Development of a New Standardized Method for the Analysis of PFAS in Consumer Products

Crafting Consensus Methods for Environmental Sampling and Measurement
Oral Presentation

Prepared by M. Deible1, L. Miller2, W. Lipps2, R. Hale1
1 - RJ Lee Group, 800 Presque Isle Drive, Headquarters, Pittsburgh, PA, 15239, United States
2 - Shimadzu Scientific Instruments, Inc., 7102 Riverwood Drive, Columbia, MD, 21046, United States


Contact Information: [email protected]; 724-3871943

ABSTRACT

Per- and polyfluoroalkyl substances (PFAS) analysis has primarily focused on PFAS within environmental matrices. The analytical instruments used in these methods are applicable to other materials such as plastics, textiles, paper, cosmetics, etc, however there are no standardized methods validated for these matrices. In response, we have chosen to develop and standardize a new PFAS method with ASTM Committee F15 on consumer products. This test method will cover the determination of PFAS in solid matrices by solvent extraction, filtering, and separation using LC-MS/MS. Additional characterization of the extracted samples was accomplished by high resolution mass spectrometry (QTOF) which provided information on interferences and other PFAS compounds not targeted in the quantitative analysis. Further characterization included total organic fluorine ion chromatography analysis. PFAS extraction from solid test specimens or subsamples utilized a basic water/methanol mixture. Following extraction, the samples undergo a sequence of centrifugation, filtration, and acidification. Aliquots of the resulting extract are transferred to a silanized vial and introduced to LC-MS/MS instrumentation for quantitation using multiple reaction monitoring (MRM). This method specifically measures nonvolatile and semi-volatile PFAS compounds that readily leach or are soluble under the extraction conditions. This method does not measure volatile PFAS or PFAS present in the form of fluoropolymers, including fluorinated organic compounds that may be present in or polymerized within plastic products. The methodology was developed using a Shimadzu triple quadrupole mass spectrometer (LCMS-8060NX) operating in negative mode, coupled with an HPLC (Nexera X3). This approach successfully encompassed 44 target PFAS compounds with an additional 20 surrogates separated within 17 minutes on a reverse phase column. Quantification was accomplished using an external calibration curve model with calibrators ranging between 5-2000 ng/L (dependent on specific target). All calibration curves maintained R2 values above 0.99 and less than 30 %RSD.