Page 22 - Application Notebook - PFAS Analysis
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Application   No. C184
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          Table 8. Average conc. (n = 7), % recovery and % RSD of surrogates in spiked samples using LCMS-8045 and LCMS-8050

                                                    LCMS-8045                             LCMS-8050
                           Fortified
            Compound
                          Conc. (ng/L)  Average Conc                         Average Conc
                                       (ng/L), n=7  % Recovery    % RSD       (ng/L), n=7  % Recovery    % RSD


             M2PFHxA          40          43           107          14           40          101           10

             M2PFDA           40          44           109          12           42          106           13

           M-N-EtFOSAA       160          175          109          14           160         100          12


          Surrogate Recovery                                       Summary and Conclusions
          Surrogate recovery was similarly investigated by first  This application note described and demonstrated the
          spiking the water samples with surrogates, prior to   use, performance and compatibility of Shimadzu
          sample extraction. The spiked water samples undergo   UFMS™ for EPA Method 537 with seven additional
          the  sample   preparation  procedures  and  LCMS      PFAS targets. In this study, all samples and blanks
          analysis. The calculated recovery of the surrogates   were extracted by the same SPE procedure and
          must be in the range of 70–130% (EPA, Section 9.3.5)  analyzed using the same LC-MS/MS method on
          to demonstrate good method performance.               different instrument models. Method detection limits of

          Seven water samples were spiked with 10 ng of         0.7–1.7 ng/L (LCMS-8050) and 0.7–3.3 ng/L (LCMS-
                                                                8045) were obtained and both systems fulfilled all of
          M2PFHxA, 10 ng of M2PFDA and 40 ng of M-N-            the EPA’s requirements for PFAS analysis in drinking
          EtFOSAA giving a concentration of 40 ng/L for         water. This was achieved with a 1 µL injection volume,
          M2PFHxA and M2PFDA and 160 ng/L for M-N-              in contrast to 10 µL as described in the original EPA
          EtFOSAA in the 250 mL water sample. The calculated    M537. The smaller injection volume (less burden on
          recoveries obtained using LCMS-8045 and LCMS-         the LCMS) would make the method more robust and
          8050 are shown in Table 8 using a Mean Response       reduce the long-term cost of ownership. Moreover,
          Factor. All recoveries were within ± 10%, well        Shimadzu’s high-speed and high-sensitivity UFMS™
          achieving EPA requirements.
                                                                instruments allow users to further increase productivity
                                                                by running multiple EPA methods on the same system,
                                                                in which case using the LCMS-8050 is recommended.

                                                                   References

                                                                [1] U.S. EPA, "EPA Method 537: Determination of
                                                                Selected Perfluorinated Alkyl Acids in Drinking Water
          UFMS, Nexera and Shim-pack are trademarks of Shimadzu
          Corporation.                                          by SPE and LC/MS/MS," Washington D.C., 2009.
          ISOLUTE is a registered trademark of Biotage AB.
                                                                [2] ASTM International, "ASTM D7979-17: Standard
                                                                Test Method for Determination of Perfluorinated
                                                                Compounds in Water, Sludge, Influent, Effluent and
                                                                Wastewater by LC/MS/MS," Conshohocken PA, 2017.

                                                                                                  First edition: January, 2019

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