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目的:评定在线固相萃取LC-MS/MS法测定人全血中依维莫司浓度的不确定度。方法:对全血依维莫司浓度测定过程中各影响因素,包括测定精密度、称量、对照品溶液的配制、标准含药全血样品的配制、在线固相萃取、仪器、标准曲线拟合等进行分析评定,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:人全血中低(0.520 ng·m L~(-1)),中(4.99 ng·m L~(-1)),高(84.99 ng·m L~(-1))质量浓度依维莫司的扩展不确定度分别为0.056、0.40、7.16 ng·m L~(-1)(P=95%,k=2)。结论:在线固相萃取LC-MS/MS法测定人全血中依维莫司浓度的不确定度主要由提取回收率(尤其是低浓度)、对照品溶液配制、仪器允差及测定精密度引入。
OBJECTIVE: To evaluate the uncertainty of determination of everolimus concentration in human whole blood using on-line solid phase extraction (LC-MS / MS). Methods: The determination of the concentration of everolimus whole blood in the process of influencing factors, including the determination of precision, weighing, the preparation of reference substance solution, preparation of standard drug-containing whole blood samples, on-line solid phase extraction, equipment, standard curve And so on. The type A evaluation procedure is used to evaluate the uncertainty caused by random effects in the analysis process. The type B evaluation procedure is used to evaluate the uncertainty caused by other factors in the analysis process. Finally, The degree of uncertainty is determined and expanded to calculate the uncertainty of each variable and the resultant uncertainty, and finally the expanded uncertainty is calculated. Results: The average concentration of human whole blood in low (0.520 ng · m L -1), medium (4.99 ng · m L -1) and high (84.99 ng · m L -1) The expanded uncertainty of the Wimmuls are 0.056,0.40,7.16 ng · m L -1 (P = 95%, k = 2). Conclusion: The uncertainty of determination of everolimus concentration in human whole blood by on-line LC-MS / MS is mainly determined by extraction recovery (especially low concentration), preparation of reference solution, instrument tolerance and determination of precision Introduced.