高速逆流色谱分离制备茶粕中茶皂素单体

Isolation and Preparation of Teasaponin Monomers from Tea Seed Cake by High-Speed Counter-current Chromatography

目的:建立一种高效、快速的分离制备茶皂素单体的高速逆流色谱方法。方法:微波辅助提取茶皂素后,用D-101大孔树脂初步纯化,所得粗品经高速逆流色谱分离纯化,乙酸乙酯-正丁醇-水(1:4:4,V/V,含体积分数3%的乙酸)为两相溶剂系统,转速800r/min、流速1.5mL/min、检测波长267nm、进样量100mg,所得分离收集液经高效液相色谱法检测。结果:从茶皂素粗提物中分离得到纯度分别为99.1%和94.5%的两种茶皂素单体,经干燥称得其质量分别为11mg和15mg。结论:该方法制备茶皂素单体简便、快速,所得产物的纯度高,为茶皂素的分离纯化提供了一种新途径。

Objective：To develop a rapid and efficient method for preparing teasaponin monomers from tea seed cake using preparative high-speed counter-current chromatography （HSCCC）. Methods：A crude extract rich in teasaponin monomers was obtained from tea seed cake by microwave-assisted extraction,and preliminarily purified by D-101 macroporous resin chromatography,followed by further HSCCC purification/fractionation with a binary phase system made up of ethyl acetate,n-butanol and 3% acetate （1：4：4,V/V） at a flow rate of 1.5 mL/min with rotation at 800 r/min under the conditions of 267 nm detection wavelength and 100 mg sample load. The final purification product was analyzed by HPLC. Results：Two teasaponin monomers with 99.1% and 94.5% purities were obtained after the HSCCC separation,and their dry weights were 11 mg and 15 mg,respectively. Conclusion：The proposed HSCCC method has the characteristics of simplicity,rapidity and high product purity,thereby providing a novel strategy for the separation of teasaponin monomers.