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目的:建立高效液相色谱-质谱/质谱联用法(HPLC-MS/MS)测定血浆中牡荆素的方法,并用于大鼠药动学研究。方法:采用Capcell Pak C18柱(50 mm×2.0 mm,I.D.,5μm),柱温25℃,流动相为甲醇∶水(95∶5,0.1%甲酸),流速为0.2 mL/min。用负离子电喷雾电离源,多反应方式检测,选择监测的离子反应为m/z 431～311(牡荆素)和m/z 269～225(大黄素,内标)。结果:牡荆素在0.5～2 000 ng/mL线性关系良好,相关系数为0.9960,最低定量限为0.5 ng/mL。加样回收率76.1%～89.0%,日内日间精密度RSD均小于11%。结论:该方法分析速度快、操作简单、灵敏度高,可用于大鼠血浆中牡荆素的浓度测定及药动学研究。
OBJECTIVE: To establish a method for the determination of vitexin in plasma by HPLC-MS / MS and to study the pharmacokinetics in rats. Methods: Capcell Pak C18 column (50 mm × 2.0 mm, I.D., 5 μm) was used. The column temperature was 25 ℃. The mobile phase was methanol: water (95: 5, 0.1% formic acid) and the flow rate was 0.2 mL / min. The negative ions electrospray ionization source, multi-reaction mode detection, the choice of monitoring ion reaction m / z 431 ~ 311 (vitexin) and m / z 269 ~ 225 (emodin, internal standard). Results: Vitexin had a good linearity of 0.5-2000 ng / mL with a correlation coefficient of 0.9960 and a minimum limit of quantification of 0.5 ng / mL. The recoveries of samples ranged from 76.1% to 89.0%. The intra-day and intra-day RSDs were less than 11%. Conclusion: The method is rapid, simple and sensitive, and can be used for the determination of vitexin in rat plasma and pharmacokinetic study.