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A highly sensitive fluorescent probe (3) for selective detection of mercury based on an azobenzene derivative with 1,3,4-triazole units has been designed, synthesized, and examined for their cation recognition abilities toward various cations by UV-vis, fluorescence. The fluorescent probe (3) exhibits a highly selective response of fluorescence enhancement toward mercury in DMF aqueous media (DMF: H2O, v/v=1:1).