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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150mm直径动态轴向压缩色谱柱的VLC,从100g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17h。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)S7-200 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 f 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≈ΔR f/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.

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