CN109550072A - 吸液溶胀的海藻酸盐壳聚糖复合纤维及其制备方法和应用 - Google Patents
吸液溶胀的海藻酸盐壳聚糖复合纤维及其制备方法和应用 Download PDFInfo
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- CN109550072A CN109550072A CN201811217466.1A CN201811217466A CN109550072A CN 109550072 A CN109550072 A CN 109550072A CN 201811217466 A CN201811217466 A CN 201811217466A CN 109550072 A CN109550072 A CN 109550072A
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- alginate
- chitosan
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Classifications
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- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/46—Deodorants or malodour counteractants, e.g. to inhibit the formation of ammonia or bacteria
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- A—HUMAN NECESSITIES
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Abstract
本发明公开了一种吸液溶胀的海藻酸盐壳聚糖复合纤维及其制备方法和应用。本发明是由海藻酸盐水溶液在凝固浴中通过凝固的方法制备而成,海藻酸盐水溶液的质量浓度为3‑6%;凝固浴包括以下重量份的组分:低聚壳聚糖1‑6份,草珊瑚提取物0.1‑1份,薄荷提取物0‑1份,透明质酸0‑1份,冰片0‑1份,氯化钙溶液或钙离子缓释体系90‑100份,氯化钙溶液或钙离子缓释体系的质量浓度为0.1‑2.0%;本发明还给出了上述复合纤维的制备方法。本发明的低聚壳聚糖等有效成分在复合纤维中的分布均匀,复合纤维吸液倍数高,有效成分吸收充分,用于伤口修复,可以为伤口愈合的不同时期提供不同的护理环境,杀菌消炎作用好,伤口愈合快。
Description
技术领域
本发明属于生物医用材料的技术领域,特别是指一种吸液溶胀的海藻酸盐壳聚糖复合纤维及其制备方法和应用。
背景技术
海藻酸是一种天然多糖,其化学组成为β-D-甘露糖醛酸(M)和a-L-古罗糖醛酸(G)经过1,4键合形成的线型共聚物,G和M在海藻酸中的含量对纤维的成胶性能有明显的影响;海藻酸在自然状态下存在于胞质中,起着强化细胞壁的作用,海藻酸与海水中各种阳离子结合成为各种海藻酸盐。以海藻酸为原料,通过湿法纺丝制备的海藻酸纤维,可以应用于纺织、服装、医疗卫生等领域,是一种具有很高附加值的功能纤维材料。作为医用敷料,海藻酸纤维从20世纪以来,就被西方医疗界广泛应用,二十世纪七十年代初期,美国FDA已将海藻酸作为“公认安全物质”的食品和药品添加剂,海藻酸基生物材料作为伤口敷料等产品已通过FDA批准上市。在创面止血领域,海藻酸敷料是临床普遍应用的创伤敷料之一,其临床效果已得到证实,并且由于其资源丰富、价格低廉、安全低风险,因此已成为临床外科止血的必选材料之一。
伤口的愈合是一个持续不断的过程,对大多数伤口来说,愈合过程一般分为四个时期,(1)出血期:在受伤的组织缺口出现局部出血和渗液,血液中的胶原蛋白促进凝血,从而伤口处会形成一个凝块,这个凝块包含了血液的各种细胞及成分;(2)充血期:由于组织液中的化学物质或缺氧引起小动脉扩张,血液流量和淋巴液流量会增加起来,各种血液细胞及游走细胞将会进入损伤发炎的地方,进入发炎区域的巨噬细胞出来吞噬细菌,结果被吞噬的细菌、异物及已坏死的组织聚集成脓,此脓液可以经由开放的伤口排出体外;(3)肉芽期:毛细血管的增殖使伤口潮红且隆起成为肉芽组织,在此肉芽期中会有自溶作用,坏死组织的移除以及组织再生作用均同时进行着,上皮组织增生;(4)收缩期:此时期由于覆在伤口上的细胞成熟,而使伤口收缩,因此使得伤口的边缘靠近而愈合,最后形成瘢痕,从而使创面愈合。
