Continuous liquid chromatograph and its application to separation of natural organic compounds.

长期以来，无论是在实验室还是在工业中，人们都感到需要一种能够连续分离天然物质和合成化合物混合物的方法，因为广泛使用的间歇色谱技术在使用柱填料时耗时且效率低下。连续色谱分离原理是马丁首先提出的。然而，连续液相色谱法的发展一直不够。本研究设计并构建了用于混合物连续分离的径向流盘式色谱仪。在该装置中，层析填料的空间在上部平板玻璃盘和下部不锈钢盘之间形成。因此，固定相的床层呈圆盘状（厚2毫米，直径270毫米）。磁盘组件由两个变速马达旋转。用硅胶- ods填料在离心力作用下，在1200转/分的转速下制备色谱盘。用该填料圆盘连续分离邻苯二甲酸二-2-乙基己酯和邻苯二甲酸二丁酯混合物，每个组分的进料速率为60mg /h，转速为2rph，甲醇-水（19:1）混合物为洗脱液，流速为8ml /min。以正己烷和乙酸乙酯为混合溶剂，在硅胶盘上以每组分180 mg/h的进料速率连续分离邻苯二甲酸酯。氨基酸、苯丙氨酸和色氨酸的混合物在亲水性聚氯乙烯凝胶上连续层析，得到了令人满意的混合物组分分离。经研究，具有旋转径向流盘的连续型液相色谱仪在混合物的制备分离中是有价值的。

The need for a process which will separate mixtures such as natural substances and synthetic compounds continuously has long been felt, both in laboratory and in industry, because the widely-used batch chromatographic techniques are time-consuming and inefficient in their use of the column packing material. The principle of continuous chromatographic separation was first presented by Martin. However development of continuous liquid phase chromatography has been insufficient.A radial-flow disk chromatograph was designed and constructed in this research for the continuous separation of mixtures. In this apparatus, the space for the chromatographic packing materials is formed between the upper flat glass disk and the lower stainless steel disk. The bed of the fixed phase is, therefore,in the shape of the disk (2 mm thick, 270 mm diameter). The disk assembly is rotated by two variable-speed motors. The chromatographic disk was made by packing with silica gel-ODS under a centrifugal-force field at 1200 rpm. The continuous separation of a mixture of di-2-ethylhexyl phthalate and dibutyl phthalate was achieved using this packed disk, at feed-rate of 60 mg/h for each component under rotation at 2 rph, with methanol-water (19:1) mixture as eluent at flow-rate of 8 ml/min. The continuous separation of the phthalates was also performed on the silica gel disk at feed-rate of 180 mg/h for each component with a mixed solvent of hexane and ethyl acetate. The continuous chromatography of the mixture of amino acids, phenylalanine and tryptophan on a hydrophilic polyvinyl gel eluting with water gave satisfactory separation of the mixture to their components. The continuous liquid chromatograph having a rotating radial-flow disk has been proved to be valuable for the preparative separation of mixtures,so far studied.