 - Josephs, R. A1 - Choteau, T. A1 - Wielgosz, R. A1 - Davies, S. A1 - Moawad, M. A1 - Tarrant, G. A1 - Chan, B. A1 - Alamgir, M. A1 - de Rego, E. A1 - Wollinger, W. A1 - Garrido, B. A1 - Fernandes, J. A1 - de Sena, R. A1 - Oliveira, R. A1 - Melanson, J. A1 - Bates, J. A1 - Mai Le, P. A1 - Meija, J. A1 - Quan, C. A1 - Huang, T. A1 - Zhang, W. A1 - Ma, R. A1 - Zhang, S. A1 - Hao, Y. A1 - He, Y. A1 - Song, S. A1 - Wang, H. A1 - Su, F. A1 - Zhang, T. A1 - Li, H. A1 - Lam, W. A1 - Wong, W. A1 - Fung, W. A1 - Philipp, Rosemarie A1 - Dorgerloh, Ute A1 - Meyer, Klas A1 - Piechotta, Christian A1 - Riedel, Juliane A1 - Westphalen, Tanja A1 - Giannikopoulou, P. A1 - Alexopoulos, Ch. A1 - Kakoulides, E. A1 - Kitamaki, Y. A1 - Yamazaki, T. A1 - Shimizu, Y. A1 - Kuroe, M. A1 - Numata, M. A1 - Pérez-Castorena, A. A1 - Balderas-Escamilla, M. A1 - Garcia-Escalante, J. A1 - Krylov, A. A1 - Mikheeva, A. A1 - Beliakov, M. A1 - Palagina, M. A1 - Tkachenko, I. A1 - Spirin, S. A1 - Smirnov, V. A1 - Tang Lin, T. A1 - Pui Sze, C. A1 - Juan, W. A1 - Lingkai, W. A1 - Ting, L. A1 - Quinde, L. A1 - Yizhao, C. A1 - Lay Peng, S. A1 - Fernandes-Whaley, M. A1 - Prevoo-Franzsen, D. A1 - Quinn, L. A1 - Nhlapo, N. A1 - Mkhize, D. A1 - Marajh, D. A1 - Chamane, S. A1 - Ahn, S. A1 - Choi, K. A1 - Lee, S. A1 - Han, J. A1 - Baek, S. A1 - Kim, B. A1 - Marbumrung, S. A1 - Jongmesuk, P. A1 - Shearman, K. A1 - Boonyakong, C. A1 - Bilsel, M. A1 - Gündüz, S. A1 - Ün, I. A1 - Yilmaz, H. A1 - Bilsel, G. A1 - Gökçen, T. A1 - Clarkson, C. A1 - Warren, J. A1 - Achtar, E. T1 - Mass fraction assignment of Bisphenol-A high purity material JF - Metrologia N2 - The CCQM-K148.a comparison was coordinated by the BIPM on behalf of the CCQM Organic Analysis Working Group for NMIs and DIs which provide measurement services in organic analysis under the CIPM MRA. It was undertaken as a "Track A" comparison within the OAWG strategic plan. CCQM-K148.a demonstrates capabilities for assigning the mass fraction content of a solid organic compound having moderate molecular complexity, where the compound has a molar mass in the range (75 - 500) g/mol and is non-polar (pKow < −2), when present as the primary organic component in a neat organic solid and where the mass fraction content of the primary component in the material is in excess of 950 mg/g. Participants were required to report the mass fraction of Bisphenol A present in one supplied unit of the comparison material. Participants using a mass balance method for the assignment were also required to report their assignments of the impurity components present in the material. Methods used by the seventeen participating NMIs or DIs were predominantly based on either stand-alone mass balance (summation of impurities) or qNMR approaches, or the combination of data obtained using both methods. The results obtained using thermal methods based on freezing-point depression methods were also reported by a limited number of participants. There was excellent agreement between assignments obtained using all three approaches to assign the BPA content. The assignment of the values for the mass fraction content of BPA consistent with the KCRV was achieved by most of the comparison participants with an associated relative standard uncertainty in the assigned value in the range (0.1 - 0.5)%. KW - Bisphenol-A KW - Purity assessment KW - Interlaboratory key comparison KW - Metrology PY - 2021 DO - https://doi.org/10.1088/0026-1394/58/1A/08015 VL - 58 IS - 1A SP - 08015 PB - IOP Publishing AN - OPUS4-54188 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -