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Determination of thyreostats in urine and thyroid gland by ultra high performance liquid chromatography tandem mass spectrometry
Authors:Madis Lõ  hmus,Kalle Kallaste,Bruno Le Bizec
Affiliation:1. Department of Chromatography, Tallinn Laboratory, Estonian Veterinary and Food Laboratory, Väike-Paala 3, 11415 Tallinn, Estonia;2. Laboratoire d’Etude des Résidus et Contaminants dans les Aliments, Ecole Nationale Vétérinaire de Nantes, Route de Gachet, BP 50707, 44307 Nantes Cedex 3, France
Abstract:
Thyreostatic compounds could be illegally administered to animals in order to obtain a weight gain due to a higher retention of water in the edible tissue and the gastro-intestinal tract. In the European Union their use for animal production is banned since 1981. Recently a highly sensitive method exploiting the determination of thyreostats with 3-iodobenzylbromide prior to purification to determine thyreostats in urine and other matrices was reported. For the first time, the UPLC instrumentation was used to separate the 3-iodobenzyl derivatives of various thyreostats. The deuterated internal standards tapazole-d3 and propylthiouracil-d5 were for the first time used for the quantification of tapazole, thiouracil, methylthiouracil, propylthiouracil, phenylthiouracil and mercaptobenzimidazole. The confirmative quantitative liquid chromatographic tandem mass spectrometric (LC–MS/MS) method was validated according to Commission Decision 2002/657/EC. The decision limit (CCα) and the detection capability (CCβ) were found to be for all compounds below the recommended value of 10 μg kg−1.
Keywords:Liquid chromatography tandem mass spectrometry (LC&ndash  MS/MS)   Deuterated internal standard   Ultra-performance liquid chromatography (UPLC)   Thyreostats   Decision limit   Detection capability
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