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目的建立三重四级杆串联质谱(LC-MS/MS)分析法同时测定乌头汤中苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、乌头碱、新乌头碱、次乌头碱含量的方法,并测定生川乌单煎液、制川乌单煎液中上述6种乌头碱型生物碱成分的含量。方法采用Hypersil GOLD-C18(100 mm×2.1 mm,1.9μm,Thermo,USA)色谱柱,乙腈-0.01%(体积分数)甲酸水溶液为流动相等度洗脱,样品经电喷雾电离离子源(ESI)正离子化后,通过Thermo TSQ三重四级杆串联质谱仪,采用选择反应监测(SRM)对6种乌头碱型生物碱成分进行含量测定。结果乌头汤中苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、乌头碱、新乌头碱、次乌头碱含量分别为98.86,12.25,155.08,0.15,0.17,0.44μg·g-1。制川乌单煎液及乌头汤中的双酯型乌头碱的含量均明显低于生川乌单煎液,且乌头汤中的单酯型乌头碱的含量低于制川乌。结论该方法快速、准确、灵敏、重复性好,可用于检测乌头汤中6种乌头碱型生物碱含量。
Objective To establish a triple quadrupole tandem mass spectrometry (LC-MS / MS) method for the simultaneous determination of benzoyl aconitine, benzoyl aconitine, benzoyl aconitine, Aconitine, mesaconitine and hypaconitine, and the contents of the above six aconitine alkaloids in Shengchuanwu Decoction and Chuanwu Decoction were determined. Methods The mobile phase consisted of Hypersil GOLD-C18 column (100 mm × 2.1 mm, 1.9 μm, Thermo, USA) and acetonitrile-0.01% (volume fraction) formic acid eluted. The electrospray ionization ionization (ESI) After cationization, the contents of six aconitine alkaloids were determined by Thermo TSQ triple quadrupole mass spectrometer using selective reaction monitoring (SRM). Results The contents of benzoyl aconitine, benzoyl aconitine, benzoyl aconitine, aconitine, mesaconitine and hypaconitine in aconite soup were 98.86,12.25 , 155.08,0.15,0.17,0.44μg · g-1. The contents of DCHF in Wuchuan Decoction and Aconite Decoction were significantly lower than that of ShengchuanWu Decoction and the content of monoester aconitine in Wudu Decoction was lower than that of Szechwan Wu Wu Decoction . Conclusion The method is rapid, accurate, sensitive and reproducible. It can be used to detect the content of six aconitine alkaloids in aconite soup.