甘脲和羟基葫芦[6]脲气相色谱固定相的制备及其色谱分离性能比较研究

Preparation of Glycoluril and Perhydroxycucurbit6uril GC Stationary Phase and Comparative Studies on Their Separation Performances

甘脲是羟基葫芦[6]脲(HOCB6)的前体,本文设计了一种在酸性条件下均匀涂渍固定液的新方法,首次将甘脲和羟基葫芦[6]脲用作气相色谱固定相.将甘脲和HOCB6填装成气相色谱填充柱后,以烷烃、卤代烃、芳香烃、醇、酮、酯、酸、胺等物质为探针,用复杂样品花露水对它们的色谱分离性能进行了比较研究.结果表明,甘脲和HOCB6都是良好的气相色谱固定相,热稳定性高,柱性能稳定.两种固定相对以上溶质探针都有较好的分离能力,HOCB6固定相(PSP)与甘脲固定相(GSP)相比较,总体上具有更好的分离选择性,对难分离的芳香族位置异构体(如二甲苯、甲基苯胺)具有良好的分离能力,显示出较高的立体选择性,对花露水中的高沸点组分有较好的分离效果.上述研究也表明,由于溶质在载气中传质比葫芦脲内腔快得多,全包结尽管有利于提高分离选择性,但展宽后的柱效不理想;适当的高柱温既保留了部分包结作用,同时存在端口协同作用,能兼顾高选择性和高柱效.

Glycoluril is the precursor for perhydroxycucurbit[6]uril （HOCB6）, and in this paper a novel method of well-proportionally coating glycoluril stationary phase （GSP） and perhydroxycucurbit[6]uril stationary phase （PSP） on a packed column under acidic condition was developed for gas chromatography. Their chromatographic separation properties were compared by using alkanes, halohydrocarbons, aromatic hydrocarbons, alcohols, esters, ketones, carboxylic acids, amines and complex samples such as toilet water. The results show that glycoluril and HOCB6 are excellent packing materials with wide operational temperature, outstanding thermostability and chromatographic repeatability. Both stationary phases exhibited good separation abilities for the above solute probes. PSP has better selectivity in general than GSP and shows a good chromatographic property for some positional isomers such as those of xylene and toluidine, especially the superior selectivity to the high boiling point ingredients of the toilet water. It can also be noticed that the complete inclusion interaction maybe led to expanding the peaks with low column efficiency because of relative high mass transfer resistance. Therefore, properly high column temperature can balance between high column efficiency and high selectivity via partial inclusion complexation and portal synergetic interactions.