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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.
J Agric Food Chem. 2005 Jun 29; 53(13):5105-9.JA

Abstract

A multicolumn solid-phase extraction cleanup for the determination of organophosphorus (OP) and organochlorine (OC) pesticides plus PCB congeners in virgin olive oil is presented. The method involves dissolution of the olive oil in hexane, followed by a cleanup system using a diatomaceous earth column (Extrelut-QE) with reversed (C(18)) 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 microg/kg olive oil for OPs, and from 1 to 6 microg/kg olive oil for OCs and PCBs. In the case of positive samples, the confirmation of pesticide identity was performed by ion-trap GC-MS/MS. The applicability of the method 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 10 microg/kg. Organochlorine pesticides were found in 5-47% of samples at very low levels ranging from 1.5 to 5.2 microg/kg. PCBs were found in 20-90% of samples, showing concentrations between 2.3 and 17.3 microg/kg.

Authors+Show Affiliations

Department of Animal Production and Food Science, Veterinary Faculty, University of Zaragoza, Spain.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

15969482

Citation

Yagüe, Cristina, et al. "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." Journal of Agricultural and Food Chemistry, vol. 53, no. 13, 2005, pp. 5105-9.
Yagüe C, Bayarri S, Conchello P, et al. 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. J Agric Food Chem. 2005;53(13):5105-9.
Yagüe, C., Bayarri, S., Conchello, P., Lázaro, R., Pérez-Arquillué, C., Herrera, A., & Ariño, A. (2005). 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. Journal of Agricultural and Food Chemistry, 53(13), 5105-9.
Yagüe C, et al. 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. J Agric Food Chem. 2005 Jun 29;53(13):5105-9. PubMed PMID: 15969482.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - 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. AU - Yagüe,Cristina, AU - Bayarri,Susana, AU - Conchello,Pilar, AU - Lázaro,Regina, AU - Pérez-Arquillué,Consuelo, AU - Herrera,Antonio, AU - Ariño,Agustín, PY - 2005/6/23/pubmed PY - 2005/8/16/medline PY - 2005/6/23/entrez SP - 5105 EP - 9 JF - Journal of agricultural and food chemistry JO - J Agric Food Chem VL - 53 IS - 13 N2 - A multicolumn solid-phase extraction cleanup for the determination of organophosphorus (OP) and organochlorine (OC) pesticides plus PCB congeners in virgin olive oil is presented. The method involves dissolution of the olive oil in hexane, followed by a cleanup system using a diatomaceous earth column (Extrelut-QE) with reversed (C(18)) 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 microg/kg olive oil for OPs, and from 1 to 6 microg/kg olive oil for OCs and PCBs. In the case of positive samples, the confirmation of pesticide identity was performed by ion-trap GC-MS/MS. The applicability of the method 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 10 microg/kg. Organochlorine pesticides were found in 5-47% of samples at very low levels ranging from 1.5 to 5.2 microg/kg. PCBs were found in 20-90% of samples, showing concentrations between 2.3 and 17.3 microg/kg. SN - 0021-8561 UR - https://www.unboundmedicine.com/medline/citation/15969482/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_ DB - PRIME DP - Unbound Medicine ER -