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Development and validation of a gas chromatography mass spectrometry method for the analysis of phytoestrogens, phytosterols and mycotoxins in estuarine water samples

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Many pollutants currently released into the environment may cause adverse effects on exposed organisms leading to disruption of the endocrine system. Among them are natural compounds such as phytoestrogens and phytosterols, found in various plants and mycotoxins produced by a wide range of fungal species. The presence of some classes of phytoestrogens and phytosterols has been demonstrated in environmental samples while little information can be found about the presence of mycotoxins. Due to the complexity of environmental matrices and the low concentrations normally found, sensitive and selective methods are required for an unequivocal quantification of this type of compounds. The aim of this study was to develop and validate an analytical method for the simultaneous quantification of seven phytoestrogens, two phytosterols and three mycotoxins in estuarine water samples. The method consisted of the preconcentration of estuarine water samples (1 L) on 200 mg OASIS HLB cartridges, followed by a clean-up step in 1 g silica cartridges and quantification by gas chromatography with mass spectrometry ion trap analyser. Validation parameters were evaluated and the method demonstrated to be selective and linear with correlations higher than 0.99. Method detection limits were in the ng L−1 levels ranging from 18.0 to 90.0 ng L−1, recovery rates ranged from 59.8% to 99.5% and precision (RSD) from 5.5% and 9.7%. The feasibility of the method was demonstrated in surface water samples from Douro River estuary, a polluted estuary, with reported incidence of endocrine-disrupting phenomena.
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Keywords: endocrine-disrupting compounds; estuarine water; gas chromatography mass spectrometry; mycotoxins; phytoestrogens; phytosterols

Document Type: Research Article

Affiliations: CESPU, Instituto de Investigação e Formação Avançada em Ciências e Tecnologias da Saúde, Gandra, PRD, 4585-116, Portugal

Publication date: February 19, 2015

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