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Considering current water situation, reuse is an effective solution to meet water demand and reduce pressure on conventional water sources. However, pharmaceutical and personal care products (PPCPs) in effluents from wastewater treatment plants (WWTPs) decrease their quality and suitability. With the aim of identifying and monitoring both the influence of PPCPs and the suitability of effluents to be reused, this study proposes the development of a composite indicator (CI) related to PPCP presence in WWTPs, through the common weight multi-criteria decision analysis (MCDA)–data envelopment analysis (DEA) model. Obtaining a CI for PPCPs is a novel approach in the published literature, showing a new perspective in PPCP management and their influence in wastewater treatment. Furthermore, this study proposes an improvement on MCDA-DEA model which maintains the initial hierarchy obtained for the units analyzed. The development of CI is based on information about the technological, environmental, social, and biological issues of WWTPs. Results show that 4 of the 33 WWTPs analysed had the best CI values, meaning that their effluents have lower environmental impact. The development of a CI related to PPCPs in WWTPs suggests that further steps are needed to manage the WWTP effluents. Hence, the need to implement preventive measures in WWTPs has been shown, even though the removal of PPCPs is not yet part of European law. This work highlights the importance of considering PPCPs as priority pollutants in wastewater management and reuse frameworks, to guarantee low environmental impact and adapt wastewater reuse based on a circular economy approach. This work has been supported by the Spanish Ministry of Economy and Competitiveness and the ERDF (European Regional Development Fund) through the project Eco2TOOLS (No. CGL2015-64454-C2-1-R, subproject Eco2RISK-DDS).

Evidence of the increase of emerging contaminants in the environment due to the COVID-19 pandemic, such as personal protective equipment (PPE), disinfectants, pharmaceuticals, etc., has enlarged. Here we explain the variety of pathways of these emerging contaminants to enter the environment, including wastewater treatment plants, improper disposal of PPE, and runoff from surfaces treated with disinfectants. We also discuss the current state-of-art of the toxicological implications of these emerging contaminants. Initial research suggests that they may have harmful effects on aquatic organisms and human health. Future directions are suggested as further research is needed to fully understand the impacts of these contaminants on the environment and humans, as well as to develop effective approaches to mitigate their potential negative effects., This work has been supported by the Generalitat Valenciana through the project ANTHROPOCENE 2.0 (CIPROM/2021/032).

Sediments are excellent archives for studying the long-term variations of pollutants in the environment. For this reason, records derived from the chemical analysis of sediment cores are useful to trace the history of pollutant emissions.This study aimed to study the vertical variation of organic contaminants (OCs) and metals sediment cores collected in two sites (northern and southern part) of the L´Albufera Natural Park (Valencia, Spain) to obtain information regarding historical variation in the composition of sediments. Other sediment characteristics, such as organic matter, organic carbon content, humidity, were also studied.A sediment core sampler (57 mm inner diameter, 1.00 m length; Beeker, Eijelkamp) was used to extract the cores from the lake of L’Albufera. The cores were sampled from boat. The sediment cores were 80–87 cm in length and 5 cm in diameter. The tubes were kept upright in a bucket with ice until they arrived at the laboratory where they were frozen. Once frozen, the tubes were cut into 8 segments of the same thickness (8 slices of 10 cm) using a stainless steel cutter. Pharmaceuticals, pesticides, poly and perfluoroalkyl substances (PFASs) and phosphorous flame retardants (PFRs) were analysed using Orbitrap Exploris 120 mass spectrometer. The compounds were extracted by different extraction methods and determined both, using wide target screening against a positive list of compounds and non-target screening applying ddMS2 of the 4 more intense ions in each cycle as well as all ions fragmentation. Both positive and negative ionization were used. Several pollutants, especially pesticides such as Azoxystrobin, Imazalil, Molinate, Tebuconazole, Thiabendazole and Tricyclazol were detected in the sediment in contact with water. Some infiltration of the compounds in the inner layers of sediments were also detected. Superficial sediments provide information on the actual deposited material and the actual status of pollution but the study of sediment profiles provides information on the historical variation in the composition of sediments settled. These sediments can also be used to examine pollution mechanisms, which are significant for predicting future pollution tendencies and assessing potential environmental risks.Acknowledgments: This work has been supported by Grant RTI2018-097158-B-C31 funded by MCIN/AEI/ 10.13039/501100011033 and by “ERDF A way of making Europe” and the grant of the Generalitat Valenciana Prometeo Programme CIPROM/2021/032. Y. Soriano also thanks MCIN/AEI/ 10.13039/501100011033 and ERDF for their Predoc contract (PRE2019-089042).

According to Buck et al. [1], the “perfluoroalkyl and polyfluoroalkyl substances” (PFASs) are a subset of highly fluorinated aliphatic substances that contain one or more C atoms, on which all the H substituents (present in the non-fluorinated analogues from which they are notionally derived) have been replaced by F atoms, in such a manner that they contain the perfluoroalkyl moiety CnF2n+1–

Predictive models were generated to evaluate the degree to which nine metals (Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, and Zn) were absorbed by the leaves, stems and roots of forage sorghum in growing media comprising soil admixed with poultry manure concentrations of 0, 10, 20, 30 and 40 g/kg. The data revealed that the greatest contents of the majority of the metals were evident in the roots rather than in the stems and leaves. A bioaccumulation factor (BAF) 1. Translocation factor values were, The authors extend their appreciation to the Deputyship for Research and Innovation, Ministry of Education in Saudi Arabia for funding this research work through the project number IFP-KKU-2020/3.

