超高效液相色谱-质谱联用法测定生物检材中乌头碱
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摘要
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.
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.
引文
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[2]靳昌山,张晓芳,赵奇,等.乌头碱中毒致死2例[J].法医学杂志,2011,27(2):153-154.
[3]刘伟,沈敏,秦志强.乌头急性中毒死亡者乌头生物碱的体内分布[J].法医学杂志,2009,25(3):176-178.
[4]王朝虹,文静,陈义华,等.液相色谱质谱联用测定乌头碱在大鼠体内代谢产物[J].中国法医学杂志,2006,21(2):88-90.
[5]张润生,余琛,刘罡一,等.血液中乌头碱、次乌头碱、新乌头碱的LC/MS/MS分析[J].中国法医学杂志,2004,19(5):265-267.
[6]Ye L,Gao S,Feng Q,et al.Development and validation of a highly sensitive UPLC-MS/MS method for simultaneous determination of aconitine,mesaconitine,hypaconitine,and five of their metabolites in rat blood and its application to a pharmacokinetics study of aconitine,mesaconitine,and hypaconitine[J].Xenobiotica,2012,42(6):518-525.
[7]Zhang P,Kong D,Du Q,et al.A conscious rat model involving bradycardia and hypotension after oral administration:a toxicokinetical study of aconitine[J].Xenobiotica,2017,47(6):515-525.
[8]Ye W,Chen R,Sun W,et al.Determination and pharmacokinetics of engeletin in rat plasma by ultra-high performance liquid chromatography with tandem mass spectrometry[J].J Chromatogr B Analyt Technol Biomed Life Sci,2017,1060:144-149.
[9]Wu J,Xie Y,Xiang Z,et al.Simultaneous determination of multiple components in guanjiekang in rat plasma via the UPLC-MS/MS method and its application in pharmacokinetic study[J].Molecules,2016,21(12):e1732.