CN115443994A - 用于不可移动文物生物病害防治的载药埃洛石纳米管缓释复合物的制备方法 - Google Patents
用于不可移动文物生物病害防治的载药埃洛石纳米管缓释复合物的制备方法 Download PDFInfo
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Abstract
本发明属公开了一种用于不可移动文物生物病害防治的载药埃洛石纳米管缓释复合物的制备方法。本发明采用真空负载法,通过减压去除埃洛石纳米管内的空气,实现了天然抑菌剂的高量负载。通过将天然抑菌剂负载在埃洛石纳米管内后,可以掩盖天然抑菌剂的颜色气味,减少其挥发,增加其水溶性和稳定性,并减缓天然抑菌剂的释放,使其可以用于户外不可移动文物的保护与修复。通过热脱水处理,能偶消除埃洛石纳米管的层间水,可以在维持其管状结构的同时,扩大管腔容积,增加载药量。酸刻蚀处理后的埃洛石纳米管的比表面积和孔隙率增加,且其表面含有活性羟基,因此可以负载更多内容物,进一步提高其载药量。
Description
技术领域
本发明属于药物缓释材料及文物保护领域,具体涉及一种用于不可移动文物生物病害防治的载药埃洛石纳米管缓释复合物的制备方法。
背景技术
不可移动文物是先民在历史、文化、建筑、艺术上的具体遗产或遗址。包含古建筑物、传统聚落、古市街,考古遗址及其他历史文化遗迹等。暴露在户外的不可移动文物易受温度、湿度、降水、大气污染和生物等环境气候因素影响,造成文化遗产的劣化。其中生物病害是造成不可移动文物劣化的主要因素。对于户外不可移动文物生物病害的长效防控是目前不可移动文物保护中面临的重要难题。
传统化学抑菌剂被广泛用于去除文物表面定殖的有害微生物,但是这些化学抑菌剂不仅会对人类健康和环境造成风险,而且存在干扰文物本体的潜在可能。随着使用化学抑菌剂问题的日益突出,利用天然物质抑菌的方法在文化遗产保护领域得到越来越多的关注。特别是植物精油(Essential Oils)及其活性抑菌物质,这些物质通常被认为是安全且环保的绿色抑菌剂。但是,这些天然抑菌剂的颜色气味、高挥发性、难溶于水以及对氧、光、热的敏感性使得它们难以用于户外不可移动文物的保护与修复。
埃洛石纳米管(Halloysite Nanotubes)具有独特的中空纳米管状结构,是一种优秀的纳米载体材料。埃洛石的纳米官腔能够用于装载多种生物或化学分子,进而对其进行保护和控制缓慢释放。与其他纳米材料相比,埃洛石纳米管作为释放载体的优势在于其独特的管状纳米结构、来源广泛、价格低廉,是一种天然缓释材料,其缓释效果好,加之其环境和生物毒性很低,是安全的纳米材料,使用过程不会对环境和生物带来潜在危害。但是,如何进一步提高埃洛石纳米管的载药量是一个亟待解决的问题。
综上所述,本发明存在如下技术问题:
(1)天然抗菌剂(如植物精油及其活性抑菌物质)作为一种安全且环保的绿色抑菌剂在文化遗产保护领域得到越来越多的关注,但是由于其颜色气味、高挥发性、难溶于水以及对氧、光、热的敏感性使得它们难以直接用于户外不可移动文物的保护与修复。
(2)埃洛石纳米管作为良好的药物缓释载体,具有独特中空管状纳米结构、来源广泛、价格低廉,环境和生物毒性很低等优点,但是较低的载药量制约了其进一步的开发利用。
