Determination of organophosphorus pesticides in fruit juices by matrix solid-phase dispersion and gas chromatography.
A rapid multiresidue method was developed for the determination of nine organophosphorus pesticides in fruit juices. The analytical procedure is based on the matrix solid-phase dispersion (MSPD) of juice samples on Florisil in small glass columns and subsequent extraction with ethyl acetate assisted by sonication. Residue levels were determined by gas chromatography with nitrogen-phosphorus detection. Spiked blank samples were used as standards to counteract the matrix effect observed in the chromatographic determination. The NPD response for all pesticides was linear in the concentration range studied with determination coefficients >0.999. Average recoveries obtained for all of the pesticides in the different juices and fortification levels were >70% with relative standard deviations of <11%. The detection limits ranged from 0.1 to 0.6 microg/kg. The identity of the pesticides was confirmed by gas chromatography with mass spectrometric detection using selected ion monitoring. The proposed MSPD method was applied to determine pesticide residue levels in fruit juices sold in Spanish supermarkets. At least one pesticide was found in most of the samples, although the levels detected were very low, far from the maximum residue levels established for raw fruit.
Albero
Beatriz
B
Departamento de Medio Ambiente, INIA, Carretera de la Coruña Km 7, 28040 Madrid, Spain.
Sánchez-Brunete
Consuelo
C
Tadeo
José L
JL
D001628:Beverages / Q000032:analysis*; D002849:Chromatography, Gas / Q000379:methods*; D005638:Fruit; D008401:Gas Chromatography-Mass Spectrometry; D007306:Insecticides / Q000032:analysis*; D009943:Organophosphorus Compounds; D010573:Pesticide Residues / Q000032:analysis*; D011786:Quality Control; D015203:Reproducibility of Results
D007306:Insecticides; D009943:Organophosphorus Compounds; D010573:Pesticide Residues