Desenvolvimento e validação de uma metodologia analítica para análise de micotoxinas em cerveja utilizando QuEChERS e UHPLC-MS/MS

Abstract

This study reports the results obtained with the development and validation of an analytical method for the simultaneous determination and quantification of nineteen mycotoxins in beers marketed in Belo Horizonte markets. A methodology was employed employing QuEChERS, with acetonitrile as solvent, without acidifying the sample. The equipment used for extract analysis was an ultra-high performance liquid chromatograph coupled with sequential mass spectrometer (UHPLC-MS / MS). The mass spectrometer operated in positive and negative mode and two transitions were chosen for each analyte. Validation was based on the Analytical Quality Assurance Manual: Food Waste and Contaminants, EC Directives 401/2006 and 2002/657 / EC and SANTE 11813/2017 and 12089/2016, and the following merit figures were assessed: selectivity, matrix effect, linearity, intermediate truth and accuracy, detection and quantification limits and measurement uncertainty. The methodology was selective for seventeen of the nineteen mycotoxins under investigation. The matrix effect was observed for 79% of the analytes. Linearity and recovery were evaluated using fortified white matrix extract, and the chosen methodology was efficient for the seventeen analytes, with recoveries ranging from 56 to 118%. The accuracy of the method was evaluated in terms of repeatability and intermediate precision and the values calculated using the Horwitz equation. The detection and quantification limits were determined from the CCα and CCβ values, respectively, to prevent these limits from falling below the calibration curve. Measurement uncertainties were based on the bottom-up methodology. Finally, ten samples obtained from local commerce of Pilsen, Lager, wheat and non-alcoholic beers were tested, and no contamination occurred in the samples. It is evaluated that the proposed methodology for mycotoxin analysis in beer was adequate to determine seventeen of the nineteen mycotoxins under study, promising to be used in fiscal analysis for quality control and food safety, following the main national and international regulations. international quality standards.