| Summary: | 碩士 === 國立中正大學 === 化學研究所 === 89 === Abstract
Capillary Electrochromatography (CEC) combines the desirable features of capillary electrophoresis (CE) and liquid chromatography. The preparation of retention frits for capillary column of CEC is one of the most important steps for this technique. In this investigation, porous silica frits were prepared via spot-heating of a silicate solution. The optimal sodium silicate concentrations were 10.8% silica and 5.6% sodium hydroxide (w/v) for outlet and inlet frits. The heating time was 5s and applied voltage was 5V. Three ODS-2 columns were prepared for the separation of four cholesterols. Buffer solution of 80%MeCN/20% Tris 10mM,pH=8.0,and running voltage of 20kV were the optimized conditions for four cholesterols. The RSD of the migration times for four cholesterols were 2.85%, 3.81%, 5.26%, and 7.09%. The separation reproducibility (RSD) was below 1.2% for each column. The results demonstrated the good reproducibility for the columns prepared by this work. This procedure was applied to pack ß-cyclodextrin (ß-CD) stationary phase for chiral separation of propranolol. The optimized conditions of the polar-organic mobile phase for chiral separation of propranolol were 95%MeCN / 5%MeOH / 1.2%HOAc / 0.8%TEA. The column efficiency (N/m) was about 130000,and reproducibility (RSD) was below 0.2%.
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