高效液相色谱法测定保健品水飞蓟片中水飞蓟宾的不确定度评定

目的 按照《中国华人民共共和国药典》一部2015版规定的高效液相色谱法对保健品水飞蓟片中水飞蓟宾含量进行测定,根据CNAS-GL006：2019要求以及JJF1059.1-2012对测定过程中影响检验结果的各个分量进行评估。方法 通过对测量重复性、标准品溶液配制、样品溶液的配制、高效液相色谱仪以及标准曲线拟合测量偏差这5个方面引入的不确定度进行分析,并确定各个不确定度分量,得到扩展不确定度。结果 经测定,保健品水飞蓟片中水飞蓟宾含量为(2.44±0.118)g/100g,P=95%,(k=2)结论 样品溶液配制和标准曲线拟合因素对测量不确定度影响显著,由检验方法重复测量和标准品溶液配制以及高效液相色谱仪体现。

Uncertainty evaluation for the determination of silybin in silybin tablets of health food by high performance liquid chromatography

Objective To evaluate the uncertainty of the determination of silybin content in silybin tablets of health food by high performance liquid chromatography (HPLC). Methods According to the Pharmacopoeia of the people''s Republic of China Part 1 2015 Edition and JJF 1059.1-2012 Measurement uncertainty and results indication, each component affecting the test result in the determination process was assessed. Through analyzing the uncertainty introduced from 5 aspects, including the repeatability of determination, the preparation of standard solution, the preparation of sample solution, high performance liquid chromatograph and the measurement deviation of standard curve fitting, each uncertainty component was determined and the expanded uncertainty was calculated. Results The content of silyin in silybin tablets was (2.440±0.093) g/100 g, P=95%(k=2). Conclusion The preparation of standard solution and method repeatability have the most significant influence on the uncertainty of measurement, which need attention in the experiment.