Study 1 was carried out to isolate and produce enzyme resistant micro and nano scale carbohydrates from soybean meal (SBM), distillers dried grains (DDG), and sugar beet pulp (SBP). All materials produced were in micro and nano scales, and the yields were different depending on the starting material. Study 2 determined the physiological stability of study 1 materials for potential encapsulation applications. Both SBM and SBP were stable under simulated physiological conditions; the stability of the SBM was higher than SBP. In study 3 the SBM nanomaterial from buffer extraction was used for in vitro fermentation by Bifidobacterium brevis. The B. brevis showed a good growth in the presence of SBM nanomaterial. Study 4 characterized the SBM- resistant starch thin films produced with pectin and carboxymethylcelllulose. The films formed with SBM-resistant starch and pectin at 3:1 and 1:3 provided good barrier and viscoelastic properties.