食品科学 ›› 2010, Vol. 31 ›› Issue (14): 275-279.doi: 10.7506/spkx1002-6630-201014063

• 分析检测 • 上一篇    下一篇

杜仲绿原酸的分离纯化及结构鉴定

卢 琪,段家彩,高 丽,陈若雯,傅虹飞,潘思轶*   

  1. 华中农业大学食品科学技术学院
  • 收稿日期:2009-10-19 出版日期:2010-07-15 发布日期:2010-12-29
  • 通讯作者: 潘思轶 E-mail:pansiyi@mail.huau.edu.cn

Purification and Structural Identification of Chlorogenic Acid from Eucommia ulmoides Leaves

LU Qi,DUAN Jia-cai,GAO Li,CHEN Ruo-wen,FU Hong-fei,PAN Si-yi*   

  1. College of Food Science and Technology, Huazhong Agricultural University, Wuhan 430070, China
  • Received:2009-10-19 Online:2010-07-15 Published:2010-12-29
  • Contact: PAN Si-yi* E-mail:pansiyi@mail.huau.edu.cn

摘要:

筛选大孔树脂纯化澄清后的杜仲绿原酸粗提液,并对纯化后的绿原酸进行初步的结构鉴定。采用壳聚糖、活性炭澄清绿原酸的粗提液,选取7 种不同类型的大孔树脂对杜仲绿原酸进行静态吸附解吸实验比较。结果表明,NKA-2 型大孔树脂对绿原酸有较好的选择性,其吸附率和解吸率分别为99.67% 和62.8%。盐酸调整洗脱液的pH 值为3,洗脱液的体积分数为30% 时,洗脱效果最好。澄清后的绿原酸粗提液经乙酸乙酯萃取除去黄酮,再用NKA-2 型树脂进行梯度洗脱,可得到纯度为76.3% 的绿原酸。HPLC-MS 分析表明,绿原酸是咖啡酸和奎尼酸缩合的缩酚酸。

关键词: 绿原酸, 大孔树脂, 纯化, 鉴定

Abstract:

Eucommia ulmoides leaves were extracted with 60% aqueous ethanol under the assistance of ultrasound. The crude extract was then condensed on a rotation evaporator, added with chitosan acetic acid solution and stirred, allowed to stand at 60℃ for 60 min for precipitate sedimentation, and filtrated. The filtrate was decolorized with activated carbon prior to 5-time ethyl acetate extraction to remove flavonoids. The lower phase was collected and a chlorpgenic acid extract was obtained. Seven types of moroporous resins were used to purify the chlorpgenic acid extract, and NKA-2 was the selected resin because it exhibited good selectivity to chlorpgenic acid and the static adsorption and desorption ratios were 99.67% and 62.8%. The use of 30% acidified ethanol (pH 3) provided an optimum elution. After NKA-2 purification in the gradient elution mode, a chlorpgenic acid product with 76.3% purity was obtained. Chlorpgenic acid was confirmed by HPLC-MS analysis to be a condensation product of caffeic acid and quinic acid.

Key words: chlorogenic acid, macroporous resin, purification, identification

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