CN111803696A - 一种用于皮肤创伤修复的广藿香油纳米复合膜的制备方法 - Google Patents
一种用于皮肤创伤修复的广藿香油纳米复合膜的制备方法 Download PDFInfo
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- CN111803696A CN111803696A CN202010660723.XA CN202010660723A CN111803696A CN 111803696 A CN111803696 A CN 111803696A CN 202010660723 A CN202010660723 A CN 202010660723A CN 111803696 A CN111803696 A CN 111803696A
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- patchouli oil
- mesoporous silicon
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- wound repair
- skin wound
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Abstract
本发明公开了一种用于皮肤创伤修复的广藿香油纳米复合膜的制备方法,通过利用超临界CO2循环渗透法,首先将广藿香油载入到介孔硅纳米粒中获得高载药量的广藿香油‑介孔硅纳米颗粒,再加入到以壳聚糖和聚乙烯醇混合后的膜基质中,经高速磁力搅拌混合、涂布、冷冻干燥而制得广藿香油纳米复合膜,可实现广藿香油的高效载入和长效缓释,达到长效抗菌抗炎的效果,同时该广藿香油纳米复合膜具有良好的拉伸强度、柔软度和保湿性能,可作为良好的皮肤敷料进行使用。此外,本发明在制备过程中也可实现CO2和未负载广藿香油的回收循环利用,提高利用率。
Description
技术领域
本发明涉及天然产物药剂学和材料工程技术领域,尤其涉及一种用于皮肤创伤修复的广藿香油纳米复合膜的制备方法。
背景技术
每年世界上都有大量患者由于皮肤创伤类疾病而受到危害,包括烧伤、溃烂、细菌感染或其他相关疾病,这些疾病通常都需要漫长的恢复过程。皮肤敷料的发展可以有效促进皮肤创伤的治疗,然而如何避免恢复过程中细菌的感染仍然是该类疾病治疗面临的巨大挑战。因此,在常规纱布及脱脂棉使用的基础上,开发出其他形式的抗菌抗炎型皮肤修复材料具有重大的意义。
研究表明,理想的伤口敷料通常应具备以下的基本性能:(1)无毒、生物相容性良好,不会对病人造成过敏反应;(2)提供物理屏障,保护伤口免受外来伤害,防止细菌、微生物等入侵伤口,以免伤口感染发炎;(3)良好的吸水性,能够有效的吸收伤口渗出的体液分泌物;(4)保湿性,伤口在湿润环境下愈合速度比直接接触空气的干燥伤口快1倍;(5)良好的透气性,为伤口创造疏松透气的环境,有利于伤口处细胞进行有氧呼吸,避免伤口处形成无氧环境而导致厌氧菌在该处生长繁殖;(6)适度的贴合性,贴合性太强容易粘连新生组织,使得更换敷料时新生组织损伤,造成二次伤害,而贴合性太弱则敷料容易脱落,带来不舒适感;(7)易于观察伤口愈合情况,不需要频繁揭开或者敷料;(8)易于制备成不同形状和大小的敷料,可根据伤口具体情况调整敷料,操作简便,容易储存;(9)力学性能稳定;(10)易于消毒。
天然高分子材料具有良好的生物相容性和可降解性,可有效应用于皮肤修复材料的构建。同时,进一步将不同天然高分子材料复合使用,可有效改善敷料的力学性能和保湿性能。在敷料中加入抗菌药物,如抗生素可改善其抗菌性能,但如何保持敷料的长效抗菌功能,降低敷料的更换频率,从而减轻患者痛苦,仍然是皮肤疾病治疗的重要课题。同时要注意的是,抗生素的大量或不当使用,容易导致耐药菌的出现,增加治疗难度。
中药提取物具有安全性高、不易产生耐药性、无副作用或不良反应小等特点,被越来越多地应用于各个领域发挥其抗菌、抗病毒等功效。其中,精油类物质具有独特的易挥发特性,可包裹于材料中通过释放发挥其活性功效。但也由于其易挥发性,通常释放迅速,不易实现长时间的抗菌抗炎的效果。
广藿香油是从广藿香中提取的精油,其易挥发、气味具有刺激性,具有多种药理活性,包括抗菌、抗病毒、抗炎、抗肿瘤作用,还有增强记忆、改善胃肠功能、抗癌、防腐等作用。广藿香油的广藿香醇、广藿香酮被认为是抗菌、抗炎的主要成分,具有良好的广谱抗菌性。将广藿香油和天然高分子材料相结合,制备成薄膜型皮肤修复材料,具有良好的临床应用价值,而目前尚未有相关报道。此外,结合广藿香油和天然高分子材料制备薄膜型皮肤修复材料,主要存在以下难点:(1)如何使材料的抗炎抗菌性能保持长期有效?(2)如何使材料具有良好的力学性能和保湿性能,满足其作为皮肤敷料使用的要求?
