Desenvolvimento e validação de um método para análise simultânea de agrotóxicos e micotoxinas em cervejas, insumos e subprodutos

Abstract

A multiclass analytical procedure for determining residues and contaminants in the beer production chain was developed and validated. Two different extraction methods were evaluated during optimization: QuEChERS and Dilute and Shoot (D&S), both of them followed by LC-MS/MS quantification. Thirty-two pesticides and 7 mycotoxins that have maximum limits in barley or malt established by the National Health Surveillance Agency (ANVISA) were evaluated during this step. The D&S approach was selected and validated according to the European guides SANTE/11813/2017 and EC/401/2006 and the Analytical Quality Assurance Manual of the Ministry of Agriculture, Livestock and Supply. Linearity, veracity, precision, measurement uncertainty, detection and quantification limits were evaluated for more than 200 pesticides and 7 mycotoxins in malt, wort residue and beer matrices. The validated method has been applied to 40 real samples so far, and 36 of them showed any of the analyzed substances presence. Among the 22 malt and wort residue samples, all showed pesticide residues, most of them unregistered or with unauthorized use. There was contamination by ochratoxin A above the maximum limits established by both the European Union and ANVISA in one of the malt samples. Detections in beer occurred at low levels, except for a sample whose concentration of pesticide picolinafem was estimated at 0.03 mg L-1. The method is reliable and easy to apply for mycotoxins and pesticides determination in complex matrices, having been evaluated in accordance with strict national and international legislation.