Desenvolvimento e validação de um método para determinação das fumonisinas B1 e B2 em milho e derivados empregando a dispersão da matriz em fase sólida e a HPLC-MS/MS

Abstract

This work describes the development and validation of a method for thedetermination of fumonisins B1 and B2 in maize. The optimization of the extraction and purification procedures was executed using matrix solid phase dispersion. The final procedure was to disperse the ground sample with silica gel; build a syringe type cartridge with the dispersed material; elute with ammonium formate buffer (pH 9):THF (70:30v/v); dilute with acetonitrile: ultrapure water (1: 1 v/v); centrifuge; filter the extract. The validated method employed HPLC-MS/MS technique for separation, identification and quantification of the fumonisin B1 and B2, evaluating one transition of mass for quantification and two for confirmation using the MRM mode. The evaluated validation parameters showed good performances: linearity (R2 >0.999), repeatability (RSD 22%), intermediate precision (RSD 18%), percentage of recovery (87-101%) and detection and quantification limits lower than the maximum residue limit of fumonisin allowed by legislation. The uncertainty assessment was also estimated, considering the analytical curve and the sample preparation procedures as the main sources.