Supercritical fluid extraction for pesticide multiresidue analysis in honey: determination by gas chromatography with electron-capture and mass spectrometry detection.
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.
Rissato
Sandra R
SR
Department of Chemistry, Faculty of Sciences, Paulista State University (UNESP), 17033-360 Bauru (SP), Brazil. srissato@fc.unesp.br
Galhiane
Mário S
MS
Knoll
Fátima R N
FR
Apon
Bernhard M
BM
D025924:Chromatography, Supercritical Fluid / Q000379:methods*; D005506:Food Contamination; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006722:Honey / Q000032:analysis*; D010575:Pesticides / Q000032:analysis*; D015203:Reproducibility of Results; D013696:Temperature; D013995:Time
D010575:Pesticides