CN117598328A - 一种含桉叶油的复合除草剂及其制备方法 - Google Patents
一种含桉叶油的复合除草剂及其制备方法 Download PDFInfo
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Classifications
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- A—HUMAN NECESSITIES
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- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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- A01N65/28—Myrtaceae [Myrtle family], e.g. teatree or clove
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- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
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- A01N35/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical
- A01N35/02—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical containing aliphatically bound aldehyde or keto groups, or thio analogues thereof; Derivatives thereof, e.g. acetals
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- A—HUMAN NECESSITIES
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- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/34—Rosaceae [Rose family], e.g. strawberry, hawthorn, plum, cherry, peach, apricot or almond
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- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P13/00—Herbicides; Algicides
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Abstract
本发明涉及一种含桉叶油的复合除草剂及其制备方法,涉及农业技术领域。本发明含桉叶油的复合除草剂,以桉叶油和麦李叶提取物为活性成分,且含有助剂3‑癸烯‑2‑酮;其中,桉叶油和麦李叶提取物的质量比为1‑2:2‑3,3‑癸烯‑2‑酮的质量为上述活性成分质量的8‑10%,桉叶油为柠檬桉叶油。本发明的除草剂对于玉米田中常见禾本科杂草和阔叶杂草均具有显著的防效,且安全无毒,不影响玉米作物的正常生长,同时具有制备方法简单的特点,适用于工业化推广应用,具有重要的经济价值。
Description
技术领域
本发明涉及农业技术领域,特别是涉及一种含桉叶油的复合除草剂及其制备方法。
