CN106730016A - 一种活性修饰改性人工韧带及其制备工艺 - Google Patents
一种活性修饰改性人工韧带及其制备工艺 Download PDFInfo
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Abstract
本发明公开了一种活性修饰改性人工韧带及其制备工艺,所述人工韧带包括韧带本体和置于所述韧带本体上的活性修饰层;所述韧带本体由蚕丝、细菌纤维素、蜘蛛丝、明胶和超高分子量聚乙烯纤维制备而成;所述活性修饰层由下列组分制备而成:石墨烯、磷酸四钙、蛋壳粉、四硼酸锶、透明质烷和六偏磷酸钠。本发明提供的采用多层结构改性人工韧带的耐疲劳断裂性能得到大幅提升,并且细胞粘附生长性良好,组织相容性较佳,可提高韧带修复速率和愈合效果,具有较佳的临床应用价值。
Description
技术领域
本发明属于生物医用材料技术领域,具体涉及一种活性修饰改性人工韧带及其制备工艺。
背景技术
随着人们运动量的增多,因运动损伤所造成的韧带断裂或损伤的问题越来越突出,若韧带断裂或治疗不及时或治疗效果不良时往往会造成关节不稳定,将会引起关节软骨损伤,甚至会导致骨关节炎等并发症。在韧带断裂或损伤的修复治疗过程中,最为简单有效的办法是植入人工韧带。目前的人工韧带材料主要包括碳素纤维、聚丙烯、碳支架结合胶原或聚酯、聚四氟乙烯纤维合成的聚合物以及涤纶等。然而这些人工韧带材料本身还存在组织相容性问题,会产生滑膜炎、异物排斥反应、感染等并发症,并且这些韧带材料的硬度相对高,力学强度不佳,易疲劳及折断,大大影响韧带的修复愈合效果。虽然对于人工韧带的性能改进的研究较多,但是所制备的人工韧带与理想的性能还存在一定的差距。因此,开发一种组织相容性好、耐疲劳断裂性能佳的修饰改性人工韧带,对于提高韧带修复治疗具有重要的意义。
发明内容
为此,本发明提供一种组织相容性好、硬度适中,耐疲劳断裂性能佳的活性修饰改性人工韧带及其制备工艺,解决现有韧带在修复治疗上的不足。
为此,本发明提供一种活性修饰改性人工韧带,所述人工韧带包括韧带本体和置于所述韧带本体上的活性修饰层;所述韧带本体由蚕丝、细菌纤维素、蜘蛛丝、明胶和超高分子量聚乙烯纤维制备而成;所述活性修饰层由下列组分制备而成:石墨烯、磷酸四钙、蛋壳粉、四硼酸锶、透明质烷、氨糖和六偏磷酸钠。
根据本发明的一个实施方式,其中,所述韧带本体和所述的活性修饰层之间还设有中间层,所述中间层由下列重量份的组分组成:2-9份蛋清、6-14份豆蔻酰四肽、2-7份碳纳米管和1-5份聚乙烯醇。
根据本发明的一个实施方式,其中,以重量份计,所述韧带本体由11-18份蚕丝、5-14份细菌纤维素、8-17份蜘蛛丝、4-9份明胶和2-6份超高分子量聚乙烯纤维制备而成。
根据本发明的一个实施方式,其中,所述活性修饰层由下列重量份的组分制备而成:石墨烯8-15份、磷酸四钙4-9份、蛋壳粉5-11份、四硼酸锶3-7份、透明质烷2-5份、氨糖1-3份和六偏磷酸钠4-8份。
根据本发明的一个实施方式,其中,所述活性修饰层的厚度为10-20微米。
根据本发明的一个实施方式,其中,所述中间层的厚度为3-8微米。
根据本发明的一个实施方式,其中,以重量份计,所述韧带本体由12-17份蚕丝、6-12份细菌纤维素、9-15份蜘蛛丝、4.5-8.2份明胶和2.3-5份超高分子量聚乙烯纤维制备而成;
所述活性修饰层由下列重量份的组分制备而成:石墨烯8.4-13份、磷酸四钙4.5-8.6份、蛋壳粉5.3-9份、四硼酸锶3.8-6.4份、透明质烷2.8-4.5份、氨糖1.2-2.7份和六偏磷酸钠4.3-7.6份。
