CN105457107A - 一种双功能层口腔修复膜及其制备方法 - Google Patents
一种双功能层口腔修复膜及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种双功能层口腔修复膜及其制备方法。修复膜由疏松多孔层与致密抑菌层两层组成。疏松多孔层是由Ⅰ型胶原、氧化多糖和β-磷酸三钙组成;致密抑菌层由Ⅰ型胶原与氧化壳聚糖复合组成。本发明的修复膜具有良好的力学性能、亲水性、生物相容性以及一定的抗菌抑菌性、适宜可控的降解吸收性,制备操作简单,既具备了良好的机械屏障作用,同时也有利于成骨细胞与膜的结合,为新牙的形成提供Ca2+、P3-等。
Description
技术领域
本发明涉及一种双功能层口腔修复膜及其制备方法,属于口腔医用材料领域。
背景技术
近些年来,随着组织工程学的不断发展进步,诞生了一种新型修复技术——膜引导组织再生术(membraneguidedboneregeneration,MGBR),MGBR的产生极大地提高了口腔修复学的水平。
口腔修复膜是利用外科手术的方式将膜置于口腔软组织与骨缺损之间建立生物屏障,以此创造一个相对封闭的骨再生环境,选择性地阻挡迁移速度较快的成纤维细胞与上皮细胞进入骨缺损区,而同时又不妨碍伤口自然愈合的一种生物相容性材料。口腔修复膜依据材料来源可细分为:胶原类膜、金属膜、合成膜与异体骨膜等;依据材料是否能被降解细分为可吸收性膜与不可吸收性膜。
胶原作为一种优良的生物医用材料,同时也是骨的主要有机成分,因此以胶原为原材料制作的口腔修复膜是可吸收材料中研究和应用最多的。胶原膜本身具有诸多优良的性能,如良好的骨组织诱导再生功能、可生物降解性、血凝作用、低抗原性、良好的组织相容性等。但其单独使用时无法满足口腔修复膜的多功能性要求,因此常与其他材料复合来达到更好的性能(TaguchiY,AmizukaN,NakadateM,etal.Ahistologicalevaluationforguidedboneregenerationinducedbyacollagenousmembrane[J].Biomaterials,2005,26(31):6158-6166.)。
壳聚糖又称为脱乙酰甲壳素,属于天然高分子聚合物,生物相容性良好,几乎没有抗原性,同时还具有诱导组织再生、止血与抗菌抑菌等功能,是一种优良的生物医用材料,但纯壳聚糖膜机械性能及生物降解性能较差,不适用于口腔修复膜材料,因此人们常对壳聚糖进行改性或与其他材料共混来提高其性能达到口腔修复膜材料的要求(PrabaharanM.Reviewpaper:chitosanderivativesaspromisingmaterialsforcontrolleddrugdelivery[J].JBiomaterAppl,2008,23(1):5-36.)。氧化的壳聚糖与Ⅰ型胶原间可产生席夫碱反应,原位交联,诱导胶原分子发生自聚集,提高了Ⅰ型胶原的生物降解性、力学性能以及稳定性。