对大面积皮肤创伤病人来说,尤其是慢性伤口表面会有大量渗出液,由于皮内组织暴露在外,很容易被细菌感染,导致伤口愈合慢,甚至感染死亡。海藻酸盐纤维做成的辅料可以有效封闭创面,高吸湿性可以加速生长因子向伤口集中而促进伤口愈合。但是,因为海藻酸盐本身没有抑菌抗菌性,不能有效的抑制真菌和细菌的生长,因此,急需寻找理想的创面敷盖物,尽早封闭创面,减少由创面致病菌引起的感染和毒血症,提高严重创伤的成活率。
壳聚糖及其衍生物已被各国学者研究证实,具有生物活性和生物相容性,具有天然的抑菌,消炎,止血,促进伤口愈合,减少伤口疤痕的功能,应用于医疗领域,是现代敷料的理想材料。但是,现有的用于伤口处理的海藻酸壳聚糖医用敷料,由于所用的壳聚糖分子比较大,壳聚糖很难进入到纤维内部,只是在医用敷料的表面,其吸收速度慢,持续抑菌灭菌效果差,使得伤口愈合速度慢。
发明内容
本发明提供一种吸液溶胀的海藻酸盐壳聚糖复合纤维及其制备方法和应用,解决了现有技术中的海藻酸壳聚糖医用敷料存在吸收慢、抑菌灭菌效果差而影响伤口愈合的问题。
本发明的一种吸液溶胀的海藻酸盐壳聚糖复合纤维,其主要是通过以下技术方案加以实现的:所述复合纤维是由海藻酸盐水溶液在凝固浴中通过凝固的方法制备而成,所述海藻酸盐水溶液的质量浓度为3-6%;所述凝固浴包括以下重量份的组分:低聚壳聚糖1-6份,草珊瑚提取物0.1-1份,薄荷提取物0-1份,透明质酸0-1份,冰片0-1份,氯化钙溶液或钙离子缓释体系90-100份,氯化钙溶液或钙离子缓释体系的质量浓度为0.1-2.0%。
本发明利用低聚壳聚糖,其分子小,容易吸收,将低聚壳聚糖、草珊瑚提取物、薄荷提取物、透明质酸和冰片多种有效成分进行复配,匹配科学合理,有效成分相辅相成,相互促进,在氯化钙溶液或钙离子缓释体系中制成凝固浴,并将海藻酸盐水溶液利用喷丝技术在凝固浴内形成复合纤维,这使得低聚壳聚糖等有效成分在复合纤维中的分布均匀;所得的复合纤维吸液倍数高,有效成分吸收充分,用于伤口修复,可以为伤口愈合的不同时期提供不同的护理环境,有效地抑制了真菌和细菌的生长,杀菌消炎作用好,伤口愈合快。
本发明在海藻酸盐壳聚糖复合纤维中添加了不同功能性材料,可以用在伤口愈合的不同时期。草珊瑚提取物有抗菌消炎,活血止痛,有缓解缩小肿胀的作用;薄荷提取物在皮肤黏膜上作用能够起到镇定止痒的作用;透明质酸抗炎,抑菌,直接促进细胞的生长、分化、重建与修复,提高伤口愈合能力,减少瘢痕;冰片消炎止痛,对液体的渗出和组织水肿等炎肿过程有抑制作用。在这种复合纤维产品中各组分的重量份为:海藻酸盐60-90份,低聚壳聚糖1-20份,草珊瑚提取物0.1-5份,钙离子5-15份,薄荷提取物0-5份,透明质酸0-5份,冰片0-5份。本发明的海藻酸盐壳聚糖复合纤维在与创面渗出液接触时,通过离子交换,使纤维中的钙离子部分或全部交换,使不溶性的海藻酸钙纤维转变成溶胀性的海藻酸盐,不仅能吸收大量的液体,还能为伤口的愈合提供一个湿润的环境;作为一种医用辅料,本发明的海藻酸盐壳聚糖复合纤维具有高吸湿性、易揭除性、高透氧性、凝胶阻塞性、生物降解和生物相容性,吸液倍数可达到40倍以上。
作为一种优选的实施方案,所述凝固浴包括以下重量份的组分:低聚壳聚糖1-6份,草珊瑚提取物0.1-1份,薄荷提取物0-0.5份,透明质酸0-0.5份,冰片0.5-1份,氯化钙溶液或钙离子缓释体系90-100份,氯化钙溶液或钙离子缓释体系的质量浓度为0.1-1.0%。本发明通过原料的凝固浴中各组分的调配,得到一种吸液倍数为中等及以上并具有杀菌止血和消肿去痛的作用,可用于伤口愈合的出血期和充血期。
