Multi-residue method for the determination of thyreostats in urine samples using liquid chromatography coupled to tandem mass spectrometry after derivatisation with 3-iodobenzylbromide

• Published in: Journal of Chromatography A 2005-09, Vol.1085 (2), p.247-252
• Main Authors: Pinel, Gaud, Bichon, Emmanuelle, Pouponneau, Karine, Maume, Daniel, André, François, Le Bizec, Bruno
• Format: Article
• Language: English
• Subjects: Animal productions; Animals; Antithyroid Agents - analysis; Antithyroid Agents - urine; Biological and medical sciences; Cattle; Chromatography, Liquid - methods; Derivatisation; Drug Residues - analysis; Drug Residues - chemistry; Feed and pet food industries; Food industries; Fundamental and applied biological sciences. Psychology; Iodobenzenes - chemistry; LC-ESI-MS/MS; Mercaptobenzimidazole; MRPL; Spectrometry, Mass, Electrospray Ionization - methods; Swine; Terrestrial animal productions; Thiouracil; Thyreostatic drugs; Urine; Vertebrates
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2005.06.055

Thyreostats are banned compounds in Europe since 1981 (directive 81/602/EC) because of their carcinogenic and teratogenic properties. The control of their illegal use in breeding animals is amongst the most difficult because of their low molecular weight, high polarity and the existence of tautomeric forms. The analytical procedure described in this paper involves, after a derivatisation step with 3-iodobenzylbromide, the detection and identification at low level (μg/L) by LC-ESI(−)-MS/MS of eight thyreostats in various biological matrices (urine, muscle, liver, thyroid, animal feed, faeces and hair). The urine method has been validated according to the EU criteria (2002/657/EC decision): CC α and CC β were found in the range (0.1–5.2 μg/L) and (2.6–23.2 μg/L), respectively. The performances fulfil the requirements of the EU regarding the provisional minimum required performance limit (MRPL) fixed at 100 μg/L in urine.