o DEVELOPMENT AND VALIDATION OF AN ANALYTICAL METHOD BY HPLC-UV FOR THE DETERMINATION OF PESTICIDE RESIDUES IN GREEN GRAPES MARKETED IN CARUARU-PE

DEVELOPMENT AND VALIDATION OF AN ANALYTICAL METHOD BY HPLC-UV FOR THE DETERMINATION OF PESTICIDE RESIDUES

Abstract

Pesticides can prevent, destroy, repel, or lessen the damage caused by pests, most crops need a maximum residue limit of these substances. There are records of analytical methods created to track them. This study sought to develop and validate an analytical method capable of quantifying pesticide residues in green grapes. The method was developed using HPLC coupled to a fixed wavelength UV spectroscopy detector in the following parameters: stationary phase in Kinetex C18 reverse phase 150 x 4.6 mm (5 μm) column and mobile phase consisting of acetonitrile and water in isocratic mode; flow of 0.8 mL/min and injection of 20 μL; detection at 220 nm. The development and validation of the analytical method were carried out in accordance with RDC 166/2017. In linearity, a 5-point calibration curve was made, in triplicate, resulting in: R=0.9915, y=20307x + 193193 for Cyromazine and, R=0.9918, y=70578.4x + 110230 for Imidacloprid. Accuracy was tested with triplicate injections, resulting in averages: 5.038; 20.091 and 41.017 μg/mL for Cyromazine and 0.502; 2,051; and 4.091 μg/mL for Imidacloprid. In the precision of the method, a solution of 20 and 2 μg/mL was injected for Cyromazine and Imidacloprid, respectively, on two different days, by different analysts, totaling 24 injections, resulting in VC below 1.85 and 1.82. The method proved to be adequate for the quantification of Cyromazine and Imidacloprid in grape samples. Of the three samples, one contained Cyromazine, not authorized in this type of culture according to the National Health Surveillance Agency.