CN115154672A - 用于治疗牙周组织炎症破坏的多功能水凝胶的制备方法 - Google Patents
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Abstract
一种用于治疗牙周组织炎症破坏的多功能水凝胶的制备方法,蚕茧顺次经碳酸钠和溴化锂溶液处理制得的丝素蛋白溶液中加入甲基丙烯酸缩水甘油酯,制得双键化丝素蛋白水凝胶,再在该水凝胶中引入自由基预得的多巴胺溶液,以提供粘附性,再引入多酚修饰过氧化钙为牙周组织提供充足氧气,联合季铵化壳聚糖抑制牙周组织周围厌氧细菌。本发明双层水凝胶的下层水凝胶具有较低的模量,适合于软组织修复,而上层水凝胶具有较高的模量,适用于硬组织的修复,再结合水凝胶的粘附抗菌释氧功能,特别适用于牙周组织炎症破坏的软硬组织修复。
Description
技术领域
本发明涉及生物材料技术领域,具体涉及一种用于治疗牙周组织炎症破坏的多功能水凝胶的制备方法。
背景技术
牙周炎是口腔常见病,它是由寄生在牙齿颈部的菌斑诱发的一类牙周组织炎性疾病。牙周袋内的菌斑主要是革兰氏阴性厌氧菌,厌氧菌对氧含量比较敏感,增加氧含量可以明显抑制厌氧菌的生长,另外抗生素虽具有良好的抑菌效果,但长期应用增加了耐药菌株产生的风险,所以天然的抗菌材料是抑制牙菌斑的一个良好选择。
牙周炎是导致成年人牙齿缺失的首要原因,轻度牙周炎病例可通过种植牙来修复,但是在重度牙周炎病例中,牙种植体周组织因长期受到炎性破坏而伴有牙槽骨低平、角化龈宽度减少、感染风险加重等表现,导致其种植修复的效果及长期成功率均远低于牙周健康者,所以需要其他生物医用材料来进行辅助治疗。医用材料的力学性能与周围组织匹配,有利于软硬组织的修复。牙周炎的修复过程中既需要修复软组织又需要修复硬组织,因此需要修复材料具有两种不同的模量。所以需要一种生物医用材料具有合适的软硬组织支持和良好的炎症控制,来保障牙周种植修复长期成功。
发明内容
本发明的目的是提供一种用于治疗牙周组织炎症破坏的粘附抗菌释氧双层水凝胶的制备方法,旨在制得的双层水凝胶具有很好的层间稳定性,且下层水凝胶对牙周组织具有良好的粘附性能,上层水凝胶具有的释氧性能以有效对抗牙周组织处的厌氧细菌。并且双层水凝胶具有不同的模量,上层具有较高模量,下层具有较低模量,使其适合于牙周炎症破坏这种软硬组织都需要修复的病症。
本发明的目的是这样实现的:一种用于治疗牙周组织炎症破坏的粘附抗菌释氧双层水凝胶的制备方法,包括以下步骤:
步骤1:将一定量的蚕茧加入到碳酸钠溶液中,煮沸30分钟,在冷水下冲洗,重复相同的处理2~5 次,烘干后得到脱胶丝素;
步骤2:将步骤1得到的脱胶蚕丝,一定量加入到溴化锂溶液中,70℃加热溶解后,透析得到丝素蛋白(SF)溶液;
步骤3:加入一定量步骤2得到的丝素蛋白溶液,再加入一定量的甲基丙烯酸缩水甘油酯,搅拌3个小时,透析3-5天后,冻干得到双键化丝素蛋白(SF-GMA);
步骤4:将一定量的CaCl2和多酚(多巴胺、单宁酸、茶多酚或表没食子儿茶素没食子酸酯等)溶解分散在乙醇中,缓慢逐滴添加一定量的NH3·H2O,在恒定搅拌下,向该混合物中加入一定量的H2O2,并使得混合物反应搅拌30分钟。随后通过将混合物离心获得多酚修饰CaO2纳米颗粒;
