改性超支化聚硅碳烷物理吸附涂层毛细管柱的分离性能研究

Study on Separation Performance of Capillary Column Coated Physically with Modified Hyperbranched Polycarbosilane

利用羟丙基-β-环糊精对合成的超支化聚硅碳烷进行表面接枝改性,通过物理吸附的方法将改性后的超支化聚硅碳烷涂覆于毛细管柱内壁表面,制备出一种新型的毛细管电泳涂层柱。选用16kV的分离电压、214nm紫外检测波长、10cm位差进样7s和40mmol/L磷酸盐缓冲体系为分离条件,考察氧氟沙星和扑尔敏两种手性异构体在涂层柱上的分离性能以及涂层柱的稳定性能。在pH3.0时,对氧氟沙星的分离度为1.81,理论塔板数为4.68×104plates/m;在连续进样100次后,分离度变化不大,理论塔板数下降率在15%以内,涂层柱运行稳定,各项性能均取得满意的效果。

A series of hyperbranched polycarbosilanes were synthesized and coated on the inner surface of fused-silica capillaries by physical adsorption. The terminational groups of the hyperbranched polycarbosilanes were modified with 2-O-（2-hydroxypropyl）-β-CD. The optimal separation conditions were the running voltage of 16 kV,the UV detector wavelength of 214 nm,the sample injected time of 7 s and the phosphate buffer solution concentration of 40 mmol/L. Under the optimum conditions,the separation performance of this chiral capillary electrophoresis column for the two chiral isomers ofloxacin and chlorpheniramine was studied and the stability of column was investigated. The results showed that the column efficiency was 4.68×10^4 plates/m with a resolution of 1.81 when ofloxacin was separated at pH 3.0. After injection 100 times,there were little changes in resolution,theoretical plate number was reduced by less than 15%,and the satisfactory results of each performance column were obtained.