Analysis of permethrin isomers in composite diet samples by molecularly imprinted solid-phase extraction and isotope dilution gas chromatography-ion trap mass spectrometry.
Determination of an individual's aggregate dietary ingestion of pesticides entails analysis of a difficult sample matrix. Permethrin-specific molecularly imprinted polymer (MIP) solid-phase extraction cartridges were developed for use as a sample preparation technique for a composite food matrix. Vortexing with acetonitrile and centrifugation were found to provide optimal extraction of the permethrin isomers from the composite foods. The acetonitrile (with 1% acetic acid) was mostly evaporated and the analytes reconstituted in 90:10 water/acetonitrile in preparation for molecularly imprinted solid-phase extraction. Permethrin elution was accomplished with acetonitrile and sample extracts were analyzed by isotope dilution gas chromatography-ion trap mass spectrometry. Quantitation of product ions provided definitive identification of the pesticide isomers. The final method parameters were tested with fortified composite food samples of varying fat content (1%, 5%, and 10%) and recoveries ranged from 99.3% to 126%. Vegetable samples with incurred pesticide levels were also analyzed with the given method and recoveries were acceptable (81.0-95.7%). Method detection limits were demonstrated in the low ppb range. Finally, the applicability of the MIP stationary phase to extract other pyrethroids, specifically cyfluthrin and cypermethrin, was also investigated.
Vonderheide
Anne P
AP
United States Environmental Protection Agency, Cincinnati, OH 45268, USA.
Boyd
Brian
B
Ryberg
Anna
A
Yilmaz
Ecevit
E
Hieber
Thomas E
TE
Kauffman
Peter E
PE
Garris
Sherry T
ST
Morgan
Jeffrey N
JN
D005504:Food Analysis; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D007536:Isomerism; D054802:Molecular Imprinting; D026023:Permethrin / Q000737:chemistry*; D010573:Pesticide Residues / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000379:methods*; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods
D010573:Pesticide Residues; D026023:Permethrin