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Examining NTA performance and potential using fortified and reference house dust as part of EPA’s Non-Targeted Analysis Collaborative Trial (ENTACT)

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Abstract

Non-targeted analysis (NTA) methods are being increasingly used to aid in the identification of unknown compounds in the environment, a problem that has challenged environmental chemists for decades. Despite its increased use, quality assurance practices for NTA have not been well established. Furthermore, capabilities and limitations of certain NTA methods have not been thoroughly evaluated. Standard reference material dust (SRM 2585) was used here to evaluate the ability of NTA to identify previously reported compounds, as well as a suite of 365 chemicals that were spiked at various stages of the analytical procedure. Analysis of the unaltered SRM 2585 extracts revealed that several previously reported compounds can be identified by NTA, and that correct identification was dependent on concentration. A manual inspection of unknown features in SRM 2585 revealed the presence of two chlorinated and fluorinated compounds in high abundance, likely precursors to perfluorooctane sulfonate (PFOS) and perfluorohexane sulfonate (PFHxS). A retrospective analysis of data from the American Healthy Homes Survey revealed that these compounds were present in 42% of sampled homes. Spiking the dust at various stages of sample preparation revealed losses from extraction, cleanup, and instrumental analysis; the log Kow for individual compounds influenced the overall recovery levels but no pattern could be discerned from the various degrees of interference that the matrix had on the ionization efficiency of the spiked chemicals. Analysis of the matrix-free chemical mixture at low, medium, and high concentrations led to more correct identifications than analysis at one, very high concentration. Varying the spiked amount and identifying reported compounds at known concentrations allowed an estimation of the lower limits of identification (LOIs) for NTA, analogous to limits of detection in targeted analysis. The LOIs were much lower than levels in dust that would be likely to cause bioactivity in humans, indicating that NTA is useful for identifying and monitoring compounds that may be of toxicological concern.

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Acknowledgments

The authors would like to acknowledge John Wambaugh for providing pharmacokinetic modeled data. We would also like to acknowledge Paul Price for first applying the concept of thresholds of toxicological concern to NTA data. Matthew Scott Clifton is acknowledged for his valuable input, particularly regarding mechanisms of matrix interference.

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Author notes

  1. Randolph R. Singh

    Present address: Luxembourg Centre for Systems Biomedicine (LCSB), University of Luxembourg, 4365, Esch-sur-Alzette, Luxembourg

  2. Sarah Laughlin-Toth

    Present address: Aflac Cancer and Blood Disorders Center, Department of Pediatrics, Emory University School of Medicine, Atlanta, GA, 30322, USA

Authors and Affiliations

  1. Center for Computational Toxicology and Exposure, Office of Research & Development, U.S. Environmental Protection Agency, Research Triangle Park, NC, 27711, USA

    Seth R. Newton, Jon R. Sobus & Elin M. Ulrich

  2. Oak Ridge Institute for Science and Education, Post-Doctoral Participant, National Exposure Research Laboratory, Office of Research & Development, U.S. Environmental Protection Agency, Research Triangle Park, NC, 27711, USA

    Randolph R. Singh, Alex Chao & Sarah Laughlin-Toth

  3. Center for Environmental Measurement and Modeling, Office of Research & Development, U.S. Environmental Protection Agency, Research Triangle Park, NC, 27711, USA

    James McCord & Mark Strynar

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Correspondence to Seth R. Newton.

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Newton, S.R., Sobus, J.R., Ulrich, E.M. et al. Examining NTA performance and potential using fortified and reference house dust as part of EPA’s Non-Targeted Analysis Collaborative Trial (ENTACT). Anal Bioanal Chem 412, 4221–4233 (2020). https://doi.org/10.1007/s00216-020-02658-w

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