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应用高速逆流色谱技术(HSCCC)从北五味子粗提物中快速分离制备木脂素类成分。采用两种溶剂系统进行洗脱,溶剂系统分别为正己烷-乙酸乙酯-甲醇-水(9∶1∶5∶5)及正己烷-乙酸乙酯-甲醇-水(9∶1∶9∶5),转速900 r·min-1,流速为2.0 mL·min-1,从五味子粗提物一次分离制备出5种单体成分。利用电喷雾多级串联质谱技术(ESI-MSn)及超高效液相色谱技术(UPLC)对高速逆流色谱分离产物进行结构鉴定及纯度分析。5种单体成分分别为五味子醇甲、戈米辛J、五味子醇乙、五味子酯甲和五味子甲素,纯度分别为98.74%、94.32%、99.53%、94.23%和98.68%。该方法快速、简便,分离效率高,适用于五味子木脂素类成分的制备。
High-speed countercurrent chromatography (HSCCC) was used to separate and prepare lignans from crude extracts of Schisandra chinensis. The solvent systems were eluted with two solvent systems: n-hexane-ethyl acetate-methanol-water (9: 1: 5: 5) and n-hexane-ethyl acetate- 5) at a rotational speed of 900 r · min-1 and a flow rate of 2.0 mL · min-1. Five monomer components were isolated from the crude extracts of Schisandra chinensis. The structure and purity of the products were analyzed by ESI-MSn and UPLC. The five monomer components were schizandrin A, Gomisin J, Schizandrol B, Schisandra ester A and Schisandrin A respectively, with the purity of 98.74%, 94.32%, 99.53%, 94.23% and 98.68%, respectively. The method is rapid, simple and has high separation efficiency and is suitable for preparing the components of the schisandrin lignans.