食品科学 ›› 2011, Vol. 32 ›› Issue (2 ): 57-61.doi: 10.7506/spkx1002-6630-201102014

• 工艺技术 • 上一篇    下一篇

柿叶黄酮化合物分离制备

孙化鹏1,钟晓红1,*,陆英1,2,周舟1   

  1. 1. 湖南农业大学园艺园林学院
    2. 湖南农业大学 湖南省天然产物工程技术研究中心
  • 收稿日期:2010-04-13 修回日期:2010-12-09 出版日期:2011-01-25 发布日期:2011-01-10
  • 通讯作者: 钟晓红 E-mail:xh-zhong@163.com
  • 基金资助:

    长沙市科技局项目(K06095-22)

Separation, Purification and Structural Analysis of Flavonoids from Diospyros kaki Leaves

SUN Hua-peng1,ZHONG Xiao-hong1,*,LU Ying1,2,ZHOU Zhou1   

  1. 1. College of Horticulture and Landscape, Hunan Agricultural University, Changsha 410128, China;
    2. Hunan Provincial Research Center of Natural Products, Hunan Agricultural University, Changsha 410128, China
  • Received:2010-04-13 Revised:2010-12-09 Online:2011-01-25 Published:2011-01-10
  • Contact: ZHONG Xiao-hong E-mail:xh-zhong@163.com

摘要:

应用高速逆流色谱法和制备型高效液相色谱法分离制备柿叶黄酮化合物并进行初步结构鉴定。采用乙酸乙酯- 甲醇- 水(5:1:5,V/V)做溶剂系统,在主机转速850r/min、流速1.5mL/min、检测波长254nm 条件下进行HSCCC分离纯化,所得流分浓缩干燥后再采用制备型HPLC 分离制备柿叶黄酮化合物,所得产物采用HPLC 检测并进行显色反应、紫外图谱和质谱分析。结果表明,从柿叶粗提物中分离所得4 种化合物是以槲皮素和山奈酚为苷元的黄酮苷类化合物。

关键词: 柿叶, 黄酮化合物, 高速逆流色谱, 制备型高效液相色谱, 结构鉴定

Abstract:

In this study, high-speed countercurrent chromatography (HSCCC) followed by preparative high performance liquid chromatography (HPLC) was used to separate and purify flavonoid monomers from the crude ethyl acetate extract from Diospyros kaki leaves. Meanwhile, the flavonoid monomers obtained were preliminarily identified by color development reaction and further structurally characterized by UV spectroscopy and mass spectroscopy. The HSCCC separation of flavonoids was achieved by using a solvent system composed of ethylacetate, methanol and water (5:1:5, V/V) at a flow rate of 1.5 mL/min and setting the rotational speed at 850 r/min with a detection wavelength set at 254 nm. For further separation, the separated fractions were then applied to preparative HPLC, and 4 flavonoid compounds, named A-Ⅱ, A-Ⅲ, B-Ⅱ and B-Ⅲ, were obtained. A-II and A-III might be quercetin flavonoids, and B-Ⅱ and B-Ⅲ might be kaemoferol.

Key words: Diospyros kaki leaves, flavonoids, HSCCC, preparative HPLC, structural identification

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