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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5μm,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。
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Abstract：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
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 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． |
| 基金项目：国家自然科学基金(重点基金29635010)以及中国科学院重大基础研究项目 作者简介：喻昕(1969-)，男，博士。 作者单位：喻昕（中国科学院化学研究所分子科学中心，北京 100080） 赵睿，（中国科学院化学研究所分子科学中心，北京 100080） 刘国诠（中国科学院化学研究所分子科学中心，北京 100080） 参考文献： ［1］Anderson D J. Anal Chem, 1993,
65(12):434R-443R |
原载于《色谱》2001 Vol.19 No.2
P.152-153
http://periodical.wanfangdata.com.cn/periodical/sp/sp2001/0101/0101ml.htm