Multi-Residue Analysis of Thyreostats in Animal Muscle Tissues by Hydrophilic Interaction Liquid Chromatography Tandem Mass Spectrometry: A Thorough Chromatographic Study
Τhyreostats (TSs) are veterinary drugs used in livestock farming for fattening. Their administration is banned in the European Union since 1981, and their monitoring for food quality and safety control requires sensitive and confirmatory methods. The present study describes the development and valid...
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2024-09-01
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| author | Anastasia S. Kritikou Marilena E. Dasenaki Niki C. Maragou Marios G. Kostakis Nikolaos S. Thomaidis |
| author_facet | Anastasia S. Kritikou Marilena E. Dasenaki Niki C. Maragou Marios G. Kostakis Nikolaos S. Thomaidis |
| author_sort | Anastasia S. Kritikou |
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| description | Τhyreostats (TSs) are veterinary drugs used in livestock farming for fattening. Their administration is banned in the European Union since 1981, and their monitoring for food quality and safety control requires sensitive and confirmatory methods. The present study describes the development and validation of a hydrophilic interaction liquid chromatography tandem mass spectrometry (HILIC-MS/MS) method for the simultaneous determination of 2-thiouracil (TU), 6-methyl-2-thiouracil (MTU), 6-propyl-2-thiouracil (PTU), 6-phenyl-2-thiouracil (PhTU), tapazole (TAP), and 2-mercaptobenzimidazole (MBI) in bovine muscle tissues. Investigation of the retention mechanism of the six analytes on the selected amide-based stationary phase showed that hydrophilic partition was the dominant interaction. The sample preparation included extraction with ACN/H<sub>2</sub>O (80/20), followed by dispersive solid-phase extraction (d-SPE) with C18 sorbent and hexane partitioning. The method was validated according to European guidelines using internal standards, including isotopically labelled ones. The method’s LODs ranged between 2.8 ng g<sup>−1</sup> (6-phenyl-2-thiouracil) and 4.1 ng g<sup>−1</sup> (2-thiouracil). Application of the proposed method to 48 bovine tissue samples showed non-detectable results. |
| format | Article |
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| issn | 2297-8739 |
| language | English |
| publishDate | 2024-09-01 |
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| spelling | doaj-art-643e8b0804244b089c6562b2a17b21ac2025-08-20T01:55:51ZengMDPI AGSeparations2297-87392024-09-0111926910.3390/separations11090269Multi-Residue Analysis of Thyreostats in Animal Muscle Tissues by Hydrophilic Interaction Liquid Chromatography Tandem Mass Spectrometry: A Thorough Chromatographic StudyAnastasia S. Kritikou0Marilena E. Dasenaki1Niki C. Maragou2Marios G. Kostakis3Nikolaos S. Thomaidis4Laboratory of Analytical Chemistry, Department of Chemistry, National and Kapodistrian University of Athens, Panepistimioupolis Zographou, 15771 Athens, GreeceLaboratory of Food Chemistry, Department of Chemistry, National and Kapodistrian University of Athens, Panepistimioupolis Zographou, 15771 Athens, GreeceLaboratory of Analytical Chemistry, Department of Chemistry, National and Kapodistrian University of Athens, Panepistimioupolis Zographou, 15771 Athens, GreeceLaboratory of Analytical Chemistry, Department of Chemistry, National and Kapodistrian University of Athens, Panepistimioupolis Zographou, 15771 Athens, GreeceLaboratory of Analytical Chemistry, Department of Chemistry, National and Kapodistrian University of Athens, Panepistimioupolis Zographou, 15771 Athens, GreeceΤhyreostats (TSs) are veterinary drugs used in livestock farming for fattening. Their administration is banned in the European Union since 1981, and their monitoring for food quality and safety control requires sensitive and confirmatory methods. The present study describes the development and validation of a hydrophilic interaction liquid chromatography tandem mass spectrometry (HILIC-MS/MS) method for the simultaneous determination of 2-thiouracil (TU), 6-methyl-2-thiouracil (MTU), 6-propyl-2-thiouracil (PTU), 6-phenyl-2-thiouracil (PhTU), tapazole (TAP), and 2-mercaptobenzimidazole (MBI) in bovine muscle tissues. Investigation of the retention mechanism of the six analytes on the selected amide-based stationary phase showed that hydrophilic partition was the dominant interaction. The sample preparation included extraction with ACN/H<sub>2</sub>O (80/20), followed by dispersive solid-phase extraction (d-SPE) with C18 sorbent and hexane partitioning. The method was validated according to European guidelines using internal standards, including isotopically labelled ones. The method’s LODs ranged between 2.8 ng g<sup>−1</sup> (6-phenyl-2-thiouracil) and 4.1 ng g<sup>−1</sup> (2-thiouracil). Application of the proposed method to 48 bovine tissue samples showed non-detectable results.https://www.mdpi.com/2297-8739/11/9/269thyreostatsHILICESI-MS/MSmeatfood safetybovine tissue |
| spellingShingle | Anastasia S. Kritikou Marilena E. Dasenaki Niki C. Maragou Marios G. Kostakis Nikolaos S. Thomaidis Multi-Residue Analysis of Thyreostats in Animal Muscle Tissues by Hydrophilic Interaction Liquid Chromatography Tandem Mass Spectrometry: A Thorough Chromatographic Study Separations thyreostats HILIC ESI-MS/MS meat food safety bovine tissue |
| title | Multi-Residue Analysis of Thyreostats in Animal Muscle Tissues by Hydrophilic Interaction Liquid Chromatography Tandem Mass Spectrometry: A Thorough Chromatographic Study |
| title_full | Multi-Residue Analysis of Thyreostats in Animal Muscle Tissues by Hydrophilic Interaction Liquid Chromatography Tandem Mass Spectrometry: A Thorough Chromatographic Study |
| title_fullStr | Multi-Residue Analysis of Thyreostats in Animal Muscle Tissues by Hydrophilic Interaction Liquid Chromatography Tandem Mass Spectrometry: A Thorough Chromatographic Study |
| title_full_unstemmed | Multi-Residue Analysis of Thyreostats in Animal Muscle Tissues by Hydrophilic Interaction Liquid Chromatography Tandem Mass Spectrometry: A Thorough Chromatographic Study |
| title_short | Multi-Residue Analysis of Thyreostats in Animal Muscle Tissues by Hydrophilic Interaction Liquid Chromatography Tandem Mass Spectrometry: A Thorough Chromatographic Study |
| title_sort | multi residue analysis of thyreostats in animal muscle tissues by hydrophilic interaction liquid chromatography tandem mass spectrometry a thorough chromatographic study |
| topic | thyreostats HILIC ESI-MS/MS meat food safety bovine tissue |
| url | https://www.mdpi.com/2297-8739/11/9/269 |
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