CN115517251A - 一种壳聚糖包封六甲螨酸的纳米杀螨剂及其制备方法 - Google Patents
一种壳聚糖包封六甲螨酸的纳米杀螨剂及其制备方法 Download PDFInfo
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Abstract
本发明涉及植物保护技术领域,公开了一种壳聚糖包封六甲螨酸的纳米杀螨剂及其制备方法,包括如下质量组份的原料:12.75份‑16.25份纯度2.53%纤维素纳米晶悬浮液、0.28份‑0.42份阿维菌素、0.33份‑0.42份纯度为98%盐酸多巴胺、4.55份‑16.25份丙酮、0.32份‑0.45份三羟甲基氨基甲烷、78.68份‑87.14份去离子水。本发明涉及生物基纳米缓释杀螨剂原料易得具有良好的农业生产与植物保护应用潜力,并且由于其简单的合成方法、绿色的合成原料以及优越的杀植食性叶螨和植物抗性诱导效果,具有较强的应用和推广价值。
Description
技术领域
本发明涉及植物保护技术领域,一种壳聚糖包封六甲螨酸的纳米杀螨剂及其制备方法。
背景技术
在追求高产的同时也需要健康绿色的食品,所以现在急需低毒高效的农药,研发高效绿色的农药很困难,植物源农药效果比较慢,化学农药的效果快,但是防治对象容易产生抗性,植食性叶螨是其中的典型代表之一。纳米技术的出现可以很好的缓解这一困境,我们可以尽可能的利用好每一滴农药,减少农药进入环境循环体系中的剂量。
植食性叶螨是我国乃至全世界分布广泛的一类极其严重的害螨。它可以为害世界各地的一百多种植物种类,其中包括几种重要的经济农业和园艺作物。由于其繁殖力强、繁殖时间短、地域有限、近交系率高、农药暴露可能性大,防治难度大。一些常见的杀螨剂如脱酚、环己素和氧化芬布他汀由于其高残留和耐药问题,在我国的应用一直受到限制或严格限制。现在迫切需要寻找新的杀螨剂。发现新型生物源农药是开发新型农药的重要途径之一。
天然生物活性就是各种生物在生命活动过程中所产生的各种化学物质。由于生物的种类非常繁多,在生物的进化过程中,每种生物都有发展自己特有的生物活动的体系,形成了生理和生化过程中的差异,由此产生出各种各样的天然物质。因此在天然物质里开发医药以及农药是创制新型药物的一种很重要的途径。我国自古代以来就利用各种药草治疗不同的疾病。鱼藤、烟草和除虫菊用作为杀虫剂也有好几百年的历史了。但是由于较早时期天然产物的相关基础学科的发展速度相对比较慢,这就使天然产物的开发及利用相对比较落后。在进入了21世纪以后,随着各种技术的不断快速发展像提取、分离分析技术等以及一系列比较先进的结构的鉴定技术的广泛应用,尤其是现代的分子生物学相关的技术迅速发展,这使得天然产物的研究以及开发重新成为现代农药与医药开发中成为特别受欢迎的热点。
纤维素((C6H10O5)n;n=10000~15000,其中n取决于纤维素原料)被定义为环状葡萄糖分子的长聚合物链,具有扁平带状构象。纤维素链羟基之间的复杂作用力而强有力的氢键网络可以纵向排列和横向稳定纤维素分子,使其成为高度有序的晶体结构。另一部分纤维素分子不能通过氢键横向稳定,会形成无定型的非晶结构,这些无序的非晶区域与有序的结晶区域相连,共同构成宏观上的纤维素纤维。纤维素纳米晶(celluosenanocrystals,CNC)是通过消除纤维素原纤维中非晶区域后保留结晶区域的一种棒状纳米结构的生物基材料,获取该材料的方式包含酸水解、超声、微波、离子液体等。其中,最常见和便捷的方法为酸水解制备CNC。在此过程中,酸分子向纤维素微纤维中的扩散,由于结晶区域比非晶区域堆叠更加紧密,所以酸优先导致纤维素原纤维的非晶区域中的分子链内的糖苷键断。因此,动力学导致非晶区和晶区的水解差异,导致纤维素链选择性断裂,而获得棒状结构的CNC。
