Triclosan　(TCS),　triclocarban　(TCC),　and　chlorophenols　(CPs)　are　broad-spectrum　antibacterials　widely　used　in　dermatological　and　oral　hygiene　products,　which　could　induce　severe　liver　and　intestine　injuries.　Hence,　it　is　essential　to　establish　a　rapid　and　sensitive　method　to　monitor　TCS,　TCC,　and　CPs　in　various　organisms.　In　this　work,　fluorine-functionalized　covalent　organic　framework　(COF–F)　was　prepared　by　using　4,4′,4＇＇-(1,3,5-triazine-2,4,6-triyl)tri-aniline　and　2,3,5,6-tetrafluoroterephthalaldehyde　as　two　building　units　and　employed　as　a　solid　phase　microextraction　(SPME)　probe　for　the　extraction　of　TCS,　TCC　and　CPs.　The　COF–F　possessed　excellent　hydrophobicity,　a　large　specific　surface　area　(1354.3　m2　g−1)　and　high　uniform　porosity　(3.2　nm),　which　facilitated　high　selectivity　and　adsorption　properties　towards　TCS,　TCC,　and　CPs.　Therefore,　the　as-prepared　COF–F-SPME　in　combination　with　electrospray　ionization　mass　spectrometry　has　been　developed　to　provide　fast　and　ultrasensitive　detection　of　TCS,　TCC,　and　CPs　in　biological　samples.　The　established　method　demonstrated　satisfactory　linear　ranges　(0.01–100.00　μg　L−1)　and　low　limits　of　detection　(0.003–0.040　μg　L−1)　for　TCS,　TCC　and　CPs.　The　developed　method　could　be　successfully　applied　to　detect　TCS,　TCC　and　CPs　in　the　liver　and　kidney　tissues　of　mice,　demonstrating　the　potential　for　the　detection　of　chlorinated　aromatic　pollutants　in　the　biological　samples.　©　2024　Elsevier　B.V.