中山大学学报自然科学版 ›› 2010, Vol. 49 ›› Issue (3): 65-69.

• 研究论文 • 上一篇    下一篇

高速逆流色谱分离制备苦茶中的苦茶碱

程悦1,严志勇1,卢嘉丽1,叶创兴2,王冬梅1   

  1. (1中山大学药学院,广东 广州 510006;2中山大学生命科学学院,广东 广州 510275)
  • 收稿日期:2009-09-07 修回日期:1900-01-01 出版日期:2010-05-25 发布日期:2010-05-25
  • 通讯作者: 王冬梅

Isolation and Preparation of Theacrine by HighSpeed CounterCurrent Chromatography from Camellia assamica var.kucha

CHENG Yue1, YAN Zhiyong1, LU Jiali1, YE Chuangxing2, WANG Dongmei1



  

  1. (1School of Pharmaceutical Sciences, Sun Yatsen University, Guangzhou 510080, China; 2School of Life Sciences, Sun Yetsan University, Guangzhou 510275, China)
  • Received:2009-09-07 Revised:1900-01-01 Online:2010-05-25 Published:2010-05-25

摘要: 应用高速逆流色谱法分离制备了苦茶中的苦茶碱。以正己烷-二氯甲烷-甲醇-水(体积比为1∶〖KG-*2〗5∶〖KG-*2〗4∶〖KG-*2〗2)为两相溶剂系统,在主机转速800 r/min、流速20 mL/min、检测波长278 nm条件下进行分离制备。所得流分经高效液相色谱法检测,与对照品进行比较,并通过质谱、核磁共振氢谱、碳谱鉴定化合物的结构。结果表明,从222 g苦茶总生物碱提取物中分离得到了3个化合物,分别为可可碱5 mg,苦茶碱389 mg,咖啡碱41 mg,纯度均在99%以上,系首次采用高速逆流色谱法对苦茶中的苦茶碱进行分离。该法具有简便、快速的优点。

关键词: 高速逆流色谱, 苦茶, 嘌呤生物碱, 苦茶碱

Abstract: Theacrine was prepared, isolated and purified from Camellia assamica var. kucha by highspeed countercurrent chromatography. A twophase solvent system composed of hexanedichloromethanemethanolwater (1∶5∶4∶2, v/v/v/v) was selected with comprehensive analysis of the settling time, the ratio of up and down phases volume and the K value. Five mg of theobromine, 389 mg of theacrine and 41 mg of caffeine with their purities over 99% were obtained from 222 g of the crude extract of Camellia assamica var. kucha under the condition of a flow rate of 20 mL/min, 800 r/min and the detection wavelength of 278 nm. The obtained fractions were analyzed by high perform liquid chromatography, compared with standard substance and identified by MS, 1H NMR and 13C NMR methods. Theacrine was the first time isolated from Camellia assamica var. kucha by HSCCC, which is a simple, rapid and effective method.

Key words: HSCCC, Camellia assamica var. kucha, purine alkaloid, theacrine

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