Determination of Polyfluoroalkyl Substances (PFAS) in Food Products

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1 Determination of Polyfluoroalkyl Substances (PFAS) in Food Products Agustin Pierri, PhD ASMS 2017 Indianapolis, IN

2 Background

3 Polyfluoroalkyl Substances (PFASs) Aliphatic backbone from C 4 on up Typically per-fluorinated Acid functional group Unique environmental chemistry Persistent Lipophilic Bioaccumulative

4 Polyfluoroalkyl Substances (PFASs) Uses? Repellents Performance chemicals Consumer and industrial goods

5 Polyfluoroalkyl Substances (PFASs) Routes of exposure Direct contact with food products Environmental exposure

6 Target compounds 6:2 FTS 8:2 FTS EtFOSA MeFOSA FOSA EtFOSE MeFOSE PFBA PFBS PFDA PFDS PFHpA PFHpS PFHxA PFHxS PFNA PFOA PFOS PFPeA PFDoA PFTeDA PFTrDA PFUdA Carboxylic acids Sulfonic acids Sulfonamides Sulfonamido-ethanols

7 Sample prep

8 Sample prep approach SPE: Only suitable for water samples Weak anion exchange offline SPE QuEChERS: Suitable for non-liquid samples

9 QuEChERS Screening: C18 d-spe C18 d-spe + hexanes PSA/GCB d-spe C18/GCB d-spe C18/GCB d-spe + hexanes EMR-L

10 EMR-Lipids procedure Weigh 2.0 grams homogenized sample into 50 ml tube Add 10 ml MeCN, vortex 3 minutes Add 2 g of EMR-L + 10 ml H 2 O Vortex 1 minute, centrifuge 5 minutes Transfer 5 ml aliquot to tube with 2.5 g NaCl/MgSO 4 Transfer 200 µl to conical vial for analysis Based on: Anumol, T., Lehotay, S.J., Stevens, J. et al. Anal Bioanal Chem (2017) 409: 2639

11 Analysis: LC/MS

12 PFAS by LC/MS Unique analytical challenges Low levels Relative polarities Isomers Contamination

13 Sensitivity 1290 LC, 6460 QQQ Choosing the right mobile phase modifier

14 Mobile phase modifiers for ESI Negative mode Ammonium salts Ammonium acetate Ammonium formate Ammonium fluoride the secret sauce (usually)

15 Mobile phase vs PFBA Ammonium acetate Acetic acid Ammonium formate Ammonium fluoride Most polar:

16 Chromatographic conditions Column: Zorbax RRHD Eclipse Plus C18 50 x μm Injection volume: 2 μl Mobile phase: A: Water with 0.05% acetic acid B: Acetonitrile with 0.05% acetic acid Flow rate: ml/min Time %B

17 Mid level chromatogram (1 ppb)

18 Low level (0.1 ppb) Low levels:

19 Solvent blank Instrument contamination:

20 Branched vs. linear sulfonates PFHxS PFOS Isobars:

21 Dynamic range Calibrates up to 0.1 ppb 1000 ppb

22 Method performance

23 Extracts Blank Milk Egg Fish Butter

24 PFBA PFPeA PFBS PFHxA PFHpA PFHxS 6:2 FTS PFOA PFHpS PFOS PFNA FOSA Me-FOSE 8:2 FTS Me-FOSA PFDA Et-FOSE Et-FOSA PFDS PFUdA PFDoA PFTrDA PFTeDA Absolute recoveries, milk 160 Milk, ESTD

25 PFBA PFPeA PFBS PFHxA PFHpA PFHxS 6:2 FTS PFOA PFHpS PFOS PFNA FOSA Me-FOSE 8:2 FTS Me-FOSA PFDA Et-FOSE Et-FOSA PFDS PFUdA PFDoA PFTrDA PFTeDA Absolute recoveries, egg 160 Egg, ESTD

26 PFBA PFPeA PFBS PFHxA PFHpA PFHxS 6:2 FTS PFOA PFHpS PFOS PFNA FOSA Me-FOSE 8:2 FTS Me-FOSA PFDA Et-FOSE Et-FOSA PFDS PFUdA PFDoA PFTrDA PFTeDA Absolute recoveries, butter 160 Butter, ESTD

27 PFBA PFPeA PFBS PFHxA PFHpA PFHxS 6:2 FTS PFOA PFHpS PFOS PFNA FOSA Me-FOSE 8:2 FTS Me-FOSA PFDA Et-FOSE Et-FOSA PFDS PFUdA PFDoA PFTrDA PFTeDA Absolute recoveries 160 Fish, ESTD

28 PFBA PFPeA PFBS PFHxA PFHpA PFHxS 6:2 FTS PFOA PFHpS PFOS PFNA FOSA Me-FOSE 8:2 FTS Me-FOSA PFDA Et-FOSE Et-FOSA PFDS PFUdA PFDoA PFTrDA PFTeDA Isotopic dilution corrected recoveries, milk 160 Milk, ESTD ISTD

29 PFBA PFPeA PFBS PFHxA PFHpA PFHxS 6:2 FTS PFOA PFHpS PFOS PFNA FOSA Me-FOSE 8:2 FTS Me-FOSA PFDA Et-FOSE Et-FOSA PFDS PFUdA PFDoA PFTrDA PFTeDA Isotopic dilution corrected recoveries, egg 160 Egg, ESTD ISTD

30 PFBA PFPeA PFBS PFHxA PFHpA PFHxS 6:2 FTS PFOA PFHpS PFOS PFNA FOSA Me-FOSE 8:2 FTS Me-FOSA PFDA Et-FOSE Et-FOSA PFDS PFUdA PFDoA PFTrDA PFTeDA Isotopic dilution corrected recoveries 160 Butter, ESTD ISTD

31 PFBA PFPeA PFBS PFHxA PFHpA PFHxS 6:2 FTS PFOA PFHpS PFOS PFNA FOSA Me-FOSE 8:2 FTS Me-FOSA PFDA Et-FOSE Et-FOSA PFDS PFUdA PFDoA PFTrDA PFTeDA Isotopic dilution corrected recoveries 160 Fish, ESTD ISTD

32 PFBA PFPeA PFBS PFHxA PFHpA PFHxS 6:2 FTS PFOA PFHpS PFOS PFNA FOSA Me-FOSE 8:2 FTS Me-FOSA PFDA Et-FOSE Et-FOSA PFDS PFUdA PFDoA PFTrDA PFTeDA Robust and versatile method for PFAS in food Challenges unique to PFAS Trace levels MRL at 0.5 ng/g Instrument contamination Resolution Handle complicated matrix Butter, ISTD

33 Questions? Agustin Pierri Weck Laboratories, Inc. Industry, CA 91745

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