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.
出处
《中国新药杂志》
CAS
CSCD
北大核心
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)
