Introduction

Per- and polyfluoroalkyl substances (PFAS) are human-made chemicals in aqueous film forming foam (AFFF) whichis used to suppress jet fuel fires and is routinely utilized on airbases. PFASs are also useful in a variety of consumerproducts such as surface treatment for textiles, packaging materials, and non-stick cookware. PFASs are stable,bioaccumulate, referred to today in the media as forever chemicals, and they have become ubiquitous throughoutthe global environment.

The EPA has established health advisory levels at 70 parts per trillion (ppt) perfluorooctanoic acid (PFOA) andperfluorooctanesulfonic acid (PFOS) in drinking water to account for an expected lifetime of exposure.

While these chemicals have been studied for many decades, PFOA replacement compounds, such as GenX andmetabolites, are also spreading throughout the environment while their toxicology studies are still beingcharacterized. The 2019 EPA PFAS Action Plan is committed to establishing requirements, including safe drinkingwater and characterizing the most commonly known PFAS among the thousands that have been identified.

EPA Method 537.1: PFAS in Drinking WaterScott Krepich1 and Agustin Pierri2, PhD1Phenomenex, Inc., 411 Madrid Ave., Torrance, CA 90501 USA2Weck Laboratories, Industry, CA 91745 USA

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Experimental Conditions

Sample Preparation:A 250 mL sample is fortified with surrogates and passed through a solid phase extraction (SPE) cartridge containingpolystyrenedivinylbenzene (SDVB), such as Strata® SDB-L 500 mg/6 mL (8B-S014-HCH). The compounds are elutedfrom the SPE sorbent with methanol. After drying the eluent with nitrogen in a heated water bath, adjust the finalvolume to 1 mL with 96:4 water in methanol (v/v) and add internal standards before analyzing by LC-MS/MS.

Overview

This technical brief outlines the solid phase extraction (SPE) and liquid chromatography (HPLC) parametersincluded in the reversed phase SPE liquid chromatography / tandem mass spectrometry (LC-MS/MS) proceduredetailed in the EPA Method 537.1.

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Column:

Dimension:

Part No.:

Mobile Phase:

Injection Volume:

Detection:

Flow Rate:

Gradient:

Luna® Omega 1.6 µm PS C18

100 x 2.1 mm

00D-4752-AN

A: 0.1% Acetic Acid in Water

B: Methanol

4 µL

Electrospray Ionization Tandem Mass Spectrometer (ESI-MS/MS)

0.7 mL/min

HPLC Parameters

Time

(min)

%A %B

0 80 20

0.5 70 30

7 10 90

7.5 0 100

9 0 100

Full Target List

Analyte RT (min) Internal Standard

PFBS 2.29 13C4-PFOS

PFHxA 3.20 13C2-PFOA

HFPO-DA 3.55 13C2-PFOA

PFHpA 4.24 13C2-PFOA

PFHxS 4.39 13C4-PFOS

ADONA 4.41 13C2-PFOA

PFOA 5.08 13C2-PFOA

PFOS 5.72 13C4-PFOS

PFNA 5.77 13C2-PFOA

9Cl-PF3ONS 6.15 13C4-PFOS

PFDA 6.35 13C2-PFOA

NMeFOSAA 6.70 d3-NMeFOSAA

PFUnA 6.83 13C2-PFOA

NEtFOSAA 6.88 d3-NMeFOSAA

11Cl-PF3OUdS 7.17 13C4-PFOS

PFDoA 7.37 13C2-PFOA

PFTrDA 7.80 13C2-PFOA

PFTA 8.18 13C2-PFOA

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Reference

EPA Method 537.1 ‘ Determination of Selected Per- and Polyfluorinated Alkyl Substances in Drinking Water

By Solid Phase Extraction and Liquid Chromatography / Tandem Mass Spectrometry’ (Version 2.0, March

2020) https://cfpub.epa.gov/si/si_public_file_download.cfm?p_download_id=537290&Lab=NERL

PFAS Replacement Compounds

Ap

p ID

25

84

3

HFPO-DA

11Cl PF3OUdS

PF3ONS9CI

-

-

ADONA

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Terms and Conditions

Subject to Phenomenex Standard Terms and Conditions, which may be viewed at www.phenomenex.com/TermsAndConditions.

Trademarks

Luna Omega and Strata are registered trademarks and BE-HAPPY is a trademark of Phenomenex.

FOR RESEARCH USE ONLY. Not for use in clinical diagnostic procedures.

© 2020 Phenomenex, Inc. All rights reserved.TN7

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