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目的建立UPLC-MS/MS法测定大鼠血浆中黄芩苷的浓度,并初步研究大鼠尾静脉注射黄芩苷纳米结晶后药动学特征。方法采用液液萃取法提取药物,以地西泮为内标,色谱柱为C8柱(100 mm×2.0mm,2.2μm),0.2%甲酸水溶液-甲醇为流动相,流速为0.4 mL·min-1。样品在三级四极杆串联质谱中经ESI源离子化后以多反应离子监测方式测定。结果黄芩苷的线性范围为5~5 000 ng·mL-1,定量下限为5 ng·mL-1,平均方法回收率在87.4%~100.9%,日内、日间变异系数均<15%。结论方法灵敏、准确、快速、专属性强,适用于黄芩苷的血药浓度测定和药物代谢动力学研究。
OBJECTIVE To establish a method for the determination of baicalin in rat plasma by UPLC-MS / MS and to study the pharmacokinetics of baicalin nano-crystals after tail vein injection in rats. Methods The drug was extracted by liquid-liquid extraction, and the internal standard was diazepam. The column was C8 column (100 mm × 2.0 mm, 2.2 μm) with 0.2% formic acid in methanol as mobile phase and the flow rate was 0.4 mL · min- 1. The samples were ionized by ESI source in triple quadrupole tandem mass spectrometry and detected by multiple reaction ion monitoring. Results The linear range of baicalin was 5 ~ 5 000 ng · mL-1 and the lower limit of quantification was 5 ng · mL-1. The average recovery was between 87.4% and 100.9%. The intra-day and inter-day coefficients of variation were all <15%. Conclusion The method is sensitive, accurate, rapid and specific. It is suitable for the determination of baicalin and its pharmacokinetic study.