In this work, we evaluated the potential application of fluorescence spectroscopy, associated with the canonical polyadic/parallel factor analysis and principal component analysis, to monitor the dissolved organic matter (DOM) generated from a slaughterhouse industry. During the monitoring process, we analyzed the residual water at the entrance and exit sites of the slaughterhouse effluent treatment as well as downstream and upstream the effluent receiving water body of a local river. The results revealed that the fluorescence analysis was able to identify proteins, chlorophylls, and humic substances at the entrance and exit sites of the slaughterhouse treatment plant and humic substances at the river water bodies. Our data also demonstrated that the industrial effluent discharged into the river did not impact the receiving water body quality as determined by the biological and humification indices obtained by fluorescence analysis, which was confirmed by conventional physicochemical analysis. In summary, the present findings indicate that fluorescence spectroscopy, in association with multivariate analysis, can be successfully applied as an analytical tool for evaluating the quality of DOM in slaughterhouse wastewater.