title: 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.
abstract: 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.
authors.affiliation: Institute of Agricultural Quality Standards and Testing Technology Research, Hubei Academy of Agricultural Science, Wuhan 430064, China; Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, China.
authors.forename: Xi-Tian
authors.initials: XT
authors.lastname: Peng
authors.affiliation: Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, China.
authors.forename: Li
authors.initials: L
authors.lastname: Jiang
authors.affiliation: Institute of Agricultural Quality Standards and Testing Technology Research, Hubei Academy of Agricultural Science, Wuhan 430064, China.
authors.forename: Yan
authors.initials: Y
authors.lastname: Gong
authors.affiliation: Institute of Agricultural Quality Standards and Testing Technology Research, Hubei Academy of Agricultural Science, Wuhan 430064, China.
authors.forename: Xi-Zhou
authors.initials: XZ
authors.lastname: Hu
authors.affiliation: Institute of Agricultural Quality Standards and Testing Technology Research, Hubei Academy of Agricultural Science, Wuhan 430064, China.
authors.forename: Li-Jun
authors.initials: LJ
authors.lastname: Peng
authors.affiliation: Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, China. Electronic address: yqfeng@whu.edu.cn.
authors.forename: Yu-Qi
authors.initials: YQ
authors.lastname: Feng
mesh_terms: D000818:Animals; D052203:Ferrosoferric Oxide / Q000737:chemistry*; D005399:Fishes / Q000378:metabolism; D005506:Food Contamination / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D006801:Humans; D057230:Limit of Detection; D059346:Magnets; D008863:Microspheres; D010575:Pesticides / Q000302:isolation & purification*; D011078:Polychlorinated Biphenyls / Q000302:isolation & purification*; D015203:Reproducibility of Results; D052617:Solid Phase Microextraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods; D015040:Zirconium / Q000737:chemistry*
chemical_list: D010575:Pesticides; D015040:Zirconium; D011078:Polychlorinated Biphenyls; C028541:zirconium oxide; D052203:Ferrosoferric Oxide
keywords: Fish; Magnetic materials; Pesticides; Polychlorinated biphenyls; QuEChERS; ZrO(2)