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Preparation of matrix reference material of aflatoxin M 1 in milk powder
Accreditation and Quality Assurance ( IF 0.8 ) Pub Date : 2021-04-07 , DOI: 10.1007/s00769-021-01460-0
Xuqian Guo , Yinghua Cai , Hongbin Liu , Ying Li , Lei Yu , Xue Han

The preparation and characterization of a matrix reference material for aflatoxin M1 in milk powder is described. Milk powder samples containing aflatoxin M1 were found in the screened natural milk samples. The preparation of matrix milk powder samples was developed through steps by vacuum concentration, spray-drying, cooling, mixing, weighing and packaging, and irradiation. This paper has developed a method for the determination of aflatoxin M1 in milk powder by isotope dilution liquid chromatography–tandem mass spectrometry (ID-LC-MS/MS) with immunoaffinity extraction as the pretreatment method, which was validated and determined the content of aflatoxin M1 in milk powder accurately. The homogeneity was studied by analyzing in triplicate for their aflatoxin M1 contents by ID-LC-MS/MS using random sampling schemes. The short-term stability was evaluated at three different storage temperatures (4, 25 and 50 °C) for 0, 3, 5, 7, 14 days, the long-term stability study comprised of measurement after 0, 1, 3, 6, 9, 12 months after storage at 4 °C, and then, analyses were investigated by ID-LC-MS/MS. After the combination determination of 8 laboratories, the final quantity value and expanded uncertainty of matrix reference material of aflatoxin M1in milk powder were: 0.49 ± 0.11 μg/kg, k = 2, P = 0.95, and the matrix reference material is homogenous and stable at 4 °C for at least 12 months, which can provide quality assurance for the later detection accuracy.



中文翻译:

奶粉中黄曲霉毒素M 1基质参考物质的制备

描述了奶粉中黄曲霉毒素M 1的基质参考物质的制备和表征。在经筛选的天然牛奶样品中发现了含有黄曲霉毒素M 1的奶粉样品。基质奶粉样品的制备通过真空浓缩,喷雾干燥,冷却,混合,称重和包装以及辐照的步骤进行。本文建立了一种以免疫亲和萃取为预处理的同位素稀释液相色谱-串联质谱(ID-LC-MS / MS)测定奶粉中黄曲霉毒素M 1的方法,验证并确定了其中的含量。黄曲霉毒素M 1准确地在奶粉中。通过使用随机采样方案通过ID-LC-MS / MS一式三份分析其黄曲霉毒素M 1含量,研究了均质性。在三种不同的存储温度(4、25和50°C)下分别评估了0、3、5、7、14天的短期稳定性,长期稳定性研究包括在0、1、3、6之后的测量在4°C下储存后的第9、9、12个月,然后通过ID-LC-MS / MS进行分析。联合确定8个实验室后,奶粉中黄曲霉毒素M 1的基质参考物质的最终量值和不确定度扩展为:0.49±0.11μg/ kg,k  = 2,P = 0.95,并且基质参考物质在4°C的温度下均质且稳定至少12个月,这可以为以后的检测准确性提供质量保证。

更新日期:2021-04-08
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