CN112753703A - 一种用于松材线虫病防治的速效打孔纳米乳剂及其应用 - Google Patents

一种用于松材线虫病防治的速效打孔纳米乳剂及其应用 Download PDF

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CN112753703A
CN112753703A CN202110073637.3A CN202110073637A CN112753703A CN 112753703 A CN112753703 A CN 112753703A CN 202110073637 A CN202110073637 A CN 202110073637A CN 112753703 A CN112753703 A CN 112753703A
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吴学民
徐勇
郭鑫宇
商洪溢
于海英
张秋梅
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Abstract

本发明公开了一种用于松材线虫病防治的速效打孔纳米乳剂及其应用。所述速效打孔纳米乳剂的质量百分比组成如下：杀线虫药剂0.5～10％；杀天牛药剂0.5～10％；植物生长调节剂0.1～5％；乳化剂5～15％；助溶剂0.5～5％；渗透传导剂0.2～2％；水10～15％；余量的溶剂。本发明选择纳米乳液进行松树树干打孔，打孔季节在松树树脂旺盛季节(5月‑7月)，纳米乳液注入后与树体流胶相结合，通过纳米尺寸乳液、亲脂载药体系以及渗透传导剂将有效成分迅速随着树胶传导至树体全身，能够快速的阻止松材线虫从树冠向下侵染，并且不被流胶旺季的松脂所堵塞。本发明含有杀线虫剂、杀天牛剂以及植物生长调节剂三种有效成分，对松材线虫的杀灭、天牛幼虫的杀灭以及松树健康情况的恢复有着十分明显的效果。

