咪唑键合硅胶固定相微柱液相色谱分离酚类和胺类化合物

Separation of hydroxybenzenes and amines by microcolumn liquid chromatography with imidazolium functionalized silica stationary phase

由于微柱液相色谱(μ-LC)具有高检测灵敏度、低溶剂消耗、可以与质谱等多种检测器联用的优点,近年来受到广泛关注。将咪唑键合硅胶固定相填充到毛细管中,在自制的微柱液相色谱系统下利用此键合相具有的弱疏水作用,采用不同的流动相对酚类和胺类化合物进行了分离。结果表明,流动相中只需添加少量的有机溶剂就可以实现对一些有机化合物的分离,甚至可以只用纯水作流动相就能分离一些弱疏水性化合物,如酚类。微柱液相色谱的流动相用量少,避免或大大减少了对环境的污染。自制微柱液相色谱系统为下一步微柱液相色谱-质谱联用奠定了一定的基础。

Microcolumn liquid chromatography （μ-LC） has been received extensive attention in recent years because of several key advantages： the ability to work at very low flow rates, which leads to a significantly lower solvent consumption; the possibility to inject very low sample size; the enhanced detection performance with the use of concentration sensitive detection devices as a result of the strongly reduced chromatographic dilution during the separation process （mass sensitivity）, the availability to hyphenate to mass spectrometry （MS）, et al. A microcolumn liquid chromatographic system was set up. The chromatographic separations of some ordinary hydroxybenzenes and amines were performed with different mobile phases using the weak hydrophobic interaction of imidazolium functionalized silica stationary phase on a microcolumn （150 mm×0.25 mm）. The results showed that the organic compounds could be well separated when a few organic solvents were added in the mobile phase, and some weak hydrophobic organic compounds such as phenols could be separated using only water as the mobile phase. For the advantages of microcolumn liquid chromatography, this experiment avoided or significantly reduced the use of organic solvents which contaminated the environment. This system provided a base for microcolumn liquid chromatography-mass spectrometry （μ-LC-MS）.