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This work was funded by FEDER through COMPETE 2020 and national funds through Fundação para a Ciência e Tecnologia (FCT) by the research project WasteMAC (POCI-01- 0145-FEDER-028598). Thanks are also due to FCT/MCTES for the financial support to UIDP/50017/2020+UIDB/50017/2020, through national funds. Guilaine Jaria thanks to FCT for her PhD grant SFRH/BD/138388/2018. Vânia Calisto and Marta Otero are thankful to FCT for the Scientific Employment Stimulus Program (CEECIND/00007/2017) and Investigator Program (IF/00314/2015), respectively. María V. Gil acknowledges support from a Ramón y Cajal grant (RYC-2017-21937) of the Spanish government, co-financed by the European Social Fund (ESF).

This work was funded by FEDER through COMPETE 2020 and national funds through Fundação para a Ciência e a Tecnologia (FCT) by the research project POCI-01-0145-FEDER-028598. Guilaine Jaria, Marta Otero and Vânia Calisto thank FCT for the grant SFRH/BD/138388/2018, Investigator Program IF/00314/2015 and CEEC Program CEECIND/00007/2017, respectively. María V. Gil acknowledges support from a Ramón y Cajal grant (RYC-2017-21937) of the Spanish government.

This work is a contribution to the project WasteMAC (POCI-01-0145-FEDER-028598) funded by FCT – Fundação para a Ciência e a Tecnologia, I.P., through national funds, and the co-funding by the FEDER, within the PT2020 Partnership Agreement and Compete 2020. Thanks are also due for the financial support to CESAM (UID/AMB/50017/2019), to FCT/MEC through national funds, and the co-funding by the FEDER, within the PT2020 Partnership Agreement and Compete 2020. Vânia Calisto is funded by national funds (OE), through FCT, I.P., in the scope of the framework contract foreseen in the numbers 4, 5 and 6 of the article 23, of the Decree-Law 57/2016, of August 29, changed by Law 57/2017, of July 19. Guilaine Jaria and Marta Otero thank FCT for the grant SFRH/BD/138388/2018 and Investigator Program IF/00314/2015, respectively.

This work was funded by FEDER through COMPETE 2020 and national funds through Fundação para a Ciência e Tecnologia (FCT) by the research project RemPharm - PTDC/AAG-TEC/1762/2014. The authors also thank FCT for funding through a PhD grant (SFRH/BD/138388/2018), Investigator Program (IF/00314/2015) and CEEC Program (CEECIND/00007/2017). M.V. Gil acknowledges support from a Ramón y Cajal grant (RYC-2017-21937) of the Spanish government, co-financed by the European Social Fund (ESF).

In the aquatic environment, organisms are exposed to complex mixtures of contaminants which may alter the toxicity profile of each compound, compared to its toxicity alone. Pharmaceutical drugs (e.g. carbamazepine (CBZ) and cetirizine (CTZ)) and metals (e.g. cadmium (Cd)) are among those contaminants that co-occur in the environment. However, most studies concerning their toxicity towards aquatic species are based on single exposure experiments. Thus, the present study aimed to evaluate single and combined effects of Cd and CBZ or CTZ (single conditions: Cd, CTZ, CBZ; combined conditions: CTZ + Cd, CBZ + Cd) on biomarkers related to oxidative stress and energy metabolism in the edible clam Ruditapes philippinarum, by exposing the organisms for 28 days to environmentally relevant concentrations of these contaminants. The biomarkers studied were: i) the electron transport system activity, protein and glycogen contents (indicators of organisms’ metabolic status and energy reserves); ii) lipid peroxidation and the ratio between reduced and oxidized glutathione (indicators of oxidative stress); iii) superoxide dismutase and catalase activities (enzymes indicators of antioxidant defence) and iv) activity of glutathione S-transferases (family of enzymes indicators of biotransformation capacity). Results obtained showed that the uptake of Cd and CBZ was not affected by the combined presence of the contaminants. However, for CTZ, the uptake was higher in the presence than in the absence of Cd. Concerning toxicity data, in general, the combined exposures (CTZ + Cd, CBZ + Cd) had lower biological effects than the contaminants alone. Nevertheless, our data showed that despite the low concentrations tested, they were enough to exert biological effects that differed between single and combined treatments, evidencing the need to conduct more co-exposure studies to increase the environmental relevance of the gathered data. published

