Desenvolvimento e validação de método para determinação simultânea de Carbadox e Olaquindox em ração para aves por cromatografia líquida de alta eficiência com confirmação em espectrometria de massas

Abstract

Among the problems faced nowadays by the Brazilian meat industry for exporting, one of the most concerning is undoubtedly the presence of veterinary drug residues in animal tissue. The use of carbadox and olaquindox as growth promoting agents in animal feed has beenbanned in Brazil since 2004 and because of this ban, the availability of rapid methods, reliable and sensitive determination of these drugs in feed are of fundamental importance. Based on these aspects, the objective of this study was to develop and validate an analytical method that uses a single extraction step for qualitative and quantitative analysis of Carbadox and Olaquindox in poultry feed by high performance liquid chromatography (HPLC) and confirmation by mass spectrometry (MS/MS). The performance parameters evaluated were: linearity, working range, matrix effect, precision and accuracy, sensitivity, detection limit,quantification limit, decision limit (CC), detection capability (CC) and uncertainty. It was observed adjustment of all determinations to the linear regression, evidenced by the values of correlation coefficients close to 1. There was no significant matrix effect on the detector response. The recovery ranged from 70 to 108% for Olaquindox and 87 to 118% for Carbadox. The detection limits were 0.0009 and 0.008g.ml-1 (9g.kg-1 and 80g.kg-1) and quantification limits were 0.0012 and 0.011g.ml-1 (12g.kg-1 and 110g.kg-1) for carbadox and olaquindox, respectively. It was concluded that the developed and validated method meets the purpose of use, because of the validation results, the short time analysis and the few analytical steps, which are desirable characteristics in a chromatographic method.