This study investigates the potential of fluorescence excitation/emission matrices (EEM) measurement as a tool to predict N-Nitrosodimethylamine (NDMA) formation in water reuse applications. In particular, samples from a pilot-scale membrane biological reactor (MBR) followed by nanofiltration (NF) advanced water treatment plant, are used for the study. Concentrations of both, specific NDMA precursors and NDMA formation potential (FP) are correlated with different EEM peaks. The specific precursors investigated are: erythromycin, azithromycin, clarithromycin, venlafaxine, o-desmethylvenlafaxine, ranitidine and citalopram, while the NDMA FP is conventionally measured by the NDMA formation potential test. EEM peaks investigated are obtained by fluorescence regional integration as well as by the peak picking method generating I1, I2, I3, I4, and I5 peaks. Results showed that protein-like materials are correlated with the bulk NDMA FP and specific NDMA precursors. Additionally, selected fluorescence peaks such as I1, I2 and I4 are strongly correlated with NDMA precursors throughout the MBR-NF pilot plant. The removal of NDMA precursors and EEM peaks also correlated well (R2 > 0.8). This data shows that fluorescence EEM can be a promising tool to monitor the concentration of NDMA precursors and their removal in water reuse application.