背景技术
桉树(Eucalyptus spp.)是一种具有极高观赏、用材以及药用等价值的优良树种。如,桉树可以用于浆粕、人造板等用料,还可以用于生产精油、柠檬酸、桉叶醇等物质,桉树还能作为医药原材料用于腹泻、炎症、镇静安神等相关药物制备。
桉树中含有大量生物成分,研究表明,各种桉树叶提取物均不同程度地具有抑制寄生虫生长的功效,桉树叶提取物对鞭毛虫、孢子虫、纤毛虫等体表、体内寄生原虫有趋避和灭杀作用。Maciel等以去离子水和3%吐温80做阴性对照,以0.196mg/mL氯氰菊酯为阳性对照,发现柠檬桉、蓝桉和Staigeriana等精油成分z-柠檬醛和α-柠檬醛、香茅醛、1,8-桉叶素等对长须罗蛉卵、幼虫、成虫有杀虫效果,其中,Staigeriana桉树提取物最佳,柠檬桉及蓝桉次之。
桉叶油是桉树中提取的一种植物精油,主要包括黄酮类、萜类等物质,具有抗氧化、抗炎、杀虫、驱蚊等诸多功效。相关研究报道表明,桉叶油对引起呼吸道疾病的金黄色葡萄球菌、化脓性链球菌、肺炎链球菌、流感嗜血杆菌、肺炎克雷伯菌等具有很强的抑制作用。目前,基于桉叶油的相关功效研究一直在探索并深入中。
除草剂是一种可使杂草彻底或选择性枯死的药剂,可以完全或部分抑制杂草植株生长,现有除草剂效果较好的多为化学除草剂,而尽管化学除草剂能实现较好的除草效果,但化学试剂的大量使用会引发一系列的环境问题。不仅如此,目前,单一组分的化学除草剂也已经难以抑制多种混生杂草的生长。现有化学药剂的使用弊端已经越来越显著,这使得对绿色、环保的植物源组分除草剂的研究更加迫切,急需提供一种高效、广谱、低毒的植物源除草剂以改善上述技术现状。
发明内容
本发明的目的是提供一种含桉叶油的复合除草剂及其制备方法,以解决上述现有技术存在的问题。
为实现上述目的,本发明提供了如下方案:
本发明提供一种含桉叶油的复合除草剂,以桉叶油和麦李叶提取物为活性成分,且含有助剂3-癸烯-2-酮;
所述桉叶油和麦李叶提取物的质量比为1-2:2-3;所述3-癸烯-2-酮的质量为所述活性成分质量的8-10%;
所述桉叶油为柠檬桉叶油;是以柠檬桉叶为原料,进行水蒸气蒸馏得到。
具体制备过程为:称取自然晾干的柠檬桉树叶,粉碎,按照1g:8-10mL的料液比,加入水中,在95~105℃进行蒸馏,冷却,静置至水油分层,收集有机层,得到桉叶油。
作为本发明的进一步优选,所述麦李叶提取物的制备方法包括以下步骤:
利用氯仿对麦李叶进行一次浸提,过滤,浓缩一次滤液,之后利用乙酸乙酯对浓缩产物进行二次浸提,过滤,收集二次滤液,浓缩干燥,得到所述麦李叶提取物。
作为本发明的进一步优选,所述一次浸提为超声浸提,超声功率为250-300W,超声时间为10-15min。
作为本发明的进一步优选,所述二次浸提的时间为15-30min。
作为本发明的进一步优选,所述复合除草剂的剂型为微乳剂或水乳剂。
作为本发明的进一步优选,所述复合除草剂中活性成分的含量为3-6.5%。
本发明还提供上述复合除草剂的制备方法,当所述复合除草剂的剂型为微乳剂时,制备方法包括以下步骤:将所述桉叶油、麦李叶提取物、3-癸烯-2-酮与有机溶剂、表面活性剂、增效剂、防冻剂和水混合,搅拌,得到所述含桉叶油的复合除草剂;
当所述复合除草剂的剂型为水乳剂时,制备方法包括以下步骤:将所述桉叶油、麦李叶提取物、3-癸烯-2-酮与有机溶剂、表面活性剂、增效剂、防冻剂、增稠剂和水混合,搅拌,得到所述含桉叶油的复合除草剂。
本发明中,制备微乳剂或水乳剂剂型的复合除草剂时,所用有机溶剂为乙醇、乙酸乙酯或二甲基甲酰胺;所用表面活性剂为烷基苯磺酸盐类,优选十二烷基苯磺酸钠;所用增效剂为油酸甲酯;所用防冻剂为乙二醇或丙二醇;所用增稠剂为黄原胶或羧甲基纤维素钠。
本发明进一步提供上述含桉叶油的复合除草剂在玉米田杂草去除中的应用。
本发明含桉叶油的复合除草剂施用量为180-320g/亩,稀释500-800倍后喷施。
