食品科学 ›› 2009, Vol. 30 ›› Issue (3): 127-129.doi: 10.7506/spkx1002-6630-200903027

• 基础研究 • 上一篇    下一篇

制备型高速逆流色谱分离纯化长松萝中的松萝酸

迟春艳1,石波1,程永强2,梁 平1,李静梅3   

  1. 1.中国农业科学院饲料研究所 2.中国农业大学食品科学与营养工程学院 3.中国农业科学院作物科学研究所
  • 收稿日期:2008-02-28 修回日期:2008-05-05 出版日期:2009-02-01 发布日期:2010-12-29
  • 通讯作者: 石波 E-mail:shibo@mail.caas.net.cn
  • 基金资助:

    “十一五”国家科技支撑计划项目(2006BAD12B05-02-01)

Isolation and Purification of Usnic Acid from Usnea longissima by Preparative High-speed Counter-current Chromatography

CHI Chun-yan1,SHI Bo1,*,CHENG Yong-qiang2,LIANG Ping1,LI Jing-mei3   

  1. (1. Feed Research Institute, Chinese Academy of Agricultural Sciences, Beijing 100081, China;
    2. College of Food and Nutritional Engineering, China Agricultural University, Beijing 100083, China;
    3. Institute of Crop Science, Chinese Academy of Agricultural Sciences, Beijing 100081, China)
  • Received:2008-02-28 Revised:2008-05-05 Online:2009-02-01 Published:2010-12-29
  • Contact: SHI Bo1,*, E-mail:shibo@mail.caas.net.cn

摘要:

利用制备型高速逆流色谱分离纯化长松萝中的松萝酸,经过高效液相色谱、核磁共振检测,确定其纯度及结构。将长松萝破碎后用石油醚(60~90℃)回流浸提4h,浸提液经过滤浓缩后得到松萝酸粗提物。采用正己烷:乙腈:乙酸乙酯:水(8:7:5:0.8,V/V)的两相体系将所得的粗提物进行制备型高速逆流色谱的分离纯化,一次进样25mg,可得到11.2mg 样品。利用高效液相色谱检测该样品纯度达到99%。将得到的样品进行1H-NMR、13C-NMR检测确定其化学结构,并确定该样品为松酸。实验证明制备型高速逆流色谱可以成功地将长松萝中的松萝酸进行分离纯化。

关键词: 制备型高速逆流色谱, 长松萝, 松萝酸, 分离, 纯化

Abstract:

Preparative high-speed counter-current chromatography (HSCCC) was used for the isolation and purification of usnic acid from Usnea longissima. Crude extract was firstly obtained by reflux extraction with petroleum ether at 60 to 90 ℃ for 4 h from dried Usnea longissima. Then hexane-acetonitrile-ethyl acetate-water (8:7:5:0.8, V/V) was used as the two-phase solvent system for purification. Finally the collected components were analyzed using high-performance liquid chromatography (HPLC) and the structure of main component was identified using 1H-NMR and 13C-NMR. By this way, the 11.2 mg of usnic acid is obtained from 25 mg of the crude extract of dried Usnea longissima with the purity of 99%.

Key words: high-speed counter-current chromatography, Usnea longissima, usnic acid, isolation, purification

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