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Sorption of γ- and δ-lactones from aqueous solutions by cryotropic gels of corn and potato starches was studied using capillary gas–liquid chromatography and Fourier transform infrared spectroscopy. The sorption patterns were similar for both types of starch. However, the sorption of lactones by potato starch was 5–10% lower than their sorption by corn starch. The amount of substances bound by cryotextures of the starches depended linearly on their initial concentrations in the gel. An increase in the length of the alkyl substituent improved sorption of lactones. It was shown that six-membered rings play a greater role in total lactone sorption than five-membered rings. The apparent constants and numbers of binding sites were estimated for compounds that reached the stage of saturation. The interaction between lactones and polysaccharides was accompanied by a decrease in their conformational mobility and changes in the rheological characteristics of thermotropic and cryotropic starch gels.