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Cryochemical methods were used to obtain superfine powder of well-known antibacterial drug dioxidine (2,3-bis(hydroxymethyl)chynoxaline-N, N’-dioxide) and its hybrid form with Ag nanoparticles. The new materials were carefully studied by different methods of chemical analysis: nuclear magnetic resonance, TEM, electron microdiffraction, UV absorption spectroscopy, X-ray diffraction, differential thermal analysis (DTA), Fourier transformation infrared spectroscopy (FTIR), which showed that obtained materials consist of dioxidine particles with different crystal packing in comparison with original pharmaceutical with a size of 40-350 nm in diameter. But in the case of hybrid composition silver nanoparticles with a size of 2-30 nm are incorporated into organic nanoparticles. Obtained cryoforms had a better dissolution rate and solubility compared to the original dioxidine.