液相色谱-串联质谱法测定氯吡格雷羧酸代谢物SR26334血药浓度的不确定度评价  

Evaluation of measurement uncertainty in determination of clopidogrel carboxylic acid metabolite SR26334 in human plasma by LC-MS/MS

作　　者：杨杰[1] 谭洁[2] 邹建军[2] 

机构地区：[1]南京医科大学附属南京市第一医院神经内科,江苏南京210006 [2]南京医科大学附属南京市第一医院临床药理实验室,江苏南京210006

出　　处：《中国新药与临床杂志》2013年第8期664-668,共5页Chinese Journal of New Drugs and Clinical Remedies

基　　金：国家自然科学基金项目(81100859);博士后基金(2012M511302);南京市医学科技发展项目(QYK10137;QYK10142;QYK11168);2012南京市科委第8批科技发展计划项目(201208008)

摘　　要：目的评价液相色谱-串联质谱法测定氯吡格雷羧酸代谢物SR26334血药浓度的不确定度,以找到影响其不确定度的因素,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》,计算各分量的相对标准不确定度和合成相对不确定度,并给出测定结果的扩展不确定度。结果 20μg·L^(-1)SR26334的标准不确定度为0.816μg·L^(-1),扩展不确定度为1.63μg·L^(-1),浓度测定结果可表示为(18.62±1.63)μg·L^(-1)。结论建立的不确定度评估方法可用于液相色谱-串联质谱法测定血浆中SR26334浓度的不确定度评估。样品前处理和标准曲线拟合是浓度测定结果的主要的不确定度来源。AIM To evaluate the uncertainty in the determination of clopidogrel carboxylic acid metabolite SR26334 in human plasma by LC- MS/MS and find out the influencing factors to provide scientific basis for the test report evaluation. METHODS The uncertainty in the determination of SR26334 in human plasma by LC-MS/MS was analyzed and evaluated according to the ＂Evaluation and Expression of Uncertainty Measurement＂ and the ＂Manual of Uncertainty Evaluation in Chemical Analysis＂ . RESULTS The standard uncertainty of SR26334 in human plasma with the dosage of 20μg·L^-1 was 0.816 μg·L^-1, and the expand uncertainty was 1.63 μg·L^-1. The result of the determination could be expressed as （ 18.62 ± 1.63） μg·L^-1.CONCLUSION The established uncertainty assessment method can be used in the uncertainty evaluation in the determination of SR26334 in human plasma by LC-MS/MS. The uncertainty of this experiment was mainly caused by the sample pretreatment and the calibration curve.

关 键 词：不确定度评价 色谱法 高压液相 串联质谱法 氯吡格雷 血药浓度 

分 类 号：R917[医药卫生—药物分析学]