Page 8 - Application Notebook - PFAS Analysis

SHIMADZU | WHITE PAPER Ultra-fast LC-MS/MS Analysis of PFAS in Environmental Waters

Table 3. LCMS system and instrument conditions.

LCMS Instrument Shimadzu LCMS-8060
Analytical Column Shim-pack GIST Phenyl-Hexyl, 2.1 mm ID × 100 mm, 3 µm particle size
Solvent Delay Column Shim-pack XR-ODS, 3 mm ID × 50 mm, 2.2 µm particle size
Column Temperature 40 C
o
Injection Volume 10 µL
LC Flow Rate 0.4 mL/min
Mobile Phase A 20 mM Ammonium Acetate in LCMS-grade Water
Mobile Phase B Acetonitrile

Time (min) % Solvent Line A % Solvent Line B
0 90 10
1 90 10
3 70 30
Gradient Conditions
14 35 65
14.1 2 98
17.1 90 10
20 90 10

Run / Acquisition Cycle Time 20 minutes (all 49 PFAS compounds are eluted in 13 minutes)
Interface Electrospray Ionization (ESI)
Interface Temperature 300 C
o
Desolvation Line Temperature 100 C
o
Heat Block Temperature 200 C
o
Heating Gas Flow 15 L/min
Drying Gas Flow 5 L/min
Nebulizing Gas Flow 3 L/min
Total MRMs 74

The described LC-MS/MS method was run exactly as PFAS-free materials, high-grade solvents and flushing
indicated in ASTM Method D7979. One such the instrument by injecting multiple method blanks.
modification concerns the ASTM liquid chromatography
(LC) conditions. Only two LC mobile phases were In this study, a solvent delay column was used to
employed in this study. Reagent C (400 mM account for the PFAS contamination present in the
ammonium acetate in 95:5% acetonitrile-water) glass containers, laboratory consumables (e.g. pipette
specified in ASTM method was not used. The LC tips) and LC system (e.g. pumps and tubing). This
mobile phases used in this study (Table 3) are easy to solvent delay column is situated before the
prepare. In addition, the shape and sensitivity of autosampler and helps delay the elution of the PFAS
chromatographic peaks obtained are similar or even present in the background. As shown in Figure 1, the
better than when using the mobile phases specified in use of the delay column and this impurity delay method
the ASTM method. allows the distinction of PFOA originating solely from
the sample. Furthermore, with Shimadzu’s team of
service engineers, we can set up the exact HPLC
configuration (involving solvent lines, tubing, bypassing
 Avoiding Contamination
of solvent lines and more) that is proven to give
PFAS may be found in sampling and storage contamination-free data.
containers and may even contaminate the samples. It
is important to account for these sources of PFAS
during and, at best, minimize them with the use of