LC-MS/MS法测定人血浆中利血平浓度的不确定度评定

Uncertainty evaluation for the determination of reserpine concentration in human plasma by LC-MS / MS

目的:评定LC-MS/MS法测定人血浆中利血平浓度的不确定度。方法:对血浆中利血平浓度测定过程中各影响因素,包括测定精密度、称量、标准溶液的配制、含药血浆的配制、血浆样品提取、仪器、标准曲线拟合等进行分析,计算各变量的不确定度和合成不确定度,最终计算扩展不确定度。结果:置信概率P为95%时,血浆低、中、高(20,10,300 pg·m L^(-1))质量浓度利血平的扩展不确定度分别为21.64,19.71和30.11 pg·m L^(-1)。结论:本方法适用于LC-MS/MS法测定血浆中利血平浓度的不确定度评定,为复杂生物基质分析过程的不确定度评定提供了参考。

Objective： To evaluate the uncertainty of the determination of reserpine concentration in human plasma by LC-MS / MS. Methods： Various factors influencing the uncertainty in the whole process of determination were analyzed and estimated,including precision,weighing,solution preparation,drug containing plasma preparation,plasma extraction,the apparatus,and calibration curves fitting. The uncertainty and synthetic uncertainty of each variable were calculated. The expanded uncertainty of all the components was analyzed. Results： When the confidence probability was P = 95%,the expanded uncertainty for low,medium and high（ 20,100 and 300pg·m L^-1） concentrations of reserpine was 21. 64,19. 97,and 30. 11 pg·m L^-1,respectively. Conclusion： This method is suitable for the uncertainty evaluation for the determination of reserpine concentration in human plasma by LC-MS / MS,and provides a reference for uncertainty evaluation of complex biological matrix analysis.