【摘要】 目的:建立测定大鼠血浆中银杏内酯B浓度的LC-MS方法。方法:取大鼠血浆50μL,加2.5mol.L-1盐酸10μL酸化后,加入内标格列本脲,以1mL乙醚萃取后取上清液挥干,用50%甲醇1mL溶解,取10μL进行LC-MS测定。色谱条件:色谱柱为HypersilODS2柱(5μm,4.6mm×150mm),流动相:甲醇-0.01%氨水(52:48);流速:1.0mL.min-1;质谱条件:电喷雾离子化(ESI)方式,以选择性负离子方式检测,银杏内酯B和内标格列本脲的选择检测离子质荷比分别为m/z423.1([M-H]-)和m/z492.1([M-H]-)。结果:银杏内酯B的线性范围为0.05～10.0μg.mL-1,最低定量限(LOQ)为0.05μg.mL-1。准确度、精密度以及稳定性均符合有关要求。结论:本方法专属性强,灵敏度高,线性关系良好,操作简便,适用于药代动力学研究。更多还原

【Abstract】 Objective:To develop an LC-MS method for the determination of ginkgolide B in rat plasma.Methods:The internal standard(glibenclamide) 10 μL was added to 50 μL rat plasma,acidified by adding 10 μL 2.5 mol·L-1 hydrochloric acid,then extracted with 1 mL diethyl ether.After transferred and evaporated,the residue was dissolved with 1 mL 50% methanol and determined by injecting 10 μL to LC-MS system.The analytes was separated on a Hypersil ODS 2 analytical column(5 μm,4.6 mm×150 mm) with methanol-0.01% ammonium hydroxide(52:48)as the mobile phase.Analysis was performed at a flow rate of 1.0 mL·min-1.MS determination was in electrospray ionization(ESI)negative mode and in the selected ion monitoring mode(SIM).Ginkgolide B was monitored at m/z 423.1 and internal standard at m/z 492.1.Results:The assay had a calibration range from 0.05 to 10.0 μg·mL-1 and the lowest limit of quantification(LOQ) of 0.05 μg·mL-1 for ginkgolide B.The accuracy,precision(intra-day and inter-day),sensitivity,specificity and stability(in ambient temperature,freeze/thaw,freeze storage) of the method fulfilled the guideline of the analytical validation criteria.Conclusion:This method is proved to be convenient,sensitive and suitable for pharmacokinetic study of ginkgolide B in rats.更多还原