Multiclass Analytical Method for Pesticide and Mycotoxin Analysis in Malt, Brewers’ Spent Grain, and Beer: Development, Validation, and Application

Abstract

A multiclass analytical method to determine pesticides and mycotoxins in beer-related matrices based on the dilute and shoot approach was optimized and validated according to the European guidelines SANTE/12682/2019 and EC/401/2006. Extraction used acidified acetonitrile at 1% (v/v) acetic acid, followed by horizontal shaking homogenization, centrifugation, freeze-out step for cleanup, another centrifugation, and injection into a high-performance liquid chromatography–tandem mass spectrometry system. Linearity, detection and quantification limits, accuracy, and measurement uncertainty were evaluated, and 201, 184, and 176 analytes were validated for malt, beer, and brewers’ spent grain, respectively. The limits of quantification ranged between 1 and 200 μg kg–1 and between 5 and 1000 μg kg–1 for beer and malt, respectively, and expanded uncertainties ranged between 9.7 and 50%, meeting the legislation requirements. A total of 40 samples have been analyzed thus far, and 36 of them exhibited the presence of some of the analyzed substances. The validated method is reliable and easy to apply for mycotoxin and pesticide determination in complex matrices.

Comprehensive Review on Monitoring, Behavior, and Impact of Pesticide Residues during Beer-Making

“…For these water-soluble pesticides, there are many analytical methods using other chromatographic techniques such as high-performance liquid chromatography (HPLC), supercritical fluid chromatography (SFC), ultrahigh-performance liquid chromatography (UHPLC), or ultra-performance convergence chromatography (UPC 2 ). A lot of analytical methods using this technique have been proposed in recent years to analyze pesticide residues in cereals, malt, hop, and beer. ,,,− …”

Comparative analysis of mycotoxin, pesticide, and elemental content of Canarian craft and Spanish mainstream beers

“…Such studies show that the most pesticide concentrations are reduced during fermentation, pasteurization, clarification and filtration [18] , [28] , [41] , [62] . These studies have shown that final pesticide levels are generally low [50] . Nonetheless, some studies have raised consumer concern by reporting pesticide levels at levels above the limit allowed in drinking water [16] , [63] , and 92% of beers on the Latvian market have been shown to contain glyphosate [30] .…”

Stability Evaluation of Aflatoxin B1 Solution Certified Reference Material via Ultra-High Performance Liquid Chromatography Coupled with High-Resolution Mass Spectrometry

“…The method has been developed to measure the fraction of AFB 1 in solutions fast and facilely using ultra-high performance liquid chromatography (UHPLC) coupled with a diode array detector (DAD) or mass spectrometry (MS). It has been considered the golden approach for the measurement of AFB 1 fractions due to its high reproducibility and accuracy. ,− Nevertheless, the accuracy of this method largely relies on the certified reference materials (CRMs) of AFB 1 solutions prepared with various organic solvents.…”

“…As one of the aflatoxins, aflatoxin B 1 (AFB 1 , its chemical structure shown in Figure ) has been classified as a group I carcinogen by the International Agency Research on Cancer (IARC) . It has been widely found in agricultural commodities and foods, i.e., grains, vegetables, oils, milk, and eggs. − In addition, AFB 1 is highly toxic and has been identified as hepatotoxic, carcinogenic, and teratogenic and can cause other specific symptoms. , Thus, AFB 1 is the subject of the regulations on foods and agricultural feeds. The corresponding legislation in over 80 countries has established the maximum permitted limit of AFB 1 in various foods and agricultural commodities aiming to protect human beings and animals. − Accurate measurement of AFB 1 in various matrices is a prerequisite for effectively limiting the fractions of AFB 1 in agricultural products and foods.…”

“…It has been considered the golden approach for the measurement of AFB 1 fractions due to its high reproducibility and accuracy. 8 , 13 − 16 Nevertheless, the accuracy of this method largely relies on the certified reference materials (CRMs) of AFB 1 solutions prepared with various organic solvents.…”