CN106106495B - 一种噻虫胺壳聚糖微球及其制备方法和应用 - Google Patents

一种噻虫胺壳聚糖微球及其制备方法和应用 Download PDF

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CN106106495B
CN106106495B CN201610424540.1A CN201610424540A CN106106495B CN 106106495 B CN106106495 B CN 106106495B CN 201610424540 A CN201610424540 A CN 201610424540A CN 106106495 B CN106106495 B CN 106106495B
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clothianidin
chitosan
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陈福良
尹明明
顺布尔
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Institute of Plant Protection of Chinese Academy of Agricultural Sciences
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    • 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
    • A01N25/08—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 solids as carriers or diluents
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Abstract

本发明属于农药领域，具体涉及一种噻虫胺壳聚糖微球及其制备方法和应用。所述噻虫胺壳聚糖微球由噻虫胺和壳聚糖组成，其中噻虫胺的质量百分比为5.0％～20.0％，优选10.0％～15.0％。其制备方法为：将噻虫胺原药直接分散于壳聚糖的稀酸溶液中，在搅拌条件下，经过喷雾干燥机喷雾干燥，收集干燥后的粉末，得到所述噻虫胺壳聚糖微球。该噻虫胺壳聚糖微球可用于防治半翅目害虫、鳞翅目害虫、鞘翅目害虫。

Description

一种噻虫胺壳聚糖微球及其制备方法和应用
技术领域
本发明属于农药领域，具体涉及一种噻虫胺壳聚糖微球及其制备方法和应用。
背景技术
常规剂型农药喷雾的有效利用率仅为20％～30％，大多数农药有效成分流失到大气、土壤、水体等环境中，造成了环境的污染和资源的浪费。因此，开发出使用安全、环境友好、持效期长的农药新剂型是未来农药剂型的发展方向之一。
微球(Microspheres或Microbeads)是近年来发展起来的具缓释功能的农药新剂型，是以淀粉、壳聚糖、聚乳酸、明胶等高分子材料为载体制备的球状制剂。微球中的药物分散或包埋在材料中而形成均匀球状实体(实心球)，是一类均相分散体系，微球粒径大小一般0.3～300μm，其中，直径小于1μm的微球称为纳米微球(Nanospheres)或毫微球。常见的微球有以明胶、阿拉伯胶等天然高分子材料通过乳化交联制备的明胶微球、由淀粉水解再经乳化聚合等制备的淀粉微球、通过乳化-溶剂挥发法制备的聚酯类微球。微球所用的高分子载体材料一般均可生物降解，环境相容性友好；随着载体的降解，其有效成分可完全释放，农药利用率高。因此，微球制剂目前在农药中成为研究的热点，国外开发了二溴磷聚碳酸酯微球、舞毒蛾性诱素聚砜微球、涕灭威羧甲基纤维素微球、氟草敏乙基纤维素微球、啶虫脒聚乳酸/聚己内酯微球等。国内开发了阿维菌素聚乳酸微球、阿维菌素明胶微球、多杀菌素聚乳酸微球、毒死蜱聚乳酸微球等。
噻虫胺(clothianidin)是二代新烟碱类中的一种杀虫剂，由拜耳公司和日本Takeda武田公司共同开发，其作用与烟碱乙酰胆碱受体类似，具有触杀、胃毒和内吸活性，主要用于水稻、蔬菜、果树及其他作物上防治蚜虫、叶蝉、蓟马、飞虱等半翅目、鞘翅目、双翅目和某些鳞翅目类害虫，具有高效、广谱、用量少、毒性低、持效期长、对作物无药害、使用安全、与常规农药无交互抗性等优点，具有卓越的内吸和渗透作用。其结构新颖、特殊，性能与传统烟碱类杀虫剂相比更为优异，有可能成为世界性的大吨位型杀虫剂品种。
壳聚糖是甲壳素脱N-乙酰基的产物，N-乙酰基脱去55％以上的甲壳素称为壳聚糖，能溶解于稀酸中。壳聚糖工业品的N-脱乙酰度在70％以上。壳聚糖能被生物体内的溶菌酶降解生成天然的代谢物，具有无毒、能被生物体完全吸收的特点，因而具有良好的生物相容性和生物降解性，具有较强的生物粘附作用，使其作为微球载体具有独特的优势。
噻虫胺现有颗粒剂、悬浮剂和水分散粒剂等剂型获得农药登记。常规农药制剂为速效性，持效期短，需要多次施药，降低了农药的利用率，增加了农药施用量和劳动力成本。
发明内容
本发明的目的是提供一种噻虫胺壳聚糖微球。
所述噻虫胺壳聚糖微球由噻虫胺和壳聚糖组成，其中噻虫胺的质量百分比为5.0％～20.0％，优选10.0％～15.0％。
本发明的另一目的是提供所述噻虫胺壳聚糖微球的制备方法。
将噻虫胺原药直接分散于壳聚糖的稀酸溶液中，搅拌，并经过喷雾干燥，收集干燥后的粉末，得到所述噻虫胺壳聚糖微球。
搅拌条件为：转速500rpm，温度70℃，搅拌时间1h。
喷雾干燥的条件为：进风口温度110～140℃、出风口温度55～70℃、蠕动泵转速300～500mL/h。
所述稀酸为盐酸、甲酸、醋酸或磷酸，其体积浓度为0.5％～1％。
所述噻虫胺、稀酸、壳聚糖的用量之比为(1～2g)：(1～2mL)：(3～4g)
本发明还提供了所述噻虫胺壳聚糖微球在农业上的应用。
该噻虫胺壳聚糖微球的施用方法为拌土撒施或在植物根部施药；拌土撒施的施药量为150～300g a.i./hm2，植物根部施药的施药量为75～150g a.i./hm2。
施用对象为粮食作物、经济作物或果树作物。所述粮食作物包括水稻、小麦，所述经济作物包括甘蔗、茶叶，所述果树作物包括苹果、柑橘、梨、桃。
所述噻虫胺壳聚糖微球可防治的害虫包括半翅目害虫、鳞翅目害虫、鞘翅目害虫。
所述半翅目害虫包括稻飞虱、稻叶蝉、稻蓟马、桔黄蓟马、茶黄蓟马、小麦蚜虫、柑桔木虱、梨木虱、苹果绵蚜、桃蚜，鳞翅目害虫包括蔗螟、二化螟、桃潜蛾、橘潜蛾、茶细蛾，鞘翅目害虫包括稻负泥虫、黄曲条跳甲、茶条金龟、蔗龟。
本发明具有以下优点：本发明所述的噻虫胺壳聚糖微球为缓释型，持效期长，可减少施药次数，并提高农药的利用率，降低了农药施用量和劳动力成本；制备方法简便，条件温和，不需要有害的有机溶剂，对环境相容性好，尤其适合工业化生产。
具体实施方式
下面结合具体实施例对本发明做进一步的说明。
实施例1：10％噻虫胺壳聚糖微球的制备
称取6g壳聚糖溶于300mL 1％(V/V)盐酸溶液中，在加热的磁力搅拌器上搅拌溶解，待溶解后加入2g噻虫胺，搅拌成悬浮液。然后进入喷雾干燥机，在进风口140℃、出风口70℃、蠕动泵转速300mL/h下喷雾干燥，获得噻虫胺壳聚糖微球粉末。经高效液相色谱仪测定，噻虫胺壳聚糖微球的载药量为10.84％。经过激光粒度仪的检测，微球的粒径D50为6.73μm，跨度为2.63。
实施例2：15％噻虫胺壳聚糖微球的制备
称取4g壳聚糖溶于400mL 1％(V/V)甲酸溶液中，在磁力搅拌器上搅拌溶解，待溶解后加入1g噻虫胺，在70℃、500rpm下搅拌1h成溶液。然后进入喷雾干燥机，在进风口110℃、出风口55℃、蠕动泵转速300mL/h下喷雾干燥，获得噻虫胺壳聚糖微球粉末。经高效液相色谱仪测定，噻虫胺微球的载药量为15.82％，包埋率为81.1％。经过激光粒度仪的检测，微球的粒径D50为21.73μm，跨度为4.54。
实施例3：13.4％噻虫胺壳聚糖微球的制备
称取4g壳聚糖溶于400mL 0.5％(V/V)醋酸溶液中，在磁力搅拌器上搅拌溶解，待溶解后加入1g噻虫胺，在70℃、500rpm下搅拌1h。然后进入喷雾干燥机，在进风口130℃、出风口65℃、蠕动泵转速500mL/h下喷雾干燥，获得噻虫胺壳聚糖微球粉末。经高效液相色谱仪测定，噻虫胺微球的载药量为13.39％，包埋率为68.7％。经过激光粒度仪的检测，微球的粒径D50为25.03μm，跨度为4.79。
实施例4：11％噻虫胺壳聚糖微球的制备
称取4g壳聚糖溶于400mL 1％(V/V)磷酸溶液中，在加热的磁力搅拌器上搅拌溶解，待溶解后加入1g噻虫胺，在6000rpm高速乳化剪切机上剪切20min。然后进入喷雾干燥机，在进风口140℃、出风口70℃、蠕动泵转速500mL/h下喷雾干燥，获得噻虫胺壳聚糖微球粉末。经高效液相色谱仪测定，噻虫胺微球的载药量为11.42％。经过激光粒度仪的检测，微球的粒径D50为7.13μm，跨度为7.36。
本发明的噻虫胺壳聚糖微球及其制备方法已经通过具体的实施例进行了描述。本领域技术人员可以借鉴本发明的内容适当改变原料、工艺条件等来实现相应的其他目的，其相关改变都没有脱离本发明的内容，所有类似的替换和改动对于本领域技术人员来说是显而易见的，都被视为包括在本发明的范围之内。

