title: Determination of steroidal oestrogens in tap water samples using solid-phase extraction on a molecularly imprinted polymer sorbent and quantification with gas chromatography-mass spectrometry (GC-MS).
abstract: An analytical method was established and validated for the analysis of steroidal oestrogens in tap water samples. Gas chromatography coupled to high-resolution mass spectrometry (GC-HRMS) and gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) were used for the identification/quantification of selected compounds and the analytical performance of these techniques was evaluated. Liquid-liquid extraction (LLE) and solid-phase extraction (SPE) with a molecularly imprinted polymer (MIP) stationary phase that was highly selective for oestrogens were used for the extraction of 100-mL aliquots of water samples. The recoveries of analytes with the described methods ranged from 92 to 114 %, while the repeatability in terms of relative standard deviations (RSDs) was in the range from 2.1 to 15.2 % (n = 5). It was concluded that SPE with MIP that was highly selective for oestrogens in combination with GC-HRMS detection is more preferable for the analysis of oestrogens in tap water samples. The typical oestrogen, 17β-estradiol (17β-E2), was detected above the method limit of quantification (m-LOQ) in 5 of 14 analysed tap water samples at concentrations from 0.09 to 0.15 ng L(-1). Despite that 17α-ethynylestradiol (17α-EE2) was not quantified in this study above m-LOQ, the presence of this chemical was qualitatively confirmed in some of the analysed samples.
authors.affiliation: Department of Chemistry, University of Latvia, Jelgavas iela 1, Riga, LV-1004, Latvia. dzintars.zachs@gmail.com.
authors.forename: D
authors.initials: D
authors.lastname: Zacs
authors.affiliation: Department of Chemistry, University of Latvia, Jelgavas iela 1, Riga, LV-1004, Latvia.
authors.forename: I
authors.initials: I
authors.lastname: Perkons
authors.affiliation: Department of Chemistry, University of Latvia, Jelgavas iela 1, Riga, LV-1004, Latvia.
authors.forename: V
authors.initials: V
authors.lastname: Bartkevics
mesh_terms: D002849:Chromatography, Gas; D060766:Drinking Water / Q000737:chemistry*; D004784:Environmental Monitoring / Q000379:methods*; D004967:Estrogens / Q000032:analysis*; D004997:Ethinyl Estradiol / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D057230:Limit of Detection; D059625:Liquid-Liquid Extraction / Q000379:methods; D054802:Molecular Imprinting; D011108:Polymers / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D060766:Drinking Water; D004967:Estrogens; D011108:Polymers; D014874:Water Pollutants, Chemical; D004997:Ethinyl Estradiol
keywords: Gas chromatography-high-resolution mass spectrometry; Gas chromatography-tandem mass spectrometry; Molecularly imprinted polymer; Solid-phase extraction; Steroidal oestrogens