发明内容
为解决上述难点和问题,本发明提供一种用于皮肤创伤修复的广藿香油纳米复合膜的制备方法,通过利用超临界CO2循环渗透法,首先将广藿香油载入到介孔硅纳米粒中获得高载药量的广藿香油-介孔硅纳米颗粒,再加入到以壳聚糖和聚乙烯醇混合后的膜基质中,制备了一种广藿香油纳米复合膜,可实现广藿香油的长效缓释,达到长效抗菌抗炎的效果,同时该广藿香油纳米复合膜具有良好的拉伸强度、柔软度和保湿性能,可作为良好的皮肤敷料进行使用。
为了实现上述目的,本发明采用了如下技术方案:
一种用于皮肤创伤修复的广藿香油纳米复合膜的制备方法,包括以下制备步骤:
S1、采用超临界CO2循环渗透技术制备广藿香油-介孔硅纳米颗粒
S11、将介孔硅纳米粒放入高压釜中后密闭,通过喷嘴A注入广藿香油;
S12、然后通过喷嘴B通入CO2使压力上升达到预设压力,同时升温至预设温度,开始超临界态下的广藿香油渗透载入过程;
S13、待系统达到平衡后,通过降温、泄压操作使系统脱离超临界态,广藿香油负载于介孔硅纳米粒中,同时回收CO2及未负载的广藿香油;
S14、重复以上步骤S11~S13操作过程3~4次,即得到高载药量的广藿香油-介孔硅纳米颗粒;
S2、广藿香油纳米复合膜的制备
S21、分别配制1%~4%的壳聚糖溶液和8%~12%的聚乙烯醇溶液,然后将两者以一定溶液质量比的比例进行混合,得到混合液;
S22、向混合液中加入一定比例的步骤S1所制得的广藿香油-介孔硅纳米颗粒,并以高速磁力搅拌混合均匀得到胶状悬浮液;
S23、将步骤S22所得的胶状悬浮液在聚四氟乙烯模具中涂布展开呈薄膜状,并冷冻干燥,即得到广藿香油纳米复合膜。
优选的,在步骤S12中,所述预设压力为18~35MPa,所述预设温度为35~50℃。在此温度和压力条件下,能够提高广藿香油的负载量。
优选的,在步骤S11和步骤S12中,所述喷嘴A和所述喷嘴B为同轴式喷嘴或两个并行独立的喷嘴。如此,便于广藿香油在超临界态下进行高效地负载于介孔硅纳米粒中。
优选的,在步骤S13中,降温操作为通过冷凝水降温釜体温度至20℃以下,冷凝水温为2~6℃;泄压操作为压力降至常压。
优选的,在步骤S21中,壳聚糖溶液和聚乙烯醇溶液的比例为6:4~8:2。如此,能够提高所制得的广藿香油纳米复合膜的性能,使其具备良好的拉伸强度、柔软度和保湿性能。
优选的,在步骤S22中,加入的广藿香油-介孔硅纳米颗粒的比例为0.5%~3.0%。通过加入合适比例的广藿香油-介孔硅纳米颗粒,使得广藿香油纳米复合膜能够实现广藿香油的长效缓释,达到长效抗菌抗炎的效果。
优选的,在步骤S22中,高速磁力搅拌过程的搅拌速度为600rpm,搅拌时间为20min。如此,能够使广藿香油-介孔硅纳米颗粒充分分散在膜基质中,保证广藿香油纳米复合膜具有最佳的性能。
优选的,在步骤S23中,冷冻干燥的条件是:冷冻温度为-35℃,抽真空12h,冻干48h。如此,所制得的广藿香油纳米复合膜的物理性能更佳。
优选的,在步骤S11中,所述介孔硅纳米粒为MCM-41型纳米球形介孔结构,粒径在100nm以下。如此,广藿香油可以大量负载在介孔硅纳米粒中,具备高载药量的效果,且广藿香油能够长时间缓慢释放挥发。
