Stable Carbon Isotope Analysis of Perfluorooctanoic Acid (PFOA) by Microflow-High Pressure Liquid Chromatography-Orbitrap Mass Spectrometry

IF 1.7 3区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Rapid Communications in Mass Spectrometry Pub Date : 2025-09-23 DOI:10.1002/rcm.10139

Paul K. Wojtal, Brett Davidheiser-Kroll, Chad S. Lane, Ralph N. Mead

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引用次数: 0

Abstract

Rationale

As contamination of perfluoroalkyl and polyfluoroalkyl substances (PFAS) in the environment becomes better understood, it is increasingly important to develop forensic tools capable of tracing contamination to emission sources. Isotopic methods have been previously inaccessible for PFAS due to limitations of the instrumentation, but high-pressure liquid chromatography (HPLC) coupled to Orbitrap mass spectrometry (Orbitrap MS) through electrospray ionization (ESI) allows measurement of the isotopic composition of individual PFAS compounds, such as perfluorooctanoic acid (PFOA).

Methods

Six separate supplier-procured powders of PFOA were analyzed for their δ¹³C isotopic composition by microflow-HPLC-ESI-Orbitrap MS.

Results

The method presented replicated, within error, the δ¹³C values measured using an elemental analyzer-isotope ratio mass spectrometer (EA-IRMS) for the six different supplier-procured PFOA powders. The offset from the EA-IRMS values for repeated analysis was between 0.2‰ and 1.1‰ and the error was between 0.8‰ and 1.5‰. Our Orbitrap-MS method requires approximately 0.04% of the material required to make an EA-IRMS measurement.

Conclusions

We developed a method capable of measuring the carbon isotopic composition of PFOA, using HPLC-Orbitrap MS, with high precision and accuracy. This will allow future research to expand analytical capabilities for additional isotopologues of PFOA and other PFAS compounds.

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微流-高压液相色谱-轨道阱质谱法分析全氟辛酸（PFOA）的稳定碳同位素

随着人们对环境中全氟烷基和多氟烷基物质（PFAS）的污染有了更好的了解，开发能够追踪污染到排放源的法医工具变得越来越重要。由于仪器的限制，以前无法使用同位素方法检测PFAS，但高压液相色谱法（HPLC）与Orbitrap质谱法（Orbitrap MS）通过电喷雾电离（ESI）可以测量单个PFAS化合物的同位素组成，如全氟辛酸（PFOA）。方法采用microflow-HPLC-ESI-Orbitrap质谱法对6种不同供应商采购的PFOA粉末的δ13C同位素组成进行了分析。结果该方法与元素分析仪-同位素比质谱仪（EA-IRMS）测量的6种不同供应商采购的PFOA粉末的δ13C值在误差范围内完全相同。与重复分析EA-IRMS值的偏移量在0.2‰~ 1.1‰之间，误差在0.8‰~ 1.5‰之间。我们的Orbitrap-MS方法所需的材料约为EA-IRMS测量所需材料的0.04%。结论建立了HPLC-Orbitrap质谱法测定PFOA碳同位素组成的方法，具有较高的精密度和准确度。这将使未来的研究能够扩大对全氟辛酸和其他全氟辛酸化合物的其他同位素物的分析能力。

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来源期刊

Rapid Communications in Mass Spectrometry 化学-分析化学

CiteScore

4.10

自引率

5.00%

发文量

219

审稿时长

2.6 months

期刊介绍： Rapid Communications in Mass Spectrometry is a journal whose aim is the rapid publication of original research results and ideas on all aspects of the science of gas-phase ions; it covers all the associated scientific disciplines. There is no formal limit on paper length ("rapid" is not synonymous with "brief"), but papers should be of a length that is commensurate with the importance and complexity of the results being reported. Contributions may be theoretical or practical in nature; they may deal with methods, techniques and applications, or with the interpretation of results; they may cover any area in science that depends directly on measurements made upon gaseous ions or that is associated with such measurements.