Wastewater-based epidemiology (WBE) estimates collective consumption or exposure to chemicals or pathogens by monitoring the substances excreted in the population’s wastewater. Advances in mass spectrometry (MS) and the application of some clinical diagnostic tools and proteomics to wastewater fingerprinting have been linked to the discovery of new biomarkers and indicators of population health and are broadening the scope of WBE that nowadays cover not only small molecule biomarkers but also genetic biomarkers, large molecules, viruses, infection diseases, resistance, etc. This mini-review highlights recent WBE advances using MS and how this progress can create a fingerprint of a city’s health hazards, habits, and lifestyle, which is gaining in public health emphasis., This work has been supported by Grant RTI2018-097158-BC31 funded by MCIN/AEI/ 10.13039/501100011033 and by “ERDF A way of making Europe”, Grant PID2020-114065RBC22 funded by MCIN/ AEI/ 10.13039/501100011033 and project ANTROPOCEN@ (PROMETEO/2018/155) funded by Generalitat Valenciana.

Measurements of chemical persistence in natural environments can provide insight into behavior not easily replicated in laboratory studies. However, it is difficult to find environmental situations suitable for such measurements, particularly for substances with half-lives exceeding several weeks. The objective of this study was to demonstrate that a strategic postflood monitoring campaign can be used to quantify transformation half-lives on the scale of months in a real aquatic system. Water samples were collected in the upper Brisbane River estuary on 36 occasions over 37 weeks and analyzed for 127 pharmaceuticals and personal care products (PPCPs), pesticides, and perfluoroalkyl substances (PFASs). High quality time trend data were obtained for 41 substances. For many of these, data on the input of a wastewater treatment plant to the upper estuary were also obtained. A mass balance model of the estuary stretch was formulated and parametrized using PFASs as persistent benchmarking chemicals. Transformation half-life estimates were obtained for 10 PPCPs and 7 pesticides ranging from 18 to 260 days. Furthermore, insight was obtained into dominant transformation processes as well as the magnitude of chemical inputs to the estuary and their sources. The approach developed shows that under certain conditions, estuaries can be used to quantify the persistence of organic contaminants with half-lives of the order of several months., R. Álvarez-Ruiz acknowledges the Spanish Ministry of Science, Innovation and Universities and the ERDF (European Regional Development Fund) for his FPI grant BES-2016−078612. This project was supported by an Australian Research Council (ARC) Linkage grant (LP180101128) and the European Union’s Horizon 2020 research and innovation program under the Marie Skłodowska-Curie grant agreement No 734522 (INTERWASTE project).

The spread of pesticides in water bodies integrated into agricultural landscapes may prevent some areas from being colonized. In this study, the effects on the colonization responses of D. magna exerted by gradients of realistic environmental concentrations of the pesticides chlorpyrifos, terbuthylazine and their mixtures were tested in a novel multicompartment non-forced exposure system. Furthermore, the effects of both pesticides and their mixtures on the swimming behavior and the neurotransmission activity of D. magna were analyzed using a traditional forced exposure system. The synthesis and concentration of the main environmental metabolites of terbuthylazine were also analyzed. Results confirmed that D. magna exposed to mixture gradients were able to detect the pollutants and their colonization dynamics were drastically inhibited. The swimming behavior increased in D. magna exposed to the highest concentration of the mixture treatment. AChE activity was only significantly inhibited in the D. magna exposed to the highest concentration of chlorpyrifos. Changes in swimming behavior could not be directly related to the effects on AChE. Furthermore, the synthesis of the metabolite terbuthylazine 2-hydroxy during the course of the experiments was confirmed. These results demonstrate the importance of integrating pesticide mixtures in both non-forced and forced exposure systems during ecotoxicological assays., This research was funded by the Spanish Ministry of Science, Innovation and Universities and the European Regional Development Fund (ERDF) through the project WETANPACK (grant number RTI2018-097158-B-C31) and MCIN/AEI/10.13039/501100011033 through the project BrEStress (PID2019-105868RA-I00).

This study aimed to develop multi-residue methods for the extraction of organic pollutants in mussels (Mytilus galloprovincialis), including 11 pharmaceuticals, 5 pesticides, 5 perfluoroalkyl substances (PFASs) and 2 illicit drugs. The combination of 4 different QuEChERS methods and 12 clean-ups (a total of 44 combinations) was tested. QuEChERS included acidified (AQ), non-acidified (SQ) and their miniaturized versions. The clean-ups included 6 different conventional dispersive solid phase extraction (dSPE) plus 2 enhanced matrix removal (EMR-Lipid) and 4 SPE procedures (including sorbents focused on phospholipid removal and polymer-based). After sample analysis via HPLC-MS/MS, the three methods that provided the best results were validated in terms of linearity, accuracy, precision, sensitivity and matrix effect. The methods selected were the combination of (i) SQ and EMR-Lipid, (ii) AQ and Z-sep+ bulk-based dSPE and (iii) AQ and graphitized carbon black (GCB)-based dSPE. Recoveries at two concentration levels (50 and 500 ng/g) ranged 54–124%, 59–124% and 60–127%, respectively, and limits of quantification (LOQs) were, The research that led to these results received funding from the Spanish Ministry of Science, Innovation and Universities and the ERDF (European Regional Development Fund) through the project WETANDPAC (RTI2018-097158-B-C31) and from the Generalitat Valenciana through the project ANTROPOCEN@ (PROMETEO/2018/155). R. Álvarez-Ruiz acknowledges the Spanish Ministry of Science, Innovation and Universities and the ERDF for his FPI grant BES-2016-078612.

