CN114214838B - 一种蚕丝/凝胶多向纤维夹芯半月板及其制备方法 - Google Patents
一种蚕丝/凝胶多向纤维夹芯半月板及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种蚕丝/凝胶多向纤维夹芯半月板及其制备方法,属于功能材料领域。本发明所述的制备半月板的方法,包括如下步骤:(1)通过机织的方法编织半月板预制体:(2)将丝胶粉和过氧化氢按照质量比1‑2:100混合进行交联反应,得到第一水凝胶;将透明质酸、壳聚糖、水按照质量比1‑3:1‑3:100混合均匀,得到第二水凝胶;将第一水凝胶和第二水凝胶按照体积比1‑3:1混合均匀,得到凝胶溶液;(3)将半月板预制体先脱胶,之后浸渍凝胶溶液,取出,定型,干燥,得到所述的蚕丝/凝胶多向纤维夹芯半月板。本发明中半月板的拉伸刚度达到0.3N以上,弹性模量达到70MPa以上,孔隙率在94%以上。
Description
技术领域
本发明涉及一种蚕丝/凝胶多向纤维夹芯半月板及其制备方法,属于功能材料领域。
背景技术
众所周知,半月板(软骨)机体中膝关节的重要解剖结构之一,具有稳定传到机体负重、缓冲压力、增大软骨接触面积、维持膝关节稳定性以及营养润滑关节软骨等作用。随着人口老龄化以及人们运动的增加,半月板损伤患者数量与日俱增,且半月板由于其特殊的血供分布特点,导致其纤维软骨组织容易高度分化,自身修复的能力较弱,导致损伤后再生能力不足,难以自行修复。半月板主要由纤维软骨组织构成,位于膝关节胫骨平台与股骨髁的间隙内,它在膝关节的稳定性方面有重要的作用。目前临床上多采用关节镜下半月板损伤缝合修复手术,对于半月板无血供区和复杂性损伤无法修复者,进行半月板全切术或次全切术,半月板切除会导致膝关节应力集中和负荷传导紊乱。
近年来,为了避免继发性骨关节炎的发生,进而加重痛感和病情,国内外许开始关注半月板重建术。目前,半月板重建术的方式包括:同种异体半月板和人工替代物。然而,同种异体半月板存在移植物来源不足、匹配困难、组织保存困难、具有疾病传播风险、免疫排斥反应和高昂费用等问题。人工合成材料相较于天然材料优势明显:第一,人工材料可通过控制聚合物分子量及组成控制水解等降解速度。第二,避免产生毒素物质,人工合成材料分解后产生的乙酸或者乙醇酸可随着机体代谢作用排出体外,有利于保持机体不受侵害。第三,人工合成材料具有良好的可塑性,可在一定的热力条件下按需加工出不同形状。因此,人工半月板成为理想候选方法。
当前,国外涉及人工半月板公司主要包括美国Ivy Sports Medicine、英国Qrteq和美国Active Implants等公司。其中,美国Ivy Sports Medicine公司对应产品为CIM,选用胶原作为原材料,但仅作为部分修复材料;英国Qrteq公司对应产品为Atifit,选用聚己内酯/聚氨酯,为降解性合成材料,但产生少量有毒二元胺,且聚氨酯1.5年降解50%;美国Active Implants公司对应产品为NUsurface,选用聚碳酸酯聚氨酯,然而临床表明,并发症及短期失败率高,临床应用不广泛,且过大尺寸容易引起中压和位移大于天然半月板。
国内专利200720131799.3,设计的半月板由蚕丝通过钩编而成,并包裹I型胶原;专利201710999938.2中,半月板支架由蚕丝经传统编织方法单层编织后层层堆积串联而成,并通过浇注方式固形,包裹固形材料如胶原、聚乙烯醇水凝胶、聚氨酯;但是这些采用的水凝胶、I型胶原和胶原等材料组织相容性较差,力学性能不佳。
发明内容
[技术问题]
目前制备的半月板材料力学性能差,会产生少量毒素,适用范围有限。
[技术方案]
为了解决上述问题,本发明通过蚕丝直接净成形成多向夹芯立体纤维半月板;其次,外浸渍水凝胶,形成蚕丝/凝胶多向纤维夹芯半月板。本发明的蚕丝/凝胶多向纤维夹芯半月板可满足支架材料无毒、材料降解产物无毒、拉伸刚度0.2-0.5N、弹性模量10-100MPa、材料降解速度与自身组织生成速度匹配、长期维持结构稳定性等需求,且支架可与周围组织缝合,保持结构及稳定性。
