超高效液相色谱－质谱联用法测定藏药萨热十三味鹏鸟丸中乌头碱类含量

摘要

目的：建立测定萨热十三味鹏鸟丸中乌头碱、次乌头碱及新乌头碱含量的超高效液相色谱－质谱联用法。方法采用显微特征鉴别法鉴别成药中的铁棒锤，色谱柱为AcQuity UPLC BEH C18柱，流动相A为甲醇，流动相B为0.1%甲酸溶液，梯度洗脱，采用电喷雾离子源（ESI）、正离子扫描（ES+）及多反应监测（MRM）测定萨热十三味鹏鸟丸中乌头碱、次乌头碱及新乌头碱的含量。结果萨热十三味鹏鸟丸成药粉末中可见铁棒锤特征性伞状或盔帽状淀粉粒；乌头碱进样量在13.15~2630.00 ng范围内与峰面积线性关系良好（ r=0.9994），平均回收率为97.34%，RSD=1.79%（ n=9）；次乌头碱进样量在32.06~3205.89 ng范围内与峰面积线性关系良好（ r=0.9999），平均回收率为96.09%，RSD=1.94%（ n=9）；新乌头碱进样量在10.23~2046.00 ng范围内与峰面积线性关系良好（ r=0.9993），平均回收率为95.94%，RSD=1.75%（ n=9）。结论该显微鉴别法简单易操作，显微特征明显，结果易辨识；该乌头碱类含量测定方法结果准确，重复性好，可用于同时测定萨热十三味鹏鸟丸中3种乌头碱类物质的含量。%Objective To establish an UPLC-MS method for the content determination of aconitine,hypaoconitine and mesaconitine in SareShisanweiPengniao Pills. Methods The microscopic identification method was used to identifythe aconitum in agents;the chro-matographic column was AcQuity UPLC BEH C18 column,mobile phase A was methanol and mobile phase B was 0. 1% formic acid, gradient elution;the electrospray ionization(ESI),positive ion scan(ES+) and multiple reaction monitoring(MRM) were used todeter-minethe contents of aconitine,hypaoconitine and mesaconitine in SareShisanweiPengniao Pills. Results The linear relationship was good in the range of 13. 15-2 630. 00 ng for aconitine( r=0. 999 4),and the average recovery rate was 97. 34%,RSD=1. 79%( n=9);the linear relationship was good in the range of 32. 06-3 205. 89 ng for hypaoconitine( r=0. 999 9),and the average recovery rate was 96. 09%,RSD=1. 94%( n=9);the linear relationship was good in the range of 10. 23-2 046. 00 ng for mesaconitine( r=0. 999 3), and the average recovery rate was 95. 94%,RSD=1. 75%( n=9). Conclusion This microscopic identification method is simple and sensitive with significantly clear characteristics and easy to identify results;the UPLC-MS method is accurate and reliable with good repeatability,and can be used for the content determination aconitine,hypaoconitine and mesaconitine in SareShisanweiPengniao Pills.