【作者】 唐光辉；

【导师】 张兴；

【作者基本信息】 西北农林科技大学 ， 农药学， 2007， 博士

【摘要】 树干注药是一种理想的环境相容性无公害施药技术。树干注药可防治多种林木害虫,尤其对于防治蛀干害虫意义重大。然而,目前国内外已开发出的专用杀虫注干药剂品种较少,直接制约了该技术的进一步应用,急需筛选开发更多安全有效的注干药剂来满足生产实践需要。本研究在大量田间药效试验基础上,筛选研制出了14%吡虫啉·敌敌畏注干液剂配方;对药剂在柳树体内的传导、分布、残留动态,对树体的安全性评价进行了研究;通过田间药效试验探讨了14%吡虫啉·敌敌畏注干液剂对光肩星天牛等林木害虫的防治效果。主要研究结果如下:1.通过对流动相配比、流速、色谱柱等条件进行优化,确定了吡虫啉及其具有生物活性代谢产物4,5-dehydroimidacloprid的HPLC分析条件:色谱柱Waters Spherisorb （ODS₂） C18, dp 5μ, 4.6 mm ID*25 cm;流动相为甲醇:水:冰乙酸（65:35:0.02,V/V）;流速0.8 mL/min;进样量20μL;检测波长270 nm。4,5-dehydroimidacloprid的保留时间为10.1 min,吡虫啉的保留时间为14.5 min。在柳树组织中进行添加回收试验,添加浓度为0.1～5 mg/kg,测得其回收率分别在82.54～93.47%,83.77～91.25%之间,符合残留分析要求。2.研究表明吡虫啉及其具有生物活性代谢产物4,5-dehydroimidacloprid在柳树体内具有良好的传导性能和较长的残留期。吡虫啉在不同组织中残留量差异较大,注药初期在各组织的残留量大小顺序为:叶片>小枝韧皮部>树干韧皮部>小枝木质部>树干木质部。随着吡虫啉在树体内的代谢降解,注药80 d后,其在各组织中趋于均匀分布。在检测期内吡虫啉活性代谢产物4,5-dehyroimid- acloprid在树体内各组织中均有分布,且含量呈波动变化。注药初期含量上升,随后随时间的延长含量整体上呈下降趋势。4,5-dehyroimidacloprid在不同组织中残留量有一定差异,注药初期在各组织的残留量大小顺序为:小枝韧皮部>树干韧皮部>叶片>小枝木质部>树干木质部。树干注药后较长时期内,吡虫啉及其活性代谢产物4,5-dehyroimidacloprid在害虫的防治中共同发挥作用。3.建立了利用超临界CO₂萃取气质联用（SFE-GC/MS）测定柳树中敌敌畏残留量的分析方法。通过此方法对柳树体内各组织中敌敌畏含量动态变化测定结果表明:敌敌畏在树体内具有良好的传导分布性能,可在柳树体内经木质部长距离传导,分布于树体各组织中。树干注药后不同时间,敌敌畏在柳树树冠内不同部位的传导、分布存在较大差异。药剂进入木质部后,首先沿注药孔上方输导组织随蒸腾流纵向传导,进入注药孔上方的叶片中。树干注药24 h各部位叶片内药剂含量差异最大,然后随时间的延长药剂在树体内逐渐降解,含量逐渐降低;各部位叶片内药剂含量差异也逐渐缩小,96 h在树冠各部位趋于均衡分布。树干注药初期叶片内药剂含量大于其他部位,随时间的延长,含量逐渐下降。注药7 d后,药剂在各部位趋于均匀分布。4.以垂柳为材料,研究了4种杀虫剂（吡虫啉、啶虫脒、吡虫啉·敌敌畏和敌畏·氧乐注干液剂）树干注药对其叶片内几项生理指标、保护酶活性及PPO、PPO同工酶变化的影响。结果表明:4种杀虫剂树干注药对柳树叶内叶绿素、可溶性蛋白、淀粉、可溶性总糖和纤维素含量均可产生显著的影响;4种杀虫剂树干注药后1个月内,均可不同程度提高SOD、PPO、PAL的活性,抑制POD活性;吡虫啉和啶虫脒树干注药均可引起垂柳叶片PPO活性上升,POD活性下降,导致PPO、PPO同工酶酶带呈现不同的变化规律。树干注药后药剂在一定时间内对树体一些生理生化代谢产生一定影响,但均未造成伤害。随着时间的延长,树体可通过自身的调节作用恢复正常的生理生化代谢水平。5.以14%吡虫啉·敌敌畏注干液剂为研究对象,开展了其制剂的研究。通过对制剂配方中溶剂、表面活性剂的筛选,研制出了溶剂A和N,N-二甲基甲酰胺组成的复合溶剂系统,采用OP-10为乳化剂,制剂的各项理化性质符合要求。该制剂配方在多数树种注干试验中,进入树体速度较快,对树体较为安全,田间防效理想。6.利用14%吡虫啉·敌敌畏注干液剂对光肩星天牛等多种林木害虫进行了田间树干注药防治试验。结果表明14%吡虫啉·敌敌畏注干液剂以1.0 mL/cm树干胸径的注药量对天牛幼虫防效可达90.7%,对大龄幼虫的防效优于对照药剂30%敌畏·氧乐注干液剂。在林间防治时,针对天牛不同危害程度,采用适当的注药技术,可获得理想的防治效果。14%吡虫啉·敌敌畏注干液剂和4.5%吡虫啉注干液剂注干后其田间持效期可达110 d以上。以0.4 mL/cm树干胸径的注药量春季注射,对一个生长周期内不同发生时间危害柳树枝梢、叶部害虫均有较好的防治效果。14%吡虫啉·敌敌畏注干液剂具有较广的杀虫谱,对多种树木害虫具有良好的防治效果。可见,14%吡虫啉·敌敌畏注干液剂在树体内具有良好的传导分布性能,对树体较为安全,对多种林木害虫具有良好的防治效果、且持效期长。具有良好的开发应用前景。更多还原

【Abstract】 Trunk injection is one of the biorational techniques used to control many pests, esp. boring pests. Presently only several special pesticides were produced domestically and overseas, so it is urgent to research and develop more safe and effective pesticides to meet the need of pest-control. Based on a large amount of field experiments, 14% imidacloprid + DDVP liquid formulation for trunk injection was researched; the transmission, distribution and residual effectiveness of this liquid formulation in willow and its safety assessment were discussed; control efficiency of this liquid formulation against Anoplophora glabripennis was tested based on field experiments. The results of the research and development show as fellows:1. A high performance liquid chromatography (HPLC) was