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.

Keywords:

• tranquiliser
• azaperone
• promazine
• carazolol
• haloperidol
• xylazine
• kidney
• recommended concentration
• MRL
• validation
• LC-MS/MS
• 2002/657/EC

Acknowledgement

The authors thank Dagmar Holzkamp and Andrej Petruck for their technical assistance in the studies.