新型离子交换硅胶键合相的制备及评价  

Preparation and Evaluation of New Ion\|Exchange Chromatographic Stationary Phase for the Use in High Performance Liquid Chromatography

作　　者：雷晓玲[1] 王俊德[1] 丛润滋[1] 

机构地区：[1]中国科学院大连化学物理研究所分析室,辽宁大连116012

出　　处：《色谱》1999年第5期431-434,共4页Chinese Journal of Chromatography

基　　金：国家自然科学基金

摘　　要：二甲基氯硅烷与硅胶表面反应，形成牢固的 Ｓｉ Ｈ 键之后，连接上活泼的中间体—— 烯丙基缩甘油醚作为柔软的分子臂，最后接上二乙基氨基，由此制得了新型的离子交换硅胶键合相。经漫反射红外光谱、元素分析和高效液相色谱法对键合相进行了鉴定和评价。结果表明：键合反应按预定路线进行，键合相具有较好的色谱性能。此种方法可有效地运用于无孔硅胶填料的制备。A new method for the bonding of diethylamine(DEA) on the surface of silica to prepare novel hydrophilic packings for HPLC has been studied. After allyl glycidyl ether being synthesized, the Si\|DEA anion\|exchange bonded phase was prepared by the reaction of the double bond in allyl group with Si\|H silica. The bonded phases obtained were characterized by elemental analysis, diffuse reflectance infrared Fourier transform(DRIFT) spectroscopy and HPLC evaluation. The methods were used for both porous silica and monodisperse non\|porous silica. The contents of carbon,hydrogen and nitrogen of porous Si\|DEA packing (MPS\|DEA) were 3.31%,0.95% and 1.34% respectively and those of monodisperse non\|porous Si\|DEA packing (NPS\|DEA) were 2.55%,0.97% and 0.96% respectively. The diethylamine absorption peak can be observed at 2 970 cm -1 from the Si\|DEA silica DRIFT spectrum. These data revealed that the diethylamine had been bonded on MPS\|DEA and NPS\|DEA packings. In HPLC tests, nucleotides and nucleosides such as cytosine, uracil, cytidine\|5′\|monophosphate, adenosine\|5′\|monophosphate, inosine\|5′\|monophosphate and guanosine\|5′\|monophosphate were satisfactorily separated on the porous anion\|exchange packing(MPS\|DEA),and a group of proteins (lysozyme, ribonuclease, ovalbumin, bovine serum albumin, insulin and γ \|globulin) were separated within 15 minutes successfuly. All test results indicated that the new method for preparing better anion\|exchange silica packings is effective for both porous silica and monodiperse non\|porous silica.

关 键 词：高效液相色谱 键合固定相 离子交换色谱 硅胶 

分 类 号：O657.720.3[理学—分析化学]