聚多巴胺(PDA)是另一种受到广泛关注的高分子近红外吸收材料。作为广泛分布于人体的黑色素的重要组成成分,PDA在生物安全性方面具有明显优势。研究显示PDA并不干扰多种哺乳动物细胞的活性和增殖能力,即使在很高剂量下,也不会产生明显的细胞毒性。更重要的是,PDA已被证实在体内可完全降解,相比其它共轭聚合物具有更高的安全性。在光学性质方面,PDA具有与黑色素相似的光吸收性能,其在紫外光到可见光的范围内有宽波段的吸收,并且光吸收一直延伸近红外区域。
发明内容
本发明意在提供一种壳聚糖包封六甲螨酸的纳米杀螨剂及其制备方法,所提供的杀螨剂以克服现有技术中农药暴露可能性大,防治难度大的问题。
为了达到上述目的,本发明的基础方案如下:一种壳聚糖包封六甲螨酸的纳米杀螨剂,包括如下质量组份的原料:12.75份-16.25份纯度2.53%纤维素纳米晶悬浮液、0.28份-0.42份阿维菌素、0.33份-0.42份纯度为98%盐酸多巴胺、4.55份-16.25份丙酮、0.32份-0.45份三羟甲基氨基甲烷、78.68份-87.14份去离子水。
进一步,包括如下质量组份的原料:12.75份份浓度2.53%纤维素纳米晶悬浮液、0.28份阿维菌素、0.33份浓度为98%盐酸多巴胺、4.55份丙酮、0.32份三羟甲基氨基甲烷、78.68份去离子水。
进一步,包括如下质量组份的原料:16.25份浓度2.53%纤维素纳米晶悬浮液、0.42份阿维菌素、0.42份浓度为98%盐酸多巴胺、16.25份丙酮、0.45份三羟甲基氨基甲烷、87.14份去离子水。
进一步,包括如下质量组份的原料:14.5份浓度2.53%纤维素纳米晶悬浮液、0.35份阿维菌素、0.38份浓度为98%盐酸多巴胺、10.4份丙酮、0.39份三羟甲基氨基甲烷、82.91份去离子水。
进一步,阿维菌素纯度为98.5%,是一种源自阿维菌素链霉菌发酵产生的十六元大环内酯化合物。
进一步,纤维素纳米晶是从短绒棉提取的天然物质,纤维素纳米晶悬浮液为短绒棉经碱处理、酸处理、透析和离心所得。
进一步,杀螨剂pH<8.5。
进一步,应用于棉叶螨、朱砂叶螨、柑橘全爪螨或茶黄螨的防治药剂。
进一步,一种壳聚糖包封六甲螨酸的纳米杀螨剂的制备方法,包括以下步骤:用丙酮将阿维菌素溶解,将2.53%纤维素纳米晶悬浮液加入到阿维菌素溶液中,500rpm磁力搅拌1h,用Tris调节混合液的酸度,随后滴加用去离子水溶解的盐酸多巴胺,用Tris调节其酸度,500rpm磁力搅拌24h后静置24h。
本发明的原理及有益效果:1、本发明所用的原料纤维素纳米晶从短绒棉中提取,具有生物相容性、安全性、易降解性等优良性能;
2、本发明的有效成分阿维菌素是一种源自阿维菌素链霉菌发酵产生的十六元大环内酯化合物;其总用方式独特,在衍生合成方面也具有极大的可塑性,有望成为先导化合物开展系列化合物的后续研发;
3、本发明所用盐酸多巴胺溶解氧化后形成的聚多巴胺是一种红外吸收材料,具有良好的光吸收性能,对环境、生物友好;
4、本发明所形成的基于纤维素纳米晶和聚多巴胺的纳米缓释杀螨剂是基于天然活性物质配制的,具有绿色、安全、高效的特点。
附图说明
图1为本发明实施例中阿维菌素和纤维素纳米晶、聚多巴胺的释放曲线的示意图;
图2为本发明实施例中阿维菌素和纤维素纳米晶、聚多巴胺扫描电镜的示意图。
具体实施方式
下面通过具体实施方式进一步详细说明:
实施例1
