*2.5. Quantification and Quality Assurance*

The two methods (LC-MS/MS and GC-MS/MS) were validated for specificity, selectivity, reproducibility, repeatability, recovery, and sensitivity according to SANTE guidance documents (applicable at the time of the study) on analytical quality control and method validation procedures for pesticide residues analysis in food and feed [18,19]. For analyte confirmation, retention time (RT) and ion ratio were used. Recoveries were estimated using internal standards and were found to vary between 65 and 120% for all the analytes. The repeatability and reproducibility of both methods were tested by the analysis of multiple spiked with the mixture of analytical standards samples at three different concentrations (at LOQ, 10LOQ, and 100LOQ). The calculated limits of quantification LOQs and other validation metrics for each individual compound are presented in the Supplementary Data (Table S1) and in previous works of our group [11,16,17]. Honey and pollen used as control samples were also analyzed to monitor background contamination. Control samples were analyzed in every sequence of samples, and no pesticide residues and their metabolites were detected in any of them.
