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

Food Chem. 2024 Mar 30;437(Pt 2):137911. doi: 10.1016/j.foodchem.2023.137911. Epub 2023 Nov 3.

Abstract

We propose a new analytical methodology to determine seven pesticides (atrazine, chlorpyrifos, chlorfenvinphos, α-endosulfan, bromopropylate, coumaphos, and τ-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 μg kg-1) and quantification (0.3-9.2 μg 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 α-endosulfan; chlorfenvinphos was determined in some fresh royal jelly samples, and no pesticide residues were detected in the propolis samples analysed.

Keywords: Food analysis; Food safety; Gas chromatography-mass spectrometry; Method validation; Pesticides; Propolis; Royal jelly; Sample treatment.

MeSH terms

  • Chlorfenvinphos* / analysis
  • Endosulfan / analysis
  • Gas Chromatography-Mass Spectrometry / methods
  • Pesticides* / analysis
  • Propolis* / chemistry
  • Solvents

Substances

  • Pesticides
  • royal jelly
  • Propolis
  • Chlorfenvinphos
  • Endosulfan
  • Solvents