Organochlorine pesticide analysis in milk by gas-diffusion microextraction with gas chromatography-electron capture detection and confirmation by mass spectrometry

J Chromatogr A. 2021 Jan 11:1636:461797. doi: 10.1016/j.chroma.2020.461797. Epub 2020 Dec 10.

Abstract

Organochlorine pesticides (OCPs) are synthetic compounds less used nowadays due to their toxicity combined with slow degradation which leads to accumulation in the environment. Gas-diffusion microextraction (GDME) was employed prior to gas chromatography with electron capture detection (GC-ECD) and mass spectrometry (GC-MS). For the first time, the low-cost, eco-friendly GDME system was used to extract the OCPs directly from milk samples and associated with GC-ECD. Parameters that affect GDME's performance (extract volume, extraction time, and temperature) were optimized. The calibration curves of all OCPs (α- and β-hexachlorocyclohexane, lindane, hexachlorobenzene, p,p'-DDE, aldrin, dieldrin, and α-endosulfan) had coefficients of determination (r2) ranging from 0.991 to 0.995, and limits of detection (LODs) values ranging from 3.7 to 4.8 µg L-1. This method also provided satisfactory values for precision with relative standard deviations (RSDs) lower than 10% and recoveries above 90%. As a proof-of-concept, several commercial milk samples were analyzed, aldrin was found in one of them but below the maximum residue limits.

Keywords: Dairy products; Food quality; Microextraction; Persistent organic pollutants; Sample preparation; Separation.

MeSH terms

  • Animals
  • Diffusion
  • Electrons*
  • Gas Chromatography-Mass Spectrometry / methods*
  • Hydrocarbons, Chlorinated / analysis*
  • Milk / chemistry*
  • Pesticide Residues / analysis
  • Pesticides / analysis*
  • Reproducibility of Results

Substances

  • Hydrocarbons, Chlorinated
  • Pesticide Residues
  • Pesticides