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Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2013;30(6):1000-11. doi: 10.1080/19440049.2013.795292. Epub 2013 Jun 14.

Development and validation of a confirmatory method for the determination of tranquilisers and a β-blocker in porcine and bovine kidney by LC-MS/MS.

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1
Federal Office of Consumer Protection and Food Safety (BVL), National Reference Laboratory for Residues and Contaminants, 10832 Berlin, Germany. claudia.bock@bvl.bund.de

Abstract

A method for the confirmation of the tranquilisers azaperone and its metabolite azaperol, of chlorpromazine, propionylpromazine and acepromazine, haloperidol, xylazine and the β-blocker carazolol in porcine and bovine kidney with LC-MS/MS was developed. Various solvents and extraction techniques and different ways of clean-up were tested and verified with incurred pig kidney from an animal study. The best extraction efficiency was reached by extraction with a mixture of ammonia in ethyl acetate and overhead shaking without SPE clean-up. The optimised method with a twofold sample extraction was validated according to Commission Decision 2002/657/EC in a matrix-comprehensive in-house validation supported by the InterVal software, taking into account the defined MRLs and recommended concentrations. The validated method can be used for residue control of the above-mentioned analytes in bovine and porcine kidney of food-producing animals in accordance with Council Directive 96/23/EC.

PMID:
23767920
DOI:
10.1080/19440049.2013.795292
[Indexed for MEDLINE]
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