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<p>Accurate determination of selenium species and elements in selenium-enriched cereals is essential for food safety assessment, nutritional evaluation, and analytical quality assurance; however, the availability of matrix-matched certified reference materials (CRMs) remains limited. In this study, two novel matrix CRMs were developed for the determination of selenium species (selenomethionine, SeMet) and elements (Cd, Cu, K, Mg, and Se) in selenium-enriched rice and wheat. Rice and wheat samples were collected from Enshi (Hubei Province) and Anyang (Henan Province), China, respectively, and were ground to &lt; 75&#xa0;μm (200 mesh) and homogenized to ensure uniformity. Homogeneity was evaluated using one-way ANOVA on 15 randomly selected units, showing satisfactory uniformity for all analytes. Short-term stability was examined at − 22 ℃ and 60 ℃, and long-term stability was assessed at seven predefined time points (0, 1, 3, 6, 10, 15, and 39 months) over the study period, both confirming good stability within the four-year validity period. Value assignment for elemental contents and Se species was performed collaboratively by nine accredited laboratories using multiple independent analytical techniques, following the metrological specification JJF 1343–2022. Combined uncertainties were estimated from homogeneity, stability, and characterization components. The developed selenium-enriched rice and wheat CRMs exhibited excellent homogeneity, long-term stability, and metrological traceability. The certified values and expanded uncertainties (95% confidence level, <i>k</i> = 2) for Cd, Cu, K, Mg, Se, and SeMet in the selenium-rich rice flour CRM were 0.045 ± 0.010&#xa0;µg/g, 2.20 ± 0.40&#xa0;µg/g, 0.080 ± 0.004%, 0.013 ± 0.003%, 0.48 ± 0.09&#xa0;µg/g, and 0.84 ± 0.07&#xa0;µg/g, respectively. Correspondingly, the certified values for the selenium-rich wheat flour CRM were (0.011) µg/g, 2.46 ± 0.40&#xa0;µg/g, 0.20 ± 0.03%, 0.072 ± 0.013%, 0.59 ± 0.12&#xa0;µg/g, and 0.83 ± 0.07&#xa0;µg/g, respectively. These CRMs provide reliable benchmarks for selenium speciation and elemental analysis, supporting method validation, quality control, and the standardization of selenium-enriched agricultural and functional food products.</p>

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Preparation and preliminary characterization of two novel certified matrix reference materials for accurate determination of selenomethionine and elements in selenium-enriched rice and wheat flour

  • 期刊论文

  • 发表日期：

    2026年2月25日

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  • Lingyang Yao,
  • Zhengyu Bao,
  • Bolun Fan,
  • Molan Tang,
  • Zhenzhen Ma,
  • Huan Tian,
  • Ziyi An

摘要

Accurate determination of selenium species and elements in selenium-enriched cereals is essential for food safety assessment, nutritional evaluation, and analytical quality assurance; however, the availability of matrix-matched certified reference materials (CRMs) remains limited. In this study, two novel matrix CRMs were developed for the determination of selenium species (selenomethionine, SeMet) and elements (Cd, Cu, K, Mg, and Se) in selenium-enriched rice and wheat. Rice and wheat samples were collected from Enshi (Hubei Province) and Anyang (Henan Province), China, respectively, and were ground to < 75 μm (200 mesh) and homogenized to ensure uniformity. Homogeneity was evaluated using one-way ANOVA on 15 randomly selected units, showing satisfactory uniformity for all analytes. Short-term stability was examined at − 22 ℃ and 60 ℃, and long-term stability was assessed at seven predefined time points (0, 1, 3, 6, 10, 15, and 39 months) over the study period, both confirming good stability within the four-year validity period. Value assignment for elemental contents and Se species was performed collaboratively by nine accredited laboratories using multiple independent analytical techniques, following the metrological specification JJF 1343–2022. Combined uncertainties were estimated from homogeneity, stability, and characterization components. The developed selenium-enriched rice and wheat CRMs exhibited excellent homogeneity, long-term stability, and metrological traceability. The certified values and expanded uncertainties (95% confidence level, k = 2) for Cd, Cu, K, Mg, Se, and SeMet in the selenium-rich rice flour CRM were 0.045 ± 0.010 µg/g, 2.20 ± 0.40 µg/g, 0.080 ± 0.004%, 0.013 ± 0.003%, 0.48 ± 0.09 µg/g, and 0.84 ± 0.07 µg/g, respectively. Correspondingly, the certified values for the selenium-rich wheat flour CRM were (0.011) µg/g, 2.46 ± 0.40 µg/g, 0.20 ± 0.03%, 0.072 ± 0.013%, 0.59 ± 0.12 µg/g, and 0.83 ± 0.07 µg/g, respectively. These CRMs provide reliable benchmarks for selenium speciation and elemental analysis, supporting method validation, quality control, and the standardization of selenium-enriched agricultural and functional food products.