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A Straightforward Method for the Extraction, Cleanup, and Quantitative Analysis of 45 PFAS in Whole Fish
Citation:
Balgooyen, S., M. Scott, B. Blackwell, Mike Mahon, R. Lepak, W. Backe, AND E. Pulster. A Straightforward Method for the Extraction, Cleanup, and Quantitative Analysis of 45 PFAS in Whole Fish. SETAC North America 45th Annual Meeting, Fort Worth, TX, October 20 - 24, 2024. https://doi.org/10.23645/epacomptox.28219952
Impact/Purpose:
This work highlights the needs for alternative analytical methods when established methods do not meet research objectives. The method outlined in this work will be broadly applied to the analysis of whole fish at GLTED which will inform trend of PFAS in fish historically, spatially, and based on trophic level.
Description:
Analytically, Per- and polyfluoroalkyl substances (PFAS) can be challenging to quantify due to the complex matrices in which they are found and/or due to their physical chemical properties which can vary widely within and between homologous series. Recently, EPA method 1633 was applied to whole-fish homogenates which resulted in substandard precision and accuracy even after various modifications. This study introduces and validates a new method for extraction and cleanup of PFAS from whole-body fish tissue. The new method uses lipid removal technology to rapidly and efficiently remove undesirable matrix interferents from the extract without the need for solid-phase extraction or evaporative concentration and solvent exchange. The analyte recovery of the presented method is high (average of 86 ± 13%) and the data produced are accurate and precise (96 ± 9% compared to spiked concentration). Twenty-three of the PFAS exhibit no matrix effects; the highest degree of matrix suppression is a reduction in signal of 48%. Additionally, 43% of the method detection limits are at or below the those outlined in EPA method 1633; only seven compounds have detection limits that exceed 3x of those reported in 1633. Lyophilization was evaluated as a preservation technique for biological tissue, which results in the loss of only a few volatile compounds. The method outlined here was demonstrated on a taxonomically diverse set of whole-fish composites from Lake Michigan collected in 1994 that were part of a larger study on environmental contaminants. The results reveal that in this set of samples the magnitude of PFAS contamination in fish is driven by collection location, while the distribution of PFAS is driven by species type. Stable isotope data and redundancy analysis demonstrate that sulfonates and sulfonamides are more common with lower trophic level fish while long-chain carboxylates are more common fish with offshore habitat use. Additionally, this method is being applied to an archive Lake Trout that has been annually collected in the Great Lakes from the 1970s’ to the current day and results of that analysis will also be presented. Disclaimer: This work does not necessarily reflect U.S. E.P.A. views or policy and any reference to commercial products does not imply an endorsement.
URLs/Downloads:
DOI: A Straightforward Method for the Extraction, Cleanup, and Quantitative Analysis of 45 PFAS in Whole Fish
ORD-060794 A STRAIGHTFORWARD METHOD FOR THE EXTRACTION, CLEANUP, AND QUANTITATIVE ANALYSIS OF 45 PFAS IN WHOLE FISH- 508.PDF (PDF, NA pp, 1846.384 KB, about PDF)