【作者】 谭辉华；

【导师】 卢植新； 杨绍龙；

【作者基本信息】 广西大学 ， 农业昆虫与害虫防治， 2004， 硕士

【摘要】 硝虫硫磷是我国四川省化学工业研究设计院创制的有机磷类杀虫杀螨剂，田间试验表明其对水稻、棉花、柑桔、蔬菜等作物的主要害虫具较好的防治效果，尤对柑桔矢尖蚧的防治效果更佳。目前硝虫硫磷在我国已获得临时登记，但有关硝虫硫磷残留分析方法及使用后的残留动态规律国内外均未见公开报道。因而，研究硝虫硫磷的残留分析方法及其在柑桔上使用后的残留动态规律，为制定该药的合理使用准则和评价其使用后的安全性提供科学依据，具有重要理论和实践意义。 本文首次报道了硝虫硫磷在柑桔和土壤中的残留分析方法。样品以丙酮提取，二氯甲烷萃取，中性氧化铝加酸洗活性炭混合柱净化，采用DB-17（15m×0.540mm×1.00μm）毛细管柱，气相色谱法FTD检测定量，最小检知量为1.4×10^-10g。当添加浓度为0.05～0.5mg·kg^-1时，硝虫硫磷在桔肉、桔皮和土壤中的回收率分别为88.37％～93.17％、87.07％～94.07％和86.47％～93.30％，变异系数为1.65％～4.14％。 在广西南宁和湖南衡阳两地连续两年进行了硝虫硫磷消解动态试验。结果表明：在1000mg（a．i．）／kg的施药条件下，硝虫硫磷在柑桔和土壤中消解比较迅速，消解半衰期分别为13～15天和10～16天， 广西大学硕士学位论文硝虫硫磷在柑桔（果皮）和土壤中的消解动态规律均符合一级动力学消解模式。 硝虫硫磷在广西南宁、湖南衡阳两年两地的最终残留试验结果表明:施药浓度300一600倍，2一3次药，饭次间隔巧天，施药后采收间隔期为14、21、28天，其结果是，在果肉中的残留量广西点为LOD一0.0109m酬kg，湖南点为LOD⁰.0307mg/kg;果皮的残留量广西点为0.7415²..086lmg/kg，湖南点为0.2080一l.3698mg/kg;全果的残留量广西点为0.0777^o.46oZm酬kg，湖南点为0.0429⁰.2959m创kg;在土壤中最终残留量广西点为0.2350¹.2103m酬电，湖南点为0.0627一0.7307m酬kg。在试验条件下，农药的最终残留量与施药的浓度、次数呈正相关性，与采收间隔期呈负相关性。 硝虫硫磷为我国新创制的新农药，国家尚未制定在柑桔上的MRL值以及安全合理使用准则，国际上也无相关的MRL值可参照，本试验残留数据为政府职能部门制定其在柑桔的M丑L值和农药合理使用准则以及进行安全性评价提供科学依据。更多还原

【Abstract】 Xiaochongliulin, invented by Sichuan Academy of Chemical Industry Research and Design, is an organophosphorous insecticide and acaricide, which is effectively against a wide range of insects, especially the citrus arrowhead scale. At present, the pesticide has been temporarily registered to control citrus arrowhead scale in China. However, the residual determination methods for this pesticide and the data of residues on orange and in soil after application have not yet been reported. Therefore, the studies are of great significance on its residual determination and degradation on orange and in soil.A method was developed for determination xiaochongliulin residues on orange and in soil by capillary gas chromatography. The samples were extracted with acetone and the extracts were partitioned with dichloromethane. After cleanup on a mixture column of aluminum oxide (neutral) and activated charcoal, the residues were analyzed using gas chromatography equipped with FTD. The DB-17 column,15m 0.540mm i.d., was used for chromatographic separation of this pesticide. The Limit of detection of this method was 1.4 10-10g. Average recoveries of xiaochongliulin from fortified orange pulp, peel and soil samples at levels of 0.05~0.5mg kg-1 were in the range from 88.37% to 93.17%, from 87.07% to 94.07% and from 86.47% to 93.30% respectively, with coefficient of variation hi the range from 1.65% to 4.14%.Residue trials of 30% xiaochongliulin EC were conducted in Guangxi and Hunan Province during 2002-2003. The results indicated that with application dose of 1000mg(a.i.)/kg the degradation of xiaochongliulin was moderate in soil and on orange peel with the decline half-lives of ranging from 10.33 to 15.20 days and from 13.58 to 14.69 days, respectively. The degradation kinetics of this pesticide in soil andon orange followed the first-degree reaction pattern.The results also indicated that the residues of this pesticide on orange pulp, on orange peel, on orange and in soil ranged from LOD to 0.0109mg/kg, from 0.7418 to 2.0861mg/kg, from 0.0777 to 0.4602mg/kg and from 0.2350 to 1.2103mg/kg respectively in Guangxi Province, and ranged from LOD to 0.0307mg/kg, from 0.2080 to 1.3698mg/kg, from 0.0429 to 0.2959mg/kg, and from 0.0627 to 0.7307mg/kg respectively in Hunan Province, when 30% xiaochongliulin was sprayed two or three tunes with the dosage of 500mg(a.i.)/kg and 1000mg(a.i.)/kg and an interval of IS days during the growing season of orange trees, and the last application was carried out 14,21 and 28d before the harvest. Under field trial conditions, there were positive relation between residue and amount as well as tunes sprayed for, and negative relation between residue and the days from last application to harvest.Xiaochongliulin was a new pesticide invented in our country and there was no reference MRL at present in FAO/WHO and other countries. The resulting residue data then were necessary for government to establish MRL and guideline for safety application of this pesticide on orange, and to conduct risk assessment of this pesticide.更多还原