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Anthropogenic debris, particularly plastic pollution, has emerged as a significant environmental threat to biodiversity. Given that seabirds interact with artificial debris through ingestion, entanglement, and nest incorporation, it is particularly important to quantify the quantity, origins, and chemical composition of these debris items. In this work, it was evaluated for the first time the occurrence of anthropogenic debris in nests of yellow-legged gull (Larus michahellis atlantis) in biosphere reserves of the Canary Islands (Spain). A total of 48 abandoned nests were collected from five remote and hardly accessible sampling areas, revealing that 81.3 % contained anthropogenic waste, with plastic accounting for 34.7 % of the debris, followed by metal (33.6 %) and paper (19.6 %). On average, 32.8 ± 40.9 items were found per nest. Regarding the origin, food packagings (47.8 %), personal hygiene products (21.7 %), and textiles (15.8 %) were identified as the predominant sources. Furthermore, the polymer composition of the plastics was characterised by means of Fourier-transform infrared spectroscopy analysis, being polyester the most abundant (38.2 %), followed by polyethylene (25.6 %) and rayon (10.3 %). The incorporation of anthropogenic debris into nest construction may result from outdoor human activities carried out far from nesting areas.
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Charadriiformes , Monitoramento Ambiental , Plásticos , Resíduos , Espanha , Animais , Resíduos/análise , Plásticos/análise , Poluição Ambiental/estatística & dados numéricos , Poluentes Ambientais/análise , Comportamento de NidaçãoRESUMO
BACKGROUND: Current trends in Analytical Chemistry are highly focused on the introduction of new extraction materials with a high selectivity towards the target analytes, high extraction capacity as well as sustainable characteristics. In this context, the introduction of smart materials able to respond to an external stimulus constitutes a promising approach in the field. However, investigations regarding the development of such stimuli-responsive polymers have been basically centered on their synthesis and the control of their properties, and hardly on exploiting such properties to generate polymers that, once their extraction function is fulfilled, they can be degraded into fragments with little or negligible toxicity, or even into their constituent monomers for an efficient recycling. RESULTS: The applicability of a degradable and recyclable dynamic covalent polymer based on the use of tetrazine as a linker was assessed as sorbent for the extraction of a group of 37 persistent organic pollutants, including 10 polycyclic aromatic hydrocarbons, 11 organochlorine pesticides, 14 polychlorinated biphenyls, and 2 antibacterial agents, from water samples. A microdispersive solid-phase extraction procedure was developed for the selective extraction of the target analytes, while their separation, determination, and quantification were achieved by gas chromatography coupled to mass spectrometry. The optimized procedure was validated for seawater and wastewater obtaining mean relative recovery values between 72 and 112 % for almost all the analytes, with satisfactory relative standard deviation values (<18 %). After extraction, the polymer could be degraded by adding the amino acid L-tyrosine, being possible a quantitative recovery of the initial functional monomer. SIGNIFICANCE: A responsive polymer based on the chemical versatility of the tetrazine ring was used as sorbent in sample preparation providing excellent results, showing good physicochemical properties and the ability to be degraded after use. This polymer constitutes an interesting alternative to reduce chemical waste through the recycling of monomers, contributing to the development of more sustainable analytical methodologies.
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Plastic pollution poses a significant threat to marine ecosystems. Microfibres from fabrics have become the most prevalent shape of microplastic found in the marine environment. The northern krill (Meganyctiphanes norvegica) is the most abundant euphausiid species in the northern hemisphere, playing a crucial role in various pelagic ecosystems. Anthropogenic microparticles in northern krill was assessed for the first time in samples collected in the Azores on two occasions - April 2019 (n = 480) and April 2023 (n = 480). Analysis of all individuals revealed 533 anthropogenic particles, with an average abundance of 0.56 ± 0.14 items per individual and, no significant differences between years. Microfibres were the most common shape (94.8 %), with the remaining items being fragments (5.2 %), and blue and black were the predominant colours. MicroFourier transform infrared spectroscopy analysis (µFTIR) of 22.1 % of the total number of particles, showed that they were mainly cellulosic (65.3 %) - either natural or semisynthetic - followed by polyester (7.6 %). Our finding of microplastics in the northern krill raises important questions due to its crucial role in marine food webs. The intake of anthropogenic particles, particularly those that are 100 % synthetic, suggests that the northern krill may act as a transfer vector of these pollutants to higher trophic levels.
