Dispersive microextraction based on water-coated Fe₃O₄ followed by gas chromatography-mass spectrometry for determination of 3-monochloropropane-1,2-diol in edible oils

J Chromatogr A. 2012 Jun 1:1240:45-51. doi: 10.1016/j.chroma.2012.03.090. Epub 2012 Apr 4.

Abstract

In the present work, we developed a novel dispersive microextraction technique by combining the advantages of liquid-phase microextraction (LPME) and magnetic solid-phase extraction (MSPE). In this method, trace amount of water directly absorbed on bare Fe₃O₄ to form water-coated Fe₃O₄ (W-Fe₃O₄) and rapid extraction can be achieved while W-Fe₃O₄ dispersed in the sample solution. The analyte adsorbed W-Fe₃O₄ can be easily collected and isolated from sample solution by application of a magnet. It was worth noting that in the proposed method water was used as extractant and Fe₃O₄ served as the supporter and retriever of water. The performance of the method was evaluated by extraction of 3-monochloropropane-1,2-diol (3-MCPD) from edible oils. The extracted 3-MCPD was then derived by a silylanization reagent (1-trimethylsilylimidazole) before gas chromatography-mass spectrometry (GC-MS) analysis. Several parameters that affected the extraction and derivatization efficiency were investigated. Our results showed that the limit of detection for 3-MCPD was 1.1 ng/g. The recoveries in spiked oil samples were in the range of 70.0-104.9% with the RSDs less than 5.6% (intra-day) and 6.4% (inter-day). Taken together, the simple, rapid and cost-effective method developed in current study, offers a potential application for the extraction and preconcentration of hydrophilic analytes from complex fatty samples.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Dietary Fats, Unsaturated / analysis*
  • Fats, Unsaturated / chemistry*
  • Ferrosoferric Oxide / chemistry*
  • Gas Chromatography-Mass Spectrometry / methods*
  • Glycerol / analogs & derivatives*
  • Glycerol / analysis
  • Hydrophobic and Hydrophilic Interactions
  • Imidazoles / chemistry
  • Limit of Detection
  • Linear Models
  • Liquid Phase Microextraction / methods
  • Reproducibility of Results
  • Solid Phase Microextraction / methods*
  • Trimethylsilyl Compounds / chemistry
  • Water / chemistry
  • alpha-Chlorohydrin

Substances

  • Dietary Fats, Unsaturated
  • Fats, Unsaturated
  • Imidazoles
  • Trimethylsilyl Compounds
  • Water
  • 1-(trimethylsilyl)-1H-imidazole
  • alpha-Chlorohydrin
  • Glycerol
  • Ferrosoferric Oxide