HPLC-MS联用同时测定血浆中舒血宁注射液中银杏内酯A、B的含量

Simultaneous Determination of Ginkgolides A,B of Shuxuening Injection in Plasma by HPLC-MS

目的:建立同时测定血浆中银杏内酯A、B含量的方法。方法:采用液-液萃取法预处理血浆样本,高效液相色谱-质谱联用测定。色谱柱为ZORBAXXDB-C18柱,流动相为甲醇-0.1%甲酸水(60:40),流速为0.3mL·min-1,进样量为20μL。质谱采用ESI源,MRM正离子检测模式。结果:建立的检测方法日内及日间变异系数<10.0%,准确率在±6%内。银杏内酯A、B的定量检测限为2μg·L-1,在2～500μg·L-1范围内;银杏内酯A、B的浓度均与峰面积积分值呈良好线性关系,且相关性良好。结论:本方法简单、准确、稳定,可作为测定血浆中银杏内酯A、B的依据。

OBJECTIVE：To establish the method for the simultaneous determination of ginkgolides A,B in plasma.METHODS：Sample pre-treatment consisted of a liquid-liquid extraction and the content of samples was determined by HPLC.The determination was performed on ZORBAX XDB-C18 column with methanol-0.1% formic acid（60：40）as mobile phase at flow rate of 0.3 mL·min-1.The injection volume was 20 μL.A tandem mass spectrometric detection was conducted using multiple reaction monitoring（MRM） under positive ionization mode with a Electrospray ionization（ESI） interface.RESULTS：The intra-day and inter-day variance coefficient of established method were 10.0%.The accuracy was within ±6%.The limit of quantitation of ginkgolide A,B was 2 μg·L-1 The linear range of ginkgolide A,B was 2～500 μg·L-1.CONCLUSION：Established method is simple,accurate and stable,and it can be used as the basis for the content determination of ginkgolides A,B in plasma.