根据本发明的一个实施方式,其中,所述中间层由下列重量份的组分组成:2.5-8.3份蛋清、6.4-12份豆蔻酰四肽、2.3-6.4份碳纳米管和1.8-4份聚乙烯醇。
为此,本发明提供一种活性修饰改性人工韧带的制备工艺,其包括以下步骤:
(1)按重量份称取原料:蚕丝、细菌纤维素、蜘蛛丝、明胶和超高分子量聚乙烯纤维;将蚕丝、细菌纤维素和蜘蛛丝纯化,然后溶解于10wt.%醋酸钠水溶液中,经过滤处理,得到溶液A备用;将明胶和超高分子量聚乙烯纤维置于乙酸中,加热搅拌均匀,然后加入溶液A,超声震荡,制成均匀溶液,经过纺丝挤出制备成丝束,再经编织成型制成人工韧带I;
(2)将石墨烯、磷酸四钙、蛋壳粉、四硼酸锶、透明质烷、氨糖和六偏磷酸钠置于乙酸中,超声分散均匀,制成溶液B;
(3)将蛋清、豆蔻酰四肽、碳纳米管和聚乙烯醇置于乙酸中,超声分散均匀,制成溶液C;
(4)将步骤(1)中制备的人工韧带置于溶液C中,真空干燥,并重复直至镀层厚度为3-8微米,在60-80℃下真空干燥24-48小时,得到人工韧带II;
(5)将步骤(4)中制备的人工韧带II置于溶液B中,真空干燥,并重复直至镀层厚度为10-20微米,在60-80℃下真空干燥24-48小时,即得活性修饰改性人工韧带。
本发明的有益效果为:
本发明提供的采用多层结构改性人工韧带的耐疲劳断裂性能得到大幅提升,其断裂强力达1924.7-1998.4N,断裂伸长率为361.7-36.7%,并且细胞粘附生长性良好,组织相容性较佳,可提高韧带修复速率和愈合效果,具有较佳的临床应用价值。
具体实施方式
下面结合实施例,对本发明作进一步详细描述。以下实施例用于说明本发明,但不用来限制本发明的范围。
实施例1
一种活性修饰改性人工韧带,所述人工韧带包括韧带本体和置于所述韧带本体上的活性修饰层;以重量份计,所述韧带本体由11份蚕丝、5份细菌纤维素、8份蜘蛛丝、4份明胶和2份超高分子量聚乙烯纤维制备而成;所述活性修饰层由下列重量份的组分制备而成:石墨烯8份、磷酸四钙4份、蛋壳粉5份、四硼酸锶3份、透明质烷2份、氨糖1份和六偏磷酸钠4份。所述韧带本体和所述的活性修饰层之间还设有中间层,所述中间层由下列重量份的组分组成:2份蛋清、6份豆蔻酰四肽、2份碳纳米管和1份聚乙烯醇。
一种活性修饰改性人工韧带的制备工艺,其包括以下步骤:
(1)按重量份称取原料:蚕丝、细菌纤维素、蜘蛛丝、明胶和超高分子量聚乙烯纤维;将蚕丝、细菌纤维素和蜘蛛丝纯化,然后溶解于10wt.%醋酸钠水溶液中,经过滤处理,得到溶液A备用;将明胶和超高分子量聚乙烯纤维置于乙酸中,加热搅拌均匀,然后加入溶液A,超声震荡,制成均匀溶液,经过纺丝挤出制备成丝束,再经编织成型制成人工韧带I;
(2)将石墨烯、磷酸四钙、蛋壳粉、四硼酸锶、透明质烷、氨糖和六偏磷酸钠置于乙酸中,超声分散均匀,制成溶液B;
(3)将蛋清、豆蔻酰四肽、碳纳米管和聚乙烯醇置于乙酸中,超声分散均匀,制成溶液C;
(4)将步骤(1)中制备的人工韧带置于溶液C中,真空干燥,并重复直至镀层厚度为3微米,在60℃下真空干燥24小时,得到人工韧带II;
(5)将步骤(4)中制备的人工韧带II置于溶液B中,真空干燥,并重复直至镀层厚度为10微米,在60℃下真空干燥24小时,即得活性修饰改性人工韧带。
实施例2
