Key comparison CCQM-K60: Total selenium and selenomethionine in selenised wheat flour

Abstract

Key comparison CCQM-K60 was performed to assess the analytical capabilities of national metrology institutes (NMIs) to accurately quantitate the mass fraction of selenomethionine (SeMet) and total selenium (at low mg kg−1 levels) in selenised wheat flour. It was organized by the Inorganic Analysis Working Group (IAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) as a follow-up key comparison to the previous pilot study CCQM-P86 on selenised yeast tablets. LGC Limited (Teddington, UK) and the Institute for National Measurement Standards, National Research Council Canada (NRCC, Ottawa, Canada) acted as the coordinating laboratories. CCQM-K60 was organized in parallel with a pilot study (CCQM-P86.1) involving not only NMIs but also expert laboratories worldwide, thus enabling them to assess their capabilities, discover problems and learn how to modify analytical procedures accordingly.Nine results for total Se and four results for SeMet were reported by the participant NMIs. Methods used for sample preparation were microwave assisted acid digestion for total Se and multiple-step enzymatic hydrolysis and hydrolysis with methanesulfonic acid for SeMet. For total Se, detection techniques included inductively coupled plasma mass spectrometry (ICP-MS) with external calibration, standard additions or isotope dilution analysis (IDMS); instrumental neutron activation analysis (INAA); and graphite furnace atomic absorption spectrometry (GFAAS) with external calibration. For determination of SeMet in the wheat flour sample, the four NMIs relied upon measurements using species-specific IDMS (using 76Se-enriched SeMet) with HPLC-ICP-MS.Eight of the nine participating NMIs reported results for total Se within 3.5% deviation from the key comparison reference value (KCRV). For SeMet, the four participating NMIs reported results within 3.2% deviation from the KCRV. This shows that the performance of the majority of the CCQM-K60 participants was very good, illustrating their ability to obtain accurate results for such analytes in a complex food matrix containing approximately 17 mg kg−1 Se.Main text.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 kcdb.bipm.org/.The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (MRA).