established for determining of residues of imidacloprid and 4,5-dehydroimidacloprid in willow tissues. When the spiked concentration of imidacloprid and 4,5-dehydroimidacloprid in willow tissues was from 0.1-5 mg/kg respectively,imidacloprid and 4,5-dehydro- imidacloprid recoveries determined by HPLC were in the range of 82.54～93.47% and 83.77～91.25% respectively.2. The results showed that imidacloprid and 4,5-dehydroimidacloprid had excellent translocation ability in willow and extended residual effectiveness. The content of imidacloprid showed a great difference in different tissues. Tissues with imidacloprid content from high to low were leaves, twigs phloem, trunk phloem, twigs xylem and trunk xylem. As the imidacloprid declined, the content tended to be balanced in different parts at 80 days after the injection. During the detected period, the content of 4,5-dehydroimidacloprid could be detected in different parts of willow, the contents indicated wave change after the injection, At the first period, the contents rise, then drop. The content of 4,5-dehydroimidacloprid indicated a great difference in different tissues: Tissues with 4,5-dehydroimidacloprid content from high to low were twigs phloem, trunk phloem, leaves, twigs xylem and trunk xylem. Imidacloprid as well as 4,5-dehydroimidacloprid could control pests effectively at the mean time during a long period after the injection.3. The insecticide dichlorvos was extracted from willow tissue by supercritical fluid extraction (SFE). The extraction conditions were at 34.48 MPa and 40℃with 1mL/min supercritical carbon dioxide modified with methanol for 20 min after 20-mintue static extraction. The extracts were collected in 5 mL of acetone. Gas chromatography/mass spectrometry was used to examine the extracts. The results showed that the transmission and the distribution of dichlorvos were different in different parts of willow crown after the injection. Following the transpiration entered into the stem translation tissue, the pesticide was transmitted firstly into the upper leaves over the injection hole. The most difference of pesticide content maximum appeared at 24 h after the injection in different parts of crown; then the content declined gradually. The content tended to be balanced in different parts of crown at 96 h after the injection. The content in leaves was higher than that in other tissues at initial stages after the injection and tended to be balanced after 7 d. Dichlorvos can be transmitted long distance through stem and distributed in different tissues after the injection.4. The effects of 4 liquid formulations (imidacolprid, acetamiprid, imidacloprid + DDVP and DDVP + omethoate) on some physiological indices in weeping willow (Salix babylonica Linn) leaves by trunk injection were reported. The result showed that all of the 4 pesticides caused the decreasing of the amount of total soluble sugar and cellulose and caused the decreasing of the amount of chlorophyll, soluble protein