title: Determination of endocrine-disrupting compounds in environmental samples using gas and liquid chromatography with mass spectrometry.
abstract: This paper describes certain applications for endocrine-disrupting compounds determination. LC-MS was applied using an electrospray ionization (ESI) technique in positive mode for alcohol polyethoxylates and nonylphenol and octylphenol polyethoxylates (NPEOn and OPEOn), and in negative mode for 4-nonylphenol (4-NP) and 4-octylphenol (4-OP) to determine targeted compounds in wastewater and sludge. GC-MS and GC-MS-MS were used to determine 4-NP, 4-tert.-octylphenol (4-t-OP), bisphenol A, estradiol-17beta, estriol estrone, testosterone, 17alpha-ethynylestradioL cholesterol, coprostan-3-ol, coprostan and coprostan-3-one in both surface water and wastewater after derivatization with N,O-bis(trimethyl-silyl)trifluoroacetamide (BSTFA). Extraction from the water samples was by an SPE technique, using either a copolymeric (Oasis HLB) or C18 silica sorbents, depending on the target contaminants. Extraction from the sludge samples was by a Soxtec system using methanol. Percentage recoveries for most of the selected compounds, using either a copolymeric (Oasis HLB) or C18 silica sorbents, were satisfactory (>60%). Quantification limits for the target compounds were at ppb levels in both water and sludge samples when using LC-ESI-MS in both positive and negative modes. They reached ppt levels in water when using GC-MS (in large volume injection mode) and GC-MS-MS. The results revealed 4-NP, NPEOn and AEOs in sludge samples at a concentration range of 1.3-8.5 microg/g, and NPEOn, OPEOn and other compounds, such as coprostan and bisphenol A, in surface water and/or wastewater samples at concentrations ranging from the ppt to ppb levels.
authors.affiliation: Service Analyse et Caractérisation Minérale, BRGM, BP 6009, 45060 Orleans Cedex 02, France. r.jeannot@brgm.fr
authors.forename: Roger
authors.initials: R
authors.lastname: Jeannot
authors.forename: Hassan
authors.initials: H
authors.lastname: Sabik
authors.forename: Emmanuel
authors.initials: E
authors.lastname: Sauvard
authors.forename: Thierry
authors.initials: T
authors.lastname: Dagnac
authors.forename: Katja
authors.initials: K
authors.lastname: Dohrendorf
mesh_terms: D002138:Calibration; D002849:Chromatography, Gas / Q000379:methods*; D002853:Chromatography, Liquid / Q000379:methods*; D004702:Endocrine Glands / Q000187:drug effects*; D004785:Environmental Pollutants / Q000032:analysis* / Q000494:pharmacology; D013058:Mass Spectrometry / Q000379:methods*; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
chemical_list: D004785:Environmental Pollutants