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《Journal of Hunan Agricultural University(Natural Sciences)》 2015-02
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Residual determination of four kinds of pesticides in soil using gas chromatography

Ren Yingjun;Gong Daoxing;Zheng Chen;Yuan Yajie;Yang Lihua;College of Resource and Environment, Hunan Agricultural University;  
In order to comprehensively evaluate the safety of soil quality and to measure type and amount of pesticide residual in soil in a fast and accurate way, a new method for determining hexaconazole, fenoxanil, spirodiclofen and difenoconazole at one time in soil was established by employing fortified recovery experiment and gas chromatography with electron capture detection(GC–ECD). Soil samples were firstly extracted with acetonitrile and ultrasonic in 15 minutes, then cleaned up with florisil-phase extraction(leaching with 50 m L of acetonitrile in several times), and finally determined using the optimized conditions of gas chromatography, they were the initial temperature was 180 ℃ for 3 min, then it was raised to 260 ℃ for 7 min at a heating rate of 20 ℃/min, and the other conditions including the injection temperature, detector temperature, the flow rate of nitrogen gas, makeup flow, the injection volume and split ratio were 280 ℃, 300 ℃, 5 m L/min, 30 m L/min, 1 μL and 20: 1, respectively. The results showed that there were good linear relation between concentration and corresponding chromatographic peak area of the four kinds of pesticides at their concentration level ranged from 0.02 to 1.00 mg/L( their correlation coefficients were all higher than 0.996 7).When the fortified level were improved from 0.05 mg/kg to 1.00 mg/kg, their average recoveries were ranged from 89.9% to 100.2%, with relative standard deviation ranged from 2.7% to 8.6%.The limit of detection and limit of quantificationfor the four pesticides were 0.05 ng and 0.05 mg/kg, respectively.
【Fund】: 湖南省科学技术厅项目(2006FJ4266)
【CateGory Index】: X833;O657.71
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