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.

Development and validation of a multi-residue method for pesticide determination in honey using on-column liquid–liquid extraction and liquid chromatography–tandem mass spectrometry

“…These studies, however, usually focused on the analysis of very few compounds, often belonging to one or two pesticide families at the most, such as organochlorine or organophosphorous residues. As demands of pesticide analysis started to be more motivated accordingly similar agrarian uses rather than similar physico-chemical properties of chemicals, multi-analyte determinations have appeared since the end of nineties, covering several classes of pesticides [2][3][4][5].…”

Current trends in sample preparation for growth promoter and veterinary drug residue analysis

“…Argauer et al developed a method to isolate ten pyrethroids from ground meat using SF-CO2 [382]. Rissato et al reported a SFE method that combined extraction and Florisil ® clean up of pyrethroids residues from honey samples [383]. More recently solid-phase microextraction (SPME), MSPD and QuEChERS have been used in the analysis of pyrethroids.…”

Multiresidue Analysis of Pesticides in Vegetables and Fruits by Supercritical Fluid Extraction and Liquid Chromatography-Tandem Mass Spectrometry

“…A number of supercritical fluid extraction SFE methods have been developed as alternatives to conventional liquid extraction methods for determining pesticide residues in foods, such as vegetables and fruits 2 -10 , cereals 11 -16 , eggs 17 , 18 , meat 19 , oil 20 , baby food 21 , and honey 22 . The main advantages of SFE are that it can lead to less solvent use and that it can be automated, reducing labor costs.…”