苯醚甲环唑在香蕉、荔枝及土壤中的残留检测研究
摘要
苯醚甲环唑是先正达公司研制开发的一种新型三唑类杀菌剂。纯品为无色固体,熔点76℃,不溶于水易于溶于有机溶剂。苯醚甲环唑不仅具有高效、广谱的特点,而且对哺乳动物低毒。本文实验内容及结果摘要如下:
1.本文报道了苯醚甲环唑在香蕉、荔枝和土壤中残留检测方法,建立了快速合理的气相色谱检测方法。其最小检出量为2.0×10~(-10)g,在香蕉、荔枝和土壤中的最低检出浓度均为0.02 mg/kg。结果表明,在0.02～2 mg/kg添加水平范围内,苯醚甲环唑在香蕉全果中的平均添加回收率在83.80%～96.01%之间,相对标准偏差在3.98%～6.11%之间;在香蕉土壤中的平均添加回收率在94.00%～97.27%之间,相对标准偏差在2.76%～5.32%之间;在0.02～2mg/kg添加水平范围内,在荔枝全果中的平均添加回收率在87.35%～93.38%之间,相对标准偏差在4.51%～9.88%之间;在荔枝土壤中的平均添加回收率在85.90%～92.81%之间,相对标准偏差在5.58%～9.94%之间。该方法的准确度,精密度和灵敏度均较高,符合农药残留分析的要求,具有简便,快速,成本低和可靠等优点。
2.本文对37%苯醚甲环唑水分散粒剂在香蕉、荔枝和土壤中的消解动态进行了研究分析。研究结果表明:苯醚甲环唑的消解动态均符合一级反应动力学模式,其结果具有较高的相关性。苯醚甲环唑在香蕉中的消解半衰期为:海口10.18d,南宁9.86d;在荔枝中消解半衰期为:海口11.27d,南宁8.61d。苯醚甲环唑在海口和南宁的土壤中消解半衰期从11.71d至22.5d不等。苯醚甲环唑在香蕉上消解动态方程为:海口C=2.9162e~(-0.0681t),r=0.9592;南宁C=2.7262e~(-0.0703t),r=0.9199。苯醚甲环唑在香蕉土壤上消解动态方程为:海口C=2.7737e~(-0.0308t),r=0.9592;南宁C=3.4468e~(-0.0454t),r=0.9917。苯醚甲环唑在荔枝上消解动态方程为:海口C=1.0613e~(-0.0615t),r=0.9892;南宁C=0.9992e~(-0.0805t),r=0.9877。苯醚甲环唑在荔枝土壤上消解动态方程为:海口C=0.2613e~(-0.0592t),r=0.9718。南宁C=0.4326e~(-0.0512t),r=0.9796
3.本文报道了苯醚甲环唑在香蕉、荔枝和土壤上的最终残留试验。结果表明,按推荐剂量在香蕉(123.3 mg/L)和荔枝(150 mg/L)中施用,建议最后一次施药与收获的安全间隔期分别暂定为15 d和7 d;苯醚甲环唑的残留量与施药浓度、施药次数呈正相关性,即残留量随着施药浓度、施药次数的增加而增加。
Difenoeonazole,which is a new compound of triazole fungicides,has been manufactured and developed by Syngenta.Pure sample is achromatous solid.Its melting point is 76℃.The compoud is not soluble in water,but it can be easily dissolve in a majority of organic solvent.Difenoeonazole not only has high efficiency and broad spectrum,but also is low toxicity to mammal.The contents and results are as follows:
1.This article discussed about the residue analysis means of difenoeonazole in banana,litchi and soil.The analysis method for determination of difenoeonazole by GC was established.The limit of quantification was 0.02mg/kg.The limit of detection was 2.0×10~(10)g in banana,litchi and soil.When concentration ranged from 0.02mg/kg to 2mg/kg of difenoeonazole,the average recovery in banana,litchi,soil sample of banana and soil sample of litchi was 83.80%～96.01%,87.35%～93.38%,94.00%～97.27%and 85.90%～92.80%,separately.At the same time,the relation standard deviation(RSD) was 3.98%～6.11%,4.51%～9.88%,2.76%～5.32%and 5.58%～9.94 %,respectively.The sensitivity and accuracy and precision of the means was accorded with the demand of the detection skill of pesticide residue.
