Аннотация:Nanofibers based on semiconductor oxide ZnO and modifiers MOx (M = FeIII, CoII,III, NiII, GaIII; [M]/([Zn] + [M]) = 15 mol%) were synthesized by electrospinning method and characterized by X-ray diffraction, scanning electron microscopy (SEM) and X-ray fluorescence analysis. Acidic properties of ZnO and ZnO/MOx nanofibers were characterized by Fourier-transform infrared spectroscopy (FTIR). The sensor properties of ZnO and ZnO/MOx nanofibers were studied towards 0.1–5 ppm of C1–C4 short-chain fatty acids (SCFAs: HCOOH, CH3COOH, C2H5COOH, C3H9COOH) in dry (relative humidity at 25 °C RH25 = 0 %) and humid (RH25 = 80 %) air. It was demonstrated that the sensitivity of ZnO/MOx nanofibers towards SCFAs is primarily influenced by the band bending at the ZnO/MOx interface, which can be characterized by the difference in the electron work function for a complex oxide MOx and for ZnO. The lowest measurable concentrations of SCFAs correspond to the sub-ppm level, including high air humidity conditions (RH25 = 80 %), that makes these materials possible candidates for use in electronic nose systems for medical analysis of SCFAs in exhaled breath.