It were performed two experiments to evaluate the utilization of industrial enzymes in the evaluation of NDF contents in high-starch materials. In the first experiment, it was verified the accuracy of estimates of neutral detergent fiber (NDF) obtained with the utilization of three industrial enzymes (Termamyl 2X, Liquozyme Supra 2.2.X, and Amylase AG 300L) at different volumes (50, 100, 250 or 500 mL/ sample). Samples were simulated to contain starch at 0, 100, 300, 500 and 1000 g/kg using purified cellulose and starch (n = 240). In the second experiment, samples of corn grain and sorghum grain were evaluated considering the same enzyme types and volumes used in the first experiment adding aliquots without using enzyme (n = 104). There was no significant bias of NDF recovery for simulated samples containing starch up to 300 g/kg. Considering those samples, none difference among enzymes was observed. It was observed a more intense decrease in NDF content according to each enzyme unit added on corn when compared to sorghum. Considering NDF evaluation in samples with mass of 0.7 to 1.0 g, it can be recommended the utilization of 250 mL the ?-amylases Termamyl and 2X Liquozyme 2.2X with activities of 240 and 300 KNU/g, respectively.