Health & Environmental Research Online (HERO)


Print Feedback Export to File
3858558 
Journal Article 
Analysis of perfluoroalkyl and polyfluoroalkyl substances in serum and plasma by solvent precipitation-isotope dilution-direct injection-LC/ MS/MS 
Harrington, LM 
2017 
Analytical Methods
ISSN: 1759-9660
EISSN: 1759-9679 
473-481 
A validated liquid chromatography tandem mass spectrometry (LC/MS/MS) method is presented for the analysis of per- and polyfluoroalkyl substances (PFAS) in serum and plasma. The method employs stableisotope labeled internal standard (IS) and surrogate recover standard (SRS) spiked serum or plasma samples that are mixed and precipitated with acetonitrile. Quantitation is performed with stable-isotope IS solvent (50 : 50 acetonitrile : water) calibration using one direct injection (DI) chromatographic analysis of precipitated sample supernate. The analytical method includes fifteen stable isotope labeled ISs, four SRSs ([1,2,3,4-C-13(4)]PFOA, [1,2-C-13(2)]PFUnA, [1,2,3,4-C-13(4)]PFOS, [2,3,4-C-13(3)]PFBA), and sixteen target analytes perfluoroalkyl carboxylic acids (PFCAs) (C4-C12), perfluoroalkyl sulfonic acids (PFSAs) (C4, C6, C8), N-ethyl perfluorooctane sulfonamido acetate (EtFOSAA), N-methyl perfluorooctane sulfonamido acetate (MeFOSAA), perfluorooctane sulfonamide (FOSA), and perfluorobutane sulfonamide (FBSA). Mean recoveries of control human plasma fortified with method target analytes over the range 2.5-175 ng mL(-1) (10-700 ng mL(-1) PFOS) are 83.7-103% with relative standard deviations (RSDs) of <= 14% (PFBA = 19%). Mean recoveries and RSDs of control human plasma fortified with mixed branched and linear isomer PFOA and PFHS (2.5 & 10.0 ng mL(-1)), and PFOS (10 & 40 ng mL(-1)) were 83.2% (RSD +/- 7.7%), 101% (RSD +/- 4.9%), and 101% (RSD +/- 6.5%) respectively. Mean recoveries of control bovine serum fortified with the method target analytes over the lower concentration range 0.250-175 ng mL(-1) (1-700 ng mL(-1) PFOS) are 82.8-103% with RSDs <= 15% (MeFOSAA = 16%, EtFOSAA = 17%). Mean recoveries and RSDs for 736 American Red Cross (ARC) study plasma samples fortified with SRSs at 1 ng mL(-1) were 89.0% (+/- 7.3% RSD) for [1,2,3,4-C-13(4)]PFOA, 91.8% (+/- 10% RSD) for [1,2-C-13(2)]PFUnA, and 89.4% (+/- 7.9% RSD) for [1,2,3,4-C-13(4)]PFOS. 
PFAS
• ^Per- and Polyfluoroalkyl Substances (PFAS)
     PFOA (335-67-1) and PFOS (1763-23-1)
          Literature Search – Adverse outcome pathway (2015-present)
               WOS
     PFUnA (2058-94-8)
          Literature Search
               WOS
     PFBA (375-22-4)
          Literature Search
               WOS
     PFOSA (754-91-6)
          Literature Search
               WOS
• PFBA
     Literature Search
          WOS
     Screening Results
          Excluded/Not on Topic
     Protocol References
• PFHxS
     Literature Search
          WOS
• PFOA (335-67-1) and PFOS (1763-23-1)
     Literature Search – Adverse outcome pathway (2015-present)
          WOS
     Screening Results
          Excluded/Not on Topic
     Literature Search Update (2013-2019)
          WOS
• PFOSA
     Literature Search
          WOS
     Screening Results
          Excluded/Not on Topic
• PFUnA
     Literature Search
          WOS
     Screening Results
          Excluded/Not on Topic