The Preparation And Application Of Capillary Liquid Columns

Capillary liquid column is a new separation medium which has developed since 1990s. Compared with the conventional chromatographic column, Capillary column has the following advantages:good permeability, small sample volume, less environmental pollution, low backpressure, fast and efficient. At present, researches on capillary column mostly focus on developing new monolithic and packing materials while only dabbling in techniques of preparing column.In this thesis, the capillary chromatography chiral columns were prepared by high pressure slurry packing, which were used for some enantiomers separation. Meanwhile, the organic copolymer capillary chromatography micro-columns were prepared in situ polymerization, then the prepared columns was evaluated by the self-installed capillary liquid chromatography system.This thesis consists of five chapters.In chapter 1, a review on the capillary liquid chromatography was presented.In chapter 2, we synthesized the cellulose tris (3,5-dimethylphenylcarbamate) chiral solid phase in the experiment. The cellulose tris (3,5-dimethylphenylcarbamate) chiral column was prepared by high pressure slurry packing. The best coated weight and chromatographic performance were achieved by capillary LC separation system. Five chiral analytes were separated. The results showed that this method of column prepared was fast, simple and easy to realize.In the chapter 3, we synthesized the L-proline bonded silica gel chiral solid phase in the experiment. An L-proline bonded silica gel chiral column was prepared by the slurry packing technique. Threeα-amino acids were enantioseparated the self-installed capillary liquid chromatography. The simple and efficient Box-Behnken experimental design was used for the optimization. The optimum conditions of these variables were predicted by using a second-order polynomial model fitted to the results. this method has wide application prospect in separating DL-α-amino. In the chapter 4, the 1-octadecene monolithic column was prepared by ultraviolet light initiation. The best percentage monomer and the key parameters such as column efficiency, column life, and column reproducibility were evaluated by means of capillary-LC. The results showed that this method of column prepared was fast, simple and easy to realize. Then, we separated SudanⅠ, SudanⅡ, SudanⅢ, three phenols and four chrysanthemum ester insecticide.In the chapter 5, the 1-octadecene monolithic column was prepared by microwave irradiation. The key parameters of column preparation, such as temperature, time, pressure, microwave power, can be controlled accurately by using microwave dissolver. Microwave radiation shortens the polymerization time greatly. The results showed that this method of column prepared was fast, simple and easy to realize.