作为一种优选的实施方案,所述凝固浴包括以下重量份的组分:低聚壳聚糖1-6份,草珊瑚提取物0.1-1份,薄荷提取物0.5-1份,透明质酸0.5-1份,冰片0-0.5份,氯化钙溶液或钙离子缓释体系90-100份,氯化钙溶液或钙离子缓释体系的质量浓度为1.0-2.0%。本发明通过原料的凝固浴中各组分的调配,还可以得到一种吸液倍数略低并具有镇定止痒、刺激细胞增殖和促进伤口愈合的作用,可用于伤口愈合的肉芽期和收缩期。
作为一种优选的实施方案,所述低聚壳聚糖的制备方法为:取脱乙酰度≥90%的壳聚糖,加入到去离子水中,使壳聚糖含量为1-15%w/v;添加双氧水,双氧水与壳聚糖的摩尔比为5:1-1:1,升温至50-80℃,持续反应4-6h,过滤,冷冻干燥,得低聚壳聚糖。本发明采用双氧水降解壳聚糖,可以得到活性壳聚糖低聚体,降解在中性条件下进行,不产生无机盐,对设备耐腐蚀性能要求低;这里使用的双氧水的质量浓度为30%,壳聚糖含量的单位是g/mL,即壳聚糖含量为15%w/v是指100mL去离子水中有15g的壳聚糖。
作为一种优选的实施方案,所述海藻酸盐为海藻酸钠、海藻酸钾、海藻酸铵中的一种或几种。本发明的这些海藻酸盐容易形成纺丝溶液,这些纺丝溶液在凝固浴中成型速度快,制备方便,所得纤维韧性好,吸液能力强。
作为一种优选的实施方案,所述钙离子缓释体系为硫酸钙/葡萄糖酸内酯体系、碳酸钙/葡萄糖酸内酯体系、磷酸二钙/葡萄糖酸内酯体系、葡萄糖酸钙溶液中的一种或几种。本发明还可以采用钙离子缓释体系制备凝固浴,这些体系均可以形成均匀的凝固浴,有利于海藻酸盐的纺丝溶液在其内成型。
本发明的一种吸液溶胀的海藻酸盐壳聚糖复合纤维的制备方法,其主要是通过以下技术方案加以实现的:包括以下步骤:1)取氯化钙水溶液或钙离子缓释体系,加入低聚壳聚糖,搅拌,调节pH值,使其pH值为4.5-6.2,加入草珊瑚提取物、薄荷提取物、透明质酸和冰片,混合均匀,得凝固浴;2)取海藻酸盐,加入去离子水中,在20-25℃下,搅拌4-6h,过滤,静置脱泡,静置脱泡时间为24-48h,得海藻酸盐溶液;3)将步骤2)所得的海藻酸盐溶液经过喷丝板喷入步骤1)所得的凝固浴中,凝固浴温度为15-25℃,牵伸,水洗,干燥,得海藻酸盐-壳聚糖复合纤维。
本发明的氯化钙水溶液或钙离子缓释体系可以是现场配制的,也可以是直接购置的现有产品,低聚壳聚糖加入其中之后,经过搅拌,使其充分溶解,调节pH值,再添加其它有效成分,将海藻酸盐的纺丝溶液喷丝到凝固浴中而得到;通过调整凝固浴中钙离子和有效成分的含量,可以有效控制纤维的吸液倍数,为伤口不同的时期及不同的伤口类型提供不同的护理环境,步骤2)中过滤包括粗滤、一滤和二滤,步骤3)中牵伸包括一牵和二牵;本发明的制备方法简单,控制方便,通过工艺参数的控制,可以控制吸液倍数,得到了一种性能良好的具有吸液溶胀性能的海藻酸盐壳聚糖复合纤维,可以为伤口愈合的不同时期提供不同的护理环境,例如:对于伤口渗出液较多的出血期和充血期,该复合纤维以吸液倍数高和抗菌消炎止痛为主,对于伤口渗液减少、肉芽组织形成、上皮细胞增生、伤口收缩以及最终形成瘢痕的肉芽期和收缩期,由于这个时期的伤口会出现瘙痒,此时复合纤维以抗菌消炎止痒为主;本发明的复合纤维对水的吸收能力可为≤25g/g、25-40g/g和≥40g/g三个等级,对生理盐水的吸收能力为22-26g/g,通过调整纺丝的线密度,可以控制壳聚糖在复合纤维中的含量,通过在凝固浴中添加不同的功能性材料,使复合纤维具有不同的功能,满足伤口愈合的不同时期对伤口辅料的不同需求。
作为一种优选的实施方案,所述步骤3)中水洗采用的是去离子水洗涤,去离子水的温度为20-40℃。本发明在制备过程中均采用无菌的去离子水,避免对复合纤维造成二次污染;在水洗的时候,调整去离子水的温度,使洗涤更加彻底干净。
作为一种优选的实施方案,所述步骤1)中采用酸调节pH值,所述酸为盐酸、醋酸、柠檬酸、硫酸、硝酸中的一种或几种。本发明采用这些小分子酸对凝固浴的pH值进行调整,使壳聚糖分子中的大部分氨基被质子化,—NH2转变成—NH3 +,—NH3 +可以和海藻酸盐分子中的—COO-交联,产生静电作用,还有大分子之间的范德华力、氢键等多种作用,增强复合纤维的性能。
本发明的一种吸液溶胀的海藻酸盐壳聚糖复合纤维的应用,其主要是通过以下技术方案加以实现的:所述海藻酸盐壳聚糖复合纤维用于伤口修复。本发明的壳聚糖分子量小,易于吸收,低聚壳聚糖与草珊瑚提取物、薄荷提取物、透明质酸和冰片有效匹配,用于伤口修复,具有很好的抑菌止血、消炎去痛和镇定止痒的效果,伤口愈合速度快,创面愈合效果好。
