Determination of Multiclass Pharmaceutical Residues in Milk Using Modified QuEChERS and Liquid-Chromatography-Hybrid Linear Ion Trap/Orbitrap Mass Spectrometry: Comparison of Clean-Up Approaches and Validation Studies
A multi-residue method was developed to identify and quantify pharmaceutical drug residues in full-fat milk, using a modified QuEChERS extraction procedure and sonication combined with Ultra-High-Performance Liquid Chromatography–High-Resolution Orbitrap Mass Spectrometry (UHPLC-HR-Orbitrap-MS). Sam...
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| Language: | English |
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MDPI AG
2023-08-01
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| Series: | Molecules |
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| Online Access: | https://www.mdpi.com/1420-3049/28/16/6130 |
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| author | Ourania Koloka Marioanna Koulama Dimitra Hela Triantafyllos Albanis Ioannis Konstantinou |
| author_facet | Ourania Koloka Marioanna Koulama Dimitra Hela Triantafyllos Albanis Ioannis Konstantinou |
| author_sort | Ourania Koloka |
| collection | DOAJ |
| description | A multi-residue method was developed to identify and quantify pharmaceutical drug residues in full-fat milk, using a modified QuEChERS extraction procedure and sonication combined with Ultra-High-Performance Liquid Chromatography–High-Resolution Orbitrap Mass Spectrometry (UHPLC-HR-Orbitrap-MS). Sample preparation involves three different QuEChERS extraction procedures and sorbents for the purification step. The optimized modified extraction method, combined with the clean-up approaches using C18 and the EMR-Lipid sorbent, has been validated in terms of linearity, recovery, precision, LOD and LOQ, matrix effects (ME) and expanded uncertainty. The optimized method showed a linearity >0.9903, recoveries within the range 65.1–120.1%, precision (expressed as %RSD) <17.5%, medium (<39.9%) to low (<16.7%) matrix effects and acceptable expanded uncertainty (<33.1%). Finally, the proposed method was applied to representative real samples of milk (by local markets), revealing the existence of one pharmaceutical drug (imidocarb) in one sample. |
| first_indexed | 2024-03-10T23:41:30Z |
| format | Article |
| id | doaj.art-72eab7ba2404443fa225803a94a63262 |
| institution | Directory Open Access Journal |
| issn | 1420-3049 |
| language | English |
| last_indexed | 2024-03-10T23:41:30Z |
| publishDate | 2023-08-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Molecules |
| spelling | doaj.art-72eab7ba2404443fa225803a94a632622023-11-19T02:25:21ZengMDPI AGMolecules1420-30492023-08-012816613010.3390/molecules28166130Determination of Multiclass Pharmaceutical Residues in Milk Using Modified QuEChERS and Liquid-Chromatography-Hybrid Linear Ion Trap/Orbitrap Mass Spectrometry: Comparison of Clean-Up Approaches and Validation StudiesOurania Koloka0Marioanna Koulama1Dimitra Hela2Triantafyllos Albanis3Ioannis Konstantinou4Department of Chemistry, University of Ioannina, 45110 Ioannina, GreeceDepartment of Chemistry, University of Ioannina, 45110 Ioannina, GreeceDepartment of Chemistry, University of Ioannina, 45110 Ioannina, GreeceDepartment of Chemistry, University of Ioannina, 45110 Ioannina, GreeceDepartment of Chemistry, University of Ioannina, 45110 Ioannina, GreeceA multi-residue method was developed to identify and quantify pharmaceutical drug residues in full-fat milk, using a modified QuEChERS extraction procedure and sonication combined with Ultra-High-Performance Liquid Chromatography–High-Resolution Orbitrap Mass Spectrometry (UHPLC-HR-Orbitrap-MS). Sample preparation involves three different QuEChERS extraction procedures and sorbents for the purification step. The optimized modified extraction method, combined with the clean-up approaches using C18 and the EMR-Lipid sorbent, has been validated in terms of linearity, recovery, precision, LOD and LOQ, matrix effects (ME) and expanded uncertainty. The optimized method showed a linearity >0.9903, recoveries within the range 65.1–120.1%, precision (expressed as %RSD) <17.5%, medium (<39.9%) to low (<16.7%) matrix effects and acceptable expanded uncertainty (<33.1%). Finally, the proposed method was applied to representative real samples of milk (by local markets), revealing the existence of one pharmaceutical drug (imidocarb) in one sample.https://www.mdpi.com/1420-3049/28/16/6130pharmaceutical drugmilkQuEChERSliquid chromatography–LTQ Orbitrap mass spectrometryuncertainty |
| spellingShingle | Ourania Koloka Marioanna Koulama Dimitra Hela Triantafyllos Albanis Ioannis Konstantinou Determination of Multiclass Pharmaceutical Residues in Milk Using Modified QuEChERS and Liquid-Chromatography-Hybrid Linear Ion Trap/Orbitrap Mass Spectrometry: Comparison of Clean-Up Approaches and Validation Studies Molecules pharmaceutical drug milk QuEChERS liquid chromatography–LTQ Orbitrap mass spectrometry uncertainty |
| title | Determination of Multiclass Pharmaceutical Residues in Milk Using Modified QuEChERS and Liquid-Chromatography-Hybrid Linear Ion Trap/Orbitrap Mass Spectrometry: Comparison of Clean-Up Approaches and Validation Studies |
| title_full | Determination of Multiclass Pharmaceutical Residues in Milk Using Modified QuEChERS and Liquid-Chromatography-Hybrid Linear Ion Trap/Orbitrap Mass Spectrometry: Comparison of Clean-Up Approaches and Validation Studies |
| title_fullStr | Determination of Multiclass Pharmaceutical Residues in Milk Using Modified QuEChERS and Liquid-Chromatography-Hybrid Linear Ion Trap/Orbitrap Mass Spectrometry: Comparison of Clean-Up Approaches and Validation Studies |
| title_full_unstemmed | Determination of Multiclass Pharmaceutical Residues in Milk Using Modified QuEChERS and Liquid-Chromatography-Hybrid Linear Ion Trap/Orbitrap Mass Spectrometry: Comparison of Clean-Up Approaches and Validation Studies |
| title_short | Determination of Multiclass Pharmaceutical Residues in Milk Using Modified QuEChERS and Liquid-Chromatography-Hybrid Linear Ion Trap/Orbitrap Mass Spectrometry: Comparison of Clean-Up Approaches and Validation Studies |
| title_sort | determination of multiclass pharmaceutical residues in milk using modified quechers and liquid chromatography hybrid linear ion trap orbitrap mass spectrometry comparison of clean up approaches and validation studies |
| topic | pharmaceutical drug milk QuEChERS liquid chromatography–LTQ Orbitrap mass spectrometry uncertainty |
| url | https://www.mdpi.com/1420-3049/28/16/6130 |
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