This paper describes the validation of a method consisting of solid-phase extraction followed by gas chromatography-tandem mass spectrometry for the analysis of the ultraviolet (UV) filters benzophenone-3, ethylhexyl salicylate, ethylhexyl methoxycinnamate and octocrylene. The method validation criteria included evaluation of selectivity, analytical curve, trueness, precision, limits of detection and limits of quantification. The non-weighted linear regression model has traditionally been used for calibration, but it is not necessarily the optimal model in all cases. Because the assumption of homoscedasticity was not met for the analytical data in this work, a weighted least squares linear regression was used for the calibration method. The evaluated analytical parameters were satisfactory for the analytes and showed recoveries at four fortification levels between 62% and 107%, with relative standard deviations less than 14%. The detection limits ranged from 7.6 to 24.1 ng L(-1). The proposed method was used to determine the amount of UV filters in water samples from water treatment plants in Araraquara and Jau in São Paulo, Brazil.
Ultraviolet (UV) filters are widely used in the formulation of personal care products (PCPs) to prevent damage to the skin, lips, and hair caused by excessive UV radiation. Therefore, large amounts of these substances are released daily into the aquatic environment through either recreational activities or the release of domestic sewage. The concern regarding the presence of such substances in the environment and the exposure of aquatic organisms is based on their potential for bioaccumulation and their potential as endocrine disruptors. Although there are several reports regarding the occurrence and fate of UV filters in the aquatic environment, these compounds are still overlooked in tropical areas. In this study, we investigated the occurrence of the organic UV filters benzophenone-3 (BP-3), ethylhexyl salicylate (ES), ethylhexyl methoxycinnamate (EHMC), and octocrylene (OC) in six water treatment plants in various cities in Southeast Brazil over a period of 6 months to 1 year. All of the UV filters studied were detected at some time during the sampling period; however, only EHMC and BP-3 were found in quantifiable concentrations, ranging from 55 to 101 and 18 to 115 ng L(-1), respectively. Seasonal variation of BP-3 was most clearly noticed in the water treatment plant in Araraquara, São Paulo, where sampling was performed for 12 months. BP-3 was not quantifiable in winter but was quantifiable in summer. The levels of BP-3 were in the same range in raw, treated and chlorinated water, indicating that the compound was not removed by the water treatment process.
The aim of this study was to assess the occurrence of zearalenone (ZEN) and its metabolites zearalanone (ZAN), α-zearalenol (α-ZEL), β-zearalenol (β-ZEL) α-zearalanol (α-ZAL), and β-zearalanol (β-ZAL) in the surface waters of northern São Paulo state (Brazil) and to evaluate the associated potential estrogenic contribution to the aquatic environment. The determination of the estrogenic mycotoxins in water samples from the Rico Stream microbasin yielded levels of up to 59 ng L-1 and their corresponding calculated estrogenic equivalent (cEEQ) values were between < 0.03 and 1.4 ng L-1, which are associated with negative effects on the reproduction and growth of some fish species. The physicochemical and microbiological parameters were evaluated to determine the water quality in the Rico stream region. This study revealed the first data about the presence of estrogenic mycotoxins in the Brazilian river waters and emphasizes the need to include these substances in future public policies concerning water quality, since these compounds are not yet legally regulated. From an environmental aspect, it is necessary to take into account the continuous introduction into surface water of microcontaminants associated with wastewater effluent, such as estrogenic mycotoxins.
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