Covalent　organic　frameworks　(COFs)　showed　great　promise　in　effective　adsorption　of　target　molecule　via　size　selectivity.　Although　various　magnetic　2D　COFs　composites　have　been　studied　and　exhibited　the　intensive　applications,　the　incorporation　of　3D　COFs　and　magnetic　nanoparticles　to　form　a　new　class　of　magnetic　adsorbents　with　enhanced　function　still　has　no　reports.　Herein,　a　novel　Fe3O4@3D　COF　with　heteroporous　structure　matching　to　the　sizes　of　bisphenol　A　(BPA)　was　firstly　synthesized　for　better　adsorption　of　BPA　than　common　magnetic　2D-COFs.　Three　Fe3O4@3D　COFs　nanospheres　were　synthesized　under　the　solvothermal　conditions　in　autoclave,　and　the　optimum　Fe3O4@3D-COF　denoted　as　Fe3O4@COF-TpTAM　(Tp,　1,3,5-triformylphloroglucinol;　TAM,　tetra(p-aminophenyl)-methane)　was　selected　and　employed.　Detailed　characteristics　of　Fe3O4@COF-TpTAM　were　evaluated　via　various　techniques　including　TEM,　FTIR,　TGA,　XRD　and　BET.　Excellent　chemical　and　thermal　stability,　high　surface　area　(294.6　m(2)　g(-1))　and　pore　volume　(0.2　m(3)　g(-1))　with　multiple　pore　sizes　comparable　with　the　simulated　three-dimensional　sizes　of　BPA　were　exhibited.　A　high　adsorption　capacity　of　BPA　up　to　209.9　mg/g　that　was　better　than　common　2D-COFs　was　achieved,　and　the　sensitive　MSPE-LC-MS　method　with　wide　linear　range　(10-5000　pg/mL),　low　detection　limit　(4　pg/mL,　S/N　=　3)　was　built.　Satisfactory　recoveries　of　BPA　as　93.8　+/-　1.4%-101.4　+/-　5.1%　(n　=　3)　and　100.4　+/-　1.9%　similar　to　107.3　+/-　1.2%　(n　=　3)　were　obtained　in　milk　and　river　water　samples,　respectively.　This　work　demonstrates　the　promising　application　of　Fe3O4@3D　COF　as　efficient　adsorbents　of　trace　BPA,　and　opens　up　a　new　access　for　the　efficient　MSPE　in　sample　pretreatment　for　food　or　environmental　safety　analysis.