Nickel doped cobalt(II, III) composite nanofibers were prepared by an electrospinning and sequential calcination process, and characterized by scanning electron microscopy, energy dispersive spectrometry, and X-ray diffraction. An electrospun nickel doped cobalt(II, III) modified carbon paste electrode was used for maltose determination using cyclic voltammetry and amperometry. Under the optimized conditions, a linear response was obtained between 0.2 and 100.0 mu M, with a low detection limit of 32.5nM.