发明内容
本发明提供了一种操作简单,成本低的用于不可移动文物生物病害防治的载药埃洛石纳米管缓释复合物的制备方法,旨在用于户外不可移动文物的生物病害长效防治。
本发明的技术方案如下:
本发明公开了一种用于不可移动文物生物病害防治的载药埃洛石纳米管缓释复合物的制备方法,包括以下步骤:
1)埃洛石纳米管热处理
将购得的埃洛石纳米管进行加热脱水处理;
2)埃洛石纳米管酸刻蚀扩容
将加热脱水处理后的埃洛石纳米管与盐酸溶液加热回流,增加其比表面积和孔隙率;
3)天然抑菌剂负载
将步骤2)中处理后的埃洛石纳米管与天然抗菌剂溶液搅拌过夜,超声混匀,真空负载,清洗干燥后得到载药埃洛石纳米管。
作为进一步地改进,本发明所述的步骤1)中,加热脱水处理在马弗炉中进行,加热温度为300-500℃,加热时间为3-8小时。
作为进一步地改进,本发明所述的步骤2)中,盐酸溶液浓度为1-5M,每克埃洛石纳米管加入20-50mL盐酸溶液,加热回流温度为80-100℃,加热时间为8-12小时。
作为进一步地改进,本发明所述的步骤3)中,真空负载步骤为将埃洛石纳米管与天然抗菌剂溶液的混合物放置在真空干燥箱内,先减压至-0.08-0.1MPa,持续30-60分钟,然后恢复至常压,持续10-30分钟,该过程反复操作3-5次。
作为进一步地改进,本发明所述的步骤3)中,天然抑菌剂为肉桂醛或百里香酚或丁香酚。
本发明的有益效果如下:
(1)采用真空负载法,通过减压去除埃洛石纳米管内的空气,实现了天然抑菌剂的高量负载。通过将天然抑菌剂负载在埃洛石纳米管内后,可以掩盖天然抑菌剂的颜色气味,减少其挥发,增加其水溶性和稳定性,并减缓天然抑菌剂的释放,使其可以用于户外不可移动文物的保护与修复。
(2)通过热脱水处理,能偶消除埃洛石纳米管的层间水,可以在维持其管状结构的同时,扩大管腔容积,增加载药量。
(3)酸刻蚀处理后的埃洛石纳米管的比表面积和孔隙率增加,且其表面含有活性羟基,因此可以负载更多内容物,进一步提高其载药量。
附图说明
图1为实施例1得到的负载肉桂醛的埃洛石纳米管的扫描电镜图;
图2为实施例1得到的负载肉桂醛的埃洛石纳米管的透射电镜图;
图3为实施例1得到的负载肉桂醛的埃洛石纳米管的缓释曲线图。
具体实施方式
下面结合说明书附图通过具体实施例对本发明进行详细说明:
实施例1.
(1)埃洛石纳米管的热处理,称取10g埃洛石纳米管粉末,置于石英坩埚中,在马弗炉中程序升温加热到300℃,经过3h加热后,冷却后得到热处理后的埃洛石纳米管。
(2)埃洛石纳米管酸刻蚀扩容,取5g经热处理后的埃洛石纳米管,置于250mL圆底烧瓶中,随后加入80mL预先配置的4M盐酸溶液,搅拌均匀后,超声10min,移至油浴锅中,温度设定为80℃,转速800rpm,加热回流8h。待酸刻蚀反应结束后,将悬浮液冷却后离心,并洗涤至中性,烘干后研磨成粉末,得到酸刻蚀扩容后的埃洛石纳米管。
(3)肉桂醛的真空负载,将2g酸刻蚀扩容后的埃洛石纳米管加入到20mL的肉桂醛溶液中,室温下搅拌过夜,超声分散,随后置于真空干燥箱中,开启真空泵抽至真空度为0.1MPa,然后关闭真空阀门,保持真空状态30min,打开真空阀门,与大气相通,使肉桂醛进入埃洛石纳米管腔内,整个抽/放真空过程重复3次。将所得悬浮液离心,用乙醇和水洗去表面吸附的多余肉桂醛,真空干燥后研磨成粉末,即得负载肉桂醛的埃洛石纳米管。