桉叶油是从桉树叶中提取的植物精油,具有芳香味及挥发性,主要化学成分是萜类化合物及其含氧衍生物。麦李(Prunus glandulosa Thunb.)为蔷薇科李属的灌木。本发明研究发现,对麦李的叶子部位进行提取,将得到的麦李叶提取物与桉叶油复配,二者能发挥协同增效作用,对于玉米田常见禾本科杂草和阔叶杂草具有显著的防效,且对玉米作物安全无毒,尤其是针对抗药性比较强、难以防治的鸭跖草也能实现理想的防效。
3-癸烯-2-酮是一种植物生长调节剂,属于α-β不饱和脂肪酮类化学物质,最近研究发现,3-癸烯-2-酮能够发挥生姜采后抑芽的作用,用3-癸烯-2-酮处理生姜可以有效降低其在25℃、相对湿度95%条件下贮藏期内的发芽率。本发明发现,将少量的3-癸烯-2-酮添加于桉叶油和麦李叶提取物的复配物中,能够提升二者的除草功效;进一步研究表明,麦李叶提取物还能一定程度加速3-癸烯-2-酮在玉米作物中降解、消除。
本发明公开了以下技术效果:
本发明以安全无毒的桉叶油与麦李叶提取物复配作为复合除草剂的活性组分,二者能够发挥协同增效作用,对于玉米田中常见禾本科杂草和阔叶杂草均具有显著的防效,且安全无毒,不影响玉米作物的正常生长。
本发明复合除草剂绿色环保,制备方法简单,适用于工业化推广应用,具有重要的经济价值。
具体实施方式
现详细说明本发明的多种示例性实施方式,该详细说明不应认为是对本发明的限制,而应理解为是对本发明的某些方面、特性和实施方案的更详细的描述。
应理解本发明中所述的术语仅仅是为描述特别的实施方式,并非用于限制本发明。另外,对于本发明中的数值范围,应理解为还具体公开了该范围的上限和下限之间的每个中间值。在任何陈述值或陈述范围内的中间值,以及任何其他陈述值或在所述范围内的中间值之间的每个较小的范围也包括在本发明内。这些较小范围的上限和下限可独立地包括或排除在范围内。
除非另有说明,否则本文使用的所有技术和科学术语具有本发明所述领域的常规技术人员通常理解的相同含义。虽然本发明仅描述了优选的方法和材料,但是在本发明的实施或测试中也可以使用与本文所述相似或等同的任何方法和材料。本说明书中提到的所有文献通过引用并入,用以公开和描述与所述文献相关的方法和/或材料。在与任何并入的文献冲突时,以本说明书的内容为准。
在不背离本发明的范围或精神的情况下,可对本发明说明书的具体实施方式做多种改进和变化,这对本领域技术人员而言是显而易见的。由本发明的说明书得到的其他实施方式对技术人员而言是显而易见得的。本发明说明书和实施例仅是示例性的。
关于本文中所使用的“包含”、“包括”、“具有”、“含有”等等,均为开放性的用语,即意指包含但不限于。
如无特别说明,本发明中所述“份”均为“质量份”。
本发明以下实施例对比例(除对比例4外)中,桉叶油是以柠檬桉的叶子为原料,经水蒸气蒸馏法制备得到:
称取自然晾干的柠檬桉树叶,粉碎,按照1g:10mL的料液比,加入水中,在95~105℃进行蒸馏,冷却,静置至水油分层,收集有机层,得到桉叶油。
实施例1
麦李叶提取物的制备:
(a)将麦李叶研磨后粉碎,之后加入5倍体积的氯仿,对体系进行超声处理(超声功率250W,提取时间为10min),过滤,收集所得滤液;
(b)将步骤(a)所得滤液浓缩除去溶剂,之后利用乙酸乙酯对浓缩产物浸提20min,过滤,收集滤液,浓缩干燥,得到麦李叶提取物,备用。
含桉叶油的复合除草剂(微乳剂)的制备:
(1)将1份桉叶油、2份麦李叶提取物加入25份乙酸乙酯中搅拌均匀,之后加入3-癸烯-2-酮(桉叶油和麦李叶提取物质量总和的10%),再次搅拌均匀;
(2)向步骤(1)得到的体系中加入5份十二烷基苯磺酸钠、8份油酸甲酯、5份乙二醇和40份水混合,搅拌,得到含桉叶油的复合除草剂(微乳剂)。
实施例2
麦李叶提取物的制备:
