Validation of LC-MS/MS method for simultaneous determination of chlorpyrifos, deltamethrin, imidacloprid and some of their metabolites in maize silage

Abstract

In this study, a validation of a multi-residue analysis method was performed for the simultaneous analysis of chlorpyrifos (CHL), deltamethrin (DEL) and Imidacloprid (IMI) residues and some of their metabolites in maize silage, by LC MS/MS. Extraction was conducted with acetonitrile acidified with 1% acetic acid. To avoid the matrix effect, a matrix matched calibration was used. The method was validated according to the SANTE/12682/2019 Guidelines. Selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), trueness (recovery %) and precision (intra-day and inter-day) parameters were evaluated in line with the SANTE document. The linearities of all compounds were quite confident (R-2 >= 0.98) and no interference was observed. The LOD and LOQ values were between 2.76 mu g kg(-1) to 53.61 mu g kg(-1) and 9.19 mu g kg(-1) to 178.71 mu g kg(-1), respectively. The recovery, repeatability RDSr and reproducibility RDSR values of compounds were calculated between 93.7-109.2%, 1-15%, and 1-13%, respectively. Consequently, results obtained with the evaluation of all parameters were found to be compatible with the SANTE validation criteria, so the method was reliable, effective and easy to use for the detection of insecticides and metabolites in maize silage with LC MS/MS.