与现有技术相比,本发明的有益效果是:本发明的低聚壳聚糖,容易吸收,低聚壳聚糖与草珊瑚提取物、薄荷提取物、透明质酸和冰片等多种功能性材料复配,在氯化钙溶液或钙离子缓释体系中制成凝固浴,并将海藻酸盐水溶液利用喷丝技术在凝固浴内形成复合纤维,低聚壳聚糖等功能性材料在复合纤维中的分布均匀;所得的复合纤维吸液倍数高,可以吸收大量伤口渗出液,有效成分吸收充分,有很好的机械和力学性能,用于伤口修复,具有很好的抑菌止血、消炎去痛和镇定止痒的效果,可以为伤口愈合的不同时期提供不同的护理环境,伤口愈合快。本发明的制备方法简单,控制方便,通过工艺参数的控制,可以控制吸液倍数,成本低,得到了一种性能良好的具有吸液溶胀性能的海藻酸盐壳聚糖复合纤维。
具体实施方式
下面将结合本发明的具体实施例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作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。
本发明的一种吸液溶胀的海藻酸壳聚糖复合纤维,所述复合纤维是由海藻酸盐水溶液在凝固浴中通过凝固的方法制备而成,所述海藻酸盐水溶液的质量浓度为3-6%;所述凝固浴包括以下重量份的组分:低聚壳聚糖1-6份,草珊瑚提取物0.1-1份,薄荷提取物0-1份,透明质酸0-1份,冰片0-1份,氯化钙溶液或钙离子缓释体系90-100份,氯化钙溶液或钙离子缓释体系的质量浓度为0.1-2.0%。
优选地,所述凝固浴包括以下重量份的组分:低聚壳聚糖1-6份,草珊瑚提取物0.1-1份,薄荷提取物0-0.5份,透明质酸0-0.5份,冰片0.5-1份,氯化钙溶液或钙离子缓释体系90-100份,氯化钙溶液或钙离子缓释体系的质量浓度为0.1-1.0%。
再次优选地,所述凝固浴包括以下重量份的组分:低聚壳聚糖1-6份,草珊瑚提取物0.1-1份,薄荷提取物0.5-1份,透明质酸0.5-1份,冰片0-0.5份,氯化钙溶液或钙离子缓释体系90-100份,氯化钙溶液或钙离子缓释体系的质量浓度为1.0-2.0%。
进一步地,所述低聚壳聚糖的制备方法为:取脱乙酰度≥90%的壳聚糖,加入去离子水中,使壳聚糖含量为1-15%w/v;添加双氧水,双氧水与壳聚糖的摩尔比为5:1-1:1,升温至50-80℃,持续反应4-6h,过滤,冷冻干燥,得低聚壳聚糖。
具体地,所述海藻酸盐为海藻酸钠、海藻酸钾、海藻酸铵中的一种或几种。
再具体地,所述钙离子缓释体系为硫酸钙/葡萄糖酸内酯体系、碳酸钙/葡萄糖酸内酯体系、磷酸二钙/葡萄糖酸内酯体系、葡萄糖酸钙溶液中的一种或几种。
本发明的一种吸液溶胀的海藻酸盐-壳聚糖复合纤维的制备方法,包括以下步骤:
1)取氯化钙水溶液或钙离子缓释体系,加入低聚壳聚糖,搅拌,调节pH值,使其pH值为4.5-6.2,加入草珊瑚提取物、薄荷提取物、透明质酸和冰片,混合均匀,得凝固浴;
2)取海藻酸盐,加入去离子水中,在20-25℃下,搅拌4-6h,过滤,静置脱泡,静置脱泡时间为24-48h,得海藻酸盐溶液;
3)将步骤2)所得的海藻酸盐溶液经过喷丝板喷入步骤1)所得的凝固浴中,凝固浴温度为15-25℃,牵伸,水洗,干燥,得海藻酸盐壳聚糖复合纤维。
优选地,所述步骤3)中水洗采用的是去离子水洗涤,去离子水的温度为20-40℃。
具体地,所述步骤1)中采用酸调节pH值,所述酸为盐酸、醋酸、柠檬酸、硫酸、硝酸中的一种或几种。
本发明的一种吸液溶胀的海藻酸盐-壳聚糖复合纤维的应用,所述海藻酸盐壳聚糖复合纤维用于伤口修复。
实施例一
本发明的一种吸液溶胀的海藻酸盐-壳聚糖复合纤维的制备方法,包括以下步骤:
1)凝固浴的配制
取氯化钙,溶解于去离子水,制成浓度为1.10%w/v(g/mL)的氯化钙水溶液,加入低聚壳聚糖,搅拌,加入适量的稀盐酸溶液,调节pH值,使其pH值为4.98,加入草珊瑚提取物、薄荷提取物和透明质酸,搅拌,混合均匀,得凝固浴;
低聚壳聚糖的添加量为去离子水的体积的5%w/v(g/mL),草珊瑚提取物的添加量为去离子水的体积的0.5%w/v(g/mL),薄荷提取物的添加量为去离子水的体积的0.6%w/v(g/mL),透明质酸的添加量为去离子水的体积的0.6%w/v(g/mL);
