Preparation And Application Of α-alkenyl-β-cyclodextrin-based Chiral Capillary Electrochromatography Monolithic Column

Capillary electrochromatography (CEC) is a novel separation technique that bringstogether the advantage of both capillary electrophoresis and high-performance liquidchromatography. The separation principle of capillary electrochromatography lies in differentinteraction between samples and stationary phase with special structure. It is important todevelop new chiral separation material for widening application of capillaryelectrochromatography in chiral separation by combining β-cyclodextrin with specialmolecular structure and monolithic material. This method has the rapid analysis, highsensitivity, high resolution, and analysis of samples with less low cost, In recent years, it is ofconcern a novel column and very promising separation method.In this paper,4-(3-acryloxy-2-hydroxy)propyloxy-β-cyclodextrin (PCD) was synthesizedfrom1-alklyloxy-2,3-epoxy propane(also named as allylglycidyl ether, AGE) and β–cyclodextrin in Alkaline conditions.The PCD and GMA act as a functional monomer, a newtype β-cyclodextrin polymer chiral capillary CEC monolithic column was prepared by thein-situ polymerization in the capillary tube. The morphology and structure of monolithiccolumn were characterized by the scanning electron microscopy (SEM)、infrared (IR) andnuclear magnetic resonance (NMR). In the optimal CEC conditions, the impact of separationconditions of the chromatographic were examined, such as column temperature, buffer type,pH value, concentration and organic phase content and so on.Through experiments that the α-alkenyl-β-cyclodextrin was prepared by thecopolymerization of α-alkenyl-β-cyclodextrin with GMA. This method increased the dosageof cyclodextrins in stationary phase, the hydrophobic region was enlarged and thehydrophobicity and the chiral resolution of the monolithic column were improved by usingthe α-alkenyl-β-cyclodextrin as the chiral stationary phase and consequently. It was propitiousto enhance synergy effects of organic molecules and chiral selectivity of monolithic column.This method can make the cyclodextrin derivatives evenly fix on the capillary monolithiccolumn which hold the macromolecule effect and high mechanical strength. The monolithiccolumn can be intermittently used for5months, and the column efficiency and separationsilectivity are still very good. In the selected chromatographic conditions, Theguaifenesin、 benserazide hydrochloride、racecadotril were separated by the new type electrochromatography monolithic column, The method is easy operation, quick and suitable,has good separation effect.