PMID- 25476287 OWN - NLM STAT- MEDLINE DCOM- 20150728 LR - 20141205 IS - 1873-3573 (Electronic) IS - 0039-9140 (Linking) VI - 132 DP - 2015 Jan TI - 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. PG - 118-25 LID - S0039-9140(14)00750-4 [pii] LID - 10.1016/j.talanta.2014.08.069 [doi] AB - 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. CI - Copyright (c) 2014 Elsevier B.V. All rights reserved. FAU - Peng, Xi-Tian AU - Peng XT AD - 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. FAU - Jiang, Li AU - Jiang L AD - Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, China. FAU - Gong, Yan AU - Gong Y AD - Institute of Agricultural Quality Standards and Testing Technology Research, Hubei Academy of Agricultural Science, Wuhan 430064, China. FAU - Hu, Xi-Zhou AU - Hu XZ AD - Institute of Agricultural Quality Standards and Testing Technology Research, Hubei Academy of Agricultural Science, Wuhan 430064, China. FAU - Peng, Li-Jun AU - Peng LJ AD - Institute of Agricultural Quality Standards and Testing Technology Research, Hubei Academy of Agricultural Science, Wuhan 430064, China. FAU - Feng, Yu-Qi AU - Feng YQ AD - 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. LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20140908 PL - Netherlands TA - Talanta JT - Talanta JID - 2984816R RN - 0 (Pesticides) RN - C6V6S92N3C (Zirconium) RN - DFC2HB4I0K (Polychlorinated Biphenyls) RN - S38N85C5G0 (zirconium oxide) RN - XM0M87F357 (Ferrosoferric Oxide) SB - IM MH - Animals MH - Ferrosoferric Oxide/*chemistry MH - Fishes/metabolism MH - Food Contamination/*analysis MH - Gas Chromatography-Mass Spectrometry/methods MH - Humans MH - Limit of Detection MH - Magnets MH - Microspheres MH - Pesticides/*isolation & purification MH - Polychlorinated Biphenyls/*isolation & purification MH - Reproducibility of Results MH - Solid Phase Microextraction/*methods MH - Tandem Mass Spectrometry/methods MH - Zirconium/*chemistry OTO - NOTNLM OT - Fish OT - Magnetic materials OT - Pesticides OT - Polychlorinated biphenyls OT - QuEChERS OT - ZrO(2) EDAT- 2014/12/06 06:00 MHDA- 2015/07/29 06:00 CRDT- 2014/12/06 06:00 PHST- 2014/06/16 00:00 [received] PHST- 2014/08/26 00:00 [revised] PHST- 2014/08/31 00:00 [accepted] PHST- 2014/12/06 06:00 [entrez] PHST- 2014/12/06 06:00 [pubmed] PHST- 2015/07/29 06:00 [medline] AID - S0039-9140(14)00750-4 [pii] AID - 10.1016/j.talanta.2014.08.069 [doi] PST - ppublish SO - Talanta. 2015 Jan;132:118-25. doi: 10.1016/j.talanta.2014.08.069. Epub 2014 Sep 8.