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C_(18)(250 mm×4.6 mm,5μm)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C_(18)(250 mm×30 mm,10μm)为第一、二维分离柱,C_(18)(80 mm×30 mm,10μm)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。
A two-dimensional reversed-phase liquid chromatography（2 D-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 C_（18） 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. C_（18） column（250 mm × 30 mm,10 μm）was selected as the first-and second-dimensional separation column. The C_（18） columns（80 mm×30 mm,10 μm）were selected as enriching columns,and water was chosen as the diluent solution. Lignans from Schisandra chinensiswere separated and purified by 2 D-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.
作者
朱靖博
李文玉
肖伟
丁燕
黄文哲
屠鹏飞
王永华
ZHU Jingbo;LI Wenyu;XIAO Wei;DING Yan;HUANG Wenzhe;TU Pengfei;WANG Yonghua(School of Food Science and Technology,Dalian Polytechnic University,Dalian 116034, China;Jiangsu Kanion Pharmaceutical Corporation Limited,Lianyungang 222001,China;Peking University, Beijing 100871, China;Northwest Agriculture and Forestry University,Yangling 712100, China)
出处
《色谱》
CAS
CSCD
北大核心
2018年第5期464-473,共10页
Chinese Journal of Chromatography
基金
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)~~
关键词
二维反相液相色谱
木脂素
五味子
色谱专家系统软件模拟
two-dimensional reversed-phase liquid chromatography （2D-RPLC）
lignans
Schisandra chinensis
chromatographic expert system software simulation
