Trimethyl-β-cyclodextrin-encapsulated monolithic capillary columns: Preparation, characterization and chiral nano-LC application

Abstract

Trimethylated-β-cyclodextrin (TM-β-CD) was encapsulated within several polymer monolithic capillary columns for reversed-phase chiral nano-liquid chromatography (nano-LC). The monolithic phases were prepared using the one-pot in situ copolymerization of ethylene glycol dimethacrylate (EDMA), glycidyl methacrylate (GMA) monomers and 1-propanol, 1,4-butanediol as progenic solvents in presence of TM-β-CD solution within fused silica capillaries (150µm I.D.). The obtained chiral monolithic stationery phases were characterized by scanning electron microscopy (SEM), N₂ adsorption/desorption isotherms, wide angle x-ray diffraction (WAXRD), thermogravimetric analysis (TGA) and differential thermal analysis (DTA). The materials characterization demonstrated that monolithic phases with higher concentration of TM-β-CD have relatively larger surface area, smaller pore size and larger total pore volume compared to those with lower concentration TM-β-CD. The prepared columns were tested for their enantioseparation efficiency of a range of racemic pharmaceuticals. The screening results demonstrated the potential of functionalizing polymer monolithic stationary phases with TM-β-CD using the in situ encapsulation approach.

Keywords: CLC; Chiral resolution; Cyclodextrin; Enantioseparation; Monolith; Nano-LC.