Claims (6)

1.一种噻虫胺壳聚糖微球的制备方法，其特征在于，将噻虫胺原药直接分散于壳聚糖的稀酸溶液中，搅拌，并经过喷雾干燥，收集干燥后的粉末，得到所述噻虫胺壳聚糖微球；
所述稀酸为盐酸、甲酸、醋酸或磷酸，其体积浓度为0.5％～1％；
喷雾干燥的条件为：进风口温度110～140℃、出风口温度55～70℃、蠕动泵转速300～500mL/h；
所述噻虫胺、稀酸、壳聚糖的用量之比为(1～2g)：(1～2mL)：(3～4g)；
所述噻虫胺壳聚糖微球中噻虫胺的质量百分比为5.0％～20.0％。
2.根据权利要求1所述的制备方法，其特征在于，搅拌条件为：转速500rpm，温度70℃，搅拌时间1h。
3.根据权利要求1所述的制备方法，其特征在于，所述噻虫胺壳聚糖微球中噻虫胺的质量百分比为10.0％～15.0％。
4.权利要求1所述的噻虫胺壳聚糖微球在农业上的应用，其特征在于，施用方法为拌土撒施或在植物根部施药；拌土撒施的施药量为150～300g a.i./hm2，植物根部施药的施药量为75～150ga.i./hm2。
5.根据权利要求4所述的应用，其特征在于，施用对象为粮食作物、经济作物或果树作物。
6.根据权利要求4所述的应用，其特征在于，所述噻虫胺壳聚糖微球可防治的害虫包括半翅目害虫、鳞翅目害虫、鞘翅目害虫。
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