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A newly synthesized reagent 2-amino-5-mercapto-[ 1, 3, 4]triazole (MATZ) has been used to fabricate self-assembled monolayers (SAMs) on gold electrode for the first time. The SAMs electrode was characterized by electrochemical methods and scanning electronic microscopy (SEM),the SAMs electrode can be used to determinate dopamine (DA) and uric acid (UA) simultaneously with a detection limit of 8×10-7 mol/L for DA and 1×10-6 mol/L for UA respectively. The SAMs can also be used to detect the contents of DA and UA in synthetic urine sample with satisfactory results.