Abstract: With the aim of producing dietary supplements for phenylketonurics, using whey hydrolysates as protein sources, the effect of some procedures over phenylalanine (Phe) removal was evaluated. Twelve whey hydrolysates were prepared by the action of a pancreatin, in three enzyme:substrate (E:S) ratios and two temperatures. Half of the samples were submitted to the ultrafiltration (UF) through 10,000 Da cut-off membranes. The activated carbon and the polymeric adsorbent XAD-4 were used for removing Phe from the hydrolysates. The results showed that the activated carbon was more advantageous than the resin, since it led to the lowest final Phe content (2.3 to 38.2 mg Phe/100 g hydrolysate). The effect of E:S ratio, temperature and ultrafiltration was also evaluated. The least final amount of Phe was obtained in absence of UF for three situations: E:S = 0.01% and 25°C, E:S = 0.1% and 50°C, E:S = 1.0% and 50°C.