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The synthetic hormone 17α ethinyl estradiol (EE2) is a molecule widely used in female contraceptives and recognized as a contaminant of attention (Watch List) in the European Union due to its high consumption, endocrine effects and occurrence in aquatic environments. Its main source of introduction is domestic sewage where it can be associated with other contaminants such as microplastics (MPs). Due to their characteristics, they can combine with each other and exacerbate their isolated effects on biota. This study evaluated the combined effects of microplastics (MPs) and 17α ethinylestradiol (EE2) on two tropical estuarine invertebrate species: Crassostrea gasar and Ucides cordatus. Polyethylene particles were spiked with EE2 and organisms were exposed to three treatments, categorized into three groups: control group (C), virgin microplastics (MPs), and spiked microplastics with EE2 (MPEs). All treatments were evaluated after 3 and 7 days of exposure. Oysters exhibited changes in phase 2 enzymes and the antioxidant system, oxidative stress in the gills, and reduced lysosomal membrane stability after exposure to MPs and MPEs. Crabs exposed to MPs and MPEs after seven days showed changes in phase 1 enzymes in the gills and changes in phases 1 and 2 enzymes in the hepatopancreas, such as disturbed cellular health. The combined effects of microplastics and EE2 increased the toxicity experienced by organisms, which may trigger effects at higher levels of biological organization, leading to ecological disturbances in tropical coastal ecosystems.

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In November 2015, the Fundão Dam break released millions of tons of metal-rich tailings into the Doce River Basin (DRB), causing catastrophic damage and potential ecological effects that reached the Atlantic Ocean. This study aimed to evaluate the geochemistry and toxicity of water and sediments collected in the DRB from 2015 to 2019 and to determine the spatial and temporal trends. Water and sediment samples were analyzed for metals and As by inductively coupled plasma optical emission spectrometry (ICP-OES), and acute toxicity for Daphnia similis or D. magna. Results were explored using geochemical indices and correlation analyzes. Overall, higher concentrations of metals and As in water and sediments were observed immediately after dam breakage, but the levels exhibited a decreasing trend over time, although the levels of some elements such as As and Mn remained high in the upper DRB. The geochemical indices indicated mostly low to moderate contamination, and the enrichment factor (EF) demonstrated a higher enrichment of Mn in the upper DRB. Acute toxicity to water fleas (D. similis and D. magna) was occasionally observed in waters and sediments, but the reference samples were toxic, and the short-term effects were not correlated with metals and As. Overall, the results showed limited bioavailability of metals and As and a decreasing trend in their concentrations, indicating an ongoing recovery process in DRB. These results are important to decision-making regarding the disaster and actions for environmental restoration.

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Marine Protected Areas (MPAs) are designed to conserve biodiversity and vulnerable ecosystems. This study aimed to assess the environmental quality of three Brazilian MPAs, based on the integrated analysis of biomarkers in pufferfish. The MPAs are differentiated by the degree of anthropogenic influences. The Barra do Una Estuary sustainable reserve (JUR) is a reference area due to its low levels of contamination and species diversity. The Cananéia Estuarine System (CAN) has been recognized as a biosphere reserve by UNESCO, as well as a Ramsar wetland. This MPA was influenced by upstream mining activities, resulting in the introduction of metals in the estuarine waters and the discharge of untreated urban sewage. The São Vicente estuary (SSV) lacks proper sanitation infrastructure. All collections were conducted during winter season, and, after collection, the animals were euthanized, their soft tissues were removed, and multiple biomarkers were analyzed in the gills and liver, as biometric, genotoxic, biochemical, and morphological. A one-factor multivariate analysis was applied to evaluate the differences between the data sets, and the matrices were analyzed using PERMANOVA to evaluate the "estuary" factor. The results were integrated using PCA with a 0.4 cut value and an Enhanced Integrated Biomarker Response (EIBR) was calculated. PCA was correlated with biochemical, genotoxic, and morphological biomarkers. In general, SVV differed from CAN and JUR as shown by both univariate and multivariate analyses. SVV also showed the highest EIBR, followed by CAN. Organisms from SSV showed greater gill pathology, elevated AChE activity and lipoperoxidation (LPO), and micronuclei frequency. CAN present intermediate EIBR, with severe pathologies in the liver. CAN seems to present an intermediate environmental quality between SSV and JUR indicating the importance of the existence of MPAs for environmental conservation and the need to monitor such areas, to maintain their suitable environmental quality.

