人血浆中依折麦布浓度测定方法的不确定度评定

Evaluation of uncertainty in the determination of ezetimibe in human plasma

目的研究高效液相色谱-串联质谱法(HPLC-MS/MS)法测定人血浆中依折麦布浓度的不确定度评定方法。方法对依折麦布浓度测定全过程进行分析,包括测定精密度、称量、标准溶液的配制、固相萃取过程、标准曲线拟合等进行分析评定,根据各分量计算出合成不确定度,由合成不确定度及其分布求得扩展不确定度。结果人血浆中依折麦布浓度为0.20、2.0、16 ng·m L-1,在置信概率为95%时的扩展不确定度分别为(0.213±0.082)、(2.07±0.15)、(16.1±1.11)ng·m L-1。结论测定中的不确定度主要来自标准曲线的拟合过程,评价方法适用于血浆中依折麦布测定的不确定度评定。

Objective To develop a method to evaluate the uncertainty in the determination of ezetimibe in human plasma by HPLC-MS/MS. Methods The uncertainty sources were obtained from the whole procedure of determina-tion, including precision, weighing, solution preparation, protein precipitation process, the apparatus and calibration fitting. The combined uncertainty and expanded uncertainty were calculated accordingly. Results The expanded uncertainty for 0.20, 2.0 and 16 ng·mL^- 1 level of ezetimibe was（0.213±0.082）,（2.07±0.15） and（16.1±1.11） ng·mL^- 1（P = 95%）. Conclusion The uncertainty is mainly caused by calibration curve. This method is suitable for the uncertainty evaluation in the determination of ezetimibe in human plasma.