The growing detection of emerging perfluoropolyether carboxylic acids (PFECAs) in food has raised considerable concerns about their high persistence, bioaccumulation, and toxicity. In this study, a pyridine-functionalized covalent organic framework (Py-COF) was synthesized by introducing basic pyridyl groups into Br-COF via Heck cross-coupling. According to density functional theory, PFECAs were adsorbed in the pore sites of Py-COF via O···HN interaction, which was the stable and predominant adsorption configuration. After systematic characterization, Py-COF was used as the coating for solid-phase microextraction combined with high-performance liquid chromatography-tandem mass spectrometry (SPME-HPLC-MS/MS) for the efficient determination of PFECAs in food. Under the optimum conditions, the method showed satisfactory linearity (R ≥ 0.998), low limits of detection (0.001-0.004 ng g), and good relative recoveries (82.5 %-112 %). The established method was satisfactorily used for the analysis of trace PFECAs in food samples.
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