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Euphausiacea , Cadeia Alimentar , Animais , Açores , Poluentes Químicos da Água/análise , Microplásticos/análise , Monitoramento AmbientalRESUMO
The surging global demand for fish has increased aquaculture practices, where antibiotics have become indispensable to prevent diseases. However, the passive incorporation of these compounds into the diet may have adverse effects on human health. In this work, the QuEChERS method combined with ultra-high-performance liquid chromatography tandem mass spectrometry was applied for the determination of 10 multiclass antibiotics (5 quinolones, 2 sulfonamides, 2 diaminopyrimidines, and 1 macrolide) in muscle tissue of farmed fish (European sea bass and gilt-head sea bream). The applied method demonstrated acceptable recovery values, mostly between 70 and 120%, with limits of quantification of the method meeting the established EU maximum residue limits. The analysis of twenty fish samples in duplicate revealed that most antibiotics were not present, with the only exception of oxolinic acid and tilmicosin in European sea bass, which were below the limit of quantification of the method.
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The potential of using organisms as bioindicators of marine litter has been an area of general interest in multiple scientific and monitoring programs across the globe. Procellariiformes seabirds are particularly vulnerable to plastic contamination, which makes them a research focus group. This study investigated plastic ingestion in deceased fledglings and adults Cory's shearwaters (Calonectris borealis) collected over eight years (2015 to 2022) at two Atlantic archipelagos: the Azores and the Canaries. Necropsies were carried out in a total of 1,238 individuals showing a high prevalence of plastic ingestion (90%), with approximately 80% of items recovered from the gizzard. Fledglings carried greater plastic loads compared to adults, yet plastic morphologies were similar between both age classes. The temporal analyses conducted with generalised additive mixed-effect models revealed a distinct temporal trend in plastic numbers, but not in terms of plastic mass. In addition, the spatial analyses showed that Cory's shearwaters from the Canary Islands ingest a higher quantity of plastic and a greater proportion of threadlike items than the Azorean birds. These results suggest higher contamination at the NW Africa foraging grounds next to the Canaries and highlight fisheries as a potential source of marine litter in that region. On the other hand, the information gathered from the Azorean birds suggests they would be able to monitor changes in the composition of the plastic items floating in the North Atlantic Subtropical Gyre. Overall, our outcomes support the use of Cory's shearwater fledglings that are victims of light pollution as a key bioindicator of plastic contamination in the North Atlantic. For its policy application, the presented threshold value in combination with the assessment method will enable effective tracking of floating plastic litter in the framework of the MSFD and OSPAR.
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Aves , Monitoramento Ambiental , Plásticos , Animais , Plásticos/análise , Monitoramento Ambiental/métodos , Poluentes Químicos da Água/análise , AçoresRESUMO
Microplastic (MPs) pollution is a current global concern that is affecting all environmental compartments and food sources. In this work, anthropogenic particles occurrence (MPs and natural and synthetic cellulosic particles), have been determined in 73 beverages packed in different containers. Overall, 1521 anthropogenic particles were found, being the lowest occurrence in water samples (7.2 ± 10.1 items·L-1) while beer had the highest (95.5 ± 91.8 items·L-1). Colourless/white particles were the most detected followed by blue and red colours. The highest mean size was 783 ± 715 µm in soft drinks. Cellulosic, both natural and semisynthetic particles, were the composition mostly found but regarding plastic polymers, it was polyester. Phenoxy resin particles from the can coatings were also identified in all metal containers which indicates that leaching from the packaging may be happening. The total estimated daily intake were 0.077 and 0.159 items·kg-1 body weight (b.w.)·day-1 for children and adult population, respectively.
