ZnO/Pd nanocomposites containing 0.5-3.0mol.% palladium and possessing improved gas-sensitive properties for VOC’s detection were prepared using solvothermal synthesis. The synthesised powders have been characterised using various methods of physicochemical analysis (DSC/TGA, XRD, SET/TEM, XPS). It is shown that Pd@PdO nanoparticles (4-7nm in diameter) are localized on the surface of ZnO nanoparticles (40-50nm in size). According to the combined XRD and XPS data, it was found that palladium is in partially oxidised state, and the nanocomposite has a structure close to "core@shell": Pd@PdO. The influence of palladium concentration in the ZnO/Pd composite on the complex of chemoresistive gas-sensitive properties was studied. It is shown that at 250°C the obtained nanocomposites demonstrate a high (up to 57.8 a.u.) response to 100 ppb–20 ppm acetone, which can be used as a part of supersensitive devices for noninvasive diagnostics of diseases.