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采用新型直立式盘管行星离心逆流色谱法从南蛇藤中制备分离纯化雷公藤红素。

Preparative isolation and purification of celastrol from Celastrus orbiculatus Thunb. by a new counter-current chromatography method with an upright coil planet centrifuge.

作者信息

Wu Shihua, Sun Cuirong, Wang Kuiwu, Pan Yuanjiang

机构信息

Department of Chemistry, Zhejiang University, Hangzhou, Zhejiang Province 310027, China.

出版信息

J Chromatogr A. 2004 Feb 27;1028(1):171-4. doi: 10.1016/j.chroma.2003.11.072.

DOI:10.1016/j.chroma.2003.11.072
PMID:14969291
Abstract

A new counter-current chromatography (CCC) method with an upright coil planet centrifuge, which holds four identical multilayer coil columns in the symmetrical positions around the centrifuge axis, was applied to the isolation and purification of celastrol from the roots of Celastrus orbiculatus Thunb. The crude celastrol was obtained by elution with light petroleum from ethanol extracts using 15 cm x 5 cm i.d. silica gel flash chromatography. Preparative CCC with a two-phase system composed of light petroleum (bp 60-90 degrees C)-ethyl acetate-tetrachloromethane-methanol-water (1:1:8:6:1, v/v) was successfully performed, yielding 798 mg celastrol at 99.5% purity from 1020 mg of the crude sample in one step separation.

摘要

一种采用直立式盘管行星离心机的新型逆流色谱(CCC)方法被应用于从南蛇藤根中分离纯化雷公藤红素。该离心机在围绕离心机轴的对称位置上装有四个相同的多层盘管柱。粗制雷公藤红素通过使用内径为15 cm×5 cm的硅胶快速柱色谱,用石油醚从乙醇提取物中洗脱获得。使用由石油醚(沸点60 - 90℃)-乙酸乙酯-四氯化碳-甲醇-水(1:1:8:6:1,v/v)组成的两相系统成功进行了制备型CCC,在一步分离中从1020 mg粗样品中获得了纯度为99.5%的798 mg雷公藤红素。

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