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Plásticos , Poluentes Químicos da Água , Criança , Humanos , Poluentes Químicos da Água/análise , Monitoramento Ambiental , Microplásticos , Bebidas GaseificadasRESUMO
BACKGROUND: Microplastics have the capability of retaining contaminants on their surface, increasing their persistence, preconcentrating them, and acting as transport vectors. Nevertheless, the determination of these compounds in plastic matrices poses several analytical issues and challenges, including the capability of many of these methods of only determining the extractable pollutants fractions, repeatability issues, etc. In this sense, it is primordial to evaluate the effect of the critical parameters that allow to obtain a quantitative extraction of the target analytes from microplastics, including the matrix effect of each of the studied polymers, the influence of particle size, and the effect of weathering. RESULTS: A simple and effective methodology for the extraction of 17 emerging organic pollutants from both pristine (polypropylene, polystyrene, and low- and high-density polyethylene) and weathered (polypropylene and polyethylene) microplastics has been developed, optimized, and validated, achieving recovery values of 70-120 % and low method quantification limits (9.2-35.5 ng/g). Results show the importance of cryomilling microplastics (as smaller particle sizes improve recovery and homogenization), something ignored in most publications. The differences in matrix effect for the studied pristine polymers highlights the importance of treating polymers individually, without extrapolating results. In weathered microplastics, matrix effect is overall higher than in their pristine counterparts, evidencing the necessity of always carrying out matrix effect and recovery studies in environmental microplastics. The analysis of 10 samples collected in Playa Grande (Tenerife, Canary Islands, Spain) revealed quantitative amounts of bisphenol A (10.8 ± 3.4 ng/g) in one of them. SIGNIFICANCE: For the first time, the effect of particle size, weathering and matrix effect have been simultaneously evaluated on microplastics, revealing the importance of their assessment to properly validate the methodology. Additionally, the method shows good performance in all the different polymers and has been successfully applied to the analysis of environmental samples of microplastics.
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Marine ecosystems pollution by microplastics (MPs) is a global problem of special concern. The present study examines the prevalence and distribution of MPs and cellulosic particles in sublittoral coastal sediments of the Canary Islands archipelago (Spain). At twenty-six different locations alongside seven islands, three samples were taken parallel to the shoreline between 1 and 10 m depth (n = 78). Sediment samples were primarily digested with a H2O2 solution followed by four flotations in a saturated NaCl solution. The mean concentration obtained was 3.9 ± 1.6 items/g of dry weight. A similar distribution pattern was observed across all islands concerning particles morphology, color, size and composition: mainly colorless/translucent and blue fibers (60.0%). Additionally, fragments were also found, and to a much lesser extent microbeads, films and tangled messes. MicroFourier Transform Infrared spectroscopy analysis of 12.5% of the fibers, showed that they were mainly cellulosic (54.5%) -either natural or semisynthetic- followed by polyester (22.7%) and acrylic (4.5%). The potential correlation between particle distribution in nearshore sediments and wave intensity was also explored. This work provides the first comprehensive report on the current MPs content of the seabed of the region.
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Despite the isolation of remote natural regions, it has been discovered that they are experiencing the accumulation of anthropogenic microparticles (i.e., microplastics or natural or semisynthetic cellulosic particles). Teide National Park (Canary Islands, Spain) is a high-mountain protected area known for its rich biodiversity. This study aims to assess the occurrence of coloured anthropogenic particles in the faecal matter of wild mammals, specifically rabbits and mouflons, residing in the park. With this purpose, faeces were collected from 68 systematically distributed sampling points. A stereomicroscopy-guided grinding process allowed a chemical-free and quick visual inspection of 616 individual excreta, revealing that 96% were particle-free. However, 37 anthropogenic particles were found, which correspond to 0.79 ± 0.20 items per gram of dry faecal matter. The archetypical particle was a cellulosic blue microfibre of 2721 ± 407 µm, though poly(ethylene-vinyl acetate) and polypropylene were also identified via micro Fourier-transform infrared spectroscopic analysis. Atmospheric deposition and touristic pressure may be the sources of the anthropogenic particles, as they were randomly found in 36% of the sampling points. These findings represent the first evidence of anthropogenic particle ingestion by wild rabbits and mouflons, signifying the introduction of microplastics into terrestrial food chains in a remote high-mountain environment.