Description

一种用于松材线虫病防治的速效打孔纳米乳剂及其应用
技术领域
本发明涉及一种用于松材线虫病防治的速效打孔纳米乳剂及其应用，属于农药技术领域。
背景技术
松材线虫病被称为松树“癌症”，属于国家重大生态灾害，是全球森林生态系统 中最具危险性、毁灭性的病害，具有极强的扩散性和破坏性。打孔注药技术于20世纪 初形成，在美国、法国、罗马尼亚、韩国用乙酰甲胺磷、乐果、磷胺等药剂进行树干 注药，防治球果花蝇、卷叶蛾、黑松蚧虫、瘿蚊,均取得了较好的防治效果。日本研 制的第三代防治松材线虫注入剂已取得很大的进展，如获得成功，将促进松材线虫病 的防治。我国自20世纪60年代开始，即有人利用“1059、3911”等内吸性杀虫剂， 采取树干涂环和干基打孔防治林果害虫，但效果不稳定。山东省自20世纪60年代。 时连同等人利用氟乙酰胺涂环、打孔防治日本松干蚧,其中打孔效果不甚理想；80年 代开始，刘建新、李洪敬等人利用氧化乐果、久效磷等内吸农药，于树干基部打孔注 药防治泡桐大袋蛾和杨树食叶害虫获得成功。
目前，对松材线虫病的防治十分依赖于对其媒介昆虫松墨天牛的间接防治，防治手段主要有化学防治、诱杀防治、生物防治和疫木除治，而对松材线虫病的直接防治 目前只有打孔注药一种方式。因此打孔注药是现阶段直接杀死松材线虫的有效手段。 然而对于松墨天牛的防治是阻止松材线虫的扩散，而对松材线虫的杀灭是阻止松材线 虫的侵染，因此对于松材线虫的防治有着极其重要的意义。
打孔注药技术在松材线虫病防治中的应用目前有很多难点，如松树表皮厚，木质部致密，药液难以渗透；并且松科植物油脂分泌旺盛，有效成分能否进入树体内以及 在树体内部的渗透和传导是否高效直接影响了对松材线虫病的防治效果。
目前的防治松材线虫病害打孔药剂所选溶剂均为DMF、DMSO等极性溶剂，乳 化性能很好，但是这种载药体系难以亲和松脂，并且极易产生药害。极性溶剂体系的 打孔药剂均需要在冬季和初春进行施药，防止夏季松脂流动旺盛将药剂瓶堵塞，然而 冬季和初春树内松脂流动缓慢也会导致药剂在树体内难以向上传导，造成了药剂的流 失。并且冬季和初春难以辨别当年发生严重的区域和目标树，该时期打药容易造成目 标选择的错误，从而造成药剂的浪费。因此进行注药的时期、载药体系的选择以及渗 透和传导能力十分重要。
发明内容
本发明的目的是提供一种用于松材线虫病防治的新型速效打孔纳米乳剂，所述打孔纳米乳剂具有纳米尺度的药液粒径，在渗透性能和传导性能方面表现优异，载药体 系与松脂兼容性高，能够迅速传导至松树全身，对松材线虫病有着快速的防治效果并 且兼具杀天牛幼虫和促进松树生长、增绿、恢复的效果。
本发明所提供的用于松材线虫病防治的速效打孔纳米乳剂，其质量百分比组成如下：
Figure BDA0002906793100000021
所述速效打孔纳米乳剂的组成优选为：
Figure BDA0002906793100000022
具体地，所述杀线虫药剂可为甲氨基阿维菌素苯甲酸盐、氟吡菌酰胺或阿维菌素，优选甲氨基阿维菌素苯甲酸盐；
所述杀线虫药剂的质量百分含量优选为3～9％、3～7％、3～5％、3％、5％、7％或9％。
具体地，所述杀天牛药剂可为吡虫啉、噻虫啉、噻虫胺或噻虫嗪，优选噻虫啉；
所述杀天牛药剂的质量百分含量优选为3～9％、3～8％、3～7％、3～5％、3％、5％、 7％、8％或9％。
具体地，所述植物生长调节剂可为芸苔素内酯、萘乙酸钠或赤霉素，优选芸苔素内酯；
所述植物生长调节剂的质量百分含量优选为0.1～0.5％，如0.1％或0.5％。
具体地，所述乳化剂可为脂肪醇聚氧乙烯醚、苯氧基苯酚聚氧乙烯醚或苯氧乙烯基苯酚聚氧乙烯醚，分子量为800～1200；
所述乳化剂的质量百分含量优选为7～12％或7～10％，如7％、8％、10％或12％。
具体地，所述助溶剂可为碳原子数为1～4的醇；
所述助溶剂的质量百分含量优选为2％。
具体地，所述渗透传导剂可为油基改性聚醚类，具体可为脂肪醇聚氧乙烯醚(如渗透剂JFC)、硅氧烷聚氧乙烯醚(如Silwet-625)；
所述渗透传导剂的质量百分含量优选为1～2％，如1％或2％。
具体地，所述溶剂可为松脂基植物油。
本发明选择纳米乳液进行松树树干打孔，打孔季节在松树树脂旺盛季节(同样也是媒介昆虫的羽化期内，5月-7月)，纳米乳液注入后与树体流胶相结合，通过纳米尺 寸乳液、亲脂载药体系以及渗透传导剂将有效成分迅速随着树胶传导至树体全身，能 够快速的阻止松材线虫从树冠向下侵染，并且不被流胶旺季的松脂所堵塞。本发明含 有杀线虫剂、杀天牛剂以及植物生长调节剂三种有效成分，对松材线虫的杀灭、天牛 幼虫的杀灭以及松树健康情况的恢复有着十分明显的效果。
本发明具有如下有益效果：
1)使用纳米乳液，纳米尺寸的液滴粒径传导速度更快，对松材线虫病的防治具有快速的防治效果。
2)使用渗透传导剂，在树体内部具有良好的渗透传导能力，能够随着树胶传导至树体全身。
3)使用对松脂高亲和力的松脂基植物油作为载药体系，具有能与松脂相容，不堵塞的优点。
4)在媒介昆虫羽化期内进行注药，能够有效地辨别需要进行防治的目标树。
5)制备方法简便、环保，易于大量生产。
具体实施方式
下述实施例中所使用的实验方法如无特殊说明，均为常规方法。
下述实施例中所用的材料、试剂等，如无特殊说明，均可从商业途径得到。
实施例1、新型速效打孔纳米乳剂
质量百分比组成如下：
甲氨基阿维菌素苯甲酸盐 5％；
噻虫啉 5％；
芸苔素内酯 0.1％；
苯氧基苯酚聚氧乙烯醚(分子量1200左右) 8％；
正丁醇 2％；
硅氧烷聚氧乙烯醚(Silwet-625) 1％；
水 10％；
松脂基植物油 补足100％。
实施例2、新型速效打孔纳米乳剂
质量百分比组成如下：
甲氨基阿维菌素苯甲酸盐 7％；
噻虫啉 5％；
芸苔素内酯 0.1％；
苯氧基苯酚聚氧乙烯醚(分子量1200左右) 8％；
正丁醇 2％；
硅氧烷聚氧乙烯醚(Silwet-625) 2％；
