Preparation and chromatographic separation of C18 bonded silica gel microspheres
Aims:C18-SiO2 microspheres with a median diameter of 12 μm were prepared and used in the column packing.The factors affecting the size and morphology of the microspheres and the conditions affecting the liquid phase separation were studied.The preparation conditions of C18-SiO2 microspheres and the conditions affecting the liquid phase separation were obtained.Methods:Using ethyl orthosilicate(TEOS)as the silicon source,hydrochloric acid(HCl)as the catalyst,and sodium dodecylbenzene the sulfonate(C18H29 NaO3S)as the surfactant,mesoporous SiO2 microspheres were synthesized by the polymerization-induced colloid condensation(PICA)method.The effect of preparation technology(reaction temperature,pH value and molar ratio N of formaldehyde and urea)on the size and morphology of SiO2 microspheres was studied;and the preparation conditions were optimized to prepare SiO2 microspheres with a median diameter of 12 μm.C18-SiO2 microspheres were prepared after modification by octadecyl trimethoxysilane(C21H46O3Si).The separation conditions of complex amino acids were studied by using it as the filler for high performance liquid chromatography(HPLC)columns.Results:The preparation conditions and liquid phase separation conditions of C18-SiO2 microspheres with a median diameter of 12 μm were obtained.Conclusions:C18-SiO2 microspheres with a median diameter of 12 μm were successfully prepared by the PICA method,with a narrow particle size distribution(D90/D10=1.63),a mesoporous diameter of 10 nm,and a specific surface area of 236.38 m2/g.Under suitable conditions of mobile phase and elution strength,C18-SiO2 microspheres can quickly separate the complex amino acid glutamic acid;and the separation degree is over 1.5.
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