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Related Experiment Video

Updated: Jul 11, 2025

Identifying Per- and Polyfluorinated Chemical Species with a Combined Targeted and Non-Targeted-Screening High-Resolution Mass Spectrometry Workflow
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Advancing PFAS characterization: Enhancing the total oxidizable precursor assay with improved sample processing and

David Patch1, Natalia O'Connor1, Taylor Vereecken1

  • 1Environmental Sciences Group, Department of Chemistry and Chemical Engineering, Royal Military College of Canada, Kingston, ON K7K 7B4, Canada.

The Science of the Total Environment
|November 12, 2023
PubMed
Summary

This study enhances the total oxidizable precursor (TOP) assay for quantifying per- and polyfluoroalkyl substances (PFAS). Optimized sample processing and UV activation improve PFAS precursor detection in environmental samples.

Keywords:
6:2 FTSAFFFAnalysisPFOAPFOSTOP assay

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Area of Science:

  • Environmental Chemistry
  • Analytical Chemistry
  • Chemical Analysis

Background:

  • Over 9000 per- and polyfluoroalkyl substances (PFAS) exist, but standard methods quantify fewer than 50.
  • The total oxidizable precursor (TOP) assay converts undetectable PFAS precursors to measurable PFAS.
  • Previous TOP assay methods suffered from significant PFAS loss during sample processing.

Purpose of the Study:

  • To investigate and optimize sample processing methods to minimize PFAS loss during the TOP assay.
  • To evaluate ultraviolet (UV) light as an alternative activation method to thermal activation in the TOP assay.
  • To assess the enhanced TOP assay's performance on real-world samples like aqueous film-forming foams (AFFF).

Main Methods:

  • Utilized mass-labelled perfluorooctane sulfonic acid (PFOS) to quantify losses during sample work-up.
  • Employed methanolic acetic acid as a chemical quencher to improve PFOS recovery.
  • Compared heat-activated and UV-activated TOP assays for perfluorooctanoic acid (PFOA), PFOS, and 6:2 fluorotelomer sulfonate (6:2 FTS) oxidation.
  • Applied the UV-activated TOP assay to AFFF formulations and field samples from firefighting vehicles, analyzed via high-resolution mass spectrometry.

Main Results:

  • Identified up to 50% loss of PFOS during sample work-up, which was corrected using mass-labelled PFOS and chemical quenching.
  • The UV-activated TOP assay achieved 100% oxidation of 6:2 FTS in 7.5 minutes with 108% ± 8% total yield of perfluorinated carboxylic acids (PFCAs).
  • Successfully identified various fluorotelomer precursors in AFFF samples using the enhanced analytical approach.

Conclusions:

  • Optimized sample processing, including chemical quenching, significantly improves PFAS recovery in the TOP assay.
  • UV activation offers a faster and more efficient alternative to thermal activation for the TOP assay.
  • The modified TOP assay, incorporating UV activation and improved sample handling, provides a more reliable and quantitative method for comprehensive PFAS characterization.