Preparation And Application Of Capillary Electrochromatographic Monolithic Column Of β-cyclodextrin Magnetic Composite Microspheres

Cyclodextrin have the abilities of inclusion sustained release, catalysis and recognition.Magnetic microspheres belong to composite microsphere with magnetism and specialstructure. So it is anticipated for β-cyclodextrin and magnetic microsphere to have a goodapplication prospect as capillary electrochromatographic solid phase to separate magneticsubstances, chiral substances, or the mixture of both.In this paper, a kind of Fe3O4magnetic microsphere was firstly prepared bysolvothermal method using six hydrated ferric chloride as an iron source and ethanediol as areducing agent and a solvent. Then under alkaline condition it was modified using TEOS asa silica source to improve its stability and disperstiveness. Furthermore, the β-cyclodextrinmagnetic composite microsphere (β-CD/Fe3O4composite microsphere) was synthesized byinverse emulsion polymerization using β-cyclodextrin and the modified magneticmicrosphere as raw materials, epichloroydrin as crosslinking agent, and kerosine as oilphase. Finally capillary electrochromatographic monolithic column was prepared withβ-CD/Fe3O4composite microspheres as solid phase. In addition, the microspheres and themonolithic column were characterized by SEM, EDS, IR, XRD and so on. With thiourea asthe marker, the performance of the monolithic column was evaluated. Then the monolithiccolumn was applied to separate D,L-phenylalanine and Guaifenesin, the chromatographicseparation conditions were investigated as column temperature, buffer pH, and operatingvoltage.The results showed that the β-CD/Fe3O4composite microsphere was successfullysynthesized. With smooth surface, uniform particle size, and more rounded shape, itsaverage particle size was of about7μm. It retained magnet, and the basic structure ofβ-cyclodextrin. D,L-phenylalanine and Guaifenesin were successfully separated by theprepared capillary electrochromatographic monolithic column of β-CD/Fe3O4compositemicrospheres. The monolithic column still had very good selectivity and separation ability.And the monolithic column still had very good stability and repeatability.