液相色谱-串联质谱测定米格列奈血药浓度的不确定度评价

目的:对采用液相色谱-串联质谱联用法测定米格列奈的血药浓度进行不确定度评价,以找到影响不确定度的因素,为评价检测报告提供科学依据。方法:根据《测量不确定度评定与表示》,并参考《化学分析中不确定度的评估指南》,对血浆中米格列奈浓度测定进行测量不确定度的分析与评定。结果:10 ng.ml-1米格列奈的标准不确定度为0.289 ng.ml-1,扩展不确定度为0.579 ng.ml-1,浓度测定结果可表示为(9.275±0.579)ng.ml-1。结论:建立的不确定评估方法可用于液相色谱-串联质谱联用法测定血浆中米格列奈浓度的不确定度评估。标准曲线拟合和样品前处理是主要的不确定度来源。测量不确定度的评定方法的确立对于血浆中米格列奈浓度测定方法标准的研究具有重要意义。

Uncertainty Evaluation in Determination of Mitiglinide in Human Plasma by LC-MS/MS

Objective： To evaluate the uncertainty in the determination of mitiglinide in human plasma by LC-MS/MS and find out the influencing factors to provide scientific basis for the test report evaluation. Method： The uncertainty in the determination of mitiglin- ide in human plasma was analyzed and evaluated according to the ＂Evaluation and Expression of Uncertainty Measurement＂ and the ＂Manwal of Uncertainty Evaluation in Chemical Analysis＂. Result： The standard uncertainty of mitiglinide in human plasma with the dosage of 10 ng ml-1 was 0.289 ng ml-1, and the expand Uncertainty was 0. 579 ng ml-1. The result of the determination could be expressed as （9.275 ±0.579） ng ml-1 Conclusion： The uncertainty of the experiment is mainly caused by the calibration curve and the sample pretreatment. The established uncertainty assessment method can be used in the uncertainty evaluation in the determination of mitiglinide in human plasma by LC-MS/MS and is valuable in the determination standard study of mitiglinide in plasma.