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

椭圆叶花锚的主要活性成分为口山酮类化合物,这类化合物具有利胆、抗炎、抗菌及抗病毒活性。应用高速逆流色谱法建立了2种高纯度口山酮苷元的分离制备方法。对椭圆叶花锚氯仿萃取部位运用高速逆流色谱分离纯化,以正己烷-乙酸乙酯-甲醇-水(5∶5∶7∶5,v/v/v/v)为两相溶剂系统,上相为固定相,下相为流动相。在主机转速800r/min,流动相流速1.5 mL/min,检测波长254 nm条件下进行分离制备。所得产物经高效液相色谱分析检测,其化学结构由核磁共振氢谱(1H NMR)和核磁共振碳谱(13C NMR)鉴定。在此条件下,从100 mg粗样品中一步分离得到18 mg 1-羟基-2,3,5-三甲氧基口山酮,14 mg 1-羟基-2,3,4,5-四甲氧基口山酮。经高效液相色谱分析,其纯度均达98%以上。该方法简便、快速,所得产物纯度高,适合于椭圆叶花锚口山酮苷元的制备分离。

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 n-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 1-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 1H nuclear magnetic resonance（1H NMR） and 13C NMR.The established method is simple,highly efficient and suitable for large scale separation of xanthones from Halenia elliptica.