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

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 Fe 3 O 4 to form water-coated Fe 3 O 4 (W-Fe 3 O 4 ) and rapid extraction can be achieved while W-Fe 3 O 4 dispersed in the sample solution. The analyte adsorbed W-Fe 3 O 4 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 Fe 3 O 4 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.