A monolithic azacalix[4]pyridine column for high-resolution and high-efficiency pressurized capillary electrochromatographic separation

Herein, a highly stable (NAllyl) 4 -bridged alyzacalix[4]pyridine monolithic column (nAC4P@capillary) was fabricated by copolymerizing nAC4P with GMA and EDMA into a stationary phase through a simple olefin addition reaction. The physicochemical properties of the prepared materials were characterized by scanning electron microscopy (SEM), thermogravimetric analysis (TGA), energy dispersive X-ray (EDS), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FT-IR) and elemental analysis (EA). A wide range of analytes with various properties was well separated and demonstrated the synergistic effect of the various interaction sites. The maximum column efficiencies (N max ) for all the analytes reached 62,368 plates/m, and the relative standard deviations (RSDs) of the daily retention times of alkylbenzenes, measured over six months were all lower than 5.63%. Non-covalent interaction analysis reveals that nAC4P@capillary can effectively combine the advantages of electronic configurations, π-π interactions, CH-π interactions, O–H…N hydrogen bonds and lone pair-π interactions, providing excellent prospects for high-performance chromatographic separation .