HPLC METHOD VALIDATION AND UNCERTAINTY DETERMINATION FOR QUANTIFICATION OF KRESOXIM METHYL FUNGICIDE IN CHILI
DOI:
https://doi.org/10.15421/jchemtech.v34i1.328444Keywords:
Kresoxim methyl; method validation; HPLC; measurement uncertaintyAbstract
A simple and efficient multi-residue analytical method was developed and validated for the determination of Kresoxim methyl (KM) fungicide applied on chili crop for controlling of several fungal diseases. The fungicide residues from chili samples were extracted using modified QuEChERS method, followed by analysis through HPLC–UV. Method validation parameters viz. specificity, linearity, matrix effects, LOD, LOQ, recovery, accuracy and precision, robustness and estimation of measurement uncertainty were evaluated. Specificity of the method based on the chromatographic peak purity was observed in the chromatograms of KM, and calibration curve was found to be linear with R2> 0.99. Matrix effect for KM in chili was < ±20 %. The recovery studies were conducted by spiking the samples at three (LOQ, 5LOQ and 10LOQ) concentration levels. The average recovery of KM at all the three concentrations ranged between 84–86 % with percent RSD < 3 %. Measurement uncertainty (MU) can be helpful while deciding the compliance of chili samples against the established MRL. Hence both type A and type B uncertainties were considered for calculation of combined uncertainty (Uc) in the method validation process. The combined uncertainty (Uc) was below 25 % default value which is normally considered satisfactory for nonfatty matrixes (fruit, vegetables, and grain) by many regulatory authorities for enforcement decisions. The proposed method validation for KM in chili was simple, rapid, and cost effective with high accuracy and sensitivity requiring minimum use of organic solvents.
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