2.The thesis was considered with the dissipation dynamics of difenoeonazole 37%water dispersible granule in banana,litchi and soil.Its result showed that the dissipation dynamics of fungicides was accoreded with C=C_0E~(-kt) in banana,litchi and soil.Moreover it had high correlation.The half-life of difenoeonazole in banana was 10.18d in HaiKou and 9.86d in NanNing.The half-life of difenoeonazole in litchi was 11.27d and 8.61d in HaiKou and NanNing,respectively.The half-life of difenoeonazole in soil ranged from 11.71d to 22.5d in HaiKou and NanNing.The results of dynamic residue of difenoeonazole in banana were accord with minus exponential equation:HaiKou C=2.9162e~(-0.0681t),r=0.9592,NanNing C=2.7262e~(-0.0703t), r=0.9199.The results of dynamic residue of difenoeonazole in litchi were accord with minus exponential equation:Halkou C=1.0613e~(-0.0615t),r=0.9892,Nanning C=0.9992e~(-0.0805t),r=0.9877.The results of dynamic residue of difenoeonazole in soil sample of banana were accord with minus exponential equation:Haikou C=2.7737e~(-0.0308t),r=0.9592,Nanning C=3.4468e~(-0.0454t),r=0.9917.The results of dynamic residue of difenoeonazole in soil sample of litchi were accord with minus exponential equation:Haikou C=0.2613e~(-0.0592t),r=0.9718.Nanning C=0.4326e~(-0.0512t), r=0.9796.
3.The paper reported the final residue experiment of difenoeonazole in banana,litchi and soil.The outcome indicated that it is recommended that the pre-harvest interval of difenoeonazole in banana is 15 days for the 123.3 mg/L treatment,and in litchi is 7 days for 225 mg/L treatment,respectively.The residue of difenoeonazole was directly related to the applying concentration and degree.Namely,the residue increased in pace of them.
1.本文报道了苯醚甲环唑在香蕉、荔枝和土壤中残留检测方法,建立了快速合理的气相色谱检测方法。其最小检出量为2.0×10~(-10)g,在香蕉、荔枝和土壤中的最低检出浓度均为0.02 mg/kg。结果表明,在0.02～2 mg/kg添加水平范围内,苯醚甲环唑在香蕉全果中的平均添加回收率在83.80%～96.01%之间,相对标准偏差在3.98%～6.11%之间;在香蕉土壤中的平均添加回收率在94.00%～97.27%之间,相对标准偏差在2.76%～5.32%之间;在0.02～2mg/kg添加水平范围内,在荔枝全果中的平均添加回收率在87.35%～93.38%之间,相对标准偏差在4.51%～9.88%之间;在荔枝土壤中的平均添加回收率在85.90%～92.81%之间,相对标准偏差在5.58%～9.94%之间。该方法的准确度,精密度和灵敏度均较高,符合农药残留分析的要求,具有简便,快速,成本低和可靠等优点。
2.本文对37%苯醚甲环唑水分散粒剂在香蕉、荔枝和土壤中的消解动态进行了研究分析。研究结果表明:苯醚甲环唑的消解动态均符合一级反应动力学模式,其结果具有较高的相关性。苯醚甲环唑在香蕉中的消解半衰期为:海口10.18d,南宁9.86d;在荔枝中消解半衰期为:海口11.27d,南宁8.61d。苯醚甲环唑在海口和南宁的土壤中消解半衰期从11.71d至22.5d不等。苯醚甲环唑在香蕉上消解动态方程为:海口C=2.9162e~(-0.0681t),r=0.9592;南宁C=2.7262e~(-0.0703t),r=0.9199。苯醚甲环唑在香蕉土壤上消解动态方程为:海口C=2.7737e~(-0.0308t),r=0.9592;南宁C=3.4468e~(-0.0454t),r=0.9917。苯醚甲环唑在荔枝上消解动态方程为:海口C=1.0613e~(-0.0615t),r=0.9892;南宁C=0.9992e~(-0.0805t),r=0.9877。苯醚甲环唑在荔枝土壤上消解动态方程为:海口C=0.2613e~(-0.0592t),r=0.9718。南宁C=0.4326e~(-0.0512t),r=0.9796
3.本文报道了苯醚甲环唑在香蕉、荔枝和土壤上的最终残留试验。结果表明,按推荐剂量在香蕉(123.3 mg/L)和荔枝(150 mg/L)中施用,建议最后一次施药与收获的安全间隔期分别暂定为15 d和7 d;苯醚甲环唑的残留量与施药浓度、施药次数呈正相关性,即残留量随着施药浓度、施药次数的增加而增加。
