限进介质烷基-二醇基硅胶(ADS)的制备

 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。

Preparation of Restricted-Access Media

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 gamma-glycidoxypropyl group was coupled onto the surface of microporous silica gel (Develosil 60-5 mu) to form epoxy-silica. Prepared epoxy-silica can react with stearic acid in organic solvent to prepare C18 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 enzymoloysis 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.