色谱

色谱 ›› 2018, Vol. 36 ›› Issue (5): 464-473.DOI: 10.3724/SP.J.1123.2017.12025

• 研究论文 • 上一篇    下一篇

二维反相液相色谱制备五味子中的木脂素

朱靖博1,2, 李文玉1, 肖伟2, 丁燕1, 黄文哲2, 屠鹏飞2,3, 王永华2,4   

  1. 1. 大连工业大学食品学院, 辽宁 大连 116034;
    2. 江苏康缘药业股份有限公司, 江苏 连云港 222001;
    3. 北京大学, 北京 100871;
    4. 西北农林科技大学, 陕西 杨凌 712100
  • 收稿日期:2017-12-27 出版日期:2018-05-08 发布日期:2014-03-21
  • 通讯作者: 朱靖博.E-mail:zhujingb@sina.com;丁燕.E-mail:dingyan_515@hotmail.com
  • 基金资助:

    国家自然科学基金-联合基金项目（U1603285）；辽宁省教育厅基本科研项目（2016J008）；江苏省"双创计划"项目（苏人才[2015]26号）；连云港市"高层次创新创业领军人才集聚工程"项目（连人才[2016]1号）.

Separation of lignans from Schisandra chinensis by two-dimensional reversed-phase liquid chromatography

ZHU Jingbo1,2, LI Wenyu1, XIAO Wei2, DING Yan1, HUANG Wenzhe2, TU Pengfei2,3, WANG Yonghua2,4   

  1. 1. School of Food Science and Technology, Dalian Polytechnic University, Dalian 116034, China;
    2. Jiangsu Kanion Pharmaceutical Corporation Limited, Lianyungang 222001, China;
    3. Peking University, Beijing 100871, China;
    4. Northwest Agriculture and Forestry University, Yangling 712100, China
  • Received:2017-12-27 Online:2018-05-08 Published:2014-03-21
  • Supported by:

    Project of Joint Fund of the National Natural Science Foundation of China (No. U1603285); Basic Scientific Research Project of Education Department of Liaoning Province of China (No. 2016J008); "Double" Project of Jiangsu Province of China (Jiangsu Talent No.[2015]26); "High Level Innovation and Entrepreneurial Talent Gathering Project" in Lianyungang City of China (Lianyungang Talent No.[2016]1).

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摘要：

应用自主研发的具有分离-富集模式的制备色谱工厂，建立了分离制备五味子木脂素有效部位及其单体化合物的方法。该方法首先以C18（250 mm×4.6 mm，5 μm）为色谱柱，水和甲醇为流动相，分离度和保留时间为考察指标，采集4个不同梯度的色谱信息，通过XTool色谱专家系统软件模拟，确定五味子木脂素第一、二维色谱条件；然后采用线性放大的方法，以C18（250 mm×30 mm，10 μm）为第一、二维分离柱，C18（80 mm×30 mm，10 μm）为富集柱，水为富集稀释液，对五味子木脂素进行二维色谱分离纯化；最后第一维分离得到9个可重复组分，第二维分离得到20个高纯度化合物，其中有6个单体化合物。结果表明该法重现性良好，可以实现五味子木脂素的系统性分离，对五味子化学成分的研究具有重要意义。

关键词: 二维反相液相色谱, 木脂素, 色谱专家系统软件模拟, 五味子

Abstract:

A two-dimensional reversed-phase liquid chromatography (2D-RPLC) method was established to separate lignan components and pure compounds from Schisandra chinensis. This method was based on the modules of separation-enrichment and self-developed with independent intellectual property rights. First, a C18 column (250 mm×4.6 mm, 5 μm) was used as the analytical column. A water-methanol mixture was selected as the mobile phase. Separation resolution and retention time were selected as indexes. Gradient chromatography of the lignan extracts was repeated four times and the information was input into XTool, a chromatographic separation software. The conditions for the first-and second-dimensional chromatographic separation were optimized by XTool. Then, linear amplification was used for preparative chromatography. C18 column (250 mm×30 mm, 10 μm) was selected as the first-and second-dimensional separation column. The C18 columns (80 mm×30 mm, 10 μm) were selected as enriching columns, and water was chosen as the diluent solution. Lignans from Schisandra chinensis were separated and purified by 2D-RPLC. Finally, nine lignan components were obtained by the first-dimensional separation. Totally, 20 high-purity compounds, containing six monomers, were obtained by the second-dimensional separation. Experimental results showed that this method has good reproducibility. This method thus allows for the systematic separation of lignans from Schisandra chinensis.

Key words: Schisandra chinensis, chromatographic expert system software simulation, lignans, two-dimensional reversed-phase liquid chromatography (2D-RPLC)

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