摘要
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 method of liquid chromatography-tandem mass spectrometry（LC-MS/MS） for the simultaneous determination of benzoylmesaconine, benzoylaconine, benzoylhypaconine, aconitine, mesaconitine and hypaconitine in Radix Aconiti Decoction formula, and to detect the contents of the 6 kinds of aconitine alkaloids in thedecoction of raw and prepared Radix Aconiti. Methods The content determination was performed on a Hypersil GOLD-C18（ 100 mm × 2.1 mm, 1.9 μm, Thermo, USA） chromatographic column, and the mobile phase consisted of acetonitrile-0.01% （volume fraction） formic acid solution. Thermo TQ Triple-stage Quadrupole mass spectrometry system equipped with an electrospray ionization source was used as the detector and operated in the positive ion mode. Selected reactions monitoring （SRM） was performed to detect the six compounds. Results The contents of benzoylmesaconine, benzoylaconine, benzoylhypaconine, aconitine, mesaconitine and hypaconitine in Radix Aconiti Decoction formula were 98.86, 12.25, 155.08, 0.15, 0.17, 0.44 μg.g-1, respectively. Diester aconitine content was lower in the decoction of prepared Radix Aconiti and Radix Aconiti Decoction formula than that in the decoction of raw Radix Aconiti, and the content of monoester aconitine in the Radix Aconiti Decoction formula was lower than that in the prepared Radix Aconiti. Conclusion An accurate, sensitive and replicable LC-MS/MS method has developed for studying the content of the six aconitine alkaloids in Radix Aconiti Decoction.
出处
《中药新药与临床药理》
CAS
CSCD
北大核心
2015年第6期833-837,共5页
Traditional Chinese Drug Research and Clinical Pharmacology
基金
广东省科技计划项目(2011B050500008)
