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We evaluated the potential application of Fourier-Transformed Infrared spectroscopy using Attenuated Total Reflectance (FTIR-ATR) to characterize and detect adulteration of whey protein concentrate (WPC). Samples were adulterated by substituting WPC by milk whey powder (MWP). Principal Component Analysis (PCA) was used to characterize the spectra. Partial Least Squares (PLS) regressions were applied to model and predict the protein content and the amount in grams of WPC and MWP in the samples. In WPC, Amide I and II bands showed decreasing trend with the protein content of the samples. The carbohydrate region between 1160 and 1000 cm⁻¹ showed spectra with opposite behavior of the Amide bands, evincing the ν Csingle bondO peak (1030 cm⁻¹) that increases as MWP was added. In PCA, PC1 (64.5%) and PC2 (18.8%) described above 80% of total variance of the spectra. PC1 variance …