UPLC-MS法测定消肿片中3个乌头碱类双酯型生物碱的含量

Quantification of three aconitine-type diester alkaloidsin Xiaozhong tablets by UPLC-MS

目的:建立同时测定消肿片中新乌头碱、乌头碱和次乌头碱3个双酯型生物碱含量的超高效液相色谱-质谱分析方法。方法:采用Agilent ZORBAX SB-C18(100 mm×2.1 mm,1.8μm)色谱柱,以乙腈-0.1%甲酸水溶液(35∶65)为流动相,流速0.3 mL·min-1,柱温35℃;ESI+模式下选择离子监测(SIM)质荷比(m/z)为632,646,616的离子。结果:新乌头碱、乌头碱、次乌头碱浓度分别在0.2250～510.0 ng.mL-1(r=0.9996)、0.2500～500.0 ng.mL-1(r=0.9996)和0.2540～508.0 ng·mL-1(r=0.9996)范围内有良好的线性关系,平均回收率(n=9)分别为95.1%,93.6%,93.0%。结论:该方法简便、快捷、准确,同时检测3个有毒生物碱,可用于消肿片的质量控制。

Objective：To establish an UPLC-MS method for simultaneous quantification of mesaconitine,aconitine and hypaconitine in Xiaozhong tablets.Methods：The separation was performed on an Agilent ZORBAX SB-C18（100 mm×2.1 mm,1.8 μm）column with acetonitrile-0.1% formic acid（35∶65）as the mobile phase.The column temperature was set at 35 ℃ with flow rate of 0.3 mL·min-1.AP-ESI at positive ion mode and the selected ion monitoring were used.Ions at m/z 632,646 and 616 were selected to quantify mesaconitine,aconitine and hypaconitine.Results：The linear ranges were 0.2250-510.0 ng·mL-1（r=0.9996）for mesaconitine,0.2500-500.0 ng·mL-1（r=0.9996）for aconitine and 0.2540-508.0 ng·mL-1（r=0.9996）for hypaconitine.The average recoveries（n=9）were 95.1% for mesaconitine,93.6% for aconitine and 93.0% for hypaconitine.Conclusion：The established method is convenient,rapid and accurate,which can be used to determine three poisonous alkaloids in Xiaozhong tablets.The study may provide a scientific basis for the quality control of this preparation.