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Plásticos , Poluentes Químicos da Água , Animais , Coelhos , Microplásticos , Animais Selvagens , Carneiro Doméstico , Monitoramento Ambiental , Poluentes Químicos da Água/análise , EcossistemaRESUMO
Gas chromatography (GC) tandem mass spectrometry (MS/MS) stands as a preeminent analytical instrument extensively employed for the surveillance of pesticide residues in food. Nevertheless, these methods are vulnerable to matrix effects (MEs), which can potentially affect accurate quantification depending on the specific combination of analyte and matrix. Among the various strategies to mitigate MEs, matrix-matched calibration represents the prevailing approach in pesticide residue applications due to its cost-effectiveness and straightforward implementation. In this study, a total of 45 representative pesticides were analyzed in three different varieties of avocado (i.e., Criollo, Hass, and Lorena) using the Quick-Easy-Cheap-Effective-Rugged-Safe (QuEChERS) method with ammonium formate and GC-MS/MS. For this purpose, 5 g of the avocado sample was extracted with 10 mL of acetonitrile, and then 2.5 g of ammonium formate was added to induce phase separation. Subsequently, the supernatant underwent a cleanup process via dispersive solid-phase extraction employing 150 mg of anhydrous MgSO4, 50 mg of primary-secondary amine, 50 mg of octadecylsilane, 10 mg of graphitized carbon black, and 60 mg of a zirconium oxide-based sorbent (Z-Sep+). The GC-MS/MS analysis was successfully performed in less than 25 min. Rigorous validation experiments were carried out to assess the performance of the method. The examination of a matrix-matched calibration curve for each variety of avocado revealed that the ME remained relatively consistent and less than 20% (considered as a soft ME) for most pesticide/variety combinations. Furthermore, the method´s limits of quantification were lower than 5 µg/kg for all three varieties. Finally, the recovery values for most pesticides fell within the acceptable range of 70-120%, with relative standard deviation values below 20%.
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Persea , Resíduos de Praguicidas , Praguicidas , Praguicidas/análise , Cromatografia Gasosa-Espectrometria de Massas/métodos , Espectrometria de Massas em Tandem/métodos , Persea/química , Resíduos de Praguicidas/análise , Extração em Fase Sólida/métodosRESUMO
The quantification of plastic debris on beaches has been extensively used as an indicator of plastic pollution in the marine environment. However, most efforts have focused on surface layers, with few investigations looking deeper into the substrate, thus underestimating total standing stocks. Such information is crucial to improve our understanding of where plastic accumulates in the oceans. In this study, we investigated the three-dimensional distribution of plastic (>1 mm) in three sandy beaches located in oceanic islands of the North Atlantic (Azores and the Canary Islands) that are known to accumulate significant quantities of small plastic debris at the surface layer. On each beach, we collected a total of 16 sediment cores down to 1 m depth, from the high tide line up to the backshore following a stratified random sampling design spread across four different levels across the beach. Samples were taken every 10 cm down to 1 m into the sand. Our results revealed the presence of plastic items in the deepest layers with subsurface layers accounting for 84 % of the total plastic abundance and with a similar pattern in terms of size, shape, colour and composition. Furthermore, we found increasing plastic concentrations towards the upper levels of the beach, indicating longer term accumulation in the backshore. Collectively, this study suggests that the plastic items reaching sandy beaches of the Macaronesia are being incorporated into its deepest layers, acting as reservoirs of plastic in the open ocean.
