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Toward the determination of estrogenic compounds in the framework of EU watch list: validation and implementation of a two-step solid phase extraction–liquid phase chromatography coupled to tandem mass spectrometry method

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Abstract

In this paper, development and optimization of a new method for determination of the three hormones (estrone, 17-β-estradiol and 17-α-ethinylestradiol) of the Watch list were described. The validated method relies on isotope dilution—two-step solid phase extraction–liquid phase chromatography mass spectrometry method. The measurement procedure validation has been performed in real matrices, including matrix with high suspended particulate matter and high organic carbon contents, to demonstrate its fitness for purpose. Method performances were in agreement with the requirements of the decision 2015/495/EU (maximal acceptable method detection limit and whole-water analysis). Limits of quantification of the method were of 0.4 ng L−1 for estrone and 17-β-estradiol and 0.1 ng L−1 for 17-α-ethinylestradiol. Expanded uncertainties (k = 2) at limit of quantification were equal to 35 % for estrone and 17-β-estradiol and 50 % for 17-α-ethinylestradiol. The method was successfully implemented to monitor French inland surface waters contamination. The survey reveals a chronic state of contamination by estrone (96 % quantification rate) and significant one by 17-β-estradiol and 17-α-ethinylestradiol (15 % quantification rate). Maximum measured concentrations are above predicted no-effect concentrations, indicating potential risk toward the environment.

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Acknowledgements

This work was supported by the French Agency for Biodiversity (AFB) and national reference laboratory for monitoring aquatic Environments (AQUAREF). The authors acknowledge the six French water agencies for sampling.

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Authors and Affiliations

  1. Laboratoire National de métrologie et d’Essais (LNE), 1 rue Gaston Boissier, 75724, Paris, France

    Sophie Lardy-Fontan, Véronique Le Diouron, Carine Fallot, Sophie Vaslin-Reimann & Béatrice Lalere

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  1. Sophie Lardy-Fontan
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  2. Véronique Le Diouron
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  3. Carine Fallot
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  4. Sophie Vaslin-Reimann
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  5. Béatrice Lalere
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Correspondence to Sophie Lardy-Fontan.

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Lardy-Fontan, S., Le Diouron, V., Fallot, C. et al. Toward the determination of estrogenic compounds in the framework of EU watch list: validation and implementation of a two-step solid phase extraction–liquid phase chromatography coupled to tandem mass spectrometry method. Accred Qual Assur 23, 285–295 (2018). https://doi.org/10.1007/s00769-018-1346-4

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  • DOI: https://doi.org/10.1007/s00769-018-1346-4

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