液质联用法测定人血浆中利培酮浓度的不确定度评定___

目的：对人血浆利培酮浓度液质联用法（HPLC/MS/MS）测定的不确定度进行评定。方法：对HPLC/MS/MS法测定血浆中利培酮浓度的全过程进行分析，对于分析过程中称量、溶液配制、液液萃取、仪器以及标准曲线拟和等影响因素引起的不确定度进行了逐层分析，用A类评定程序评价了分析过程中随机效应引起的不确定度，用B类评定程序评价了分析过程的其他因素引起的不确定度，最后根据各分量计算出合成不确定度并进行了扩展。结果：置信概率P为95％时，血浆低（0.65 ng•mL-1）、中（10.86 ng•mL-1）、高（21.72 ng•mL-1）浓度利培酮的扩展不确定度分别为0.24、0.35、0.70 ng•mL-1。结论：该方法适用于HPLC/MS/MS法测定血浆中利培酮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重要参考。

Objective: To evaluate the uncertainty of risperidone in human plasma by HPLC/MS/MS. Method: The uncertainty caused by various factors in the whole process of determination, including balancing, solution preparation, extraction process, calibration fitting and the equipment, was estimated. The uncertainty caused by random effects was evaluated with type A and others were by type B. The combined uncertainty was calculated with all the components. Results: The expanded uncertainty for low, medium and high level of risperidone was 0.24, 0.35 and 0.70 ng•mL-1, respectively (P=95%). Conclusion: This method is applicable for the uncertainty evaluation of risperidone determination in human plasma. It provides an important reference for the uncertainty evaluation for the determination in complex bio-matrix.