The long, uniform and smooth Ni(NO3)(2)-loaded polyvinyl alcohol nanofibers were prepared via electrospinning on a nonconductive quartz plate. The nanofibers were stabilized at 300 degrees C for 3 h in nitrogen atmosphere, and then the continuous heating to 800 degrees C at the rate of 2 degrees C min(-1) keeping 3 h was used to prepare nickel-doped carbon nanofibers (Ni:CNFs). The composites were characterized with Raman spectroscopy, X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The Ni:CNFs were used as the working electrode to sense paracetamol (PCT) and glucose (GLU), respectively. When sensing PCT, the Ni: CNFs electrode showed an electrochemical behavior like on macroelectrode; but for GLU, it displayed an electrochemical behavior like on microelectrode. For both of the species, higher sensitivities on the Ni:CNFs electrodes were obtained than those on bulk glassy carbon and nickel electrodes. (C) 2014 Elsevier Ltd. All rights reserved.