CN114072226B - 一种获得高稳定性天然除虫菊酯微生物胶囊的方法和过程 - Google Patents
一种获得高稳定性天然除虫菊酯微生物胶囊的方法和过程 Download PDFInfo
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- CN114072226B CN114072226B CN202080046321.9A CN202080046321A CN114072226B CN 114072226 B CN114072226 B CN 114072226B CN 202080046321 A CN202080046321 A CN 202080046321A CN 114072226 B CN114072226 B CN 114072226B
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Abstract
本发明描述了一种方法，用于获得作为活性物质的一种或多种除虫菊酯的微生物胶囊，属于生物农药生产技术领域。天然除虫菊酯是从菊属植物的花中提取的广谱杀虫剂，易被空气和光分解。本发明增加了除虫菊酯的稳定性，相比现有技术的其他解决方案，能够更长时间有效。方法和过程包括以下步骤：准备油阶段的第一步、乳化混合物的第二步和包封的第三步。结果是尺寸在0.5至5微米之间的除虫菊酯微生物胶囊的产品，具有更高的稳定性。该过程不会降低除虫菊酯的杀虫能力。
Description
技术领域
本发明属于化学工业领域应用领域，致力于纳米生物农药的生产，具体涉及除虫菊酯纳米乳剂的生产方法。
背景技术
随着社会的发展和农业面积的扩大，产生了对新型、更高效以及安全的杀虫剂的需求。一些高效的化学制剂迅速出现，但在分析作物时出现了大量残留。然而，随着近年来环保意识和认证的发展以及生物技术的进步，杀虫剂生产商开始采取安全、高效、循环经济和人性化的准则，从而实现了无毒、生态和零残留产品。生物农药已成为农化行业的优先生产线。
天然除虫菊酯作为杀虫剂的使用有着悠久的历史，可用于防治影响人类和作物的害虫。天然除虫菊酯是从除虫菊(pyretheum)花朵(除虫菊(Chrysanthemumcinerariaefolium))中提取的杀虫剂，易被光、空气、水和微生物降解。除虫菊酯对破坏作物的昆虫有剧毒，但对温血动物是安全的、无污染、且不留残留物。
为防治害虫，除虫菊酯通常以固体、油、可湿性粉剂和可乳化浓缩物的形式存在。在除虫菊油和浓缩乳液的情况下，其通常与物质和植物衍生物混合，这些是水和环境的污染物。除虫菊酯的包封不仅考虑需要较低剂量的除虫菊酯，而且还保护环境、降低生产成本、增加杀虫剂与其他供应物或其他杀虫剂接触的有效性并阻止活性物质的难闻气味。含有拟除虫菊酯、植物油、溶剂和乳化表面活性剂体系的杀虫剂组合物是已知的(EP 567,368)。同样，含有拟除虫菊酯、可含有植物油的赋形剂、表面活性剂体系和可选的溶剂和稳定剂的可乳化浓缩物是已知的(GB 2,058,569)。含有拟除虫菊酯、植物油和表面活性剂体系的组合物也是已知的，例如由非离子和阴离子表面活性剂的混合物组成(US 4,617,3318)，例如含有拟除虫菊酯、植物油或其他酯的组合物，例如有机溶剂(ES 2,144,618)。然而，这些文件中没有一个声称、提及或能从描述中删去拟除虫菊酯微胶囊。
