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Scrubber water, a waste stream generated by ships exhaust gas cleaning systems, may pose a threat when released into the marine environment due to potential contamination with polycyclic aromatic hydrocarbons (PAHs) and their alkyl derivatives (alkyl-PAHs). This study aims to develop a reliable analytical procedure combining headspace solid-phase microextraction (HS-SPME) with gas chromatography coupled to triple quadrupole tandem mass spectrometry (GC–MS/MS) to simultaneously separate and determine target compounds in aqueous samples. Method validation demonstrated good linearity up to 200 ng L−1 (r2> 0.996) and low limits of detection (0.33 to 1.67 ng L−1, except for naphthalene at 3.3 ng L−1). The method shows good precision (RSD

Fe2O3/TiO2 nanocomposites were fabricated via a facile impregnation/calcination technique employing different amounts iron (III) nitrate onto commercial TiO2 (P25 Aeroxide). The as-prepared Fe2O3/TiO2 nanocomposites were characterized by X-ray diffraction (XRD), Raman spectroscopy (RS), scanning electron microscopy/energy-dispersive spectroscopy (SEM/EDXS), X-ray photoelectron spectroscopy (XPS), Brunauer–Emmett–Teller analysis (BET), electron impedance spectroscopy (EIS), photoluminescence spectroscopy (PL), and diffuse reflectance spectroscopy (DRS). As a result, 5% (w/w) Fe2O3/TiO2 achieved the highest photocatalytic activity in the slurry system and was successfully immobilized on glass support. Photocatalytic activity under visible-light irradiation was assessed by treating pharmaceutical amoxicillin (AMX) in the presence and absence of additional oxidants: hydrogen peroxide (H2O2) and persulfate salts (PS). The influence of pH and PS concentration on AMX conversion rate was established by means of statistical planning and response surface modeling. Results revealed optimum conditions of [S2O82−] = 1.873 mM and pH = 4.808; these were also utilized in presence of H2O2 instead of PS in long-term tests. The fastest AMX conversion possessing a zero-order rate constant of 1.51 × 10−7 M·min−1 was achieved with the photocatalysis + PS system. The AMX conversion pathway was established, and the evolution/conversion of formed intermediates was correlated with the changes in toxicity toward Vibrio fischeri. Reactive oxygen species (ROS) scavenging was also utilized to investigate the AMX conversion mechanism, revealing the major contribution of photogenerated h+ in all processes.

Vinasse, a liquid waste which originates from the production of ethanol fuel from sugarcane, has been widely used as soil amendment in Brazil. An important concern that arises from vinasse reuse is the dissemination of antibiotics to the environment through crop soils. This work evaluated the performance of Pressurized Liquid Extraction (PLE) and QuEChERS (quick, easy, cheap, effective, rugged and safe) to extract several multiple-class antibiotics, such as cephalosporins, fluoroquinolones, ionophores, lincosamides, macrolides, quinolones, streptogramin, sulfonamides, tetracyclines and others, from agricultural soils. The performance of several parameters was evaluated for both PLE and QuEChERS, such as the extraction temperature (for PLE), solvents composition, pH and the addition of EDTA. Both methods were able to extract most target antibiotics. However, QuEChERS showed higher recoveries for macrolides and nitroimidazoles, while PLE was more suitable for fluoroquinolones and ionophores (i.e. monensin). The use of citrate-phosphate buffer at pH 7.0, in combination with methanol for PLE and with acetonitrile for QuEChERS, provided the highest antibiotic recoveries for both methods. The use of EDTA did not increase antibiotic recovery rates for QuEChERS, while the temperature had almost no influence on the extraction efficiency in PLE. • Citrate-phosphate buffer at pH 7.0 provided higher antibiotic recoveries for QuEChERS and PLE. • The combination buffer-methanol provided higher recoveries for PLE. • QuEChERS and PLE methods were able to extract most of the target antibiotics.

We provide a workflow to extract unidentified signals from chromatography-high resolution mass spectrometry (LC-HRMS) data of wastewater samples as a pre-step of a non-targeted analysis of dissolved organic matter (DOM). We provide detailed methodology on data processing and cleanup using MS processing software MZmine 2 and an own set of functions in R developed for wastewater analysis. The processing involves signal extraction, linear mass correction, reduction of noise, grouping of isotopologues, molecular formula assignment and merging of replicates. The article contains software settings and reasoning behind the choice of data extraction options. The supplementary information contains a script for the correction of signal masses using internal standards and templates of internal standard lists. We included a reproducible example as an R notebook with data cleansing workflow and data exported from MZmine. The data were used according to the described methodology in the article “A non-targeted high-resolution mass spectrometry data analysis of dissolved organic matter in wastewater treatment” by Verkh et al., 2018. • Includes a linear mass correction algorithm for LC-HRMS signals. • Describes a pipeline of non-targeted processing of LC-HRMS data of wastewater using free software. • Provides tests and reasons for parameter choice in non-targeted LC-HRMS wastewater data extraction. Method name: Combined MZmine 2.26 and R extraction workflow of LC-HRMS wastewater data, Keywords: Water screening, Molecular formula prediction, R, MZmine

