HPLC-MS/MS法测定人血浆中马来酸甲麦角新碱浓度的不确定度评价  

Uncertainty evaluation in determination of methylergometrine in human plasma by HPLC- MS /MS

作　　者：齐会红[1,2,3] 李扬[2,3] 史爱欣[2,3] 胡欣[2,3] 毕开顺[1] 王铁杰[1,4] 

机构地区：[1]沈阳药科大学药学院,沈阳110016 [2]卫生部北京医院药学部,北京100730 [3]药物临床风险与个体化应用评价北京市重点实验室,北京100730 [4]深圳市药品检验所,深圳518057

出　　处：《中国新药杂志》2014年第10期1127-1132,共6页Chinese Journal of New Drugs

基　　金：国家"重大新药创制"科技重大专项(2012ZX09303-008-002)

摘　　要：目的:评定HPLC-MS/MS法测定人血浆中马来酸甲麦角新碱浓度的不确定度。方法:对马来酸甲麦角新碱浓度测定过程各影响因素,包括测定精密度、称量、标准溶液的配制、含药血浆的配制、血浆提取、仪器、标准曲线拟合等进行分析评定,计算各变量的不确定度和合成不确定度,最终计算扩展不确定度。结果:人血浆中15.000 ng·mL-1马来酸甲麦角新碱的扩展不确定度为1.127 ng·mL-1(P=95%,k=2)。结论:HPLC-MS/MS法测定人血浆中马来酸甲麦角新碱浓度的不确定度主要由回收率、对照品溶液的配制和仪器引入。Objective： To evaluate the uncertainty of methylergometrine in human plasma determined by HPLC-MS / MS. Methods： The uncertainty caused by various influencing factors in the whole process of determination,including repeatability,balancing,standard solution preparation,drug-spiked plasma,extraction process,the equipment,calibration fitting,and so on. The expanded uncertainty was obtained by calculating each component of uncertainty and the combined uncertainty. Results： The obtained expand uncertainty of 15. 000 ng·mL^-1was 1. 127 ng·mL^-1（P =95%,k =2）. Conclusion： The uncertainty determined by HPLC-MS/MS is mainly caused by extraction recovery,solution preparation and the equipment.

关 键 词：马来酸甲麦角新碱 高效液相色谱-串联质谱法 血浆浓度 不确定度 

分 类 号：R917[医药卫生—药物分析学]