关于获得微胶囊的过程，从20世纪70年代初至今，微胶囊技术已开始应用于农药剂型加工。但是，具有微胶囊活性物质的产品数量相当有限。1976年，美国Pennwalt公司推出了第一款微胶囊杀虫剂：甲基对硫磷，其可显著降低产品的毒性并延长其作用时间。Pennwalt公司还通过复杂且高成本的过程包封了来自Pennwalt公司的除虫菊酯ES8506420。此后，在微胶囊开发领域进行了不同的调查，特别是在农业领域，至今有200多家农化公司在微胶囊的开发和应用方面具有研究项目。因此，农药微胶囊的发展已有40多年的历史，但与医药行业的发展相比，这是相当缓慢的。因此，市场上基于农药微胶囊的产品种类还很少。
目前的农药微胶囊方法主要包括：聚合、内聚分离阶段和溶剂蒸发。这些方法不仅复杂而且成本高。还大量使用有机溶剂，造成污染。
尽管存在所有这些现有的替代方案，仍然需要提供一种获得除虫菊酯微生物胶囊的过程，该过程不会影响杀虫能力，从而可以用于害虫防治。
发明内容
本发明通过以下方式进行设计，以提供根据本发明的第一方面的，一种获得作为活性物质的一种或多种除虫菊酯的微生物胶囊的过程，该过程包括三个步骤：
1.油制备阶段，由浓度介于48％-80％之间的作为活性物质的一种或多种除虫菊酯以1:20的比例溶解在一种或多种植物油中，可选地进行搅拌，可选地可以加入溶剂，溶剂可以是脂肪酸、醇、精油或它们的混合物，然后对混合物进行搅拌。
2.乳化阶段，其中加入乳化剂和可选的稳定剂和/或防腐剂，同时进行搅拌。此外，可以加入具有抗氧化性能的共配制剂、防腐剂和/或消泡剂。
3.获得微生物胶囊的阶段，其中通过混合过程，优选使用混合器，例如具有桨式搅拌器的混合器，结果是获得介于4-25％p/v，优选4-8％w/v之间，且尺寸在0.5至5微米之间的除虫菊酯微生物胶囊，具有更高的稳定性。
本发明中，除虫菊酯微胶囊是指：具有外膜的微米颗粒，其中含有作为活性物质的除虫菊酯。
在阶段(1)中，加入一种或多种植物油，它们选自由向日葵、玉米、大豆、鳄梨、荷荷巴油、南瓜、葡萄籽、芝麻、榛子油、甘油三己辛酸酯或分子式为R9COOR10的植物油组成的组，其中R9表示包含7至29个碳原子的高级脂肪酸的部分，R10表示包含3至30个碳原子的直链或支链烃链，特别是烷基或烯基、十一烯酸、肉豆蔻油酸、棕榈油酸，油酸、亚油酸、亚麻酸、蓖麻油酸、二十碳烯酸或二十二碳烯酸(存在于松树、玉米、向日葵、大豆、葡萄干种子、亚麻或荷荷巴油中)。作为脂肪酸的优选示例，可以提及包含不饱和分子的脂肪酸，例如油酸类型，其通过双键缩合反应低聚。该反应产生基本上包括二聚体和三聚体的混合物。脂肪酸的二聚体和三聚体是指2或3个相同或不同单体的低聚物。有利地，这些饱和或不饱和的脂肪酸包括12至100个碳原子，更有利地包含24至90个。
在阶段(1)中，以60-150RPM进行搅拌。
在阶段(1)中，温度为20℃至40℃，优选在25℃-35℃之间。
在阶段(1)中，可以加入选自不饱和脂肪酸及其衍生物的溶剂：亚油酸、亚麻酸、油酸、叶酸及其衍生物、泛醌和泛醇及其衍生物、生育酚及其衍生物。
在阶段(1)中，可加入溶剂，溶剂选自乙醇、异丙醇等低级醇；甘油、丙二醇、二丙二醇、山梨糖醇等多元醇；
在阶段(1)中，可以加入选自天然或合成精油的溶解剂，例如桉树油、薰衣草油、薰衣草、香根草、山苍子、柠檬、檀香、迷迭香、洋甘菊、香薄荷、肉豆蔻、肉桂、牛膝草、香菜、橙子、天竺葵、杜松和佛手柑。
在阶段(2)中，加入非离子乳化剂，其以组合物的10至50％重量，优选地，相对于组合物总重量的15至30％重量的比例出现。
