title: Gas chromatographic-mass spectrometric method for the determination of bisphenol A and its chlorinated derivatives in urban wastewater.
abstract: The simultaneous determination of trace amounts of endocrine disruptors such as bisphenol A (BPA) and its monochloro, dichloro, trichloro and tetrachloro derivatives in wastewater has been developed using gas chromatography-mass spectrometry (GC-MS). Compounds were previously extracted from the aqueous samples using a liquid-liquid extraction procedure with a mixture of dichloromethane:carbon tetrachloride (25/75). After extraction, solvent was removed and a silylation step was carried out with N,O-bis(trimethylsilyl) trifluoroacetamide (BSTFA). The silylated compounds were identified and quantified by GC-MS using an HP1-MS column. The retention times were 6.64 min for BPA silylated, 7.26 min for Cl-BPA silylated, 7.99 min for Cl(2)-BPA silylated, 8.85 min for Cl(3)-BPA silylated and 9.95 min for Cl(4)-BPA silylated. A clean-up is not necessary using SIM mode. Deuterated anthracene (2H(10)-anthracene) was used as an internal standard. The detection limits obtained were 0.3, 0.6, 2.0, 4.5 and 13.0 ng L(-1) for silylated BPA, Cl-BPA, Cl(2)-BPA, Cl(3)-BPA and Cl(4)-BPA, respectively. The proposed method was applied satisfactory to the determination of these chemicals, in different types of wastewater previously spiked with different amounts of these chemicals at concentration levels ranging from 0.01 to 2.50 microg L(-1) for BPA, 0.05-2.50 micro L(-1) for Cl-BPA and 0.05-5.00 microg L(-1) for Cl(2)-BPA, Cl(3)-BPA and Cl(4)-BPA, respectively. The method was validated following standard addition methodology.
authors.affiliation: Department of Analytical Chemistry, University of Granada, E-18071, Granada, Spain.
authors.forename: Alberto
authors.initials: A
authors.lastname: Zafra
authors.forename: Monsalud
authors.initials: M
authors.lastname: del Olmo
authors.forename: Beatriz
authors.initials: B
authors.lastname: Suárez
authors.forename: Ernesto
authors.initials: E
authors.lastname: Hontoria
authors.forename: Alberto
authors.initials: A
authors.lastname: Navalón
authors.forename: José Luís
authors.initials: JL
authors.lastname: Vílchez
mesh_terms: D001559:Benzhydryl Compounds; D002713:Chlorine / Q000737:chemistry*; D002853:Chromatography, Liquid; D002947:Cities; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D010636:Phenols / Q000032:analysis* / Q000737:chemistry*; D012680:Sensitivity and Specificity; D014874:Water Pollutants, Chemical / Q000032:analysis*; D000098826:Bisphenol A Compounds
chemical_list: D001559:Benzhydryl Compounds; D002713:Chlorine; D010636:Phenols; D014874:Water Pollutants, Chemical; C006780:bisphenol A; D000098826:Bisphenol A Compounds