黄豆黄素纯度标准物质研制

Development of glycitein purity reference material

建立黄豆黄素纯度标准物质的研制方法。选择纯度大于98%(质量分数)的黄豆黄素标准品作为标准物质候选物,通过加热和冷冻干燥去除多余的水分。通过红外、质谱、核磁氢谱进行结构确证和表征后分装,采用质量平衡法进行均匀性和稳定性检验。结果显示,标准物质均匀性良好,在常温条件下保存12个月稳定;采用质量平衡法和定量核磁法进行纯度定值,质量平衡法的定值结果为99.09%,定量核磁法的定值结果为99.13%,取平均值99.1%作为最终定值结果;对定值、均匀性和稳定性引入的不确定度进行了系统评定,扩展不确定度为0.3%(k=2)。研制的黄豆黄素纯度标准物质已申报国家一级标准物质,编号为GBW10171。该标准物质可用于食品、保健品、饲料中黄豆黄素含量检测。

A method for preparation of the certified reference materials(CRM)of glycitein was established.The glycitein standard with purity greater than 98%(mass fraction)was selected as the standard material candidate,and the excess water was removed by heating and freeze-drying.After structural confirmation and characterization by infrared spectroscopy,mass spectrometry,and H NMR spectroscopy,the partitioning was performed,and the homogeneity and stability of the CRM were carried out by mass balance method(MB).The results showed that the CRM had good homogeneity and was stable for 12 months at room temperature.The purity was characterized by MB method and quantitative NMR method(qNMR).The result of MB method was 99.09%,and that of qNMR method was 99.13%.The average value of 99.1%was taken as the final determination result.The uncertainties of characterization,homogeneity and stability were systematically evaluated,and the extended uncertainty was 0.3%(k=2).The developed CRM for the purity of glycitein has been declared as national CRM with the number GBW 10171.The CRM can be used for the detection of glycitein content in food,health products and feed.