22 Environmental Laboratory - Spotlight on PFAS
Figure 3. TIC of an 80 ng/L extracted fortifi ed laboratory fi eld blank sample containing all method analytes, surrogates, and internal standards. a. Experimental DL was determined from ten LFB replicates fortifi ed at ~4.0 ng/L measured over three days and calculated according to section 9.2.8 in EPA Method 537.1 rev 2.0
b. Reference DL values from EPA Method 537.1 rev 2.0 (Table 5) determined from seven LFB replicates fortifi ed at 4.0 ng/L measured over three days and calculated according to section 9.2.8
c. Experimental LCMRLs were determined from ten replicates each at fi ve fortifi cation levels ranging from ~0.2 – 80 ng/L using the EPA LCMRL Calculator.11 d. Reference LCMRL values from EPA Method 537.1 rev 2.0 (Table 5).
e. Experimental MRLs were determined from seven LFBs fortifi ed at concentrations ranging from ~0.2 to 4.0 ng/L according to section 9.2.6 of EPA Method 537.1 rev 2.0 using the Half Range prediction interval method with confi rmed upper and lower Prediction Interval Results (PIR) ≤150% and ≥50%, respectively.
Table 3. Method detection limits and lowest concentration minimum reporting limits and minimum reporting levels determined experimentally on the QSight® LC/MS/MS system and compared to reference values report in EPA Method 537.1.
Analyte PFBS PFHxA
HFPO-DA PFHpA PFHxS ADONA PFOA PFOS PFNA
9Cl-PF3ONS PFDA
NMeFOSAA PFUnA
NEtFOSAA
11Cl-PF3OUdS PFDoA PFTrDA PFTA
Experimental DL (ng/L)a
1.1 1.5 1.5 1.6 1.2 1.4 1.3 1.4 1.6 1.1 1.1 1.2 1.3 1.2
0.66 1.2 1.0
0.86
EPA 537.1 DL (ng/L)b
6.3 1.7 4.3
0.63 2.4
0.55 0.82 2.7
0.83 1.8 3.3 4.3 5.2 4.8 1.5 1.3
0.53 1.2
spectrometer to eliminate the leaching of fl uorochemicals from components within the systems. Manual SPE confi gurations also require mitigative steps to eliminate any components constructed of PTFE to minimize or eliminate any PFAS contamination. PerkinElmer offers kits and knowhow to streamline remediation. The use of high-grade reagents and PFAS-free laboratory accessories are also critical. By implementing steps to remove or reduce background contamination and appropriate sample preparation, PerkinElmer’s highly sensitive QSight®
220 LC/MS/MS system
Experimental LCMRL (ng/L)c
0.72 0.93 0.57 0.10 0.60 ND
0.34 1.0
0.50 0.68 0.40 0.22 0.30 0.73 0.39 0.19 0.82 1.5
EPA 537.1 LCMRL (ng/L)d
1.8 1.0 1.9
0.71 1.4
0.88 0.53 1.1
0.70 1.4 1.6 2.4 1.6 2.8 1.5 1.2
0.72 1.1
Experimental MRL (ng/L)e
1.4
0.30 1.6 1.6
0.29 0.28 0.30 0.29 1.6 1.5
0.30 0.30 1.6 1.6
0.28 0.30 4.0 4.0
has proven to be extremely capable of meeting the challenging demands of low-level PFAS analysis in drinking water. Validation studies demonstrated that the instrument easily meets stringent requirements of EPA 537.1 and 533 regulations for all targeted analytes.
References 1. Nakayama, S. F. et al., Worldwide trends in tracing poly- and
IET JANUARY / FEBRUARY 2023
perfl uoroalkyl substances (PFAS) in the environment. Trends in Analytical Chemistry [Accessed August 30th, 2022] https://doi. org/10.1016/
j.trac.2019.02.011
2. Agency for Toxic Substances and Disease Registry, “Per- and Polyfl uoroalkyl Substances (PFAS) and Your Health”, last review July 6th, 2022 [Accessed August 30th, 2022]
https://www.atsdr.
cdc.gov/pfas/index.html.
3. Lindstrom, A. B. et al., Polyfl uorinated Compounds: Past, Present, and Future, Environ. Sci. Technol. 2011, 45, 7954– 7961.
4. Ciofi , L.; Renai, L.; Rossini, D.; Ancillotti, C.; Falai, A.; Fibbi, D.; Bruzzoniti, M.; Santana-Rodriguez, J. J.; Orlandini, S.; Del Bubba, M.; Applicability of the direct injection liquid chromatographic tandem mass spectrometric analytical approach to the sub-ng /L determination of perfl uoro-alkyl acids in waste, surface, ground and drinking water samples, Talanta, 2018, 176, 412- 421.
5. Schultz, M. M.; Barofsky, D. F.; Field, J. A.; Quantitative determination of fl uorinated alkyl substances by large- volumeinjection liquid chromatography tandem mass spectrometry characterization of municipal wastewaters, Environ. Sci. Technol. 2006, 40 (1), 289–295.
6. Sébastien Sauvé et al., Worldwide drinking water occurrence and levels of newly-identifi ed perfl uoroalkyl and polyfl uoroalkyl substances, Science of The Total Environment, 2018, 616–617, 1089-1100.
9. Shoemaker, J. and Dan Tettenhorst. Method 537.1: Determination of Selected Per- and Polyfl uorinated Alkyl Substances in Drinking Water by Solid Phase Extraction and Liquid Chromatography/Tandem Mass Spectrometry (LC/ MS/ MS). U.S. Environmental Protection Agency, Offi ce of Research and Development, National Center for Environmental Assessment, Washington, DC, 2018
10. ISO 25101:2009 Water quality — Determination of perfl uorooctanesulfonate (PFOS) and perfl uorooctanoate (PFOA) — Method for unfi ltered samples using solid phase extraction and liquid chromatography/mass spectrometry [Accessed August 30th, 2022]
https://www.iso.org/ standard/
42742.html
11. USA EPA Method 533 [Accessed August 30th, 2022] Method 533: Determination of Per- and Polyfl uoroalkyl Substances in Drinking Water by Isotope Dilution Anion Exchange Solid Phase Extraction and Liquid Chromatography/ Tandem Mass Spectrometry (
epa.gov)
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