title: An improved method for the simultaneous analysis of phenolic and steroidal estrogens in water and sediment.
abstract: 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 chromatography-tandem mass spectrometry (GC-MS/MS). The analytes were 4-tert-octylphenol, 4-nonylphenol, bisphenol A, estrone, 17beta-estradiol, 17alpha-ethynylestradiol and 16alpha-hydroxyestrone. The optimised GC-MS/MS method produces increased selectivity and sensitivity compared to GC-MS, 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 (86-102%) 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.
authors.affiliation: Department of Biology and Environmental Science, School of Life Sciences, University of Sussex, Falmer, Brighton, UK.
authors.forename: A
authors.initials: A
authors.lastname: Hibberd
authors.forename: K
authors.initials: K
authors.lastname: Maskaoui
authors.forename: Z
authors.initials: Z
authors.lastname: Zhang
authors.forename: J L
authors.initials: JL
authors.lastname: Zhou
mesh_terms: D002849:Chromatography, Gas / Q000379:methods; D052244:Endocrine Disruptors / Q000032:analysis; D004967:Estrogens / Q000032:analysis*; D019015:Geologic Sediments; D013058:Mass Spectrometry / Q000379:methods; D008872:Microwaves; D010636:Phenols / Q000032:analysis*; D011725:Pyridines / Q000032:analysis; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction / Q000379:methods; D012997:Solvents; D013256:Steroids / Q000032:analysis*; D014867:Water / Q000737:chemistry*; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D052244:Endocrine Disruptors; D004967:Estrogens; D010636:Phenols; D011725:Pyridines; D012997:Solvents; D013256:Steroids; D014874:Water Pollutants, Chemical; D014867:Water; C023666:pyridine