Organic monolithic capillary columns coated with cellulose tris(3,5-dimethylphenyl carbamate) for enantioseparations by capillary HPLC

R. ECHEVARRÍA, S. KEUNCHKARIAN, J. VILLARROEL-ROCHA, K. SAPAG, M. RETA

MICROCHEMICAL JOURNAL

ELSEVIER SCIENCE BV

Lugar: Amsterdam; Año: 2019

0026-265X

A new chiral monolithic column for enantiomer separation in capillary LC was easily prepared by coating the chiralselector cellulose tris(3,5-dimethylphenyl carbamate) onto an organic polymer. This polymer with optimized porousproperties has been prepared in situ in pretreated fused-silica capillaries by thermal polymerization of 2-hydroxyethylmethacrylate and ethylene glycol dimethacrylate in the presence of a binary porogenic mixture (1-dodecanol andcyclohexanol). The chiral selector was synthesized from microcrystalline cellulose by a simple reaction and depositedonto the monolithic support to obtain a stable and reproducible chiral stationary phase. The column was used undernormal phase mode with different compositions of n-hexane and 2-propanol. The effect of acidic or basic additives onthe enantioresolution was studied. Several chiral acid, neutral and basic compounds (profens, 􀀀-blockers, pesticides,among others) were partially or completely resolved in short analysis times using an HPLC equipment adapted to aminiaturized scale. The new monolithic chiral column exhibited good stability, and low relative standard deviations forinter- and intra-day reproducibility. This work is the first report on enantiomeric separations by cLC using 2-hydroxyethyl methacrylate and ethylene glycol dimethacrylate (poly(HEMA-co-EDMA)) monolith coated with cellulosetris(3,5-dimethylphenyl carbamate).