Difenoeonazole,which is a new compound of triazole fungicides,has been manufactured and developed by Syngenta.Pure sample is achromatous solid.Its melting point is 76℃.The compoud is not soluble in water,but it can be easily dissolve in a majority of organic solvent.Difenoeonazole not only has high efficiency and broad spectrum,but also is low toxicity to mammal.The contents and results are as follows:
1.This article discussed about the residue analysis means of difenoeonazole in banana,litchi and soil.The analysis method for determination of difenoeonazole by GC was established.The limit of quantification was 0.02mg/kg.The limit of detection was 2.0×10~(10)g in banana,litchi and soil.When concentration ranged from 0.02mg/kg to 2mg/kg of difenoeonazole,the average recovery in banana,litchi,soil sample of banana and soil sample of litchi was 83.80%～96.01%,87.35%～93.38%,94.00%～97.27%and 85.90%～92.80%,separately.At the same time,the relation standard deviation(RSD) was 3.98%～6.11%,4.51%～9.88%,2.76%～5.32%and 5.58%～9.94 %,respectively.The sensitivity and accuracy and precision of the means was accorded with the demand of the detection skill of pesticide residue.
2.The thesis was considered with the dissipation dynamics of difenoeonazole 37%water dispersible granule in banana,litchi and soil.Its result showed that the dissipation dynamics of fungicides was accoreded with C=C_0E~(-kt) in banana,litchi and soil.Moreover it had high correlation.The half-life of difenoeonazole in banana was 10.18d in HaiKou and 9.86d in NanNing.The half-life of difenoeonazole in litchi was 11.27d and 8.61d in HaiKou and NanNing,respectively.The half-life of difenoeonazole in soil ranged from 11.71d to 22.5d in HaiKou and NanNing.The results of dynamic residue of difenoeonazole in banana were accord with minus exponential equation:HaiKou C=2.9162e~(-0.0681t),r=0.9592,NanNing C=2.7262e~(-0.0703t), r=0.9199.The results of dynamic residue of difenoeonazole in litchi were accord with minus exponential equation:Halkou C=1.0613e~(-0.0615t),r=0.9892,Nanning C=0.9992e~(-0.0805t),r=0.9877.The results of dynamic residue of difenoeonazole in soil sample of banana were accord with minus exponential equation:Haikou C=2.7737e~(-0.0308t),r=0.9592,Nanning C=3.4468e~(-0.0454t),r=0.9917.The results of dynamic residue of difenoeonazole in soil sample of litchi were accord with minus exponential equation:Haikou C=0.2613e~(-0.0592t),r=0.9718.Nanning C=0.4326e~(-0.0512t), r=0.9796.
3.The paper reported the final residue experiment of difenoeonazole in banana,litchi and soil.The outcome indicated that it is recommended that the pre-harvest interval of difenoeonazole in banana is 15 days for the 123.3 mg/L treatment,and in litchi is 7 days for 225 mg/L treatment,respectively.The residue of difenoeonazole was directly related to the applying concentration and degree.Namely,the residue increased in pace of them.
引文
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