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(2.1mm×50mm, 1.7μm)column. The mobile phase consisted of acetonitrile-0.1% formic acid with gradient elution, at a flow rate of 0.4 mL/min, at 40℃. UPLC-MS/MS was performed in ESI source with MRM mode for quantification. Results The linear range of the concentration were 0.5~500ng/mL in blood and 1~1000ng/mL 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.%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0.4mL/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/mL,尿液1~1000ng/mL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.
展开▼