UPLC-MS/MS法检测黄草乌中毒人体肝脏中的主要生物碱成分

Determination of Mainly Alkaloid Components in Human Liver of Aconitum Vilmorimianum Kom Poisoning by UPLC-MS/MS Method

目的建立人体肝脏中粗茎乌头碱甲、滇乌碱和塔拉萨敏的超高效液相色谱—串联质谱(UPLC-MS/MS)检测方法。方法样品经处理后,采用电喷雾离子源正离子多反应监测模式进行质谱分析,以特征离子对和保留时间对人体肝脏和黄草乌块根中的粗茎乌头碱甲、滇乌碱和塔拉萨敏进行定性分析,外标标准曲线法进行定量分析。结果粗茎乌头碱甲、滇乌碱和塔拉萨敏在1~100 ng·m L-1范围内线性关系良好(r>0.999 0),粗茎乌头碱甲、滇乌碱和塔拉萨敏的检出限均低于0.05 ng·m L-1,定量限均低于0.10 ng·m L-1;方法回收率高于80%,RSD小于5%。结论本文建立的粗茎乌头碱甲、滇乌碱和塔拉萨敏的UPLC-MS/MS检测方法灵敏度高、准确度好,适用于黄草乌中毒案件生物检材中粗茎乌头碱甲、滇乌碱和塔拉萨敏的分析检测。

ObjectiveAn UPLC-MS/MS method was established to detect the crassicauline A,yunaconitine and talatisamine in human liver.MethodsThe samples were extracted and analyzed by UPLC MS/MS.The mass spectrometric acquisition was carried out by electospray ionization in positive mode with multiple reaction monitoring method,multiple characteristic ion pairs and retention time were adopted to crassicauline A,yunaconitine and talatisamine in human liver and aconitum vilmorimianum kom for qualitative analysis,and the external curve standard method was adopted to crassicauline A,yunaconitine and talatisamine for quantitative analysis.ResultsThe linear ranges were1~100ng·mL-1for crassicauline A,yunaconitine and talatisamine,and the linear relationships were well with the correlation coefficient were above0.9990,the qualitative and quantitative restriction were under0.05ng·mL-1and0.10ng·mL-1respectively.The recoveries were above80%,the precisions(RSD)were all less than5%.ConclusionThe UPLC MS/MS method for crassicauline A,yunaconitine and talatisamine is accurate and sensitive,which is used to detect crassicauline A,yunaconitine and talatisamine in biological sample of aconitum vilmorimianum kom poisoning or events.