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The degradation of asulam herbicide by photo electro-Fenton (PEF) and solar photo electro-Fenton (SPEF) processes was studied using an undivided electrochemical BDD/carbon-felt cell to generate H2O2 continuously. A central composite design combined with response surface methodology was applied to determine the optimal operating conditions of current intensity = 0.30 A, [Fe2+] = 0.3 mM, and [Na2SO4] = 0.11 M at pH 3 to achieve the complete degradation of asulam by electro-Fenton. Subsequently, the SPEF process was more efficient treatment compared to PEF, achieving a complete degradation of asulam and 98% of mineralization in 180 min. Moreover, 4-aminobenzenesulfonamide, 4-aminophenol, and 4-benzoquinone were detected as aromatic intermediates, whereas acetic acid, oxalic acid, and NO3- ions were identified as final degradation by-products. Thus, the SPEF process is an efficient alternative for the complete degradation and mineralization of herbicide asulam in an aqueous solution under natural sunlight.

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The ecological risk associated with five endocrine-disrupting compounds (EDCs) was studied in four wastewater treatment plants (WWTPs) in Monterrey, Mexico. The EDCs, 17ß-estradiol (E2), 17α-ethinylestradiol (EE2), bisphenol A (BPA), 4-nonylphenol (4NP), and 4-tert-octylphenol (4TOP) were determined by SPE/GC-MS method, where EE2 and 4TOP were the most abundant in effluents at levels from 1.6 - 26.8 ng/L (EE2) and < LOD - 5.0 ng/L (4TOP), which corroborate that the wastewater discharges represent critical sources of EDCs to the aquatic environments. In this study, the potential risk associated with selected EDCs was assessed through the risk quotients (RQs) and by estimating the estrogenic activity (expressed as EEQ). This study also constitutes the first approach for the ecological risk assessment in effluents of WWTPs in Northeast Mexico. The results demonstrated that the effluents of the WWTPs represent a high risk for the organisms living in the receiving water bodies because the residual estrogens effect E2 and EE2 with RQ values up to 49.1 and 1165.2. EEQ values between 6.3 and 24.6 ngEE2/L were considered the most hazardous compounds among the target EDCs, capable of causing some alterations in the endocrine system of aquatic and terrestrial organisms due to chronic exposition.

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A high-performance liquid chromatography with diode array detector (HPLC-DAD) method was developed and validated for the simultaneous quantification of 4 xenoestrogens in water for monitoring their photocatalytic degradation in synthetic water. The analytical parameters evaluated were linearity, limits of detection, and quantification (LODs and LOQs), selectivity, and accuracy, according to the US Food and Drug Administration (FDA) and Eurachem guidelines. The developed method shows good linearity (R2 > 0.995 for all compounds), and LODs ranged from 0.02 to 0.04 mg L-1, while LOQs ranged from 0.05 to 0.11 mg L-1. Moreover, accuracy expressed as recovery and precision were within the required limits. Therefore, the developed method was considered accurate, and reliable. In addition, it was successfully applied for monitoring a mixture of 4 xenoestrogens in water during the photocatalytic treatment.•An HPLC-DAD method was developed to quantify 4 xenoestrogens in water simultaneously.•The developed HPLC-DAD method shows excellent linearity, selectivity, and accuracy.•A mixture of 4 xenoestrogens was reliably monitored during their photocatalytic degradation.

RESUMEN

In aquatic systems, some substances considered as endocrine disruptors have been detected, which can be due to their incomplete elimination in wastewater treatment plants (WWTPs) and inadequate disposal of pharmaceuticals. Among these contaminants are 17α-ethinylestradiol (EE2) and caffeine (CAF). Moreover, it has been reported that this kind of contaminants may provoke different adverse effects in many aquatic organisms. Because of that, in the present study, up-flow anaerobic sludge blanket reactors (UASB) coupled with the Fenton process was evaluated for EE2 and CAF removal spiked in wastewater samples. First, the best reaction conditions were established in each process. For UASB reactor, two hydraulic retention times (HRT 8 and 24 h) were evaluated, achieving the highest chemical organic demand (COD) removal (70 %) and drug elimination (84 %-86 %) with HRT 24 h. Subsequently, Fenton process was conducted at pH 3 with different levels of Fe2+ (0.05-0.5 mmol/L) and molar ratios Fe2+:H2O2 (1:1-1:10). Better results were obtained with 0.5 mmol Fe2+/L, and 1:10 ratio molar Fe2+:H2O2. Finally, UASB-Fenton coupled system allowed 80 % of COD decrease, almost complete removal of drugs and the toxicity of samples on Vibrio fischeri was reduced from 73 % to 30 %, demonstrating that this coupled system is a promising and efficient system for pharmaceutical compounds removal from wastewater.

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Five endocrine-disrupting compounds (EDCs) were determined in four urban wastewater treatment plants (WWTPs) of the Metropolitan Area of Monterrey (MAM) in two seasonal periods (winter and summer). The MAM, one of the most urbanized areas in Mexico, is characterized by high industrial activity and population density, leading to extensive use of several EDCs. In the MAM, ∼90% of urban and industrial wastewater is treated in WWTPs, where EDCs can be partially eliminated. In this work, dissolved levels of 17ß-estradiol (E2), 17α-ethinyl estradiol (EE2), bisphenol A (BPA), 4-nonylphenol (4NP), and 4-tert-octylphenol (4TOP) in wastewater were determined. The EDCs' determination was carried out through solid-phase extraction (SPE) and gas chromatography coupled to mass spectrometry (GC-MS). High EDCs levels (0.4-450 ng/L) were found in the influents of WWTPs, while concentrations in the effluents ranged from 0.2 to 26.8 ng/L, with E2, EE2, and 4TOP being the most persistent. The Spearman correlation analysis revealed the association between E2 and EE2 (r = 0.4835, p < 0.05), and between BPA and 4NP (r = 0.5180, p < 0.05), suggesting that these EDCs have similar sources. Also, E2, BPA, and 4TOP were positively correlated with the chemical oxygen demand (COD), biochemical oxygen demand (BOD), and total suspended solids (TSS) (r = 0.4080-0.5694, p < 0.05), indicating the association of the EDCs with the organic matter in the wastewater. The factor analysis confirmed the significant correlation of COD, BOD, TSS, temperature, and pH with the high occurrence of 4TOP during the summer. It was also confirmed that summer warmer temperatures favored the removal of BPA and 4NP in the studied WWTPs. Finally, the studied sites were classified by cluster analysis in three groups, revealing the impact that seasonality has on the behavior of the selected EDCs.

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