title: Automated one-step supercritical fluid extraction and clean-up system for the analysis of pesticide residues in fatty matrices.
abstract: An automated supercritical fluid extraction and in-line clean-up system has been developed for organochlorine and organophosphate pesticide residues contained in fats. This procedure utilizes supercritical carbon dioxide modified with 3% acetonitrile at 27.58 MPa and 60 degrees C to extract and separate the pesticide residues from the fat on a C1 bonded phase preparative column at 95 degrees C. The automated C1 system recovers 86 of 117 nonpolar to moderately polar organochlorine and organophosphate pesticides from fats. Ten of the 31 pesticides not recovered through the system are not recovered through the conventional clean-up sorbent, Florisil. Pesticide residues can be separated from 0.68 g of butter fat and 0.67 g corn oil, resulting in 2.9 mg of butterfat and 2.1 mg corn oil residue co-eluting into the pesticide fraction. Also, this integrated method can extract and clean-up a 5 g sample of fatty foods containing < 18% fat and 70% moisture. The automated C1 system is reproducible and the amount of co-extracted sample residue in the pesticide fraction yields results comparable to the current methodology, which uses organic solvent extraction and gel permeation chromatography, along with a final Florisil column clean-up step. This automated C1 system simplifies the extraction and clean-up step while reducing solvent usage and hazardous waste.
authors.affiliation: US Food and Drug Administration, Total Diet and Pesticide Research Center, Lenexa, KS 66285-5905, USA. Marvin Hopper@kan.tdrc@fdaoraswr
authors.forename: M L
authors.initials: ML
authors.lastname: Hopper
mesh_terms: D019840:2-Propanol; D000096:Acetone; D001322:Autoanalysis; D002079:Butter / Q000032:analysis; D002623:Chemistry Techniques, Analytical / Q000295:instrumentation / Q000379:methods*; D004041:Dietary Fats / Q000032:analysis*; D004042:Dietary Fats, Unsaturated / Q000032:analysis; D007202:Indicators and Reagents; D007306:Insecticides / Q000032:analysis; D017633:Magnesium Silicates; D009943:Organophosphorus Compounds; D010573:Pesticide Residues / Q000032:analysis*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
chemical_list: D004041:Dietary Fats; D004042:Dietary Fats, Unsaturated; D007202:Indicators and Reagents; D007306:Insecticides; D017633:Magnesium Silicates; D009943:Organophosphorus Compounds; D010573:Pesticide Residues; C005013:Florisil; D000096:Acetone; D002079:Butter; D019840:2-Propanol