A novel one-step method has been carried out for synthesizing high-quality rhodium nanoparticle-loaded carbon nanofibers (nano-Rh/CNF) for the first time by using an electrospinning technology. The new hybrid material shows high electrocatalytic activity for hydrazine oxidation and can be potentially used for the amperometric sensing of hydrazine with high sensitivity and good selectivity. (C) 2010 Elsevier B.V. All rights reserved.