水 12％；
松脂基植物油 补足100％。
实施例3、新型速效打孔纳米乳剂
质量百分比组成如下：
甲氨基阿维菌素苯甲酸盐 7％；
噻虫啉 7％；
芸苔素内酯 0.5％；
脂肪醇聚氧乙烯醚(分子量800左右) 10％；
正丁醇 2％；
硅氧烷聚氧乙烯醚(Silwet-625) 2％；
水 10％；
松脂基植物油 补足100％。
实施例4、新型速效打孔纳米乳剂
质量百分比组成如下：
甲氨基阿维菌素苯甲酸盐 5％；
噻虫啉 8％；
芸苔素内酯 0.1％；
苯氧基苯酚聚氧乙烯醚(分子量1200左右) 8％；
甲醇 2％；
硅氧烷聚氧乙烯醚(Silwet-625) 2％；
水 10％；
松脂基植物油 补足100％。
实施例5、新型速效打孔纳米乳剂
质量百分比组成如下：
甲氨基阿维菌素苯甲酸盐 3％；
噻虫啉 3％；
芸苔素内酯 0.1％；
苯氧基苯酚聚氧乙烯醚(分子量1200左右) 7％； 正丁醇 2％；
硅氧烷聚氧乙烯醚(Silwet-625) 1％；
水 10％；
松脂基植物油 补足100％。
实施例6、新型速效打孔纳米乳剂
质量百分比组成如下：
甲氨基阿维菌素苯甲酸盐 9％；
噻虫啉 9％；
芸苔素内酯 0.1％；
脂肪醇聚氧乙烯醚(分子量800左右) 12％；
甲醇 2％；
硅氧烷聚氧乙烯醚(Silwet-625) 2％；
水 10％；
松脂基植物油 补足100％。
实施例7、新型速效打孔纳米乳剂
质量百分比组成如下：
甲氨基阿维菌素苯甲酸盐 10％；
噻虫啉 10％；
芸苔素内酯 0.1％；
脂肪醇聚氧乙烯醚(分子量1000左右) 12％；
甲醇 2％；
脂肪醇聚氧乙烯醚(渗透剂JFC) 2％；
水 10％；
松脂基植物油 补足100％。
实施例8、新型速效打孔纳米乳剂
质量百分比组成如下：
甲氨基阿维菌素苯甲酸盐 10％；
噻虫啉 5％；
芸苔素内酯 0.1％；
苯氧基苯酚聚氧乙烯醚(分子量1000左右) 10％；
正丁醇 2％；
脂肪醇聚氧乙烯醚(渗透剂JFC) 1％；
水 10％；
松脂基植物油 补足100％。
实施例9、新型速效打孔纳米乳剂的传导性能评价
实施例1-8接受在树体流胶旺盛时期(5-7月份)对松树进行打孔注干试验，15 天后将松树伐倒分段取样检测，使用HPLC测定了松树不同部位中甲氨基阿维菌素苯 甲酸盐的含量，使用市售10％甲氨基阿维菌素苯甲酸盐·吡虫啉可溶液剂进行对比。结 果如表1所示。
表1新型速效打孔纳米乳剂传导性能评价结果(15天)
Figure BDA0002906793100000061
Figure BDA0002906793100000071
从传导性能结果可以看出，各实施例药剂均能迅速、有效地传导至松树上部，而市售产品基本全部堵塞，无法传导。
实施例10、新型速效打孔纳米乳剂的储存稳定性
实施例1-8接受在54±2℃条件下为期14天的稳定性测试，用高效液相色谱-紫外检测器(HPLC-UVD)测定了有效成分的含量变化，结果如表2所示。用动态光散射 (DLS)分析测试前后的纳米乳液粒径变化，检测结果如表3所示。
表2新型速效打孔纳米乳剂有效成分含量分析(14天)
Figure BDA0002906793100000072
Figure BDA0002906793100000081
表3新型速效打孔纳米乳剂粒径稳定性分析(14天)
序号 贮前粒径D<sub>50</sub>(nm) 贮后粒径D<sub>50</sub>(nm)
实施例1 18.25 18.66
实施例2 17.39 18.01
实施例3 20.03 20.00
实施例4 20.51 20.55
实施例5 22.63 23.17
实施例6 25.83 25.87
实施例7 25.13 25.32
实施例8 26.90 27.14
从贮存稳定性结果可以看出，各实施例纳米乳液有效成分含量、粒径均无明显变化，稳定性良好。
实施例11、新型速效打孔纳米乳剂对松材线虫病的防治效果
试验药剂：实施例1新型速效打孔纳米乳剂。
对照药剂：10％甲氨基阿维菌素苯甲酸盐·吡虫啉可溶液剂。
试验对象：黑松。
试验方法：在媒介天牛羽化期内(5-8月)，使用本发明药剂对50棵松材线虫病 疫区内黑松进行打孔注药，并且对照药剂可溶液剂使用同种方法进行打孔注药试验， 试验树50棵。设置不注药组作为空白对照，试验树50棵。试验时间1年，监测试验 组、对照药剂和空白对照的松材线虫病发病情况。发病率计算方法如下：
Figure BDA0002906793100000082
A：当年发病树数量；
S：该组试验树总数。
试验结果：见表4，与空白对照相比新型速效打孔纳米乳剂对松材线虫病有很 好的防治效果，而对照药剂由于被松脂堵塞，难以传导，对松材线虫病防治几乎无 效果。
表4新型速效打孔纳米乳剂对松材线虫病防治效果
Figure BDA0002906793100000091
实施例12、新型速效打孔纳米乳剂对天牛的防治效果
试验药剂：实施例4新型速效打孔纳米乳剂。
对照药剂：10％甲氨基阿维菌素苯甲酸盐·吡虫啉可溶液剂。
试验对象：黑松。
试验方法：使用本发明药剂对5棵松材线虫病疫区内已经感病的黑松进行打孔 注药，并且对照药剂2可溶液剂使用常规打孔方法进行注药，试验树的选择与试验 组相同，数量5棵。设置不注药组作为空白对照，试验树的选择与试验组相同，数 量5棵。注药15天后将所有组别树伐倒劈开，统计树内天牛幼虫死亡情况。松墨 天牛死亡率计算方法如下：
Figure BDA0002906793100000092
D：松墨天牛幼虫死亡数；
M：该组共发现松墨天牛幼虫总数。
试验结果：见表5，与空白对照相比本发明的新型速效打孔纳米乳剂对松树内 部松墨天牛迅速杀灭效果显著，防效达90％以上。而对照药剂由于被松脂所堵塞， 传导效率低，防效较差。
表5新型速效打孔纳米乳剂对松墨天牛防治效果
Figure BDA0002906793100000093