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The most extensive oil spill ever recorded in tropical oceans occurred between August 2019 and March 2020, affecting approximately 3000 km of the Brazilian coast. This study assessed the chemical contamination and toxicity of sediments collected from affected reef areas during two sampling surveys conducted 17 and 24 months after the peak of oil slick inputs. Our results indicated that neither PAH levels nor measured toxicity showed a significant contribution from the spilled oil, with concentrations and biological effects indistinguishable from those in unaffected areas. Similarly, no differences were observed between seasons. Furthermore, there was no discernible relationship between sediment toxicity results and the measured PAH concentrations. Therefore, while biological responses indicated toxicity in most assessed areas, these responses are likely related to other local sources. This evidence suggests a natural oil attenuation process contributing to local environmental recovery. Nonetheless, further investigation is needed for other areas affected by oil spills.

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Biocides used in antifouling (AF) paints, such as 4,5-dichlorine-2-n-octyl-4-isothiazole-3-one (DCOIT), can gradually leach into the environment. Some AF compounds can persist in the marine environment and cause harmful effects to non-target organisms. Nanoengineered materials, such as mesoporous silica nanocapsules (SiNCs) containing AF compounds, have been developed to control their release rate and reduce their toxicity to aquatic organisms. This study aimed to evaluate the acute toxicity of new nanoengineered materials, SiNC-DCOIT and a silver-coated form (SiNC-DCOIT-Ag), as well as the free form of DCOIT and empty nanocapsules (SiNCs), on the sun coral Tubastraea coccinea. T. coccinea is an invasive species and can be an alternative test organism for evaluating the risks to native species, as most native corals are currently threatened. The colonies were collected from the Alcatrazes Archipelago, SP, Brazil, and acclimatized to laboratory conditions. They were exposed for 96 h to different concentrations of the tested substances: 3.33, 10, 33, and 100 µg L-1 of free DCOIT; 500, 1000, 2000, and 4000 µg L-1 of SiNC; and 74.1, 222.2, 666.7, and 2000 µg L-1 of SiNC-DCOIT and SiNC-DCOIT-Ag. The test chambers consisted of 500 mL flasks containing the test solutions, and the tests were maintained under constant aeration, a constant temperature of 23 ± 2 °C, and photoperiod of 12 h:12 h (light/dark). At the end of the experiments, no lethal effect was observed; however, some sublethal effects were noticeable, such as the exposure of the skeleton in most of the concentrations and replicates, except for the controls, and embrittlement at higher concentrations. Adults of T. coccinea were considered slightly sensitive to the tested substances. This resistance may indicate a greater capacity for proliferation in the species, which is favored in substrates containing antifouling paints, to the detriment of the native species.

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Sedimentary aliphatic hydrocarbons and polycyclic aromatic hydrocarbons (PAHs) were studied in subtropical estuaries with distinct degrees of legal protection, located in the Southwestern Atlantic Ocean, São Paulo State, Brazil. A multivariate approach was adopted, using the Hierarchical cluster analysis followed by the Principal Matrix Factorization analysis to support the hydrocarbons sources findings using diagnostic ratios. In general, the sites with the highest values of hydrocarbons were in the vicinity of well-urbanized cities, where sewage discharge, harbor and industrial activities take place. Pyrolitic PAHs were the predominant source of PAHs in the sites. The region can be considered not highly contaminated by hydrocarbons; however, specific sites under local anthropogenic impact from sewage and/or urban drainage, presented relatively high hydrocarbons levels. These findings highlight the importance of sources identification as reliable approach to be included in the management plan of protected areas under the inputs of several vectors of contamination.

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Glitter particles are considered a model of microplastics, which are used in a wide range of products. In this study, we evaluated the toxicity of two types of glitter (green and white, with distinct chemical compositions) dispersions on the embryonic development of the sea urchins Echinometra lucunte, Arbacia lixula, and the mussel Perna perna. The Toxicity Identification and Evaluation (TIE) approach was used to identify possible chemicals related to toxicity. Glitter dispersions were prepared using 0.05% ethanol. The tested dispersions ranged from 50 to 500 mg/L. The white glitter was composed of a vinyl chloride-methyl acrylate copolymer. The effective concentrations of green glitter to 50% embryos (EC50) were 246.1 (235.8-256.4) mg/L to A. lixula, 23.0 (20.2-25.8) mg/L to P. perna and 105.9 (61.2-150.2) mg/L, whereas the EC50 of white glitter to E. lucunter was 272.2 (261.5-282.9) mg/L. The EC50 for P. perna could not be calculated; however, the lowest effect concentration was 10 mg/L-that was the lowest concentration tested. The filtered suspension of green glitter had Ag levels exceeding the legal standards for marine waters. TIE showed that metals, volatiles, and oxidant compounds contribute to toxicity. The results showed that glitter may adversely affect marine organisms; however, further studies are necessary to determine its environmental risks.

