An improved method for the simultaneous analysis of phenolic and steroidal estrogens in water and sediment

Publisher:
Elsevier Inc
Publication Type:
Journal Article
Citation:
Talanta, 2009, 77 (4), pp. 1315 - 1321
Issue Date:
2009-01
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This paper describes an improved method for the extraction and analysis of seven endocrine disrupting chemicals with wide-ranging polarities from water and sediments using gas chromatographytandem mass spectrometry (GCMS/MS). The analytes were 4-tert-octylphenol, 4-nonylphenol, bisphenol A, estrone, 17ß-estradiol, 17a-ethynylestradiol and 16a-hydroxyestrone. The optimised GCMS/MS method produces increased selectivity and sensitivity compared to GCMS, with limit of detection ranging from 0.01 to 0.49 ng L-1 in water and from 0.05 to 0.14 ng g-1 in sediment. Extraction from aqueous samples was performed by solid-phase extraction (SPE) and from sediment samples by microwave-assisted extraction (MAE). The improved method for the clean-up of sediment extracts carried out by SPE enhanced EDC recovery (86102%) while reducing matrix interference and sample drying time. Derivatisation of final sample extracts was achieved using N,O-bis(trimethylsilyl)trifluoroacetamide and pyridine, and their stability was enhanced by reconstituting the derivatised extracts with hexane. The method was validated by spiking experiments which showed good recovery and reproducibility. The method was applied to samples taken from the Medway estuary in Kent, UK, where non-conservative behaviour of EDCs was demonstrated.
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