硫酸软骨素是一种糖胺聚糖,具有抗炎、加速伤口愈合等作用。透明质酸是一种酸性粘多糖,具有特殊的保水作用,是目前发现的自然界中保湿性最好的物质,可促进创伤的愈合,同时与其他营养成分配合使用,可以起到促进营养吸收的效果。β-磷酸三钙具有良好的生物相容性、生物活性以及生物降解性,是理想的人体硬组织修复和替代材料,同时还可为新牙的形成提供Ca2+、P3-等。氧化硫酸软骨素或氧化透明质酸与Ⅰ型胶原间也可产生席夫碱反应,原位交联,诱导胶原分子发生自聚集,提高了Ⅰ型胶原的生物降解性、力学性能以及稳定性。
与现今同类口腔修复膜相比,本发明采用双功能层,致密抑菌层由氧化壳聚糖与Ⅰ型胶原组成,具有良好的机械屏障作用与抗菌抑菌效果;疏松多孔层由Ⅰ型胶原、氧化多糖、β-磷酸三钙组成,具有良好的诱导作用并可参与口腔修复的代谢过程。制作工艺上,疏松多孔结构经过离子沥滤法、两次交联与两次真空冷冻干燥过程,其均匀多孔结构有利于细胞的粘附与分化生长,起到诱导牙缺损的修复再生。
发明内容
本发明的目的是为口腔医用材料领域提供一种具有良好的机械屏障作用、诱导作用以及能够参与代谢过程的多功能性口腔修复膜及其制备方法。
本发明的目的是由以下技术措施来实现的:
一种双功能层口腔修复膜材料,其特征在于该膜包括疏松多孔层与致密抑菌层,疏松多孔层是由Ⅰ型胶原、氧化多糖和β-磷酸三钙组成;致密抑菌层由Ⅰ型胶原与氧化壳聚糖组成。双功能层口腔修复膜材料的制备方法包括以下步骤:
(1)致密抑菌层的制备:
①将氧化壳聚糖溶解在醋酸溶液中,配制成3~5g/L的氧化壳聚糖溶液;
②将Ⅰ型胶原溶解在0.1~0.5M的醋酸溶液中,在4℃下搅拌配成3~5g/L的I型胶原溶液;
③将步骤①与②的溶液混合,搅拌30~60min,加入乙醇消泡,再经超声消泡后,倒入模具中,风干成膜备用;
④将膜浸入交联液中交联8~24h后,风干备用;
(2)疏松多孔层的制备:
(ⅰ)将Ⅰ型胶原溶解在稀盐酸或醋酸溶液中,在4℃下搅拌使之完全溶解,配制成2~6g/L的I型胶原溶液;
(ⅱ)在配制好的I型胶原溶液中加入氧化多糖,在4℃下搅拌使之溶解完全,得A溶液;
(ⅲ)在搅拌条件下,向步骤(ⅱ)所得A溶液中缓慢加入纳米级β-磷酸三钙粉末,在4℃下搅拌使之形成均匀的悬浮液,即B溶液;
(ⅳ)将NaCl颗粒溶于去离子水中,配制成0.2~1.0mol/L的NaCl溶液,然后将NaCl溶液缓慢的加入到步骤(ⅲ)所得B溶液中,得C溶液;
(ⅴ)将步骤(ⅳ)所得C溶液倒入模具中,置于真空冷冻干燥机中冷冻干燥备用;
(ⅵ)将第一次真空冷冻干燥的膜进行脱氢加热交联,温度为100~115℃,交联处理时间为0.5~2.5h;
(ⅶ)将步骤(ⅵ)所得膜材料浸泡于交联剂溶液中交联4~18h后,用去离子水反复浸泡清洗备用;
(3)双功能层口腔修复膜的制备:
(Ⅰ)将步骤(2)所得疏松多孔层浸泡于去离子水中,浸泡5~30min后,取出放入-80℃冰箱中预冻3~30min,使膜材料表面为冰-水复合形式,再将步骤(1)所得的致密抑菌层紧密地粘附其上,继续进行第二次真空冷冻干燥;
(Ⅱ)经灭菌处理,即得双功能层口腔修复膜。
