Triclosan　(TCS)　and　triclocarban　(TCC)　are　widely　used　as　bactericides　in　personal-care　products.　They　are　frequently　found　in　environmental　water　and　have　the　potential　to　cause　a　number　of　environmental　and　human　health　problems.　In　this　study,　we　investigated　adsorption　and　magnetic　extraction　for　efficient　removal　of　TCS　and　TCC　from　water　and　serum　samples　by　core-shell　structured　magnetic　covalent　organic　framework　nanocomposites　(Fe3O4@COFs).　The　as-prepared　Fe3O4@COFs　was　fabricated　on　the　Fe3O4　nanoparticles　in　situ　growth　strategy　at　room　temperature　via　condensation　reaction　of　1,3,5-tris(4-aminophenyl)　benzene　(TAPB)　and　terephthaldicarbox-aldehyde　(TPA)　in　the　presence　of　dimethyl　sulfoxide　(DMSO).　The　whole　process　of　adsorption　was　monitored　by　ultrahigh　performance　liquid　chromatography-tandem　mass　spectrometry　(UHPLC-MS/MS)　analysis　with　high　sensitivity.　The　adsorption　behaviors　showed　high　adsorption　capacity　and　fast　adsorption.　Furthermore,　the　adsorption　performance　through　Langmuir　and　Freundlich　isotherms　showed　multilayer　adsorption　through　the　interactions　of　space　embedding　effect,　van　der　Waals　forces,　and　benzene　ring　π-πstacking　at　a　low　concentration　range　and　monolayer　adsorption　through　strong　π-πstacking　at　a　high　concentration　range　between　the　interface　of　TCS　or　TCC　and　Fe3O4@COFs　at　a　high　concentration　range.　Results　indicated　that　the　adsorption　of　TCS　and　TCC　onto　Fe3O4@COFs　can　be　better　represented　by　the　pseudo-second-order　model.　Good　removal　efficiencies　(82.3∼95.4%)　and　recoveries　(92.9∼109.5%)　of　TCS　and　TCC　in　fetal　bovine　serum　(FBS)　and　reusability　at　least　10　times　were　achieved.　The　Fe3O4@COFs　exhibited　high　stability　and　excellent　performance　for　the　removal　of　TCS　and　TCC　from　water　and　biological　samples.　The　results　presented　here　thus　reveal　the　exceptional　potential　of　COFs　for　high-efficient　environmental　remediation.　©　2019　American　Chemical　Society.