液质联用法测定人血浆中来曲唑浓度的不确定度评定

Uncertainty Evaluation on the Determination of Letrozole in Human Plasma by HPLC-MS/MS

目的:评价液质联用(HPLC-MS/MS)测定人血浆中来曲唑浓度方法的测量不确定度方法:对HPLC-MS/MS法测定血浆中来曲唑浓度的全过程进行分析分析测量不确定度的来源,用A类评定程序评价分析过程中随机效应引起的不确定度,用B类评定程序评价其他因素引起的不确定度,量化各个不确定度分量,最后根据各分量计算出合成标准测量不确定度,并给出扩展测量不确定度报告结果:置信概率P为95%时,血浆高(79.28 ng·ml^(-1))、中(8.378 ng·ml^(-1))、低(0.099 97 ng·ml^(-1))三个浓度的扩展不确定度分别为3 99,0.417,0.035 32 ng·ml^(-1)。结论:本方法不确定度主要来自标准曲线的拟合过程,其适用于HPLC-MS/MS法测定血浆来曲唑的不确定度评定,为用HPLC-MS/MS法测定血浆浓度的不确定度评定提供了重要参考。

Objective：To evaluate the uncertainty of the letrozole determination in human plasma hy HPLC-MS/MS.Method;The uncertainty sources were obtained from the whole procedure analysis of HPLC-MS/MS method.The uncertainty caused by random effects was evaluated with type A and the others were by type B.Each active components of the uncertainty was calculated,and the extended uncertainty was obtained.Result;The expanded uncertainty for low（0.099 97 ng ？ ml^（-1））,medium（8.378 ng ？ ml^（-1） ） and high（79.28 ng？ml^（-1） ） level of letrozole were 0.035 32,0.417 and 3.99 ng ？ ml^（-1）,respectively（P=95%）.Conclusion：The uncertainty of the method is mainly caused by the calibration curve.The method is applicable in the uncertainty evaluation of the letrozole deteiTnination in human plasma.It provides important reference for the uncertainty evaluation of the drug determination in human plasma by HPLC-MS/MS.