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. 2025 Jun 17:29:102674.
doi: 10.1016/j.fochx.2025.102674. eCollection 2025 Jul.

Advancing PFASs monitoring in food: from targeted SPE-LC-MS/MS to non-targeted QuEChERS-LC-HRMS approaches

Cassandre Jeannot  1   2 , Nicolas Macorps  1 , Bruno Le Bizec  1 , Julien Parinet  2 , Gaud Dervilly  1
Affiliations

Advancing PFASs monitoring in food: from targeted SPE-LC-MS/MS to non-targeted QuEChERS-LC-HRMS approaches

Cassandre Jeannot et al. Food Chem X. .

Abstract

Per- and polyfluoroalkyl substances (PFASs) are increasingly recognized as emerging contaminants, with some classified as persistent organic pollutants (POPs) and four recently regulated in food in the EU. However, due to the large structural diversity of PFASs, comprehensive monitoring remains essential. This study aimed to develop and apply a suspect and non-targeted screening approach to identify PFASs beyond those conventionally monitored in foodstuffs. The methodology combined optimized QuEChERS sample preparation, LC-HRMS acquisition, and prioritization of fluorinated signals, applying both suspect screening (SS) and non-targeted screening (NTS) strategies. Compared to targeted solid-phase extraction (SPE) coupled with MS/MS (QqQ) acquisition, this approach detected a broader range of PFASs in various food samples. Notably, as one of the first studies to apply NTS-a method typically used in environmental analysis-to food, it demonstrated the ability to detect both known and previously unlisted PFASs, such as PFPrA in an egg sample. This expanded approach enhances exposure assessment and supports the implementation of HRMS-based strategies for regulatory control and risk assessment.

Keywords: NTS; PFASs; QuEChERS; Sample preparation.

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Conflict of interest statement

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Figures

Fig. 1
Fig. 1
Detailed sample preparation steps using SPE and QuEChERS methods.
Fig. 2
Fig. 2
Relative signal Intensities (TICs) observed by LC-(ESI-)MS/MS for the analysis of PFASs in spiked milk (10 ng/mL) extracted by QuEChERS comparing 5 different solvent mixtures: ACN/H2O (grey), ACN/FA (red), ACN/H2O/FA (blue), MeOH (yellow) et MTBE/H2O (purple). (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)
Fig. 3
Fig. 3
Concentrations of 4 selected PFASs (PFOA, PFOS, PFNA, PFHxS) measured by LC-MS/MS following the application of either the SPE or QuEChERS extraction protocol, with supplementation at three levels (1, 5, and 10 μg·kg−1, wet weight) across 20 food items.
Fig. 4
Fig. 4
Chromatographic profiles of PFPeA obtained from (1) an egg sample and (2) a crustacean sample in SS acquisition mode, comparing the extraction protocols: SPE and QuEChERS.
Fig. 5
Fig. 5
a) Kendrick mass defect for CF2 repeating unit vs m/z of 28 PFASs standard listed in our internal database and classified by family: PFCA (n = 11), PFSA (n = 10), Cl-PFESA (n = 2) and others PFASs (n = 5). Homologous series are identified by shifts in the x-axis divisible by 49.9968 (CF2) and the same CF2 normalized mass defect. In yellow, a suspect PFASs signal highlighted by NTS data processing. b) Chromatogram profile for PFPrA standard. c) Chromatogram profile for PFPrA in an egg sample. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)
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