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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