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| Determination of Nine Phthalic Acid Esters in Tilapia by Solid Phase Extraction Coupled with High Performance Liquid Chromatography-Tandem Mass Spectrometry |
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| DOI：10.3969/j.issn.1004-4957.年份.月份 |
| KeyWord:high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） tilapia PAEs solid phase extraction residues |
| Author | Institution |
| 李拥军,熊文明,陈坚文,温贤有,李谦,刘正华,李盛安 |
1.中山市农产品质量监督检验所;2.中国广州分析测试中心广东省分析测试技术公共实验室;3.小榄镇农业服务中心 |
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| Abstract: |
| A high performance liquid chromatography-tandem mass spectrometric（HPLC-MS/MS）method was developed for the determination of nine PAEs,including bis（2-methoxyethyl） phthalate（DMEP）,diethyl phthalate（DEP）,benzyl butyl phthalate（BBP）,bis（2-n-butoxyethyl） phthalate（DBEP）,dipentyl phthalate（DPP）,bis-4-methyl-2-pentyl） phthalate（BMPP）,dihexyl phthalate（DHXP）,bis（2-ethyl-h exyl） phthalate（DEHP）and di-n-octyl phthalate（DNOP） residues in tilapia sample.The samples were extracted with ethyl acetate,and purified with LC-Si solid phase extraction column.Methanol and formic acid-ammonium acetate buffer were used as mobile phase by gradient elution.The analysis of target compounds was carried out by HPLC-MS/MS with positive electrospray ionization（ESI+） under multiple reaction monitoring（MRM） mode.A matrix matched external standard was used for the quantitative analysis.The calibration curves for nine PAEs were in good linearities between their peak areas and concentrations of 1.0-200.0 μg?L-1 with correlation coefficients not less than 0.991 8.The average spiked recoveries ranged from 75% to 107%.The relative standard deviations of intra-batch and inter-batch were in the ranges of 1.9%-11.8% and 3.6%-13.1%,respectively.The proposed method was simple,rapid,sensitive and accutate,and could meet the requirements for residue analysis. |
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