This study assesses the extraction of eleven pharmaceuticals, five pesticides, five perfluoroalkyl substances, and two illicit drugs in hemolymph from (Mytilus Galloprovincialis). Four extraction procedures using Phree™ Phospholipid Removal cartridges were tested using different volumes of methanol (400 and 600 μL) and acetonitrile (300 and 450 μL). The pollutants were determined by high-performance liquid chromatography–tandem mass spectrometry. The use of methanol gave several problems during the extraction procedure, such as longer times and sample loss. Three methods (acetonitrile 300 and 450 μL; and methanol 600 μL) were validated. Recoveries at three concentration levels (5, 50, and 100 ng/mL) ranged 35.1–129.0 and 29.3–133.0% for acetonitrile 300 and 450 μL, respectively, while recoveries for methanol 600 μL ranged 52.2–166.0%. Limits of detection were < 10 ng/mL for most analytes using any of the methods. Methanol 600 μL was the only method capable to extract the illicit drug 4-methoxyphencyclidine and provided a better peak shape and higher signal-noise ratio. When applied to non-spiked samples from local markets salicylic acid and diclofenac were detected at 33.50-97.79 and 28.30-30.31 ng/mL respectively. To our knowledge, there are no methods to determine organic contaminants in hemolymph and this is the first application of Phree™ cartridges for mussel hemolymph extraction., The research that led to these results received funding from the Spanish Ministry of Science, Innovation and Universities and the European Regional Development Fund through the project WETANDPAC (RTI2018-097158-B-C31) and from the Generalitat Valenciana through the project ANTROPOCEN@ (PROMETEO/2018/155). R. Álvarez-Ruiz acknowledges the Spanish Ministry of Science, Innovation, and Universities and the ERDF (European Regional Development Fund) for his FPI grant BES-2016-078612.

Two solid-phase extraction methods were systematically studied to determine 32 pharmaceuticals and personal care products in water and sediments by ultrahigh-performance liquid chromatography–tandem mass spectrometry. One involves HLB cartridges activated with sodium dodecyl sulfate before the passage of the sample to form an ion pair with cationic analytes, and the other uses mixed HLB–cation exchange cartridges. The accuracy of the sodium dodecyl sulfate method was good for most compounds (recoveries of 61–120% with relative standard deviation less than 23%). However, the recoveries for atorvastatin, codeine, paracetamol, flufenamic acid, and salicylic acid were approximately 50% and for omeprazole and triclocarban were even lower (from 0 to 12%). The detection limits were 1.65–25 ng L-1 in water and 0.33–4.00 ng g-1 (dry weight) in sediment. The recoveries for the mixed-mode cartridge (Strata-X-CW) method ranged from 57% to 120% with relative standard deviation less than 21%, with the exception of codeine [25% (water)], metformin [11% (sediment)], paracetamol [48% (sediment)], and salicylic acid [32% (sediment)]. The detection limits were 1.65–38.35 ng L-1 in water and 0.33–10 ng g-1 (dry weight) in sediment. Both methods followed the same pattern when applied to water. For sediments, the recoveries, which offer good performance, were not very high, although 60% of the compounds had recoveries greater 80%. The methods were applied to the analysis of surface water and sediments from the Albufera Natural Park (Spain). Twenty-seven of 32 analytes were detected in the samples analyzed., The research that led to these results received funding from the Spanish Ministry of Science, Innovation and Universities and the European Regional Development Fund through the project WETANDPAC (RTI2018-097158-B-C31) and from the Generalitat Valenciana through the project ANTROPOCEN@ (PROMETEO/2018/155). Daniele Sadutto acknowledges the Generalitat Valenciana for his Santiago Grisolia grant: “GRISOLIAP/ 2018/102, Ref CPI-18-118.”.

