CN108184908A - 一种植物源自乳化纳米杀虫剂及其制备方法和应用 - Google Patents
一种植物源自乳化纳米杀虫剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种植物源自乳化纳米杀虫剂及其制备方法和应用，成分包括银杏外种皮乙醇粗提物2％～5％；溶剂乙醇与银杏外种皮粗提物质量比为1:1；表面活性剂含量为2.5％～3％；助表面活性剂含量为2％～2.5％。其应用对象为害虫，包括：鳞翅目小菜蛾、粘虫、棉铃虫等。在本发明的优点在于：采用天然表面活性剂，将无水的自乳化纳米乳液引入农药杀虫剂中，能有效提高天然产物源农药的生物活性，有利于提高产品质量和产量，同时降低生产成本，对其防效均高于90％，对蚜虫防效亦高于90％。
Description
技术领域
本发明涉及农药技术领域，特别涉及一种植物源自乳化纳米杀虫剂，还涉及该杀虫剂的制备方法和应用。
背景技术
随着时代的发展，人们的环境保护观念和食品安全意识越来越强，“环保、高效、安全、经济”成为农药研发的主要目标。大多数具有生物活性的农药原药都不溶或微溶于水，因而需要加工成农药剂型才能更方便的使用并更好的发挥其生物活性。过去农药生产中常用的剂型是乳油和粉剂。乳油中含有大量的有机溶剂，如甲醇、甲苯和二甲苯等，对环境污染严重。而粉剂的制备和使用过程中，容易发生漂移，造成大气污染。因此，开发环保、安全、水基性的制剂成为农药剂型开发的研究热点。目前，水基性的农药剂型主要有微乳剂、悬浮剂、水剂、水乳剂、悬乳剂和微胶囊悬浮剂等。微乳剂制备简单，形成液滴的直径小，表面张力低，对叶面润湿性和渗透性好，但是制备需要大量表面活性剂，有效成分含量低。与微乳剂相比，水乳剂表面活性剂含量低，但是液滴粒径变大，开发周期长，制备过程常常需要高剪切和高压均质等专用设备输入能量。悬浮剂可以与水以任意比例混合，使用方便，不受稀释介质的影响，环境安全。但是，悬浮剂的制备常用湿法超微粉碎，设备成本高。
纳米乳液作为载药系统，能够提高难溶性药物的溶解度和生物利用度；对于一些不稳定的药物，能够提高其稳定性；纳米乳液包封的药物可在生物体内缓慢释放并具有靶向作用；生物相容性好，能够有效减少药物引起的不良反应和副作用；粒径小，动力学稳定，贮藏稳定性好。但是有关纳米乳液作为农药制剂防治农业害虫，目前在国内研究的较少。Wang等选择环境友好且刺激性小的脂肪酸甲酯为溶剂，采用低能乳化法制备了高效氯氰菊酯纳米乳载药体系。与市售微乳剂相比，纳米乳液载药体系对氯氰菊酯的增溶能力较强，稀释24h后无晶体析出。Liu等混合离子型和非离子型表面活性剂，采用高能乳化法制备了稳定性好，质量标准符合FAO(联合国粮食及农业组织)的O/W型联苯菊酯纳米乳液。Song等采用自乳化法制备三唑磷纳米乳液，能够有效提高三唑磷在酸碱环境中的稳定性，同时还能阻止三唑磷水解作用的发生。
银杏是我国多年生落叶乔木，银杏外种皮是其包裹种子的外部肉质部分，其主要成分为银杏黄酮，银杏内脂以及银杏酚酸等化合物。有研究表明，银杏外种皮有效活性物质具有杀虫作用，但是目前在农业领域该天然产物应用较少，对农业害虫的作用方式作用机理尚不明确。植物源农药具有绿色环保等优点，将其开发成具有商业价值的农药具有十分重要的意义。然而，一些植物源农药有效活性成分含量低，生产成本高，阻碍了植物源农药进一步的开发和利用。
发明内容
本发明针对现有技术的缺陷，提供了一种植物源自乳化纳米杀虫剂及其制备方法和应用，能有效的解决上述现有技术存在的问题。
为了实现以上发明目的，本发明采取的技术方案如下：
一种植物源自乳化纳米杀虫剂，包括以下重量百分比的成分：
银杏外种皮乙醇粗提物2％～5％；
溶剂乙醇与银杏外种皮粗提物质量比为1:1；
表面活性剂含量为2.5％～3％；
助表面活性剂含量为2％～2.5％。
进一步地，所述表面活性剂为聚氧乙烯蓖麻油或聚氧乙烯氢化蓖麻油。
进一步地，所述的助表面活性剂为乙二醇、甘油、正丁醇、聚乙二醇400其中的一种。
