Ethanol-modified subcritical water extraction combined with solid-phase microextraction for determining atrazine in beef kidney |
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| Authors: | Curren M S King J W |
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| Institution: | National Center for Agricultural Utilization Research, USDA, Agricultural Research Service, 1815 North University Street, Peoria, Illinois 61604, USA. currenms@mail.ncaur.usda.gov |
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| Abstract: | The determination of the levels of pesticides in food products has prompted the development of sensitive and rapid methods of analysis that are solvent-free or utilize solvents that are benign to the environment and laboratory worker. In this study we have developed a novel extraction method that utilizes ethanol-modified subcritical water in combination with solid-phase microextraction (SPME) for the removal of atrazine from beef kidney. In situ sample cleanup was achieved using the technique of matrix solid-phase dispersion. A cross-linked polymer, XAD-7 HP, was utilized as a dispersing material for kidney samples. Subcritical water extractions were performed with a pressurized solvent extraction unit at 100 degrees C and 50 atm. Experimental parameters investigated were the volume of solvent and amount of modifier required for the complete extraction of atrazine and optimization of the extraction time. It was determined that 30% ethanol in water (v/v) is adequate for the complete extraction of atrazine. A Carbowax-divinylbenzene SPME fiber was used to sample the aqueous extracts. Analysis of the fiber contents was by ion-trap GC/MS utilizing the single ion mode. The total time of analysis for a single kidney sample is 90 min. The average percent recoveries from samples spiked to the concentrations of 2 and 0.2 microg/g were 104 and 111, respectively. The average relative standard deviations were 10 and 9, respectively. The method limit of detection for beef kidney spiked with atrazine was found to be 20 ng/g of sample. |
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