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This study aimed to evaluate B[a]P and low-density polyethylene microplastics (MPs) toxicty, alone and in mixture (0.03 to 30 µg L-1 of B[a]P; and 5, 50 and 500 mg L-1 for MPs). Five mg L-1 of MPs is considerably higher than commonly reported environmental concentrations, although it has been reported for marine environments. Individual (sea urchin embryo-larval development and mortality of mysids) and sub-individual responses (LPO and DNA damage in mysids) were assessed. The toxicity increased as the B[a]P concentration increased, and microplastics alone did not cause toxicity. B[a]P toxicity was not modified by the lowest concentration of MPs (5 mg L-1), but at higher MPs concentrations (50 and 500 mg L-1), the effects of B[a]P on sea urchin development and in biomarkers in mysids were diminished. Microplastics interacted with B[a]P in seawater, reducing its toxicity, probably due to adsorption of B[a]P to the surface of microplastics.

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Organotin-based (OTs: TBT and TPT) antifouling paints have been banned worldwide, but recent inputs have been detected in tropical coastal areas. However, there is a lack of studies evaluating the toxicity of both legacy and their substitute antifouling booster biocides (e.g., Irgarol and diuron) on neotropical species. Therefore, the acute toxicity of four antifouling biocides (TBT, TPT, Irgarol, and diuron) was investigated using the marine planktonic organisms Acartia tonsa and Mysidopsis juniae, the estuarine tanaid Monokalliapseudes schubarti (water exposure), and the burrowing amphipod Tiburonella viscana (spiked sediment exposure). Results confirmed the high toxicity of the OTs, especially to planktonic species, being about two orders of magnitude higher than Irgarol and diuron. Toxic effects of antifouling compounds were observed at levels currently found in tropical coastal zones, representing a threat to planktonic and benthic invertebrates. Furthermore, deterministic PNECmarine sediment values suggest that environmental hazards in tropical regions may be higher due to the higher sensitivity of tropical organisms. Since regulations on antifouling biocides are still restricted to a few countries, more ecotoxicological studies are needed to derivate environmental quality standards based on realistic scenarios. The present study brings essential contributions regarding the ecological risks of these substances in tropical and subtropical zones.

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We analyzed per- and polyfluoroalkyl substances (PFAS) in aqueous film-forming foams (AFFFs) used to extinguish a major fire in a petrochemical terminal from the Port of Santos (Brazil). Eight AFFFs from seven known commercial brands and one unknown sample (AFFF-1 to AFFF-8) were evaluated. 17 PFAS were identified and quantified using high performance liquid chromatography (LC/MS). The concentrations of Σ17 PFAS in the AFFFs ranged from 500 to 9000 ng/g, with prevalence of short chain PFAS (~85 %), followed by long chain PFAS. Perfluorooctane sulfonic acid (PFOS) and perfluorooctanoic acid (PFOA), included in the global treaty of the Stockholm Convention, were also detected. We estimated that at least 635.96 g of PFAS were introduced in the estuary, representing a massive input of these substances. This investigation reports the PFAS composition of AFFFs used in firefighting in the GRULAC Region (Group of Latin American and Caribbean countries).

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The gastrointestinal tract and its enteric nervous system are the first routes of food and xenobiotics uptake. Considering the importance of this organ, this study evaluated intestinal biomarkers of Sphoeroides testudineus integrating the data to generate tools for pollution assessment. The fish were collected in three sites of São Paulo Coast and their intestines were analyzed for biochemical, histology, and neuronal density and morphometry biomarkers. To evaluate the differences among the data, a PERMANOVA was applied, followed by a FA/PCA. The PERMANOVA indicated differences (P < 0.001) between the regions (RA, A1, and A2). Four factors were extracted from the FA/PCA (62% cumulative), showing that the animals from A2 presented severe alterations, mainly in intestinal morphometry and neuronal density. A1 alterations refer mainly to the increase of neuronal metabolism. Our results also evidence a gradient of environmental quality related to the protection level (AR > A1 > A2).