本申请提供一种壳聚糖包封六甲螨酸的纳米杀螨,包括如下质量组份的原料:12.75份-16.25份纯度2.53%纤维素纳米晶悬浮液、0.28份-0.42份阿维菌素、0.33份-0.42份纯度为98%盐酸多巴胺、4.55份-16.25份丙酮、0.32份-0.45份三羟甲基氨基甲烷、78.68份-87.14份去离子水。
实施例2
一种壳聚糖包封六甲螨酸的纳米杀螨,包括如下质量组份的原料:包括如下质量组份的原料:12.75份份浓度2.53%纤维素纳米晶悬浮液、0.28份阿维菌素、0.33份浓度为98%盐酸多巴胺、4.55份丙酮、0.32份三羟甲基氨基甲烷、78.68份去离子水。
实施例3
一种壳聚糖包封六甲螨酸的纳米杀螨,包括如下质量组份的原料:16.25份浓度2.53%纤维素纳米晶悬浮液、0.42份阿维菌素、0.42份浓度为98%盐酸多巴胺、16.25份丙酮、0.45份三羟甲基氨基甲烷、87.14份去离子水。
实施例4
一种壳聚糖包封六甲螨酸的纳米杀螨,包括如下质量组份的原料:14.5份浓度2.53%纤维素纳米晶悬浮液、0.35份阿维菌素、0.38份浓度为98%盐酸多巴胺、10.4份丙酮、0.39份三羟甲基氨基甲烷、82.91份去离子水。
上述实施例1至实施例4中,阿维菌素纯度为98.5%,是一种源自阿维菌素链霉菌发酵产生的十六元大环内酯化合物。
阿维菌素的分子式为C49H74O14,分子量为887.11,熔点150℃-155℃,储存条件为室温,对眼睛、呼吸道和皮肤有一定的刺激作用,阿维菌素化学结构式如下:
本申请中2.53%纤维素纳米晶悬浮液具有生物和相容性、安全性、易降解性等优良性能,纤维素的结构式如下:
本实施例中,纤维素纳米晶的制备方法为:本申请所用的纤维素纳米晶(CNC)由棉短绒通过硫酸水解制备,具体步骤如下:
S1:将50g棉花加入2000mL的2wt%NaOH溶液中并通过机械搅拌在室温下搅拌12h,随后用蒸馏水反复冲洗,直到中性,放入鼓风烘箱中,干燥备用。
S2:取12.5g干燥后的棉短绒,加入250mL 64%v/v硫酸溶液中(冰水浴下,将126mL98%的H2SO4缓慢加入到124mL蒸馏水中),在45℃油浴下机械搅拌1h。
S3:待反应结束后,立即将反应液倒入800mL的冰水中,终止水解反应,用蒸馏水连续离心洗涤(4000rpm,5min),以除去多余的H2SO4,将悬浮液倒入透析袋中透析至中性(约5天),冷冻干燥得纤维素纳米晶粉末(CNC)。
一种壳聚糖包封六甲螨酸的纳米杀螨剂的制备方法,上述实施例1至实施例4任意一个实施例的质量组份的原料,包括如下步骤:在转速为500rpm的条件下,先在4g纤维素纳米晶悬浮液中加入10mg的阿维菌素搅拌1h后,滴加7mL1%盐酸多巴胺溶液,然后加入纯度为98的%Tris颗粒调节酸度再搅拌24h后形混合液。,然后静置24h后在12000rpm的转速下用高速离心机离心。
本申请中,将上述所制备的杀螨剂应用于棉叶螨、朱砂叶螨、柑橘全爪螨或茶黄螨的防治药剂。
按照如下实验进行测定:
收取适量的上清检测包覆率,用高效液相色谱仪检测得到六甲螨酸的包覆率为95.6%;阿维菌素和纤维素纳米晶通过简单粘结和氢键物理作用粘结在一起,聚多巴胺通过氢键作用对载有阿维菌素的纤维素纳米晶实现包封,在高速旋转的条件下形成较小的颗粒,增加了药物的包覆率。
如表1所示,六甲螨酸@壳聚糖对朱砂叶螨处理48h的LC50为0.011mg/mL,六甲螨酸的LC50值为0.083mg/mL,明显的降低了原药的用量。
表1六甲螨酸和壳聚糖对朱砂叶螨雌成螨的致死作用
