摘要
本研究采用"一锅法",制备薯蓣皂苷键合硅胶固定相(D),苯基异氰酸酯、3,5-二甲基苯基异氰酸酯分别对其衍生,制备苯基异氰酸酯-薯蓣皂苷键合硅胶固定相(Phe-D)和3,5-二甲基苯基异氰酸酯-薯蓣皂苷键合硅胶固定相(DMP-D)。采用元素分析、电镜、热重分析和红外光谱等手段对三种固定相进行结构表征。以苯同系物、多环芳烃等溶质为探针,初步考察了三种新型固定相的色谱性能。结果表明薯蓣皂苷配体已键合至硅胶基质上,根据元素分析结果,按照含碳量计算得到D的表面键合量为152.61μmol/g,Phe-D的表面键合量为140.68μmol/g,DMP-D的表面键合量为151.97μmol/g;薯蓣皂苷及其衍生物固定相的反相色谱性能类似于十八烷基键合硅胶固定相(ODS),分离原理与疏水性作用有关。该衍生化反应简便易行,有望为薯蓣皂苷及其衍生物功能化色谱固定相的大规模制备提供方法学参考。
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.
引文
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