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Preparation of mesoporous ZrO2-coated magnetic microsphere and its application in the multi-residue analysis of pesticides and PCBs in fish by GC-MS/MS

文献类型： 外文期刊

作者： Peng, Xi-Tian 1 ; Jiang, Li 2 ; Gong, Yan 1 ; Hu, Xi-Zhou 1 ; Peng, Li-Jun 1 ; Feng, Yu-Qi 2 ;

作者机构： 1.Hubei Acad Agr Sci, Inst Agr Qual Stand & Testing Technol Res, Wuhan 430064, Peoples R China

2.Wuhan Univ, Dept Chem, Key Lab Analyt Chem Biol & Med, Minist Educ, Wuhan 430072, Peoples R China

关键词： Pesticides;Polychlorinated biphenyls;ZrO2;Magnetic materials;QuEChERS;Fish

期刊名称：TALANTA （ 影响因子：6.057； 五年影响因子：5.386 ）

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收录情况： SCI

摘要： A novel mesoporous ZrO2 immobilized magnetic Fe3O4 microsphere (m-ZrO2@Fe3O4) was successfully synthesized and characterized by transmission electron microscope (TEM). X-ray diffractometer (XRD), nitrogen adsorption measurement (NAM), energy-dispersive X-ray analysis (EDX), vibrating sample magnetometer (VSM). Then the resultant m-ZrO2@Fe3O4 and an n-octadecylphosphonic acid modified magnetic microsphere (Fe3O4-OPA) were employed as clean-up co-adsorbents of QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) method for the analysis of 42 pesticides and 7 polychlorinated biphenyls (PCBs) in fish samples. Lipid co-extractives such as fatty acids in QuEChERS extracts could be efficiently removed through the Lewis acid-Lewis base interaction between m-ZrO2@Fe3O4 and carboxylic groups, while some other apolar interferents could be adsorbed through hydrophobic interaction by Fe3O4-OPA. Meanwhile, the magnetic property of adsorbents endows the clean-up procedure with manipulative convenience. Several parameters affecting the clean-up performance were investigated. Under the optimal conditions, the modified QuEChERS method combined with gas chromatography-tandem mass spectrometry (GC-MS/MS) for the multi-class, multi-residue analysis of pesticides and PCBs in fish samples was validated according to linearility, recovery and precision. Good linearities were obtained for all analytes with R-2 larger than 0.9903. Limits of detection (LODs) were found to be in the range of 0.02-4.40 ng/g. The method recoveries of all analytes spiked at three concentration levels in blank fish samples were from 69.8% to 117.1%, with the intra-day and inter-day relative standard deviations (RSDs) less than 13.4% and 16.5%, respectively. (C) 2014 Elsevier B.V. All rights reserved.

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