非离子乳化剂应理解为是指两性的、阴离子的，优选阳离子的。两性或两性乳化剂应理解为那些表面活性剂化合物，其除了含有8至18个碳原子的烷基或酰基外，分子中还含有至少一个游离氨基和至少一个-COOH或-SO3H基团，适合形成内盐。合适的两性表面活性剂的示例是N-烷基甘氨酸、N-烷基丙酸、N-烷基氨基丁酸、N-烷基亚氨基二丙酸、N-羟乙基-N-烷基酰胺丙基甘氨酸、N-烷基牛磺酸、N-烷基肌氨酸、2-烷基氨基丙酸和烷基氨基乙酸，在每种情况下在烷基中具有约8至18个碳原子。阴离子乳化剂应理解为具有负电荷的那些乳化剂，阴离子表面活性剂的示例是，例如链长为8至18个C原子的烷基硫酸盐、疏水部分中具有8至18个C原子的烷基或烷基芳基醚硫酸盐和最多40个环氧乙烷或环氧丙烷单元、具有8至18个碳原子的烷基或烷基芳基磺酸盐、磺基琥珀酸与一元醇或烷基酚的酯和半酯、烷基或烷基芳基磺酸盐、羟基链烷醇硫酸盐、具有8至24个碳原子的饱和和不饱和链的脂肪酸及其氧化烯化酯，以及聚乙氧基化链烷醇的硫酸盐和磷酸盐。阳离子乳化剂应理解为在水溶液中含有正电荷的那些乳化剂、胺类以及季铵化合物。阳离子乳化剂的示例是具有7至25个碳原子的烷基胺，具有7至25个碳原子的N，N-二甲基-N-(羟烷基)铵盐，与烷基化剂季铵化的单-和二-(具有7至25个碳原子)-烷基二甲基铵盐，诸如酯化的季单-、二-或三链烷醇胺等的酯季铵盐，其与具有8至22个碳原子的羧酸酯化，以及诸如通式I或II的1-烷基咪唑啉盐等的咪唑啉季铵盐。
在阶段(2)中，使用的阳离子乳化剂是季铵化合物，观察到它增加了根据所述过程得到的产品的杀虫能力。
在阶段(2)中，可选地，可以加入第二乳化剂，当使用乳化剂组合时，有利的是使用相对疏水的乳化剂与相对亲水的试剂的组合，或者组合使用阴离子乳化剂与非离子试剂。
在阶段(2)中，通常可以以相对于组合物总重量的10至50％重量，优选15至30％重量的比例，向组合物中加入第二乳化剂。
在阶段(2)中，另外，可以加入共配制剂，其可以选自抗氧化剂例如生育酚和没食子酸丙酯、硝基氧化物、BHT-丁基羟基甲苯、BHA-丁基羟基茴香醚和/或酸化剂，例如，柠檬酸、乳酸和苹果酸、盐酸、酒石酸、磷酸、乳酸、磺酸和/或消泡剂；包含14-24个碳原子的至少一种硅基或氟基脂肪酸。
在阶段(2)中，温度在10-45℃之间，优选在25-35℃之间。
在阶段(3)中，以60-300RPM进行搅拌1至36小时，优选1至4小时。该阶段在密度为0.910-0.980g/cm3和pH值在5-10之间，优选在6.5-8.5之间的受控条件下工作。所述过程的最终结果是获得尺寸在0.5-5μm之间、具有规则形态和光滑表面的除虫菊酯微生物胶囊。
另一方面，本发明涉及本发明的微生物胶囊作为杀虫剂的用途。更具体地，本发明涉及本发明的微胶囊用于防治节肢动物害虫用途，节肢动物例如为昆虫，优选蚜虫和蚂蚁。通过此过程获得的杀虫产品的有效性可持续长达2年。
附图说明
为了补充所做出的描述并帮助更好地理解本发明的特征，附上一组附图作为所述描述的组成部分，其中出于说明性和非限制性的目的，表示以下内容：
图1示出了在正常条件下和14天后在同一化合物中应用MT 46.3方法所得组合物的色谱图。
图2示出了除虫菊酯微生物胶囊的照片，其中观察落射荧光显微镜(Axioplan，ZEISS)。将样品滴放置在具有20×物镜的载玻片(20×40×0.25mm)上。
图3示出了除虫菊酯微生物胶囊的照片，其中标明了它们的大小和单分散性：
1.长度5.14μm
2.长度4.42μm
3.长度5.48μm
4.长度5.14μm
具体实施方式
本发明将通过发明人进行的试验说明如下，这些试验表明了本发明过程的有效性：
实施例1
将73g菊花精制提取物EDEOIL混合作为60％(w/w)的除虫菊酯来源；除虫菊酯I、瓜菊酯I、茉莉宁I、除虫菊酯II、瓜菊酯II和茉莉宁II，除虫菊酯I和除虫菊酯II的比例为1.85，其中557g的大豆油含有50％的亚油酸和25％的油酸，还含有月桂酸、肉豆蔻酸、棕榈酸、硬脂酸和亚麻酸，在HI/>中25℃温度下以60rpm的转速进行搅拌，并加入1g富含生育酚E306的提取物，继续搅拌20分钟，然后不停搅拌，加入158g的99.5％丙二醇和185g的97％聚山梨醇酯80/>然后加入15g浓度为94％的D-柠檬烯(苦橙)和8g植物甘油E-422，作为共制剂，从而提高制剂的张力活性。以120rpm转速搅拌约2小时，观察微生物胶囊的外观(图2)，然后根据(图3)测量微胶囊及其形状。
