A highly sensitive fluorescent probe 1 for selective detection ofHg ion in mixed N,N-dimethylformamide aqueous media wasdesigned and prepared by incorporating the well-known Rhodamine6G fluorophore and a carbohydrazone binding unit into onemolecule. The fluorescent probe 1 can detect the parts per billionlevel of HgII in a mixed aqueous environment and displays a highlyselective response of fluorescence enhancement toward HgII.