In the work presented here, Nickel electrode by NiOOH was prepared by galvanostatic deposition. This electrode was used for electrocatalytic activities towards the oxidation of acetaminophen in alkaline solutions. Various techniques such as cyclic voltammetery (CV), chronoamperometry (CA) and impedance spectroscopy (EIS) were utilized to study the samples. The cyclic voltammogramofNi proved the formation of á/ß crystallographic forms of the nickel oxyhydroxide under prolonged repetitive potential cycling in alkaline solution. InCVstudiesNi/NiOOHmodified electrode showed a significantly response to the acetaminophen oxidation. This work clearly revealed that this electrode is an effective electrocatalyst for detection of acetaminophen.