Desenvolvimento e validação de métodos multiresíduos para determinação de medicamentos veterinários em alimentos e em ração utilizando CL-EM/EM

Abstract

This work reports the house validation of quantitative and qualitative methods for multiresidue determination of veterinary drugs in foods. A new method for extraction and clean up has been developed and it was named Liquid-Liquid Extraction with Fast Partition at Very Low Temperature (LLE-FPVLT). In addition, refinements of the QuEChERS (Quick, Easy, Cheap, Effective, Safe and Ruged) procedure were introduced in order to cover the extraction of residues of veterinary drugs in complex matrices such as tissues, milk and animal feed. These procedures use the analytical techniques High Performance or Ultra Efficiency Liquid Chromatography coupled to Tandem Mass Spectrometry. The validation procedures are in accordance with national and international protocols, and the parameters investigated were: linearity, matrix effect, selectivity, accuracy, precision (repeatability and intermediate precision), limits of detection and quantification, limits of decision (CCá), detection capacity (CCâ) and expanded uncertainty. The applicability of the proposed procedures was demonstrated in the validation of five quantitative methods: determination of 15 sulfonamides in porcine liver, multiresidue determination (27veterinary drugs) in bovine milk; multiresidue determination (21 veterinary drugs) in chicken, multiresidue determination (32 drugs veterinarians) in fish Sparus aurata and determination of 13 sulfonamides in animal feed, and a qualitative method: multiresidue determination (37 veterinary drugs) in porcine muscle. All methods demonstrated to be suitable for their purpose of use.