实施例2
为了确定通过如实施例1中所述的本发明过程获得的产物的稳定性，方法MT 46.3(J.Zhang等人，色谱法杂志A辑(J.of Chromatography A.)1218(2011)6621-6629，DeanBan等人，非洲生物技术期刊(Afr.J.of Biotechnology)，卷9(18)，第2702-2708页，2010年5月3日)通过热刺激使制剂老化并模拟包封和储存的产品(图1)。通过测试的制剂被认为至少可以使用2年。
表I
54℃下储存稳定性
Claims (13)
1.一种获得除虫菊酯微生物胶囊的过程，包括以下几个步骤：(1)准备油相，包括将浓度介于48％-80％w/w之间的作为活性物质的一种或多种除虫菊酯以1:20的比例溶解在一种或多种植物油中的溶液，并且向其中加入溶剂混合物，所述溶剂混合物包括：生育酚、甘油、丙二醇和橙油；(2)准备乳化相，向油相中加入乳化剂，其中所述乳化剂占相对于组合物总重量的10至50％重量；(3)通过混合乳化相过程准备4-25％w/v的尺寸在0.5μm到5μm的除虫菊酯微生物胶囊，其中，在pH5-10的条件下以60-150RPM搅拌1至36小时。
2.根据权利要求1所述的获得除虫菊酯微生物胶囊的过程，其特征在于在步骤(1)中，植物油选自由向日葵、玉米、大豆、鳄梨、荷荷巴油、南瓜、葡萄籽、芝麻、榛子、甘油三己辛酸酯或分子式为R9COOR10的植物油组成的组，其中R9表示包括7至29个碳原子的高级脂肪酸的部分，R10表示包含3至30个碳原子的直链或支链烃链。
3.根据权利要求1所述的获得除虫菊酯微生物胶囊的过程，其特征在于在步骤(1)中，温度为20℃至40℃。
4.根据权利要求1所述的过程，其中，加入的所述乳化剂是非离子两性或两性类型的。
5.根据权利要求4所述的过程，其中，相对疏水的第二乳化剂与相对亲水的试剂组合加入。
6.根据权利要求5所述的过程，其中所述第二乳化剂是与非离子试剂组合的阴离子。
7.根据权利要求1所述的过程，其中，还加入共配制剂。
8.根据权利要求7所述的过程，其中，所述共配制剂是抗氧化剂。
9.根据权利要求7所述的过程，其中，所述共配制剂是酸化剂。
10.根据权利要求7所述的过程，其中，所述共配制剂是消泡剂。
11.根据权利要求1所述的获得除虫菊酯微生物胶囊的过程，其特征在于在步骤(2)中，温度在10℃-45℃之间。
12.根据权利要求1所述的获得除虫菊酯微生物胶囊的过程，其特征在于在步骤(3)中，所述除虫菊酯微生物胶囊的密度在0.910g/cm3至0.980g/cm3之间。
13.根据权利要求1所述的过程得到的微生物胶囊的用途为防治害虫。
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| ES2794124B8 (es) | 2021-10-07 |
| CN114072226A (zh) | 2022-02-18 |
| US20220225619A1 (en) | 2022-07-21 |
| PE20220385A1 (es) | 2022-03-18 |
| BR112021023036A2 (pt) | 2021-12-28 |
| CL2021003028A1 (es) | 2022-06-17 |
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