优选的,所述介孔硅纳米粒的制备方法为:将3g十六烷基三甲基溴化铵加入到60mL的去离子水中,95℃水浴,于350r/min搅拌完全溶解后加入120μL二乙醇胺,混匀后45分钟内加入4.5mL正硅酸四乙酯,继续反应1h,静置放冷得到淡蓝色乳状液;加入甲醇稀释并进行离心,之后浸泡在60℃的乙醇/浓硫酸体系反应24h,再加入去离子水多次离心至溶液为中性,得到介孔硅材料;最后用乙醇冲洗介孔硅材料,在烘箱中55℃干燥6h后得到干燥的介孔硅纳米粒产物,收集备用。
与现有技术相比,本发明提供了一种用于皮肤创伤修复的广藿香油纳米复合膜的制备方法,具备以下有益效果:
本发明通过利用超临界CO2循环渗透法,首先将广藿香油载入到介孔硅纳米粒中获得高载药量的广藿香油-介孔硅纳米颗粒,再加入到以壳聚糖和聚乙烯醇混合后的膜基质中,制备了一种广藿香油纳米复合膜,可实现广藿香油的高效载入和长效缓释,达到长效抗菌抗炎的效果,同时该广藿香油纳米复合膜具有良好的拉伸强度、柔软度和保湿性能,可作为良好的皮肤敷料进行使用。此外,本发明在制备过程中也可实现CO2和未负载广藿香油的回收循环利用,提高利用率。
经检测,通过本发明制备方法所得广藿香油-介孔硅纳米粒颗粒的载药量>32%,由该广藿香油-介孔硅纳米粒颗粒进一步所制得的广藿香油纳米复合膜的吸湿增重可达到3~6倍,且在30min内迅速膨胀然后缓慢达到饱和;拉伸强度>0.1MPa,伸长率>50%;广藿香油纳米复合膜中广藿香油可在5天内持续少量释放,并保持显著的抗菌效果,且在产生抗菌效果的浓度下对皮肤细胞无毒性作用。
具体实施方式
下面将对本发明的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明的一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
下面通过详细的实施例对本发明作进一步详细描述。
本发明所用的广藿香油由江西安邦药业有限公司提供,药品级,符合药典标准。
介孔硅纳米粒的制备方法为:将3g十六烷基三甲基溴化铵(CTAB)加入到60mL的去离子水中,95℃水浴,于350r/min搅拌使其完全溶解后加入120μL二乙醇胺(DEA),混匀后45分钟内以少量多次的方式慢慢加入4.5mL正硅酸四乙酯(TEOS),继续反应1h,静置放冷得到淡蓝色乳状液;接着,按照甲醇:去离子水=2:1的比例加入甲醇稀释并进行离心1次,再加入去离子水继续离心多次至表面活性剂基本除尽;之后将其浸泡在60℃的乙醇/浓硫酸体系(8/1,v/v)反应24h,除去表面活性剂模板,再加入去离子水多次离心至溶液为中性,得到介孔硅材料;最后用乙醇冲洗介孔硅材料以去除游离的CTAB并替换掉介孔硅材料孔道里面的水分,在烘箱中55℃干燥6h后得到干燥的介孔硅纳米粒(MSNs)产物,收集备用。
实施例1
本实施例提供了一种用于皮肤创伤修复的广藿香油纳米复合膜的制备方法,包括以下制备步骤:
(S1)采用超临界CO2循环渗透技术制备广藿香油-介孔硅纳米颗粒
S11、首先,将200mg直径在80nm左右的介孔硅纳米粒(MCM-41介孔硅)放入高压釜中后密闭,通过喷嘴A注入2mL广藿香油;
S12、然后通过喷嘴B通入CO2使压力上升达到18MPa,同时升温至40℃,开始超临界态下的广藿香油渗透载入介孔硅纳米粒的过程;
