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Suitable chemical components in water systems for human health are a crucial prerequisite for mankind's survival. Simple and effective innovations are being developed to efficiently monitor healthy and toxic substances. Here, with a hydrothermal technique, a novel thermostable metal–organic framework (MOF) [Cd2(L)(bib)0.5(H2O)3]n·1.75n(H2O) (MOF-1, H4L = biphenyl-2,3,3′,5′-tetracarboxylic acid, bib = 1,4-bis(imidazolyl)butane) was designed and synthesized. MOF-1 shows a 4,5-connection binodal 3D fsx-type topological net with irregular cages, which the bulk materials show high phase purity, excellent thermo/aqua-stability and intense fluorescence. The luminescent MOF was studied for the highly sensitive detection of trace amounts of Fe3+ ions and nitrobenzene and shows high KSV values of 4.653 × 104 and 5.724 × 104, respectively. It was also demonstrated that MOF-1 possesses superior probing ability towards nine other nitroaromatic explosives with remarkable quenching percentages. These results offer a new possibility for the potential multiple recognition of various chemical substances in human body and water systems by utilizing novel dual-functionalized luminescent MOF sensors.