Extraction and cleanup of organochlorine and organophosphorus pesticide residues in fats by supercritical fluid techniques.
A supercritical fluid extraction and cleanup procedure was developed for separating organochlorine and organophosphorus pesticides from fats. Supercritical carbon dioxide modified with 3% (v/v) acetonitrile was used to extract the pesticides at 60 degrees C and separate the pesticides from the fats at 4000 psi and 95 degrees C on an in-line, C1 silica-based column. The extraction and cleanup procedure gave good recoveries for 43 of 62 nonpolar to moderately polar organochlorine and organophosphorus pesticides from fats, whereas 49 were recovered through conventional Florisil column cleanup before quantitation. This procedure can extract and clean up pesticide residues from 0.65 g animal-based fat and 1.0 g oils. Coeluted residues in the pesticide fraction ranged from 2.5 mg for butterfat to 0.8 mg for corn oil. Results for samples analyzed with this integrated extraction cleanup procedure were reproducible and comparable with results obtained with the current Total Diet Study methodology.
Hopper
M L
ML
U.S. Food and Drug Administration, Total Diet and Pesticide Research Center, Lenexa, KS 66285-5905, USA.
D002849:Chromatography, Gas; D004041:Dietary Fats / Q000032:analysis*; D005504:Food Analysis; D005506:Food Contamination; D006843:Hydrocarbons, Chlorinated; D007306:Insecticides / Q000302:isolation & purification*; D017633:Magnesium Silicates; D009943:Organophosphorus Compounds; D010573:Pesticide Residues / Q000302:isolation & purification*
D004041:Dietary Fats; D006843:Hydrocarbons, Chlorinated; D007306:Insecticides; D017633:Magnesium Silicates; D009943:Organophosphorus Compounds; D010573:Pesticide Residues; C005013:Florisil