title: 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.
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.
authors.affiliation: Federal Office of Consumer Protection and Food Safety (BVL), National Reference Laboratory for Residues and Contaminants, 10832 Berlin, Germany. claudia.bock@bvl.bund.de
authors.forename: C
authors.initials: C
authors.lastname: Bock
authors.forename: C S
authors.initials: CS
authors.lastname: Stachel
mesh_terms: D000319:Adrenergic beta-Antagonists / Q000032:analysis*; D000818:Animals; D002138:Calibration; D002417:Cattle; D002853:Chromatography, Liquid / Q000379:methods*; D057230:Limit of Detection; D015203:Reproducibility of Results; D052616:Solid Phase Extraction; D013552:Swine; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014149:Tranquilizing Agents / Q000032:analysis*
chemical_list: D000319:Adrenergic beta-Antagonists; D014149:Tranquilizing Agents