原位合成一体化多孔聚合物毛细管色谱柱的研制及其应用

In-Situ Preparation and Applications of Integrated Capillary Chromatographic Column

采用全新的两步原位合成法,制备高效一体化U型多孔层聚合物颗粒PLOTPora U毛细管色谱柱。先将带有双活性反应基团的γ 三甲氧基硅丙基异丁烯酸酯中的CH3—O—Si—基团与石英毛细管内壁表面的Si—OH反应,在石英毛细管内壁键合上带有活性基团的中间有机层,再原位合成多孔聚合物。该色谱柱具有良好的惰性和较强的分离能力。与一般的商品化PLOT U色谱柱相比,热稳定性和机械强度有明显的改善和提高,色谱柱最高使用温度提高了20℃,达到210℃,对强极性物质、强活性化合物、永久性气体以及低碳化合物有较好的分离。

A new method to prepare polymeric PLOT columns by using a twostep insitu polymerization technology is described. The integrated method involves a straight forward insitu polymerization of monomers. By using the γ(trimethoxysilyl)propyl methacrylate (TMSPM) as a bridge the porous polymer is bonded to the column, and itself is crosslinked so that the new column eliminates the defects in traditional polymer PLOT columns where particles are released and swept through the column, which may cause blockage or spiking detection signals. This new type of PLOT column (PLOT Pora U) is coated with a divinylbenzeneethylene glycol dimethacrylate copolymer. The retention characteristics of this porous polymer were evaluated and found to be comparable with those of HP PLOTU. The inertness of the porous polymer allows a symmetrical elution of a range of apolar and polar compounds, especially the most active and polar compounds such as H2O, H2S. It has been stabilized to withstand temperatures up to 210 ℃. With this new type of capillary columns, significantly better mechanical stability, thermal stability, reproducibility, strong separation power and good inertness are obtained in combination with short analysis time.