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Methods to assess the effects of contaminants on marine organisms typically involve euthanasia to obtain samples, but less invasive techniques may be more appropriate for working with threatened species. In this study, were assessed the biological responses of crabs exposed to microplastics and contaminants of emerging concern. Biochemical and cellular effects (lipid peroxidation, DNA damage, cholinesterase activity, and lysosomal membrane stability) in hemolymph were analyzed in a kinetic study, at 3 and 7 days, in U. cordatus exposed to microplastics spiked with Triclosan (TCS) or 17α-Ethynylestradiol (EE2). The results showed that the contaminants were produced toxic effects in the crabs exposed either to the microplastics alone (oxidative stress, genotoxicity, and neurotoxicity), or to microplastics with TCS or EE2 adsorbed (neurotoxic and cytotoxic). The present study showed the responsiveness of non-lethal analyzes to understanding the biological effects of combined exposure to microplastics and chemical pollution.

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Recent advances in nanotechnology have allowed the encapsulation of hazardous antifouling (AF) biocides in silica mesoporous nanocapsules (SiNC) reducing their short-term toxicity. However, the chronic effects of such novel nanoadditives remain understudied. The present study aimed to assess short- and long-term sub-lethal effects of soluble forms (DCOIT and Ag) and nanostructured forms (SiNC-DCOIT and SiNC-DCOIT-Ag) of two AF biocides and the "empty" nanocapsule (SiNC) on juveniles of Crassostrea gigas after 96 h and 14 days of exposure. Juvenile oysters exposed for a short period to free DCOIT and AgNO3 presented worse physiological status comparing with those exposed to the nanostructured forms. The long-term exposure to DCOIT and Ag+ caused an extensive biochemical impairment comparing with the tested nanomaterials, which included oxidative damage, activation of the antioxidant defense system, and neurotransmission impairment. Despite the negative effects mostly observed on the health condition index and AChE, the encapsulation of the abovementioned AF biocides into SiNC seems to be a technological advantage towards the development of AF nanoadditives with lower long-term toxicity comparing with the soluble forms of such biocides.

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This study investigated the sublethal effects of environmentally relevant concentrations of DCOIT on the neotropical oyster Crassostrea brasiliana. Gills and digestive glands of animals exposed to increasing concentrations of DCOIT were analyzed for biochemical, cellular, and histopathological responses. Exposure to DCOIT (0.2 to 151 µg L-1) for 120 h triggered oxidative stress in both tissues (through the modulation of GPX, GST, GSH and GR), which led to damage of membrane lipids (increase of LPO and reduction of the NRRT). DCOIT increased histopathological pathologies in gills, such as necrosis, lymphocyte infiltration and epithelial desquamation. This study showed that short term exposure to environmental concentrations of DCOIT causes negative effects on C. brasiliana at biochemical, physiological, and histological levels. Therefore, the use of DCOIT as a booster biocide in antifouling paints should be further assessed, as it may cause environmental hazards to marine organisms.

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Cocaine (COC) is a powerful illicit drug frequently detected in the aquatic environment. COC acts by inhibiting the reuptake of dopamine (DOPA) and 5-hydroxytryptamine (5-HT - serotonin) and causes endocrine disturbances in mammals. This study investigated similar effects from cocaine exposure in the marine mussel Perna perna, as well as neurotoxicity and energy imbalances. Mussels were exposed to COC (0.2 µg.L-1 and 2 µg.L-1) for periods of 48, 96, and 168 h. Acetylcholinesterase (AChE) was measured in adductor muscle tissue to determine neurotoxicity, and neurotransmitter levels (DOPA and 5-HT), monoamine oxidase (MAO) and cyclooxygenase (COX) activity, and energy status (mitrochondrial electron transport, MET, and total lipids, TLP) were evaluated in the mussels' gonads. COC decreased AChE activity in the mussels exposed to 0.2 µg.L-1 and 2 µg.L -1 after 168 h, and all concentrations of COC increased neurotransmitter levels. Increases in MET (0.2 µg.L -1, for all exposure periods) and TLP (0.2 µg.L 1 after 48 h, and 2 µg.L -1 after 96 h and 168 h) were also observed. No significant change was detected in MAO activity. COC also decreased COX activity in the mussels exposed to 0.2 µg.L -1 (48 h and 96 h) and 2 µg.L -1 (96 h). These results suggest that COC may compromise neurotransmitter levels and COX activity. Furthermore, the changes in MET and LPT suggest that COC affects the energy balance of the mussels, and could negatively affect physiological processes such as metabolism, hormone production, and embryonic development.

