Multicolumn Solid-Phase Extraction Cleanup of Organophosphorus and Organochlorine Pesticide Residues in Vegetable Oils and Butterfat

Gillespie, Allesia M.; Daly, Sean L; Gilvydis, Dalia M; Schneider, F. H.; Walters, Stephen M

doi:10.1093/jaoac/78.2.431

Cited by 27 publications

(6 citation statements)

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“…The proposed method to determine 23 pesticides and PCBs in virgin olive oil by GC-NPD/ECD is based on a previously published method for the analysis of six OCs and four OPs in vegetable oils and butterfat by GC with electron-capture and flame photometric detectors (16). The original method was modified by using acetonitrile saturated with hexane as eluting solvent for sample preparation and cleanup, allowing for the elution of the most currently used organophosphorus insecticides in olive tree treatment in Spain (dimethoate, diazinon, and parathion-methyl) and a wide range of organochlorine pesticides and polychlorinated biphenyls.…”

Section: Resultsmentioning

confidence: 99%

“…The method proposed is based on a previous technique for OPs and OCs (16), which was modified by using acetonitrile saturated with hexane as eluting solvent for sample preparation and cleanup, allowing for the elution and subsequent determination of the most currently used organophosphorus insecticides in olive tree treatment in Spain (dimethoate, diazinon, and parathion-methyl), and a wide range of organochlorine pesticides and polychlorinated biphenyls. Other modifications were necessary for the GC-NPD/ECD conditions to optimize the separation of all compounds.…”

Section: Discussionmentioning

confidence: 99%

“…Other authors have analyzed olive oil without cleanup (14), or by using a low-temperature cleanup method (15). Many of the more recent methods reported a combination of two or more steps for the cleanup (16,17). A more sophisticated and automated method by on-line reversedphase liquid chromatography-gas chromatography using the through oven transfer adsorption-desorption interface has been recently published (8).…”

Section: Introductionmentioning

confidence: 99%

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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

Yagüe

Bayarri

Conchello

et al. 2005

J. Agric. Food Chem.

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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.

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Section: Resultsmentioning

confidence: 99%

Section: Discussionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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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

Yagüe

Bayarri

Conchello

et al. 2005

J. Agric. Food Chem.

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“…Many multiresidue procedures employing different cleanup techniques and a variety of detection methods have been reported for the determination of organophosphorus pesticide residues in olive oil. In brief, they can be classified into procedures using gas chromatography (GC) after a cleanup step based on partitioning between hexane or light petroleum and acetonitrile (AOAC, 1984;FDA, 1982), gel permeation chromatography (Specht, 1987), and solid-phase extraction using a multicartrige system (Di Muccio et al, 1990;Gillespie et al, 1995). The main disadvantage of these methods is the small sample manipulation (1-3 g) resulting in low analyte detectability.…”

Section: Introductionmentioning

confidence: 99%

Determination of Organophosphorus Pesticide Residues in Greek Virgin Olive Oil by Capillary Gas Chromatography

Hiskia¹,

Atmajidou²,

Tsipi³

1998

J. Agric. Food Chem.

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In this study, the occurrence of 15 organophosphorus pesticide residues in Greek virgin olive oil was investigated. Analysis was carried out using capillary gas chromatography with specific detectors (FPD and NPD), after sample extraction with n-hexane and cleanup by partitioning between n-hexane and acetonitrile. Sixty-two samples of virgin olive oil were taken from the major production areas and packing companies of Greece during 1992-1994. In 46 samples, 9 organophosphorus pesticides, namely dimethoate, fenthion, omethoate, chlorpyrifos, methamidophos, parathion-methyl, parathion, methidathion, and malathion, were found, in concentrations ranging from 0.0005 to 0.1800 mg/kg. Diazinon, pirimiphos-methyl, paraoxon-methyl, malaoxon, carbophenothion, and azinphos-ethyl were not detected in any sample. In most samples pesticide residues were below the detection limits (0.0001 and 0.001 mg/kg), and most of the positive findings were a fraction (i.e., <0.09-18%) of the FAO/WHO Codex Alimentarius maximum residue limits (MRLs) except for dimethoate, which was ranged between 1 and 45%. Only one sample contained dimethoate residue that exceeded the Codex MRL for refined olive oil.

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“…Even a small amount of lipids can cause deterioration of the column and contamination of the GC-electron capture detection (ECD) system. Conventional gravity flow Florisil column and mixed column 12,13 methods were reported to remove residual fat from sample extracts after partial clean-up by liquid-liquid partition for the quantification of organophosphorus, organochlorine and pyrethroid compounds. In general, an acetonitrile-hexane partition step has been used to remove the lipids from oil/fat samples followed by Florisil column chromatography.…”

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confidence: 99%

Rapid preconcentration method for the determination of pyrethroid insecticides in vegetable oils and butter fat and simultaneous determination by gas chromatography–electron capture detection and gas chromatography–mass spectrometry

Ramesh

1998

Analyst

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A simple and rapid solid-phase extraction (SPE)-GC method for the preconcentration and quantification of pyrethroids at low nanogram levels in oils and high fat content samples is presented. The method was studied using seven highly persistent pyrethroid insecticides, viz., cypermethrin, deltamethrin, fenvalerate, cyfluthrin, allethrin, cyhalothrin and permethrin. Preconcentration was achieved by treating the oil samples with methyltrioctylammonium chloride and subsequent elution of the pyrethroid molecules from a graphitized carbon black SPE cartridge using 5 ml of acetonitrile. Pyrethroid quantification was achieved by GC with electron capture detection. Recoveries of the pyrethroids at fortification levels of 0.05-0.5 ppm were 94-105%. Storage on graphitized carbon black for 30 d lowered the recovery of the pyrethroids by only 3-6%. The method compared well with results obtained by a GC-MS method. The relative standard deviation at a concentration level of 0.05-0.2 microgram ml-1 ranged from 1.31 to 5.16%. The limit of detection achieved was 0.002 microgram ml-1 without any additional clean-up and with little interference from lipids during analysis.

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Multicolumn Solid-Phase Extraction Cleanup of Organophosphorus and Organochlorine Pesticide Residues in Vegetable Oils and Butterfat

Cited by 27 publications

References 0 publications

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

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

Determination of Organophosphorus Pesticide Residues in Greek Virgin Olive Oil by Capillary Gas Chromatography

Rapid preconcentration method for the determination of pyrethroid insecticides in vegetable oils and butter fat and simultaneous determination by gas chromatography–electron capture detection and gas chromatography–mass spectrometry

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