Chemometric procedures are usually applied to near-infrared (NIR) spectra in order to obtain prediction models. These procedures include the application of different combinations of spectral mathematical pretreatments for the improvement of calibrations and the selection of the best model on the basis of validation results. In this work, we used an automatic routine to obtain calibrations for unground and ground compound feedingstuffs (N=354 samples), including 49 combinations of pretreatments (first and second derivatives, an auto scaling procedure, detrending and two versions of multiplicative scatter correction). Calibrations for crude fiber and crude protein were developed without elimination of outliers and with 2 or 9 maximum passes of elimination of outliers. Validation statistics were highly influenced by the pretreatments used, as a combined result of their ability to improve the detection of outliers and the model adjustment. The standard error of prediction (SEP) values ranged from 0.61 to 1.27 for crude protein (CP) and from 0.74 to 1.33 for crude fiber (CF). In spite of the fact that validation statistics did not show a clear distribution pattern, some combinations of pretreatments provided consistently better results.