Phthalate　esters　(PAEs)　are　a　typical　group　of　endocrine-disrupting　chemicals　(EDCs)　and　widely　found　in　the　environment,　which　have　attracted　great　concern　due　to　the　potential　risks　to　environment　and　human　health.　It　is　urgent　to　develop　a　high-efficiency　and　high-sensitivity　analytical　approach　for　enrichment　and　determination　of　ultra-trace　PAEs.　Herein,　magnetic　covalent　organic　frameworks　(Fe3O4@TAPB-DVA)　were　fabricated　via　a　one-pot　approach　at　room　temperature　and　explored　as　a　magnetic　enrichment　probe　with　high　surface　area　(275.50　m2/g),　good　crystallinity,　regular　pore　size　distribution　(3.1　nm)　and　outstanding　saturation　magnetization　(26.5　emu/g).　Accordingly,　a　simple　and　sensitive　method　based　on　magnetic　solid-phase　extraction　(MSPE)　combined　with　HPLC-MS/MS　was　established　to　detect　ultra-trace　PAEs　from　fine　particulate　matter　(PM2.5)　samples.　The　proposed　method　showed　wide　linear　ranges　(1-400　ng/L),　good　linearity　(r　＞　0.9978)　and　high　enrichment　factors　(EFs,　6.99-95.01　folds)　with　low　detection　limits　(LODs)　ranged　from　0.01　to　0.5　ng/L　(S/N　≥　3).　On　this　basis,　the　proposed　method　was　substantially　employed　for　sensitive　detection　of　low-　abundance　PAEs　from　PM2.5　samples,　suggesting　the　promising　application　of　the　Fe3O4@TAPB-DVA　in　sample　enrichment.　©　2022　Elsevier　B.V.