A glassy carbon electrode was modified with PdO-NiO composite nanofibers (PdO-NiO-NFs) and applied to the electrocatalytic reduction of hydrogen peroxide (H2O2). The PdO-NiO-NFs were synthesized by electrospinning and subsequent thermal treatment, and then characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction, and X-ray photoelectron spectroscopy. Factors such as the composition and fraction of nanofibers, and of the applied potential were also studied. The sensor exhibits high sensitivity for H2O2 (583.43 mu A center dot mM(-1) center dot cm(-2)), a wide linear range (from 5.0 mu M to 19 mM), a low detection limit (2.94 mu M at an SNR of 3), good long term stability, and is resistant to fouling.