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制备型高速逆流色谱分离纯化长松萝中的松萝酸
引用本文:迟春艳,石波,程永强,梁平,李静梅. 制备型高速逆流色谱分离纯化长松萝中的松萝酸[J]. 食品科学, 2009, 30(3): 127-129. DOI: 10.7506/spkx1002-6630-200903027
作者姓名:迟春艳  石波  程永强  梁平  李静梅
作者单位: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
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  
收稿时间:2008-02-28

Isolation and Purification of Usnic Acid from Usnea longissima by Preparative High-speed Counter-current Chromatography
CHI Chun-yan,SHI Bo,CHENG Yong-qiang,LIANG Ping,LI Jing-mei. Isolation and Purification of Usnic Acid from Usnea longissima by Preparative High-speed Counter-current Chromatography[J]. Food Science, 2009, 30(3): 127-129. DOI: 10.7506/spkx1002-6630-200903027
Authors:CHI Chun-yan  SHI Bo  CHENG Yong-qiang  LIANG Ping  LI Jing-mei
Affiliation:(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)
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%.
Keywords:high-speed counter-current chromatography  Usnea longissima  usnic acid  isolation  purification  
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