(4)负载肉桂醛的埃洛石纳米管的形貌表征,取负载肉桂醛的埃洛石纳米管样品5mg,加入5mL去离子水,配置成浓度为1mg/mL的悬浮液,超声分散5min后,用铜网在悬浮液中捞取三次,随后将铜网在烘箱60℃烘干后,借助透射电镜进行观察,拍照。使用塑料滴管将悬浮液滴加在锡箔纸上,在烘箱60℃烘干后,裁剪成合适大小,粘贴在导电胶上,喷金处理后通过扫描电镜进行观察,拍照。
其扫描电镜图参见图1。可以看出负载肉桂醛的埃洛石纳米管呈现典型的细长棒状结构。其长度约为2μm,直径约为50nm。
其透射电镜图参见图2。可以看出负载肉桂醛的埃洛石纳米管是中空的管状结构,管径约为40nm。
(5)负载肉桂醛的埃洛石纳米管的缓释性能测试,称取负载肉桂醛的埃洛石纳米管样品10mg,放入透析管中(截留分子量为3500Da),在透析管外侧加入10mLPBS缓冲溶液,随后置于摇床上震荡。每过一段时间,取定量的释放液,稀释后通过紫外分光光度计测定其吸光度,根据标准曲线计算浓度,并补充等量的缓冲液。
其肉桂醛释放曲线参见图3。可以看出负载肉桂醛的埃洛石纳米管在前期表现为快速释放,在第3天释放量达到54.78%后,释放速率开始变缓慢,符合药物扩散规律,具有缓释效果。
实施例2.
(1)埃洛石纳米管的热处理,称取10g埃洛石纳米管粉末,置于石英坩埚中,在马弗炉中程序升温加热到300℃,经过3h加热后,冷却后得到热处理后的埃洛石纳米管。
(2)埃洛石纳米管酸刻蚀扩容,取5g经热处理后的埃洛石纳米管,置于250mL圆底烧瓶中,随后加入80mL预先配置的4M盐酸溶液,搅拌均匀后,超声10min,移至油浴锅中,温度设定为80℃,转速800rpm,加热回流8h。待酸刻蚀反应结束后,将悬浮液冷却后离心,并洗涤至中性,烘干后研磨成粉末,得到酸刻蚀扩容后的埃洛石纳米管。
(3)百里香酚的真空负载,将2g酸刻蚀扩容后的埃洛石纳米管加入到20mL百里香酚的乙醇溶液(10g百里香酚溶于20mL乙醇溶液中),室温下搅拌过夜,超声分散,随后置于真空干燥箱中,开启真空泵抽至真空度为0.1MPa,然后关闭真空阀门,保持真空状态30min,打开真空阀门,与大气相通,使百里香酚进入埃洛石纳米管腔内,整个抽/放真空过程重复3次。将所得悬浮液离心,用乙醇和水洗去表面吸附的多余百里香酚,真空干燥后研磨成粉末,即得负载百里香酚的埃洛石纳米管。
(4)负载百里香酚的埃洛石纳米管的形貌表征,取负载百里香酚的埃洛石纳米管样品5mg,加入5mL去离子水,配置成浓度为1mg/mL的悬浮液,超声分散5min后,用铜网在悬浮液中捞取三次,随后将铜网在烘箱60℃烘干后,借助透射电镜进行观察,拍照。
(5)负载百里香酚的埃洛石纳米管的缓释性能测试,称取负载百里香酚的埃洛石纳米管样品10mg,放入透析管中(截留分子量为3500Da),在透析管外侧加入10mLPBS缓冲溶液,随后置于摇床上震荡。每过一段时间,取定量的释放液,稀释后通过紫外分光光度计测定其吸光度,根据标准曲线计算浓度,并补充等量的缓冲液。
实施例3.
