W.C.K Pomerantz James L. Gray Laura E. Hubbard Dana W. Kolpin W.A. Arnold K.A. Faber 2025 <p><span>Fluorinated organic contaminants, including per- and polyfluoroalkyl substances (PFASs) and fluorinated pesticides and pharmaceuticals (FPPs), pose a persistent threat to environmental health. Widely used liquid chromatography-tandem mass spectrometry (LC-MS/MS) methods fail to capture large fractions of total organofluorine in environmental samples, confounding the assessment of fluorinated contamination. Fluorine-19 nuclear magnetic resonance spectroscopy (</span>¹⁹<span>F-NMR) is an inclusive method for total and class-based organofluorine analysis. Here, we apply&nbsp;</span>¹⁹<span>F-NMR to 31 effluent, surface water, and foam samples collected at 13 potential organofluorine point sources or source regions and compare the results to targeted LC-MS/MS for 34 or 64 PFASs. LC-MS/MS detected a median of 11.4% of total organofluorine detected by&nbsp;</span>¹⁹<span>F-NMR (range: nondetect to 8190 nM F&nbsp;</span>¹⁹<span>F-NMR; nondetect to 8010 nM F LC-MS/MS). The highest&nbsp;</span>¹⁹<span>F-NMR total organofluorine concentrations, detected in wastewater treatment plant (WWTP)-associated foam and at a soy oil production facility, arose from resonances characteristic of per- and polyfluorinated alkyl chains.&nbsp;</span>¹⁹<span>F-NMR resonances from aryl CF</span>₃<span>&nbsp;moieties were abundant in the WWTP-associated samples, consistent with prior reports of substantial contributions from pharmaceuticals to WWTP effluents.&nbsp;</span>¹⁹<span>F-NMR enables the quantitative assessment of total organofluorine and qualitative insight into fluorinated structures, providing complementary analysis of organofluorine compounds missed by targeted mass spectrometry-based protocols.</span></p> application/pdf 10.1021/acs.est.5c05079 en ACS Publications Revealing organofluorine contamination in effluents and surface waters with complementary analytical approaches: Fluorine-19 nuclear magnetic resonance spectroscopy (19F-NMR) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) article