Emergent micropollutants have become a serious global problem with a large impact in the environment and human health, while their presence in aquatic systems has been registered as ranging from ng/L-1 to ug/L-1. Pharmaceuticals are ubiquitous micropollutants since their continuous consumption and consequent release via human excretions into aqueous systems are inevitable. Due to their usually low concentrations in aqueous samples, the development of a pre-concentration technique in order to continuously quantify and to monitor these components in aqueous streams is of major relevance. Aqueous biphasic systems (ABS) composed of ionic liquids (ILs) can be seen as more sustainable separation processes since they avoid the use of volatile and hazardous organic solvents (VOCs). As liquid-liquid systems, ABS can be used as extraction, purification and concentration platforms. Due to the outstanding tunable properties of ILs, IL-based ABS provide higher and more selective extraction efficiencies for a wide range of compounds when compared to traditional polymer-based ABS. IL-based ABS were already employed and adequately characterized for the extraction and concentration of endocrine disruptors, either from biological fluids or aqueous matrices. The aim of this work is to demonstrate the applicability of IL-based ABS to completely extract and concentrate, in one-step, two different and representative pharmaceutical pollution tracers, namely caffeine (CAF) and carbamazepine (CBZ). The low concentration of these persistent pollutants (usually found in ug/L-1 and ng/L-1 levels) does not allow a proper detection and quantification by conventional analytical equipment without a previous concentration step. However, pre-concentration methods commonly applied are costly, time-consuming, provide irregular recoveries and/or use VOCs. In this work, ABS composed of the IL tetrabutylammonium chloride ([N4444]Cl) and the salt K3C6H5O7 was investigated, demonstrating to be able to completely extract and concentrate CAF and CBZ in a single-step. Moreover, with this pre-treatment step it was demonstrated to be possible to overcome the detection limits of a high performance liquid chromatography coupled to an UV-Vis detector equipment. The results obtained demonstrate that IL-based ABS are versatile pre-concentration techniques, and can be used for the extraction and concentration of a large plethora of other micropollutants from environmental aqueous matrices. published

Pharmaceuticals are ubiquitous micropollutants due to their continuous consumption and consequent release via human excretions into aqueous systems. The low concentrations of these compounds in aqueous samples (from ng·L-1 to μg·L-1) results in the need of developing efficient pre-treatment/concentration techniques to accurately quantify and monitor these components in aqueous streams. As an alternative to the currently used concentration methods, mainly based on solid-phase extractions (SPE), liquid-liquid extraction based on aqueous biphasic systems (ABS) composed of ionic liquids (ILs) can be seen as more sustainable processes. In fact, ABS do not require the use of volatile and hazardous organic solvents (VOCs) typically employed in SPE and liquid-liquid extractions. Furthermore, the tunable properties of ILs are transferred to IL-based ABS, and high extraction efficiencies and selectivities have been reported for a wide range of compounds. In this work, we demonstrate the applicability of IL-based ABS for the concomitant extraction and concentration of several water pollution tracers, namely ethinylestradiol (EE2), caffeine, and carbamazepine, in which concentration factors up to 1000-fold have been gathered in a single-step. The increase in the concentration of pollution tracers from ng·L-1 to μg·L-1 allowed the use of high-performance liquid chromatography with fluorescence detection for their analysis/monitoring. published

