title: Sensitive gas chromatographic-mass spectrometric method for the determination of phthalate esters, alkylphenols, bisphenol A and their chlorinated derivatives in wastewater samples.
abstract: Phthalate esters, alkylphenols, bisphenol A and their chlorinated derivatives are the suspected endocrine disrupters or mutagens. These compounds, commonly called endocrine disrupter chemicals (EDCs), are widely used as plastic additives, lacquers, resins, or surfactants and can be usually found in environmental samples, namely wastewaters. An accurate and reproducible gas chromatographic-mass spectrometric (GC-MS) method is proposed to measure these compounds in wastewater samples of Granada city (Spain). A solid-phase extraction with LiChrolut RP-18 cartridges was carried out and the elution was performed with a diethyl ether/methanol mixture. After isolation, solvent was removed and a silylation step was carried out using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA). Phthalate esters and silylated compounds were identified and quantified by GC-MS using a ZB-5 MS column. Bisphenol F was used as a surrogate. Quantification limits found were between 20 ng L(-1) for 4-nonylphenol and 400 ng L(-1) for benzylbutyl phthalate while inter and intra-day variability was under 5% in all cases. Recoveries for spiked samples were over 95% and under 105%. The method was validated using standard addition calibration and recovery assays.
authors.affiliation: Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Avda. Fuentenueva s/n, E-18071 Granada, Spain.
authors.forename: Oscar
authors.initials: O
authors.lastname: Ballesteros
authors.forename: Alberto
authors.initials: A
authors.lastname: Zafra
authors.forename: Alberto
authors.initials: A
authors.lastname: Navalón
authors.forename: José Luis
authors.initials: JL
authors.lastname: Vílchez
mesh_terms: D001559:Benzhydryl Compounds; D052244:Endocrine Disruptors / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006843:Hydrocarbons, Chlorinated / Q000032:analysis*; D007220:Industrial Waste; D010636:Phenols / Q000032:analysis*; D010795:Phthalic Acids / Q000032:analysis*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D014874:Water Pollutants, Chemical / Q000032:analysis*; D000098826:Bisphenol A Compounds
chemical_list: D001559:Benzhydryl Compounds; D052244:Endocrine Disruptors; D006843:Hydrocarbons, Chlorinated; D007220:Industrial Waste; D010636:Phenols; D010795:Phthalic Acids; D014874:Water Pollutants, Chemical; C006780:bisphenol A; D000098826:Bisphenol A Compounds