本发明的第一个目的是提供一种制备蚕丝/凝胶多向纤维夹芯半月板的方法,包括如下步骤:
(1)通过机织的方法编织半月板预制体
所述的半月板预制体为三层结构,以蚕丝纤维网为芯层,上、下层为蚕丝平纹织物;之后通过蚕丝纱线缝合为一个整体,且芯层的厚度为1-3mm,缝合点之间的距离为4-6mm;所述的半月板预制体形状类似为“C”型,整体截面为内侧低、外侧高的楔形结构;
(2)制备凝胶溶液
将丝胶粉和过氧化氢按照质量比1-2:100混合进行交联反应,得到第一水凝胶;
将透明质酸、壳聚糖、水按照质量比1-3:1-3:100混合均匀,得到第二水凝胶;
将第一水凝胶和第二水凝胶按照体积比1-3:1混合均匀,得到凝胶溶液;
(3)制备蚕丝/凝胶多向纤维夹芯半月板
将步骤(1)的半月板预制体先脱胶,之后浸渍步骤(2)的凝胶溶液,取出,定型,干燥,得到所述的蚕丝/凝胶多向纤维夹芯半月板。
在本发明的一种实施方式中,步骤(1)所述的蚕丝纱的原料选用新产的秋蚕茧,茧身洁白、饱满,质量等级为A5。
在本发明的一种实施方式中,步骤(1)所述的蚕丝纤维网的规格为10-30g/m2。
在本发明的一种实施方式中,步骤(1)所述的蚕丝纱的规格为150-250tex。
在本发明的一种实施方式中,步骤(1)所述的蚕丝平纹织物编织采用的蚕丝纱的规格为150-250tex。
在本发明的一种实施方式中,步骤(2)所述的丝胶粉的规格为60-100目,纯度大于99%。
在本发明的一种实施方式中,步骤(2)所述的过氧化氢为质量分数为30%的过氧化氢水溶液。
在本发明的一种实施方式中,步骤(2)所述的交联反应的条件为300-500rpm、常温(20-30℃)反应15-40s。
在本发明的一种实施方式中,步骤(2)所述的透明质酸、壳聚糖、水的混合均匀为300-500rpm、常温(20-30℃)反应15-30min。
在本发明的一种实施方式中,步骤(1)所述的壳聚糖的乙酰度大于95%,黏度为150~200MPa·s;透明质酸的分子量为40-130万,纯度为98%以上。
在本发明的一种实施方式中,步骤(2)所述的第一水凝胶和第二水凝胶的混合均匀为100-300rpm、常温(20-30℃)反应15-20min。
在本发明的一种实施方式中,步骤(3)所述的脱胶是将半月板预制体置于质量分数为0.5%的Na2CO3溶液中煮沸30min,后用水彻底冲洗以去除丝胶和残留碳酸钠。
在本发明的一种实施方式中,步骤(3)所述的浸渍是常温(20-30℃)浸渍5-10min。
在本发明的一种实施方式中,步骤(3)所述的定型是采用模具将浸渍凝胶溶液的预制体定型。
在本发明的一种实施方式中,步骤(3)所述的干燥是在50-70℃下干燥3-4h。
本发明的第二个目的是本发明所述的方法制备得到的蚕丝/凝胶多向纤维夹芯半月板。
[有益效果]
(1)本发明采用蚕丝纤维和水凝胶材料制备的夹芯半月板结构,具有生物相容性良好、免疫性低、降解速度适中且力学性能优异,是作为半月板支架的理想材料之一。
(2)本发明的蚕丝/凝胶多向纤维夹芯半月板具有较高的孔隙率,具有与正常半月板相似的生物力学性能,且可降解支架无毒性,蚕丝纤维和水凝胶材料及其降解产物不会引起免疫排斥反应。
(3)本发明所述的蚕丝/凝胶多向纤维夹芯半月板的制备方法不受产品尺寸和形状限制,设备简单、投资少、见效快,且工艺简单、生产技术易掌握。
(4)本发明的蚕丝/凝胶多向纤维夹芯半月板利于运输,传递力、减震、关节润滑,维持关节稳定性。
(5)本发明的蚕丝/凝胶多向纤维夹芯半月板的拉伸刚度达到0.3N以上,弹性模量达到70MPa以上,孔隙率在94%以上,且8周降解率达到14.6%以上。
附图说明
图1为本发明所述的蚕丝/凝胶多向纤维夹芯半月板的结构示意图,其中1为半月板结构;2为蚕丝纤维多向夹芯立体半月板预制体局部。
具体实施方式
以下对本发明的优选实施例进行说明,应当理解实施例是为了更好地解释本发明,不用于限制本发明。
实施例中蚕丝纱的原料选用新产的秋蚕茧,茧身洁白、饱满,质量等级为A5;壳聚糖的乙酰度大于95%,黏度为150~200MPa·s;透明质酸的分子量为110万,纯度为98%以上。