Biochar produced by pyrolysis of organic residues is increasingly used for soil amendment and many other applications. However, analytical methods for its physical and chemical characterization are yet far from being specifically adapted, optimized and standardized. Therefore, the COST Action TD1107 conducted an inter-laboratory comparison, in which 22 laboratories from twelve countries analyzed three different types of biochar for 38 physical-chemical parameters (macro- and micro-elements, heavy metals, polycyclic aromatic hydrocarbons, pH, electrical conductivity, and specific surface area) with their preferential methods. The data was evaluated in detail using professional inter-laboratory testing software. Whereas intra-laboratory repeatability was generally good or at least acceptable, inter-laboratory reproducibility was mostly not (20% < mean reproducibility standard deviation < 460%). This paper contributes to better comparability of biochar data published already, and provides recommendations to improve and harmonize specific methods for biochar analysis in the future.

In the marine environment, organisms are exposed to a high and increasing number of different contaminants that can interact among them. In addition, abiotic factors can change the dynamics between contaminants and organisms, thus increasing or even decreasing the toxic effect of a particular compound. In this study, the effects of caffeine (CAF) and functionalized multi-walled carbon nanotubes (f-MWCNTs) induced in the clam Ruditapes philippinarum were evaluated, acting alone and in combination (MIX), under two temperature levels (18 and 21 °C). To assess the impact of such compounds, their interaction and the possible influence of temperature, biochemical and histopathological markers were investigated. The effects of f-MWCNTs and caffeine appear to be clearly negative at the control temperature, with lower protein content in contaminated clams and a significant decrease in their metabolism when both pollutants were acting in combination. Also, at control temperature, clams exposed to pollutants showed increased antioxidant capacity, especially when caffeine was acting alone, although cellular damages were still observed at CAF and f-MWCNTs treatments. Increased biotransformation capacity at 18 °C and MIX treatment may explain lower caffeine concentration observed. At increased temperature differences among treatments were not so evident as at 18 °C, with a similar biological pattern among contaminated and control clams. Higher caffeine accumulation at MIX treatment under warming conditions may result from clams’ inefficient biotransformation capacity when exposed to increased temperatures.

15 páginas.-- 2 figuras.-- 1 tablas.-- 42 referencias.-- Supporting Information The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.jafc.5b05055.-- Bachmann, Hans Jörg et al. (2016) Journal of Agricultural and Food Chemistry 64(2): 513–527, Biochar produced by pyrolysis of organic residues is increasingly used for soil amendment and many other applications. However, analytical methods for its physical and chemical characterization are yet far from being specifically adapted, optimized, and standardized. Therefore, COST Action TD1107 conducted an interlaboratory comparison in which 22 laboratories from 12 countries analyzed three different types of biochar for 38 physical–chemical parameters (macro- and microelements, heavy metals, polycyclic aromatic hydrocarbons, pH, electrical conductivity, and specific surface area) with their preferential methods. The data were evaluated in detail using professional interlaboratory testing software. Whereas intralaboratory repeatability was generally good or at least acceptable, interlaboratory reproducibility was mostly not (20% < mean reproducibility standard deviation < 460%). This paper contributes to better comparability of biochar data published already and provides recommendations to improve and harmonize specific methods for biochar analysis in the future., The biochar-producing companies Pyreg GmbH, Sonnenerde GmbH, and Swiss Biochar GmbH are acknowledged for sample donation. We are grateful to the IBI and the EBC for fruitful discussions about analytical method standardization. D.F., A.B., and A.G.R. thank the Universitàdi Bologna and Regione Emilia Romagna (Italy) APQ Ricerca Intervento a “Sostegno dello sviluppo dei Laboratori di ricerca nei campi della nautica e dell’energia per il Tecnopolo di Ravenna” and Denis Zannoni for laboratory assistance. F.Z. thanks the laboratory staff at the Institute of Soil Research, University of Natural Resources and Life Sciences (BOKU), Vienna, Austria., We thank the European Cooperation in Science and Technology (COST) for financial support