Synthesis of C8F13-SiO2 stationary phase for chromatographic separation of highly polar compounds

Fluorine-containing stationary phases were synthesized by a multi-modification approach and applied for separation of compounds with strong polarity (nucleosides, ginsenosides, sulfonamides, and benzoylurea insecticides (BUs)). • C8F13-SiO 2 SP was prepared by a multi-step modification strategy. • Morphology and pore structure of the C8F13-SiO 2 SP was characterized carefully. • A column efficiency of 30,220 plates/m for ginsenoside Re was obtained. • The resulting materials possess good reproducibility, repeatability and stability. Up to now, the chromatographic separation and analysis of highly polar compounds are still challenging because of low retention ability and selectivity of conventional stationary phases (SPs). Developing new SPs to achieve high-resolution and high-efficiency separation of polar compounds is of great importance for health and medicine, food safety, environmental protection, etc. . Herein, an influential multi-step modification strategy (modification with 1H,1H,2H,2H-perfluorooctyltriethoxysilane on the silica twice and end-capped with trimethylchlorosilane once) is introduced to prepare C8F13-SiO 2 SP. The physical properties of C8F13-SiO 2 SP, including morphologies, pore structures and carbon content were fully characterized by various instrumental techniques. The packed HPLC column with C8F13-SiO 2 SP exhibited high column efficiency, good peak shape (tailing factors for most analytes are between 0.9 and 1.3), and resolution for simultaneous separation of ginsenosides, sulfonamides, nucleosides, and benzoylurea insecticides (BUs); meanwhile, the retention mechanism of typical reversed-phase liquid chromatography (RPLC) mode was observed. A column efficiency of 30,220 plates/m for separation of ginsenoside Re was obtained. Furthermore, the resulting columns benefit from the advantages of supreme reproducibility, repeatability and stability. Importantly, the chromatographic properties (e.g. column efficiencies, chromatographic peak shapes, retention ability and resolution) of the C8F13-SiO 2 SP for the polar analytes were superior to those of the commercial SPs (including commercial amino-modified silica SP, diol-modified silica SP and commercial PFP-SiO 2 SP). Thus, the C8F13-SiO 2 SP is able to satisfy the strict requirements of highly polar compounds separation.