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)

Environ Monit Assess. 2016 Jul;188(7):433. doi: 10.1007/s10661-016-5435-8. Epub 2016 Jun 25.

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.

Keywords: Gas chromatography-high-resolution mass spectrometry; Gas chromatography-tandem mass spectrometry; Molecularly imprinted polymer; Solid-phase extraction; Steroidal oestrogens.

MeSH terms

  • Chromatography, Gas
  • Drinking Water / chemistry*
  • Environmental Monitoring / methods*
  • Estrogens / analysis*
  • Ethinyl Estradiol / analysis*
  • Gas Chromatography-Mass Spectrometry / methods
  • Limit of Detection
  • Liquid-Liquid Extraction / methods
  • Molecular Imprinting
  • Polymers / chemistry*
  • Solid Phase Extraction / methods
  • Tandem Mass Spectrometry / methods
  • Water Pollutants, Chemical / analysis*

Substances

  • Drinking Water
  • Estrogens
  • Polymers
  • Water Pollutants, Chemical
  • Ethinyl Estradiol