浸渍法制备C_(18)反相高效液相色谱固定相  

Preparation of C_(18) bonded reversed-phase chromatographic stationary phase using impregnation method

作　　者：李瑞沙 LI Rui-sha(School Pharmaceutical Science and Technology,Tianjin University,Tianjin 30007)

机构地区：[1]天津大学药物科学与技术学院,天津300072

出　　处：《分析试验室》2018年第9期1075-1079,共5页Chinese Journal of Analysis Laboratory

摘　　要：提出了一种浸渍法制备C18高效液相色谱固定相的方法。以十八烷二甲基氯硅烷(ODC)为键合试剂、六甲基二硅氮烷(HMDS)为封尾试剂,通过浸渍法制备得到C18高效液相色谱固定相。采用红外光谱(FTIR)、元素分析(EA)和氮气吸附与解吸附(BET)对该合成材料进行了表征,并通过SRM870评价体系对其疏水选择性、金属离子以及硅羟基活性进行评价。与商品柱Kromasil C18相比,浸渍法制备的C18固定相具有较少的金属离子活性及较低的硅羟基残余量。通过重复性考察,说明浸渍法制备的C18柱键合层稳定,对溶质的保留重现性良好。A practical and simple impregnation method for preparing C18 bonded chromatographic stationary phase was developed in this paper. Firstly, ODC was adsorbed on the surface of the silica, then reacted with the silanol groups by heating, and then HMDS as the endcapping reagent was used to endeap, finally the Cl8 stationary phase was obtained directly. The material was characterized by FTIR, EA and the BET data. And the chromatographic behavior of the C18 stationary phase was investigated by SRM870 mixtures test. The results were compared with the commercial product Kromasil C18, which revealed less metal ions and residual silanol groups. Besides, the behavior of reproducibility was confirmed by separating SRM870 mixtures test and EA. Impregnation method provides a new way for the preparation of chromatographic stationary.

关 键 词：高效液相色谱法 反相色谱固定相 浸渍法 SRM870 重复性 

分 类 号：O657.7[理学—分析化学]