关键词: 薯蓣皂苷, 键合硅胶固定相, 结构表征, 色谱性能评价

Abstract: A kind of new stationary phase was prepared by one-pot reaction method which was dioscin bonded stationary phase(D),and two derivative stationary phases were prepared using phenyl isocyanate and 3,5-dimethyl phenyl isocyanate based on D,namely the phenyl isocyanate-dioscin bonded silica stationary phase(Phe-D) and the 3,5-dimethyl phenyl isocyanate-dioscin bonded silica stationary phase(DMP-D).Elemental analysis,scanning Electron Microscope (SEM),thermogravimetric Analysis and infrared spectroscopy were done to investigate the structural characteristics of dioscin and its derivative stationary phases.The results verified that the dioscin ligand has successfully bonded to the silica base material and the derivatization reactions had taken place properly.Benzene homologues and PAHs were used as solute probes to evaluate the chromatographic performance of three new stationary phases.The results showed that three new stationary phases had typical reversed-phase chromatographic performance,which were similar to the ODS,and the separation principle was related to hydrophobic effect.According to the results of elemental analysis,the surface bonding amount of D was 152.61 μmol/g,the phe-D was 140.68 μmol/g,and the DMP-D was 151.97 μmol/g.The bonding and derivatization methods were considered simple to apply,and provided the methodological reference for preparing stationary phases of dioscin and its two derivative functionalized silica gel on a large scale.

Key words: dioscin, bonded silica stationary phase, structural characteristics, chromatographic evaluation