步骤5:首先将一定量的壳聚糖溶解在1%的醋酸溶液中,再将一定量的环氧丙基三甲基氯化铵溶解在水中,然后将环氧丙基三甲基氯化铵溶液滴加到壳聚糖溶液中并搅拌均匀。混合溶液在80℃反应10 h,然后将其倒入冷的丙酮中,在冰箱放置24h,之后将丙酮倒出,留下凝胶状产物。将产物溶解在甲醇中,然后倒入一定比例的乙醇/丙酮混合溶液中,使产物沉淀出来。将产物在室温下用去离子水透析4天,得到季铵化壳聚糖(QCS);
步骤6:将一定量的双键化丝素蛋白和多酚修饰的CaO2纳米颗粒以一定的比例混合均匀,再加入交联剂,助剂和引发剂制备得到上层水凝胶,再将其泡入一定浓度的乙醇中一段时间,以调控其模量适合牙周硬组织;
步骤7:将多巴胺与水按一定的比例混合均匀,加入引发剂和助剂使其预聚15min。加入SF-GMA和QCS,再加入交联剂,助剂和引发剂,将该混合溶液倒入含有上层水凝胶的模具中,完全成胶后得到双层水凝胶。
本发明的有益效果是:
(1)本发明为双层水凝胶,上层水凝胶通过浸泡乙醇,水凝胶中的丝素蛋白的构象大多转变为β折叠,可以大幅提高水凝胶的模量,使其适用于骨修复;粘附层水凝胶中丝素蛋白大多为游离的多肽,模量较低,适用于软组织修复;双层水凝胶都是双键聚合,所以两层之间具有良好的稳定性。
(2)下层水凝胶中通过引入自由基预聚的多巴胺,能够有效的赋予丝素蛋白水凝胶粘附性,使其能长期有效的粘附在潮湿的牙周组织上,实现持续的修复。
(3)双层水凝胶中季铵化壳聚糖的杀菌和多酚修饰过氧化钙纳米颗粒的释氧联合作用,能够有效的对抗牙周组织处的厌氧细菌。
(4)双层水凝胶中引入了大量的多酚,可以有效的控制牙周组织的炎症,以及调控牙周组织处免疫反应。
本发明的粘附抗菌释氧双层水凝胶用于牙周组织炎症破坏的治疗与修复。在双键化丝素蛋白水凝胶中引入自由基预聚的多巴胺溶液,以提供粘附性,使双层水凝胶粘附在湿润口腔环境的牙周组织上。多酚修饰过氧化钙的引入可为牙周低氧环境下的组织修复提供充足的氧气,并且可与季铵化壳聚糖相互促进抑制牙周环境周围的厌氧细菌。利用乙醇对丝素蛋白的构象进行控制,使其游离的多肽转变为稳定的β折叠,可以调控丝素蛋白水凝胶的模量,使其适合于软硬组织。
附图说明
图1为实施例中治疗牙周炎的粘附抗菌释氧双层水凝胶示意图。
图2为实施例中双层水凝胶的实物图。
图3 为实施例中上层水凝胶的氧气释放性能测试。
图4 为实施例中下层水凝胶的粘附性能测试。
具体实施方式
下面结合附图和实施例对本发明进一步说明。
一种用于种用于治疗牙周组织炎症破坏的粘附抗菌释氧双层水凝胶的制备方法,包括以下步骤:
步骤1:将40 g的蚕茧加入到2%碳酸钠溶液中,煮沸30分钟,在冷水下冲洗,重复相同的处理2~5 次,烘干后得到脱胶丝素。
步骤2:将步骤得到的脱胶蚕丝,20 g加入到9.3 M的溴化锂溶液中,70℃加热溶解后,透析得到丝素蛋白溶液。
步骤3:加入100 ml步骤2得到的丝素蛋白溶液,再加入16 ml的甲基丙烯酸缩水甘油酯,搅拌3个小时,透析3-5天后,冻干得到双键化丝素蛋白。
步骤4:将5g的CaCl2和0.05 g多巴胺溶解分散在300 ml乙醇中,缓慢逐滴添加25ml的0.1 M的NH3·H2O,在恒定搅拌下,向该混合物中加入25 ml的H2O2,并使得混合物反应搅拌30分钟。随后通过将混合物离心获得多酚修饰CaO2纳米颗粒。
