用氟核磁共振波谱法对包括三氟乙酸在内的总 PFAS 进行定量,Analytical Chemistry

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用氟核磁共振波谱法对包括三氟乙酸在内的总 PFAS 进行定量
Analytical Chemistry ( IF 6.7 ) Pub Date : 2023-03-22 , DOI: 10.1021/acs.analchem.2c05354
Dino Camdzic ₁ , Rebecca A Dickman ₁ , Abigail S Joyce ₂ , Joshua S Wallace _{1,

3} , P Lee Ferguson ₂ , Diana S Aga _{1,

3}

Affiliation

氟核磁共振 ( ¹⁹ F-NMR) 光谱已被证明是一种强大的工具，能够量化复杂样品中全氟烷基物质和多氟烷基物质 (PFAS) 的总量。该技术依赖于烷基链中的特征末端-CF ₃位移(-82.4 ppm)进行定量，并且不会由于样品制备或基质效应而引入偏差。传统的 PFAS 定量分析技术，例如液相色谱-质谱 (LC-MS) 和燃烧离子色谱 (CIC)，存在固有的局限性，使得总氟分析具有挑战性。在这里，我们报告了一种用于分析总 PFAS 的灵敏^{19 F-NMR 方法，检测限为 99.97 nM，即 50 μg/L 全氟磺酸。}^{为了证明19} F-NMR的功能，该技术与两种常用的 PFAS 分析方法进行了比较：总可氧化前体 (TOP) 测定和 LC-高分辨率 MS 分析，用于目标定量和疑似筛查。在这两种情况下，¹⁹ F-NMR 分析检测到的 PFAS 总量高于 TOP 测定 (63%) 或 LC-MS 分析 (65%)，这表明 LC-MS 和 TOP 测定可能导致 PFAS 漏报。重要的是，¹⁹ F-NMR 检测到三氟乙酸的浓度超过使用 LC-MS 在废水样品中定量的总 PFAS 浓度的五倍。因此，使用¹⁹ F-NMR 定量高度复杂样品中的总 PFAS 可以补充经典的 TOP 或 LC-MS 方法，从而更准确地报告环境中的 PFAS 污染。

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Quantitation of Total PFAS Including Trifluoroacetic Acid with Fluorine Nuclear Magnetic Resonance Spectroscopy

Fluorine nuclear magnetic resonance (¹⁹F-NMR) spectroscopy has been shown to be a powerful tool capable of quantifying the total per- and polyfluoroalkyl substances (PFAS) in a complex sample. The technique relies on the characteristic terminal −CF₃ shift (−82.4 ppm) in the alkyl chain for quantification and does not introduce bias due to sample preparation or matrix effects. Traditional quantitative analytical techniques for PFAS, such as liquid chromatography–mass spectrometry (LC-MS) and combustion ion chromatography (CIC), contain inherent limitations that make total fluorine analysis challenging. Here, we report a sensitive ¹⁹F-NMR method for the analysis of total PFAS, with a limit of detection of 99.97 nM, or 50 μg/L perfluorosulfonic acid. To demonstrate the capabilities of ¹⁹F-NMR, the technique was compared to two commonly used methods for PFAS analysis: total oxidizable precursor (TOP) assay and LC-high resolution MS analysis for targeted quantification and suspect screening. In both cases, the ¹⁹F-NMR analyses detected higher total PFAS quantities than either the TOP assay (63%) or LC-MS analyses (65%), suggesting that LC-MS and TOP assays can lead to underreporting of PFAS. Importantly, the ¹⁹F-NMR detected trifluoroacetic acid at a concentration more than five times the total PFAS concentration quantified using LC-MS in the wastewater sample. Therefore, the use of ¹⁹F-NMR to quantify the total PFAS in highly complex samples can be used to complement classic TOP or LC-MS approaches for more accurate reporting of PFAS contamination in the environment.

更新日期：2023-03-22

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