LC-MS/MS法测定人血浆中双氯芬酸浓度的不确定度评定

Evaluation of uncertainty for the determination of diclofenac in human plasma by LC- MS / MS

目的研究高效液相色谱—串联质谱法(LC-MS/MS)法测定人血浆中双氯芬酸浓度的不确定度评定方法。方法对双氯芬酸浓度测定全过程进行分析,包括测定精密度、称量、标准溶液的配制、蛋白沉淀过程、标准曲线拟合等进行分析评定,最后根据各分量计算出合成不确定度并进行了扩展。结果置信概率为95%时,人血浆中2.0、50.0、1 600μg·L-1浓度双氯芬酸的扩展不确定度分别为(1.97±1.482)、(46.97±3.72)、(1 494±87.2)μg·L-1。结论该方法不确定度主要来自标准曲线的拟合过程,该法适用于评定LC-MS/MS法测定血浆中双氯芬酸的不确定度研究。

Objective To develop a method to evaluate the uncertainty in the determination of diclofenac in human plasma by LC-MS/MS.Methods The uncertainty sources were obtained from the determination of the whole procedure,including repeatability,weighing, solution preparation,protein precipitation process,the apparatus and calibration fitting.The combined uncertainty and expanded uncer-tainty were calculated accordingly.Results The expanded uncertainty for 2.0,50.0,1 600μg· L^-1 level of diclofenac was （1.97 ± 1.482）、（46.97 ±3.72）,and（1 494 ±87.2）μg· L^-1 respectively （P=95%）.Conclusion The uncertainty is mainly caused by calibration curve.This method is suitable for the uncertainty evaluation in human plasma by LC-MS/MS.