Microwave-assisted extraction followed by gas chromatography-mass spectrometry for the determination of endocrine disrupting chemicals in river sediments

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Journal Article
Journal of Chromatography A, 2004, 1038 (1-2), pp. 19 - 26
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In this study, microwave-assisted extraction (MAE) followed by gas chromatography (GC)-mass spectrometry (MS) analysis has been successfully developed for the simultaneous extraction and determination of contrasting endocrine disrupting chemicals (EDCs) including 17β-estradiol, estrone, 17α-ethynylestradiol, 16α-hydroxyestrone, 4-nonylphenol, 4-tert-octylphenol and bisphenol A in river sediments. For MAE, the effects of various parameters on the extraction efficiency were investigated. It is shown that the most efficient extraction (recovery >74%) of the target compounds was achieved by using methanol as the solvent, an extraction temperature of 110°C and 15 min of holding time. The cleanup of extracts was carried out by passage through a non-deactivated silica gel column, and a satisfactory elution efficiency of all compounds was achieved using a solvent mixture of ethyl acetate-hexane (4:6, v/v). The spiking experiments show that the mean recovery of the target compounds exceeded 61% at a spiking level of 5 ng/g dry mass, and 73% at 10, 40 and 100 ng/g dry mass with a good reproducibility. The method developed was applied to the determination of target EDCs in river sediments collected from rivers Uck and Ouse, UK, and results revealed the presence of the chosen compounds at low ng/g level. © 2004 Elsevier B.V. All rights reserved.
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