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Nanometal-containing biocomposites find wide use in many industries and fields of science. The physicochemical properties of these materials depend on the character of the polymer, the size and shape of the metallic nanoparticles, and the interactions between the biopolymer and the nanoparticles. The aim of the work was to synthesise and study the effect of plasma-treated water on the properties of the obtained metallic nanoparticles as well as the physicochemical and functional properties of nanocomposites based on potato starch. The metallic nanoparticles were synthesised within a starch paste made in distilled water and in distilled water exposed to low-temperature, low-pressure plasma. The materials produced were characterised in terms of their physicochemical properties. Studies have shown that gold and silver nanoparticles were successfully obtained in a matrix of potato starch in distilled water and plasma water. SEM (Scanning Electron Microscopy) images and UV-Vis spectra confirmed the presence of nanosilver and nanosilver in the obtained composites. On the basis of microscopic images, the size of nanoparticles was estimated in the range from 5 to 20 nm for nanoAg and from 15 to 40 nm for nanoAu. The analysis of FTIR-ATR spectra showed that the type of water used and the synthesis of gold and silver nanoparticles did not lead to changes in the chemical structure of potato starch. DLS analysis showed that the nanoAg obtained in the plasma water-based starch matrix were smaller than the Ag particles obtained using distilled water. Colour analysis showed that the nanocomposites without nanometals were colourless, while those containing nanoAg were yellow, while those with nanoAu were dark purple. This work shows the possibility of using plasma water in the synthesis of nanometals using potato starch, which is a very promising polysaccharide in terms of many potential applications.

Double-layered active films based on furcellaran (1st layer—FUR), chitosan, and gelatin hydrolysates (2nd layer—CHIT+HGEL) were successfully prepared. Bioactive ingredients were added to the 1st film layer: AgNPs, which were synthesized in situ with yerba mate extract; montmorillonite clay (MMT); and different loads of ethanolic curcumin (CUR) extract enriched with rosemary essential oil (REO). SEM images confirmed the presence of AgNPs with a size distribution of 94.96 ± 3.33 nm throughout the films, and AFM and SEM photos indicated that the higher substance concentrations had rougher and more porous film microstructures. However, the water vapor transmission rate was reduced only at the lowest load of this ingredient. Despite the tensile strength of the films having decreased, the incorporation of the compounds showed a tendency towards reducing the modulus of elasticity, resulting in a lower stiffness of the composites. The addition of CUR and AgNPs improved the UV light barrier properties of the materials. The presented films showed quick reactions to changes in the pH value (from orange to red along with an increase in pH from 2 to 10), which indicates their potential use as indicators for monitoring the freshness of food products. Composite No. 2 showed the highest antimicrobial potential, while none of the presented films showed an antifungal effect. Finally, the antioxidant activities of the films increased dramatically at higher AgNP and CUR loads, suggesting an outstanding potential for active food packaging applications.