所述的双功能层口腔修复膜,其特征在于,所述氧化壳聚糖溶液与I型胶原溶液的共混体积比为1:1~3:1。
所述的双功能层口腔修复膜,其特征在于,所述交联剂为1-乙基-3-(3-二甲基胺丙基)-碳化二亚胺、N-羟基琥珀酰亚胺、京尼平、原花青素、甲醛的任一种或两种。
所述的双功能层口腔修复膜,其特征在于,所述氧化多糖为氧化硫酸软骨素和氧化透明质酸的任意一种,质量分数为1.0%~3.0%。
所述的双功能层口腔修复膜,其特征在于,所述Ⅰ型胶原与纳米级β-磷酸三钙的质量比为1:1~1:3。
本发明具有以下优点:
1.本发明采用Ⅰ型胶原、氧化多糖、β-磷酸三钙与氧化壳聚糖为原料,利用氧化多糖与Ⅰ型胶原和氧化壳聚糖与Ⅰ型胶原间产生席夫碱反应而原位交联,诱导胶原分子发生自聚集,提高了Ⅰ型胶原的生物降解性、力学性能及其结构稳定性。双功能层口腔修复膜具有良好的生物相容性与适宜可控的降解吸收率;
2.本发明采用双功能层结构,其致密抑菌层由氧化壳聚糖与Ⅰ型胶原组成,具有良好的机械屏障作用与抗菌抑菌效果;疏松多孔层由Ⅰ型胶原、氧化多糖、β-磷酸三钙组成,具有良好的诱导作用并可参与口腔修复的代谢过程;
3.疏松多孔结构是通过离子沥滤法、两次交联与两次真空冷冻干燥过程获得的,其均匀的多孔结构对于细胞的粘附与分化生长极为有利,因而可以诱导牙缺损的修复再生。
具体实施方式
下面通过实施对本发明进行具体的描述,有必要在此指出的是本实施例只用于对本发明进行进一步说明,而不能理解为对本发明保护范围的限制,该领域的技术熟练人员可以根据上述发明的内容作出一些非本质的改进和调整。
实施例1
双功能层口腔修复膜材料的制备方法包括以下步骤:
(1)致密抑菌层的制备:
①将氧化壳聚糖溶解在醋酸溶液中,配制成3g/L的氧化壳聚糖溶液;
②将Ⅰ型胶原溶解在0.5M的醋酸溶液中,在4℃下搅拌配成3g/L的I型胶原溶液;
③将步骤①与②的溶液混合,搅拌40min,加入乙醇消泡,再经超声消泡后,倒入模具中,风干成膜备用;
④将膜浸入交联液中交联8h后,风干备用;
(2)疏松多孔层的制备:
(ⅰ)将Ⅰ型胶原溶解在稀盐酸或醋酸溶液中,在4℃下搅拌使之完全溶解,配制成3g/L的I型胶原溶液;
(ⅱ)在配制好的I型胶原溶液中加入氧化硫酸软骨素,在4℃下搅拌使之溶解完全,得A溶液;
(ⅲ)在搅拌条件下,向步骤(ⅱ)所得A溶液中缓慢加入纳米级β-磷酸三钙粉末,在4℃下搅拌使之形成均匀的悬浮液,即B溶液;
(ⅳ)将NaCl颗粒溶于去离子水中,配制成0.5mol/L的NaCl溶液,然后将NaCl溶液缓慢的加入到步骤(ⅲ)所得B溶液中,得C溶液;
(ⅴ)将步骤(ⅳ)所得C溶液倒入模具中,置于真空冷冻干燥机中冷冻干燥备用;
(ⅵ)将第一次真空冷冻干燥的膜进行脱氢加热交联,温度为110℃,交联处理时间为2h;
(ⅶ)将步骤(ⅵ)所得膜材料浸泡于交联剂溶液中交联6h后,用去离子水反复浸泡清洗备用;
(3)双功能层口腔修复膜的制备:
(Ⅰ)将步骤(2)所得疏松多孔层浸泡于去离子水中,浸泡20min后,取出放入-80℃冰箱中预冻15min,使膜材料表面为冰-水复合形式,再将步骤(1)所得的致密抑菌层紧密地粘附其上,继续进行第二次真空冷冻干燥;
