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Validation of a method for determination of organophosphates in black-bean samples

Author: 
Joyce Aparecida Tavares de Miranda, Lucia Maria Jaeger de Carvalho, Izabela Miranda de Castro, Ana Cláudia de Macêdo Vieira, Verônica de Oliveira Figueiredo, Marianna Ramos dos Anjos and Gisela Maria Dellamora Ortiz
Subject Area: 
Life Sciences
Abstract: 

The presence of pesticides residues above the Acceptable Daily Intake values and the Maximum Residue Limits is worrying in the point of view of food safety. In order to identify and determine the presence of organ phosphorus pesticides in bean samples, a multiresidue technique of extraction method was applied, and the analyses were conducted by gas chromatography coupled to a thermoionic flame detector (GC-FTD). This study aimed to validate the methodology of determination of organophosphates by studies of selectivity, linearity, intermediate precision, limit of detection, limit of quantification, and accuracy study by addition and recovery. The method was selective for all analytes, because there was no interference higher than 30% of the limit of quantification. The limits of detection were between 1.60 and 52.96 ng.kg-1 and the quantification limits were between 3.30 and 176.0 ng.kg-1. Regarding intermediate precision, the differences of area values were ≤ 15%, in different concentrations, except for phorate. The correlation coefficients (r) of linearity curves were higher than 0.99 for all active ingredients, within the working range applied. The recovery percentage was between 70 and 120%, except for phorate. Thus, the methodology was satisfactory for identification and determination of ten from the eleven organophosphates analyzed in beans.

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