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作 者:于晓礼[1,2] 皮子凤[1] 胡秀丽[2] 宋凤瑞[1] 刘志强[1]
机构地区:[1]中国科学院长春应用化学研究所长春质谱中心,吉林长春130022 [2]吉林大学药学院,吉林长春130021
出 处:《药学学报》2014年第1期78-82,共5页Acta Pharmaceutica Sinica
基 金:科技部创新方法工作专项资助项目(2012IM030600);吉林省自然科学基金资助项目(201015101)
摘 要: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 counter-current chromatography (HSCCC) was used to high performance separate and prepare lignans from Schisandrae chinensis fructus. The solvent system is composed of n-hexane-ethyl acetate-methanol-water (9 : 1 : 5 : 5) and n-hexane-ethyl acetate-methanol-water (9 : 1 : 9 : 5), speed is at 900 r.min-1, and flow rate is at 2.0 mL min-1. Five fractions from Schisandrae chinensis fructus extract were separated and prepared with one HSCCC process. They were identified as schisandrin, gomisin J, schisandrol B, schisantherin A and deoxyschizandrin by electrospray ionization-multiple tandem mass spectrometry (ESI-MS n), respectively. Their contents were obtained in 98.74%, 94.32%, 99.53%, 94.23% and 98.68% by ultra high performance liquid chromatography (UPLC), separately. The rapid and simple method can be applied for the preparation of lignans from Schisandrae chinensis fructus.
关 键 词:高速逆流色谱 电喷雾多级串联质谱 五味子 木脂素
分 类 号:R917[医药卫生—药物分析学]
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