Droxidopa is a prescribed medication for the treatment of orthostatic hypertension in patients with pure autonomic failure and multiple system atrophy, which causes symptoms of lightheadedness and Parkinson’s disease. In the current study, a simple electrochemical sensor designed for simultaneously determination of droxidopa and carbidopa via using 2-(4-ferrocenyl-[1,2,3]triazol-1-yl)-1-(naphthalen2-yl) ethanone (2FTNE) modified NiFe2O4 nanoparticles paste electrode (2FTNENFOCPE). The 2FTNENFOCPE exhibited exceptional electrochemical catalytic behavior against droxidopa and carbidopa. Chronoamperometry, cyclic voltammetry and differential pulse voltammetry (DPV) were used to explore the analytical performance of 2FTNENFOCPE for co-detection of droxidopa and carbidopa. The 2FTNENFOCPE is able to separate oxidation peak potentials of droxidopa and carbidopa about 440 mV. The detection limits achieved via DPV, for droxidopa and carbidopa were 6.0 108 and 3.0 107 M. In the final, the 2FT