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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

A 100–250 mL sample is fortified with isotopically labeled analogues of the method analytes that function as isotope dilution standards. The sample is passed through an SPE cartridge containing polystyrene divinylbenzene with a positively charged diamino ligand to extract the method analytes and isotope dilution analogues. The cartridge is rinsed with sequential washes of aqueous ammonium acetate followed by methanol, then the compounds are eluted from the solid phase sorbent with methanol containing ammonium hydroxide. The extract is concentrated to dryness with nitrogen in a heated water bath. The extract volume is adjusted to 1.0 mL with 20% water in methanol (v/v), and three isotopically labeled isotope performance standards are added. Extracts are analyzed by LC-MS/MS in the MRM detection mode. The concentration of each analyte is calculated using the isotope dilution technique. For QC purposes, the percent recoveries of the isotope dilution analogues are calculated using the integrated peak areas of isotope performance standards, which are added to the final extract and function as traditional internal standards, exclusively applied to the isotope dilution analogues.

This is a solid phase extraction (SPE) liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of select per- and polyfluoroalkyl substances (PFAS) in drinking water. Method 533 requires the use of MS/MS in Multiple Reaction Monitoring (MRM) mode to enhance selectivity. Accuracy and precision data have been generated in reagent water and drinking water for the compounds included in the Analyte List.

This method is intended for use by analysts skilled in the performance of solid phase extractions, the operation of LC-MS/MS instrumentation, and the interpretation of the associated data.

Office of Water (MS-140)
EPA Document No. 815-B-19-020
EPA contract EP-C-17-014
November 2019