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精恶唑禾草灵在土壤及甘蓝中残留动态及在土壤中吸附特性研究

The Residual Dynamics in Cabbage and Soil and Adsorption Study of Fenoxaprop-p-ethyl

【作者】 贾福艳

【导师】 逯忠斌;

【作者基本信息】 吉林农业大学 , 环境工程, 2004, 硕士

【摘要】 精恶唑禾草灵是一种芳氧苯氧丙酸类除草剂,用于防除禾本科杂草。本文对精恶唑禾草灵及其代谢物在土壤及甘蓝中的残留分析方法、残留动态,以及精恶唑禾草灵在土壤中的吸附特性进行了研究。为制定残留标准提供依据。 土壤样品以乙酸乙酯和碳酸氢钠水溶液提取,将母体与代谢物分离后分别净化。母体过氧化铝柱净化,代谢物则通过调节水相酸碱度用二氯甲烷净化。最后将母体与代谢物同时收集浓缩,选择Zorbax18柱以甲醇水混合液为流动相,进行高效液相色谱(HPLC)分析。甘蓝样品中,母体以丙酮和碳酸氢钠水溶液提取,并用氧化铝柱净化,分析条件同土壤样品。代谢物则用甲醇和0.1mol/1 HC1溶液提取,用二氯甲烷萃取浓缩后,过硅胶柱净化,选择ZorbaxC18柱以甲醇和乙酸酸化的水溶液为流动相进行HPLC分析。方法的回收率为83.28-90.00%,变异系数为0.88-3.88%。母体在土壤和甘蓝中的最小检出浓度为0.01mg/kg,代谢物在土壤和甘蓝中的最小检出浓度为0.02mg/kg。 通过在吉林省2001年、2002年两年田问试验,对精恶唑禾草灵在以360mL/hm2用量处理的土壤和甘蓝样品作残留动态分析。降解过程符合一级反应动力学模式C=Coe-kt。在土壤中两年的动态方程分别是:2001年,C=0.1929e-0.0113t,半衰期为44.3小时。2002年,C=0.2003e-0.0115t,半衰期为43.2小时。代谢物在施药后5小时开始检出,72小时浓度达到最大后降低。在甘蓝中两年的动态方程是:2001年,C=0.2376e-0.1489t,半衰期为6.4小时。2002年,C=0.2596e-0.1562t,半衰期为6.0小时。代谢物在3小时后开始检出,8小时达到最大浓度后降低。精恶唑禾草灵在收获期甘蓝和土壤中均未检出。结果表明:精恶唑禾草灵在土壤和甘蓝中易降解,且在甘蓝中降解速度比在土壤中快。 土壤对精恶唑禾草灵的吸附试验,选取了有机质含量不同的两种类型土壤:草甸黑土和风沙土。采用经典的振荡平衡法进行研究。在5克土壤中加入0.81mg/kg精恶唑禾草灵饱和水溶液。在25℃水浴中振荡,不同时间内取水溶液用正己烷提取后进行气相色谱(GC)法分析。结果表明,两种土壤对精恶唑禾草灵均有极强的吸附性。

【Abstract】 Fenoxaprop-p-ethyl (FNE) is a selective post-emergence herbicide controlling annual grass weed in dicotyledonous crops. The determination and degradation of FNE and its metabolite, fenoxaprop-p (FNA), in soil and cabbage were studied. The adsorption of FNE by soil was also studied.The soil samples were extracted with ethyl acetate-sodium hydrogen Carbonate solution. After partition of the parent compound and its metabolite, the organic phase containing FNE was cleaned up with dichloromethane. Then combine the FNE and FNA. HPLC analysis was performed with Zorbax C18 column. FNA and FNE were eluted with methanol-water mixtures. The cabbage samples were extracted with acetone-sodium hydrogen carbonate solution mixtures to attain FNE, and then cleaned up with alumna. The HPLC analysis is the same as the soil. In order to attain FNA, the cabbage samples were extracted with hydrochloric acid-methanol mixtures and cleaned up with silica. The HPLC analysis was performed with Zebra C8 column. FNA was eluted with methanol-glacis acetic acid solution. The recovery of the method was 83.28-90.00% and C.V. was 0.88-3.88%. The detect limit of FNE in soil and cabbage was 0.01ug/g, and FNA was 0.02ug/g.The degradation of FNE and FNA in soil and cabbage was studied by HPLC method and a 2-yr field experiment in Jilin province. The soil and cabbage were treated with FNE at 360mL/hm2. Sample the soil and cabbage at different time to do degradation dynamics analysis. The degradation procedure of FNE was correspond to the mathematic pattern, C=C0e-kt. In soil, the dynamic equation in 2001 was c=0.1929e-0.0113t and the half-life was 44.3h, and the dynamic equation in 2002 was c=0.2003e-0.0115t and half-life was 43.2h. FNA was detected in soil after 5h and the highest amount was at 72h. In cabbage, the dynamic equation in 2001 was c=0.2376e-0.1489t and the half-life was 6.4h, and the dynamic equation in 2002 was c=0.2596e-0.1562t and half-life was 6.0h. FNA was detected in cabbage after 3h and the highest amount was at 8h. FNE and FNA were not detected in soil and cabbage at harvest. The result showed that FNE was dissipated in soil and cabbage rapidly and the degradation of FNE in cabbage was more quickly than in soil.The adsorption of FNE by soil was studied by the equilibrium method. Two different soil types were used in the study.0.81ug/g FNE solutions (25mL) was added to soil (5g) and was shaken on a shaker at 25C. Sample the FNE solutions at different time. A GC method wascarried out to detect the FNE amount in water. The result showed that FNE could be adsorbed by the two soils strongly.

【关键词】 精恶唑禾草灵HPLC残留甘蓝土壤吸附
【Key words】 fenoxaprop-p-ethylHPLCresiduesoilcabbageadsorption
  • 【分类号】X592
  • 【被引频次】4
  • 【下载频次】242
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