A great number of dose–response studies indicate that hormesis is a common phenomenon, occurring in numerous organisms exposed to singular or combined environmental stressors, such as pharmaceuticals, heavy metals, micro/nanoplastics, organic flame retardants, pesticides, and rare earths. (1−6) While biological responses to low exposure levels are often beneficial, exposure to doses below the no-observed-adverse-effect-level (NOAEL; hereafter subthreshold doses) does not always translate to beneficial responses. (2,4) For example, subthreshold contaminant doses can enhance the virulence of phytopathogenic microbes and promote the resistance of crop pests with significant implications for crop production. (2,7,8) Subthreshold contaminant exposures can also stimulate infectious animal/human pathogens and promote their resistance to antibiotics and other drugs, threatening long-term sustainability. Importantly, the hormetic function of common pathways that regulate cancer progress indicate that current regulatory standards may not protect adequately against cancer risks. (9−11), We are grateful to Dr. Patrick H. Brown, Distinguished Professor of Plant Science at the University of California, Davis, U.S.A., and Dr. Adrian Covaci, Professor of Environmental Toxicology and Chemistry at the University of Antwerp, Belgium, for comments and suggestions on an early draft of the paper. This study did not receive a specific grant from funding agencies in the public, commercial, or not-for-profit sectors. E.A. acknowledges support from the National Natural Science Foundation of China (No. 4210070867), The Startup Foundation for Introducing Talent of Nanjing University of Information Science & Technology (NUIST), Nanjing, China (No. 003080), and the Jiangsu Distinguished Professor program of the People’s Government of Jiangsu Province. E.J.C. acknowledges longtime support from the U.S. Air Force (AFOSR FA9550-13-1-0047) and ExxonMobil Foundation (S18200000000256). The sponsors were not involved in the study design; the collection, analysis or interpretation of the data; the preparation of the manuscript or the decision where to submit the manuscript for publication. All authors hold senior editorial positions in various scientific journals. The views presented herein are those of the authors and do not represent views of journals’ editorial board as a unit, journals’ editorial office, journals themselves or their publishers, authors’ institutions, or scientific societies where authors hold senior positions.

Wastewater-based epidemiology (WBE) is a new complementary alternative to traditional epidemiological surveillance approaches for community health surveys. It provides objective, flexible, and comprehensive data on diseases, exposure to toxicants and pathogens, social habits, and lifestyle. Wastewater is regarded as an integrated pooled sample of the entire population served by a certain wastewater system, thus providing an average picture of its health status. WBE relies on the extraction, analysis, and subsequent interpretation of appropriate health status indicators, including both chemical and biological components, either exogenous or endogenous, altogether constituting the exposome. Instrumental development, especially mass spectrometry (MS) for the chemical analysis of small and large molecules, has been critical to the success achieved through WBE. Whereas all previous studies have been restricted to small molecules, the use of proteomics in WBE is an obvious extension of the intensive ongoing pursuit of biomarkers for community surveillance of diseases and health status. The relevance of human proteins present in wastewater as potential WBE indicators of population-prevalent diseases has been previously postulated, although no real examples to demonstrate their feasibility have been available until recently. These findings provide new insights into the characterization of wastewater proteomics useful for practical purposes related not only to WBE applications but also to environmental monitoring and wastewater treatment plant management.

Wastewater-based epidemiology is an additional indicator of drug use that is gaining reliability to complement the current established panel of indicators. The aims of this study were to: (i) assess spatial and temporal trends of population-normalized mass loads of benzoylecgonine, amphetamine, methamphetamine and 3,4-methylenedioxymethamphetamine (MDMA) in raw wastewater over 7 years (2011-17); (ii) address overall drug use by estimating the average number of combined doses consumed per day in each city; and (iii) compare these with existing prevalence and seizure data.Analysis of daily raw wastewater composite samples collected over 1 week per year from 2011 to 2017.Catchment areas of 143 wastewater treatment plants in 120 cities in 37 countries.Parent substances (amphetamine, methamphetamine and MDMA) and the metabolites of cocaine (benzoylecgonine) and of ΔBenzoylecgonine was the stimulant metabolite detected at higher loads in southern and western Europe, and amphetamine, MDMA and methamphetamine in East and North-Central Europe. In other continents, methamphetamine showed the highest levels in the United States and Australia and benzoylecgonine in South America. During the reporting period, benzoylecgonine loads increased in general across Europe, amphetamine and methamphetamine levels fluctuated and MDMA underwent an intermittent upsurge.The analysis of wastewater to quantify drug loads provides near real-time drug use estimates that globally correspond to prevalence and seizure data.

A single workflow based on three approaches (target, suspected and non-target screening) using liquid chromatography coupled to quadrupole-time-of-flight mass spectrometry (LC-QTOF-MS) in data independent acquisition mode (DIA) was developed to assess the presence of emerging pollutants (EPs) in water and sediments from a Mediterranean River Basin. Identification of potential contaminants was based on mass accuracy, isotopic ratio pattern, theoretical fragmentation, and retention time using Waters UNIFI software. In the suspect screening against a library containing 2200 components, 68 contaminants were tentatively identified, 6 of which were confirmed and quantified with analytical standards. Non-target screening (NTS) required additional manual processing and the aid of an on-line database (ChemSpider) to tentatively identify compounds. Eprosartan, an antihypertensive drug not included in the library used for suspected screening, was confirmed and semi-quantified. The identification of Eprosartan proved the workflow to be functional for NTS. Target screening of 171 pesticides and 33 pharmaceuticals and personal care products (PPCPs) including the compounds confirmed using suspect and non target screening achieved monitoring of the most abundant contaminants from the head to the mouth of the Turia basin to establish their spatial distribution. QTOF-MS screening versatility with its high-resolution capability allows for a comprehensive assessment of EPs in the aquatic environment., This work has been supported by the Spanish Ministry of Science, Innovation and Universities and the ERDF (European Regional Development Funds) through the project GCL2015-64454-C2-1-R (ECO2risk-dds) and the project RTI2018-097158-B-C31(Wetanpack) and through the Generalitat Valenciana (ANTROPOCEN@, PROMETEO/2018/155). A. Ccanccapa gratefully acknowledges the Conselleria D'Educació, Cultura i Sport de la Generalitat Valenciana for the financial support through “Santiago Grisolía” Scholarship Program.