S13、待系统达到平衡后(即保持超临界约1小时后,在介孔硅纳米粒内外的广藿香油的浓度达到平衡),通过釜体冷凝水系统降温釜体温度至18℃,冷凝水温为2~6℃,使系统脱离超临界态,之后缓慢排出CO2进行泄压至常压,使广藿香油负载于介孔硅纳米粒(MCM-41介孔硅)之中,同时回收CO2及未负载的广藿香油;
S14、重复以上步骤S11~S13操作过程4次,开釜收集载有广藿香油的纳米药物固态粉体,即得到高载药量的广藿香油-介孔硅纳米颗粒产物241.3mg,所得产物的载药量达到34.2%(wt%);
(S2)广藿香油纳米复合膜的制备
S21、分别配制2%(w/v)的壳聚糖溶液和10%(w/v)的聚乙烯醇(PVA)溶液,然后将两者以7:3的比例进行混合,得到混合液;
S22、向混合液中加入0.5%(w/w)的步骤S1所制得的广藿香油-介孔硅纳米颗粒,并以高速磁力搅拌混合均匀得到胶状悬浮液;高速磁力搅拌过程的搅拌速度为600rpm,搅拌时间为20min。
S23、将步骤S22所得的胶状悬浮液在聚四氟乙烯模具中涂布展开呈薄膜状,并冷冻干燥,即得到广藿香油纳米复合膜。其中,聚四氟乙烯模具为100x100mm平板,边缘有挡隔。在涂布时,将12mL胶状悬浮液倒入聚四氟乙烯模具中以刮板均匀分布为薄膜状。冷冻干燥的条件是:冷冻温度为-35℃,抽真空12h,冻干48h。
经测试,所得的广藿香油纳米复合膜吸湿30min后重量为未吸湿前的3.98倍;抗拉强度为0.142MPa,伸长率为81.0%;置于水中24h后广藿香油释放率为15.6%,120h后释放率为58.2%;将广藿香油纳米复合膜置于1.5×103cfu/mL的金黄色葡萄球菌培养液中48h后,抑菌率100%,120h后抑菌率99.1%。
实施例2
本实施例提供了一种用于皮肤创伤修复的广藿香油纳米复合膜的制备方法,包括以下制备步骤:
(S1)采用超临界CO2循环渗透技术制备广藿香油-介孔硅纳米颗粒
S11、首先,将200mg直径在80nm左右的介孔硅纳米粒(MCM-41介孔硅)放入高压釜中后密闭,通过喷嘴A注入2mL广藿香油;
S12、然后通过喷嘴B通入CO2使压力上升达到25MPa,同时升温至45℃,开始超临界态下的广藿香油渗透载入介孔硅纳米粒的过程;
S13、待系统达到平衡后(即保持超临界约1小时后,在介孔硅纳米粒内外的广藿香油的浓度达到平衡),通过釜体冷凝水系统降温釜体温度至18℃,冷凝水温为2~6℃,使系统脱离超临界态,之后缓慢排出CO2进行泄压至常压,使广藿香油负载于介孔硅纳米粒(MCM-41介孔硅)之中,同时回收CO2及未负载的广藿香油;
S14、重复以上步骤S11~S13操作过程4次,开釜收集载有广藿香油的纳米药物固态粉体,即得到高载药量的广藿香油-介孔硅纳米颗粒产物242.1mg,所得产物的载药量达到35.3%(wt%);
(S2)广藿香油纳米复合膜的制备
S21、分别配制2%(w/v)的壳聚糖溶液和10%(w/v)的聚乙烯醇(PVA)溶液,然后将两者以6:4的比例进行混合,得到混合液;
S22、向混合液中加入1.0%(w/w)的步骤S1所制得的广藿香油-介孔硅纳米颗粒,并以高速磁力搅拌混合均匀得到胶状悬浮液;高速磁力搅拌过程的搅拌速度为600rpm,搅拌时间为20min。
S23、将步骤S22所得的胶状悬浮液在聚四氟乙烯模具中涂布展开呈薄膜状,并冷冻干燥,即得到广藿香油纳米复合膜。其中,聚四氟乙烯模具为100x100mm平板,边缘有挡隔。在涂布时,将12mL胶状悬浮液倒入聚四氟乙烯模具中以刮板均匀分布为薄膜状。冷冻干燥的条件是:冷冻温度为-35℃,抽真空12h,冻干48h。
