Combining supercritical fluid extraction of soil herbicides with enzyme immunoassay analysis.
Supercritical fluid extraction (SFE) of soil herbicides followed by enzyme immunoassay analysis (EIA) is explained in a step-by-step process. Extracted herbicides, include 2,4-D, simazine, atrazine, and alachlor. The herbicide, trifluralin was not successfully analyzed by EIA because of crossreacting metabolites. Problems with SFE, including uneven packing of cells, leaks, uneven flow and clogging, can largely be eliminated as the method parameters are optimized. It was necessary to add modifiers including methanol or acetone to the SF CO2 to increase the solubility of the analytes. Detection limits of 2.5 ng/g soil for atrazine and alachlor and 15 ng/g soil for simazine and 2,4-D without concentration of the sample were achieved. Recoveries above 80% and relative standard deviations (RSDs) less than 15% for 2,4-D simazine, atrazine and alachlor were achieved. Atrazine and alachlor recoveries were above 90% with RSDs below 10%. Forty soil samples could be extracted and analyzed in an 8-h day.
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Center for the Management, Utilization and Protection of Water Resources, Tennessee Technological University, Box 5033, Cookeville, TN 38505-0001, USA.
D015084:2,4-Dichlorophenoxyacetic Acid / Q000032:analysis; D000081:Acetamides / Q000032:analysis; D000096:Acetone / Q000494:pharmacology; D001280:Atrazine / Q000032:analysis; D025924:Chromatography, Supercritical Fluid / Q000379:methods*; D006540:Herbicides / Q000032:analysis*; D007124:Immunoenzyme Techniques / Q000379:methods*; D000432:Methanol / Q000494:pharmacology; D015203:Reproducibility of Results; D012839:Simazine / Q000032:analysis; D012989:Soil Pollutants; D013997:Time Factors
D000081:Acetamides; D006540:Herbicides; D012989:Soil Pollutants; D000096:Acetone; C000188:alachlor; D015084:2,4-Dichlorophenoxyacetic Acid; D001280:Atrazine; D012839:Simazine; D000432:Methanol