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A simple QuEChERS extraction procedure has been employed for quantifying the PFAS with normal dSPE cleanup.
This method complies with all acceptance criteria (as per AOAC SMPR 2023.003) without using ISTDs.
Method with shorter run time can contribute to achieving high throughputs in testing laboratories.
Simultaneous Quantitation of 32 PFAS in Baby
Food by LC-MS/MS
PFAS (Per- and polyfluoroalkyl substances) are a class of highly
persistent chemicals widely known as "forever chemicals" due
to their strong resistance to environmental degradation (Figure
1). Found in products like firefighting foams, non-stick
cookware, and water-resistant fabrics, PFAS are now recognized
as major environmental and health concerns. These substances
accumulate in soil, water, and living organisms, including
humans, where they may cause serious health impacts over
time.
Given their potential for long-term contamination, the
detection and quantification of PFAS are critical. Advanced
analytical methods, particularly LC-MS/MS with Multiple
Reaction Monitoring (MRM), offer the specificity and sensitivity
needed to accurately measure PFAS concentrations. However,
one of the primary challenges in PFAS analysis is minimizing
background contamination from PFAS residues within the LC
system and during sample collection and preparation. Effective
strategies to reduce these sources of contamination are
essential for reliable results in PFAS quantification.
In this application news, we describe a single laboratory
validation study with a rapid extraction of trace level
concentrations of 32 PFAS (Table 1) in infant formula (baby
food) involving the use of the QuEChERS as an extraction
technique followed by mass spectrometric analysis using a
Shimadzu LCMS-8060NX triple quadrupole mass spectrometer
coupled to a Shimadzu Nexera X3 liquid chromatograph
(Figure 2).
Liquid Chromatograph Mass Spectrometer LCMS-8060NX
Samruddha Chavan, Shalu Nair, Nitish Suryawanshi, Nitin Shukla, Devika Tupe, Siddhesh
Ghadi, Ramesh Manigiri, Jitendra Kelkar and Pratap Rasam
Shimadzu Analytical (India) Pvt. Ltd.
Introduction
Material and Method
Compared the recovery and precision against the requirements
of AOAC SMPR 2023.003. In addition, we determined the Limit
of Quantitation (LOQ) as the lowest concentration meeting
recovery accuracy and precision. All recovery, precision, and
LOQ’s met the acceptance criteria. We optimized the
chromatography and instrument operating parameters to
achieve excellent peak shape, separation, and sensitivity
(Figure 3).
Sample Preparation
The reference standards were procured from Dr. Ehrenstorfer
with below catalogue numbers:
EPA Method 533 PFAS Mixture 151 100 µg/mL (DRE-
A50000151MW).
The calibration standards were analyzed in the range of 0.005
to 10 μg/L (for some compounds 0.05-10 μg/L and for PFBA was
0.25-10 μg/L). Calibration curves were generated by external
standard method with weighted regression of 1/C
2
. Fortified
samples were prepared in six replicates of each 0.01, 0.05 and
0.25 μg/kg.
5.0 g of Infant formula
sample
15 mL of water, vortex
for 2.0 mins
5.0 mL Acetonitrile
Shake well and vortex it for
2.0 mins
Add 4.0 g of MgSO₄,
Shake well
Add 1.0 g of Sodium
acetate
Vortex it for 2.0 mins and
centrifuge for 10.0 mins at
7800 rpm
Collect the supernatant
Add dSPE sorbent to
clean-up
Vortex it for 1.0 mins and
centrifuge for 5.0 mins at
7800 rpm
Collect the supernatant
2.0 mL of aliquot and
Evaporate under
Nitrogen steam
Concentrate and
reconstitute to 1.0 mL
Fill the vial
Analyse it with LC-MS/MS
MeOH:Water (80:20) v/v
Figure 1: Structure of PFHxS, PFNA and PFOS
Figure 2: Shimadzu LCMS-8060NX triple quadrupole mass
spectrometer coupled to a Nexera
TM
X3 UHPLC
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