含杯[4]芳烃毛细管固定相的制备与色谱性能

杯芳烃是由对位取代的苯酚在邻位通过亚甲基连接起来的环状化合物,由于具有可调节大小的空腔,不仅能络合无机离子,而且还可络合有机分子,在分析分离方面有极好的应用前景［１,２］．杯芳烃已用于气相色谱［３,４］、离子选择性萃取［５,６］、液相色谱［７,８］和...

Preparation and Chromatographic Characteristics of Fused Silica Capillary Column Based on Tetra-o-benzylated Calix[4] arene

5-1',1'-Dimethylundecenyloxyphenylmethyl-11,17,23 tri 1",1" -dimethylethyl-25,26,27,28-tetrahydroxycalixarene was synthesized from 1,1-dimethylundecenyloxyphenylmethylphenol and bishydroxymethylated p tert butylphenol formaldehyde trimer (3-[3-[3-(hydroxymethyl)-5-tert butylsalicyl]-5-tert-butylsalicyl]-5-tert-butyl-2-hydroxybenzyl-alcohol) by '3+'1 fragment condensation in dioxane with TiCl₄ as condensation agent. It was subjected to benzylation with benzyl chloride in NaOHaqueous solution in the presence of Bu₄N⁺Br^- as PTCagent. The yield of the tetra-o-benzylated calix[4]arene was 78%. The tetra-o-benzylated calix[4]arene and OV-1701 were crosslinked in situ with DCUPonto the surface of fused silica capillary column. The resulted column exhibited high column efficiency(4379 plates/m, naphthalene 120 ℃) and excellent separation abilities for various positional isomers.