Model bioactive compounds with different molecular and functional characteristics were entrapped in gel beads prepared by polyelectrolyte complexation of chitosan and pentasodium tripolyphosphate (TPP). Three compounds of interest to the food and biomedical industries were tested: (1) lysine, (2) bovine serum albumin (BSA), and (3) P-galactosidase. Effects of the compound concentration in the initial chitosan solution, pH of the curing solution, and length of the curing phase on the capture efficiency were evaluated. Release rates for lysine and BSA into a phosphate buffer, distilled water, and a synthetic ocean solution were observed, and the activity of the entrapped P-galactosidase was determined. The capture efficiencies for lysine and BSA decreased as the concentration increased. The capture efficiency for lysine ranged from 90% at pH 5 to 20% at pH 8.6. There was no significant effect of the release media on the rate of release. BSA and lysine release reached 90% of the maximum after 100 and 50 min, respectively. The capture efficiency of P-galactosidase was not affected by the pH of TPP; however, enzyme activity in the beads decreased as the pH increased. Beads prepared in the pH 8.6 TPP solution had significantly higher rates of enzyme release over time.