UPLC-MS法测定消肿片中3个乌头碱类双酯型生物碱的含量

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,1.8 μm)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.