<abstract xmlns="http://www.w3.org/1999/xhtml">
A rapid liquid chromatography tandem mass spectrometry method was developed and validated to detect and confirm five thyreostatic drugs: tapazole, thiouracil, methylthiouracil, propylthiouracil, and phenylthiouracil in animal feeding stuff samples. Thyreostats were extracted from feed with methanol, and then degreasing of the extract with petroleum ether was performed, followed by the derivatisation of the compounds with 3-iodobenzylbromide in basic medium (pH 8.0). The derivatives were extracted with diethyl ether and analysed by gradient elution on a Poroshell 120-EC C18 column with triple quadrupole MS detection with turbo spray source in positive ionisation mode. The method was validated in accordance with the Commission Decision 2002/657/EC. For validation level of 10 ļig kg-1, the recovery ranged from 82% to 97.5% for all examined compounds. The repeatability and reproducibility did not exceed the limit of 20% for all analytes. The linearity was good for all thyreostats in the whole range of tested concentrations, as proved by the correlation coefficients greater than 0.99. The decision limits (CCa) ranged from 1.63 ļig kg-1 to 3.95 ļig kg-1, whereas the detection capabilities (CCß) ranged from 2.74 ļig kg-1 to 6.73 ļig kg-1. The developed analysis is sensitive and robust, and therefore useful for quantification and confirmation of thyreostats in residue control programme.
</abstract>

A rapid liquid chromatography tandem mass spectrometry method was developed and validated to detect and confirm five thyreostatic drugs: tapazole, thiouracil, methylthiouracil, propylthiouracil, and phenylthiouracil in animal feeding stuff samples. Thyreostats were extracted from feed with methanol, and then degreasing of the extract with petroleum ether was performed, followed by the derivatisation of the compounds with 3-iodobenzylbromide in basic medium (pH 8.0). The derivatives were extracted with diethyl ether and analysed by gradient elution on a Poroshell 120-EC C18 column with triple quadrupole MS detection with turbo spray source in positive ionisation mode. The method was validated in accordance with the Commission Decision 2002/657/EC. For validation level of 10 ļig kg-1, the recovery ranged from 82% to 97.5% for all examined compounds. The repeatability and reproducibility did not exceed the limit of 20% for all analytes. The linearity was good for all thyreostats in the whole range of tested concentrations, as proved by the correlation coefficients greater than 0.99. The decision limits (CCa) ranged from 1.63 ļig kg-1 to 3.95 ļig kg-1, whereas the detection capabilities (CCß) ranged from 2.74 ļig kg-1 to 6.73 ļig kg-1. The developed analysis is sensitive and robust, and therefore useful for quantification and confirmation of thyreostats in residue control programme.

Determination of the Thyreostats in Animal Feeding Stuffs Using Liquid Chromatography-Tandem Mass Spectrometry

Department of Pharmacology and Toxicology

Journal of Veterinary Research

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

A rapid liquid chromatography tandem mass spectrometry method was developed and validated to detect and confirm five thyreostatic drugs: tapazole, thiouracil,...

Determination of the Thyreostats in Animal Feeding Stuffs Using Liquid Chromatography-Tandem Mass Spectrometry

Online veröffentlicht: 01. Okt. 2014

Seitenbereich: 413 - 419

Eingereicht: 06. Aug. 2014

Akzeptiert: 21. Aug. 2014

DOI: https://doi.org/10.2478/bvip-2014-0064

Schlüsselwörter
feeding stuff, thyreostats, liquid chromatography, mass spectrometry

© 2014 National Veterinary Research Institute in Pulawy

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

Determination of the Thyreostats in Animal Feeding Stuffs Using Liquid Chromatography-Tandem Mass Spectrometry

Online veröffentlicht: 01. Okt. 2014

Seitenbereich: 413 - 419

Eingereicht: 06. Aug. 2014

Akzeptiert: 21. Aug. 2014

DOI: https://doi.org/10.2478/bvip-2014-0064

Schlüsselwörterfeeding stuff, thyreostats, liquid chromatography, mass spectrometry

© 2014 National Veterinary Research Institute in Pulawy

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

Schlüsselwörter
feeding stuff, thyreostats, liquid chromatography, mass spectrometry