Page 57 - Application Notebook - PFAS Analysis
P. 57

No. SSI-LCMS-119






                                         Liquid Chromatography Mass Spectrometry

                                          Are there PFAS in my water?

                                          A detailed look into bottled
                                          water
             No. LCMS-119



               ■ Introduction
               The presence of Per- and Polyfluorinated Alkyl     Chromatography was adjusted to obtain maximum
               Substances (PFAS) in drinking water is being       resolution between peaks in the shortest time
               thoroughly studied due to the persistence of these   possible with minimum co-elution of isomers. The
               compounds in the environment and their potential   total run time of 21 minutes includes a final wash
               health effects. However, there is limited knowledge   out with concentrated acetonitrile to flush the
               about the occurrence of these chemicals in bottled   column, remove background residuals contaminants
               water, despite the increasing concerns about PFAS in   and restore column performance before starting the
               the food supply. This work presents results from a   next run. The method could easily be modified to
               fast and simple direct injection method similar to EPA   include isotopic dilution or internal calibration if
               method 8237, using the Shimadzu LCMS-8050 to       needed for quantifying the concentrations.
               analyze seven commercially available samples of
               bottled water for 24 PFAS. The results demonstrate   Calibration Standards
               that the instrument’s performance exceeds the      Standards available from Wellington Laboratories
               requirements  in FDA draft method C-010.01 for     were used for these studies (Catalog no. PFAC-
               other matrices, including milk (which is the most   24PAR and MPFAC-24ES). These standards were
               similar to water), as well as the limits established by   then diluted to working standards using 95:5
               the EPA for drinking water.                        acetonitrile:water as the diluent. The working
                                                                  standards were used to create a calibration curve
               While the origin of the water itself maybe the source   ranging from 5-200 ppt with the injection solvent
               of PFAS in bottled water, we also wanted to        consisting of 50:50 water:methanol with 0.1%
               investigate the importance of the type of materials.   acetic acid in order to match the injection solvent for
               Migration of PFAS from Food Contact Materials      the extracted samples. Filtration was not performed
               (FCM) is known to occur in all kinds of food       on the calibration standards.
               containers. In this study, we procured bottled water
               in several different bottle materials, as well as two   Sample Preparation
               types of water source. These included spring and   Seven  types of bottled water as sample matrices
               purified water, and bottles made from 5 different   were tested using reagent water as the blank. Each
               kinds of container materials: plastic (virgin and   sample was diluted 50:50 with MeOH and 0.1%
               recycled), glass, metal, and cardboard. Preliminary   acetic acid, spiked with isotopically labeled
               results indicate that observed PFAS levels seem to   surrogates and vortexed for 2 min. The samples were
               depend on both the bottle material and the water   then filtered through 0.2 μm syringe filters and
               source.                                            analyzed by LC/MS/MS.

               ■ Methodology                                      All compound parameters, including precursor ion,
               We analyzed 24 target PFAS compounds and 19        product ion, and collision energies, were optimized.
               surrogates in various types of water. The analysis of   There are at least two multiple reaction monitoring
               PFAS was performed using a Shimadzu Nexera X2      (MRM) transitions for most of the analytes.
               SIL-30AC autosampler and a LCMS-8050 triple
               quadrupole mass spectrometer. An injection volume
               of 30 µL was used in this study.  A detailed
               description of the LC/MS/MS parameters is included
               in Table 1.
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