液相色谱-电喷雾质谱联用研究吴茱萸化学成分的溶出规律

Extraction method of constituents in Fructus Evodiae by liquid chromatography-electrospray ionization tandem mass spectrometry

目的:应用LC-ESI-MS-MS技术快速分析吴茱萸化学成分,考察其成分溶出规律。方法:用半仿生提取法、水煎煮法、甲醇超声提取法、70%乙醇超声提取法和95%乙醇超声提取法提取吴茱萸的成分,以乙腈-水(含0.5%甲酸及0.2%氨水)为流动相,采用梯度洗脱程序经C18柱分离,通过LC-ESI-MS-MS技术获得化学成分信息。结果:半仿生提取法和水煎煮法主要提取其水溶性成分,而醇类超声提取法有利于其主要活性成分(吴茱萸碱、吴茱萸次碱、去氢吴茱萸碱、羟基吴茱萸碱和吴茱萸内酯)的溶出。结论:LC-ESI-MS-MS技术能快速、灵敏分析吴茱萸化学成分,醇类超声提取法有利于吴茱萸生物碱的提取。

AIM ： To study the extraction of constituents in Fructus Evodiae by a liquid chromatography-electro- spray ionization （ESI） tandem mass spectrometry （LC-ESI-MS） and evaluate advantages and disadvantages of each exaction. METHODS： Fructus Evodiae was extracted by ultrasonic extraction using methanol, 95% ethanol and 70% ethanol or by semi-bionic extraction and water decoction, and then was separated on a C18 column, with ace- tonitrile-water （with 0.5% methyl acid and 0.2% ammonia） as mobile phase. The gradient program was used. Constituents of extractions of Fructus Evodiae were identified by LC-ESI-MS-mass spectrometry. RESULTS ： Water and acid were not appropriate to extraction of evodiamine and rutaecarpine. Alcohol could extract four major alka- loids （ evodiamine, rutaecarpine, dehydroevodiamine and hydroxyevodiamine） and limonin. CONCLUSION ： The method is rapid and sensitive, and it is suitable for the identification of constituents of Fructus Evodiae. Alcohol is prior to extract lipophilic constituents from Evodia rutaecarpa.