Determination of Pesticides and PCBs in Virgin Olive Oil by Multicolumn Solid-Phase Extraction Cleanup Followed by GC-NPD/ECD and Confirmation by Ion-Trap GC-MS

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• 作者：Cristina Yag&uuml ; e ; Susana Bayarri ; Pilar Conchello ; Regina Lá ; zaro ; Consuelo Pé ; rez-Arquillué ; Antonio Herrera ; and Agustí ; n Ari&ntilde ; o
• 刊名：Journal of Agricultural and Food Chemistry
• 出版年：2005
• 出版时间：June 29, 2005
• 年：2005
• 卷：53
• 期：13
• 页码：5105 - 5109
• 全文大小：46K
• 年卷期：v.53,no.13(June 29, 2005)
• ISSN：1520-5118

文摘

A multicolumn solid-phase extraction cleanup for the determination of organophosphorus (OP) andorganochlorine (OC) pesticides plus PCB congeners in virgin olive oil is presented. The methodinvolves dissolution of the olive oil in hexane, followed by a cleanup system using a diatomaceousearth column (Extrelut-QE) with reversed (C₁₈) and normal (alumina) phase SPE columns.Determination of OPs was by GC-NPD, while the OCs and PCBs were analyzed using GC-ECD.Recovery assays for OPs varied from 81.7% to 105.3%, for OCs ranged between 74.3% and 99.4%,while for PCBs were from 60.1% to 119.2%. Quantitation limits ranged from 10 to 25 mages/entities/mgr.gif">g/kg olive oilfor OPs, and from 1 to 6 mages/entities/mgr.gif">g/kg olive oil for OCs and PCBs. In the case of positive samples, theconfirmation of pesticide identity was performed by ion-trap GC-MS/MS. The applicability of themethod was assayed with 19 virgin olive oil samples collected from different olive mills of Aragón(Spain). Only one OP pesticide (acephate) was detected in one sample at a concentration of 10mages/entities/mgr.gif">g/kg. Organochlorine pesticides were found in 5-47% of samples at very low levels ranging from1.5 to 5.2 mages/entities/mgr.gif">g/kg. PCBs were found in 20-90% of samples, showing concentrations between 2.3 and17.3 mages/entities/mgr.gif">g/kg.Keywords: Virgin olive oil; organophosphorus pesticides; organochlorine pesticides; polychlorinatedbiphenyls; capillary gas chromatography-mass spectrometric detection