Preparation And Application Of Acryloyl-β-Cyclodextrin Chiral Monolithic Column For Capillary Electrochromatography

Capillary electrochromatography is a new separation technique that brings together theadvantage of both capillary electrophoresis and micro-high performance liquid chromato-graphy. Especially, organic polymer monolithic materials have good structural stability,strong permeability, fast mass transfer rate, high enrichment, stable property and easymodification, which can be widely used as the stationary phase for CEC. The monolithiccolumn which was prepared with cyclodextrins derivatives stationary phase has become thedevelopment trend in the field of capillary electrochromatography research.In this paper, acryloyl-β-cyclodextrins was synthesized by acylation reaction betweenpropylene carbonyl chlorides with β-cyclodextrins on the conditions of tempreture0℃,nitrogen and triethylamine basic environmental, N, N-dimethylformamide (DMF) was used assolvent, ethylene eimethacrylate (EDMA) as crosslinker, cyclohexanol and dodecanol asporogen, acryloyl-β-cyclodextrin as the monomers, azodiisobutyronitrile, azobisisobut-yronitrile (AIBN) as initiator, and2-acrylamido-2-methylpropane sulfonicacid (AMPS) asthe produce agent of electricity seepage in situ polymerization, the capillary chiral monolithiccolumn was prepared. Many factors were studied to optimize the preparation conditions ofcapillary chiral monolithic column, such as the column temperature, the reaction time, theconcentration of β-cyclodextrin and its derivatives. The prepared column has goodpermeability and higher theoretical plate number. The microstructure and morphology ofmonolithic column were characterized by FT-IR and SEM. The concentratin, pH value,column temperature and other factors were also studied. The monolithic column of themodified cyclodextrin derivatives as a functional monomer had good retention properties tothe chiral compounds with hydrophobic, containing amino and benzene ring. Besides, thestability and the reproducibility of the monolithic column were also studied, and theexperimental data revealed that the standard deviation of the separation factor (α) of Alanineis1.36%and1.12%. The monolithic column can be intermittently used for2months, and thecolumn efficiency and separation silectivity are still very good. Proglumide Etilefrine,Hydrochloride and Mexiletine Hydrochloride were successfully separated with shortretention time and high separation efficiency.by the chiral monolihcolumn in the optimizedconditions.