(1)埃洛石纳米管的热处理,称取10g埃洛石纳米管粉末,置于石英坩埚中,在马弗炉中程序升温加热到300℃,经过3h加热后,冷却后得到热处理后的埃洛石纳米管。
(2)埃洛石纳米管酸刻蚀扩容,取5g经热处理后的埃洛石纳米管,置于250mL圆底烧瓶中,随后加入80mL预先配置的4M盐酸溶液,搅拌均匀后,超声10min,移至油浴锅中,温度设定为80℃,转速800rpm,加热回流8h。待酸刻蚀反应结束后,将悬浮液冷却后离心,并洗涤至中性,烘干后研磨成粉末,得到酸刻蚀扩容后的埃洛石纳米管。
(3)丁香酚的真空负载,将2g酸刻蚀扩容后的埃洛石纳米管加入到20mL的丁香酚溶液中,室温下搅拌过夜,超声分散,随后置于真空干燥箱中,开启真空泵抽至真空度为0.1MPa,然后关闭真空阀门,保持真空状态30min,打开真空阀门,与大气相通,使丁香酚进入埃洛石纳米管腔内,整个抽/放真空过程重复3次。将所得悬浮液离心,用乙醇和水洗去表面吸附的多余丁香酚,真空干燥后研磨成粉末,即得负载丁香酚的埃洛石纳米管。
(4)负载丁香酚的埃洛石纳米管的形貌表征,取负载丁香酚的埃洛石纳米管样品5mg,加入5mL去离子水,配置成浓度为1mg/mL的悬浮液,超声分散5min后,用铜网在悬浮液中捞取三次,随后将铜网在烘箱60℃烘干后,借助透射电镜进行观察,拍照。
(5)负载丁香酚的埃洛石纳米管的缓释性能测试,称取负载丁香酚的埃洛石纳米管样品10mg,放入透析管中(截留分子量为3500Da),在透析管外侧加入10mLPBS缓冲溶液,随后置于摇床上震荡。每过一段时间,取定量的释放液,稀释后通过紫外分光光度计测定其吸光度,根据标准曲线计算浓度,并补充等量的缓冲液。
以上所述仅为本发明的优选实施例,并不用于限制本发明,在不脱离所附权利要求书所限定的本发明的精神和范围内,在形式上和细节上可以对本发明做出各种更改,均应该为本发明的保护范围。
Claims (5)
1.一种用于不可移动文物生物病害防治的载药埃洛石纳米管缓释复合物的制备方法,其特征在于,包括以下步骤:
1)埃洛石纳米管热处理
将购得的埃洛石纳米管进行加热脱水处理;
2)埃洛石纳米管酸刻蚀扩容
将加热脱水处理后的埃洛石纳米管与盐酸溶液加热回流,增加其比表面积和孔隙率;
3)天然抑菌剂负载
将步骤2)中处理后的埃洛石纳米管与天然抗菌剂溶液搅拌过夜,超声混匀,真空负载,清洗干燥后得到载药埃洛石纳米管。
2.根据权利要求1所述的用于不可移动文物生物病害防治的载药埃洛石纳米管缓释复合物的制备方法,其特征在于,所述的步骤1)中,加热脱水处理在马弗炉中进行,加热温度为300-500℃,加热时间为3-8小时。
3.根据权利要求1所述的用于不可移动文物生物病害防治的载药埃洛石纳米管缓释复合物的制备方法,其特征在于,所述的步骤2)中,所述的盐酸溶液浓度为1-5M,每克埃洛石纳米管加入20-50mL盐酸溶液,加热回流温度为80-100℃,加热时间为8-12小时。
4.根据权利要求1所述的用于不可移动文物生物病害防治的载药埃洛石纳米管缓释复合物的制备方法,其特征在于,所述的步骤3)中,所述的真空负载步骤为将埃洛石纳米管与天然抗菌剂溶液的混合物放置在真空干燥箱内,先减压至-0.08-0.1MPa,持续30-60分钟,然后恢复至常压,持续10-30分钟,该过程反复操作3-5次。
5.根据权利要求1所述的用于不可移动文物生物病害防治的载药埃洛石纳米管缓释复合物的制备方法,其特征在于,所述的步骤3)中,所述天然抑菌剂为肉桂醛或百里香酚或丁香酚。
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