步骤5:将12 g的壳聚糖加入到400 ml的2%的乙酸溶液中,再将37.5 g的环氧丙基三甲基氯化铵溶解在50 ml去离子水中,然后将环氧丙基三甲基氯化铵溶液缓慢滴加到壳聚糖溶液中并搅拌均匀。混合溶液在80℃反应10 h,然后将其倒入冷的丙酮中,在冰箱放置24h,之后将丙酮倒出,留下凝胶状产物。将产物溶解在甲醇中,然后倒入一定比例的乙醇/丙酮混合溶液中,使产物沉淀出来。将产物在室温下用去离子水透析4天,得到季铵化壳聚糖(QCS)。、
步骤6:将2g的双键化丝素蛋白和1%的多酚修饰的CaO2纳米颗粒加入到10 ml去离子水中,再加入300μl的Pegda,25μl四甲基乙二胺和0.2 g的过硫酸铵制备得到上层水凝胶,再将其泡入乙醇(60%、70%、80%、90%、100%)中100min,以调控其模量适合牙周硬组织。
步骤7:将0.003 g多巴胺加入到10 ml水中,加入0.05 g过硫酸铵和20μl四甲基乙二胺使其预聚15 min。加入2g的SF-GMA和0.1 g的QCS,再加入300μl的Pegda,25μl四甲基乙二胺和0.2 g的过硫酸铵,将该混合溶液倒入含有上层水凝胶的模具中,完全成胶后得到双层水凝胶。
图1是双层水凝胶的设计示意图,上层水凝胶具有释放氧气的功能,具有较高的模量;下层水凝胶具有抗菌的功能,具有较低的模量。
图3是上层水凝胶的氧气释放性能测试图,可以看见多巴胺修饰的过氧化钙的引入能够赋予水凝胶释放氧气的能力,使其在低氧条件下持续释放氧气长达30 h,并且瞬时的氧气浓度可高达8mg/L。
图4是下层水凝胶的粘附性能测试图,可以看见多巴胺的引入能够提高丝素蛋白水凝胶的粘附性能,对各种基材都有较好的粘附性。
Claims (1)
1.一种用于治疗牙周组织炎症破坏的多功能水凝胶的制备方法,包括以下步骤:
步骤1:将一定量的蚕茧加入到碳酸钠溶液中,煮沸30分钟,在冷水下冲洗,重复相同的处理2~5 次,烘干后得到脱胶丝素;
步骤2:将步骤1得到的脱胶蚕丝,一定量加入到溴化锂溶液中,70℃加热溶解后,透析得到丝素蛋白溶液;
步骤3:加入一定量步骤2得到的丝素蛋白溶液,再加入一定量的甲基丙烯酸缩水甘油酯,搅拌3个小时,透析3-5天后,冻干得到双键化丝素蛋白;
步骤4:将一定量的CaCl2和多酚(多巴胺、单宁酸、茶多酚或表没食子儿茶素没食子酸酯等)溶解分散在乙醇中,缓慢逐滴添加一定量的NH3·H2O,在恒定搅拌下,向该混合物中加入一定量的H2O2,并使得混合物反应搅拌30分钟,随后通过将混合物离心获得多酚修饰CaO2纳米颗粒;
步骤5:首先将一定量的壳聚糖溶解在1%的醋酸溶液中,再将一定量的环氧丙基三甲基氯化铵溶解在水中,然后将环氧丙基三甲基氯化铵溶液滴加到壳聚糖溶液中并搅拌均匀;混合溶液在80℃反应10 h,然后将其倒入冷的丙酮中,在冰箱放置24h,之后将丙酮倒出,留下凝胶状产物;将产物溶解在甲醇中,然后倒入一定比例的乙醇/丙酮混合溶液中,使产物沉淀出来,将产物在室温下用去离子水透析4天,得到季铵化壳聚糖(QCS);
步骤6:将一定量的双键化丝素蛋白和多酚修饰的CaO2纳米颗粒以一定的比例混合均匀,再加入交联剂,助剂和引发剂制备得到上层水凝胶,再将其泡入一定浓度的乙醇中一段时间,以调控其模量适合牙周硬组织;
步骤7:将多巴胺与水按一定的比例混合均匀,加入引发剂和助剂使其预聚15 min,加入SF-GMA和QCS,再加入交联剂,助剂和引发剂,将该混合溶液倒入含有上层水凝胶的模具中,完全成胶后得到双层水凝胶。
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