高速逆流色谱快速分离山竹子素的制备方法实验研究  

Preparative Isolation and Purification of Garcinol by High-Speed Countercurrent Chromatography

作　　者：张宝军[1,2] 房庆伟 谭红胜[1,2] 郑昌武[1,2] 付文卫[1,2] 

机构地区：[1]上海中医药大学中药学院,上海201203 [2]中药创新药物研发上海高校工程研究中心,上海201203

出　　处：《世界科学技术-中医药现代化》2017年第2期254-259,共6页Modernization of Traditional Chinese Medicine and Materia Medica-World Science and Technology

基　　金：上海中医药大学预算内项目(2016YSN06):菲岛福木果实抗肿瘤活性成分研究;负责人:付文卫;上海中医药大学青年基金项目(81602990):岭南山竹子中活性提取化合物的合成;结构修饰及抗EV71病毒研究;负责人:郑昌武

摘　　要：目的:制备山竹子素(garcinol)化学对照品。方法:采用高速逆流色谱法,从多花山竹子、山木瓜、大叶藤黄三种藤黄属植物粗提物中快速分离化合物garcinol,溶剂系统为正己烷-乙酸乙酯-95%乙醇-水(8:8:12:4,体积比),上相做固定相,下相做流动相,仪器转速850 rpm,温度25℃,检测波长254 nm,目标化合物馏分经Sephadex LH-20凝胶柱柱色谱纯化,所得样品由高效液相色谱法检测纯度。结果:可从104.765 g多花山竹子枝、105.270 g山木瓜枝、102.318 g大叶藤黄果实中分离得到garcinol的量分别为45 mg、281 mg、4080 mg,纯度分别为98.72%、98.36%、98.42%。结论:通过对比三种植物样品处理方法,结果以大叶藤黄果实作为原料时,正己烷-乙酸乙酯-95%乙醇-水(5:5:5:5,体积比)萃取的上相浸膏,经高速逆流色谱法结合凝胶柱柱色谱法,可快速高效、大量制备化合物garcinol。实验表明该方法效率高,可操作性强,制备量大。This study aimed at preparing the chemical reference substance of garcinol.A preparative high-speed countercurrent chromatography（HSCCC） was adopted for the isolation of garcinol from the twigs of Garcinia multiflora Champ, G. esculenta Y. H. Li and the fruits of G. xanthochymus Hook. f. ex T. Anders. The crude extracts were separated by HSCCC with two phase solvent systems composed of n-hexane-ethyl acetate-95% ethanol-water（8？8？12？4, volume ratio） using the upper stationary phase and the lower mobile phase. Under the conditions of a flow rate of 2.0 and 4.0 m L·min-1, and the apparatus rotation at 850 rpm, the column temperature at 25℃ and the detection wavelength at 254 nm,the fraction containing garcinol was purified by the Sephadex LH20 chromatography. The purity test in the extracts was determined by high-performance liquid chromatography. As a result, the contents of garcinol were 45, 281 and 4080 mg respectively separated from 104.765 g twigs of G. multiflora Champ, 105.270 g G. esculenta Y. H. Li and 102.318 g the fruits of G. xanthochymus Hook. f. ex T. with the purity of 98.72%, 98.36% and 98.42%. Compared with the sample pretreatments and separation efficiency of the three plants, it was found that the fat-soluble extracts rapidly and efficiently extracted using n-hexane-ethyl acetate-95% ethanol-water（5？5？5？5, volume ratio） contained abundant garcinol taking fruits of G. xanthochymus Hook. f. ex T as the raw material with the combination of HSCCC and Sephadex LH-20 chromatography. In conclusion, it was indicated that the combination method is efficient with high operability and large preparation quantity.

关 键 词：高速逆流色谱 大叶藤黄 山竹子素 制备方法 

分 类 号：R93[医药卫生—生药学]