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A luminescence sensor based on an europium(III)-based lanthanide–organic framework, [Eu(BCB)(DMF)]·(DMF)1.5(H2O)2 (1), was synthesized via a solvothermal method using 4,4′,4′′-benzenetricarbonyltribenzoic acid (H3BCB) as a bridging ligand. Single-crystal X-ray diffraction indicates that Eu centers are eight-coordinated with a trigonal dodecahedron and a square antiprismatic configuration, and adjacent Eu atoms are bridged by BCB organic linkers to form a 3D rod-packing structure. Photoluminescence studies show that compound 1 emits bright red luminescence and behaves as a multi-responsive luminescent sensor toward 4-nitrophenol (4-NP) and I− and Fe3+ ions in water with high sensitivity, selectivity and low detection limits. Furthermore, the possible luminescence sensing mechanisms were also investigated by PXRD analysis, UV-vis spectroscopy and X-ray photoelectron spectroscopy (XPS). The recognition mechanism for 4-NP and I− ions can be attributed to the competition absorption and that for Fe3+ ions is considered to be a multi-quenching mechanism dominated by competition absorption. This study demonstrates that the lanthanide-based MOF might be a promising candidate for the detection of 4-NP and I− and Fe3+ ions in aqueous medium. [ABSTRACT FROM AUTHOR]