Wastewater-based epidemiology (WBE) has been consolidated as a tool to provide real-time information on consumption of legal and illegal drugs of abuse by the population. However, WBE is expected to achieve more ambitious objectives such as establishing exposure to certain agents (pesticides, personal care products, persistent organic pollutants, and pathogens), incidence of specific diseases (diabetes, allergies, oxidative stress, and cancer), and determination of some lifestyle consequences (exposure to personal care products, consumption of doping substances or products for the treatment of erectile dysfunction) or environmental factors (increase in temperature) in populations. Herein, we outlined the state-of-the-art applications of WBE including its advantages and disadvantages as well as the prospects for achieving a broader assessment of the habits and health of populations. WBE needs to be further strengthened to help epidemiologists and health authorities to correctly assess fingerprints of human activities in wastewater., This work has been supported by the Generalitat Valenciana (local government of the Valencian Community) through the project ANTROPOCEN@ http://www.antropocena.com (PROMETEO/2018/155).

The analysis, prevention, and removal of microplastics (MPs) pollution in water is identified as one major problem the world is currently facing. MPs can be directly released to water or formed by the degradation of bigger plastics. Nowadays, it is estimated that annually between 4 and 12 million tonnes of plastic go into the seas and oceans-with a forecast for them to outweigh the amount of fish in 2050. Based on the existing studies, the characterization of MPs in waters is still one of the remaining challenges because they can be easily confused with organic or other types of matter. Consequently, there is an urgent necessity to establish pathways for the chemical identification of the MP nature. In this perspective, the recent techniques and instrumentation for MP characterization (Raman and Fourier-transform infrared spectroscopies and microscopies, pyrolysis and thermal desorption gas chromatography, imaging techniques, etc.) are discussed including considerations to the multidimensionality of the problem. This perspective also summarizes and provides updated data on the sources and occurrence, transport and fate of MPs in aquatic ecosystems, as well as influencing conditions and factors affecting dispersal. Additionally, how engineering and biotechnological tools, such as advanced water treatments, would help to control, reduce, or even eliminate MP pollution in the near future is outlined. © 2019 American Chemical Society., This work has been supported by the Spanish Ministry of Science, Innovation and Universities and the ERDF (European Regional Development Fund) through the project Eco2RISK-DDS (CGL2015-64454-C2-1), by the Generalitat Valenciana through the project ANTROPOCEN@ (PROMETEO/2018/ 155) and the Generalitat de Catalunya (Consolidated Research Groups 2017 SGR 1404water and soil quality unit).

The present study focused on the occurrence, distribution and risk assessment of 32 pharmaceuticals and personal care products (PPCPs) in water and sediment, as well as the surrounding soil of the irrigation channels and lake of a Mediterranean coastal wetland, the Albufera Natural Park (Valencia, Spain). Moreover, the influent and effluent of ten wastewater treatment plants (WWTPs) that treat wastewater from Valencia and the surrounding areas were also studied. BPA, caffeine, diclofenac, ethyl paraben, methyl paraben, metformin, tramadol and salicylic acid were the predominant PPCPs detected in the channels and the lake, and are in good agreement with those detected in the effluent. Furthermore, 22 PPCPs were detected in >47% of the sediment samples. Of them, BPA, ethyl paraben, furosemide, ibuprofen and salicylic acid were at higher concentrations. In contrast, only seven PPCPs were detected in >44% of the soil samples. Spatial variation showed that the concentration of many PPCPs was higher in the northern area of the park, whereas the ibuprofen concentrations were higher in the south. Differences were also observed according to the type of water used for irrigation and the land uses of the area. A risk assessment based on the hazardous quotient (HQ) indicated that caffeine is a compound of concern, and tramadol at the highest concentration showed a moderate risk for the organisms assessed. Considering the mixture of the PPCPs found at each sampling point, the green algae are at risk, particularly in those points located near the city of Valencia (the most important nearby human settlement). These results indicate the need for further studies., The research that led to these results received funding from the Spanish Ministry of Science, Innovation and Universities and the European Regional Development Fund through the project WETANDPAC (RTI 2018-097158-B-C31) and from the Generalitat Valenciana through the project ANTROPOCEN@ (PROMETEO/2018/155). Daniele Sadutto acknowledges the Generalitat Valenciana for his Santiago Grisolia grant: “GRISOLIAP/2018/102, Ref CPI-18-118”. Jarko Akkanen and Timo Ilo acknowledge the funding from “Kone Foundation”.

This study aimed to develop multi-residue methods for the extraction of organic pollutants in mussels (Mytilus galloprovincialis), including 11 pharmaceuticals, 5 pesticides, 5 perfluoroalkyl substances (PFASs) and 2 illicit drugs. The combination of 4 different QuEChERS methods and 12 clean-ups (a total of 44 combinations) was tested. QuEChERS included acidified (AQ), non-acidified (SQ) and their miniaturized versions. The clean-ups included 6 different conventional dispersive solid phase extraction (dSPE) plus 2 enhanced matrix removal (EMR-Lipid) and 4 SPE procedures (including sorbents focused on phospholipid removal and polymer-based). After sample analysis via HPLC-MS/MS, the three methods that provided the best results were validated in terms of linearity, accuracy, precision, sensitivity and matrix effect. The methods selected were the combination of (i) SQ and EMR-Lipid, (ii) AQ and Z-sep+ bulk-based dSPE and (iii) AQ and graphitized carbon black (GCB)-based dSPE. Recoveries at two concentration levels (50 and 500 ng/g) ranged 54-124%, 59-124% and 60-127%, respectively, and limits of quantification (LOQs) were 30 ng/g for most analytes using any of the methods. The three methods were tested in non-spiked mussel samples purchased in local markets, but organic pollutants were not detected in any sample. However, the methods probed to successfully extract a wide range of organic pollutants families in mussel samples from the market and from bioaccumulation trials.

