PFAS residue analysis in fish and fish feed by applying a modified QuEChERS method in combination with LC-HRMS detection
A targeted method for the quantitative determination of PFAS residues in fish feed and marine aquaculture fish species was developed and validated in the current study. This method combines a modified QuEChERS extraction methodology that includes sonication followed by Liquid Chromatography- Linear...
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KeAi Communications Co., Ltd.
2025-06-01
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| Series: | Emerging Contaminants |
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| Online Access: | http://www.sciencedirect.com/science/article/pii/S2405665025000010 |
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| author | Ourania Koloka Vasiliki Boti Dimitra Hela Triantafyllos Albanis Ioannis Konstantinou |
| author_facet | Ourania Koloka Vasiliki Boti Dimitra Hela Triantafyllos Albanis Ioannis Konstantinou |
| author_sort | Ourania Koloka |
| collection | DOAJ |
| description | A targeted method for the quantitative determination of PFAS residues in fish feed and marine aquaculture fish species was developed and validated in the current study. This method combines a modified QuEChERS extraction methodology that includes sonication followed by Liquid Chromatography- Linear Ion Trap/Orbitrap High Resolution Mass Spectrometry (LC- LTQ/Orbitrap HRMS) analysis. The original QuEChERS method was selected with some modifications and the clean-up step was performed using Enhanced Matrix Removal-Lipid (EMR-Lipid) as the dispersive solid-phase extraction (dSPE) agent. The optimization of the sample preparation included different sorbents in the clean-up step for the fish feed matrix, and various sample amounts and sonication treatment times were tested for both matrices. The optimized modified extraction procedure for the analysis of PFAS residues in fish feed was fully validated exhibiting recoveries between 51.1 % and 101.2 %, relative standard deviations (RSDs) < 20.7 % and LOQs between 0.03 ng/g and 0.50 ng/g. Furthermore, the current study provides validation data for the analysis of PFAS residues in fish tissues according to the analytical method proposed for PFAS analysis in fish feed, with linearity values ≥ 0.9901, recoveries ranging from 55.5 to 113.3 % and precision values < 20.0 % (%RSD). Matrix effect studies demonstrated low, and medium values and the method showed an acceptable expanded uncertainty of <57.66 %. Finally, the modified method was applied to analyze fish and fish feed samples from Greek aquaculture facilities. No PFAS residues were detected in any of the fish samples, whereas two fish feeds contained PFOS residues and one contained the target PFOA. |
| format | Article |
| id | doaj-art-6a30a4f387834fd7a62dd71f70f536eb |
| institution | Kabale University |
| issn | 2405-6650 |
| language | English |
| publishDate | 2025-06-01 |
| publisher | KeAi Communications Co., Ltd. |
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| series | Emerging Contaminants |
| spelling | doaj-art-6a30a4f387834fd7a62dd71f70f536eb2025-01-09T06:14:14ZengKeAi Communications Co., Ltd.Emerging Contaminants2405-66502025-06-01112100467PFAS residue analysis in fish and fish feed by applying a modified QuEChERS method in combination with LC-HRMS detectionOurania Koloka0Vasiliki Boti1Dimitra Hela2Triantafyllos Albanis3Ioannis Konstantinou4Department of Chemistry, University of Ioannina, Ioannina, 45110, GreeceDepartment of Chemistry, University of Ioannina, Ioannina, 45110, Greece; Unit of Environmental, Organic and Biochemical high-resolution analysis-Orbitrap-LC-MS, University of Ioannina, Ioannina, 45110, GreeceDepartment of Chemistry, University of Ioannina, Ioannina, 45110, Greece; Unit of Environmental, Organic and Biochemical high-resolution analysis-Orbitrap-LC-MS, University of Ioannina, Ioannina, 45110, GreeceDepartment of Chemistry, University of Ioannina, Ioannina, 45110, Greece; Unit of Environmental, Organic and Biochemical high-resolution analysis-Orbitrap-LC-MS, University of Ioannina, Ioannina, 45110, GreeceDepartment of Chemistry, University of Ioannina, Ioannina, 45110, Greece; Unit of Environmental, Organic and Biochemical high-resolution analysis-Orbitrap-LC-MS, University of Ioannina, Ioannina, 45110, Greece; Corresponding author. Department of Chemistry, University of Ioannina, Ioannina, 45110, Greece.A targeted method for the quantitative determination of PFAS residues in fish feed and marine aquaculture fish species was developed and validated in the current study. This method combines a modified QuEChERS extraction methodology that includes sonication followed by Liquid Chromatography- Linear Ion Trap/Orbitrap High Resolution Mass Spectrometry (LC- LTQ/Orbitrap HRMS) analysis. The original QuEChERS method was selected with some modifications and the clean-up step was performed using Enhanced Matrix Removal-Lipid (EMR-Lipid) as the dispersive solid-phase extraction (dSPE) agent. The optimization of the sample preparation included different sorbents in the clean-up step for the fish feed matrix, and various sample amounts and sonication treatment times were tested for both matrices. The optimized modified extraction procedure for the analysis of PFAS residues in fish feed was fully validated exhibiting recoveries between 51.1 % and 101.2 %, relative standard deviations (RSDs) < 20.7 % and LOQs between 0.03 ng/g and 0.50 ng/g. Furthermore, the current study provides validation data for the analysis of PFAS residues in fish tissues according to the analytical method proposed for PFAS analysis in fish feed, with linearity values ≥ 0.9901, recoveries ranging from 55.5 to 113.3 % and precision values < 20.0 % (%RSD). Matrix effect studies demonstrated low, and medium values and the method showed an acceptable expanded uncertainty of <57.66 %. Finally, the modified method was applied to analyze fish and fish feed samples from Greek aquaculture facilities. No PFAS residues were detected in any of the fish samples, whereas two fish feeds contained PFOS residues and one contained the target PFOA.http://www.sciencedirect.com/science/article/pii/S2405665025000010Per- and polyfluoroalkyl substancesAquacultureFeedEMR-LipidAquatic environmentHigh resolution mass spectrometry |
| spellingShingle | Ourania Koloka Vasiliki Boti Dimitra Hela Triantafyllos Albanis Ioannis Konstantinou PFAS residue analysis in fish and fish feed by applying a modified QuEChERS method in combination with LC-HRMS detection Emerging Contaminants Per- and polyfluoroalkyl substances Aquaculture Feed EMR-Lipid Aquatic environment High resolution mass spectrometry |
| title | PFAS residue analysis in fish and fish feed by applying a modified QuEChERS method in combination with LC-HRMS detection |
| title_full | PFAS residue analysis in fish and fish feed by applying a modified QuEChERS method in combination with LC-HRMS detection |
| title_fullStr | PFAS residue analysis in fish and fish feed by applying a modified QuEChERS method in combination with LC-HRMS detection |
| title_full_unstemmed | PFAS residue analysis in fish and fish feed by applying a modified QuEChERS method in combination with LC-HRMS detection |
| title_short | PFAS residue analysis in fish and fish feed by applying a modified QuEChERS method in combination with LC-HRMS detection |
| title_sort | pfas residue analysis in fish and fish feed by applying a modified quechers method in combination with lc hrms detection |
| topic | Per- and polyfluoroalkyl substances Aquaculture Feed EMR-Lipid Aquatic environment High resolution mass spectrometry |
| url | http://www.sciencedirect.com/science/article/pii/S2405665025000010 |
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