Preparation And Application Of Electrochromatographic Column Based On β-cyclodextrin Derivatives And Tungsten Oxide

In this work, the double monomer(6-O-butylene acid monoester)-β-Cyclodextrin(CPD-β-CD) was synthesized by maleic anhydride modifying β-Cyclodextrin. The nanometer metal tungsten oxide(WO3) with special morphology was prepared by sodium tungstate as tungsten source through solvent hot method, moreover, modified by hydroxyl silicon. The electrochromatography monolithic column of CPD-β-CD and β- cyclodextrin derivatives and tungsten oxide was prepared by one-step reaction, at the same time, the main influencing factors of prepared column were also investigated to obtain the optimal conditions of prepared column. The obtained products were characterized by infrared spectrum(IR), scanning electron microscope(SEM), X-ray diffraction(XRD), X-ray photoelectron spectroscopy(XPS), X-ray energy spectrum(EDS) and thermogravimetric analysis(TG). The results show that the CPD-β-CD and hydroxyl silicon modifying WO3 was successfully achieved, the optimum conditions of prepared column were listed as follows: the molar ratio of CPD-β-CD and EDMA is 0.12:0.08, the modified nanometer tungsten oxide is 0.30 g, the reaction time is 13 h and the temperature of water bath is at 40 ℃. The prepared monolithic columns have mesh structure with uniform pore size, and the content of tungsten oxide in stationary phase was about 16.6%. The monolithic columns have good reproducibility and stability, and the better ability of chiral separation. In conditions of the same electric chromatographic, the comparison and evaluation of two monolithic columns were also carried out by the separation of Thiourea and DL-Stamic acid, the average column efficiency of CPD-β-CD was up to 41,108 plates/m, and the relative standard deviation of retention time was 1.59%, the average column efficiency of β-cyclodextrin derivatives and tungsten oxide was up to 71,560 plates/m, and the relative standard deviation of retention time was 0.89%, two monolithic columns have better column efficiency and better the separation effect. Under the optimum electrochromatographic conditions of the column temperature, operating voltage and the pH value of buffer solution, the baseline separation of three chiral drugs including metoprolol, atenolol and sotalol were obtained by the prepared monolithic columns.