Preparation and evaluation of 1,6-hexanediol ethoxylate diacrylate-based alkyl methacrylate monolithic capillary column for separating small molecules

Due to the high porosity, good thermal stability, and good physical stability at high pressure, polymer monoliths have been successfully utilized as the stationary phases for capillary liquid chromatography (LC) analysis. In this study, we introduced 1,6-hexanediol ethoxylate diacrylate (HEDA) as a cross-linker to prepare alkyl methacrylate monoliths for efficient separation of polar small molecules. HEDA provided additional dipole–dipole interactions between the monolithic stationary phases and polar analytes. For comparison, ethylene dimethacrylate and 1,6-hexanediol dimethacrylate were also utilized as cross-linkers to prepare alkyl methacrylate monoliths. A series of alkyl methacrylate polymeric monoliths were synthesized in fused-silica capillaries using the three different cross-linkers. The porosity, permeability and column efficiency of the synthesized alkyl methacrylate monoliths were characterized. A mixture of phenol derivatives was employed to evaluate the applicability of the prepared monolithic columns for separating small molecules using capillary LC. The HEDA-based alkyl methacrylate monoliths offered the most efficient chromatographic separation for phenol derivatives. Moreover, the capability of applying the novel HEDA-based alkyl methacrylate monolithic columns for potential environmental analysis was demonstrated by separating eight phenylurea herbicides.