Simultaneous determination of endocrine disrupting phenolic compounds and steroids in water by solid-phase extraction–gas chromatography–mass spectrometry

• Published in: Journal of Chromatography A Vol. 1022; no. 1; pp. 179 - 189
• Main Authors: Liu, R, Zhou, J.L, Wilding, A
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 02.01.2004; Elsevier
• Subjects: Analysis methods; Applied sciences; Calibration; Endocrine disruptors; Endocrine Glands - drug effects; Environmental Pollutants - analysis; Environmental Pollutants - pharmacology; Exact sciences and technology; Gas Chromatography-Mass Spectrometry; Natural water pollution; Phenolic compounds; Phenols - analysis; Phenols - pharmacology; Pollution; Reproducibility of Results; Sensitivity and Specificity; Steroids; Steroids - analysis; Steroids - pharmacology; Water analysis; Water treatment and pollution; Endocrine disruptors; Phenolic compounds; Water analysis; Steroids; Steroid; Solid phase extraction; Mimetic hormone; Chemical analysis; Coupled method; Silylation; Estrogen; Endocrine disruptor; Derivatization; Chemical enrichment; Bisphenol A; Gas chromatography; Sample preparation; Surface water; Simultaneous measurement; Water pollution; River water; Mass spectrometry; Seawater
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2003.09.035

A solid-phase extraction (SPE)–gas chromatography (GC)–mass spectrometry (MS) analytical method for the simultaneous separation and determination of endocrine disrupting chemicals (EDCs) from water samples is described in detail. Important and contrasting EDCs including estrone, 17β-estradiol, 17α-ethynylestradiol, 16α-hydroxyestrone, 4-nonylphenol, bisphenol A and 4- tert-octylphenol were selected as the target compounds. The SPE technique, followed by the derivatisation with bis (trimethylsilyl) trifluoroacetamide was used for the extraction recoveries of target compounds from water samples. A number of parameters that may affect the recovery of EDCs, such as the type of SPE cartridges, eluents, as well as water properties including pH value, and concentration of salts and humic substances were investigated. It is shown that the Oasis cartridges produced the best recoveries of target EDCs while ethyl acetate was efficient in eluting EDCs from SPE cartridges. The recovery of some EDCs was enhanced by the addition of salt, but reduced by the increase in pH value and humic acid concentration. The optimised method was further verified by performing spiking experiments in natural river water and seawater matrices, with good recovery and reproducibility for all the selected compounds. The established method was successfully applied to environmental water samples from East and West Sussex, UK, for the determination of the target EDCs.