2)海藻酸盐纺丝溶液的配制
取海藻酸钠,加入去离子水中,配置成质量浓度为4%的海藻酸钠溶液,在20℃下,搅拌4h,过滤,静置脱泡,静置脱泡时间为24h,得海藻酸钠溶液;
3)复合纤维的制备
将步骤2)所得的海藻酸钠溶液经过喷丝板挤入步骤1)所得的凝固浴中,凝固浴温度为20℃,喷丝板孔径为7μm,两道牵伸,水洗,上油、纤维装盘,冷冻干燥,得海藻酸盐壳聚糖复合纤维。
实施例二
本发明的一种吸液溶胀的海藻酸盐-壳聚糖复合纤维的制备方法,包括以下步骤:
1)凝固浴的配制
取葡萄糖酸钙,溶解于去离子水,制成浓度为0.8%w/v(g/mL)的葡萄糖酸钙溶液,加入低聚壳聚糖,搅拌,加入适量的醋酸溶液,调节pH值,使其pH值为5.1,加入草珊瑚提取物、透明质酸和冰片,得凝固浴;
低聚壳聚糖的添加量为去离子水的体积的2%w/v(g/mL),草珊瑚提取物的添加量为去离子水的体积的1%w/v(g/mL),透明质酸的添加量为去离子水的体积的0.1%w/v(g/mL),冰片的添加量为去离子水的体积的0.7%w/v(g/mL);
低聚壳聚糖的制备方法为:取脱乙酰度≥90%的壳聚糖,加入去离子水中,使壳聚糖含量为10%w/v(g/mL)的;添加双氧水,双氧水与壳聚糖的摩尔比为4:1,升温至60℃,持续反应5h,过滤,冷冻干燥,得低聚壳聚糖;
2)海藻酸盐纺丝溶液的配制
取海藻酸钾,加入去离子水中,配置成质量浓度为3%的海藻酸钾溶液,在25℃下,搅拌6h,过滤,静置脱泡,静置脱泡时间为48h,得海藻酸钾溶液;
3)复合纤维的制备
将步骤2)所得的海藻酸钾溶液经过喷丝板挤入步骤1)所得的凝固浴中,凝固浴温度为15℃,喷丝板孔径为7μm,两道牵伸,水洗,水洗采用的是去离子水洗涤,去离子水的温度为40℃,冷冻干燥,得海藻酸盐壳聚糖复合纤维。
实施例三
本发明的一种吸液溶胀的海藻酸盐-壳聚糖复合纤维的制备方法,包括以下步骤:
1)凝固浴的配制
取质量浓度为2%的碳酸钙/葡萄糖酸内酯体系,加入低聚壳聚糖,搅拌,加入适量的柠檬酸溶液,调节pH值,使其pH值为6.2,加入草珊瑚提取物,得凝固浴;
低聚壳聚糖的添加量为去离子水的体积的6%w/v(g/mL),草珊瑚提取物的添加量为去离子水的体积的0.1%w/v(g/mL);
低聚壳聚糖的制备方法为:取脱乙酰度≥90%的壳聚糖,加入到去离子水中,使壳聚糖含量为1%w/v(g/mL);添加双氧水,双氧水与壳聚糖的摩尔比为1:1,升温至80℃,持续反应6h,过滤,冷冻干燥,得低聚壳聚糖;
2)海藻酸盐纺丝溶液的配制
取海藻酸铵,加入去离子水中,配置成质量浓度为6%的海藻酸铵溶液,在25℃下,搅拌6h,过滤,静置脱泡,静置脱泡时间为36h,得海藻酸铵溶液;
3)复合纤维的制备
将步骤2)所得的海藻酸铵溶液经过喷丝板挤入步骤1)所得的凝固浴中,凝固浴温度为25℃,喷丝板孔径为7μm,两道牵伸,二次水洗,水洗采用的是去离子水洗涤,去离子水的温度为20℃,冷冻干燥,得海藻酸盐壳聚糖复合纤维。
实施例四
本发明的一种吸液溶胀的海藻酸盐-壳聚糖复合纤维的制备方法,包括以下步骤:
1)凝固浴的配制
取氯化钙,溶解于去离子水,制成浓度为0.6%w/v(g/mL)的氯化钙溶液,加入低聚壳聚糖,搅拌,加入适量的硫酸溶液,调节pH值,使其pH值为4.5,加入草珊瑚提取物、薄荷提取物、透明质酸和冰片,得凝固浴;
低聚壳聚糖的添加量为去离子水的体积的4%w/v(g/mL),草珊瑚提取物的添加量为去离子水的体积的0.3%w/v(g/mL),薄荷提取物的添加量为去离子水的体积的0.2%w/v(g/mL),透明质酸的添加量为去离子水的体积的0.3%w/v(g/mL),冰片的添加量为去离子水的体积的1%w/v(g/mL);
低聚壳聚糖的制备方法为:取脱乙酰度≥90%的壳聚糖,加入到去离子水中,使壳聚糖含量为15%w/v(g/mL);添加双氧水,双氧水与壳聚糖的摩尔比为5:1,升温至60℃,持续反应4h,过滤,冷冻干燥,得低聚壳聚糖;
2)海藻酸盐纺丝溶液的配制
取海藻酸钠,加入去离子水中,配置成质量浓度为4%的海藻酸钠溶液,在25℃下,搅拌5h,经过粗滤、一滤和二滤等三次过滤,静置脱泡,静置脱泡时间为36h,得海藻酸钠溶液;
