ANALYTICAL METHOD FOR DETERMINATION OF AURAMINE DYES IN ECOTOXICITY TESTS AND IN SURFACE WATERS. Dyes can be considered important environmental contaminants. Auramine dyes, known commercially as Solvent Yellow 34 and Basic Yellow 2, are used in several industrial products, including textile and paper. In this study, an analytical method was developed and validated using Liquid-Liquid Extraction and High-Performance Liquid Chromatography coupled to Diode Array Detector (LLE and HPLC-DAD) to determine the exposure concentrations in the ecotoxicological tests with auramine dyes, increasing the results reliability about the hazard of these compounds. The method was also used to monitor auramine dyes in surface water samples, in a region considered one of the most critical regions for dyes contamination in Brazil. The results showed no risk for the aquatic organisms considering the analyzed samples. The method using simple instrumentation showed the results of selectivity, linearity (R2> 0.99), precision (CV: 5.6-29%) and accuracy (recovery: 82-90%) considered satisfactory for the two purposes with Instrumental LOQ of the 12 µg L-1; and the Method LOQ of the 12 ng L-1;. The results indicated that the proposed method was effective and practical for the auramine determination in environmental levels and will be an important tool to verify the potential risk of auramine dyes in future studies.

Plastic pollution is a major societal, economic, and environmental issue. Upon release into the environment, plastics are altered by biological and physicochemical processes that influence their fate and transport within ecosystems. Large plastic debris can fragment into smaller pieces and are called microplastics (MPs) when occurring at sizes between 1 µm and 5 mm, fragmented or produced in this range. These small pieces of plastics are ubiquitous anthropogenic contaminants found throughout the world; however, the environmental consequences and effects on biota are not clearly understood. Scientific literature on the environmental implications of MP pollution is expanding rapidly and critical review of this literature is necessary to identify areas of evolving consensus and remaining gaps in knowledge. Herein a comprehensive literature review was performed to assess (i) the sources and distribution of MPs in different environmental compartments, (ii) the analytical methods that have been applied worldwide, and the key analytical challenges that remain in assessing MPs in the environment, and, finally, (iii) to integrate the findings of Brazilian MP research, which showed that since 2004 (80 papers up to 2020) has documented the presence of MPs in aquatic matrices and sediments with focus on marine ecosystems, mainly identified by visual inspection.

Emerging contaminants have been considered one of the main concerns for ensuring the quality of water around the world. This work presents the results of 10 years of analyses carried out in the state of São Paulo (Brazil) that has the high population density and intense agricultural and industrial activities. In this work 58 compounds (9 hormones, 14 pharmaceuticals and personal care products, 8 industrial compounds, 17 pesticides and 10 illicit drugs) were determined from 2006 to 2015 in 708 samples including raw and treated sewage, surface and ground and drinking waters. A preliminary risk assessment for aquatic life protection identified potential risks for caffeine, paracetamol, diclofenac, 17α-ethynylestradiol, 17β-estradiol, estriol, estrone, testosterone, triclosan, 4-n-nonylphenol, bisphenol A, atrazine, azoxystrobin, carbendazim, fipronil, imidacloprid, malathion and tebuconazole. Drinking water criteria were available only for 22 compounds and for them no adverse effects were expected at the concentrations found, except for 17β-estradiol.

Emerging contaminants occur in parts per trillion or less in aquatic matrices. The effects related to the exposure of aquatic biota and human to them have been identified for different compounds. The knowledge about the concentrations of the exposure is the first step to perform risk assessments. The present work describes a literature review about occurrence in Brazilian aquatic matrices, and a discussion about biological effects, legislation and analytical aspects involving the presence of emerging compounds. The review includes 58 papers published between 1997 and 2016, considering the occurrence of personal care and pharmaceutical compounds, illicit drugs, hormones, pesticides and some other endocrine disruptors compounds in the matrices sewage, surface, ground and drinking waters. The concentrations varied from ng L-1 to µg L-1, depending on the region and the compound. However, the contamination scenario was aggravated by the combination of poor sanitation status - such as low investment in sewage treatment plants, which led to an expressive contamination of the receiving waters with sewage - and the current goods consumption level, which is similar to that of developed countries. These data provide a good insight into the particular levels of contamination and can be used both for further researches and decision making in the regulation area of public policy.

Um método foi otimizado usando extração em fase sólida (SPE) e cromatografia líquida de alta eficiência (HPLC) com detecção por ultravioleta com arranjo de diodos (UV/DAD) ou fluorescência (FLD) para a determinação de 15 contaminantes emergentes em águas superficiais, a saber: acetoaminofenol, ácido salicílico, diclofenaco, ibuprofeno, cafeína, 17β-estradiol, estrona, progesterona, 17α-etinilestradiol, levonorgestrel, dietilftalato, dibutilftalato, 4-octilfenol, 4-nonilfenol e bisfenol A. Os parâmetros de qualidade do método proposto mostraram a linearidade com r² > 0,996, coeficiente de variação menor que 5%, recuperações entre 80 e 120% para Milli-Q fortificada com 10 µg L-1 de cada um dos quinze compostos. O menor limite de detecção (LOD) foi 38 ng L-1 para cafeína e o maior 170 ng L-1 para ibuprofeno. O método foi aplicado para o monitoramento espacial e sazonal destes compostos na bacia do rio Atibaia, principal manancial de abastecimento público da cidade de Campinas-SP, Brasil. Dentre os 15 contaminantes emergentes estudados, 10 foram detectados em pelo menos uma amostra. A menor concentração determinada foi de 0,096 µg L-1 para o diclofenaco e a maior foi de 127 µg L-1 para cafeína.

A single run optimization chromatographic method for the determination of 15 emerging contaminants in surface water was optimized using solid-phase extraction (SPE) and high performance liquid chromatography (HPLC) with detection through ultraviolet-diode array (UV-DAD) or fluorescence (FLD). Selected compounds included acetaminophen, acetylsalicylic acid, diclofenac, ibuprofen, caffeine, 17β-estradiol, estrone, progesterone, 17α-ethynylestradiol, levonorgestrel, diethylphthalate, dibutylphthalate, 4-octylphenol, 4-nonylphenol and bisphenol A. Quality parameters of the proposed method showed a linearity r² > 0.996, coefficient of variation lower than 5%, recoveries between 80 to 120% for a spike of 10 µg L-1 for each of the 15 compounds. The lowest limit of detection (LOD) was 38 ng L-1 for caffeine, whereas the highest value was 170 ng L-1 for ibuprofen. The method was applied to the spatial and seasonal monitoring of these compounds in the Atibaia River, which is the main drinking water source for Campinas City (São Paulo State, Brazil). Among the 15 selected emerging contaminants, 10 were detected at least once. The lowest concentration determined was 0.096 µg L-1 for diclofenac, whereas caffeine showed concentrations as high as 127 µg L-1.