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To overcome this, we develop an analytical model for the simultaneous determination of triclosan and naphthol from mixed solutions of the compounds. A linear calibration plot from 1.7 to 34 µM was obtained for both triclosan and naphthol with limit-of-detection (LOD) of 0.62 µM and 1.03 µM respectively. The developed protocol was tested for the analysis of water samples collected from various environmental sources spiked with different concentrations of triclosan and naphthol. The samples were enriched by solid-phase-extraction which al