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Carried out experiments with fibers by using Raman spectroscopy and microscopy methods. We found the two characteristic properties of the gelatin spectra and the four of the PLA spectra in the studied experimental system. Found the best parameters for the experimental system analyzing. In the spectra recorded from the fibers of a mixture of PLA and gelatin, peaks of both components were observed. It has been shown that PLA and gelatin form mixed fibers, rather than single-component fibers.