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. 2021 Nov 19;8(12):1085-1090.
doi: 10.1021/acs.estlett.1c00901.

Identification of an Analytical Method Interference for Perfluorobutanoic Acid in Biological Samples

Jacqueline T Bangma  1 , Jessica Reiner  2 , Rebecca C Fry  3 , Tracy Manuck  4 , James McCord  5 , Mark J Strynar  5
Affiliations

Identification of an Analytical Method Interference for Perfluorobutanoic Acid in Biological Samples

Jacqueline T Bangma et al. Environ Sci Technol Lett. .

Abstract

The investigation of per- and polyfluorinated alkyl substances (PFAS) in environmental and biological samples relies on both high- and low-resolution mass spectrometry (MS) techniques. While high-resolution MS (HRMS) can be used for identification and quantification of novel compounds, low-resolution MS is the more commonly used and affordable approach for studies examining previously identified PFAS. Of note, perfluorobutanoic acid (PFBA) is one of the smaller PFAS observed in biological and environmental samples and has only one major MS/MS transition, preventing the use of qualitative transitions for verification. Recently, our laboratories undertook a targeted investigation of PFAS in the human placenta from high-risk pregnancies utilizing low-resolution, targeted MS/MS. Examination of placental samples revealed a widespread (n = 93/122 (76%)) chemical interferent in the quantitative ion channel for PFBA (213 → 169). PFBA concentrations were influenced by up to ∼3 ng/g. Therefore, additional chromatographic and HRMS/MS instrumentation was utilized to investigate the suspect peak and putatively assign the identity of the interfering compound as the saturated oxo-fatty acid (SOFA) 3-oxo-dodecanoic acid.

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Conflict of interest statement

The research presented was not performed or funded by EPA and was not subject to EPA’s quality system requirements. The views expressed in this article are those of the author(s) and do not necessarily represent the views or the policies of the U.S. Environmental Protection Agency. The authors declare no competing financial interest.

Figures

Figure 1.
Figure 1.
(A) Low-resolution MS/MS analysis of a placental sample for PFBA internal standard (13C4–PFBA) and PFBA mass transition ion channels (precursor > product ion). (B) High-resolution MS analysis of a placental sample for 13C4PFBA precursor ion and native PFBA precursor ion. (C) On the high-resolution MS, a simulated low-resolution mass window (±0.5 m/z) was set around the mass of the PFBA precursor ion in placentas with high level of chemical interferent (P1), midlevel of chemical interferent (P2 and P3), and levels below detection for the low-resolution method (P4 and P5). (D) Identified interfering compound at mass 213.1496 m/z. All extracted ion chromatograms in each window are normalized to the largest peak to maintain scale across grouped traces.
Figure 2.
Figure 2.
Structure of 3-oxo-dodecanoic acid with major (59.0139) and minor (169.1598) ion fragmentation annotated.
See this image and copyright information in PMC

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