一种活性修饰改性人工韧带,所述人工韧带包括韧带本体和置于所述韧带本体上的活性修饰层;以重量份计,所述韧带本体由18份蚕丝、14份细菌纤维素、17份蜘蛛丝、9份明胶和6份超高分子量聚乙烯纤维制备而成;所述活性修饰层由下列重量份的组分制备而成:石墨烯15份、磷酸四钙9份、蛋壳粉11份、四硼酸锶7份、透明质烷5份、氨糖3份和六偏磷酸钠8份。所述韧带本体和所述的活性修饰层之间还设有中间层,所述中间层由下列重量份的组分组成:9份蛋清、14份豆蔻酰四肽、7份碳纳米管和5份聚乙烯醇。
一种活性修饰改性人工韧带的制备工艺,其包括以下步骤:
(1)按重量份称取原料:蚕丝、细菌纤维素、蜘蛛丝、明胶和超高分子量聚乙烯纤维;将蚕丝、细菌纤维素和蜘蛛丝纯化,然后溶解于10wt.%醋酸钠水溶液中,经过滤处理,得到溶液A备用;将明胶和超高分子量聚乙烯纤维置于乙酸中,加热搅拌均匀,然后加入溶液A,超声震荡,制成均匀溶液,经过纺丝挤出制备成丝束,再经编织成型制成人工韧带I;
(2)将石墨烯、磷酸四钙、蛋壳粉、四硼酸锶、透明质烷、氨糖和六偏磷酸钠置于乙酸中,超声分散均匀,制成溶液B;
(3)将蛋清、豆蔻酰四肽、碳纳米管和聚乙烯醇置于乙酸中,超声分散均匀,制成溶液C;
(4)将步骤(1)中制备的人工韧带置于溶液C中,真空干燥,并重复直至镀层厚度为8微米,在80℃下真空干燥48小时,得到人工韧带II;
(5)将步骤(4)中制备的人工韧带II置于溶液B中,真空干燥,并重复直至镀层厚度为20微米,在80℃下真空干燥48小时,即得活性修饰改性人工韧带。
实施例3
一种活性修饰改性人工韧带,所述人工韧带包括韧带本体和置于所述韧带本体上的活性修饰层;以重量份计,所述韧带本体由12份蚕丝、6份细菌纤维素、9份蜘蛛丝、4.5份明胶和2.3份超高分子量聚乙烯纤维制备而成;所述活性修饰层由下列重量份的组分制备而成:石墨烯8.4份、磷酸四钙4.5份、蛋壳粉5.3份、四硼酸锶3.8份、透明质烷2.8份、氨糖1.2份和六偏磷酸钠4.3份。所述韧带本体和所述的活性修饰层之间还设有中间层,所述中间层由下列重量份的组分组成:2.5份蛋清、6.4份豆蔻酰四肽、2.3份碳纳米管和1.8份聚乙烯醇。
一种活性修饰改性人工韧带的制备工艺,其包括以下步骤:
(1)按重量份称取原料:蚕丝、细菌纤维素、蜘蛛丝、明胶和超高分子量聚乙烯纤维;将蚕丝、细菌纤维素和蜘蛛丝纯化,然后溶解于10wt.%醋酸钠水溶液中,经过滤处理,得到溶液A备用;将明胶和超高分子量聚乙烯纤维置于乙酸中,加热搅拌均匀,然后加入溶液A,超声震荡,制成均匀溶液,经过纺丝挤出制备成丝束,再经编织成型制成人工韧带I;
(2)将石墨烯、磷酸四钙、蛋壳粉、四硼酸锶、透明质烷、氨糖和六偏磷酸钠置于乙酸中,超声分散均匀,制成溶液B;
(3)将蛋清、豆蔻酰四肽、碳纳米管和聚乙烯醇置于乙酸中,超声分散均匀,制成溶液C;
(4)将步骤(1)中制备的人工韧带置于溶液C中,真空干燥,并重复直至镀层厚度为5微米,在70℃下真空干燥36小时,得到人工韧带II;
(5)将步骤(4)中制备的人工韧带II置于溶液B中,真空干燥,并重复直至镀层厚度为18微米,在75℃下真空干燥30小时,即得活性修饰改性人工韧带。
实施例4
一种活性修饰改性人工韧带,所述人工韧带包括韧带本体和置于所述韧带本体上的活性修饰层;以重量份计,所述韧带本体由17份蚕丝、12份细菌纤维素、15份蜘蛛丝、8.2份明胶和5份超高分子量聚乙烯纤维制备而成;所述活性修饰层由下列重量份的组分制备而成:石墨烯13份、磷酸四钙8.6份、蛋壳粉9份、四硼酸锶6.4份、透明质烷4.5份、氨糖2.7份和六偏磷酸钠7.6份。所述韧带本体和所述的活性修饰层之间还设有中间层,所述中间层由下列重量份的组分组成:8.3份蛋清、12份豆蔻酰四肽、6.4份碳纳米管和4份聚乙烯醇。
