title: Dispersive microextraction based on water-coated Fe₃O₄ followed by gas chromatography-mass spectrometry for determination of 3-monochloropropane-1,2-diol in edible oils.
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.
authors.affiliation: Key Laboratory of Analytical Chemistry for Biology and Medicine-Ministry of Education, Department of Chemistry, Wuhan University, Wuhan 430072, China.
authors.forename: Qin
authors.initials: Q
authors.lastname: Zhao
authors.forename: Fang
authors.initials: F
authors.lastname: Wei
authors.forename: Neng
authors.initials: N
authors.lastname: Xiao
authors.forename: Qiong-Wei
authors.initials: QW
authors.lastname: Yu
authors.forename: Bi-Feng
authors.initials: BF
authors.lastname: Yuan
authors.forename: Yu-Qi
authors.initials: YQ
authors.lastname: Feng
mesh_terms: D004042:Dietary Fats, Unsaturated / Q000032:analysis*; D005224:Fats, Unsaturated / Q000737:chemistry*; D052203:Ferrosoferric Oxide / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D005990:Glycerol / Q000031:analogs & derivatives* / Q000032:analysis; D057927:Hydrophobic and Hydrophilic Interactions; D007093:Imidazoles / Q000737:chemistry; D057230:Limit of Detection; D016014:Linear Models; D059627:Liquid Phase Microextraction / Q000379:methods; D015203:Reproducibility of Results; D052617:Solid Phase Microextraction / Q000379:methods*; D014297:Trimethylsilyl Compounds / Q000737:chemistry; D014867:Water / Q000737:chemistry; D000517:alpha-Chlorohydrin
chemical_list: D004042:Dietary Fats, Unsaturated; D005224:Fats, Unsaturated; D007093:Imidazoles; D014297:Trimethylsilyl Compounds; D014867:Water; C054025:1-(trimethylsilyl)-1H-imidazole; D000517:alpha-Chlorohydrin; D005990:Glycerol; D052203:Ferrosoferric Oxide