LC-MS/MS法测定人血浆中氟吡汀及其代谢产物D-13223浓度的不确定度评定  

Uncertainty Evaluation for the Determination of Flupirtine and Its Metabolite D-13223 in Human Plasma by LC-MS/MS

作　　者：刘艳芳[1] 霍花[1] 李大兵 卢新阳 王童超[1] 杨绍青[1] 

机构地区：[1]沈阳军区总医院药研办临床药学技术中心,沈阳110840 [2]沈阳药科大学生命科学与生物制药学院

出　　处：《中国药师》2018年第9期1598-1603,共6页China Pharmacist

摘　　要：目的:评价LC-MS/MS方法测定人血浆中氟吡汀及代谢产物D-13223浓度的不确定度。方法:对氟吡汀及代谢产物D-13223浓度测定过程中影响因素,包括重复性、称量、标准溶液配制、含药血浆配制、萃取过程、线性回归、仪器量化等进行分析评定和计算,根据各分量计算出合成不确定度并进行扩展。结果:置信概率P为95%时,人血浆中氟吡汀低、中、高浓度可表示为:(20.5±1.49),(200±14.4),(1 527±121)ng·ml-1;人血浆中D-13223低、中、高浓度可表示为:(3.93±0.34),(39.6±3.27),(301±24.5)ng·ml^(-1)。结论:本方法适用于LC-MS/MS法测定血浆中氟吡汀及代谢产物D-13223的不确定度评定,为复杂生物基质分析过程的不确定度评定提供了参考。Objective： To evaluate the uncertainty in the determination of flupirtine and its metabolite D-13223 in human plasma by LC-MS/MS. Methods： The influencing factors in the whole process of determination were analyzed and calculated including preci- sion, weighing, standard solution preparation, drug-spiked plasma preparation, extraction process, calibration curve fitting and equip- ment factor. The combined uncertainty was obtained by synthesizing the uncertainties of various component variables and then extend- ed. Results： When the confidence probability was 95% , the low, medium and high concentration of flnpirtine in human plasma could be respectively expressed as （20.5 ± 1.49 ） , （200 ±14.4） and （ 1 527 ±121 ） ng · ml - 1 , the low, medium and high concentration of D-13223 could be respectively expressed as （3.93 ±0.34）, （39.6 ±3.27） and （301 ±24.5）ng · ml -1. Conclusion： The method is suitable for the uncertainty evaluation for flupirtine and its metabolite D-13223 in human plasma by LC-MS/MS, and provides reference for the uncertainty assessment of complex biological matrix analysis.

关 键 词：氟吡汀 D-13223 高效液相色谱-质谱联用法 不确定度 

分 类 号：R917[医药卫生—药物分析学]