Comparison of cleanup methods for fipronil and its degradation products in sediment extracts.
Gel permeation chromatography (GPC) and solid phase extraction (SPE) were compared for cleaning extracts containing fipronil, fipronil-sulfide, and fipronil-sulfone at sub-ppb concentrations in sediment. With both methods, analytes were extracted using accelerated solvent extraction, and analyzed with gas chromatography equipped with an electron capture detector. The GPC was performed with a Waters Envirogel GPC column with dichloromethane as the mobile phase, while SPE was conducted with dual-layer cartridges containing graphitized carbon black and primary and secondary amines with a mixture of acetone and hexane as the eluting solvent. Method detection limits for fipronil, fipronil-sulfide, and fipronil-sulfone from three sediments with varying organic carbon content ranged from 0.12 to 0.52 microg/kg dry weight, while percent recoveries were 72-119% from sediment aged from 0.24 to 14d. Although both methods were effective at analyzing fipronil and its degradation products, SPE was the less expensive and less labor-intensive method.
Fisheries and Illinois Aquaculture Center & Department of Zoology, 171 Life Science II, Southern Illinois University, Carbondale, IL 62901, USA.
Amanda A
AA
Brennan
Jing
J
You
Michael J
MJ
Lydy
D000977:Antiparasitic Agents; D002850:Chromatography, Gel / Q000191:economics / Q000379:methods / Q000592:standards*; D003666:Decontamination / Q000379:methods; D052918:Environmental Restoration and Remediation / Q000379:methods*; D019015:Geologic Sediments / Q000737:chemistry*; D007306:Insecticides; D008722:Methods; D011720:Pyrazoles / Q000302:isolation & purification*; D052616:Solid Phase Extraction / Q000191:economics / Q000379:methods / Q000592:standards*; D012997:Solvents
D000977:Antiparasitic Agents; D007306:Insecticides; D011720:Pyrazoles; D012997:Solvents; C082360:fipronil