一种活性修饰改性人工韧带的制备工艺,其包括以下步骤:
(1)按重量份称取原料:蚕丝、细菌纤维素、蜘蛛丝、明胶和超高分子量聚乙烯纤维;将蚕丝、细菌纤维素和蜘蛛丝纯化,然后溶解于10wt.%醋酸钠水溶液中,经过滤处理,得到溶液A备用;将明胶和超高分子量聚乙烯纤维置于乙酸中,加热搅拌均匀,然后加入溶液A,超声震荡,制成均匀溶液,经过纺丝挤出制备成丝束,再经编织成型制成人工韧带I;
(2)将石墨烯、磷酸四钙、蛋壳粉、四硼酸锶、透明质烷、氨糖和六偏磷酸钠置于乙酸中,超声分散均匀,制成溶液B;
(3)将蛋清、豆蔻酰四肽、碳纳米管和聚乙烯醇置于乙酸中,超声分散均匀,制成溶液C;
(4)将步骤(1)中制备的人工韧带置于溶液C中,真空干燥,并重复直至镀层厚度为6微米,在75℃下真空干燥30小时,得到人工韧带II;
(5)将步骤(4)中制备的人工韧带II置于溶液B中,真空干燥,并重复直至镀层厚度为18微米,在65℃下真空干燥30小时,即得活性修饰改性人工韧带。
实施例5
一种活性修饰改性人工韧带,所述人工韧带包括韧带本体和置于所述韧带本体上的活性修饰层;以重量份计,所述韧带本体由15份蚕丝、10份细菌纤维素、12份蜘蛛丝、6.8份明胶和4.4份超高分子量聚乙烯纤维制备而成;所述活性修饰层由下列重量份的组分制备而成:石墨烯9.6份、磷酸四钙7.4份、蛋壳粉6.8份、四硼酸锶5.2份、透明质烷3.7份、氨糖1.5份和六偏磷酸钠5.4份。所述韧带本体和所述的活性修饰层之间还设有中间层,所述中间层由下列重量份的组分组成:7.6份蛋清、10.5份豆蔻酰四肽、4.8份碳纳米管和2.6份聚乙烯醇。
一种活性修饰改性人工韧带的制备工艺,其包括以下步骤:
(1)按重量份称取原料:蚕丝、细菌纤维素、蜘蛛丝、明胶和超高分子量聚乙烯纤维;将蚕丝、细菌纤维素和蜘蛛丝纯化,然后溶解于10wt.%醋酸钠水溶液中,经过滤处理,得到溶液A备用;将明胶和超高分子量聚乙烯纤维置于乙酸中,加热搅拌均匀,然后加入溶液A,超声震荡,制成均匀溶液,经过纺丝挤出制备成丝束,再经编织成型制成人工韧带I;
(2)将石墨烯、磷酸四钙、蛋壳粉、四硼酸锶、透明质烷、氨糖和六偏磷酸钠置于乙酸中,超声分散均匀,制成溶液B;
(3)将蛋清、豆蔻酰四肽、碳纳米管和聚乙烯醇置于乙酸中,超声分散均匀,制成溶液C;
(4)将步骤(1)中制备的人工韧带置于溶液C中,真空干燥,并重复直至镀层厚度为6微米,在75℃下真空干燥36小时,得到人工韧带II;
(5)将步骤(4)中制备的人工韧带II置于溶液B中,真空干燥,并重复直至镀层厚度为15微米,在75℃下真空干燥28小时,即得活性修饰改性人工韧带。
对比例1
本对比例与实施例1的不同之处仅在于:本对比例中不包括中间层及其相关步骤。
对比例2
本对比例与实施例1的不同之处仅在于:本对比例中所述活性修饰层中不添加石墨烯、氨糖和透明质烷及其相关步骤。
材料的性能测试
以上各实施例和对比例所制备的韧带材料的相关性能测试结果如下表所示:
断裂强力/N | 断裂伸长率/% | 细胞粘附生长性 | |
实施例1 | 1924.7 | 36.7 | 良好 |
实施例2 | 1976.2 | 35.2 | 良好 |
实施例3 | 1989.6 | 33.4 | 良好 |
实施例4 | 1993.2 | 32.8 | 良好 |
实施例5 | 1998.4 | 31.7 | 良好 |
对比例1 | 1848.5 | 35.2 | 一般 |
对比例2 | 1815.7 | 32.9 | 一般 |
