Development and validation of an analytical methodology based on solvent extraction and gas chromatography for determining pesticides in royal jelly and propolis

We propose a new analytical methodology to determine seven pesticides (atrazine, chlorpyrifos, chlorfenvinphos, alpha-endosulfan, bromopropylate, coumaphos, and tau-fluvalinate) in royal jelly and propolis products using gas chromatography-mass spectrometry. Sample treatment, with minor modifications for propolis, consisted of a solvent extraction with a hexane and isopropanol mixture, and a further clean-up step. Meanwhile, chromatographic analysis (<25 min) was performed in a DB-5MS column under programmed temperature conditions. In all cases we validated the method in terms of selectivity, limits of detection (0.1-2.8 mu g kg(-1)) and quantification (0.3-9.2 mu g kg(-1)), linearity, matrix effect (<+/- 20 %), trueness (recoveries between 93 % and 118 %), and precision (relative standard deviation < 11 %). All royal jelly liquid dietary supplements were positive for chlorfenvinphos and, in the case of one of them, for alpha-endosulfan; chlorfenvinphos was determined in some fresh royal jelly samples, and no pesticide residues were detected in the propolis samples analysed.