| In this paper, a new kind of composites was prepared, then, particles immobilizedmonolithic column was got with the composites as capillary electrochromatographicstationary, and this monolithic column was applied to separate chiral compounds. At first,carbon microspheres were synthesized with glucose and starch by hydrothermal method andhigh-temperature carbonization method,-cyclodextrin/carbon microspheres composites weresynthesized with-cyclodextrin and carbon microspheres, epichlorhydrin as crosslinker, byinverse emulsion method. Structures and properties of these products were characterized byfourier-transform infrared spectroscopy, scanning electron microscopy, biological digitalmicroscope, N2adsorption-desorption, X-ray diffraction, X-ray photoelectron spectroscopy,thermal gravimetric analysis and so on. In addition, particles immobilized monolithic columnwas got with the composites as chiral stationary by sol-gel method, and the performance ofthe monolithic column was evaluated with thiourea as a neutral marker. This column wasused for the separation of Norfenefrine hydrochloride enantiomers. Effects of injectionconditions, buffer pH, separation voltage, temperature on resolution were investigated. Theresults showed that carbon microspheres in the size range of nano-and micron-scale wereobtained with glucose and soluble starch as materials, respectively. The carbon microspheresfrom soluble starch had the particle size of5μm or so, good monodispersity, and mesoporousstructure on the surface;-cyclodextrin/carbon microspheres composites were preparedsuccessfully, which had smooth surface, regular shape, relatively uniform particle size with10μm or so, relatively ordered structure and good thermal stability; Particles immobilizedmonolithic column was got with the composites as stationary phase, average columnefficiency was up to257,534plates/m with thiourea as a neutral marker, the column had goodreproducibility and stability; Under optimal conditions of5mmol/L NaH2PO4buffer (pH=5.5), operating voltage12kV, injection conditions:5kV×2s, column temperature22℃,detection wavelength at200nm, hydrochloric norfenefrine enantiomers got baselineseparation. |
