title: Estrogens determination in wastewater samples by automatic in-syringe dispersive liquid-liquid microextraction prior silylation and gas chromatography.
abstract: A new procedure for the extraction, preconcentration and simultaneous determination of the estrogens most used in contraception pharmaceuticals (estrone, 17β-estradiol, estriol, and 17α-ethynylestradiol), cataloged as Contaminants of Emergent Concern by the Environmental Protection Agency of the United States (US-EPA), is proposed. The developed system performs an in-syringe magnetic stirring-assisted dispersive liquid-liquid microextraction (in-syringe-MSA-DLLME) prior derivatization and gas chromatography (GC-MS). Different extraction (carbon tetrachloride, ethyl acetate, chloroform and trichloroethylene) and disperser solvents (acetone, acetonitrile and methanol) were tested. Chloroform and acetone were chosen as extraction and disperser solvent, respectively, as they provided the best extraction efficiency. Then, a multivariate optimization of the extraction conditions was carried out. Derivatization conditions were also studied to ensure the conversion of the estrogens to their respective trimethylsilyl derivatives. Low LODs and LOQs were achieved, i.e. between 11 and 82ngL(-1), and 37 and 272ngL(-1), respectively. Good values for intra and inter-day precision were obtained (RSDs≤7.06% and RSD≤7.11%, respectively). The method was successfully applied to wastewater samples.
authors: Group of Analytical Chemistry, Automation and Environment, Department of Chemistry, University of the Balearic Islands, E-07122 Palma de Mallorca, Spain.
authors: Alba
authors: A
authors: González
authors: Sciware Systems, S.L. Spin-off of the University of the Balearic Islands, E-07193 Bunyola, Spain.
authors: Jessica
authors: J
authors: Avivar
authors: Group of Analytical Chemistry, Automation and Environment, Department of Chemistry, University of the Balearic Islands, E-07122 Palma de Mallorca, Spain. Electronic address: victor.cerda@uib.es.
authors: Víctor
authors: V
authors: Cerdà
mesh_terms: D004958:Estradiol / Q000032:analysis; D004964:Estriol / Q000032:analysis; D004967:Estrogens / Q000032:analysis*; D004970:Estrone / Q000032:analysis; D004997:Ethinyl Estradiol / Q000032:analysis; D008401:Gas Chromatography-Mass Spectrometry; D057230:Limit of Detection; D059627:Liquid Phase Microextraction / Q000379:methods; D012997:Solvents / Q000737:chemistry; D013594:Syringes; D014297:Trimethylsilyl Compounds / Q000737:chemistry*; D014481:United States; D062065:Wastewater / Q000737:chemistry*
chemical_list: D004958:Estradiol; D004964:Estriol; D004967:Estrogens; D004970:Estrone; D004997:Ethinyl Estradiol; D012997:Solvents; D014297:Trimethylsilyl Compounds; D062065:Wastewater
keywords: Automation; Estrogens; Gas chromatography (GC); In-syringe magnetic stirring-assisted dispersive liquid–liquid microextraction (in-syringe-MSA-DLLME); Wastewater samples