色谱2012,Vol.30Issue(5):543-546,4.DOI:10.3724/SP.J.1123.2012.01017
高速逆流色谱分离制备椭圆叶花锚中的2种(口山)酮苷元
Preparative separation of two xanthones from Halenia elliptica by high-speed counter-current chromatography
摘要
Abstract
A high performance method for isolation and purification of two xanthones from a crude extract of Halenia elliptica was successfully established by utilizing high-speed counter-current chromatography (HSCCC). The separation was performed with a two-phase solvent system composed of w-hexane-ethyl acetate-methanol-water (5:5:7=5, v/v/v/v) with the lower phase as the mobile phase at a flow rate of 1.5 mL/min. The apparatus was rotated at 800 r/min. The effluent was detected at 254 nm. Under the optimized conditions, 18 mg of 1-hydroxy-2,3, 5-trimethoxyxanthone and 14 mg of l-hydroxy-2, 3 , 4, 5-tetramethoxyxanthone were obtained from 100 mg of the crude extract of Halenia elliptica in one-step separation within 360 min. The results of high performance liquid chromatographic ( HPLC) analysis showed that the purity of each of the target compounds was over 98%. The chemical structures of the two compounds were confirmed by 'H nuclear magnetic resonance ('H NMR) and 13C NMR. The established method is simple, highly efficient and suitable for large scale separation of xanthones from Halenia elliptica.关键词
高速逆流色谱/1-羟基-2,3,5-三甲氧基(口山)酮/1.羟基-2,3,4,5-四甲氧基(口山)酮/椭圆叶花锚Key words
high-speed counter-current chromatography (HSCCC)/ l-hydroxy-2, 3 , 5-trimethoxyxanthone / l-hydroxy-2,3 ,4,5-tetramethoxyxanthone/ Halenia elliptica分类
化学化工引用本文复制引用
刘永玲,陈涛,王萍,尤进茂,刘永军,李玉林..高速逆流色谱分离制备椭圆叶花锚中的2种(口山)酮苷元[J].色谱,2012,30(5):543-546,4.基金项目
中国科学院知识创新工程重要方向项目. ()