Analysis of Per-and Polyfluoroalkyl Substances (PFAS) Specified in EPA M533 Using the Triple Quadrupole LCMSMS

Polyfluoroalkyl Substances (PFAS) in the Environment
Poster Presentation

Prepared by R. Marfil-Vega, C. Gilles, W. Lipps
Shimadzu Scientific Instruments, 7102 Riverwood Drive, Columbia, MD, 21046, United States

Contact Information: [email protected]; 410-910-0884


Recently, EPA announced a new method for testing short chain per and polyfluoroalkyl substances (PFAS) in drinking water. Method 533 measures PFAS by isotope dilution anion exchange solid phase extraction and liquid chromatography/tandem mass spectrometry (LC-MS/MS). The lowest concentration minimum reporting levels (LCMRLs) for the method analytes range from 1.4 to 16 nanograms/L ((ng/L) or parts per trillion (ppt)). Shimadzu Scientific Instruments was one of eight laboratories that participated in providing EPA with outside laboratory validation data along with a review of the method draft. This poster includes Shimadzu Scientific Instruments data from the validation study.
The LC/MS/MS analysis was performed using a UHPLC system coupled with Shimadzu LCMS -8045 triple quadrupole mass spectrometer. Chromatography was adjusted to obtain maximum resolution between peaks in the shortest time possible with minimum co-elution of isomers. Compounds, including PFHxS and PFOS isomers, were separated using optimized conditions.
A thirteen-point calibration was performed ranging from 0.1 ppt to 100 ppt, all compounds were linear with r2 values greater than 0.99. Accuracies for all calibration levels and check standards were within 70-130% with percent relative standard deviation (%RSD) below 20%. Data for the precision and accuracy studies in reagent water (RW) and tap water (TW) was performed at 10 ppt concentration level, recoveries of all analytes within a range of 70-130% with %RSD’s below 20% for all method analyte.