UPLC-MS/MS测定补肾填精口服液中乌头碱类生物碱的含量

Determination of aconitine alkaloids in Bushen Tianjing oral liquid by UPLC-MS/MS

目的采用超高效液相色谱-三重四极杆质谱联用仪测定补肾填精口服液中6种乌头碱类生物碱的含量。方法将样品用甲醇稀释后进行分析:采用Welch UPLC Ultimate LPC_(18)柱(2.1 mm×100 mm,1.8μm),以0.2%甲酸溶液-甲醇为流动相,梯度洗脱,采用电喷雾离子源,在正离子模式下,进行多反应监测模式监测,采用标准曲线法进行含量计算。结果6种生物碱在相应浓度范围内与峰面积呈良好的线性关系,r^(2)为0.9982~0.9996,方法的定量限为0.185~0.690μg·L^(-1),检测限为0.096~0.246μg·L^(-1),平均加样回收率为82.1%~121.2%。结论所采用的方法灵敏度高,专属性强,前处理简单高效,可用于补肾填精口服液中乌头碱类生物碱的含量测定。

Objective To determine 6 aconitine alkaloids in Bushen Tianjing oral liquid by UPLC-MS/MS.Methods The sample was diluted by methanol,and analyzed on a Welch UPLC Ultimate LP-C_(18)column(2.1 mm×100 mm,1.8μm).The mobile phase was 0.2%formic acid solution-methanol by gradient elution,and the target compounds were analyzed in the multiple reaction monitoring mode with positive electrospray ionization.The concentration was calculated by standard curve method.Results The linearity corresponded well to concentration ranges,and the correlation coefficient ranged 0.9982~0.9996.The limit of quantity was 0.185~0.690μg·L^(-1).The limit of detection was 0.096~0.246μg·L^(-1).The average recovery was 82.1%~121.2%.Conclusion The method is sensitive and specific for the simultaneous detection of aconitine alkaloids in Bushen Tianjing oral liquid.