Core-shell　structured　magnetic　covalent　organic　framework　(Fe3O4@COF)　nanocomposites　were　synthesized　via　a　facile　approach　at　room　temperature　and　explored　as　an　absorbent　for　magnetic　solid-phase　extraction　(MSPE)　of　bisphenols　(BPs)　from　human　serum　sample.　The　as-prepared　Fe3O4@COF　nanocomposites　with　core-shell　structure　possessed　high　specific　surface　area　(181.36　m(2)/g),　uniform　mesoporous　size　(similar　to　3.6　nm),　high　saturation　magnetization　(42.7　emu/g),　and　excellent　thermal　and　chemical　stability,　rendering　it　as　an　ideal　adsorbent　with　high　adsorption　efficiency　and　size　selectivity.　The　experimental　parameters　influencing　extraction　efficiency,　including　adsorbent　dosage,　extraction　time,　pH　and　ion　strength,　desorption　solvent　and　time,　were　investigated　in　detail.　Taking　these　advantages　together,　a　simple,　fast,　effective　and　sensitive　method　that　MPSE　followed　by　HPLC-MS,　was　proposed　to　detect　five　BPs,　which　exhibited　good　linearity　(r　＞　0.9982)　within　the　concentration　ranges　of　0.1-50　mu　g/L.　Moreover,　the　low　detection　limits　(1.0-78.1　ng/L),　signal-to-noise　ratio　(S/N　=　3),　the　high　enrichment　factors　(56-95　fold),　and　good　recoveries　(93.0-107.8%)　with　relative　standard　deviations　(RSDs)　less　than　3.4%　for　inter-day　and　6.9%　for　infra-day　were　achieved.　The　developed　method　was　also　successfully　applied　to　the　analysis　of　trace　BPs　in　human　serum　sample,　which　demonstrated　the　most　promising　potential　of　the　Fe3O4@COF　nanocomposites　as　good　adsorbent　in　sample　pretreatment.