Journal of AOAC International · 2003 · 5.5K citations · 5 references
PharmacyFood ScienceChromatographic AnalysisFood AnalysisMass Spectrometric AnalysisChromatographyExtraction TechniquesPesticide ChemistryPesticide Residue AnalysisPesticide ResiduesSolid-phase ExtractionAnalytical Methods DevelopmentDispersive Solid-phase ExtractionFood Sample PreparationGas Chromatography-mass SpectrometryPesticide DetectionPesticide RemovalPesticide Residue RemovalSolid-liquid Partitioning
The study presents a simple, fast, and inexpensive method for determining pesticide residues in fruits and vegetables. The method uses a single‑phase acetonitrile extraction of 10 g samples, liquid‑liquid partitioning with MgSO₄ and NaCl, simultaneous water removal and cleanup via dispersive solid‑phase extraction with MgSO₄ and PSA, followed by GC/MS analysis, allowing a single chemist to process six samples in under 30 min at roughly $1 per sample. Recoveries ranged from 85 % to 101 % (mostly >95 %) with repeatabilities below 5 % for a broad spectrum of fortified pesticides, including polar and basic compounds.
A simple, fast, and inexpensive method for the determination of pesticide residues in fruits and vegetables is introduced. The procedure involves initial single-phase extraction of 10 g sample with 10 mL acetonitrile, followed by liquid-liquid partitioning formed by addition of 4 g anhydrous MgSO4 plus 1 g NaCl. Removal of residual water and cleanup are performed simultaneously by using a rapid procedure called dispersive solid-phase extraction (dispersive-SPE), in which 150 mg anhydrous MgSO4 and 25 mg primary secondary amine (PSA) sorbent are simply mixed with 1 mL acetonitrile extract. The dispersive-SPE with PSA effectively removes many polar matrix components, such as organic acids, certain polar pigments, and sugars, to some extent from the food extracts. Gas chromatography/mass spectrometry (GC/MS) is then used for quantitative and confirmatory analysis of GC-amenable pesticides. Recoveries between 85 and 101% (mostly > 95%) and repeatabilities typically < 5% have been achieved for a wide range of fortified pesticides, including very polar and basic compounds such as methamidophos, acephate, omethoate, imazalil, and thiabendazole. Using this method, a single chemist can prepare a batch of 6 previously chopped samples in < 30 min with approximately 1 dollar (U.S.) of materials per sample.
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