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Sorption studies involving microplastics (MPs) are essential to understand the mechanisms implicated in contaminant retention. In this research, a complete study of the sorption behaviour of a hormonal contraceptive -levonorgestrel- in MPs of different composition in two distinct matrices was performed, using high-performance liquid chromatography coupled to a UV detector for the determination of levonorgestrel. Characterization of the studied MPs was achieved by X-ray diffraction, differential scanning calorimetry, and Fourier-transformed infrared spectroscopy. Kinetic and isotherm studies were performed using a batch design under controlled conditions: 500 mg of MPs pellets of 3-5 mm diameter, agitation at 125 rpm, and 30 °C. The comparison of results in ultrapure water and artificial seawater, revealed changes in sorption capacity, and the predominant sorption mechanisms involved. Overall, all studied MPs showed sorption affinity towards levonorgestrel, being low-density polyethylene the one with the highest sorption capacity in ultrapure water and polystyrene in seawater.
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Microplásticos , Poluentes Químicos da Água , Microplásticos/química , Poliestirenos/química , Polietileno/química , Polipropilenos , Plásticos/química , Levanogestrel/análise , Água , Poluentes Químicos da Água/análise , AdsorçãoRESUMO
The purpose of this study was to investigate the occurrence of microplastics (MPs) in drinking water in Spain by comparing tap water from different locations using common sampling and identification procedures. We sampled tap water from 24 points in 8 different locations from continental Spain and the Canary Islands by means of 25 µm opening size steel filters coupled to household connections. All particles were measured and spectroscopically characterized including not only MPs but also particles consisting of natural materials with evidence of industrial processing, such as dyed natural fibres, referred insofar as artificial particles (APs). The average concentration of MPs was 12.5 ± 4.9 MPs/m3 and that of anthropogenic particles 32.2 ± 12.5 APs/m3. The main synthetic polymers detected were polyamide, polyester, and polypropylene, with lower counts of other polymers including the biopolymer poly(lactic acid). Particle size and mass distributions were parameterized by means of power law distributions, which allowed performing estimations of the concentration of smaller particles provided the same scaling parameter of the power law applies. The calculated total mass concentration of the identified MPs was 45.5 ng/L. The observed size distribution of MPs allowed an estimation for the concentration of nanoplastics (< 1 µm) well below the ng/L range; higher concentrations are not consistent with scale invariant fractal fragmentation. Our findings showed that MPs in the drinking water sampled in this work do not represent a significant way of exposure to MPs and would probably pose a negligible risk for human health.
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Água Potável , Poluentes Químicos da Água , Humanos , Microplásticos , Plásticos , Água Potável/análise , Espanha , Cidades , Poluentes Químicos da Água/análise , Monitoramento Ambiental , PolímerosRESUMO
Human activities have introduced high amounts of microplastics (MPs) into the atmosphere that can be transported long distances and be later deposited in terrestrial and aquatic ecosystems with precipitation (rain or snow). In this work, it has been assessed the presence of MPs in the snow of El Teide National Park (Tenerife, Canary Islands, Spain, 2150-3200 m above sea level) after two storm episodes (January-February 2021). The data set (63 samples) was divided into three groups: i) samples from "accessible areas" (after the first storm episode and in places with a strong previous/recent anthropogenic activity); ii) "pristine areas" (after the second storm episode, in places with no previous anthropogenic activity), and iii) "climbing areas" (after the second storm episode, in places with a soft recent anthropogenic activity). Similar pattern profiles were observed among sampling sites in terms of morphology, colour and size (predominance of blue and black microfibers of 250-750 µm length), as well as in composition (predominance of cellulosic -either natural or semisynthetic-, with a 62.7 %, polyester, 20.9 %, and acrylic, 6.3 %, microfibers); however, significant differences in MPs concentrations were found between samples collected in pristine areas (average concentration of 51 ± 72 items/L) and those obtained in places with a previous anthropogenic activity (average concentration of 167 ± 104 and 188 ± 164 items/L in "accessible areas" and "climbing areas", respectively). This study shows, for the first time, the presence of MPs in snow samples from a high altitude protected area on an insular territory and suggests that the sources of these contaminants could be atmospheric transport and local human outdoor activities.