上述杀虫剂的制备方法包括以下步骤：
自乳化法制备纳米乳液，银杏乙醇粗提物的油相和表面活性剂和助表面活性剂(表面活性剂与助表面活性剂质量比，混合物)组成的有机相加入水相中，室温下搅拌15min。
作为优选，搅拌的转速为500rpm。
作为优选，固定水相浓度为质量百分比96％。
上述乳化纳米杀虫剂，应用对象为多种害虫，包括：鳞翅目小菜蛾、粘虫、棉铃虫等。
与现有技术相比本发明的优点在于：采用天然表面活性剂，将无水的自乳化纳米乳液引入农药杀虫剂中，能有效提高天然植物源农药的生物活性，有利于提高产品质量和产量，同时降低生产成本，对鳞翅目农业害虫的防效均高于90％，对蚜虫防效亦高于90％。
附图说明
图1为本发明实施例自乳化纳米乳液透射电镜图；
图2为本发明实施例自乳化纳米乳液液滴粒径分布图。
具体实施方式
为使本发明的目的、技术方案及优点更加清楚明白，以下参照附图并举实施例，对本发明做进一步详细说明。
一种植物源自乳化纳米杀虫剂，包括以下重量百分比的成分：
银杏外种皮乙醇粗提物2％～5％；
溶剂乙醇与银杏外种皮粗提物质量比为1:1；
表面活性剂含量为2.5％～3％；
助表面活性剂含量为2％～2.5％。
所述表面活性剂为聚氧乙烯蓖麻油(Cremophor EL)或聚氧乙烯氢化蓖麻油(Cremophor RH 40)。
所述的助表面活性剂为乙二醇、甘油、正丁醇、聚乙二醇400(PEG400)其中的一种。
上述杀虫剂的制备方法包括以下步骤：
自乳化法制备纳米乳液，油相(银杏乙醇粗提物)，表面活性剂和助表面活性剂组成的有机相加入水相中，室温下搅拌15min，转速为500rpm。除非特别强调，固定水相浓度为96％(w/w)。
本发明所述自乳化纳米杀虫剂，应用对象为多种农业害虫，包括鳞翅目小菜蛾、粘虫、棉铃虫等，防效均高于90％。此外，对蚜虫防效亦高于90％。
相图的绘制：滴定法绘制相图，观察不同组分的动态相行为。设表面活性剂:助表面活性剂质量比(Smix)＝4:1、3:1、2:1、1:1、1:0、1:2、1:3，表面活性剂：油相质量比(SOR)＝9:1、8:2、7:3…2:8、1:9。准确称取油相，表面活性剂和助表面活性剂，50℃下搅拌均匀后，冷却至室温。偏光显微镜观察是否出现液晶相，电导率仪测定体系电导率判断相变点。
乳液粒径大小及粒径分布：采用动态激光散射法(DLS)测定乳液的液滴粒径和分散情况，仪器使用Nano Zetasize光子相关光谱仪，测量参数为：25℃，4m W氦-氖光源设定波长633nm，散射角173°，后向散射模式。
电导率的测定：取一定量的油相和表面活性剂/助表面活性剂混合，逐滴加入0.01mol/L NaCl水溶液，测定体系电导率变化。随着水含量的增加，电导率值逐渐增大，到达临界最大值后突然降低，这个突变点即为相转变点。
新鲜制备样品乳液液滴粒径大小和粒径大小分布，如图1和图2所示；
通过将样品在60℃贮存15天，在0℃贮存7天，其物理性能稳定性监测结果如表1，化学稳定性检测结果如表2。
表1
表2
为了更好的理解本发明的实质，下面通过对小菜蛾的室内及大田生物活性实验来进行说明。
银杏外种皮乙醇提取物自乳化纳米乳液对小菜蛾的室内拒食活性测定。挑选头胸等宽，健康有活力的小菜蛾3龄幼虫，给药前饥饿3～4h。用打孔器打成直径为9mm的叶片，银杏纳米乳液中浸渍6～8s，置于滤纸上晾干后，在放入垫有潮湿滤纸的培养皿内。将饥饿处理过的小菜蛾幼虫接入培养皿内，每皿10头，每组5个重复，放入人工气候箱中(25℃,70％RH)。分别于12h，24h，36h和48h检查结果，用毛笔轻触虫体无反应则判断为死亡，结果如表3所示；
表3
结果表明，在银杏外中皮提取物和其纳米乳液处理过的叶片，小菜蛾3龄幼虫出现明显的拒食现象，小菜蛾幼虫的存活受到明显的抑制。此外，银杏外种皮提取物对小菜蛾幼虫还有一定的胃毒作用，中毒试虫表现为腹泻，呕吐，虫体失水，死亡。由表3还可以明显看出，银杏外种皮纳米乳液对小菜蛾的毒杀作用明显高于其粗提物和市售3.0％氯氟氰菊酯，对小菜蛾幼虫毒杀作用快，毒杀作用随着作用时间的延长而增强。
