UV-Vis spectroscopy for monitoring of aromatic compound degradation during electrooxidation is completely restricted by ⁻OCl/ClO₂ produced in the system. The ⁻OCl/ClO₂ absorbance masks the aromatic compounds absorbance in the UV region (260–350 nm). This study presents a method for the qualitative monitoring of degradation of aromatic compounds which has an absorbance at a UV region (260–350 nm) of the spectrum by simply removing ⁻OCl/ClO₂ from the solution using sodium meta-bisulfite (SMBS). The strategy was evaluated by monitoring of in situ hypochlorite mediated electrooxidation of real textile effluent. The degradation of aromatic compounds measured by UV-Vis spectrum analysis was supported by fluorescence spectroscopy analysis and HPLC analysis. This method can be a handy tool to monitor the degradation of any organic compounds which has an absorbance in the 250–300 nm region during an advanced electrooxidation process in the presence of chloride.