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LC-MS Analysis of PFAS Compounds in EPA Methods 537.1, 533 and 8327

Petra Lewits, Product Manager Analytical Chromatography, HPLC Columns, Cory Muraco, Product Manager, Liquid Chromatography Technology

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Article from Analytix Reporter - Issue 13

Introduction

PFAS (Per- and poly-fluoroalkyl substances) are persistent, man-made organic compounds, widely found in the environment. Recent awareness has brought attention to the toxicity of these substances. The U.S. Food and Drug Administration (FDA) and the U.S. Environmental Protection Agency (EPA) have initiated actions against PFAS. For determination of PFASs, liquid chromatography–mass spectrometry (LC-MS) is a commonly used technique.

The EPA has developed, validated, and published three methods to support the analysis of 29 PFAS in drinking water, method 533, 537 and 537.1. EPA 8327 covers the analysis of selected per- and polyfluoroalkyl substances (PFAS) in prepared extracts of various matrices (e.g., waters and solids) by liquid chromatography/tandem mass spectrometry (LC-MS/MS) analysis.

The Ascentis® Express PFAS HPLC column is designed for the separation of novel and legacy short-chain and long-chain PFAS compounds containing branched and linear isomers, whilst adhering to EPA methodology requirements.

Furthermore, a specific PFAS delay column prevents background PFAS contamination from interfering with the sample results in quantitative LC-MS methods (Figure 1).

LC-MS instrumental set-up for PFAS analysis & results of perfluorooctanoic acid (PFOA) (MRM 413.0>368.0) using a delay column

Figure 1.LC-MS instrumental set-up for PFAS analysis & results of perfluorooctanoic acid (PFOA) (MRM 413.0>368.0) using a delay column

The selectivity data for the different EPA method compounds under the conditions outlined in Table 1 is displayed in Figure 2-4 and Table 2.

LC-MS/MS analysis of PFAS compounds with Ascentis® Express PFAS column and PFAS Delay column under A) EPA Method 533 conditions; B) EPA Method 537.1 conditions and C) EPA Method 8327 conditions

Figure 2.PFAS analysis with Ascentis® Express PFAS column and PFAS Delay column under EPA Method 533 conditions (Peak IDs in Table 2)

LC-MS/MS analysis of PFAS compounds with Ascentis® Express PFAS column and PFAS Delay column under A) EPA Method 533 conditions; B) EPA Method 537.1 conditions and C) EPA Method 8327 conditions

Figure 3.PFAS analysis with Ascentis® Express PFAS column and PFAS Delay column under EPA Method 537.1 conditions (Peak IDs in Table 2)

LC-MS/MS analysis of PFAS compounds with Ascentis® Express PFAS column and PFAS Delay column under A) EPA Method 533 conditions; B) EPA Method 537.1 conditions and C) EPA Method 8327 conditions

Figure 4.PFAS analysis with Ascentis® Express PFAS column and PFAS Delay column under EPA Method 8327 conditions (Peak IDs in Table 2)

Table 1.LC-MS Conditions
Table 2.MS transition and retention data

Learn more about PFAS analysis at SigmaAldrich.com/PFAS

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1.
EPA Method 533: Determination of Per- and Polyfluoroalkyl Substances in Drinking Water by Isotope Dilution Anion Exchange Solid Phase Extraction and Liquid Chromatography/Tandem Mass Spectrometry. [Internet]. Available from: https://www.epa.gov/dwanalyticalmethods/method-533-determination-and-polyfluoroalkyl-substances-drinking-water-isotope
2.
EPA 537.1 Determination of Selected Per- and Polyfluorinated Alkyl Substances in Drinking Water by Solid Phase Extraction and Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS). [Internet]. Available from: https://nepis.epa.gov/Exe/ZyPURL.cgi?Dockey=P10111J4.txt
3.
EPA Method 8327 Per-and Polyfluoroalkyl Substances (PFAS) by Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS). [Internet]. Available from: https://www.epa.gov/hw-sw846/sw-846-test-method-8327-and-polyfluoroalkyl-substances-pfas-liquid-chromatographytandem
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