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Soils play a very important role in ecosystems sustainability, either natural or agricultural ones, serving as an essential support for living organisms of different kinds. However, in the current context of extremely high plastic pollution, soils are highly threatened. Plastics can change the chemical and physical properties of the soils and may also affect the biota. Of particular importance is the fact that plastics can be fragmented into microplastics and, to a final extent into nanoplastics. Due to their extremely low size and high surface area, nanoplastics may even have a higher impact in soil ecosystems. Their transport through the edaphic environment is regulated by the physicochemical properties of the soil and plastic particles themselves, anthropic activities and biota interactions. Their degradation in soils is associated with a series of mechanical, photo-, thermo-, and bio-mediated transformations eventually conducive to their mineralisation. Their tiny size is precisely the main setback when it comes to sampling soils and subsequent processes for their identification and quantification, albeit pyrolysis coupled with gas chromatography-mass spectrometry and other spectroscopic techniques have proven to be useful for their analysis. Another issue as a consequence of their minuscule size lies in their uptake by plants roots and their ingestion by soil dwelling fauna, producing morphological deformations, damage to organs and physiological malfunctions, as well as the risks associated to their entrance in the food chain, although current conclusions are not always consistent and show the same pattern of effects. Thus, given the omnipresence and seriousness of the plastic menace, this review article pretends to provide a general overview of the most recent data available regarding nanoplastics determination, occurrence, fate and effects in soils, with special emphasis on their ecological implications.
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Microplásticos , Solo , Plásticos/análise , Ecossistema , AgriculturaRESUMO
In this work, several eutectic mixtures formed by fenchol and acetic acid at seven molar ratios (between 4:1 and 1:4) were characterized and studied for the first time for their possible application as extraction solvents in dispersive liquid-liquid microextraction based on the solidification of the floating organic droplet (DLLME-SFO). A group of 13 emerging contaminants (gemfibrozil, bisphenol F, bisphenol A, 17ß-estradiol, testosterone, estrone, levonorgestrel, 4-tert-octylphenol, butyl benzyl phthalate, dibutyl phthalate, 4-octylphenol, 4-nonylphenol, and dihexyl phthalate) was selected and determined by liquid chromatography with ultraviolet and tandem mass spectrometry detection. Among the studied mixtures, only those of 2:1 and 1:1 provided the suitable features from an operational and repeatability point of view, suggesting that several eutectic mixtures of the same components may also provide similar results. Once the extraction conditions of both mixtures were optimized, the method was applied to the extraction of sea water, urine, and wastewater at different concentration levels, allowing the achievement of absolute recovery values between 49 and 100% for most analytes with relative standard deviation values below 19%. In addition, several samples of each type were analyzed, finding bisphenol A and gemfibrozil in some of them. The greenness of the method was also evaluated using the AGREEprep metric. The DLLME-SFO procedure was found to be very simple, quick, and effective and with a good sample throughput.
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A chain-shattering polymer (CSP) has been proposed as a microdispersive solid-phase extraction (µdSPE) sorbent in a proof-of-concept study of degradable materials for analytical purposes. The responsive CSP was synthesized from 1,3,5-tris(bromomethyl)-2-nitrobenzene acting as the self-immolative trigger responsive unit and 2,6-naphthalenedicarboxylic acid as aromatic linker to enhance noncovalent aromatic interactions with the analytes. The CSP was characterized and applied as a µdSPE sorbent of a group of plasticizers, which were selected as model analytes, from different types of environmental water samples (tap, waste, and spring waters). Gas chromatography coupled to mass spectrometry detection was used for analyte determination. Mean recovery values were in the range of 80%-118% with RSD values below 22%. After the extraction, the polymer could be efficiently degraded by UV irradiation or by chemical reduction, recovering the aromatic linker. This work has proved the potential of CSPs as recyclable sorbents, paving the way to more environmentally benign analytical procedures.
