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A novel coagulation combined with UV/O₃ process was employed to remove the effluent organic matter (EfOM) from a biotreated pharmaceutical wastewater for harmlessness. The removal behavior of EfOM by UV/O₃ process was characterized by synchronous fluorescence spectroscopy (SFS) integrating two-dimensional correlation (2D-COS) and principal component analysis (PCA) technology. The highest dissolved organic carbon (DOC) and ratio of UV₂₅₄ and DOC (SUVA) removal efficiency reached 55.8% and 68.7% by coagulation-UV/O₃ process after 60 min oxidation, respectively. Five main components of pharmaceutical tail wastewater (PTW) were identified by SFS. Spectral analysis revealed that UV/O₃ was selective for the removal of different fluorescent components, especially fulvic acid-like fluorescent (FLF) component and humus-like fluorescent (HLF) component. Synchronous fluorescence/UV-visible two-dimensional correlation spectra analysis showed that the degradation of organic matter occurred sequentially in the order of HLF, FLF, microbial humus-like fluorescence component (MHLF), tryptophan-like fluorescent component (TRLF), tyrosine-like fluorescent component (TYLF). The UV/O₃ process removed 95.6% of HLF, 80.0% of FLF, 56.0% of TRLF, 50.8% of MHLF and 44.4% of TYLF. Therefore, the coagulation-UV/O₃ process was proven to be an attractive way to reduce the environmental risks of PTW.