Sciensano, Chemical and Physical Health Risks, Organic Contaminants and Additives, Leuvensesteenweg 17, 3080 Tervuren, Belgium.
Earth and Life Institute-Applied Microbiology (ELIM), Université catholique de Louvain (UCL), Croix du Sud 2 bte L7.05.06, 1348 Louvain-la-Neuve, Belgium.
Toxins (Basel). 2021 Mar 30;13(4):245. doi: 10.3390/toxins13040245.
The development of incurred reference materials containing citrinin (CIT) and their successful application in a method validation study (MVS) in order to harmonize CIT determination in food and food supplements are demonstrated. CIT-contaminated materials made of red yeast rice (RYR), wheat flour, and leaves (GBL), as well as food supplements made of red yeast rice (FS-RYR) and leaves (FS-GBL), were manufactured in-house via fungal cultivation on collected raw materials. The homogeneity and stability from randomly selected containers were verified according to the ISO 13528. CIT was found to be homogenously distributed and stable in all contaminated materials, with no significant degradation during the timescale of the MVS when storage was performed up to +4 °C. Next, an MVS was organized with eighteen international laboratories using the provided standard operating procedure and 12 test materials, including three RYRs (blank, <50 µg/kg, <2000 µg/kg), two wheat flours (blank, <50 µg/kg), two GBL powders (blank, <50 µg/kg), three FS-RYRs (blank, <50 µg/kg, <2000 µg/kg), and two FS-GBLs (blank, <50 µg/kg). The results of seven CIT-incurred materials showed acceptable within-laboratory precision (RSDr) varying from 6.4% to 14.6% and between-laboratory precision (RSDR) varying from 10.2% to 37.3%. Evidenced by HorRat values < 2.0, the results of the collaborative trial demonstrated that the applied analytical method could be standardized. Furthermore, the appropriateness of producing CIT reference materials is an important step towards food and feed quality control systems and the organization of proficiency tests.
本文展示了如何开发含有桔青霉素（CIT）的人工污染参考物质，并成功将其应用于方法验证研究（MVS）中，以协调食品和食品补充剂中 CIT 的测定。通过在收集的原材料上进行真菌培养，在内部制造了受桔青霉素污染的红米（RYR）、小麦粉和 叶（GBL）材料，以及由红米（FS-RYR）和 叶（FS-GBL）制成的食品补充剂。根据 ISO 13528，对随机选择的容器进行了均匀性和稳定性验证。研究发现，在所有污染材料中，CIT 分布均匀且稳定，在 MVS 的时间范围内，当储存温度高达+4°C 时，没有明显降解。接下来，根据提供的标准操作程序和 12 种测试材料，组织了 18 个国际实验室的 MVS，其中包括 3 个 RYR（空白、<50 µg/kg、<2000 µg/kg）、2 个小麦粉（空白、<50 µg/kg）、2 个 GBL 粉末（空白、<50 µg/kg）、3 个 FS-RYR（空白、<50 µg/kg、<2000 µg/kg）和 2 个 FS-GBL（空白、<50 µg/kg）。结果表明，七种 CIT 人工污染材料的结果具有可接受的实验室内精密度（RSDr），范围为 6.4%至 14.6%，以及实验室间精密度（RSDR），范围为 10.2%至 37.3%。根据 HorRat 值<2.0，协作试验的结果表明，所应用的分析方法可以标准化。此外，生产 CIT 参考物质是食品和饲料质量控制系统以及能力验证组织的重要步骤。
