CN109090130A - 缓释型天然除虫菊素驱蚊粉剂的制备 - Google Patents
缓释型天然除虫菊素驱蚊粉剂的制备 Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- 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
- A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- 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
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- 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
- A01N25/22—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 ingredients stabilising the active ingredients
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- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
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Abstract
本发明公开了一种缓释型天然除虫菊素驱蚊粉剂的制备方法。主要成份为(质量百分比)：天然除虫菊素活性物含量1％‑4％，抗氧剂0.2％～1％、稳定剂0.2％～1％，NaY型微孔分子筛3％～12％，滑石粉82％～95.6％。本发明的特点是：驱蚊效果好，采用GB/T13717.9‑2009标准测试，有效驱蚊时间在10小时以上，达到A级标准；产品稳定性好，存放2年依然有效；不含有机溶剂、助剂，对人体无毒副作用；具有广谱驱避作用，可广泛用于驱除蚊、蝇、蠓、蜱等多种害虫。
Description
技术背景
本发明涉及一种天然除虫菊素制剂，具体是一种缓释型天然除虫菊素驱蚊粉剂的制备。
除虫菊(pyrethrum)是菊科菊属中的一个种多年生草本植物，从它的干花中可以萃取出除虫菊素的六种杀虫活性成分(商品名：天然除虫菊酯)。外观：浅黄色油状液体，不溶于水，能溶于乙醇、石油醚、四氯化碳、二氯甲烷等溶剂；见光或暴露于空气中易氧化慢慢分解成水(H2O)和二氧化碳(CO2)而失去杀虫活性，因此必须避光冷藏。由于哺乳动物体内有能将天然除虫菊素分解的酶，在哺乳动物体内不会蓄积残留，无潜在致畸、致癌、致突变等慢性毒性；除虫菊素兔急性经皮LD50是2370mg/Kg，大白鼠急性经口LD50＞5000mg/Kg，按我国农药毒性分级标准，属低毒杀虫剂，是国际公认的最安全的无公害天然杀虫剂，是一种安全有效的天然植物源杀虫剂，具有活性高、作用范围广，高效广谱等优点。主要用于防治卫生害虫，如蚊、蝇、臭虫等具有杀死、击倒、驱赶三种功效。
沸石分子筛是一种具有网状晶体结构的硅铝酸盐，这些网状的晶体结构互相连接，形成具有分子尺寸的规则孔道和晶穴的多孔四面体结构，它们的大小与形状相同，能被客体分子所充满，对物质的吸附来源于物理吸附(范德华力)，其晶体孔穴内部有很强的极性和库仑场，对极性分子和不饱和分子表现出强烈的吸附能力。不同类型的微孔分子筛其晶穴直径或形状各不相同，分为A型、X型、Y型。微孔分子筛都具有小于2nm的均匀开孔结构，孔体积约为0.2～0.3ml/g，比表面积约为750～1000，具有很大的表面积且是内表面积，外表面积仅占总表面积的1％左右，NaY型是上述Y型常规低硅铝比沸石分子筛中的一种。
驱避剂作为蚊虫防控传病的重要手段，对人类健康有着重要意义。蚊虫驱避剂的剂型分主要有膏霜剂、水剂和气雾剂等；蚊虫驱避剂按来源分为天然蚊虫驱避剂和人工合成蚊虫驱避剂，即植物性驱避剂和化学合成驱避剂。植物性蚊虫驱避剂具有气味清新、低毒或无毒、低残留、易降解、对皮肤不产生灼热感、安全环保等化学合成驱避剂不可企及的许多优点，由于皮肤的吸收和驱避剂在皮肤上蒸发损失，大多数驱避剂有效时间为3～4h，因此，驱避剂的研发目标是①通过剂型改造，改进驱避剂的物理性质，可提高驱避效果和安全性，减少皮肤吸收和解决蒸发损失；②开发应用安全高效、无污染的植物源驱避剂；③通过发展实用新剂型的开发，扩大现有驱避剂的应用范围，延长驱避效果，增强市场的竞争力；④加强研究蚊虫生理和行为与驱避剂的关系，驱避剂对蚊虫的作用机理等；⑤改进使用方法，达到节约用药、有效用药的目的。实践表明，缓释技术作为一种新兴的制剂加工技术，可以有效解决活性组分释放速度快、有效作用时间短的问题，缓释剂可将驱避活性成分暂时“储存”起来的同时让其缓慢释出，对活性物起到减少损耗、保护药效，达到长效驱避的目的。
