于晓礼, 皮子凤, 胡秀丽, 宋凤瑞, 刘志强. 高速逆流色谱结合电喷雾多级串联质谱方法高效分离制备、鉴定五味子木脂素类成分J. 药学学报, 2014,49(1): 78-82.
引用本文: 于晓礼, 皮子凤, 胡秀丽, 宋凤瑞, 刘志强. 高速逆流色谱结合电喷雾多级串联质谱方法高效分离制备、鉴定五味子木脂素类成分J. 药学学报, 2014,49(1): 78-82.
YU Xiao-li, PI Zi-feng, HU Xiu-li, SONG Feng-rui, LIU Zhi-qiang. High performance preparation and structural confirmation of lignans from Schisandrae chinensis fructus by using HSCCC combined with ESI-MSn methodJ. Acta Pharmaceutica Sinica, 2014,49(1): 78-82.
Citation: YU Xiao-li, PI Zi-feng, HU Xiu-li, SONG Feng-rui, LIU Zhi-qiang. High performance preparation and structural confirmation of lignans from Schisandrae chinensis fructus by using HSCCC combined with ESI-MSn methodJ. Acta Pharmaceutica Sinica, 2014,49(1): 78-82.

高速逆流色谱结合电喷雾多级串联质谱方法高效分离制备、鉴定五味子木脂素类成分

High performance preparation and structural confirmation of lignans from Schisandrae chinensis fructus by using HSCCC combined with ESI-MSn method

  • 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。

     

    Abstract: 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-MSn), 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.

     

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