title: Development of multiresidue analysis for twenty phthalate esters in edible vegetable oils by microwave-assisted extraction-gel permeation chromatography-solid phase extraction-gas chromatography-tandem mass spectrometry.
abstract: A novel multiresidue analysis method is developed for the determination of twenty phthalate esters at the μg/kg level in edible vegetable oils by microwave-assisted extraction-gel permeation chromatography-solid phase extraction-high resolution gas chromatography-tandem mass spectrometry (MAE-GPC-SPE-HRGC-MS/MS). The samples were extracted with methanol under microwave incubation. Cleanup was carried out with GPC followed by a further C18 SPE column and then separated by the HP-5MS capillary column under a temperature program. The eluents were qualitatively and quantitatively determined by tandem mass analyzer with selected reaction monitoring (SRM) type and positive ion mode. The calibration curves showed good linearity in the range 5 μg/kg to 2.50 mg/kg with correlation coefficients larger than 0.999. Low detection limits (LODs) of 0.218-1.367 μg/kg and quantification limits (LOQ) of 0.72-4.51 μg/kg were achieved. The mean recoveries were in the range from 93.04% to 104.6% at 5, 15, and 40 μg/kg spiked levels, and the relative standard deviations (RSDs) were in the range of 1.01% and 5.26% (n = 7). This method could potentially overcome the interference from large amounts of lipids and pigment. The real sample test showed this method can be used for sensitive and accurate determination and confirmation of phthalate ester residues in high-fat and complex samples.
authors.affiliation: College of Chemistry and Environmental Science, Hebei University, Key Laboratory of Analytical Science and Technology of Hebei Province, Baoding, China. hanwen@hbu.cn
authors.forename: Hanwen
authors.initials: H
authors.lastname: Sun
authors.forename: Yanlei
authors.initials: Y
authors.lastname: Yang
authors.forename: Hui
authors.initials: H
authors.lastname: Li
authors.forename: Jingxuan
authors.initials: J
authors.lastname: Zhang
authors.forename: Na
authors.initials: N
authors.lastname: Sun
mesh_terms: D002850:Chromatography, Gel / Q000379:methods*; D004952:Esters / Q000032:analysis* / Q000302:isolation & purification; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D008872:Microwaves; D010795:Phthalic Acids / Q000032:analysis* / Q000302:isolation & purification; D010938:Plant Oils / Q000032:analysis*; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods
chemical_list: D004952:Esters; D010795:Phthalic Acids; D010938:Plant Oils; C032279:phthalic acid