在申请号为CN90110039.0，名称为驱蚊爽身粉的专利，介绍了一种驱蚊爽身粉的制备方法，该专利所述驱蚊粉剂组成为滑石粉92％～94.5％，复配驱蚊剂5.5％～8％，包括避蚊胺(DEET)2.5％～5％，邻苯二甲酸二甲酯0％～1.5％，樟脑0.5％～2％，驱蚊灵67号0％～2.5％，薄荷脑0.5％～1％，该复配驱蚊剂所含避蚊胺、邻苯二甲酸二甲酯、樟脑等药物直接和皮肤接触，药物在被皮肤吸收的同时也加速了蒸发，对人体有刺激性且影响神经系统，毒副作用大，残留药物还污染环境，影响部分淡水鱼类的生长；近年来，DEET的使用中出现许多问题，最为突出的是研究发现当人体有复杂气味存在时，DEET反而显著增强蚊虫向宿主定向飞行，增加了蚊虫叮咬概率；另外DEET对皮肤有一定刺激性，DEET对合成纤维、皮革、塑料等有破坏性。目前已经发现蚊虫对DEET产生抗药性的可能和数种对其产生抗药性的蚊虫。临床文献报告DEET引起的脑病变14例，其中13例是8岁以下儿童，14例接触性荨麻疹和刺激性皮炎。DEET毒性问题日益引起关注，目前泰国和我国台湾地区已禁止使用避蚊胺等。其次，采用滑石粉为基质，无孔道吸附，药物直接暴露在阳光和空气中，加速药物衰减，降低药物有效驱蚊时间和保质期。
发明内容
本发明的目的是提供一种不含对人体和环境有毒有害的产品，所制备的缓释型天然除虫菊素驱蚊粉剂以微孔分子筛(A型、X型、Y型)中的一种为载体，本发明采用Y型中NaY型分子筛为载体，以广谱、高效、安全、无污染的植物源驱避剂-天然除虫菊素为活性物，滑石粉为填料，制备过程中不添加对人体有害、污染环境的有机溶剂、助剂等。其原理是由于微孔分子筛孔径小于2nm，活性药物粒子吸附于分子筛孔道和晶穴的内表面，产生较强的范德华力作用，活性药物的稳定性显著增加，使物质熔化和汽化需要更多的能量，熔点、沸点升高，蒸发量降低，在降低药物用量、延长活性药物有效驱蚊时间的同时，提高了驱避效果。
吸附量为每100gNaY分子筛吸附20g～35g原药。
本发明产品外观为米白色粉末，具有天然除虫菊素的芬香气味，无油腻感，涂布性好，具有以下特点：1、药物基本吸附在分子筛的内表面，药物与人体表皮接触极少(仅1％左右)，表皮对药物吸收量极低，同时避免了刺激皮肤，提高了产品的安全性。2、不影响皮肤毛孔的透气性，人体舒适性好。3、驱虫效果好，采用GB/T13717.9-2009标准测试，有效驱蚊时间在10h以上，达到A级标准。4、产品质量稳定性好，放置2年以上依然有效。5、具有广谱驱避作用，可广泛用于驱除蚊、蝇、蠓、蜱等多种害虫。
本发明的目的通过以下技术方案来实现。
一种缓释型天然除虫菊素驱蚊粉剂，其特征在于：微孔NaY型分子筛、滑石粉、天然除虫菊素活性成分、抗氧剂、稳定剂组成；其质量百分比为：NaY型分子筛3％～12％、滑石粉82％～95.6％、天然除虫菊素活性成分1％～4％、抗氧剂0.2％～1％、稳定剂0.2％～1％。
本发明中，所述天然除虫菊素含50％的活性成分，所述抗氧剂为枸橼酸等多羧酸化台物，所述稳定剂为2，6-二叔丁基-4-甲基苯酚或2，5-二叔丁基对苯二酚，抗氧剂和稳定剂在分子筛内共同起到了抑制和延缓药物氧化降解的作用。
本发明所述缓释型天然除虫菊素驱蚊粉剂由下列方法制备(按质量百分比)：
1)取稳定剂0.2％～1％，抗氧剂0.2％～1％研磨，过筛(40～120目，下同)；
2)取天然除虫菊素活性成分1％～4％，将1)搅拌加入；
3)取NaY型分子筛3％～12％放入烘箱，在200℃烘2hr，脱附，取出降至低温，粉碎过筛；
4)将2)搅拌加入3)中；
5)滑石粉82％～95.6％放入烘箱中200℃烘2hr，脱水，取出降至低温，粉碎过筛；
6)将4)边搅拌边倒入5)中，混匀，过筛后分装密封，制得成品；
实施案例I
1)取稳定剂0.2％，抗氧剂0.2％研磨，过筛(40～120目，下同)；
2)取天然除虫菊素活性成分1％，将1)搅拌加入；
3)取NaY型分子筛3％放入烘箱，在200℃烘2hr，脱附，取出降至低温，粉碎过筛；
4)将2)搅拌加入3)中；
5)滑石粉95.6％放入烘箱中200℃烘2hr，脱水，取出降至低温，粉碎过筛；
6)将4)边搅拌边倒入5)中，混匀，过筛后分装密封，制得成品；
实施案例II
1)取稳定剂1％，抗氧剂1％研磨，过筛(40～120目，下同)；
2)取天然除虫菊素活性成分4％，将1)搅拌加入；
3)取NaY型分子筛12％放入烘箱，在200℃烘2hr，脱附，取出降至低温，粉碎过筛；
4)将2)搅拌加入3)中；
5)滑石粉82％放入烘箱中200℃烘2hr，脱水，取出降至低温，粉碎过筛；
6)将4)边搅拌边倒入5)中，混匀，过筛后分装密封，制得成品。
Claims (1)
1.一种缓释型天然除虫菊素驱蚊粉剂，其特征在于：它由天然除虫菊素为活性成分、以微孔分子筛(A型、X型、Y型)等为载体、抗氧剂、稳定剂、滑石粉组成，质量百分比组成为：天然除虫菊素活性成0.8％～4％，NaY型微孔分子筛3％～12％、滑石粉82％～95.6％、天然除虫菊素活性成分1％～4％、抗氧剂0.2％～1％、稳定剂0.2％～1％。；所述活性成分为天然除虫菊素提取物，所述抗氧剂为枸橼酸等多羧酸化合物；所述稳定剂为2，6-二叔丁基-4-甲基苯酚或2，5-二叔丁基对苯二酚。
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