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.
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July 2012
An EI-GC/MS method for the determination of pesticide residues in vegetable matrices with high water content was validated using papaya samples. The validation of a multi-residue pesticide method was in agreement with national and international regulations enabling the Ministry of the Agriculture, Livestock and Food Supply of Brazil to cover a large number of matrices and pesticide residues in its monitoring and control programmes. The extraction used 60 mL of ethyl acetate and 30 g of sample previously processed.
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July 2012
A method using QuEChERS extraction and LC-MS/MS in electrospray positive ionisation mode was developed and validated for the analysis of 90 pesticides in a high water content matrix (tomato) in a single chromatographic run. To assess the intra-laboratory reproducibility of the method, validation was conducted on four different days by two different analysts. The validation data was treated using a spreadsheet developed in-house, which sets the most appropriate model for linear fit by determining whether the residuals of the calibration curves are homocedastic or heterocedastic.
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