Polyvinyl alcohol (PVA) is highly compatible polymer with biological environments. Specifically, it has been used as a trap for different types of microorganisms in Bio-MEMS, and its properties can be modified to act as an electrode for electrochemical analysis. This study presents a nano-composite developed with PVA, multiwall carbon nanotubes (CNTs) doped with nitrogen, which changes the electrical properties of the polymer and its viscosity to obtain nanofibers by electro-spinning. The proposed nanocomposite was characterized using Fourier transform-infrared and Raman spectroscopy techniques, confirming the presence of the CNTs immersed in the polymer. High-resolution transmission electron microscopy was used to obtain the micrographs that showed the characteristic interplanar distances of the multiwall CNT in the polymeric matrix with values of 3.63 Å. Finally, the CNx mats were exposed to various aqueous solutions in a po-tentiostat to demonstrate the effectiveness of the nanofibers for electrochemical analysis. The CNx-induced changes in the electrical properties of the polymer were identified using cyclic voltammograms, while the electrochemical analysis revealed supercapacitor behavior.