and starch in willow leaves in a short period after treatments. The result showed the wave change of SOD appeared after the injection. At the first period, the activity of SOD showed the tendency of rising, dropping, and rising again. The 4 pesticides could improve the activities of PPO and PAL, and reduce the activity of POD. The content of dissociate proline had also descended after treatment by the 4 pesticides through trunk injection. The two pesticides imidacolprid and acetamiprid affected activities of PPO and POD as well as spectrums and activities of their isozymes after the injection. While the activity of PPO was increased, the activity of POD was decreased. The changes of spectrums and activities of their isozymes caused by the two pesticides were different. The pesticide could affect some physiological characters of willow after the injection, but willow could self-adjust and resume the normal physiological level as time went along. The results showed that the liquid formulation is safe to trees.5. 14% imidacloprid + DDVP liquid formulation for trunk injection was studied. A compound liquid formulation composed of solvent A and N,N-Dimethvlformamide was researched and developed with OP-10 emulsification, the physiological quality of which accorded with the criterion. Tested in trunk injection experiments on many different trees, this formulation showed the characters of fast transmission, safety to trees, and better control efficiency.6. The field bioassay of 14% Imidacloprid + DDVP liquid formulation for trunk injection was conducted against Anoplophora glabripennis. The control efficiency against large-big larvae of the two pests with the formulation of 14%Imidacloprid+DDVP reached 90.7% by using a dose of 1.0ml for each centimeters trunk diameter, which was better than the control pesticide formulation of 30%DDVP + Omethoate. Three effective controlling strategies were carried out by the field bioassay according to different damage degrees.14% Imidacloprid + DDVP and 4.5% Imidacloprid exhibited high efficiency and provided extended residual effectiveness, up to 110 days under optimum conditions. After trunk injection by the dosage of 0.4 mL/cm trunk diameter in spring, the pesticides can control pest occurred in different time during one growth periodicity. Pest control trails showed that 14% Imidacloprid + DDVP liquid formulation can suppress the population of many pests when it was injected into the stem of trees to control different pests, e.g. Anoplophora glabripennis, Brontispa longissima, Plagildera versiclolora, Aphis farinosa, Holotrichia oblita, Psylla wilieti, Aphis robiniae, Stephanitis nashi, Lycorma delicatula, Panonychus citri, etc.The above indicated that 14% imidacloprid + DDVP liquid formulation for trunk injection had the ability of excellent translocation and distribution in trees, better and long-term control efficiency on many pests, and was safe to trees. It would have good development and application prospect.更多还原