Fabrication of nano AuRh nanoparticles film modified GCE has been successfully carried out using 0.5 M H2SO4 as electrolyte. AuRh nanoparticles film modified GCE electrodes examined using atomic force microscopy (AFM), SEM and X-ray diffraction studies (XRD). Fabricated nano AuRh particles average diameter have been found as 55 nm. The nano AuRh nanoparticles modified GCE successfully reduces the over potential and shows the well defined oxidation peaks for the detection of ascorbic acid (AA), dopamine (DA), reduction of bromate and simultaneous determination of AA and dopamine (DA) (in pH 7.0 phosphate buffer solution (PBS)) using cyclic voltammetry (CV) and linear sweep voltammetry (LSV). Also, the AuRh nanoparticles modified GCE exhibits good linear range for the simultaneous detection of AA and DA in lab and real samples using LSV.