高效液相色谱法测定头痛宁胶囊中天麻素含量的不确定度评定

Evaluation of Uncertainty in Determination of Gastrodin in Toutongning Capsule by HPLC

目的建立高效液相色谱法测定头痛宁胶囊中天麻素含量的不确定度评估方法。方法结合CNAS-GL06-2006《化学分析中不确定度的评估指南》和JJF 1059.1-2012《测量不确定度评定与表示》,通过分析头痛宁胶囊中天麻素的测定过程,对各不确定度分量分析和计算,计算出合成标准不确定度和扩展不确定度。结果天麻素含量为(1.12±0.02)mg/g,k=2。测量不确定度的主要来源为标准品溶液配制、标准曲线拟合和回收率引入的不确定度,其次是稀释定容和样品重复性测定引入的不确定度,样品称量产生的不确定度较小,可忽略不计。结论本文建立的不确定度评估方法可用于头痛宁胶囊中天麻素含量测定的评定,为提高测定结果的准确度提供数据支持。

Objective To establish a method for the evaluation of the uncertainty in the determination of gastrodin in Toutongning capsule by RP-HPLC. Methods Based on the principle and method of JJF 1059.1-2012 Measurement Uncertainty Evaluation and Representation and CNAS-GL06-2006 Uncertainty Evaluation in Chemical Analysis, each components of uncertainty was calculated by analyzing the various variable parameters among the procedures. The combined standard uncertainty and the expanded uncertainty were then finally obtained by synthesizing the uncertainties of viarious component variables. Results The results showed that the content of gastrodin was（1.12±0.02） mg/g, k=2. The main sources of measurement uncertainty and the uncertainty introduced by the configuration of standard curve fitting, the preparation of standard solution and the recovery rate, followed by the repeated measurement and the thinning of standard solution, while the sample weighing of the uncertainty generated is small and negligible.Conclusion The method of the evaluation of uncertainty measurement established in this paper is reasonable and reliable for the evaluation of the uncertainty in the content determination of gastrodin in Toutongning capsule by RP-HPLC.