3)复合纤维的制备
将步骤2)所得的海藻酸钠溶液经过喷丝板挤入步骤1)所得的凝固浴中,凝固浴温度为18℃,喷丝板孔径为7μm,两道牵伸,二次水洗,水洗采用的是去离子水洗涤,去离子水的温度为30℃,冷冻干燥,得海藻酸盐壳聚糖复合纤维。
实施例五
本发明的一种吸液溶胀的海藻酸盐-壳聚糖复合纤维的制备方法,包括以下步骤:
1)凝固浴的配制
取氯化钙,溶解于去离子水,制成浓度为0.1%w/v(g/mL)的氯化钙溶液,加入低聚壳聚糖,搅拌,加入适量的硝酸溶液,调节pH值,使其pH值为5.3,加入草珊瑚提取物、薄荷提取物、透明质酸和冰片,得凝固浴;
低聚壳聚糖的添加量为去离子水的体积的1%w/v(g/mL),草珊瑚提取物的添加量为去离子水的体积的1%w/v(g/mL),薄荷提取物的添加量为去离子水的体积的1%w/v(g/mL),透明质酸的添加量为去离子水的体积的1%w/v(g/mL),冰片的添加量为去离子水的体积的0.3%w/v(g/mL);
低聚壳聚糖的制备方法为:取脱乙酰度≥90%的壳聚糖,加入到去离子水中,使壳聚糖含量为5%w/v(g/mL);添加双氧水,双氧水与壳聚糖的摩尔比为3:1,升温至60℃,持续反应5h,过滤,冷冻干燥,得低聚壳聚糖;
2)海藻酸盐纺丝溶液的配制
取海藻酸钠,加入去离子水中,配置成质量浓度为5%的海藻酸钠溶液,在22℃下,搅拌5h,过滤,静置脱泡,静置脱泡时间为40h,得海藻酸钠溶液;
3)复合纤维的制备
将步骤2)所得的海藻酸盐溶液经过喷丝板挤入步骤1)所得的凝固浴中,凝固浴温度为22℃,喷丝板孔径为7μm,两道牵伸,二次水洗,水洗采用的是去离子水洗涤,去离子水的温度为26℃,冷冻干燥,得海藻酸盐壳聚糖复合纤维。
实验一
将本发明实施例一至实施例五所得到的五份海藻酸盐壳聚糖复合纤维以及现有的将壳聚糖水溶液与海藻酸钠水溶液混合之后直接在氯化钙水溶液的凝固浴中喷丝而成的海藻酸钠壳聚糖复合材料(即对照样)分别进行性能测试实验,包括复合纤维的断裂强度、断裂伸长率、吸液倍数(水和盐水溶液),实验结果如表1所示。
其中,断裂强度按照GB/T 14337-2008《化学纤维短纤维拉伸性能试验》规定的方法进行测试,断裂伸长率按照GB/T 14337-2008《化学纤维短纤维拉伸性能试验》规定的方法进行测试,吸液倍数包括吸收水和吸收质量浓度为0.9%的氯化钠水溶液,并按照YYT0471.1-2004《接触性创面敷料试验方法第1部分液体吸收性》规定的方法进行测试。
由表1可以看出,本发明所得的海藻酸盐壳聚糖复合纤维的断裂强度在1.19-2.50之间,本发明所得的海藻酸盐壳聚糖复合纤维的断裂伸长率在12.1-16.8之间,本发明所得的海藻酸盐壳聚糖复合纤维中对水的吸液倍数在19.8-51.3之间,并且,其对盐水溶液的吸液倍数在22.7-25.9之间,本发明所得的海藻酸盐壳聚糖复合纤维的对水和盐水溶液的吸液倍数均明显高于对照样,这说明本发明所得的海藻盐壳聚糖复合纤维有较高的吸液倍数,可快速的吸收伤口的渗出液。本发明的复合纤维对水的吸收能力可为≤25g/g、25-40g/g和≥40g/g三个等级,凝固浴中钙含量>1.0%时,可以得到吸水能力≤25g/g的复合纤维,凝固浴中钙含量在0.6-0.1%之间时,可以得到吸水能力为25-40g/g的复合纤维,凝固浴中钙含量≤0.6%时,可以得到吸水能力≥40g/g的复合纤维,本发明的复合纤维对生理盐水的吸收能力为22-26g/g,满足了伤口愈合的不同时期对伤口辅料吸液量的不同需求。
表1不同海藻酸盐壳聚糖复合纤维的强度和吸水性能测定结果
实验二
将本发明实施例五所得的海藻酸盐壳聚糖复合纤维通过调整海藻酸盐基础的泵供量以及两道牵伸辊之间的牵伸比,得到不同线密度的复合纤维,对各复合纤维进行性能测试实验,包括复合纤维的线密度及其氮元素含量,并通过计算得壳聚糖在复合纤维中的含量,实验结果如表2所示。
表2海藻酸盐壳聚糖复合纤维的线密度及组分含量测定结果
