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Developing analytical approaches to explore the connection between endocrine-active pharmaceuticals in water to effects in fish

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Abstract

The emphasis of this research project was to develop and optimize a solid-phase extraction method and high-performance liquid chromatography-electrospray ionization-mass spectrometry method, such that a linkage between the detection of endocrine-active pharmaceuticals (EAPs) in the aquatic environment and subsequent effects on fish populations could eventually be studied. Four EAPs were studied: tamoxifen (TAM), exemestane (EXE), letrozole (LET), anastrozole (ANA); and three TAM metabolites: 4-hydroxytamoxifen, e/z endoxifen, and n-desmethyl tamoxifen. In aqueous matrices, the use of isotopically labeled standards for the EAPs allowed for the generation of good recoveries, greater than 80 %, and low relative standard deviations (% RSDs) (3 to 27 %). TAM metabolites had lower recoveries in the spiked water matrices: 35 to 93 % in waste/source water compared to 58 to 110 % in DI water. The precision in DI water was acceptable ranging from 8 to 38 % RSD. However, the precision in real environmental wastewaters could be poor, ranging from 15 to 120 % RSD, dependent upon unique matrix effects. In plasma, the overall recoveries of the EAPs were acceptable: 88 to 110 %, with %RSDs of 6 to 18 % (Table 3). The spiked recoveries of the TAM metabolites from plasma were good, ranging from 77 to 120 %, with %RSDs ranging from 27 to 32 %. Two of the TAM metabolites, 4-hydroxytamoxifen and n-desmethyl tamoxifen, were confirmed in most of the environmental aqueous samples. The discovery of TAM metabolites demonstrates that the source of the TAM metabolites, TAM, is constant, introducing a pseudo-persistence of this chemical into the environment.

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Acknowledgments

TLJL would like to thank her anonymous reviewers for their considerate and careful reviews. This paper is dedicated in memory of Dr. Theo Colburn, a pioneer in the study of environmental endocrine disruption; she was a true champion for the environment.

Notice

The US Environmental Protection Agency through its Office of Research and Development funded and managed the research described here. It has been subjected to the agency’s administrative review and approved for publication. Mention of trade names or commercial products does not constitute endorsement or recommendation for use.

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Authors and Affiliations

  1. US Environmental Protection Agency, National Exposure Research Laboratory, Office of Research and Development, P.O. Box 93478, Las Vegas, NV, 89193, USA

    Tammy L. Jones-Lepp, Randi L. Taniguchi-Fu, Jade Morgan, Trevor Nance Jr. & Matthew Ward

  2. US Geological Survey-Columbia Environmental Research Center, 4200 New Haven Road, Columbia, MO, 65201, USA

    David A. Alvarez

  3. US Environmental Protection Agency, National Human Health and Exposure Research Laboratory, Office of Research and Development, Narragansett, RI, 02882, USA

    Lesley Mills

Authors
  1. Tammy L. Jones-Lepp
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  2. Randi L. Taniguchi-Fu
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  3. Jade Morgan
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  4. Trevor Nance Jr.
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  5. Matthew Ward
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  6. David A. Alvarez
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  7. Lesley Mills
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Corresponding author

Correspondence to Tammy L. Jones-Lepp.

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Jones-Lepp, T.L., Taniguchi-Fu, R.L., Morgan, J. et al. Developing analytical approaches to explore the connection between endocrine-active pharmaceuticals in water to effects in fish. Anal Bioanal Chem 407, 6481–6492 (2015). https://doi.org/10.1007/s00216-015-8813-0

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  • DOI: https://doi.org/10.1007/s00216-015-8813-0

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