测试方法:
1、拉伸模量测试:根据国标GB/T528-2009《硫化橡胶或热塑性橡胶拉伸应力应变性能的测定》进行力学性能测试。本实验采用Instron 5982电子万能材料试验机进行拉伸测试实验,拉伸速率为200mm/min,每次测量采用5个样品,平行测量取平均值。
2、弹性模量测试:根据国标GB/T 7757-2009《硫化橡胶或热塑性橡胶压缩应力应变性能的测定》进行压缩模量测试。采用电子万能试验机(珠海三思试验设备有限公司,CMT4204型)进行压缩实验,以10mm/min的速度压缩各试样,直至应变达到25%为止,继而以相同的速度放松试样。如此重复压缩和放松三次,以四次压缩周期为一个连续的程序,记录力-变形曲线。四次压缩周期中,前三次视为机械调节,第四次作为正式实验。每次测量采用5个试样进行平行实验,结果取平均值。
3、孔隙率测试:选10个样品,将它们浸泡于水中至24小时,保证样品的充分浸透后,以滤纸把样品表面的水分迅速擦掉,随后称重;然后,将样品放于70℃真空干燥箱内12小时后称重。孔隙率用公式(1)来计算。
其中,ε是孔隙率,mwet和mdry分别代表浸水时和干燥后的样品质量,ρ代表水的密度,s代表半月板面积,d是半月板厚度,样品的孔隙率通过计算10个样品的孔隙率求均值得到。
4、降解测试:每组取3个样品,称取重量标记为(W0),然后将样品浸泡于磷酸缓冲盐溶液中,放置于37℃孵箱内,待半月板彻底被浸透后,分别于2、4、6、8周取出,用去离子水冲洗干净,然后冻干,半月板干重被记录为W1。
半月板降解率根据公式(2)计算得出
降解率=(W0-W1)/W0×100% (2)
实施例1
一种制备蚕丝/凝胶多向纤维夹芯半月板的方法,包括如下步骤:
(1)通过机织的方法编织半月板预制体
所述的半月板预制体为三层结构,以蚕丝纤维网(30g/m2)为芯层,上、下层为1/1蚕丝平纹织物(蚕丝纱线的规格为200tex);之后通过蚕丝纱线(200tex)缝合为一个整体,且芯层的厚度为2mm,缝合点之间的距离为5mm;所述的半月板预制体形状类似为“C”型,整体截面为内侧低、外侧高的楔形结构;
(2)制备凝胶溶液
将丝胶粉(80目,纯度大于99%)和质量分数为30%的过氧化氢水溶液按照质量比1.5:100混合,在400rpm、25℃下进行交联反应30s,得到第一水凝胶;
将透明质酸、壳聚糖、水按照质量比2:2:100,在400rpm、25℃反应20min,得到第二水凝胶;
将第一水凝胶和第二水凝胶按照体积比1:1,在100rpm、25℃)反应15min,得到凝胶溶液;
(3)制备蚕丝/凝胶多向纤维夹芯半月板
将步骤(1)的半月板预制体置于质量分数为0.5%的Na2CO3溶液中煮沸30min,后用水彻底冲洗以去除丝胶和残留碳酸钠,重复两次后置于70℃干燥箱中烘干;
之后在25℃浸渍步骤(2)的凝胶溶液5min,取出,采用模具定型,和模具一起在在55℃烘箱中放置3h,得到所述的蚕丝/凝胶多向纤维夹芯半月板。
实施例2
调整实施例1步骤(2)中丝胶粉(80目,纯度大于99%)和质量分数为30%的过氧化氢水溶液的质量比为1:1;其他和实施例1保持一致,得到蚕丝/凝胶多向纤维夹芯半月板。
实施例3
调整实施例1步骤(2)中丝胶粉(80目,纯度大于99%)和质量分数为30%的过氧化氢水溶液的质量比为2:1;其他和实施例1保持一致,得到蚕丝/凝胶多向纤维夹芯半月板。
实施例4
调整实施例1步骤(2)中第一水凝胶和第二水凝胶的体积比为2:1;其他和实施例1保持一致,得到蚕丝/凝胶多向纤维夹芯半月板。
实施例5
调整实施例1步骤(1)中芯层的厚度为3mm;其他和实施例1保持一致,得到蚕丝/凝胶多向纤维夹芯半月板。
对比例1
调整实施例1步骤(1)中的蚕丝纤维网(30g/m2)为1/1蚕丝平纹织物;其他和实施例1保持一致,得到半月板。
对比例2
省略实施例1步骤(1)中的蚕丝纤维网(30g/m2);其他和实施例1保持一致,得到半月板。
对比例3
省略实施例1步骤(2)中的第一凝胶;仅采用第二凝胶,其他和实施例1保持一致,得到半月板。