(Ⅱ)经灭菌处理,即得双功能层口腔修复膜。
实施例2
双功能层口腔修复膜材料的制备方法包括以下步骤:
(1)致密抑菌层的制备:
①将氧化壳聚糖溶解在醋酸溶液中,配制成4g/L的氧化壳聚糖溶液;
②将Ⅰ型胶原溶解在0.2M的醋酸溶液中,在4℃下搅拌配成4g/L的I型胶原溶液;
③将步骤①与②的溶液混合,搅拌60min,加入乙醇消泡,再经超声消泡后,倒入模具中,风干成膜备用;
④将膜浸入交联液中交联12h后,风干备用;
(2)疏松多孔层的制备:
(ⅰ)将Ⅰ型胶原溶解在稀盐酸或醋酸溶液中,在4℃下搅拌使之完全溶解,配制成4g/L的I型胶原溶液;
(ⅱ)在配制好的I型胶原溶液中加入氧化透明质酸,在4℃下搅拌使之溶解完全,得A溶液;
(ⅲ)在搅拌条件下,向步骤(ⅱ)所得A溶液中缓慢加入纳米级β-磷酸三钙粉末,在4℃下搅拌使之形成均匀的悬浮液,即B溶液;
(ⅳ)将NaCl颗粒溶于去离子水中,配制成0.6mol/L的NaCl溶液,然后将NaCl溶液缓慢的加入到步骤(ⅲ)所得B溶液中,得C溶液;
(ⅴ)将步骤(ⅳ)所得C溶液倒入模具中,置于真空冷冻干燥机中冷冻干燥备用;
(ⅵ)将第一次真空冷冻干燥的膜进行脱氢加热交联,温度为110℃,交联处理时间为1.5h;
(ⅶ)将步骤(ⅵ)所得膜材料浸泡于交联剂溶液中交联8h后,用去离子水反复浸泡清洗备用;
(3)双功能层口腔修复膜的制备:
(Ⅰ)将步骤(2)所得疏松多孔层浸泡于去离子水中,浸泡20min后,取出放入-80℃冰箱中预冻20min,使膜材料表面为冰-水复合形式,再将步骤(1)所得的致密抑菌层紧密地粘附其上,继续进行第二次真空冷冻干燥;
(Ⅱ)经灭菌处理,即得双功能层口腔修复膜。
实施例3
双功能层口腔修复膜材料的制备方法包括以下步骤:
(1)致密抑菌层的制备:
①将氧化壳聚糖溶解在醋酸溶液中,配制成5g/L的氧化壳聚糖溶液;
②将Ⅰ型胶原溶解在0.5M的醋酸溶液中,在4℃下搅拌配成5g/L的I型胶原溶液;
③将步骤①与②的溶液混合,搅拌50min,加入乙醇消泡,再经超声消泡后,倒入模具中,风干成膜备用;
④将膜浸入交联液中交联10h后,风干备用;
(2)疏松多孔层的制备:
(ⅰ)将Ⅰ型胶原溶解在稀盐酸或醋酸溶液中,在4℃下搅拌使之完全溶解,配制成5g/L的I型胶原溶液;
(ⅱ)在配制好的I型胶原溶液中加入氧化硫酸软骨素,在4℃下搅拌使之溶解完全,得A溶液;
(ⅲ)在搅拌条件下,向步骤(ⅱ)所得A溶液中缓慢加入纳米级β-磷酸三钙粉末,在4℃下搅拌使之形成均匀的悬浮液,即B溶液;
(ⅳ)将NaCl颗粒溶于去离子水中,配制成0.5mol/L的NaCl溶液,然后将NaCl溶液缓慢的加入到步骤(ⅲ)所得B溶液中,得C溶液;
(ⅴ)将步骤(ⅳ)所得C溶液倒入模具中,置于真空冷冻干燥机中冷冻干燥备用;
(ⅵ)将第一次真空冷冻干燥的膜进行脱氢加热交联,温度为100℃,交联处理时间为2.5h;
(ⅶ)将步骤(ⅵ)所得膜材料浸泡于交联剂溶液中交联8h后,用去离子水反复浸泡清洗备用;
