OTIMIZAÇÃO E VALIDAÇÃO DE MÉTODO ANALÍTICO PARA PREPARO DA AMOSTRA E DETERMINAÇÃO SIMULTÂNEA DE SULFONAMIDAS EM MEL

Abstract

This work presents and discusses the results of the validation of a method for determination of sulfonamide residues in honey bees africanized of the Alto Turi - MA. In preparation of the honey samples, was used acid hydrolysis and employed a system of solid phase extraction in cartridge ABS - Elut Nexus. The eluate was analyzed by liquid chromatography with diode array detection. To determine the limits of detection and quantification, standard curves were constructed with solutions in concentrations ranging from 0.025 to 5.0 μg mL-1, the method was linear in this range. The correlation coefficients obtained ranged from 0.9994 to 0.9999 for the study sulfonamides. The limits of detection and quantification were calculated according to conventional statistical procedures and results were considered satisfactory for the purpose of the method. The recoveries were obtained in the range from 63 to 98%, with a coefficient of variation from 0,4 to 9,9%, which is satisfactory for complex matrices. The maximum sulfonamide residues in honey is 50 μg kg-1, however due to the complexity of the sample for quantification was possible only at a concentration of 100 μg kg-1. It was also made the physicochemical characterization of the honey samples using a method based on CODEX Alimentarius and Association of Official Analytical Chemists, in which it was found that all samples were within the standards established by the Brazilian legislation regarding the index diastasis, minerals, color and hydroxymethylfurfural. Regarding the acidity, 71% of the samples had high values, already on the moisture content and insoluble solids, only two samples were higher than those recommended by Instruction nº11 of the Ministry of Agriculture, Livestock and Supply.