对比例4
省略实施例1步骤(2)中的第二凝胶;仅采用第一凝胶,其他和实施例1保持一致,得到半月板。
对比例5
省略实施例1步骤(3)中的脱胶,其他和实施例1保持一致,得到半月板。
将实施例1-5和对比例1-5得到的半月板进行测试,测试结果如下:
表1
例 | 拉伸刚度(N) | 弹性模量(MPa) | 孔隙率(%) |
实施例1 | 0.5 | 80 | 97 |
实施例2 | 0.4 | 72 | 95 |
实施例3 | 0.4 | 73 | 94 |
实施例4 | 0.4 | 76 | 95 |
实施例5 | 0.3 | 70 | 98 |
对比例1 | 0.6 | 81 | 88 |
对比例2 | 0.2 | 68 | 99 |
对比例3 | 0.1 | 60 | 90 |
对比例4 | 0.2 | 50 | 90 |
对比例5 | 0.01 | 30 | 99 |
表2
降解率(%) | 2周 | 4周 | 6周 | 8周 |
实施例1 | 3.1 | 5.3 | 12.1 | 14.6 |
实施例2 | 2.7 | 4.1 | 9.1 | 10.4 |
实施例3 | 3.2 | 3.9 | 5.1 | 5.7 |
实施例4 | 2.3 | 4.4 | 10.8 | 12.6 |
实施例5 | 2.8 | 5.3 | 11.4 | 12.1 |
对比例1 | 1.1 | 3.4 | 7.2 | 9.1 |
对比例2 | 1.5 | 4.2 | 8.6 | 10.3 |
对比例3 | 3.2 | 6.1 | 12.5 | 15.1 |
对比例4 | 2.6 | 3.1 | 5.7 | 9.6 |
对比例5 | 0.5 | 2.2 | 3.4 | 6.3 |
虽然本发明已以较佳实施例公开如上,但其并非用以限定本发明,任何熟悉此技术的人,在不脱离本发明的精神和范围内,都可做各种的改动与修饰,因此本发明的保护范围应该以权利要求书所界定的为准。
Claims (5)
1.一种制备蚕丝/凝胶多向纤维夹芯半月板的方法,其特征在于,包括如下步骤:
(1)通过机织的方法编织半月板预制体
所述的半月板预制体为三层结构,以蚕丝纤维网为芯层,上、下层为蚕丝平纹织物;之后通过蚕丝纱线缝合为一个整体,且芯层的厚度为1-3mm,缝合点之间的距离为4-6mm;所述的半月板预制体形状类似为“C”型,整体截面为内侧低、外侧高的楔形结构;
(2)制备凝胶溶液
将丝胶粉和过氧化氢按照质量比1-2:100混合进行交联反应,得到第一水凝胶;
将透明质酸、壳聚糖、水按照质量比1-3:1-3:100混合均匀,得到第二水凝胶;
将第一水凝胶和第二水凝胶按照体积比1-3:1混合均匀,得到凝胶溶液;
(3)制备蚕丝/凝胶多向纤维夹芯半月板
将步骤(1)的半月板预制体先脱胶,之后浸渍步骤(2)的凝胶溶液,取出,定型,干燥,得到所述的蚕丝/凝胶多向纤维夹芯半月板;
其中,步骤(1)所述的蚕丝纤维网的规格为10-30g/m2;
步骤(2)所述的交联反应的条件为300-500rpm、20-30℃反应15-40s;
步骤(2)所述的透明质酸、壳聚糖、水的混合均匀为300-500rpm、20-30℃反应15-30min;
步骤(3)所述的脱胶是将半月板预制体置于质量分数为0.5%的Na2CO3溶液中煮沸30min,后用水彻底冲洗以去除丝胶和残留碳酸钠;
步骤(3)所述的浸渍是20-30℃浸渍5-10min。
2.根据权利要求1所述的方法,其特征在于,步骤(1)所述的蚕丝纱的规格为150-250tex。
3.根据权利要求1所述的方法,其特征在于,步骤(2)所述的第一水凝胶和第二水凝胶的混合均匀为100-300rpm、20-30℃反应15-20min。
4.根据权利要求1所述的方法,其特征在于,步骤(3)所述的干燥是在50-70℃下干燥3-4h。
5.权利要求1-4任一项所述的方法制备得到的蚕丝/凝胶多向纤维夹芯半月板。
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