| Summary: | The<b> </b>simultaneous determination of hydroquinone and catechol was conducted in aqueous and real samples by means of differential pulse voltammetry (DPV) using a glassy carbon electrode modified with Gold Nanoparticles (AuNP) and functionalized multiwalled carbon nanotubes by drop coating. A good response was obtained in the simultaneous determination of both isomers through standard addition to samples prepared with analytical grade water and multivariate calibration by partial least squares (PLS) in winery wastewater fortified with HQ and CT from 4.0 to 150.00 µM. A sensitivity of 0.154 µA µM<sup>−</sup><sup>1</sup> and 0.107 µA µM<sup>−1</sup>, and detection limits of 4.3 and 3.9 µM were found for hydroquinone and catechol, respectively. We verified the reliability of the developed method by simultaneously screening analytes in spiked tap water and industrial wastewater, achieving recoveries over 80%. In addition, this paper demonstrates the applicability of chemometric tools for the simultaneous quantification of both isomers in real matrices, obtaining prediction errors of lower than 10% in fortified wastewater.
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