由上表可知,本发明提供的采用多层结构改性人工韧带的耐疲劳断裂性能得到大幅提升,其断裂强力达1924.7-1998.4N,断裂伸长率为361.7-36.7%,并且细胞粘附生长性良好,组织相容性较佳,可提高韧带修复速率和愈合效果,具有较佳的临床应用价值。
Claims (9)
1.一种活性修饰改性人工韧带,其特征在于,所述人工韧带包括韧带本体和置于所述韧带本体上的活性修饰层;所述韧带本体由蚕丝、细菌纤维素、蜘蛛丝、明胶和超高分子量聚乙烯纤维制备而成;所述活性修饰层由下列组分制备而成:石墨烯、磷酸四钙、蛋壳粉、四硼酸锶、透明质烷、氨糖和六偏磷酸钠。
2.根据权利要求1所述的一种活性修饰改性人工韧带,其特征在于,所述韧带本体和所述的活性修饰层之间还设有中间层,所述中间层由下列重量份的组分组成:2-9份蛋清、6-14份豆蔻酰四肽、2-7份碳纳米管和1-5份聚乙烯醇。
3.根据权利要求1或2所述的一种活性修饰改性人工韧带,其特征在于,以重量份计,所述韧带本体由11-18份蚕丝、5-14份细菌纤维素、8-17份蜘蛛丝、4-9份明胶和2-6份超高分子量聚乙烯纤维制备而成。
4.根据权利要求1或2所述的一种活性修饰改性人工韧带,其特征在于,所述活性修饰层由下列重量份的组分制备而成:石墨烯8-15份、磷酸四钙4-9份、蛋壳粉5-11份、四硼酸锶3-7份、透明质烷2-5份、氨糖1-3份和六偏磷酸钠4-8份。
5.根据权利要求1或2所述的一种活性修饰改性人工韧带,其特征在于,所述活性修饰层的厚度为10-20微米。
6.根据权利要求2所述的一种活性修饰改性人工韧带,其特征在于,所述中间层的厚度为3-8微米。
7.根据权利要求1所述的一种活性修饰改性人工韧带,其特征在于,以重量份计,所述韧带本体由12-17份蚕丝、6-12份细菌纤维素、9-15份蜘蛛丝、4.5-8.2份明胶和2.3-5份超高分子量聚乙烯纤维制备而成;
所述活性修饰层由下列重量份的组分制备而成:石墨烯8.4-13份、磷酸四钙4.5-8.6份、蛋壳粉5.3-9份、四硼酸锶3.8-6.4份、透明质烷2.8-4.5份、氨糖1.2-2.7份和六偏磷酸钠4.3-7.6份。
8.根据权利要求2所述的一种活性修饰改性人工韧带,其特征在于,所述中间层由下列重量份的组分组成:2.5-8.3份蛋清、6.4-12份豆蔻酰四肽、2.3-6.4份碳纳米管和1.8-4份聚乙烯醇。
9.一种活性修饰改性人工韧带的制备工艺,其特征在于,其包括以下步骤:
(1)按重量份称取原料:蚕丝、细菌纤维素、蜘蛛丝、明胶和超高分子量聚乙烯纤维;将蚕丝、细菌纤维素和蜘蛛丝纯化,然后溶解于10wt.%醋酸钠水溶液中,经过滤处理,得到溶液A备用;将明胶和超高分子量聚乙烯纤维置于乙酸中,加热搅拌均匀,然后加入溶液A,超声震荡,制成均匀溶液,经过纺丝挤出制备成丝束,再经编织成型制成人工韧带I;
(2)将石墨烯、磷酸四钙、蛋壳粉、四硼酸锶、透明质烷、氨糖和六偏磷酸钠置于乙酸中,超声分散均匀,制成溶液B;
(3)将蛋清、豆蔻酰四肽、碳纳米管和聚乙烯醇置于乙酸中,超声分散均匀,制成溶液C;
(4)将步骤(1)中制备的人工韧带置于溶液C中,真空干燥,并重复直至镀层厚度为3-8微米,在60-80℃下真空干燥24-48小时,得到人工韧带II;
(5)将步骤(4)中制备的人工韧带II置于溶液B中,真空干燥,并重复直至镀层厚度为10-20微米,在60-80℃下真空干燥24-48小时,即得活性修饰改性人工韧带。
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