UPLC-MS/MS法测定小鼠血浆尼古丁浓度的不确定度评定

Uncertainty in the determination of nicotine in mouse plasma by UPLC-MS/MS

目的评定液质联用法(UPLC-MS/MS)测定小鼠血浆中尼古丁浓度的不确定度。方法分析UPLC-MS/MS法在测定小鼠血浆中尼古丁浓度时的不确定度来源,根据实验数据计算各不确定度分量并进行合成和扩展。结果小鼠血浆中尼古丁低浓度6 ng·mL-1和高浓度300 ng·mL-1的扩展不确定度分别为0.65 ng·mL-1和20.26 ng·mL-1(P=95%,k=2)。结论UPLC-MS/MS法测定小鼠血浆中尼古丁浓度的不确定度在低浓度时主要由回收率、基质效应、重复性、生物样品配制和标准液配制引入;在高浓度时主要由生物样品配制、标准液配制、回收率和重复性引入。

Objective To evaluate the uncertainty in the determination of nicotine in mouse plasma by UPLCMS/MS.Methods The whole process of nicotine determination was analyzed and uncertainty from various sources was calculated and combined.Results The expanded uncertainty of nicotine at 6 ng·mL-1 and 300 ng·mL-1 was 0.65 ng·mL-1 and 20.26 ng·mL-1,respectively(P=95%,k=2).Conclusion The uncertainty in the determination of nicotine in mouse plasma by UPLC-MS/MS is mainly caused by recovery,matrix effect,repeatability,sample preparation and solution preparation at low concentrations,while at high level the uncertainty is mainly caused by sample preparation,solution preparation,recovery and repeatability.