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高速逆流色谱分离纯化蔓荆子中的活性成分
  • 期刊名称:色谱
  • 时间:0
  • 页码:1043-1047
  • 语言:中文
  • 分类:O658[理学—分析化学;理学—化学]
  • 作者机构:[1]山东中医药大学,山东济南250355, [2]山东省分析测试中心,内东省大型精密分析仪器应用技术重点实验室,山东济南250014, [3]山东省中医药研究院,山东济南250014
  • 相关基金:国家自然科学基金项目(No.20872083); 山东省科技攻关项目(No.2010GSF10287); 济南市高等院所自主创新计划项目(No.201004010)
  • 相关项目:基于可逆络合反应的高速逆流色谱分离体系及分离机理研究
作者: 王晓|
中文摘要:

应用高速逆流色谱法(HSCCC)分离纯化蔓荆子中的活性成分。以石油醚-乙酸乙酯-甲醇-水(体积比为3:6:3.6:3)为两相溶剂体系,在转速为800r/min、流速为1.5mL/min、检测波长为254nm的条件下进行分离,所得馏分经高效液相色谱法(HPLC)检测,并经电喷雾电离(ESI)质谱和核磁共振谱(NMR)鉴定化合物的结构。从250mg蔓荆子粗提物中一次性分离得到4个化合物,分别为23mg对羟基苯甲酸、15mg3,6,7-三甲基槲皮万寿菊素、24mg蔓荆子黄素和5mg蒿黄素,其纯度约为93.1%、97.3%、98.7%和98.5%。该法具有简便、快速、重复性好的优点,为分离蔓荆子中的活性成分提供了新的方法。

英文摘要:

Vitex trifolia L.var.simplicifolia Cham.is widely distributed in Asia,and its fruits are used as a folk medicine for headaches,colds,migraine,eyepain,etc.In order to effectively separate high-purity active components from the seeds of Vitex trifolia L.var.simplicifolia Cham.,a high-speed counter-current chromatography(HSCCC)procedure was performed to separate four components from the crude extract of the fruits.A two-phase solvent system composed of light petroleum-ethyl acetate-methanol-water(3:6:3.6:3,v/v/v/v)was used.Within 230 min,23 mg of 4-hydroxybenzoic acid,15 mg of 3,6,7-trimethylquercetagetin,24 mg of casticin and 5 mg of artemetin were obtained from250 mg of the crude extract of Viticis Fructus in one-step elution under the conditions of a flow rate of 1.5 mL/min,800 r/min and the detection wavelength of 254 nm.The purities of the four fractions were 93.1%,97.3%,98.7%and 98.5%,respectively.The obtained fractions were analyzed by high performance liquid chromatography(HPLC),and identified by electrospray ionization mass spectrometry(ESI-MS),1 H-nuclear magnetic resonance(NMR)and 13C-NMR.The results indicate that HSCCC is a powerful technique for the purification of active components from Viticis Fructus.

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