硅藻土载负葫芦[7]脲气相色谱固定相的制备及其性能评价

在酸性条件下,将自制的葫芦7]脲均匀地涂覆到102白色硅藻土担体上,制得葫芦7]脲气相色谱固定相.采用红外光谱、质谱、元素分析和热重分析表征了葫芦7]脲在载体表面的结构.利用相关探针测定了新固定相的麦氏常数,表征了其基本色谱性能.考察了葫芦7]脲气相色谱固定相填充柱对芳香烃、卤代烃、醇、酮、酯及硅氧烷的分离能力.结果表明,葫芦7]脲固定相热稳定性高,柱色谱性能稳定,对较广泛的化合物尤其对高沸点的酯类及硅氧烷类化合物显示出良好的色谱分离能力(7 min内分离),作为气相色谱固定相有较好的应用前景.初步讨论了葫芦7]脲固定相对上述化合物的分离机理.

Preparation and Property Evaluation of Cucurbit[ 7]uril Coated Celite as Gas Chromatography Stationary Phase

The synthesized and purified cucurbit7]uril(CB7]) was coated on a 102 white celite carrier under acidic conditions as a new gas chromatography(GC) stationary phase.The chemical structure of the CB7] was characterized by infrared spectroscopy,mass spectrometry,elemental analysis and thermogravity analysis.The McReynolds constants of the new stationary phases were determined by using different probes in order to characterize its basic chromatographic property.The separation abilities of some aromatic hydrocarbons,halohydrocarbons,alcohols,ketones,esters,siloxanes were investigated on the packed column of CB7] coated stationary phase,respectively.The results showed that new CB7] stationary phase exhibited not only a good thermal stability and also a better separation selectivity for different analytes,indicating that the CB7] stationary phase has a great potential in GC separations.Especially,some high boiling point esters and siloxanes can be successfully separated within 7 min.Additionally,the retention mechanism of the CB7] stationary phase was also discussed.