目的:评定LC-MS/MS法测定人血浆和尿中匹诺塞林浓度的不确定度,并对二者进行对比分析。方法:分析评定2种生物基质中匹诺塞林浓度测定过程中的影响因素,依次计算各变量的不确定度、合成不确定度和扩展不确定度,对比分析影响2种生物基质中匹诺塞林浓度不确定度差异的影响因素。结果:人血浆中50 ng·mL^-1和人尿中40 ng·mL^-1匹诺塞林的扩展不确定度分别为3.36 ng·mL^-1和3.94 ng·mL^-1(P=95%,k=2)。结论:LC-MS/MS法测定人血浆中匹诺塞林浓度的不确定度主要由标准曲线拟合、标准溶液和血浆提取引入,而人尿中匹诺塞林浓度的不确定度主要由尿样提取、标准曲线拟合和标准溶液的配制引入,不同生物基质中匹诺塞林的测定不确定度及其主要影响因素是不一致的,主要是由样品提取方法不同所引起。
Objective: To evaluate the uncertainty of the pinocembrin concentration in human plasma and urine by LC- MS /MS determination,and make a comparative analysis. Methods: Factors which affected detection process were analyzed,and then component of uncertainty,combined uncertainty and expanded uncertainty were respectively calculated. Comparative analysis was performed to identify the influencing factors which resulted in the difference of the uncertainty for the determination of pinocembrin in two kinds of biological matrix. Results: The expand uncertainty of 50 ng·mL- 1in plasma and 40 ng·mL- 1in urine was 3. 36 ng·mL- 1and 3. 94 ng·mL- 1,respectively( P =95%,k =2). Conclusions: Uncertainty of the pinocembrin determination in human plasma was mainly caused by the standard curve fitting,sample pretreatment and solution preparation,while uncertainty of the pinocembrin determination in human urine was mainly caused by sample pretreatment,the standard curve fitting and solution preparation. Uncertainty of pinocembrin determination in different biological matrix was inconsistent,which was caused by different extraction methods.