© 2021 by the authors., The use of psychoactive substances is a serious problem in today’s society and reliable methods of analysis are necessary to confirm their occurrence in biological matrices. In this work, a green sample preparation technique prior to HPLC-MS analysis was successfully applied to the extraction of 14 illicit drugs from urine samples. The isolation procedure was a dispersive liquid–liquid microextraction based on the use of a low transition temperature mixture (LTTM), composed of choline chloride and sesamol in a molar ratio 1:3 as the extracting solvent. This mixture was classified as LTTM after a thorough investigation carried out by FTIR and DSC, which recorded a glass transition temperature at −71 °C. The extraction procedure was optimized and validated according to the main Food and Drug Administration (FDA) guidelines for bioanalytical methods, obtaining good figures of merit for all parameters: the estimated lower limit of quantitation (LLOQ) values were between 0.01 µg L−1 (bk-MMBDB) and 0.37 µg L−1 (PMA); recoveries, evaluated at very low spike levels (in the ng-µg L−1 range), spanned from 55% (MBDB) to 100% (bk-MMBDB and MDPV); finally, both within-run and between-run precisions were lower than 20% (LLOQ) and 15% (10xLLOQ)., This research was funded by “Sapienza University”, research project “Low transitions temperature mixtures as microextraction solvents”, grant number RG11916B6451D44A.

Coastal environments are heavily influenced by human activities. Chemical substances considered as emerging contaminants (ECs) are one of the most important indicators of the anthropic influence on the environment, and they have recently shown to interact with microplastics (MPs). Mussels are suitable for in-lab bioacumulation studies providing insight about the occurrence and fate of contaminants in the organisms. In this study, bioacummulation of 20 chemical substances catalogued as ECs, including pharmaceuticals and personal care products (PPCPs), pesticides, and perfluoroalkyl substances (PFASs) in Mytilus galloprovincialis was assessed, with or without the influence of the presence of MPs. Mussels were distributed in three groups: control (B), exposed to ECs (C) and exposed to ECs and polyethylene MPs (C+M). The study was carried out for 58 days separated in two stages (i) exposure during days 0–28, and (ii) depuration during days 29–58. Visceral mass and haemolymph of the mussels were extracted separately, using QuEChERS and solid phase extraction (SPE), respectively. Then, extracts were analysed via UHPLC-MS/MS. Results showed that 3 PPCPs, 4 pesticides and 3 PFASs accumulated in visceral mass with bioconcentration factors (BCFs) ranging 6.7–15000 L/kg/d. In addition, 2 PPCPs, 2 pesticides and PFPeA were detected in haemolymph showing BCFs ranging 0.9–3.3 L/kg/d. When comparing C and C+M, MPs worked as a vector for the accumulation of the PFASs: PFOA, PFOS, PFDA and PFPeA; showing higher BCFs in the presence of MPs. Furthermore, the elimination of PFDA and PFOS was slower in the mussels exposed to MPs. On the other hand, the pesticides terbuthylazine and chlorpyrifos showed lower BCFs and more rapid elimination in the mussels exposed to MPs., The research that led to these results received funding from the Spanish Ministry of Science, Innovation and Universities and the European Regional Development Fund through the project WETANDPAC (RTI2018-097158-B-C31) and from the Generalitat Valenciana through the project ANTROPOCEN@ (PROMETEO/2018/155). R. Álvarez-Ruiz acknowledges the Spanish Ministry of Science, Innovation and Universities and the ERDF (European Regional Development Fund) for his FPI grant BES-2016-078612.

In this study, the occurrence of 12 organophosphorus flame retardants (OPFRs), 64 pesticides, 21 perfluoroalkyl substances (PFASs) and 34 pharmaceuticals and personal care products (PPCPs) in surface water, sediments and vegetation collected from seven locations along the South Riyadh and six locations along the Al-Jubail industrial city (Saudi Arabia) were reported. The median of the concentrations of ƩOPFRs, ƩPesticides, ƩPFASs and ƩPPCPs in water was 297, 231, 29.7 and 3794 ng L−1, respectively, in sediments 56.2, 40.4, 5.66 and 419 ng g−1 d.w., in crops for human consumption of 45.6, 42.0, 0.46 and 42.0 ng g−1, in farm crops of 13.4, 57.5, 3.2 and 637 ng g−1, and in natural vegetation of 51.7, 10.3, 1.88 and 1580 ng g−1. Predominant compounds in all matrices were tris-(1,3-dichloro-2-propyl)phosphate (TClPP), acetamiprid, imidacloprid, caffeine, bisphenol A (BPA), diclofenac and ibuprofen. Tris(2-butoxyethyl) phosphate (TBEP), tris-(2-ethylhexyl)phosphate (TPhP), perfluoroctanoic acid (PFOA), perfluoroalkyl sulfonate (PFOS) and paracetamol were also in many samples but at low concentrations. The contaminants' levels showed similar values in both cities. However, pesticide levels were significantly higher in surface water (p < 0.05) and lower in natural vegetation (p < 0.05) of Riyadh than those of Al-Jubail. The risk assessment for the aquatic biota showed that abamectin, diazinon (pesticides), bisphenol A and caffeine (PPCPs) had the highest risk levels. The cumulative risk assessment showed that the contaminant mixture in all water samples is of concern. As far as the risk to human health is concerned, individual contaminants did not show a significant hazard for the population. However, OPFRs and pesticide requires a closed monitoring since % of admissible daily intakes (ADIs) or reference doses (RfD) are high. This is one of the most comprehensive study covering environmental and human risk assessment of emerging contaminants carried out in Saudi Arabia., The financial support from the project number (RSP-2021/11) King Saud University, Riyadh, Saudi Arabia.

