Simultaneous opto-electrochemical monitoring of carbamazepine and its electro-oxidation by-products in wastewater

The growing human impact on aquatic environments deriving from the extensive use of pharmaceuticals and the release of persistent pollutants necessitates the implementation of new, widespread methods for characterising and quantifying such contaminants and their related degradation products. Carbamazepine, 5 H-dibenzo[b,f]azepine-5-carboxamide, (CBZ) is a widely used anti-epileptic drug characterised by limited removal by conventional wastewater treatments and high persistency in the environment. In this work, CBZ detection and quantification was performed in phosphate buffer, as well as in samples of complex matrix-like landfill leachates and treated wastewater originating from a medical facility, and simultaneously by optical and electrochemical methods using a novel transparent carbon-based nanostructured electrode. Coupling electrochemical (differential pulse voltammetry) with optical (UV–visible spectroscopy) methods, it has been possible to reach the limit of detection (LOD) for CBZ at the levels of 4.7 μM for the electrochemical method, 10.3 μM for the spectroscopic method, and 3.6 μM for the opto-electrochemical method. Raman spectroscopy and ultra-high performance liquid chromatography coupled with tandem mass spectrometry techniques were employed to support and validate the combined technique. The novel developed technique showed high selectivity to carbamazepine and its by-products, even in environmental samples. Thus, this environmentally friendly, fast and accurate detection method is believed to be successfully implementable in investigating other pharmaceutical and chemical contaminates of concern. [Display omitted] •Advanced combined method for monitoring of carbamazepine was designed.•Differential pulse voltammetry/Raman spectroscopy enhances carbamazepine detection.•Vertically aligned graphene at boron doped diamond served as monitoring electrode.•Carbamazepine was detected in landfill leachates and healthcare facility wastewater.•By-products from the electro-oxidation process of carbamazepine were studied.