限进介质烷基-二醇基硅胶(ADS)的制备  

Preparation of Restricted-Access Media——Alkyl-Diol Silica (ADS) by an Improved Method

作　　者：喻昕[1] 赵睿[1] 刘国诠[1] 

机构地区：[1]中国科学院化学研究所分子科学中心,北京100080

出　　处：《色谱》2001年第2期152-153,共2页Chinese Journal of Chromatography

基　　金：国家自然科学基金! (重点基金 2 963 5 0 10 );中国科学院重大基础研究项目

摘　　要：烷基 二醇基硅胶 (ADS)系限进介质的一种 ,可用于含生物大分子的复杂生物样品的直接进样与分析。一种新的、非常经济的方法可用于烷基 二醇基硅胶的制备。首先 ,将γ 环氧丙基氧丙基三甲氧基硅烷基键合至微孔硅胶上 (粒度 5 μm ,孔径 6nm)以制备环氧基硅胶 ,再令环氧基硅胶与硬脂酸在有机溶液中进行反应以制备酯型十八烷基反相填料。将制得的反相填料填充至色谱柱中 ,并令含有酯酶的溶液通过色谱柱。通过酶解作用可将硅胶表面的酯基除去 ,而硅胶的内孔表面仍保持疏水特性不变 ,这是由于硅胶上的小孔对酶分子具有体积排除作用。色谱评价证实了所制备填料的限进色谱行为。Alkyl diol silica (ADS) is a kind of restricted access media, which can be used for direct injection and analysis of complex biological samples containing bio macromolecules. A new economical procedure has been developed to prepare ADS packing. At first γ glycidoxypropyl group was coupled onto the surface of microporous silica gel (Develosil 60 5μ) to form epoxy silica. Prepared epoxy silica can react with stearic acid in organic solvent to prepare C 18 ester bonded reversed phase packing. The packing was packed into a column and then the solution of pancreatic lipase was pumped into the column to create enzymolysis reaction. The stearyl groups on the surface of packing can be removed by the enzymolysis to form a hydrophilic surface. At the same time, inner surface of micropore remains hydrophobic nature due to size exclusion effect of micropore to enzyme molecules. Chromatographic evaluations were carried out and the typical ADS behavior was confirmed.

关 键 词：液相色谱法 限进介质 烷基-二醇基硅胶 固定相 制备 色谱柱 

分 类 号：O657.72[理学—分析化学]