(a)将麦李叶研磨后粉碎,之后加入4倍体积的氯仿对体系进行超声处理(超声功率250W,提取时间为10min),过滤,收集所得滤液;
(b)将步骤(a)所得滤液浓缩除去溶剂,之后利用乙酸乙酯对浓缩产物浸提15min,过滤,收集滤液,浓缩干燥,得到麦李叶提取物,备用。
含桉叶油的复合除草剂(水乳剂)的制备:
(1)将2份桉叶油、3份麦李叶提取物加入25份二甲基甲酰胺中搅拌均匀,之后加入3-癸烯-2-酮(桉叶油和麦李叶提取物质量总和的8%),再次搅拌均匀;
(2)向步骤(1)得到的体系中加入5份十二烷基苯磺酸钠、8份油酸甲酯、5份丙二醇、0.5份黄原胶和40份水混合,搅拌,得到含桉叶油的复合除草剂(水乳剂)。
实施例3
麦李叶提取物的制备:
(a)将麦李叶研磨后粉碎,之后加入3倍体积的氯仿,对体系进行超声处理(超声功率250W,提取时间为10min),过滤,收集所得滤液;
(b)将步骤(a)所得滤液浓缩除去溶剂,之后利用乙酸乙酯对浓缩产物浸提20min,过滤,收集滤液,浓缩干燥,得到麦李叶提取物,备用。
含桉叶油的复合除草剂(微乳剂)的制备:
(1)将2份桉叶油、3份麦李叶提取物加入25份乙醇中搅拌均匀,之后加入3-癸烯-2-酮(桉叶油和麦李叶提取物质量总和的8%),再次搅拌均匀;
(2)向步骤(1)得到的体系中加入5份十二烷基苯磺酸钠、8份油酸甲酯、5份乙二醇和40份水混合,搅拌,得到含桉叶油的复合除草剂(微乳剂)。
对比例1
与实施例1不同之处仅在于:
将麦李叶替换成同为蔷薇科李属灌木的樱桃李的叶子;并将得到的樱桃李叶提取物等质量替换复合除草剂(微乳剂)中麦李叶提取物组分。
对比例2
与实施例1不同之处仅在于,将乙酸乙酯替换成叔丁醇。
对比例3
与实施例1不同之处仅在于,将氯仿替换成乙醇。
对比例4
与实施例1不同之处仅在于,所用桉叶油是以巨桉树叶为原料,经水蒸气蒸馏得到:
称取自然晾干的巨桉树叶,粉碎,按照1g:10mL的料液比,加入水中,在95~105℃进行蒸馏,冷却,静置至水油分层,收集有机层,得到桉叶油。
对比例5
与实施例1不同之处仅在于,不添加3-癸烯-2-酮。
效果验证例1:
试验对象:a.禾本科杂草:鸭跖草、马唐;b.阔叶杂草:刺菜、车前草。
试验方法:
实验分为4个组,分别计为实验组1-3和空白对照组。
实验各组采用等面积小区(1m2),播种鸭跖草种子30颗、马唐种子30颗、刺菜种子30颗、车前草种子30颗以及玉米幼苗12株。在同样的环境条件下培养2周,之后进行剔草处理,保证各组中各杂草数量均等同(均为30株)。
实验组1所用除草剂:实施例1的复合除草剂;
实验组2所用除草剂:与实施例1复合除草剂相比,不含有麦李叶提取物;
实验组3所用除草剂:与实施例1复合除草剂相比,不含有桉叶油;
空白对照组:不喷施除草剂,采用等量水替代。
除草剂施用量为280g/亩,稀释500倍后喷施。喷施7天后,统计杂草防效。
根据Gowing法评价杂草防效:
杂草防效(%)=(空白对照鲜重-实验组鲜重)/空白对照组鲜重×100%。
理论防效(%)E0=X+Y-XY/100;
其中,X、Y分别为单种活性组分的杂草防效(%),即桉叶油和麦李叶提取物单用的除草剂的防效。当实际防效-理论防效>10%时表现为增效作用。
结果如表1所示:
表1杂草防效
实验组1 | 实验组2 | 实验组3 | 空白对照组 | 理论防效 | |
鸭跖草 | 80.2% | 57.1% | 42.5% | - | 75.3% |
马唐 | 92.1% | 72.2% | 31.4% | - | 80.9% |
刺菜 | 91.5% | 70.5% | 33.6% | - | 80.4% |
车前草 | 94.8% | 66.7% | 47.3% | - | 82.5% |
由表1可以看出,桉树油与麦李叶提取物复配相对于两种组分单一使用时效果显著优异,除鸭跖草外,均能实现协同增效作用。
