液相色谱-质谱法测定云南草乌中双酯型生物碱的含量

Determination of the Content of Diester Type Aconitum Alkaloids in Yunnan Kusnezoff Monkshood by Liquid Chromatography- tandem Mass Spectrometry

目的采用液相色谱-串联质谱法测定云南4种不同产地草乌中双酯型生物碱（乌头碱、次乌头碱、新乌头碱）的含量.方法草乌块根粉碎后经甲醇浸泡,用液相色谱-串联质谱仪检测,分别采用多个特征离子和外标标准曲线法对3种乌头碱进行定性、定量分析.结果乌头碱、次乌头碱、新乌头碱在1-100 ng/m L范围内线性关系良好（r分别为0.999 9,1.000 0和0.999 9）,检出限分别为0.33 ng/m L、0.15 ng/m L和0.03 ng/m L;回收率均高于98%,日内及日间精密度均小于5%.测定结果表明,4种草乌中均含有乌头碱、次乌头碱和新乌头碱,但含量有差异.结论液相色谱-串联质谱法简便快速,可试用于生物样品中乌头碱、次乌头碱和新乌头碱的检验.

Objective To determine the content of four different origin type double ester alkaloids of radix aconiti（ aconitine, hypaconitinen and new aconitine） in Yunnan Kusnezoff Monkshood by LC-MS/MS method.Methods The roots of radix aconiti kusnezoffii were soaked with methanol after crushed,which were analysed by LC-MS/MS, multiple characteristic ion pairs and the external standard method were dopted to aconitine、 hypaconitine and mesaconine for qualitative and quantitative analysis respectively.Results The linear ranges were 1 ~100 ng/m L for three alkaloids（correlation coefficient are 0.9999, 1.000 0, 0.999 9respectively）.The detection limits were 0.33 ng/m L,0.15 ng/m L and 0.03 ng/m L respectively.The recoveries were above 98%,intra- and inter-day precisions were all less than 5%.The determination results showed that there were aconitine, hypaconitine and mesaconine in 4 radix aconiti kusnezoffii, but the contents were different.Conclusion The method is accurate, sensitive,specific and simple,can be used to detect aconitine,hypaconitine and mesaconine in biological samples.