(3)双功能层口腔修复膜的制备:
(Ⅰ)将步骤(2)所得疏松多孔层浸泡于去离子水中,浸泡10min后,取出放入-80℃冰箱中预冻10min,使膜材料表面为冰-水复合形式,再将步骤(1)所得的致密抑菌层紧密地粘附其上,继续进行第二次真空冷冻干燥;
(Ⅱ)经灭菌处理,即得双功能层口腔修复膜。
Claims (6)
1.一种双功能层口腔修复膜材料,其特征在于该膜包括疏松多孔层与致密抑菌层,疏松多孔层是由Ⅰ型胶原、氧化多糖和β-磷酸三钙组成;致密抑菌层由Ⅰ型胶原与氧化壳聚糖组成。
2.权利要求1中所述的一种双功能层口腔修复膜材料的制备方法,其特征在于,制备方法包括以下步骤:
(1)致密抑菌层的制备:
①将氧化壳聚糖溶解在醋酸溶液中,配制成3~5g/L的氧化壳聚糖溶液;
②将Ⅰ型胶原溶解在0.1~0.5M的醋酸溶液中,在4℃下搅拌配成3~5g/L的I型胶原溶液;
③将步骤①与②的溶液混合,搅拌30~60min,加入乙醇消泡,再经超声消泡后,倒入模具中,风干成膜备用;
④将膜浸入交联液中交联8~24h后,风干备用;
(2)疏松多孔层的制备:
(ⅰ)将Ⅰ型胶原溶解在稀盐酸或醋酸溶液中,在4℃下搅拌使之完全溶解,配制成2~6g/L的I型胶原溶液;
(ⅱ)在配制好的I型胶原溶液中加入氧化多糖,在4℃下搅拌使之溶解完全,得A溶液;
(ⅲ)在搅拌条件下,向步骤(ⅱ)所得A溶液中缓慢加入纳米级β-磷酸三钙粉末,在4℃下搅拌使之形成均匀的悬浮液,即B溶液;
(ⅳ)将NaCl颗粒溶于去离子水中,配制成0.2~1.0mol/L的NaCl溶液,然后将NaCl溶液缓慢的加入到步骤(ⅲ)所得B溶液中,得C溶液;
(ⅴ)将步骤(ⅳ)所得C溶液倒入模具中,置于真空冷冻干燥机中冷冻干燥备用;
(ⅵ)将第一次真空冷冻干燥的膜进行脱氢加热交联,温度为100~115℃,交联处理时间为0.5~2.5h;
(ⅶ)将步骤(ⅵ)所得膜材料浸泡于交联剂溶液中交联4~18h后,用去离子水反复浸泡清洗备用;
(3)双功能层口腔修复膜的制备:
(Ⅰ)将步骤(2)所得疏松多孔层浸泡于去离子水中,浸泡5~30min后,取出放入-80℃冰箱中预冻3~30min,使膜材料表面为冰-水复合形式,再将步骤(1)所得的致密抑菌层紧密地粘附其上,继续进行第二次真空冷冻干燥;
(Ⅱ)经灭菌处理,即得双功能层口腔修复膜。
3.权利要求1所述的双功能层口腔修复膜,其特征在于,所述氧化壳聚糖溶液与I型胶原溶液的共混体积比为1:1~3:1。
4.权利要求1所述的双功能层口腔修复膜,其特征在于,所述交联剂为1-乙基-3-(3-二甲基胺丙基)-碳化二亚胺、N-羟基琥珀酰亚胺、京尼平、原花青素、甲醛的任一种或两种。
5.权利要求1所述的双功能层口腔修复膜,其特征在于,所述氧化多糖为氧化硫酸软骨素和氧化透明质酸的任意一种,质量分数为1.0%~3.0%。
6.权利要求1所述的双功能层口腔修复膜,其特征在于,所述Ⅰ型胶原与纳米级β-磷酸三钙的质量比为1:1~1:3。
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