Data obtained from wastewater analysis can provide rapid and complementary insights in illicit drug consumption at community level. Within Europe, Spain is an important country of transit of both cocaine and cannabis. The quantity of seized drugs and prevalence of their use rank Spain at the top of Europe. Hence, the implementation of a wastewater monitoring program at national level would help to get better understanding of spatial differences and trends in use of illicit drugs. In this study, a national wastewater campaign was performed for the first time to get more insight on the consumption of illicit drugs within Spain. The 13 Spanish cities monitored cover approximately 6 million inhabitants (12.8% of the Spanish population). Untreated wastewater samples were analyzed for urinary biomarkers of amphetamine, methamphetamine, MDMA, cocaine, and cannabis. In addition, weekend samples were monitored for 17 new psychoactive substances. Cannabis and cocaine are the most consumed drugs in Spain, but geographical variations showed, for instance, comparatively higher levels of methamphetamine in Barcelona and amphetamine in Bilbao, with about 1-fold higher consumption of these two substances in such metropolitan areas. For amphetamine, an enantiomeric profiling was performed in order to assure the results were due to consumption and not to illegal dumping of production residues. Furthermore, different correction factors for the excretion of cannabis were used to compare consumption estimations. All wastewater results were compared with previously reported data, national seizure data and general population survey data, were a reasonable agreement was found. Daily and yearly drug consumption were extrapolated to the entire Spanish population with due precautions because of the uncertainty associated. These data was further used to estimate the retail drug market, where for instance cocaine illicit consumption alone was calculated to contribute to 0.2–0.5% of the Spanish gross domestic product (ca. 3000–6000 million Euro/year)., This study was supported by MINECO/AEI projects (CTM2016-81935-REDT, CTM2017-84763-C3-2-R, CTM2017-84763-C3-1-R, CTM2017-84763-C3-3-R, RTI2018-097158-B-C31 and CTM2017-90890-REDT), MICINN project (CEX2018-000794-S), Galician Council of Culture, Education and Universities (ED481D-2017/003, ED431C-2017/36 and ED481A-2020/258), cofounded by FEDER/ERDF. The UJI and CIDE (CSIC-UV-GV) authors acknowledge the financial support of Generalitat Valenciana (Excellence Research Group, Prometeo 2019/040 and Prometeo 2018/150, respectively). IDAEA-CSIC authors acknowledge the financial support of Generalitat de Catalunya (Exp. Num. SA-2018-780 and Consolidated Research Group 2017 SGR 01404) and the Spanish Ministry of Science and Innovation (Project CEX2018-000794-S). Alberto Celma acknowledges the Spanish Ministry of Economy and Competitiveness for his predoctoral Grant (BES-2016-076914). Elena Pitarch acknowledge the financial support of University Jaume I of Castellón, Spain (project UJI-B2018-55). Andreu Rico is supported by a postdoctoral grant provided by the Spanish Ministry of Science, Innovation and University (IJCI–2017–33465).

In this study, water of the channels and ponds that conduct residual water in two most important cities of Saudi Arabia were assessed to ascertain the influence of the population on the occurrence and pollution characteristics of microplastics (MPs) (> 20 µm in size). Riyadh has 7.6 million inhabitants and is an urban city even though also have industry while Al-Jubail has only 0.78 and is the biggest industrial city. MPs showed an average of 3.2 items/L in Riyadh and 0.2 items/L in Al-Jubail showing a statistically significant difference between both cities. Sampling with a Turton Tow Net of 20 µm mesh, fibers were dominant in all sites (60%). MPs size was mainly distributed between 80 and 250 µm (60%), and their major colors were white (40%), red (25%) and blue (20%). Infrared spectral analysis revealed that most of the selected particles were identified as MPs of polypropylene and polyethylene (48.3%). The risk assessment was carried out using both the hazard index (HI) and the pollution load index (PLI). The results showed that, in this case, the decisive index is the PLI since the main difference in the MPs characteristics between the two cities is their concentration., The financial support from the project number (RSP-2020/11) King Saud University, Riyadh, Saudi Arabia.

