UPLC-MS/MS同时测定十一方药酒中的马钱子碱与士的宁的含量

Simultaneows Determination of Strychnine and Brucine in Shiyifang Vinum by LC-MS/MS

目的:建立UPLC-MS/MS法同时测定十一方药酒中马钱子碱与士的宁的含量。方法:色谱柱为Agilent Zorbax SB-C_(18)(2.1 mm×100 mm,3.5μm),流动相为甲醇-10 mmol·L^(-1)甲酸铵溶液(25∶75,用甲酸调节pH至3.0),流速0.2 ml·min^(-1),柱温为30℃,进样量为1μl;采用电喷雾离子源(ESI)进行正离子模式将样品离子化,多反应监测(MRM)模式下对马钱子碱(m/z 395.2→243.8;m/z 395.2→212.8)和士的宁(m/z 335.2→183.9;m/z 335.2→155.9)进行定量分析。结果:马钱子碱浓度在0.242~7.733μg·ml^(-1),士的宁在0.302~9.661μg·ml^(-1)范围内线性关系良好,平均回收率分别为100.1%(RSD=0.8%)、99.4%(RSD=1.4%)(n=6)。结论:本方法准确、可靠,可用于十一方药酒中马钱子碱与士的宁的定量测定。

Objective：To develop a determination method for strychnine and brucine in Shiyifang vinum by LC-MS/MS.Methods：The samples were separated on an Agilent Zorbax SB-C_（18）column（2.1 mm×100 mm,3.5μm）.The mobile phase was methanol-10 mmol·L^（-1）ammonium formate solution（adjusting pH to 3.0 with methane acid）（25∶75）,and the flow rate was 0.2 ml·min^（-1）.The eletrospray ionization（ESI）with positive source of the mass spectrometer and multiple reaction monitor（MRM）mode were used to detect strychnine（m/z 395.2→243.8;m/z 395.2→212.8）and brucine（m/z 335.2→183.9;m/z 335.2→155.9）.Results：The linear range of strychnine was 0.242-7.733μg·ml^（-1）,and that of brucine was 0.302-9.661μg·ml^（-1）.The average recovery was 100.1%（RSD=0.8%,n=6）and 99.4%（RSD=1.4%,n=6）,respectively.Conclusion：The method is simple and accurate,which can be used to determine the contents of strychnine and brucine in Shiyifang vinum.