色谱

色谱 ›› 2010, Vol. 28 ›› Issue (11): 1043-1047.

• 研究论文 • 上一篇    下一篇

高速逆流色谱分离纯化蔓荆子中的活性成分

管仁军1,2, 王岱杰2, 于宗渊3, 王晓2*, 蓝天凤1   

  1. 1. 山东中医药大学, 山东 济南 250355; 2. 山东省分析测试中心, 山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
  • 收稿日期:2010-07-12 修回日期:2010-08-18 出版日期:2010-11-28 发布日期:2010-11-28
  • 通讯作者: 王晓,博士,研究员.
  • 基金资助:

    国家自然科学基金项目(No. 20872083)、山东省科技攻关项目(No. 2010GSF10287)和济南市高等院所自主创新计划项目(No. 201004010).

Preparative isolation and purification of the active components from Viticis Fructus by high-speed counter-current chromatography

GUAN Renjun1,2, WANG Daijie2, YU Zongyuan3, WANG Xiao2*, LAN Tianfeng1   

  1. 1. Shandong University of Traditional Chinese Medicine, Jinan 250355, China; 2. Shandong Analysis and Test Center, Key Laboratory for Applied Technology of Sophisticated Analytical Instrument of Shandong Province, Jinan 250014, China; 3. Shandong Academy of Chinese Medicine, Jinan 250014, China
  • Received:2010-07-12 Revised:2010-08-18 Online:2010-11-28 Published:2010-11-28

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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800 r/min、流速为1.5 mL/min、检测波长为254 nm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250 mg蔓荆子粗提物中一次性分离得到4个化合物,分别为23 mg对羟基苯甲酸、15 mg 3,6,7-三甲基槲皮万寿菊素、24 mg蔓荆子黄素和5 mg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。

关键词: 3,6,7-三甲基槲皮万寿菊素, 对羟基苯甲酸, 高速逆流色谱, 蒿黄素, 蔓荆子, 蔓荆子黄素

Abstract: 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 from 250 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),1H-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.

Key words: 3,6,7-trimethylquercetagetin, 4-hydroxybenzoic acid, artemetin, casticin, Viticis Fructus, high-speed counter-current chromatography (HSCCC)

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