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Preparation And Application Of Capillary Electrochromatography Monolithic Column Of Acrylamide-β-cyclodcxtrin

Posted on:2013-04-02Degree:MasterType:Thesis
Country:ChinaCandidate:H M DingFull Text:PDF
GTID:2231330374496537Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
Acrylamide-β-cyclodextrin (AM-β-CD) and glycidyl methacrylate acting (GMA) asfunctional monomers, and ethylene glycol dimethacrylate (EDMA) acting as cross-linkingagent, and azodiisobutyronitrile (AIBN) acting as initiator agent, the chiral capillary monoli--thic column of acrylamide-β-cyclodextrin was prepared by in-situ polymerization method.This one-step method was easy to operate, and it also increased the dosage of β-cyclodextrinsin stationary phase. Consequently, the chiral separating ability of the monolithic column waseffectively enhanced. The influences of monomer and crosslinker content, porogen compo-sition, temperature, reaction time on the permeability were investigated in the monolithiccolumn preparing, and the optimal preparation conditions have been obtained through theexperiment. The structure and morphology of the monolithic column were characterized byinfra-red (IR) and scanning electron microscopy (SEM). Meanwhile, the stability andreproducibility of the phenylanine as investigating object were also observed. The resultsshowed that relative standard deviation (RSD) of the phenylanine were4.89%and1.5%respectively, the retention value had the good reproducibility. The monolithic column can becontinued for12hours and intermittently used for3months, the capillary monolithic columnof acrylamide-β--cyclodextrin had the good separation ability and the column efficiency.In capillary electrochromatography (CEC) mode, the enantiomers of etilefrine hydro--chloride, rosiglitazone and fenfluramine hydrochloride were separated by the chiral capillarymonolithic column of acrylamide-β-cyclodextrin. Herein, the baseline resolutions of theenantiomers were completely reached. Besides, in order to optimize the separation conditionsin capillary electrochromatography, column temperature, the buffer pH value, voltage,organic additive and other factors were also studied. This paper provides the experimentalmethods and theoretical reference for the separation of chiral substances in the capillaryelectrochromatography mode.
Keywords/Search Tags:Acrylamide-β-cyclodextrin, Monolithic column, Capillary electrochromatogra-phy, Chiral drugs
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