Claims (9)

1.一种用于松材线虫病防治的速效打孔纳米乳剂，其质量百分比组成如下：
Figure FDA0002906793090000011
余量的溶剂。
2.根据权利要求1所述的速效打孔纳米乳剂，其特征在于：所述杀线虫药剂为甲氨基阿维菌素苯甲酸盐、氟吡菌酰胺或阿维菌素。
3.根据权利要求1或2所述的速效打孔纳米乳剂，其特征在于：所述杀天牛药剂为吡虫啉、噻虫啉、噻虫胺或噻虫嗪。
4.根据权利要求1-3中任一项所述的速效打孔纳米乳剂，其特征在于：所述植物生长调节剂为芸苔素内酯、萘乙酸钠或赤霉素；
所述植物生长调节剂的质量百分含量为0.1～0.5％。
5.根据权利要求1-4中任一项所述的速效打孔纳米乳剂，其特征在于：所述乳化剂为脂肪醇聚氧乙烯醚、苯氧基苯酚聚氧乙烯醚或苯氧乙烯基苯酚聚氧乙烯醚；
所述乳化剂的质量百分含量为7～15％。
6.根据权利要求1-5中任一项所述的速效打孔纳米乳剂，其特征在于：所述助溶剂为碳原子数为1～4的醇；
所述助溶剂的质量百分含量为2～5％。
7.根据权利要求1-6中任一项所述的速效打孔纳米乳剂，其特征在于：所述渗透传导剂为油基改性聚醚类；
所述渗透传导剂的质量百分含量为1～2％。
8.根据权利要求1-7中任一项所述的速效打孔纳米乳剂，其特征在于：所述溶剂为松脂基植物油。
9.权利要求书1-8中任一项所述速效打孔纳米乳剂在防治松材线虫病和/或树内松墨天牛幼虫中的应用；
在5～7月进行注药。
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