Phthalates are widely used plasticizers that produce endocrine-disrupting disorders. Quantifying exposure is crucial to perform risk assessments and to develop proper health measures. Herein, a wastewater-based epidemiology approach has been applied to estimate human exposure to six of the mostly used phthalates within the Spanish population. Wastewater samples were collected over four weekdays from seventeen wastewater treatment plants serving thirteen cities and ca. 6 million people (12.8 % of the Spanish population). Phthalate metabolite loads in wastewater were transformed into metabolite concentrations in urine and into daily exposure levels to the parent phthalates. Considering all the sampled sites, population-weighted overall means of the estimated concentrations in urine varied between 0.7 ng/mL and 520 ng/mL. Very high levels, compared to human biomonitoring data, were estimated for monomethyl phthalate, metabolite of dimethyl phthalate. This, together with literature data pointing to other sources of this metabolite in sewage led to its exclusion for exposure assessments. For the remaining metabolites, estimated concentrations were closer to those found in urine. Their 4-days average exposure levels ranged from 2 to 1347 μg/(day∙inh), exceeding in some sites the daily exposure thresholds set for di-i-butyl phthalate and di-n-buthyl phthalate by the European Food Safety Authority., Financial support. This study was supported by MCIU/AEI (projects CTM2016-81935-REDT, CTM2017-84763-C3-1-R, CTM2017-84763-C3-2-R, CTM2017-84763-C3-3-R, and CEX2018-000794-S), Galician Council of Culture, Education and Universities (ED481D 2017/003 and ED431C2017/36), Generalitat Valenciana (projects Prometeo/2018/155 and Prometeo/2019/040) and Universitat Jaume I (project UJI-B2018-55). Several of the above mentioned projects are cofunded by FEDER/ERDF. Sampling, sample and data provision and/or analytical support: Viaqua and Concello de Santiago de Compostela, EMAYA (Palma), Jordi Palatsi from Aqualia (Lleida WWTP), Cristian Mesa and Angela Vidal from Aigues de Barcelona (Barcelona WWTP), Iñigo González (Consorcio de Aguas de Bilbao-Bizkaia), the Public Entity of Wastewater Treatment (EPSAR) of the Generalitat Valenciana and especially Fernando Llavador. Luis Aceiton, Enrique Albors, Angel Jiménez, Maria José Tarrega, Sonia Tristante and all the personal of the WWTPs (Aguas de Valencia, Spain), are acknowledged for their help with the sampling. Sociedad de Fomento Agrícola Castellonense (FACSA, Castellon), and especially WWTP operators Santiago Querol and Sara Gargallo are acknowledged for providing wastewater samples from Castellón, as well as Subdirección General de Gestión del Agua, Ayuntamiento de Madrid, for allowing the collection of samples from Madrid centro.

Within the last years aspects such as green, eco-friendly and sustainable are making their way into analytical chemistry. The field has changed with the introduction of these concepts. Information on the consumption of toxic solvents and energy is now a part of everyday life. This green analytical chemistry could be playing a pioneering role in the analysis of micro(nano)plastics in the environment. We discuss the roles of green analytical and sustainability within micro(nano) plastics determination and its possible applications. We explain its many advantages, like their function to preserve the environment and operator health or their role in the so-called eco-friendly methodologies, but we also highlight points such as an efficiency in the determination that should be viewed critically. Finally, we describe how micro(nano)plastics analysis is implementing the green analytical chemistry and the challenges faced., This work has been supported by Grant RTI2018-097158-B-C31 funded by MCIN/AEI/ 10.13039/501100011033 and by “ERDF A way of making Europe”, and project ANTROPOCEN@ (PROMETEO/2018/155) funded by Generalitat Valenciana.

From the issue entitled "Special Issue: Understanding effects of global change on water quantity and quality in river basins", INTRODUCTION: The Consolider-Ingenio 2010 project SCARCE, with the full title "Assessing and predicting effects on water quantity and quality in Iberian Rivers caused by global change" aims to examine and predict the relevance of global change on water availability, water quality, and ecosystem services in Mediterranean river basins of the Iberian Peninsula, as well as their socio-economic impacts. Starting in December 2009, it brought together a multidisciplinary team of 11 partner Spanish institutions, as well as the active involvement of water authorities, river basin managers, and other relevant agents as stakeholders. METHODS: The study areas are the Llobregat, Ebro, Jucar, and Guadalquivir river basins. These basins have been included in previous studies and projects, the majority of whom considered some of the aspects included in SCARCE but individually. Historical data will be used as a starting point of the project but also to obtain longer time series. The main added value of SCARCE project is the inclusion of scientific disciplines ranging from hydrology, geomorphology, ecology, chemistry, and ecotoxicology, to engineering, modeling, and economy, in an unprecedented effort in the Mediterranean area. The project performs data mining, field, and lab research as well as modeling and upscaling of the findings to apply them to the entire river basin. RESULTS: Scales ranging from the laboratory to river basins are addressed with the potential to help improve river basin management. The project emphasizes, thus, linking basic research and management practices in a single framework. In fact, one of the main objectives of SCARCE is to act as a bridge between the scientific and the management and to transform research results on management keys and tools for improving the River Basin Management Plans. Here, we outline the general structure of the project and the activities conducted within the ten Work Packages of SCARCE., This work has been supported by the Spanish Ministry of Science and Innovation through the project Consolider-Ingenio 2010 CSD2009-00065. Special thanks are due to all partners of the SCARCE consortium and the peer review panel for ensuring quality results and fruitful collaboration within the project.