PMID- 22587575 OWN - NLM STAT- MEDLINE DCOM- 20120917 LR - 20191210 IS - 1520-5118 (Electronic) IS - 0021-8561 (Linking) VI - 60 IP - 22 DP - 2012 Jun 6 TI - 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. PG - 5532-9 LID - 10.1021/jf3009603 [doi] AB - A novel multiresidue analysis method is developed for the determination of twenty phthalate esters at the mug/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 mug/kg to 2.50 mg/kg with correlation coefficients larger than 0.999. Low detection limits (LODs) of 0.218-1.367 mug/kg and quantification limits (LOQ) of 0.72-4.51 mug/kg were achieved. The mean recoveries were in the range from 93.04% to 104.6% at 5, 15, and 40 mug/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. FAU - Sun, Hanwen AU - Sun H AD - College of Chemistry and Environmental Science, Hebei University, Key Laboratory of Analytical Science and Technology of Hebei Province, Baoding, China. hanwen@hbu.cn FAU - Yang, Yanlei AU - Yang Y FAU - Li, Hui AU - Li H FAU - Zhang, Jingxuan AU - Zhang J FAU - Sun, Na AU - Sun N LA - eng PT - Evaluation Study PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20120525 PL - United States TA - J Agric Food Chem JT - Journal of agricultural and food chemistry JID - 0374755 RN - 0 (Esters) RN - 0 (Phthalic Acids) RN - 0 (Plant Oils) RN - 6O7F7IX66E (phthalic acid) SB - IM MH - Chromatography, Gel/*methods MH - Esters/*analysis/isolation & purification MH - Gas Chromatography-Mass Spectrometry/*methods MH - Microwaves MH - Phthalic Acids/*analysis/isolation & purification MH - Plant Oils/*analysis MH - Solid Phase Extraction/*methods MH - Tandem Mass Spectrometry/methods EDAT- 2012/05/17 06:00 MHDA- 2012/09/18 06:00 CRDT- 2012/05/17 06:00 PHST- 2012/05/17 06:00 [entrez] PHST- 2012/05/17 06:00 [pubmed] PHST- 2012/09/18 06:00 [medline] AID - 10.1021/jf3009603 [doi] PST - ppublish SO - J Agric Food Chem. 2012 Jun 6;60(22):5532-9. doi: 10.1021/jf3009603. Epub 2012 May 25.