MSPD procedure for determining buprofezin, tetradifon, vinclozolin, and bifenthrin residues in propolis by gas chromatography–mass spectrometry

A simple and effective extraction method based on matrix solid-phase dispersion (MSPD) was developed to determine bifenthrin, buprofezin, tetradifon, and vinclozolin in propolis using gas chromatography–mass spectrometry in selected ion monitoring mode (GC–MS, SIM). Different method conditions were evaluated, for example type of solid phase (C 18 , alumina, silica, and Florisil), the amount of solid phase and eluent ( n -hexane, dichloromethane, dichloromethane– n -hexane (8:2 and 1:1, v / v ) and dichloromethane–ethyl acetate (9:1, 8:2 and 7:3, v / v )). The best results were obtained using 0.5 g propolis, 1.0 g silica as dispersant sorbent, 1.0 g Florisil as clean-up sorbent, and dichloromethane–ethyl acetate (9:1, v / v ) as eluting solvent. The method was validated by analysis of propolis samples fortified at different concentration levels (0.25 to 1.0 mg kg −1 ). Average recoveries (four replicates) ranged from 67% to 175% with relative standard deviation between 5.6% and 12.1%. Detection and quantification limits ranged from 0.05 to 0.10 mg kg −1 and 0.15 to 0.25 mg kg −1 propolis, respectively.