一种反相毛细管液相色谱整体柱的制备方法及其色谱性能

Preparation and Evaluation of Monolithic Silica Column for Capillary Liquid Chromatography

在优化条件下成功制备了50μm、75μm、100μm和200μm等多种口径的硅胶基质毛细管液相色谱整体柱,克服了文献报道中常见的开裂、重现性差等缺点。考察了柱压降与流速的关系,以多环芳烃系列化合物评价了自制的C18硅胶基质毛细管液相色谱整体柱的色谱性能,在以甲醇-水为流动相的反相色谱条件下,5种化合物(苯、萘、联萘、芴和蒽)得到了基线分离。该柱对萘的柱效达到了67000塔板/米。

A series of silica-based capillary monolithic columns for capillary high performance liquid chromatography （μ-HPLC） with diameters of 50 μm, 75 μm, 100 μm and 200 μm were prepared under optimal conditions. The influence of the various synthesis parameters, such as the pretreatment of capillary, the ageing and drying of the gel, was discussed. The preparation method reported here overcomes the common shortcomings of dehiscence and bad repeatability. The column back-pressure and linear velocity of mobile phase were evaluated for fast separation. The chromatographic performance of the C18 silica-based capillary monolithic column prepared by our group was test by a series of aromatic compounds, The baseline separation of 5 compounds （benzene, naphthalene, diphenyl, fluorene and anthracene） can be obtained under optimized capillary chromatographyic conditions. Column efficiency of 67000 plates/m was achieved for naphthalene.