食品科学

• 分析检测 • 上一篇    下一篇

高效逆流色谱分离化橘红中黄酮类化合物及组分结构鉴定

尹 鹭,曹学丽,徐 静,成 超,王 尉,乐胜峰,周晓晶   

  1. 1.北京工商大学食品学院,食品添加剂与配料北京高校工程研究中心,北京 100048;
    2.北京市理化分析测试中心,北京 100089
  • 出版日期:2013-10-25 发布日期:2013-09-28

Preparative Separation of Flavonoids from Exocarpium Citri grandis by High Performance Countercurrent Chromatography

YIN Lu,CAO Xue-li,XU Jing,CHENG Chao,WANG Wei,YUE Sheng-feng,ZHOU Xiao-jing   

  1. 1. Beijing Higher Institution Engineering Research Center of Food Additives and Ingredients,School of Food and Chemical Engineering, Beijing Technology and Business University, Beijing 100048, China;
    2. Beijing Center for Physical and Chemical Analysis, Beijing 100089, China
  • Online:2013-10-25 Published:2013-09-28

摘要:

应用高效逆流色谱法分离纯化了化橘红中两种黄酮类化合物。以乙酸乙酯-正丁醇-水(1:4:5,V/V )为两相溶剂系统,从1g粗提物中可1次分离得到纯度大于98%的柚皮苷单体83.3mg。以二氯甲烷-甲醇-水(10:7:4,V/V)和正己烷-乙酸乙酯-甲醇-水(1:1:1:1,V/V)为溶剂系统,可从1g粗提物的酸解物中经2次分离得到纯度大于98%的柚皮素单体27.5mg。两种物质的分离时间均在60min内,该法简便、快速、制备量大,可用于化橘红中黄酮类化合物的快速分离制备。

关键词: 高效逆流色谱, 化橘红, 柚皮苷, 柚皮素

Abstract:

Two flavonoids were isolated and purified from the extract of Exocarpium Citri grandis by high performance
countercurrent chromatography (HPCCC). A two-phase solvent systems composed of ethyl acetate-1-butanol-water (1:4:5,
V/V) was used to separate naringin directly from the crude extract of Exocarpium Citri grandis. The method allowed the
separation of 83.3 mg of individual naringin with purity of over 98% from 1 g of crude extract. A solvent system composed
of dichloromethane, methanol and water (10:7:4, V/V), or hexane, ethyl acetate, methanol and water (1:1:1:1, V/V) was used
in two steps to separate naringenin from the acid hydrolyzed product of crude extract. The method allowed the separation
of 27.5 mg of individual naringenin with purity of over 98% from 1 g of acid hydrolyzed product. Separation of the two
compounds was achieved within 60 min. The HPCCC method is a relatively simple and fast method with a high-loading
capacity suitable for the isolation and purification of flavonoids from Exocarpium Citri grandis.

Key words: high-performance counter-current chromatography (HPCCC), Exocarpium Citri grandis, naringin, naringenin