色谱

色谱 ›› 2016, Vol. 34 ›› Issue (6): 591-595.DOI: 10.3724/SP.J.1123.2016.03009

• 研究论文 • 上一篇    下一篇

制备色谱法分离纯化高良姜黄酮中高良姜素和山柰素

侯红瑞1, 黄吉东2, 陈玲2,3, 黄嫣然3, 王春晓1   

  1. 1. 茂名职业技术学院, 广东 茂名 525000;
    2. 广东中轻枫泰生化科技有限公司, 广东 茂名 525427;
    3. 华南理工大学食品科学与工程学院, 广东 广州 510640
  • 收稿日期:2016-03-06 出版日期:2016-06-08 发布日期:2013-01-23
  • 通讯作者: 陈玲
  • 基金资助:

    茂名市科技计划项目([2015]14)

Isolation and purification of galangin and kaempferide from Alpinia officinarum Hance by preparative high-performance liquid chromatography

HOU Hongrui1, HUANG Jidong2, CHEN Ling2,3, HUANG Yanran3, WANG Chunxiao1   

  1. 1. Maoming Polytechnic, Maoming 525000, China;
    2. Guangdong Zhongqing FONTI Biochemical Science & Technology Co., Ltd., Maoming 525427, China;
    3. School of Food Science and Engineering, South China University of Technology, Guangzhou 510640, China
  • Received:2016-03-06 Online:2016-06-08 Published:2013-01-23
  • Supported by:

    Maoming Science and Technology Project, China (No. [2015]14).

PDF

262

被引次数

3

摘要：

建立了制备型高效液相色谱(Prep-HPLC)分离高良姜黄酮中高良姜素和山柰素的方法。高良姜黄酮经HPD-600树脂吸附洗脱纯化后,采用Prep-HPLC分离高良姜黄酮中高良姜素和山柰素。制备色谱条件:流动相为甲醇-0.6%(v/v)乙酸水溶液(58:42, v/v),柱温为常温,流速为7.0 mL/min,检测波长为360 nm,进样量为700 μ L,上样质量浓度为10.0 g/L。分离的单体由质谱和核磁共振氢谱、碳谱鉴定确证为高良姜素和山柰素,HPLC外标法定量,纯度分别为99.5%和99.7%。该方法分离效果好、高效、低毒,可用于高良姜中高良姜素和山柰素的分离制备。

关键词: 纯化, 分离, 高良姜, 高良姜素, 山柰素, 制备色谱

Abstract:

A method of the preparation of galangin and kaempferide from Alpinia officinarum Hance flavonoids using preparative high-performance liquid chromatography (Prep-HPLC) was established. After the Alpinia officinarum Hance flavonoids was purified by HPD-600 resin-based column chromatography, the flavonoid components were separated by Prep-HPLC on a Venusil XBP-C18 column (250 mm×21 mm, 5.0 μ m). The mixture of methanol and 0.6% (v/v) acetic acid solution (58:42, v/v) was used as mobile phase at a flow rate of 7.0 mL/min. The sample volume was 700 μ L and the UV detection wavelength was 360 nm. With MS and NMR, the structures of component I and component II of the Alpinia officinarum Hance flavonoids were identified. The average relative molecular mass of the component I was 269, the same as galangin; and that of the component II was 299, the same as kaempferide. HPLC analysis showed that the purities of galangin and kaempferide were 99.5% and 99.7% respectively. The method is simple and of low toxicity. It can be applied to the separation and preparation of galangin and kaempferide.

Key words: Alpinia officinarum Hance, galangin, isolation, kaempferide, preparative high-performance liquid chromatography (Prep-HPLC), purification

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