This manuscript summarizes the main results obtained in various monitoring studies conducted in the Llobregat and the Ebro River basins to evaluate the occurrence of pharmaceuticals and drugs of abuse in their aquatic environments and the potentially derived risks for environmental and human health. The occurrence of these compounds in surface waters, located downstream the point of discharge of sewage treatment plants (STP), points out STPs effluents as the main source of these substances in the aquatic environment. Both river basins had similar pharmaceutical contamination patterns. However, hazard quotients (HQ) calculated for three different trophic levels (algae, daphnia and fish) pointed out sulfamethoxazol (sulfamide antibiotic) for algae, gemfibrozil (lipid regulator) for algae and fish, clofibric acid (lipid regulator) and erythromycine (macrolide antibiotic) for daphnia, and ibuprofen (analgesic anti-inflammatory) for all investigated tropic levels, as the compounds with the highest ecotoxicological risk in the Llobregat. In the Ebro River, the most problematic pharmaceuticals were sulfamethoxazol for algae, and erythromycine, clofibric acid and fluoxetine (anti-depressive) for daphnids. Levels of drugs of abuse measured in surface waters of the Ebro River were one and two orders of magnitude lower than those observed in effluent and influent sewage waters, respectively. Lack of data about their ecotoxicity does not allow calculation of HQ for these compounds. The presence of pharmaceuticals and drugs of abuse in surface and drinking waters is not subjected to regulation; hence, they are not considered priority pollutants to be included in monitoring programs. However, due to their possible harmful outcomes in wildlife, research on their potential effects in human health is indispensable.Este trabajo resume varios estudios de monitorización de fármacos y drogas de abuso llevados a cabo en el medio ambiente acuático de las cuencas de los ríos Llobregat y Ebro con el fin de evaluar la calidad del agua en relación a la presencia de estas substancias y su potencial riesgo para la salud ambiental y pública. La identificación de estos compuestos aguas abajo del punto de vertido de las plantas depuradoras apunta a la descarga de agua residual tratada como la principal fuente de emisión de estos contaminantes en el medio acuático. El perfil de contaminación por fármacos fue bastante similar en ambas cuencas. No obstante, los índices de riesgo (HQ) calculados para los fármacos en diferentes niveles tróficos (algas, dáfnidos y peces) indican que los compuestos que presentan un mayor riesgo ecotóxico en el Llobregat son el sulfametoxazol (antibiótico sulfamida) para las algas, el gemfibrozil (regulador de lípidos) para las algas y los peces, el ácido clofíbrico (regulador de lípidos) y la eritromicina (antibiótico macrólido) para los dáfnidos, y el ibuprofeno (analgésico anti-inflamatorio) para todos los eslabones tróficos. En el Ebro, los compuestos más problemáticos son el sulfametoxazol para las algas, y la eritromicina, el ácido clofíbrico y la fluoxetina (antidepresivo) para los dáfnidos.Los niveles de drogas de abuso (y sus metabolitos) determinados en la cuenca del Ebro son aproximadamente uno y dos órdenes de magnitud más bajos respectivamente que los determinados en las aguas de salida y de entrada a las depuradoras. Sin embargo, debido a la falta de datos sobre su ecotoxicidad, no se han podido calcular índices de riesgo.La presencia de estos compuestos (fármacos y drogas) en aguas superficiales y de bebida aun no está regulada y, por lo tanto, no constituyen parámetros de obligado control. Aún es imprescindible seguir investigando para poder evaluar su posible efecto en la salud humana.

Este trabajo resume varios estudios de monitorización de fármacos y drogas de abuso llevados a cabo en el medio ambiente acuático de las cuencas de los ríos Llobregat y Ebro con el fin de evaluar la calidad del agua en relación a la presencia de estas substancias y su potencial riesgo para la salud ambiental y pública. La identificación de estos compuestos aguas abajo del punto de vertido de las plantas depuradoras apunta a la descarga de agua residual tratada como la principal fuente de emisión de estos contaminantes en el medio acuático. El perfil de contaminación por fármacos fue bastante similar en ambas cuencas. No obstante, los índices de riesgo (HQ) calculados para los fármacos en diferentes niveles tróficos (algas, dáfnidos y peces) indican que los compuestos que presentan un mayor riesgo ecotóxico en el Llobregat son el sulfametoxazol (antibiótico sulfamida) para las algas, el gemfibrozil (regulador de lípidos) para las algas y los peces, el ácido clofíbrico (regulador de lípidos) y la eritromicina (antibiótico macrólido) para los dáfnidos, y el ibuprofeno (analgésico anti-inflamatorio) para todos los eslabones tróficos. En el Ebro, los compuestos más problemáticos son el sulfametoxazol para las algas, y la eritromicina, el ácido clofíbrico y la fluoxetina (antidepresivo) para los dáfnidos. Los niveles de drogas de abuso (y sus metabolitos) determinados en la cuenca del Ebro son aproximadamente uno y dos órdenes de magnitud más bajos respectivamente que los determinados en las aguas de salida y de entrada a las depuradoras. Sin embargo, debido a la falta de datos sobre su ecotoxicidad, no se han podido calcular índices de riesgo. La presencia de estos compuestos (fármacos y drogas) en aguas superficiales y de bebida aun no está regulada y, por lo tanto, no constituyen parámetros de obligado control. Aún es imprescindible seguir investigando para poder evaluar su posible efecto en la salud humana.