Abstract. The use of supercritical fluid extraction (SFE) to recover pesticides from environmental matrices was investigated using chlorpyrifos methyl spiked on a wheat kernel substrate. Volume-based extraction recovery profiles were generated to determine the pressure, temperature, and fluid composition that yielded the maximum analyte recovery and minimum extraction time. On-line coupled microcolumn liquid chromatography-gas chromatography (LC-GC) with electron capture detection was used to effect cleanup of the extracts and to determine the recoveries of chlorpyrifos methyl.With unmodified CO, as the extraction solvent, we obtained only 65% recovery of chlorpyrifos methyl spiked at the 50 parts per billion (ppb) level on the wheat. The use of CO, mixed with 2% methanol, however, yielded recoveries averaging 97.8%, with a relative standard deviation of 4.0%. Extraction times were 10 min or less for a 1-g sample size. The use of PEEK sealing material in the extraction vessels and in the ferrules of the finger-tight fittings in the SFE system permitted rapid cycling between multiple samples and reliable, leak-free operation. This approach could significantly shorten the sample preparation time associated with pesticide residue analysis.
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