由表2可以看出,本发明所得的海藻酸盐壳聚糖复合纤维的线密度在1.45-3.59之间时,通过这种不同大小的线密度可以得到壳聚糖含量不同的复合纤维。本发明所得的海藻酸盐壳聚糖复合纤维中含氮量的最小值在0.05-0.53之间,通过计算得到海藻酸盐壳聚糖复合纤维中壳聚糖含量的最小值在0.58-6.10之间;本发明所得的海藻酸盐壳聚糖复合纤维中含氮量的最大值在0.09-0.72之间,通过计算得到海藻酸盐壳聚糖复合纤维中壳聚糖含量的最小值在1.31-10.38之间;本发明的海藻酸盐壳聚糖复合纤维通过调整纺丝的线密度,可以控制壳聚糖在复合纤维中的含量,通过在凝固浴中添加不同的功能性材料,使复合纤维具有不同的功能,以满足伤口愈合的不同时期对伤口辅料的不同需求。
实验三
将本发明实施例一至实施例五所得到的五份海藻酸盐壳聚糖复合纤维以及现有的将壳聚糖水溶液与海藻酸钠水溶液混合之后直接在氯化钙水溶液的凝固浴中喷丝而成的海藻酸钠壳聚糖复合材料(即对照样)分别进行抑菌性能测试实验,包括复合纤维对大肠杆菌、金黄色葡萄球菌和白色念珠菌的抑菌率,实验结果如表3所示,抑菌性能测试实验依据GB/T 20994.3-2008《纺织品抗菌性能的评价第3部分:震荡法》由国家生态纺织品质量监督检验中心进行检测。
表3不同海藻酸盐壳聚糖复合纤维的抑菌性能测定结果
样品 | 大肠杆菌(%) | 金黄色葡萄球菌(%) | 白色念珠菌(%) |
实施例一 | 99.2 | 99.9 | 99.8 |
实施例二 | 99.6 | 99.8 | 99.9 |
实施例三 | 99.4 | 99.9 | 99.4 |
实施例四 | 99.9 | 99.7 | 99.7 |
实施例五 | 99.8 | 99.6 | 99.7 |
对照样 | 89.5 | 87.4 | 88.7 |
由表3可以看出,本发明所得的海藻酸盐壳聚糖复合纤维的对于大肠杆菌的抑菌率在99.2-99.9%之间,这明显优于对照样对大肠杆菌的抑菌率;本发明所得的海藻酸盐壳聚糖复合纤维的对于金黄色葡萄球菌的抑菌率在99.6-99.9%之间,这明显优于对照样对金黄色葡萄球菌的抑菌率;本发明所得的海藻酸盐壳聚糖复合纤维的对于白色念珠菌的抑菌率在99.4-99.8%之间,这明显优于对照样对白色念珠菌的抑菌率。因此,本发明所得的海藻酸盐壳聚糖复合纤维在壳聚糖、草珊瑚提取物、薄荷提取物、透明质酸和冰片的作用下,具有更好的抗菌和抑菌活性,杀菌消毒效果更好,可以根据伤口愈合不同时期对伤口辅料的不同需求选择不同的配方,充分满足了伤口不同愈合时期对医用辅料的要求。
实验四
将本发明实施例一至实施例五所得到的五份海藻酸盐壳聚糖复合纤维以及现有的将壳聚糖水溶液与海藻酸钠水溶液混合之后直接在氯化钙水溶液的凝固浴中喷丝而成的海藻酸钠壳聚糖复合材料(即对照样)分别进行动物模型实验,实验结果如表4所示。
实验方法:取健康60只SD大鼠,随机均分为6组,每组10只,包括五个实验组和一个对照组,采用戊巴比妥麻醉(30mg/Kg),在其背部脊柱一侧旁开一个长度为1cm的小口,利刀全层切除皮肤,形成面积为1cm2的圆形全层皮肤切除创面,对侧对称部位皮肤作为正常自身对照;将本发明实施例一至实施例五所得到的五份海藻酸盐壳聚糖复合纤维以及对照样分别贴于创面,贴敷10天,观察大鼠创面恢复情况,计算并记录创面伤口大小情况。
实验过程中观察到,贴敷有本发明实施例一至实施例五所得到的五份海藻酸盐壳聚糖复合纤维的五个实验组的大鼠,其受试侧皮肤均未出现红斑、水肿、湿疹等异常,观察期内动物均无死亡,未出现中毒体征,大体病理解剖学检查未见异常;因此,本发明的海藻酸盐壳聚糖复合纤维,对皮肤无刺激,对受试者无毒,具有使用安全性。
由表4可以看出,贴敷有本发明所得的海藻酸盐壳聚糖复合纤维的五个实验组的大鼠,第2天创面有所缩小;伤后第4天,在真皮层可见肉芽组织生成;伤后第5天时,60%以上的创面愈合;伤后第10天,伤口全部愈合,结痂脱落;在受伤至痊愈后未见明显细菌感染情况,且无脂肪液化现象发生,痊愈后创面平整无暗色,皮肤光滑。贴敷有对照样的大鼠,其创面在第2天之后也有所缩小;伤后第5天时,创面愈合不足50%;伤后第10天,有结痂未脱落;在受伤至痊愈后少量细菌感染情况,出现小面积脂肪液化,痊愈后创面处有明显疤痕。这说明本发明所得的复合纤维用于伤口修复时,其吸液倍数高,有效成分吸收快,具有很好的抑菌止血、消炎去痛和镇静止痒的效果,可以为伤口愈合的不同时期提供不同的护理环境,伤口愈合快。
