超高效液相色谱-质谱联用法测定生物检材中乌头碱

Determination of aconitine in biological human sample by UPLC-MS/MS

目的建立一种简单、快速测定生物检材(血液、尿液、胃内容物)乌头碱的超高效液相色谱-质谱联用法。方法样品采用乙腈沉淀处理。色谱柱为UPLC C18(2.1mm×50mm,1.7μm),流动相为乙腈-0.1%甲酸,梯度洗脱,流速为0.4m L/min,柱温40℃。采用ESI离子源,MRM模式检测。结果乌头碱在血液0.5~500ng/m L,尿液1~1000ng/m L浓度范围内线性良好(r>0.995)。乌头碱方法回收率在91.3%~110.2%之间;提取回收率在72.8%~83.5%之间;日内、日间RSD均小于14%。结论本方法简单、快速检测生物检材中乌头碱。

Objective To develop a simple and fast UPLC-MS/MS method for determination of aconitine in biological human sample. Methods The biological human sample was treated by acetonitrile precipitation, and then analyzed on a UPLC C18（2.1 mm×50 mm, 1.7μm）column. The mobile phase consisted of acetonitrile-0.1% formic acid with gradient elution, at a flow rate of 0.4 m L/min, at 40℃. UPLC-MS/MS was performed in ESI source with MRM mode for quantification. Results The linear range of the concentration were 0.5~500 ng/m L in blood and 1~1000 ng/m L for aconitine in blood for aconitine（r〉0.995）. The relative recoveries of aconitine were in the range of 91.3%~110.2%, and the extraction recoveries were in the range of 72.8%~83.5%. The RSDs of intra-days and inter-day were both less than 14%. Conclusion The method is a simple, fast and could be used for determination of aconitine in biological human sample.