Análise de resíduos de pesticidas em farinha de trigo integral usando método QuEChERS modificado e determinação por LC-MS/MS

Abstract

Due to the frequent use of agrochemicals, it is important to control the same. Thereby, instrumental analytical methods, particularly liquid chromatography analyzes, are able to qualitatively and quantitatively evaluate mixtures of these substances. The objective of this study was to develop and validate a method of extraction for simultaneous determination of pesticide residues in whole wheat flour. The QuEChERS method was modified in the extraction stage using in place of magnesium sulfate, sodium sulfate in the first step also the modified method not performed the step of clean up. After the modified method was validated and the chromatographic conditions used. For the extraction was used acetonitrile with 1% acetic acid, sodium sulfate, sodium acetate and sodium citrate sesquihydrate. Was not carried out the clean up step. The method was validated by evaluating the following parameters: selectivity, linearity, limit of detection, limit of quantification, precision, accuracy and robustness. The linear range evaluated in this study was 1.0 to 200 mg L-1. Agrochemicals analyzed showed r² of at least 0.99 is considered acceptable by the rules of ANVISA. The quantification limit of the modified QuEChERS method showed equal and/or lower than the maximum residue limits established by Brazilian legislation (ANVISA) values. Of agrochemicals analyzed in whole wheat flour, 84% presented with percentage recovery between 70-120%, with repeatability and intermediate precision with RSD ≤ 20%. The 2,4-D agrochemicals, Cartap Hidrocloride, Cyproconazole, Ethyl Paraquat, Parathion-methyl and fenitrothion, were not quantified with safety in fortification levels evaluated presenting mean recovery values outside the reliable range for residue analysis. Evaluating the samples collected in Serra Gaucha region, all agrochemicals detected in wholewheat flour, were carbendazim, chlorpyrifos, Deltamitrina, Imidacloprid, Malathion, Pendimentalina, Pirimiphos-methyl, and Triamedifom Triadimenol, had values below the MRL established by ANVISA, Codex Alimentarius and the European Union. The developed and validated method was adequate and can therefore be applied in the determination of agrochemicals residues in whole wheat flour.