Development, optimization and validation of a highly sensitive and selective method for the determination of PFAS in animal-based food.

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Title: Development, optimization and validation of a highly sensitive and selective method for the determination of PFAS in animal-based food.
Authors: Koenig, Pascal1 (AUTHOR) pascal.koenig@cvua-westfalen.de, Brand, Benedikt1 (AUTHOR), Hamscher, Gerd2 (AUTHOR), Stahl, Thorsten3 (AUTHOR)
Source: Chemosphere. Mar2025, Vol. 372, pN.PAG-N.PAG. 1p.
Subjects: Liquid chromatography-mass spectrometry, Fluoroalkyl compounds, Solid phase extraction, Food safety, Fluid foods
Abstract: Perfluorocarboxylic acids and perfluorosulfonic acids accumulate in food webs, thus posing a serious threat to food safety. The European Food Safety Authority (EFSA) derived a tolerable weekly intake (TWI) of 4.4 ng/kg body weight for the sum of the four so-called EFSA-PFAS in 2020. More sensitive analytical methods are urgently needed, not only to monitor maximum levels, but also for future toxicological assessments of these substances. Therefore, in the present study a dual SPE approach for the purification of the extracts was chosen to attain high and valid sensitivity for the matrices egg, liver, milk and dairy products using liquid chromatography coupled with tandem mass spectrometry. This method achieved limits of quantification of 2.60 (PFOS) - 6.80 ng/kg (PFHxS) for egg, 9.80 (PFOS) - 46.0 ng/kg (PFHxS) for liver and 0.165 (PFNA) - 0.455 ng/kg (PFOS) for milk for the 4 EFSA-PFAS. Summed medians for the 4 EFSA-PFAS of 396 ng/kg in bovine liver and 54.0 ng/kg in pork liver, as well as 8.46 ng/kg in cheese and 4.57 ng/kg in milk were detected. The results were subjected to correlation analysis. Statistically significant strong correlations were identified between bovine and porcine liver for PFNA, PFDA, PFUnDA and PFOS. To summarize the PFAS content and the PFAS spectrum detected depend on the animal species examined. Furthermore, an estimation of the exhaustion of the TWI for children, women and men was conducted. In our model, a TWI exhaustion of more than 27.0% (children) was calculated for liver, milk and cheese. [Display omitted] • New method for the determination of PFAS on a ng/kg level in animal-based food • PFAS method validation in accordance to the Implementing Regulation (EU) 2022/1428 • First results for cheese, bovine liver, pork liver and milk • Cheese, milk and liver contribute a remarkable amount to the exhaustion of the TWI • Noticeable difference in PFOS content between bovine liver and pork liver [ABSTRACT FROM AUTHOR]
Copyright of Chemosphere is the property of Pergamon Press - An Imprint of Elsevier Science and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)
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  Data: Development, optimization and validation of a highly sensitive and selective method for the determination of PFAS in animal-based food.
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  Data: <searchLink fieldCode="AR" term="%22Koenig%2C+Pascal%22">Koenig, Pascal</searchLink><relatesTo>1</relatesTo> (AUTHOR)<i> pascal.koenig@cvua-westfalen.de</i><br /><searchLink fieldCode="AR" term="%22Brand%2C+Benedikt%22">Brand, Benedikt</searchLink><relatesTo>1</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Hamscher%2C+Gerd%22">Hamscher, Gerd</searchLink><relatesTo>2</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Stahl%2C+Thorsten%22">Stahl, Thorsten</searchLink><relatesTo>3</relatesTo> (AUTHOR)
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  Data: <searchLink fieldCode="JN" term="%22Chemosphere%22">Chemosphere</searchLink>. Mar2025, Vol. 372, pN.PAG-N.PAG. 1p.
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  Data: <searchLink fieldCode="DE" term="%22Liquid+chromatography-mass+spectrometry%22">Liquid chromatography-mass spectrometry</searchLink><br /><searchLink fieldCode="DE" term="%22Fluoroalkyl+compounds%22">Fluoroalkyl compounds</searchLink><br /><searchLink fieldCode="DE" term="%22Solid+phase+extraction%22">Solid phase extraction</searchLink><br /><searchLink fieldCode="DE" term="%22Food+safety%22">Food safety</searchLink><br /><searchLink fieldCode="DE" term="%22Fluid+foods%22">Fluid foods</searchLink>
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  Label: Abstract
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  Data: Perfluorocarboxylic acids and perfluorosulfonic acids accumulate in food webs, thus posing a serious threat to food safety. The European Food Safety Authority (EFSA) derived a tolerable weekly intake (TWI) of 4.4 ng/kg body weight for the sum of the four so-called EFSA-PFAS in 2020. More sensitive analytical methods are urgently needed, not only to monitor maximum levels, but also for future toxicological assessments of these substances. Therefore, in the present study a dual SPE approach for the purification of the extracts was chosen to attain high and valid sensitivity for the matrices egg, liver, milk and dairy products using liquid chromatography coupled with tandem mass spectrometry. This method achieved limits of quantification of 2.60 (PFOS) - 6.80 ng/kg (PFHxS) for egg, 9.80 (PFOS) - 46.0 ng/kg (PFHxS) for liver and 0.165 (PFNA) - 0.455 ng/kg (PFOS) for milk for the 4 EFSA-PFAS. Summed medians for the 4 EFSA-PFAS of 396 ng/kg in bovine liver and 54.0 ng/kg in pork liver, as well as 8.46 ng/kg in cheese and 4.57 ng/kg in milk were detected. The results were subjected to correlation analysis. Statistically significant strong correlations were identified between bovine and porcine liver for PFNA, PFDA, PFUnDA and PFOS. To summarize the PFAS content and the PFAS spectrum detected depend on the animal species examined. Furthermore, an estimation of the exhaustion of the TWI for children, women and men was conducted. In our model, a TWI exhaustion of more than 27.0% (children) was calculated for liver, milk and cheese. [Display omitted] • New method for the determination of PFAS on a ng/kg level in animal-based food • PFAS method validation in accordance to the Implementing Regulation (EU) 2022/1428 • First results for cheese, bovine liver, pork liver and milk • Cheese, milk and liver contribute a remarkable amount to the exhaustion of the TWI • Noticeable difference in PFOS content between bovine liver and pork liver [ABSTRACT FROM AUTHOR]
– Name: AbstractSuppliedCopyright
  Label:
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  Data: <i>Copyright of Chemosphere is the property of Pergamon Press - An Imprint of Elsevier Science and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract.</i> (Copyright applies to all Abstracts.)
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      – Type: doi
        Value: 10.1016/j.chemosphere.2025.144123
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      – Code: eng
        Text: English
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        PageCount: 1
        StartPage: N.PAG
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      – SubjectFull: Liquid chromatography-mass spectrometry
        Type: general
      – SubjectFull: Fluoroalkyl compounds
        Type: general
      – SubjectFull: Solid phase extraction
        Type: general
      – SubjectFull: Food safety
        Type: general
      – SubjectFull: Fluid foods
        Type: general
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      – TitleFull: Development, optimization and validation of a highly sensitive and selective method for the determination of PFAS in animal-based food.
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            NameFull: Koenig, Pascal
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            NameFull: Brand, Benedikt
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            – D: 01
              M: 03
              Text: Mar2025
              Type: published
              Y: 2025
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              Value: 372
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