表4伤口面积大小随时间的变化
与现有技术相比,本发明的有益效果是:本发明的低聚壳聚糖,容易吸收,低聚壳聚糖与草珊瑚提取物、薄荷提取物、透明质酸和冰片等多种功能性材料复配,在氯化钙溶液或钙离子缓释体系中制成凝固浴,并将海藻酸盐水溶液利用喷丝技术在凝固浴内形成复合纤维,低聚壳聚糖等功能性材料在复合纤维中的分布均匀;所得的复合纤维吸液倍数高,可以吸收大量伤口渗出液,有效成分吸收充分,有很好的机械和力学性能,用于伤口修复,具有很好的抑菌止血、消炎去痛和祛痱止痒的效果,可以为伤口愈合的不同时期提供不同的护理环境,伤口愈合快。本发明的制备方法简单,控制方便,通过工艺参数的控制,可以控制吸液倍数,成本低,得到了一种性能良好的具有吸液溶胀性能的海藻酸盐壳聚糖复合纤维。
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。
Claims (10)
1.一种吸液溶胀的海藻酸盐壳聚糖复合纤维,其特征在于:所述复合纤维是由海藻酸盐水溶液在凝固浴中通过凝固的方法制备而成,所述海藻酸盐水溶液的质量浓度为3-6%;
所述凝固浴包括以下重量份的组分:低聚壳聚糖1-6份,草珊瑚提取物0.1-1份,薄荷提取物0-1份,透明质酸0-1份,冰片0-1份,氯化钙溶液或钙离子缓释体系90-100份,氯化钙溶液或钙离子缓释体系的质量浓度为0.1-2.0%。
2.根据权利要求1所述的吸液溶胀的海藻酸盐壳聚糖复合纤维,其特征在于:所述凝固浴包括以下重量份的组分:
低聚壳聚糖1-6份,草珊瑚提取物0.1-1份,薄荷提取物0-0.5份,透明质酸0-0.5份,冰片0.5-1份,氯化钙溶液或钙离子缓释体系90-100份,氯化钙溶液或钙离子缓释体系的质量浓度为0.1-1.0%。
3.根据权利要求1所述的吸液溶胀的海藻酸盐壳聚糖复合纤维,其特征在于:所述凝固浴包括以下重量份的组分:
低聚壳聚糖1-6份,草珊瑚提取物0.1-1份,薄荷提取物0.5-1份,透明质酸0.5-1份,冰片0-0.5份,氯化钙溶液或钙离子缓释体系90-100份,氯化钙溶液或钙离子缓释体系的质量浓度为1.0-2.0%。
4.根据权利要求1所述的吸液溶胀的海藻酸盐壳聚糖复合纤维,其特征在于:所述低聚壳聚糖的制备方法为:
取脱乙酰度≥90%的壳聚糖,加入到去离子水中,使壳聚糖含量为1-15%w/v;添加双氧水,双氧水与壳聚糖的摩尔比为5:1-1:1,升温至50-80℃,持续反应4-6h,过滤,冷冻干燥,得低聚壳聚糖。
5.根据权利要求1所述的吸液溶胀的海藻酸盐壳聚糖复合纤维,其特征在于:
所述海藻酸盐为海藻酸钠、海藻酸钾、海藻酸铵中的一种或几种。
6.根据权利要求1所述的吸液溶胀的海藻酸盐壳聚糖复合纤维,其特征在于:
所述钙离子缓释体系为硫酸钙/葡萄糖酸内酯体系、碳酸钙/葡萄糖酸内酯体系、磷酸二钙/葡萄糖酸内酯体系、葡萄糖酸钙溶液中的一种或几种。
7.根据权利要求1-6中任意一项所述的吸液溶胀的海藻酸盐壳聚糖复合纤维的制备方法,其特征在于:包括以下步骤:
1)取氯化钙水溶液或钙离子缓释体系,加入低聚壳聚糖,搅拌,调节pH值,使其pH值为4.5-6.2,加入草珊瑚提取物、薄荷提取物、透明质酸和冰片,混合均匀,得凝固浴;
2)取海藻酸盐,加入去离子水中,在20-25℃下,搅拌4-6h,过滤,静置脱泡,静置脱泡时间为24-48h,得海藻酸盐溶液;
3)将步骤2)所得的海藻酸盐溶液经过喷丝板喷入步骤1)所得的凝固浴中,凝固浴温度为15-25℃,牵伸,水洗,干燥,得海藻酸盐壳聚糖复合纤维。
8.根据权利要求7所述的吸液溶胀的海藻酸盐壳聚糖复合纤维的制备方法,其特征在于:
所述步骤3)中水洗采用的是去离子水洗涤,去离子水的温度为20-40℃。
9.根据权利要求7所述的吸液溶胀的海藻酸盐壳聚糖复合纤维的制备方法,其特征在于:
所述步骤1)中采用酸调节pH值,所述酸为盐酸、醋酸、柠檬酸、硫酸、硝酸中的一种或几种。
10.根据权利要求1-6中任意一项所述的吸液溶胀的海藻酸盐壳聚糖复合纤维的应用,其特征在于:
所述海藻酸盐壳聚糖复合纤维用于伤口修复。
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