Abstract
A highly sensitive, efficient and rugged analytical method was developed and validated for determination of residues of more than 400 multiclass pesticides in honey using QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) approach in combination with liquid and gas chromatography coupled to tandem mass spectrometry (LC-MS/MS and GC-MS/MS). Various combinations of extracting solvents and cleanup sorbents were evaluated to optimize the sample preparation step. The method involving acetonitrile as extracting solvent and primary secondary amine (PSA) with magnesium sulphate (MgSO4) as cleanup sorbent proved to be the most effective. The analytical method was validated at 5, 10, and 20 µg kg−1 in accordance with SANTE/11312/2021 and FDA guidelines and found suitable for simultaneous determination of 206 pesticides on LC-MS/MS and 197 pesticides on GC-MS/MS with acceptable recovery (70–120%), precision (RSD <20.0%), linearity (correlation coefficient ≥ 0.99) at limit of quantification (LOQ) ranging from 5 and 10 µg kg−1. The method was successfully applied to monitor pesticide residues in 80 market honey samples collected from different parts of India. The developed method enabled the quantitative determination of a wide spectrum of pesticide residues in honey in a single chromatographic run.
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