UPLC-MS/MS法测定大鼠血浆中黄芩苷的浓度

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5⁵ 000 ng·mL-1,定量下限为5 ng·mL-1,平均方法回收率在87.4%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。

UPLC-MS/MS determination of baicaline in rat plasma

Objective To develop a liquid chromatography-electrography tandem mass spectrometry method to determine baicaline in rat plasma and perform a preliminary research on pharmacokinetics of baicaline nanocrystals in rats after intravenous administration. Methods Diazepam was used as the internal standard. After liquid-liquid extraction, plasma samples were separated on a Shim-pack C8 column （100 mm× 2.0 mm, 2.2 μm）. The mobile phase consisted of 0.2% acetic acid-methanol with a flow rate of 0.4 mL·min^-1. The electrospray ion tandem mass spectrum in a positive mode and multitude reaction monitor （MRM） were utilized to detect plasma baicaline concentrations. Results The response was linear at 5 - 5 000 ng ·mL^-1 of baicaline. The lower limit of quantification （LLOQ） was 5 ng ·mL^-1. The relative recovery was 87.4% - 100.9%, and it had a good precision with relative standard deviation of less than 15%. Conclusion This method is sensitive, accurate, quick, specific and suitable for the determination of baicaline in the plasma and pharmacokinetics study.