Bile　acids,　a　representative　diagnostic　indicator　of　liver　function,　are　used　to　visualize　the　extent　of　liver　injury.　Numerous　studies　have　shown　that　triclosan　(TCS)　exposure　leads　to　abnormal　bile　acid　metabolism.　As　a　result,　there　is　a　requirement　to　develop　a　fast　and　smart　means　to　quantitatively　monitor　abnormal　bile　acids　from　exposure　to　triclosan　in　bio-sample.　In　this　work,　solid-phase　microextraction　(SPME)　probes　of　sea　urchin-like　covalent　organic　frameworks　(COF)　were　in　situ　synthesized　on　steel　needles　by　using　1,3,5-tris(4-aminophenyl)benzene　(TAPB)　and　2,5-dimethoxybenzene-1,4-dicarboxaldehyde　(DMTP)　as　two　organic　units　and　employed　for　extraction　of　bile　acids.　This　TAPB-DMTP-COF-SPME　possessed　an　excellent　specified　surface　area　(3351　m2　g−1)　and　a　high　regular　porosity　(∼3.6　nm),　which　was　an　ideal　adsorbent　to　concentrate　bile　acids　efficiently.　The　created　probe,　together　with　electrospray　ionization　mass　spectrometry　(ESI/MS),　proved　to　be　a　fast　and　specific　assay　for　the　detection　of　bile　acids　in　bio-samples.　The　proposed　method　had　a　low　limitation　of　detection　(0.03　μg　L−1),　good　linearity　(R2　≥　0.9931),　wide　linear　range　(0.10–1000.00　μg　L−1)　and　excellent　enrichment　factor　(63.60–252.00).　Based　on　these　excellent　properties,　it　was　successful　application　for　the　analyzing　of　bile　acids　in　mice　liver　and　feces,　demonstrating　the　great　potential　of　TAPB-DMTP-COF-SPME-ESI/MS　in　bile　acids　detection　and　liver　injury　diagnosis.　©　2024　Elsevier　B.V.