In this study, a version of the "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) method was modified to use ethyl acetate (EtOAc) rather than acetonitrile (MeCN) for extraction in the determination of multiple pesticide residues in fruits and vegetables. EtOAc is better suited than MeCN for gas chromatographic (GC) analysis with electron capture detection (ECD) and nitrogen-phosphorus detection (NPD). The method entailed extraction of 30 g chopped sample plus 5 g NaHCO(3) and 30 g anhydrous Na(2)SO(4) with 60 mL EtOAc using a probe blender. After a centrifugation step, removal of residual water and cleanup were performed using dispersive solid-phase extraction (dispersive-SPE) with MgSO(4) and primary secondary amine (PSA) sorbent. (14)C-labeled chlorpyrifos with liquid scintillation counting was used to assist in optimizing and characterizing the method, and GC-ECD and GC-NPD were used for analysis of 24 selected pesticides. The method was validated using tomato, apple and frozen green bean matrices spiked at 0.05, 0.5, and 5 mg/kg. For 22 of the analytes, recoveries averaged 93% for all three commodities over the validation range with a relative standard deviation of 10% (n = 1182). Lower recoveries of dichlorvos were obtained with the method and iprodione determination was compromised in the green beans by an interfering peak. Typical limits of detection were 0.005-0.01 mg/kg with the method.
An olive tree was treated twice in the field with 14C-dimethoate (237.7 muCi, 2.4 g) and 14C residues were determined in the olive fruits at harvest. The fruits were crushed and pressed to extract the crude oil, then refined by neutralization, bleaching and deodorization. The crude oil contained 14.1% of the total 14C in the olive fruits. Neutralization resulted in a reduction of 14C by about 50% of the total 14C residues in oil. Bleaching and deodorization processes further reduced the 14C residues and the refined oil contained 31.6% (which corresponds to 4.4% of 14C residues of the total 14C in olive fruits) of the total 14C in the crude oil. Industrially extracted crude oil was fortified with 14C-dimethoate at 1.8 mg kg-1 (0.02 muCi) level and subjected to the same refining process. A sharp decrease in the amount of 14C was observed by neutralization and the amount of 14C remaining in the refined oil was about 7.3% of the total 14C in the crude fortified oil. The data suggest that the 14C residues in the aged and the fortified oil amples were not of the same nature. The terminal 14C residue in the refined oil obtained from the field experiment did not contain dimethoate and/or its oxon.
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