A　hollow　microtubular　covalent　organic　framework　(denoted　as　TatDha-COF)　was　synthesized　by　solvothermal　method　for　the　enrichment　and　determination　of　quinones.　The　TatDha-COF　showed　large　specific　surface　area　(2057　m2　g−1),　good　crystal　structure,　ordered　pore　size　distribution　(2.3　nm),　stable　chemical　properties　and　good　reusability.　Accordingly,　a　simple　and　efficient　method　based　on　dispersive　solid-phase　extraction　(d-SPE)　and　atmospheric　pressure　gas　chromatography　tandem　mass　spectrometry　(APGC-MS/MS)　was　developed　for　the　determination　of　quinones　in　complex　samples.　The　established　method　demonstrated　a　wide　liner　range,　good　linearity　(r>0.9990),　high　enrichment　factors　(EFs,　24–69-folds)　and　low　detection　limits　(LODs,　0.200–30.0　pg　L−1,　S/N≥3).　On　this　basis,　the　suggested　method　was　successfully　applied　to　sensitively　detect　the　eight　ultratrace　quinones　in　mice　plasma.　Overall,　the　established　method　has　provided　a　powerful　tool　for　the　enrichment　and　detection　of　ultratrace　quinones　in　complex　samples,　presenting　the　promising　application　of　TatDha-COF　in　sample　pretreatment.　Graphical　abstract:　[Figure　not　available:　see　fulltext.]　©　2023,　The　Author(s),　under　exclusive　licence　to　Springer-Verlag　GmbH　Austria,　part　of　Springer　Nature.