pH梯度洗脱高速逆流色谱制备性分离决明子中的橙黄决明素和大黄酸

Preparative Separation of Aurantio-obtusin and Rhein from Semen cassiae by High Speed Counter-current Chromatography Using pH-gradient Elution

摘要: 目的建立一种从决明子提取物中分离特征性成分橙黄决明素的高效制备性分离方法。方法采用高速逆流色谱技术，针对目的化合物选择合适的两相溶剂体系，水相为流动相并采用pH梯度洗脱。结果采用制备性高速逆流色谱技术一次性从150 mg决明子提取物中分离得到了28 mg橙黄决明素以及30 mg大黄酸，其纯度分别为98.7%和95.5%。结论采用pH梯度洗脱的方法能快速的分离得到中草药中的蒽醌类化合物。

Abstract: OBJECTIVE To establish an efficient method for preparative separation of the characteristic constituent aurantio-obtusin from the crude extract of Semen cassiae.METHODS High speed counter-current chromatography was employed and the optimum two-phase solvent system methyl tert.-butyl ether-water was selected for the target compounds with a pH-gradient elution.RESULTS 28 mg aurantio-obtusin at over 98.7% purity and 30 mg of rhein at over 95.5% purity by high-performance liquid chromatography (HPLC) analysis were isolated by preparative high speed counter-current chromatograpy from 150 mg of the crude extract and their structures were identified by 1H-NMR.CONCLUSION A simple and quick preparative separation method was presented for purification of hydroxyanthraquinones from the traditional Chinese herb.