摘要
为了全面评价土壤质量安全,及时、准确地测量土壤中残留农药的种类和含量水平,采用添加回收率试验,借助气相色谱–电子捕获检测器（GC–ECD）,建立了同时分析和检测己唑醇、稻瘟酰胺、螺螨酯和苯醚甲环唑在土壤中残留量的方法。结果表明：土壤样品用乙腈经超声波提取15 min,再用弗罗里硅土柱净化后（用50 m L乙腈分次淋洗）,在优化后的气相色谱条件（初始温度180℃,保持3 min,以20℃/min升至260℃,保持7 min,进样口温度280℃,检测器温度300℃,载气（N2）流速为5 m L/min,尾吹流速30 m L/min,进样量1μL,分流比20∶1）下对土壤样品进行分析检测,当4种农药的质量浓度为0.02-1.00 mg/L时,4种供试农药的浓度与相应色谱峰峰面积呈良好的线性关系（相关系数≥0.996 7,均达极显著水平）,在0.05、0.50、1.00 mg/kg3个添加水平下的平均回收率为89.9%-100.2%,相对标准偏差为2.7%-8.6%,最小检出量均为0.05 ng,方法的定量限均为0.05 mg/kg。
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.
出处
《湖南农业大学学报（自然科学版）》
CAS
CSCD
北大核心
2015年第2期209-213,共5页
Journal of Hunan Agricultural University(Natural Sciences)
基金
湖南省科学技术厅项目(2006FJ4266)
关键词
土壤
农药残留量
己唑醇
稻瘟酰胺
螺螨酯
苯醚甲环唑
气相色谱法
soil
amount of pesticide residues
hexaconazole
fenoxanil
spirodiclofen
difenoconazole
gas chromatography
