大鼠血浆中的银杏内酯B的液相色谱-电喷雾串联质谱法测定

目的 建立快速、灵敏、简单的液相色谱-串联质谱( LC-MS/MS)法测定大鼠血浆中的银杏内酯B.方法 血浆样品经乙酸乙酯液-液萃取后,采用Symmetry C18(3.9 mm×150 mmID,5μm)柱分离,以甲醇-乙酸铵溶液(10 mmol·L-1) (85:15,V/V)为流动相,流速为0.8 ml·min-1.采用电喷雾离子化源(ESI)三重四级杆串联质谱,在负离子多反应监测(MRM)模式下进行检测.结果 血浆中银杏内酯B的线性浓度范围为1.0～200 ng·ml-1,定量下限为1.0ng·m1-1,日内、日间精密度(RSD)均小于4.88％,准确度(RE)在±2.61％范围内.未观察到GB明显的基质效应.结论 该方法操作简便、快速、灵敏度高,分析时间短,适用于银杏内酯B的大鼠药代动力学研究.

LC-MS/MS Method for the Determination of Ginkgolide B in Rat Plasma

Objective To develop a rapid and sensitive liquid chromatography-tandem mass spectrometric(LC-MS/MS) method for the determination of Ginkgolide B in rat plasma.Methods The plasma sample was extracted with ethyl acetate,then separated on a symmetry shield RP18(3.9 mm×150 mm ID,5 μm) column eluted with a mobile phase consisting of methanol-ammonium acetate(10 mM)(85:15,v/v) at a flow rate of 0.8 ml·min-1.The electrospray ionization(ESI) source was performed on a triple quadrupole tandem mass spectrum by multiple reaction monitoring(MRM) mode using the technique in negative ionization mode.Results The linear calibration curves were obtained in the concentration range of 1.0～200 ng·ml-1 with a lower limit of quantification of 1.0 ng·ml-1.Intra-and inter-day precision were both less than 4.88% and the accuracy was within ±2.61%.No significant matrix effect was observed for Ginkgolide B.Conclusion The method is convenient,rapid and sensitive,and suitable to the pharmacokinetic study of Ginkgolide B in rats after intravenous administration.