As　a　class　of　persistent　organic　pollutants　(POPs),　polychlorinated　biphenyls　(PCBs)　are　highly　hazardous　to　the　ecosystem,　and　their　effective　and　facile　detection　is　of　high　importance.　Herein,　we　present　two　nanoporous　metal-organic　frameworks　(MOFs),　(Me2NH2)[In(CPTTA)]·(DMF)1.5(H2O)3.5　(BUT-174)　and　(Et2NH2)[In(CPTTA)]·(DEF)(H2O)3　(BUT-175),　constructed　by　In3+　ions　and　the　aromatic-rich　tetratopic　carboxylate　ligands,　5′-(4-carboxylatophenyl)-[1,1′:3′,1″-terphenyl]-3,4′′,5-tricarboxylate　(CPTTA4-),　which　exhibit　highly　efficient　turn-down　fluorescence　response　toward　12　PCBs,　especially　for　three　highly　toxic　non-ortho-substituted　PCBs　(PCB-77,　-126,　and　-169)　with　the　so-called　＇coplanar＇molecular　configuration　in　various　solvents　with　the　limits　of　detection　(LODs)　down　to　the　ppb　level　owing　to　the　inner　filter　effect　between　MOFs　and　PCBs.　In　addition,　the　MOFs　show　high　sensing　selectivity　toward　PCBs　over　many　relevant　interferents,　including　hexabromocyclododecane　(HBCD),　decabromodiphenyl　oxide　(DBDPO),　perfluorobutanoic　acid　(PFBA),　and　perfluorooctanoic　acid　(PFOA),　as　well　as　good　recyclability　and　stability.　It　is　demonstrated　by　this　work　that　structurally　well-defined　MOFs　could　be　promising　sensory　materials　for　the　detection　of　highly　toxic　PCBs　in　a　facile　way.　©　2022　American　Chemical　Society.