2.银杏外种皮乙醇提取物自乳化纳米乳液对小菜蛾的大田活性测定。在室内生物活性测定的基础上，为了进一步明确5％银杏外种皮自乳化纳米乳液在田间的最佳剂量和防效，进行了田间试验。田间试验在湖南省永州市零陵区双牌县甘蓝地进行，试验地地势平坦，灌溉条件良好；甘蓝生长整齐旺盛，之前未施用过任何化学药剂。设置不同浓度的药剂以及3.0％氟氯氰菊酯和清水为对照，施药期选择田间小菜蛾3龄盛发期，采用农用16L手动喷雾器，在甘蓝叶面和叶背均匀喷药，结果如表4所示：
表4
研究5％银杏外种皮粗提物对小菜蛾的田间防效，施药1d后，银杏外种皮纳米乳液对小菜蛾的防效为15％作用，但施药3d后，其药效明显提高，防效为80％左右，施药7d后，银杏外种皮纳米乳液可使小菜蛾田间防效高达95％。与市售3％氯氟氰菊酯相比，银杏外种皮纳米乳液见效慢，但是防效更高。
本领域的普通技术人员将会意识到，这里所述的实施例是为了帮助读者理解本发明的实施方法，应被理解为本发明的保护范围并不局限于这样的特别陈述和实施例。本领域的普通技术人员可以根据本发明公开的这些技术启示做出各种不脱离本发明实质的其它各种具体变形和组合，这些变形和组合仍然在本发明的保护范围内。
Claims (7)
1.一种植物源自乳化纳米杀虫剂，其特征在于，包括以下重量百分比的成分：
银杏外种皮乙醇粗提物2％～5％；
溶剂乙醇与银杏外种皮粗提物质量比为1:1；
表面活性剂含量为2.5％～3％；
助表面活性剂含量为2％～2.5％。
2.根据权利要求1所述的杀虫剂，其特征在于：所述表面活性剂为聚氧乙烯蓖麻油Cremophor EL或聚氧乙烯氢化蓖麻油Cremophor RH 40。
3.根据权利要求1所述的杀虫剂，其特征在于：所述的助表面活性剂为乙二醇、甘油、正丁醇、聚乙二醇400其中的一种。
4.根据权利要求2或3所述的杀虫剂，其特征在于：杀虫剂应用对象为害虫，包括：鳞翅目小菜蛾、粘虫、棉铃虫。
5.根据权利要求1所述杀虫剂的制备方法，其特征在于：包括以下步骤：
自乳化法制备纳米乳液，银杏乙醇粗提物的油相和表面活性剂和助表面活性剂组成的有机相加入水相中，室温下搅拌15min。
6.根据权利要求5所述的制备方法，其特征在于：搅拌的转速为500rpm。
7.根据权利要求5所述的制备方法，其特征在于：固定水相浓度为质量百分比96％。
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| CN110521737A (zh) * | 2019-07-19 | 2019-12-03 | 湖南科技学院 | 一种防治链格孢菌所致植物真菌病害的菌剂组合物及其制备方法和用途 |
| CN113951259A (zh) * | 2021-11-02 | 2022-01-21 | 徐州三农生物科技有限公司 | 一种银杏酚酸乳浊液剂 |
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| CN101124917A (zh) * | 2007-09-06 | 2008-02-20 | 江苏大学 | 银杏杀钉螺微乳剂及其制备方法 |
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| CN110521737A (zh) * | 2019-07-19 | 2019-12-03 | 湖南科技学院 | 一种防治链格孢菌所致植物真菌病害的菌剂组合物及其制备方法和用途 |
| CN113951259A (zh) * | 2021-11-02 | 2022-01-21 | 徐州三农生物科技有限公司 | 一种银杏酚酸乳浊液剂 |
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