Development of methods for the detection of an analyte at low concentration with less time for analysis has become a prior point of interest to every analyst. In reflection of this fact, an effort has been made to synthesize 5% barium doped zinc oxide nanoparticles and was characterized by using XRD, EDX, SEM, and TEM. Further, 5% barium doped zinc oxide nanoparticle modified glassy carbon electrode was used for investigating the electro-chemical behavior of nimesulide. Voltammograms obtained in a range of 3.0-112 (I = 0.2 M) pH had a maximum peak current at pH 7.0. Various physio-chemical parameters such as, process on the surface of the electrode, which was found to be diffusion controlled, heterogeneous rate constant, number of electrons transferred and charge transfer coefficient were estimated. Further, a method for nimesulide determination in a linear range of 1.0 x 10(-5) to 1.0 x 10(-7) M with LOD 1.794 nM was proposed. This technique was later used for analytical application. (C) 2015 Elsevier B.V. All rights reserved.