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Organic matter can be considered one of the most important indicators of the extent of soil desertification processes. Among the causes of desertification, salinization induced by different factors is raising the greatest concern in the Mediterranean area. In the present research, hydrophilic (HI) and hydrophobic (HO) fractions of dissolved organic matter (DOM) extracted from soils at different degrees of salinization have been investigated by means of spectroscopic techniques such as tridimensional fluorescence spectroscopy in the mode of emission excitation matrix (EEM) and Fourier transform infrared spectroscopy (FT-IR). The FT-IR spectra were distinctive in differentiating HI from HO fractions and each DOM fraction as a function of soil salinity. The EEM spectra of HO fractions exhibited a shift toward longer emission wavelengths and higher fluorescence intensity (FI) values as compared to that of the HI fractions. These results could be ascribed to the different molecular complexities of HI and HO fractions. Further, a marked quenching effect was observed in the FI of both the DOM fractions with increasing soil salinity, which allowed to obtain immediate information on the soil salinity degree by comparing the fluorescence intensity.