An amine capillary column was developed in a fused-silica capillary as stationary phase and applied to separation of basic compounds by capillary electrochromatography (CEC). The functionalized capillary was prepared ...An amine capillary column was developed in a fused-silica capillary as stationary phase and applied to separation of basic compounds by capillary electrochromatography (CEC). The functionalized capillary was prepared by inmobilization of 3-Aminopropyl)triethoxysilane (APTES). The CEC conditions including APTES and buffer concentration, pH and applied voltage were investigated to obtain the optimal CEC system for the separation of three anesthetics as basic test molecules. The capillary column provided an efficiency of up to 20,000 plates/m. Lidocaine, ketamine and xilacine were baseline separated under the running conditions with 10 mM Na2HPO4 pH 9.0 as BGE. The applied voltage was 5 kV temperature was set at 25oC and UV detection was performed. The resolutions were 4.97 and 1.53 for ketamine, lidocaine and xilacine, respectively. The column used in CEC mode showed better separation of the anesthetics compared with those used in the capillary zone mode. The comparison with reversed stationary phases used in HPLC in terms of resolution (Rs), sensitivity (LOD), efficiency (N), precision (RSD), asymmetry (T) was also performed. This study provided an alternative way for the CEC separation of basic compounds and demonstrated the improvement in the chromatographic parameters.展开更多
文摘An amine capillary column was developed in a fused-silica capillary as stationary phase and applied to separation of basic compounds by capillary electrochromatography (CEC). The functionalized capillary was prepared by inmobilization of 3-Aminopropyl)triethoxysilane (APTES). The CEC conditions including APTES and buffer concentration, pH and applied voltage were investigated to obtain the optimal CEC system for the separation of three anesthetics as basic test molecules. The capillary column provided an efficiency of up to 20,000 plates/m. Lidocaine, ketamine and xilacine were baseline separated under the running conditions with 10 mM Na2HPO4 pH 9.0 as BGE. The applied voltage was 5 kV temperature was set at 25oC and UV detection was performed. The resolutions were 4.97 and 1.53 for ketamine, lidocaine and xilacine, respectively. The column used in CEC mode showed better separation of the anesthetics compared with those used in the capillary zone mode. The comparison with reversed stationary phases used in HPLC in terms of resolution (Rs), sensitivity (LOD), efficiency (N), precision (RSD), asymmetry (T) was also performed. This study provided an alternative way for the CEC separation of basic compounds and demonstrated the improvement in the chromatographic parameters.
