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The procedure for simultaneous extraction from soil and determination by means of GC-ECD insecticides: aldrin, dieldrin, endrin and herbicide: atrazine was worked out. The proposed GC-ECD technique provides limits of detection in range 12 μg/mL - 18 μg/mL and 2 μg/mL, for insecticides and atrazine, respectively. Two different types of extraction: microwave assisted extraction (MAE) and ultrasound assisted extraction (UAE) with different solvents were tested to choose the procedure that provides the highest recoveries of analytes and low detection limits, typical for trace analysis (100 ppm or 100 mg/g, IUPAC). On the basis of recoveries and precision both extraction methods were compared. The insecticides recovery from soil samples obtained by UAE were in range 40-85%, coefficient of variation (CV): 1.3-5.0%, whereas for atrazine recovery was below 15% (CV: 8-18%). The most efficient and precise extraction procedure turned out to be MAE with n-hexane: acetone. The recoveries were in range 70-85% for insecticides and 84% for atrazine, CV: 0.4-2.2% and 5.3% for insecticides and atrazine, respectively. The presented MAE-GC-ECD procedure enables extraction and determination of aldrin, dieldrin, endrin and atrazine in soil samples with high recoveries, precision and limits of detections in range 6 ng/g - 8 ng/g in the case of insecticides and 1.5 ng/g for atrazine. The MAE-GC-ECD procedure was applied for the above mentioned pesticides determination in environmental samples. Soils were collected in agricultural as well as rural areas in Poland. In all cases atrazine was determined in concentration range: 0.0187 mg/g - 0.1107 mg/g. Aldrin and dieldrin was detected in soil samples from two locations.
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