采用与实验组1相同的实验条件验证实施例2-3及对比例1-5的除草剂防效,结果如表2所示:
表2杂草防效
实施例2 | 实施例3 | 对比例1 | 对比例2 | 对比例3 | 对比例4 | 对比例5 | |
鸭跖草 | 80.4% | 80.6% | 57.5% | 58.2% | 57.8% | 51.6% | 70.1% |
马唐 | 91.8% | 91.5% | 72.6% | 73.1% | 72.7% | 47.1% | 81.8% |
刺菜 | 90.7% | 91.0% | 71.1% | 70.9% | 71.4% | 46.5% | 78.6% |
车前草 | 93.9% | 92.7% | 67.5% | 67.8% | 67.2% | 58.5% | 87.2% |
试验过程中,观察各组玉米生长情况均正常,没有任何病变情况,说明本发明的除草剂对玉米安全、无害。
效果验证例2
于两块等面积小区中分别种植80株玉米幼苗,计为处理组A和处理组B;分别采用实施例1和“效果验证例1”中实验组2的除草剂对玉米植株进行喷施(施用量为280g/亩,稀释500倍后喷施)。各组进行3组平行实验。
以除草剂喷施日为起始日,间隔5天从各组选取3株玉米,截取同等位置相同长度的茎叶,粉碎,利用高效液相色谱仪测定样品中3-癸烯-2-酮的含量。结果如表3所示。
表3
本发明上述研究发现,麦李叶提取物的存在,还能一定程度促进有机物3-癸烯-2-酮在玉米作物中的降解。
以上所述的实施例仅是对本发明的优选方式进行描述,并非对本发明的范围进行限定,在不脱离本发明设计精神的前提下,本领域普通技术人员对本发明的技术方案做出的各种变形和改进,均应落入本发明权利要求书确定的保护范围内。
Claims (9)
1.一种含桉叶油的复合除草剂,其特征在于,以桉叶油和麦李叶提取物为活性成分,且含有助剂3-癸烯-2-酮;
所述桉叶油和麦李叶提取物的质量比为1-2:2-3;所述3-癸烯-2-酮的质量为所述活性成分质量的8-10%;
所述桉叶油为柠檬桉叶油。
2.根据权利要求1所述的含桉叶油的复合除草剂,其特征在于,所述麦李叶提取物的制备方法包括以下步骤:
利用氯仿对麦李叶进行一次浸提,过滤,浓缩一次滤液,之后利用乙酸乙酯对浓缩产物进行二次浸提,过滤,收集二次滤液,浓缩干燥,得到所述麦李叶提取物。
3.根据权利要求2所述的含桉叶油的复合除草剂,其特征在于,所述一次浸提为超声浸提,超声功率为250-300W,超声时间为10-15min。
4.根据权利要求2所述的含桉叶油的复合除草剂,其特征在于,所述二次浸提的时间为15-30min。
5.根据权利要求1所述的含桉叶油的复合除草剂,其特征在于,所述复合除草剂的剂型为微乳剂或水乳剂。
6.根据权利要求5所述的含桉叶油的复合除草剂,其特征在于,以质量分数计,所述复合除草剂中活性成分的含量为3-6.5%。
7.如权利要求5所述的含桉叶油的复合除草剂的制备方法,其特征在于,当所述复合除草剂的剂型为微乳剂时,制备方法包括以下步骤:将所述桉叶油、麦李叶提取物、3-癸烯-2-酮与有机溶剂、表面活性剂、增效剂、防冻剂和水混合,搅拌,得到所述含桉叶油的复合除草剂;
当所述复合除草剂的剂型为水乳剂时,制备方法包括以下步骤:将所述桉叶油、麦李叶提取物、3-癸烯-2-酮与有机溶剂、表面活性剂、增效剂、防冻剂、增稠剂和水混合,搅拌,得到所述含桉叶油的复合除草剂。
8.如权利要求1-6任一项所述的含桉叶油的复合除草剂在玉米田杂草去除中的应用。
9.根据权利要求8所述的应用,其特征在于,所述含桉叶油的复合除草剂施用量为180-320g/亩,稀释500-800倍后喷施。
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