Determining estrogenic steroids in Taipei waters and removal in drinking water treatment using high-flow solid-phase extraction and liquid chromatography/tandem mass spectrometry

Determining estrogenic steroids in Taipei waters and removal in drinking water treatment using... River water and wastewater treatment plant (WWTP) effluents from metropolitan Taipei, Taiwan were tested for the presence of the pollutants estrone (E 1 ), estriol (E 3 ), 17β-estradiol (E 2 ), and 17α-ethinylestradiol (EE 2 ) using a new methodology that involves high-flow solid-phase extraction and liquid chromatography/tandem mass spectrometry. The method was also used to investigate the removal of the analytes by conventional drinking water treatment processes. Without adjusting the pH, we extracted 1-L samples with PolarPlus C 18 Speedisks under a flow rate exceeding 100 mL/min, in which six samples could be done simultaneously using an extraction station. The adsorbent was washed with 40% methanol/60% water and then eluted by 50% methanol/50% dichloromethane. The eluate was concentrated until almost dry and was reconstituted by 20 μL of methanol. Quantitation was done by LC-MS/MS-negative electrospray ionization in the selected reaction monitoring mode with isotope-dilution techniques. The mobile phase was 10 mM N -methylmorpholine aqueous solution/acetonitrile with gradient elution. Mean recoveries of spiked Milli-Q water were 65–79% and precisions were within 2–20% of the tested concentrations (5.0–200 ng/L). The method was validated with spiked upstream river water; precisions were most within 10% of the tested concentrations (10–100 ng/L) with most RSDs < 10%. LODs of the environmental matrixes were 0.78–7.65 ng/L. A pre-filtration step before solid-phase extraction may significantly influence the measurement of E 1 and EE 2 concentrations; disk overloading by water matrix may also impact analyte recoveries along with ion suppression. In the Taipei water study, the four steroid estrogens were detected in river samples (ca. 15 ng/L for E 2 and EE 2 and 35−45 ng/L for E 1 and E 3 ). Average levels of 19–26 ng/L for E 1 , E 2 , and EE 2 were detected in most wastewater effluents, while only a single effluent sample contained E 3 . The higher level in the river was likely caused by the discharge of untreated human and farming waste into the water. In the drinking water treatment simulations, coagulation removed 20–50% of the estrogens. An increased dose of aluminum sulfate did not improve the performance. Despite the reactive phenolic moiety in the analytes, the steroids were decreased only 20–44% of the initial concentrations in pre- or post-chlorination. Rapid filtration, with crushed anthracite playing a major role, took out more than 84% of the estrogens. Except for E 3 , the whole procedure successfully removed most of the estrogens even if the initial concentration reached levels as high as 500 ng/L. http://www.deepdyve.com/assets/images/DeepDyve-Logo-lg.png Science of the Total Environment Elsevier

Determining estrogenic steroids in Taipei waters and removal in drinking water treatment using high-flow solid-phase extraction and liquid chromatography/tandem mass spectrometry

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Publisher
Elsevier
Copyright
Copyright © 2007 Elsevier B.V.
ISSN
0048-9697
eISSN
1879-1026
DOI
10.1016/j.scitotenv.2007.02.038
Publisher site
See Article on Publisher Site

Abstract

River water and wastewater treatment plant (WWTP) effluents from metropolitan Taipei, Taiwan were tested for the presence of the pollutants estrone (E 1 ), estriol (E 3 ), 17β-estradiol (E 2 ), and 17α-ethinylestradiol (EE 2 ) using a new methodology that involves high-flow solid-phase extraction and liquid chromatography/tandem mass spectrometry. The method was also used to investigate the removal of the analytes by conventional drinking water treatment processes. Without adjusting the pH, we extracted 1-L samples with PolarPlus C 18 Speedisks under a flow rate exceeding 100 mL/min, in which six samples could be done simultaneously using an extraction station. The adsorbent was washed with 40% methanol/60% water and then eluted by 50% methanol/50% dichloromethane. The eluate was concentrated until almost dry and was reconstituted by 20 μL of methanol. Quantitation was done by LC-MS/MS-negative electrospray ionization in the selected reaction monitoring mode with isotope-dilution techniques. The mobile phase was 10 mM N -methylmorpholine aqueous solution/acetonitrile with gradient elution. Mean recoveries of spiked Milli-Q water were 65–79% and precisions were within 2–20% of the tested concentrations (5.0–200 ng/L). The method was validated with spiked upstream river water; precisions were most within 10% of the tested concentrations (10–100 ng/L) with most RSDs < 10%. LODs of the environmental matrixes were 0.78–7.65 ng/L. A pre-filtration step before solid-phase extraction may significantly influence the measurement of E 1 and EE 2 concentrations; disk overloading by water matrix may also impact analyte recoveries along with ion suppression. In the Taipei water study, the four steroid estrogens were detected in river samples (ca. 15 ng/L for E 2 and EE 2 and 35−45 ng/L for E 1 and E 3 ). Average levels of 19–26 ng/L for E 1 , E 2 , and EE 2 were detected in most wastewater effluents, while only a single effluent sample contained E 3 . The higher level in the river was likely caused by the discharge of untreated human and farming waste into the water. In the drinking water treatment simulations, coagulation removed 20–50% of the estrogens. An increased dose of aluminum sulfate did not improve the performance. Despite the reactive phenolic moiety in the analytes, the steroids were decreased only 20–44% of the initial concentrations in pre- or post-chlorination. Rapid filtration, with crushed anthracite playing a major role, took out more than 84% of the estrogens. Except for E 3 , the whole procedure successfully removed most of the estrogens even if the initial concentration reached levels as high as 500 ng/L.

Journal

Science of the Total EnvironmentElsevier

Published: Jun 1, 2007

References

  • Oestrogens and oestrogenic activity in raw and treated water in Severn Trent Water
    Fawell, J.K.; Sheahan, D.; James, H.A.; Hurst, M.; Scott, S.
  • Estimating steroid oestrogen inputs into activated sludge treatment works and observations on their removal from the effluent
    Johnson, A.C.; Belfroid, A.; Di Corcia, A.
  • Effects of chlorine on the decrease of estrogenic chemicals.
    Lee, B.C.; Kamata, M.; Akatsuka, Y.; Takeda, M.; Ohno, K.; Kamei, T.
  • Validation of a quantitative assay using GC/MS for trace determination of free and conjugated estrogens in environmental water samples
    Mouatassim-Souali, A.; Tamisier-Karolak, S.L.; Perdiz, D.; Cargouet, M.; Levi, Y.
  • Substances with estrogenic activity in effluents of sewage treatment plants in southwestern Germany. 1. Chemical analysis
    Spengler, P.; Korner, W.; Metzger, J.W.
  • River water quality
    TDEP (Taipei Department of Environmental Protection)
  • Occurrence and fate of hormone steroids in the environment
    Ying, G.G.; Kookana, R.S.; Ru, Y.J.
  • Analysis of disinfection by-products in drinking water by LC-MS and related MS techniques
    Zwiener, C.; Richardson, S.D.

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