经测试,所得的广藿香油纳米复合膜吸湿30min后重量为未吸湿前的6.24倍;抗拉强度为0.131MPa,伸长率为76.3%;置于水中24h后广藿香油释放率为17.8%,120h后释放率为66.5%;将广藿香油纳米复合膜置于1.5×103cfu/mL的金黄色葡萄球菌培养液中48h后,抑菌率100%,120h后抑菌率99.7%。
实施例3
本实施例提供了一种用于皮肤创伤修复的广藿香油纳米复合膜的制备方法,包括以下制备步骤:
(S1)采用超临界CO2循环渗透技术制备广藿香油-介孔硅纳米颗粒
S11、首先,将200mg直径在80nm左右的介孔硅纳米粒(MCM-41介孔硅)放入高压釜中后密闭,通过喷嘴A注入2mL广藿香油;
S12、然后通过喷嘴B通入CO2使压力上升达到30MPa,同时升温至48℃,开始超临界态下的广藿香油渗透载入介孔硅纳米粒的过程;
S13、待系统达到平衡后(即保持超临界约1小时后,在介孔硅纳米粒内外的广藿香油的浓度达到平衡),通过釜体冷凝水系统降温釜体温度至18℃,冷凝水温为2~6℃,使系统脱离超临界态,之后缓慢排出CO2进行泄压至常压,使广藿香油负载于介孔硅纳米粒(MCM-41介孔硅)之中,同时回收CO2及未负载的广藿香油;
S14、重复以上步骤S11~S13操作过程3次,开釜收集载有广藿香油的纳米药物固态粉体,即得到高载药量的广藿香油-介孔硅纳米颗粒产物240.7mg,所得产物的载药量达到32.8%(wt%);
(S2)广藿香油纳米复合膜的制备
S21、分别配制2%(w/v)的壳聚糖溶液和10%(w/v)的聚乙烯醇(PVA)溶液,然后将两者以8:2的比例进行混合,得到混合液;
S22、向混合液中加入2.0%(w/w)的步骤S1所制得的广藿香油-介孔硅纳米颗粒,并以高速磁力搅拌混合均匀得到胶状悬浮液;高速磁力搅拌过程的搅拌速度为600rpm,搅拌时间为20min。
S23、将步骤S22所得的胶状悬浮液在聚四氟乙烯模具中涂布展开呈薄膜状,并冷冻干燥,即得到广藿香油纳米复合膜。其中,聚四氟乙烯模具为100x100mm平板,边缘有挡隔。在涂布时,将12mL胶状悬浮液倒入聚四氟乙烯模具中以刮板均匀分布为薄膜状。冷冻干燥的条件是:冷冻温度为-35℃,抽真空12h,冻干48h。
经测试,所得的广藿香油纳米复合膜吸湿30min后重量为未吸湿前的3.11倍;抗拉强度为0.155MPa,伸长率为88.7%;置于水中24h后广藿香油释放率为14.3%,120h后释放率为51.9%;将广藿香油纳米复合膜置于1.5×103cfu/mL的金黄色葡萄球菌培养液中48h后,抑菌率100%,120h后抑菌率99.3%。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
此外,应当理解,虽然本说明书按照实施例加以描述,但并非每个实施例仅包含一个独立的技术方案,说明书的这种叙述方式仅仅是为清楚起见,本领域技术人员应当将说明书作为一个整体,各实施例中的技术方案也可以经适当组合,形成本领域技术人员可以理解的其他实施例。
Claims (10)
1.一种用于皮肤创伤修复的广藿香油纳米复合膜的制备方法,其特征在于,包括以下制备步骤:
S1、采用超临界CO2循环渗透技术制备广藿香油-介孔硅纳米颗粒
S11、将介孔硅纳米粒放入高压釜中后密闭,通过喷嘴A注入广藿香油;
S12、然后通过喷嘴B通入CO2使压力上升达到预设压力,同时升温至预设温度,开始超临界态下的广藿香油渗透载入过程;
S13、待系统达到平衡后,通过降温、泄压操作使系统脱离超临界态,广藿香油负载于介孔硅纳米粒中,同时回收CO2及未负载的广藿香油;
S14、重复以上步骤S11~S13操作过程3~4次,即得到高载药量的广藿香油-介孔硅纳米颗粒;
S2、广藿香油纳米复合膜的制备
S21、分别配制1%~4%的壳聚糖溶液和8%~12%的聚乙烯醇溶液,然后将两者以一定溶液质量比的比例进行混合,得到混合液;
S22、向混合液中加入一定比例的步骤S1所制得的广藿香油-介孔硅纳米颗粒,并以高速磁力搅拌混合均匀得到胶状悬浮液;
S23、将步骤S22所得的胶状悬浮液在聚四氟乙烯模具中涂布展开呈薄膜状,并冷冻干燥,即得到广藿香油纳米复合膜。
2.根据权利要求1所述的用于皮肤创伤修复的广藿香油纳米复合膜的制备方法,其特征在于,在步骤S12中,所述预设压力为18~35MPa,所述预设温度为35~50℃。
3.根据权利要求1所述的用于皮肤创伤修复的广藿香油纳米复合膜的制备方法,其特征在于,在步骤S11和步骤S12中,所述喷嘴A和所述喷嘴B为同轴式喷嘴或两个并行独立的喷嘴。
4.根据权利要求1所述的用于皮肤创伤修复的广藿香油纳米复合膜的制备方法,其特征在于,在步骤S13中,降温操作为通过冷凝水降温釜体温度至20℃以下,冷凝水温为2~6℃;泄压操作为压力降至常压。
5.根据权利要求1所述的用于皮肤创伤修复的广藿香油纳米复合膜的制备方法,其特征在于,在步骤S21中,壳聚糖溶液和聚乙烯醇溶液的比例为6:4~8:2。
6.根据权利要求1所述的用于皮肤创伤修复的广藿香油纳米复合膜的制备方法,其特征在于,在步骤S22中,加入的广藿香油-介孔硅纳米颗粒的比例为0.5%~3.0%。
7.根据权利要求1所述的用于皮肤创伤修复的广藿香油纳米复合膜的制备方法,其特征在于,在步骤S22中,高速磁力搅拌过程的搅拌速度为600rpm,搅拌时间为20min。
8.根据权利要求1所述的用于皮肤创伤修复的广藿香油纳米复合膜的制备方法,其特征在于,在步骤S23中,冷冻干燥的条件是:冷冻温度为-35℃,抽真空12h,冻干48h。
9.根据权利要求1所述的用于皮肤创伤修复的广藿香油纳米复合膜的制备方法,其特征在于,在步骤S11中,所述介孔硅纳米粒为MCM-41型纳米球形介孔结构,粒径在100nm以下。
10.根据权利要求1所述的用于皮肤创伤修复的广藿香油纳米复合膜的制备方法,其特征在于,所述介孔硅纳米粒的制备方法为:
将3g十六烷基三甲基溴化铵加入到60mL的去离子水中,95℃水浴,于350r/min搅拌完全溶解后加入120μL二乙醇胺,混匀后45分钟内加入4.5mL正硅酸四乙酯,继续反应1h,静置放冷得到淡蓝色乳状液;加入甲醇稀释并进行离心,之后浸泡在60℃的乙醇/浓硫酸体系反应24h,再加入去离子水多次离心至溶液为中性,得到介孔硅材料;最后用乙醇冲洗介孔硅材料,在烘箱中55℃干燥6h后得到干燥的介孔硅纳米粒产物,收集备用。
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