A new optical sensor was developed for the rapid sensing of total phenolic content, which is simple, cheap, and sensitive, using the Eu(III)-(NTA)2-(Phen) complex [NTA = 1-(2-naphthoyl)-3,3,3-trifluoroacetone and Phen = 1,10 phenanthroline] as a luminescent probe at pH 7.5 using PIPES buffer. This method was based on luminescence quenching. The type of quenching during the reaction between the Eu(III)-(NTA)2-(Phen) complex and the phenolic compounds is dynamic quenching; the binding site is close to 1, and the reaction is endothermic, spontaneous, and involves hydrophobic attraction forces. The calibration curves were plotted using a sigmoidal fit giving an LOD of 0.01 μg mL-1, and the correlation coefficients are more than 0.99. For the first time, the time-resolved fluorescence technique was utilized in microtiter plates to enable the determination of 96 samples within two minutes with high sensitivity and selectivity. The proposed method was applied to three industrial wastewater samples and compared with the standard method for phenolic content determination, yielding high recoveries. This is the first luminescence method based on lanthanide complexes as probes for determining the total phenolic content in water samples.