Preparation And Application Of2,6-di-o-carboxymethyl-β-cyclodextrin/SiO₂/TiO₂Organic-inorganic Hybrid Capillary Electrochromatography Open Tubular Column

Capillary electrochromatography （CEC） is the rapid development of new micro-columnseparation method, in recent years, which combines characteristics of the high selectivity ofHPLC and the efficiency CE, will be one of the most development potential separationtechnology. The research of capillary electrochromatography column technology andstationary phase has been begun to study, so the research for reliably prepared column methodand suitable chromatography stationary phase are an important topic of the development ofthe electric chromatography.Herein, a novel organic-inorganic hybrid capillary electrochromatography open tubularcolumn, which titanate （TBOT） and silicate （TEOS） as inorganic precursors andCarboxymethyl-β-cyclodextrin （CM-β-CD） as organic groups, was prepared by sol-gelmethod. The structure and morphology of the hybrid open tubular column were characterizedin details by scanning electron microscopy （SEM） and infrared spectroscopy （IR）. Duringpreparation of hybrid open tubular column, the effect of the molar ratio of organic andinorganic components, the volume ratio of TBOT and TEOS, the amount of ethanol solvent,pH value, the amount of water, the temperature of the hydrolysis, the temperature and time ofsolvothermal have been studied. At the same time, the stability and the reproducibility of theopen column were evaluated with thiourea as the marker of electro-osmotic flow, theseparation efficiency of108043plates/m was obtained, and the experimental data revealedthat the standard deviation of the rentention time of the thiourea is up to3.1%, the separationeffect of the hybrid open tubular column was still very good after being runned continuously18d in the buffer solution and used intermittently4months, its reproducibility and stabilitywas also good.In CEC mode, the separation conditions of the chromatographic were examined, such ascolumn temperature, pH in buffer, operating voltage, concentrations of buffer solution andorganic modifier content and so on. The prepared hybrid open tubular column was evaluatedby separating amino acid enantiomers and amino acid mixture. Chlorphenesin, BenserazideHydrochloride, Ketoprofen were successfully separated by the prepared open tubular column.The experimental results show that: the stationary phases of CM-β-cyclodextrin/SiO₂/TiO₂ organic-inorganic hybrid capillary electrochromatography exhibit good mechanical strengthand comparatively favorable chemical stability in CEC.