如图1所示,在释放3天后已经达到释放率为69.5%,所以壳聚糖作为壁材时药物的释放比较容易,可以较快地控制害螨危害。
六甲螨酸壁材的选择:
表2六甲螨酸和壳聚糖的制备
表2可知六甲螨酸的适合壁材为壳聚糖,壳聚糖作为六甲螨酸的壁材的包覆率高于纤维素纳米晶悬浮液。
如图2所示,纳米六甲螨酸和壳聚糖的尺寸为25nm左右,大小比较均匀,且六甲螨酸和壳聚糖中的六甲螨酸易释放,可以达到快速控制害螨的效果。
本发明涉及生物基纳米缓释杀螨剂原料易得具有良好的农业生产与植物保护应用潜力,并且由于其简单的合成方法、绿色的合成原料以及优越的杀植食性叶螨和植物抗性诱导效果,具有较强的应用和推广价值。
以上所述的仅是本发明的实施例,方案中公知的具体结构和/或特性等常识在此未作过多描述。应当指出,对于本领域的技术人员来说,在不脱离本发明结构的前提下,还可以作出若干变形和改进,这些也应该视为本发明的保护范围,这些都不会影响本发明实施的效果和专利的实用性。本申请要求的保护范围应当以其权利要求的内容为准,说明书中的具体实施方式等记载可以用于解释权利要求的内容。
Claims (9)
1.一种壳聚糖包封六甲螨酸的纳米杀螨剂,其特征在于:包括如下质量组份的原料:12.75份-16.25份纯度2.53%纤维素纳米晶悬浮液、0.28份-0.42份阿维菌素、0.33份-0.42份纯度为98%盐酸多巴胺、4.55份-16.25份丙酮、0.32份-0.45份三羟甲基氨基甲烷、78.68份-87.14份去离子水。
2.根据权利要求1所述的壳聚糖包封六甲螨酸的纳米杀螨剂,其特征在于:包括如下质量组份的原料:12.75份份浓度2.53%纤维素纳米晶悬浮液、0.28份阿维菌素、0.33份浓度为98%盐酸多巴胺、4.55份丙酮、0.32份三羟甲基氨基甲烷、78.68份去离子水。
3.根据权利要求1所述的壳聚糖包封六甲螨酸的纳米杀螨剂,其特征在于:包括如下质量组份的原料:16.25份浓度2.53%纤维素纳米晶悬浮液、0.42份阿维菌素、0.42份浓度为98%盐酸多巴胺、16.25份丙酮、0.45份三羟甲基氨基甲烷、87.14份去离子水。
4.根据权利要求1所述的壳聚糖包封六甲螨酸的纳米杀螨剂,其特征在于:包括如下质量组份的原料:14.5份浓度2.53%纤维素纳米晶悬浮液、0.35份阿维菌素、0.38份浓度为98%盐酸多巴胺、10.4份丙酮、0.39份三羟甲基氨基甲烷、82.91份去离子水。
5.根据权利要求1~4任意一项所述的壳聚糖包封六甲螨酸的纳米杀螨剂,其特征在于:阿维菌素纯度为98.5%,是一种源自阿维菌素链霉菌发酵产生的十六元大环内酯化合物。
6.根据权利要求1~4任意一项所述的壳聚糖包封六甲螨酸的纳米杀螨剂,其特征在于:纤维素纳米晶是从短绒棉提取的天然物质,纤维素纳米晶悬浮液为短绒棉经碱处理、酸处理、透析和离心所得。
7.根据权利要求1~4任意一项所述的壳聚糖包封六甲螨酸的纳米杀螨剂及其制备方法,其特征在于:杀螨剂pH<8.5。
8.根据权利要求1~4任意一项所述的壳聚糖包封六甲螨酸的纳米杀螨剂,其特征在于,应用于棉叶螨、朱砂叶螨、柑橘全爪螨或茶黄螨的防治药剂。
9.一种壳聚糖包封六甲螨酸的纳米杀螨剂的制备方法,其特征在于:包括以下步骤:用丙酮将阿维菌素溶解,将2.53%纤维素纳米晶悬浮液加入到阿维菌素溶液中,500rpm磁力搅拌1h,用Tris调节混合液的酸度,随后滴加用去离子水溶解的盐酸多巴胺,用Tris调节其酸度,500rpm磁力搅拌24h后静置24h。
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