HPLC-MS/MS法测定人血浆中硫酸双肼屈嗪浓度的不确定度评价  

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

作　　者：安胜男 谢潘潘 齐文渊[2,3] 李博[1,2,3] 严蓓[2,3] 李扬[2,3] 胡欣[2,3] 史爱欣[1,2,3] 

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

出　　处：《中国新药杂志》2015年第19期2191-2196,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法测定人血浆中双肼屈嗪浓度的不确定度。方法:对双肼屈嗪浓度测定过程中各影响因素进行分析,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,以此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:人血浆中硫酸双肼屈嗪(40 ng·m L-1)的扩展不确定度为2.342 18 ng·m L-1(P=95.45%,k=2)。结论:HPLC-MS/MS法测定人血浆中双肼屈嗪浓度的不确定度主要由标准曲线拟合和仪器引起。Objective： To evaluate the uncertainty of determination of dihydralazine in human plasma 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,and calibration fittingand so on were analyzed. The expanded uncertainty was obtained by calculating individual uncertainty of each component and the combined uncertainty. Results： The expanded uncertainty 40ng·m L^- 1was 2. 342 18 ng·m L^- 1（ P = 95. 45%,k = 2）. Conclusion： The uncertainty of determination by HPLCMS/MS is mainly caused by calibration fitting and the equipment.

关 键 词：高效液相色谱-质谱联用法 双肼屈嗪 血浆 不确定度 影响因素 

分 类 号：R969[医药卫生—药理学]