Preparation And Application Of A Chiral Monolithic Column Containing Nanometer Rare Earth Materials

The society pays more attention to the chiral drugs because of their different pharmacological activities.In order to improve the safety of chiral drugs,chiral separation becomes particularly important.Nano rare earth materials have small size effect,large specific surface area and unique physicochemical properties.Cyclodextrins and their derivatives have specific chemical structures and good chiral recognition effects.The combination of them as the chiral stationary phase for the preparation of chromatographic columns has a good practical value.In this paper,the chiral monolithic column containing nano-rare earth materials was prepared with allyl-?-cyclodextrin,modified nano-yttrium oxide and polyglycidyl methacrylate(GMA)as functional monomers,n-dodecanol as porogen and ethylene glycol dimethacrylate(EDMA)as crosslinking agent by using one-step bonding method.Meanwhile the preparation conditions were optimized.And then the monothic columns were characterized by infrared spectroscopy(IR),scanning electron microscopy(SEM)and X-ray energy spectrum(EDS)and the application of chiral separation was studied.The results showed that the self-prepared monolithic columns had network structure,good permeability and reproducibility.The optimal reaction conditions expressed that the amounts of modified nano-yttrium oxide and n-dodecanol were 2.0 mg and 240.0 mg respectively,the reaction temperature was 43 ?,and the reaction time was 14 h.The column efficiency of the monolithic column(three monolithic columns,thiourea as a marker)reached more than 50000 plates/m,and the relative standard deviation(RSD)of column efficiency was less than 0.083%.Five chiral drugs were resolved by baseline under the optimal conditions using the self-prepared monolithic column in CEC separation mode.The resolutions of D,L-histidine,D,L-lysine,pheniramine,bromopheniramine,chlorpheniramine were 1.88,1.77,1.73,2.54 and 2.29,respectively.This research not only provides a simple and efficient method for the separation and analysis of chiral drugs but also has the important practical significance.