HPLC-MS/MS法测定血浆中百草枯浓度的不确定度评定  

Uncertainty evaluation on the determination of paraquat concentration in plasma by HPLC-MS/MS

作　　者：李鹏飞[1] 范家明 张茜[1] 杜萍[1] 刘河[1] 刘洪川[1] 刘丽宏[1] LI Peng-fei;FAN Jia-ming;ZHANG Xi;DU Ping;LIU He;LIU Hong-chuan;LIU Li-hong(Department of Pharmacy,Beijing Chaoyang Hospital,Capital Medical University,Beijing 100020,China;Department of Human Resource,Peking University First Hospital,Beijing 100034,China)

机构地区：[1]首都医科大学附属北京朝阳医院药事部,北京100020 [2]北京大学第一医院人力资源处,北京100034

出　　处：《中国临床药理学杂志》2020年第23期3938-3942,共5页The Chinese Journal of Clinical Pharmacology

基　　金：科技部重大新药创制课题资助项目(2017ZX09101001);国家自然科学基金资助项目(81501655)。

摘　　要：目的评定HPLC-MS/MS测定血浆中百草枯质量浓度的不确定度。方法本研究对百草枯质量浓度测定过程中各影响因素,包括测定精密度、称量、标准溶液和生物样品的配制、生物样品前处理和提取过程、仪器、标准曲线拟合等进行分析评定,用A类评定程序评价了分析过程中随机效应引起的不确定度,用B类评定程序评价了分析过程的其他因素引起的不确定度,根据各分量计算得到扩展不确定度和合成不确定度。结果用HPLC-MS/MS测定血浆中百草枯时,低、中和高浓度质控样品均值及扩展不确度分别表示为(3.17±1.54),(15.31±1.77)和(80.93±5.60)ng·mL^-1,(扩展因子k=2,置信概率P=95%)。结论 HPLC-MS/MS测定血浆中百草枯质量浓度的不确定度主要由标准曲线拟合和回收率引入。Objective To evaluate the uncertainty of paraquat concentration in plasma by HPLC-MS/MS method. Methods The uncertainties caused by various factors in the whole process of determination, such as precision, weighing, preparation of standard solution and biological sample, biological sample pretreatment and extraction process, the apparatus and calibration curve fitting, were comprehensively estimated. The uncertainty caused by random effects and others was elucidated in terms of type A and type B, respectively. The expanded uncertainties and combined uncertainties were analyzed with all the components. Results When paraquat was determind in plasma by using HPLC-MS/MS method, the mean value and expanded uncertainties of quality control samples with low, medium and high concentrations were(3.17±1.54),(15.31±1.77) and(80.93±5.60) ng·mL^-1, respectively(k=2, P=95%). Conclusion The uncertainty of the HPLC-MS/MS method was mainly caused by calibration curve fitting and recovery.

关 键 词：百草枯 不确定度 HPLC-MS/MS 

分 类 号：R97[医药卫生—药品]