Selenium-enriched yeast possesses the unique ability of transforming chemical selenium, such as sodium selenite, into a biologically active form, which mitigates its toxic effects on the human body. The transformation product of this process, selenomethionine, can be safely and effectively absorbed and utilized by the human body; hence, it has been spiked into a selenium-enriched supplement. This study employs two distinct measurement strategies to determine the selenomethionine content in two candidate reference materials, a selenium-enriched yeast powder and supplement, using both organic and inorganic mass spectrometry. The concentrations of selenomethionine in the selenium-enriched yeast were determined using HPLC-ICP-MS and HPLC- ESI-MS/MS, with mass fractions measured at 718 mg SeMet kg⁻¹ and 715 mg SeMet kg⁻¹, respectively. Notably, both methods yielded consistent results for the selenium supplement, with a selenomethionine mass fraction of 59 mg SeMet kg⁻¹. Ultimately, the certified values of these candidate reference materials were determined as 716 mg kg⁻¹ and 59 mg SeMet kg⁻¹ with expanded uncertainties of 36 mg SeMet kg⁻¹ (k = 2) and 5 mg SeMet kg⁻¹ (k = 2), respectively. The development of these candidate reference materials serves as a valuable reference for diverse methods aiming to determine the value of organic selenium speciation in complex food substrates.

It is well established that arsenic (As) has many toxic compounds, and in particular, inorganic As (iAs) has been classified as a type-1 carcinogen. The measuring of As species in rice flour is of great importance since rice is a staple of the diet in many countries and a major contributor to As intake in the Asian diet. In this study, several solvents and techniques for the extraction of As species from rice flour samples prior to their analysis by HPLC-ICP-MS were investigated. The extraction methods were examined for their efficiency in extracting various arsenicals from a rice flour certified reference material, NMIJ-7532a, produced by the National Metrology Institute of Japan. Results show that ultrasound-assisted extraction at 60 °C for 1 h and then heating at 100 °C for 2.5 h in the oven using a thermostable α-amylase aqueous solution was highly effective in liberating the arsenic species. The recoveries of iAs and dimethylarsinic acid (DMA) in NMIJ-7532a were 99.7% ± 1.6% (n = 3) and 98.1% ± 2.3% (n = 3), respectively, in comparison with the certificated values. Thus, the proposed extraction method is a green procedure that does not use any acidic, basic, or organic solvents. Moreover, this extraction method could effectively maintain the integrity of the native arsenic species of As(III), As(V), monomethylarsonate (MMA), DMA, arsenobetaine (AsB) and arsenocholine (AsC). Under the optimum extraction, chromatography and ICP-MS conditions, the limits of detection (LOD) obtained were 0.47 ng g⁻¹, 1.67 ng g⁻¹ and 0.80 ng g⁻¹ for As(III), As(V) and DMA, respectively, while the limits of quantification (LOQ) achieved were 1.51 ng g⁻¹, 5.34 ng g⁻¹ and 2.57 ng g⁻¹ for As(III), As(V) and DMA, respectively. Subsequently, the proposed method was successfully applied to As speciation analysis for several rice flour samples collected from contaminated areas in China.

The isotopic composition of isotopically enriched materials is essential for isotope dilution mass spectrometry and calibrated mass spectrometry, which are considered to be potential primary methods/authority methods of the highest metrological quality for the analysis of elemental content or isotopic compositions. In this study, a total evaporation (TE) technique was developed for accurate determination of isotopic compositions for seven enriched molybdenum materials with the utilization of negative ion-thermal ionization mass spectrometry (NTIMS). By using La(NO ₃ ) ₃ as an activator, the sample was efficiently ionized into for NTIMS measurement. To achieve highly precise results, the oxygen isotope interference in on Mo isotopic analysis was corrected by using the IUPAC recommended isotopic compositions for atmospheric O ₂ . Various sources of uncertainty to TE-NTIMS, such as measurement repeatability, oxide interference correction, and the ion loss before and after measurement were discussed with respect to the determination of their uncertainty contribution and their influence on the results. As a result, the major isotope abundance for each enriched Mo material were determined as ( k = 2): x ( ⁹² Mo) = 0.974 69 ± 11 for enriched Mo-92, x ( ⁹⁴ Mo) = 0.920 26 ± 11 for enriched Mo-94, x ( ⁹⁵ Mo) = 0.965 50 ± 20 for enriched Mo-95, x ( ⁹⁶ Mo) = 0.967 59 ± 12 for enriched Mo-96, x ( ⁹⁷ Mo) = 0.942 06 ± 13 for enriched Mo-97, x ( ⁹⁸ Mo) = 0.984 56 ± 11 for enriched Mo-98, and x ( ¹⁰⁰ Mo) = 0.993 655 ± 12 for enriched Mo-100, respectively. These measurement results have been compared to those determined by a multi-collector inductively coupled plasma mass spectrometry via the mathematical iteration method in our previous work. Identical major isotope-abundance values were achieved within their combined standard uncertainties, indicating that the TE technique is a powerful and alternative tool for accurate determination of the isotopic composition for isotopically enriched materials. The potential influence owing to the variations of O isotopic compositions during NTIMS measurements were also investigated by applying the ‘In-run O’ isotope-abundance values reported in recent literatures for O isotope interference correction. The corrected Mo isotope abundances of either the major or the minor isotopes were in good agreement with that corrected by using the IUPAC atmospheric O ₂ isotopic compositions.

Creative use of 3D printing to create analytical standards greatly increased the sample homogeneity and the accuracy of the desired concentration.