高效液相色谱法测定硝苯地平中杂质Ⅰ的不确定度评定

Uncertainty Evaluation on Determination of Impurity Ⅰ in Nifedipine by High Performance Liquid Chromatography

目的提高高效液相色谱法测定硝苯地平有关物质杂质Ⅰ的含量检验结果的准确性,确定检验过程中的关键影响因素。方法依据《中国药典》2020年版硝苯地平有关物质项下方法进行测定,列出影响因素,建立量化模型,参照JJF 1059.1-2012《测量不确定度评定与表示》,计算合成不确定度U和扩展不确定度U。结果当取包含因子k=2,置信概率为95%时,高效液相色谱法测定硝苯地平有关物质杂质Ⅰ的扩展不确定度为0.002%,测量结果表示为(0.04±0.002)%。结论杂质Ⅰ含量较低,高效液相色谱法测定硝苯地平杂质Ⅰ的不确定度主要来源于随机因素样品的重复性。

Objective To improve the accuracy of high performance liquid chromatography(HPLC)results for the determination of related substances impurity Ⅰ in nifedipine,and to identify the key influencing factors in the test process.Methods According to the method of Chinese pharmacopoeia(2020 edition)nifedipine related substances determination results,the influencing factors were listed and the quantitative model was established,according to JJF 1059.1-2012"Evaluation and Expression of Measurement Uncertainty",the combined uncertainty U and expanded uncertainty U were calculated.Results When the inclusion factor k=2 and the confidence probability was 95%,the expanded uncertainty of high-performance liquid chromatography determination of nifedipine-related substance impurity Ⅰ was 0.002%,and the measurement result was expressed as(0.04±0.002)%.Conclusion Due to the low content of impurity Ⅰ,the uncertainty of HPLC determination of nifedipine impurity Ⅰ mainly comes from the repeatability of random factor samples.