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Accidents involving fuels and oil spills are among the main sources of hydrocarbons to the marine ecosystems and often damage the biota. Diesel and bunker oil are two examples of fuels with broad application that release hydrocarbons to the aquatic environment and little is known about their toxicity on tropical organisms. This study aimed to assess the toxicity of the water-soluble fraction (WSF) of diesel and bunker oils to neotropical marine invertebrates. Commercial fuels were purchased for WSF extraction, analyzed for total petroleum hydrocarbons (TPH), and polycyclic aromatic hydrocarbons (PAHs), and acute and chronic toxicity determined. The WSF analyzed contained varied levels of TPH and PAHs mixtures, especially low molecular weight PAHs; bunker WSF presented higher amounts of TPH and PAHs. Both WSFs tested produced significant mortality of the brine shrimp Artemia salina, affected the reproduction rate of the copepod Nitokra sp, and impaired the embryo-larval development of the mussel Perna perna and of the sea urchin Lytechinus variegatus. In general WSF from diesel was more toxic to the organisms tested, but bunker WSF was more toxic to embryos of L. variegatus. Toxicity started from concentrations of 3% WSF, which can be environmentally relevant after an oil spill, indicating that marine biota may be adversely affected in short term.

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Recent studies have shown that the effectiveness of establishing Marine Protected Areas (MPAs) is threatened by toxic effects of contaminants. São Paulo is the most economically developed state of Brazil, and its coast is protected by a system of MPAs, including the North Shore Marine Protected Area (NSMPA). The present study provides a first assessment of sediment quality in NSMPA and two reference sites. Concentrations of arsenic (As), metals (Al, Fe, Cd, Cr, Cu, Ni, Pb, and Zn) and polycyclic aromatic hydrocarbons (PAHs) and its sources were determined. Comparisons with sediment quality guidelines indicated low contamination, as confirmed by the Geoaccumulation Index, which classified the results as background levels. Whole-sediment exposures of the amphipod Tiburonella viscana were performed to estimate possible acute effects, but samples exhibited no toxicity. The results presented in this study represent a baseline for further monitoring programs of MPAs, supporting conservation actions of management plans.

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Fire suppression agents are recommended for extinguishing fires by flammable liquids and frequently end in water bodies, combined with the fuels. There is a lack of toxicity information on these commercial formulations and the effects of mixtures of fire suppression agents and fuels. The aim of the present study was to evaluate the toxic effects of different fire suppression agents, the gasoline water-soluble fraction (GWSF), and mixtures of each fire suppression agent and GWSF. Individual tests were performed with Daphnia similis and Artemia sp.; the most toxic fire suppression agents to D. similis and Artemia sp. were F-500®, Cold Fire®, Agefoam®, and Kidde Sintex® 1%; the GWSF was the least toxic. The concentration addition model was used to predict the mixture effects and evaluate synergism/antagonism, dose ratio dependence, and dose level dependence. Cold Fire with GWSF showed dose level deviation to D. similis, marked mainly by synergism; for Artemia sp., the dose ratio pattern was predicted, with a synergistic response mainly by Cold Fire. Agefoam and GWSF behaved additively for D. similis and dose ratio for Artemia sp., with synergism being caused by Agefoam. Kidde Sintex 1% with GWSF were dose ratio for both organisms, with Kidde Sintex 1% being responsible for synergism. Our results show that some mixtures of fire suppression agents and GWSF may cause toxicity to aquatic organisms, posing risk in a real environmental scenario, such as a major fire combat. Environ Toxicol Chem 2021;40:767-779. © 2020 SETAC.

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Sediment dredging impacts coastal environments by promoting the resuspension of fine particles and remobilization of contaminants that may trigger toxic effects. In this study, we evaluated the sediment quality in harbor areas of Mucuripe bay, a semi-arid ecosystem located in Ceará state (Brazil), which is subject to dredging activities. A sampling survey was conducted right after dredging operations and data compared to another survey performed prior dredging. Sediments were analyzed for fine particles, organic carbon, nutrients, metals, hydrocarbons, and tributyltin (TBT). Toxicity of whole-sediment and liquid phase exposures were also determined. The concentrations of Cd, Cr, Cu, and Zn decreased after dredging, which was confirmed by the geoaccumulation index. Levels of TBT dropped while phosphorus, aliphatic and polycyclic aromatic hydrocarbons increased. Toxic effects persisted, indicating a post-dredging recontamination combined with other sources such as urban runoff, wastewater discharges, harbor activities, and antifouling particles. Data from Mucuripe and Pecém harbors were compiled and site-specific sediment quality values (SQVs) were developed by using multivariate methods. The threshold values proposed by our study were lower and more effective to predict toxicity compared to international guidelines, indicating levels of contamination for this tropical region in which toxic effects may occur. Considering the large geographic area with different sediment characteristics of the Brazilian coast, this study represents a significant contribution to sediment toxicity assessment of dredging activities in semi-arid environments.

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