自动真空液相色谱装置的研制及其在五味子成分分离中的应用  

Development of an automatic vacuum liquid chromatographic device and its application in the separation of the components from Schisandra chinensis(Turcz)Baill.

作　　者：朱靖博[1,2] 刘宝月[1] 单世波 丁燕[1,2] 寇自农[2,3] 萧伟[4] 

机构地区：[1]大连工业大学食品学院,辽宁大连116034 [2]大连工业大学植物资源化学与应用研究所,辽宁大连116034 [3]大连工业大学实验仪器中心,辽宁大连116034 [4]江苏康缘药业股份有限公司,江苏连云港222001

出　　处：《色谱》2015年第8期864-868,共5页Chinese Journal of Chromatography

基　　金：大连市科技计划项目(2014E12SF065);辽宁省高等学校重大科技平台项目(辽教发[2011]191号)

摘　　要：为满足天然产物高效分离的需求,本文研制了自动真空液相色谱（AUTO-VLC）装置并用于五味子石油醚萃取物的分离。该装置由自主设计的流动相储备系统、10通分流切换阀、3通切换阀、3个不同规格的动态轴向压缩色谱柱、10通馏分收集阀和馏分收集器组成,采用可编程逻辑控制器（PLC）S7-200实现了分离过程的不同比例流动相切换、不同规格色谱柱选择、分离时间设定及馏分收集的自动控制及监测。应用于五味子成分分离的结果表明：采用150 mm直径动态轴向压缩色谱柱的VLC,从100 g五味子石油醚萃取物中一次分离得到6个组成明显不同的样品（S1～S6）。建立了通过多次薄层色谱（TLC）展开筛选VLC分离条件的方法,并进行了分离验证。VLC分离条件选择方法：自动真空液相色谱的初始洗脱剂的比例以首次TLC展开时全部目标化合物的比移值（Rf）介于0～0.45时展开剂的组成为宜;梯度洗脱比例变化以k值（展开次数（n）与Rf的线性函数斜率）和TLC分离度为依据选择;不同Rf范围内洗脱次数由n≈ΔRf/k计算。采用选择的条件从样品S5中分离得到了13个组分和4个纯度在85%以上的化合物,仅耗时17 h。AUTO-VLC的研制对于中药成分的自动和系统性分离具有重要价值。In order to meet the needs of efficient purification of products from natural resources, this paper developed an automatic vacuum liquid chromatographic device （AUTO- VLC） and applied it to the component separation of petroleum ether extracts of Schisandra chinensis （Turcz） Baill. The device was comprised of a solvent system, a 10-position distribu- tion valve, a 3-position changes valve, dynamic axis compress chromatographic columns with three diameters, and a 10-position fraction valve. The programmable logic controller （PLC） $7- 200 was adopted to realize the automatic control and monitoring of the mobile phase changing, column selection, separation time setting and fraction collection. The separation results showed that six fractions （S1-S6） of different chemical components from 100 g Schisandra chinensis （Turcz） Baill. petroleum ether phase were obtained by the AUTO-VLC with 150 mm diameter dynamic axis compress chromatographic column. A new method used for the VLC separation parameters screened by using multiple development TLC was developed and confirmed. The ini- tial mobile phase of AUTO-VLC was selected by taking R_r of all the target compounds ranging from 0 to 0.45 for fist development on the TLC ; gradient elution ratio was selected according to k value （ the slope of the linear function of Rf value and development times on the TLC ） and the resolution of target compounds ; elution times （n） were calculated by the formula n ≈ ΔRf/k. A total of four compounds with the purity more than 85% and 13 other components were separa- ted from S5 under the selected conditions for only 17 h. Therefore, the development of the au- tomatic VLC and its method are significant to the automatic and systematic separation of tradi- tional Chinese medicines.

关 键 词：真空液相色谱 自动化装置 应用 五味子 分离 

分 类 号：O658[理学—分析化学]