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Polímeros , Poluentes Químicos da Água , Cromatografia Gasosa-Espectrometria de Massas/métodos , Limite de Detecção , Polímeros/química , Extração em Fase Sólida/métodos , Poluentes Químicos da Água/análiseRESUMO
Oil residues have been frequently found on the coasts all over the world as a result of different accidental releases. Their partial evaporation and solidification onto the coastal rocks can produce the formation of a new solid structure forming an agglomerate with other materials, mainly microplastics (though wood, glass, sand and rocks were also found), yielding to a new plastic formation, name herein for the first time as "plastitar". These new formations have been found in several of the islands of the Canary Islands archipelago (Spain). Their study has shown that these new formations can be permanently attached to the rock, occupying even a 56% of the sampled area with an heterogeneous distribution. It was also observed that the studied plastitar was composed mainly of tar and polyethylene (90.6% of the studied particles) and polypropylene (9.4% of the studied particles) microplastics, primarily fragments (82.5%), pellets (15.7%) and lines (1.8%). The ever more frequent presence of plastics and, in particular, microplastics in coastal environments can lead to the common occurrence of these new plastic formations (probably present in other parts of the world), which long-term effects on the coasts should be further investigated.
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Plásticos , Poluentes Químicos da Água , Monitoramento Ambiental , Microplásticos , Polietileno/análise , Poluentes Químicos da Água/análiseRESUMO
Microplastic pollution has an extremely widespread distribution, to the extent that microplastics could be ingested by aquatic organisms, including species of commercial importance for fisheries and aquaculture. In this work, the anthropogenic particles content of the gastrointestinal tracts of 86 individuals of cultivated European sea bass (Dicentrarchus labrax, n = 45) and gilt-head sea bream (Sparus aurata, n = 41) from Tenerife (Canary Islands, Spain) was determined. Samples were bought at local markets and directly transported to the laboratory. After the dissection of the fishes and digestion of the gastrointestinal tracts in 10% KOH (w/v) at 60 °C for 24 h, the digests were filtered (50 µm stainless-steel mesh) and visualized under a stereomicroscope, finding that most of the items were colourless (47.7% for Dicentrarchus labrax and 60.9% for Sparus aurata) and blue (35.3% vs. 24.8%) microfibers, with an average length of 1957 ± 1699 µm and 1988 ± 1853 µm, respectively. Moreover, 15.3% of the microfibres were analysed by Fourier transform infrared spectroscopy, showing the prevalence of cellulosic fibres together with polyester, polyacrylonitrile, and poly(ether-urethane). This pattern (microplastics shapes, colours, sizes, and composition) clearly agrees with previous studies carried out in the Canary Islands region regarding the determination of microplastics in the marine environment.
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In this work, the ammonium formate version of the QuEChERS method has been applied for the first time to the extraction of a group of nine phthalic acid esters and one adipate from three types of coffee (maximum intensity, intermediate intensity and decaffeinated) prepared from coffee capsules, using gas chromatography coupled to mass spectrometry for analytes separation and determination. Matrix-matched calibration showed good linearity with determination coefficients (R2) higher than 0.9983 for all analytes and matrices. In general, matrix effect assessment revealed a medium effect of signal suppression, while mean relative recovery values were in the range 70-120% with relative standard deviation values ≤19% for most analytes. Several samples of each type of coffee obtained from capsules made of different materials were also analysed, finding concentrations of DBP, DEHA and DEHP in the range 29.3-734 ng/capsule, below the tolerable daily intake established for some of them.