Supercritical fluid extraction for pesticide multiresidue analysis in honey: determination by gas chromatography with electron-capture and mass spectrometry detection
ABSTRACT An analytical procedure using supercritical fluid extraction (SFE) and capillary gas chromatography with electron-capture detection was developed to determine simultaneously residues of different pesticides (organochlorine, organophosphorus, organonitrogen and pyrethroid) in honey samples. Fortification experiments were conducted to test conventional extraction (liquid-liquid) and optimize the extraction procedure in SFE by varying the CO2-modifier, temperature, extraction time and pressure. Best efficiency was achieved at 400 bar using acetonitrile as modifier at 90 degrees C. For the clean-up step, Florisil cartridges were used for both methods LLE and SFE. Recoveries for majority of pesticides from fortified samples of honey at fortification level of 0.01-0.10 mg/kg ranged 75-94% from both methods. Limits of detection found were less than 0.01 mg/kg for ECD and confirmation of pesticide identity was performed by gas chromatography-mass spectrometry in selected-ion monitoring mode. The multiresidue methods in real honey samples were applied and the results of developed methods were compared.
SourceAvailable from: Marcello Locatelli
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ABSTRACT: In the present work, an easy, fast, and effective approach is developed for the extraction and enrichment of triazole and triazine pesticides in honey by air-assisted liquid–liquid microextraction coupled with gas chromatography-flame ionization detection. Initially, honey is dissolved in an acetonitrile: water mixture and after that a few microliter of a less soluble organic solvent in aqueous phase is added. In order to form a cloudy solution, the extractant mixed with aqueous phase is repeatedly sucked and expelled by a syringe needle into a glass tube. After centrifugation, the sedimented phase (1 mL) is removed with a syringe and injected into de-ionized water. By this action, the settled phase volume is reduced to 10 μL and the analytes are concentrated, too. Under optimum extraction conditions, limits of detection and quantitation for the studied pesticides are in the ranges of 2 to 5 and 6 to 17 ng/g, respectively. Extraction recoveries and enrichment factors are from 61% to 95% and 61 to 95, respectively.Practical ApplicationThe proposed approach can be applied for determination of pesticide in honey and may be developed to other complex matrices.Journal of Food Science 09/2014; 79(10). DOI:10.1111/1750-3841.12597 · 1.79 Impact Factor