A high-throughput small volume matrix based calibration using isotope dilution liquid chromatography tandem mass spectrometry analysis for 42 per and polyfluoroalkyl substances in groundwater

Abstract

A novel method for the determination of per- and polyfluoroalkyl substances (PFAS) in groundwater is presented using a subsample, matrix-matched calibrators, 96-well plate solid phase extraction (SPE), and ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Accuracy, precision, measurement of uncertainty (MOU), method detection limit (MDL), method quantitation limit (MQL), analytical measurement range, interferences/ion suppression, and analyte stability were determined as part of the in-house method validation. The method quantitates 42 PFAS compounds from nine different compound classes. Accuracy for the reference material (RM) and matrix spike (MS) ranged from 52.3 to 117.8 %, and precision for the MS and matrix spike duplicate (MSD) had a coefficient of variation (CV) from 2.0 % to 23.3 %. MDLs spanned from 0.07 to 1.97 ng L−1, with MQLs ranging from 0.20 to 5.90 ng L−1. Suppression studies determined that iron and manganese have effects on analytes that do not have paired isotopically labeled standards. The results from the in-house validation indicated that this Michigan Department of Health and Human Services laboratory developed test meets the necessary accuracy, precision, MDL, MQL and reporting limits requirement established by the laboratory's quality system essentials (QSEs) and select criteria from the Department of Defense (DoD) Quality Systems Manual for Environmental Laboratories and American Industrial Hygiene Association Laboratory Accreditation Program, LLC (AIHA LAP, LLC) accrediting International Standard Organization (ISO/IEC 17025:2017) check list.