The wet chemical analysis of feed samples is time consuming and expensive. Near infrared spectroscopy (NIRS) was developed as a rapid technique to predict the chemical composition of feeds. The prediction of accuracy of NIRS relies heavily on obtaining a calibration set which represents the variation in the main population, accurate laboratory analyses and the application of the best mathematical procedures. In this study NIRS was used to determine the chemical composition of total mixed rations (TMRs) used in ostrich diets. A sample population of 479 ostrich feed samples was used in the calibration and 94 samples were used in the independent validation of dry matter (DM), ash, crude protein (CP), ether extract (EE), crude fibre (CF), acid detergent fibre (ADF), neutral detergent fibre (NDF), gross energy (GE), calcium (Ca) and phosphorus (P). Coefficient of determination in validation (r2v) and standard error of prediction (SEP) was satisfactory (r2v values higher than 0.80). Coefficient of determination and SEP values for CP, EE, CF, ADF, NDF and GE were 0.97% and 0.74%, 0.89% and 0.50%, 0.94% and 1.41%, 0.89% and 2.67%, 0.95% and 2.81% and 0.80% and 0.28 MJ/kg, respectively. Less accurate values (r2v below 0.80) were obtained for DM, ash, Ca and P being 0.57% and 0.28%, 0.67% and 1.29%, 0.43% and 0.59% and 0.49% and 0.11%, respectively. The study indicated that NIRS is a suitable tool for a rapid, non-destructive and reliable prediction of the chemical composition of ostrich TMRs.