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新型拟除虫菊酯化合物HNPC-A9908的残留分析方法及残留动态研究

Studies on the Residue Analysis Method and Residue Dynamics of HNPC-A9908 Which is a New Compound of Pyrethroids

【作者】 吴鸿琳

【导师】 王国平; 廖晓兰;

【作者基本信息】 湖南农业大学 , 农药学, 2003, 硕士

【摘要】 HNPC-A9908是近几年由湖南化工研究院研制开发的,一种结构全新的具有颇好杀虫活性的非羧酸酯肟醚类拟除虫菊酯化合物。纯品为无色固体,熔点27.3-27.7℃,不溶于水易溶于大部分有机溶剂。不仅具有拟除虫菊酯高效、广谱、快速击倒的活性特点,而且对哺乳动物低毒,且合成也比较简单。10%HNPC-A9908水乳剂是一种良好的防治十字花科蔬菜菜青虫药剂,对作物安全无药害。为了开发应用并即将申请登记,本论文采用高效液相色谱紫外检测器检测法,对该化合物在其登记代表作物白菜和土壤中的残留量进行了初步研究。其试验内容及结果摘要如下: 1 本文报道了该化合物母体在白菜及土壤中的残留分析方法。色谱条件为: 色谱仪:LC-10AT 色谱柱:Kromasil C18柱,250×4.6mm(id),5μm 检测器:紫外吸收检测器 流速:1.0mL/min 流动相:甲醇:水=9:1(v/v) 检测波长:220nm 柱温:35℃ 进样量:20μL 保留时间:14.50min 外标峰面积法定量。方法最小检出量为6.5×10-10g,最低检出浓度为0.0162mg/kg。HNPC-A9908的浓度在0.1294~6.470mg/L范围内,线性关系良好。以0.0647mg/kg、0.6470mg/kg、1.2940mg/kg三个浓度进行空白样品添加试验,白菜的平均回收率为88.15%~99.86%,变异系数为0.84%~10.15%;土壤的平均回收率为83.45%~93.07%,变异系数为5.82%~6.57%。该方法的灵敏度、准确度、精密度均符合农药残留技术测定要求。 2 对10%HNPC-A9908水乳剂在白菜及土壤中的降解动态进行了初步研究。结果表明,HNPC-A9908在白菜及土壤中的残留消解动态符合一级动力学反应模式,其结果具有较高的相关性。在田间自然条件下,该化合物在白菜上的半衰期为2.66天,在冬季无植被的土壤中降解半衰期为6.94天。 3 本论文报道了10%HNPC-A9908水乳剂在白菜上的最终残留试验。结果表明,白菜及土壤中的HNPC-A9908残留量与施药浓度、施药次数呈正相关,即残留量随着施药浓量、施药次数的增加而增加。同时,10%HNPC-A9908水乳剂在作物白菜上使用后残留量较低,对白菜的食用较安全,并且对土壤污染可能性极小。

【Abstract】 HNPC-A9908, which is a new compound of non-ester oxime aether pyrethroids and possesses characteristic of considerably fine insecticide , has been manufactured and developed by Hunan Chemical Research Institute in recent years. Pure sample is achromatous solid. Its melting point is 27.3-27.7 C. The compound is not soluble for water, but it is easily soluble for a majority of organic solvent. HNPC-A9908 not only has high efficiency and low toxicity and broad spectrum, but also is somewhat poisonous to mammal. Moreover its synthesis is relatively simple. 10%HNPC-A9908 emulsion is a kind of fine pesticide that prevents and cures cabbage caterpillar in cruciferae vegetables. In addition, it does no harm to them. In order to develop and apply for register, the paper was researched initially by HPLC with UV on the residue of the compound in cabbage being its register representative crop and soil. The contents and results are as follows:1 This article discussed about the residue analysis means of HNPC-A9908 in cabbage and soil. HPLC condition is next:Chromatography: LC-10ATColumn: Kromasil C18 Column(250+4.6mm(id),5m)The detector: UVFlowing velocity: 1.1mL/minMobile phase: carbinol:water(9:1,v/v)Wavelength: 220nmColumn temperature: 35 CAmount: 20LRettime: 14.50minExternal standard area method was to quantify. Minimal determination quantity (MDQ) was 6.5+10-10g, while minimal determination concentration (MDC) in cabbage and soil was 0.0162mg/kg without exception. When concentration ofHNPC-A9908 ranged from 0.1294mg/L to 6.470mg/L, it had fine linear relation, when the addictive amount was 0.0647mg/kg,0.6470mg/kg,1.2940mg/kg, the average recovery of HNPC-A9908 in cabbage and soil was 88.15%-99.86% and 83.45%-93.07%, separately. At the same time, the coefficient of variation of this method was 0.84%-10.15%,5.82%-6.57% respectively. Therefore, The sensitivity and accuracy and precision of the means accorded with demand of the detection skill of pesticide residue.2 The thesis considered tentatively about the dissipation dynamics of 10%HNPC-A9908 emulsion in cabbage and soil. Its result showed that the dissipation dynamics of pesticide accorded with C = C0E-kt in cabbage as well as in soil. Moreover it had high correlation. Under field environment, the half-lives was 2.66 days and 6.94 days, separately.3 The paper reported the final residue experiment of HNPC-A9908 in cabbage and soil. The outcome indicated that the residue of HNPC-A9908 was directly related to the applying concentration and degree. Namely, the residue increased in pace of them. After HNPC-A9908 was used in cabbage, its residue was rather low. For this reason, the edible cabbage was quite safe. Besides, the possibility of pollution of soil was pindling.

  • 【分类号】S481.8
  • 【被引频次】3
  • 【下载频次】113
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