CN117065075A - 一种纳米纤维抗菌敷料及其制备方法 - Google Patents
一种纳米纤维抗菌敷料及其制备方法 Download PDFInfo
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- CN117065075A CN117065075A CN202310917459.7A CN202310917459A CN117065075A CN 117065075 A CN117065075 A CN 117065075A CN 202310917459 A CN202310917459 A CN 202310917459A CN 117065075 A CN117065075 A CN 117065075A
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- wool keratin
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Abstract
本发明提供了一种纳米纤维抗菌敷料及其制备方法,属于医用材料技术领域。本发明制备的纳米纤维抗菌敷料由羊毛角蛋白/PVA纳米纤维膜、间隔织物、吸液无纺布和医用压敏胶带四层结构组成。本发明的纳米纤维抗菌敷料通过羊毛角蛋白/PVA纳米纤维膜层进行伤口处的抗菌处理,经间隔织物在保证伤口再生修复适宜条件的基础上,赋予敷料缓压功能,避免伤口遭受外力伤害,再由吸液无纺布进行吸收液体,防止液体回流到伤口处,减少敷料更换频率,最后医用压敏胶带有利于敷料在伤口处的固定,且便于成片更换。
Description
技术领域
本发明涉及医用材料技术领域,尤其涉及一种纳米纤维抗菌敷料及其制备方法。
背景技术
创面愈合是指由于致伤因子的作用造成组织缺失后,局部组织通过再生、修复、重建,进行修补的一系列病理生理过程。本质上是机体对各种有害因素作用所致的组织细胞损伤的一种固有的防御性适应性反应。抗菌敷料的使用,能够在很大程度上阻止微生物、灰尘进入创伤组织,便于伤口的护理,促进伤口快速愈合,传统的抗菌敷料为纱布类敷料,主要是以棉或麻材质基布为原料,经抗菌或灭菌处理制得,具有使用方便、适用范围广等优点。
现有的抗菌敷料通透性太高,容易使创面脱水;粘着创面,更换时会造成再次性机械性损伤;外界环境微生物容易通过,交叉感染的机会较高。
发明内容
有鉴于此,本发明的目的在于提供一种纳米纤维抗菌敷料,所述纳米纤维抗菌敷料(Antibacterial dressings)由羊毛角蛋白/PVA纳米纤维膜(Nanofiber membranes)、间隔织物(Spacer fabric)、吸液无纺布(Liquid absorbentnon-woven fabric)和医用压敏胶带(Medical pressure-sensitive tape)四层结构组成。其通过羊毛角蛋白/PVA纳米纤维膜层进行伤口处的抗菌处理,经间隔织物在保证伤口再生修复适宜条件的基础上,赋予敷料缓压功能,避免伤口遭受外力伤害,再由吸液无纺布进行吸收液体,防止液体回流到伤口处,减少敷料更换频率,最后医用压敏胶带有利于敷料在伤口处的固定,且便于成片更换。
本发明提供的纳米纤维抗菌敷料,从上至下依次包括羊毛角蛋白/PVA纳米纤维膜、间隔织物、吸液无纺布和医用压敏胶带;所述羊毛角蛋白/PVA纳米纤维膜的厚度为0.2mm,所述间隔织物的厚度为3.8mm,所述吸液无纺布的厚度为1.2mm,所述医用压敏胶带的厚度为0.2mm。
所述间隔织物是一种具有三维结构的纺织材料,包括上下两个网孔面层以及将其连接起来的间隔丝三部分。在本发明的具体实施例中,所述间隔织物购自深圳市鸿泰轩纺织品有限公司(型号为白色4mm加密双底1.5m×0.5m)。
所述吸液无纺布由合成纤维混合而成,由不同比例的粘胶和聚酯组成。在本发明的具体实施例中,所述吸液无纺布购自金士达医疗(咸宁)有限公司(型号为折叠后10cm×10cm-4层,5片/灭菌装)。
所述医用压敏胶带以聚乙烯为基材,涂以医用热熔胶制成,医用压敏胶带的一面具有粘附性。在本发明的具体实施例中,所述医用压敏胶带购自振德医疗用品股份有限公司(型号为10cm×10m,透气舒适型)。
优选的,所述羊毛角蛋白/PVA纳米纤维膜的制备方法,包括以下步骤:
(1)制备纳米氧化锌颗粒:将金银花提取液与二水合乙酸锌溶液按照50~55:80~85的体积比混合,在80℃的磁力搅拌机中搅拌,边搅拌边滴加NaOH溶液来调整PH值为8,搅拌完成后进行抽滤,抽滤后煅烧得到纳米氧化锌颗粒;
所述金银花提取液的制备方法为:
称量5.0g金银花清洗干净,然后放入烧杯中,加入50mL去离子水,使用保鲜膜对烧杯口进行密封,并用橡皮筋扎紧,浸泡24h,之后对烧杯中的液体进行过滤,滤掉烧杯中的叶片,保留所得液体,得到金银花提取液;
(2)制备纳米氧化锌/有机硅季铵盐复合抗菌剂:按照纳米氧化锌质量占比为1.0%~1.4%,将有机硅季铵盐和步骤(1)制备的纳米氧化锌颗粒混合,搅拌15~20分钟后升温至55~65℃,继续搅拌2~3h,最后采用超声震荡处理,得到所述纳米氧化锌/有机硅季铵盐复合抗菌剂;
(3)制备羊毛角蛋白/PVA抗菌纳米纤维膜:将羊毛角蛋白和PVA粉末置于甲酸中,得到羊毛角蛋白/PVA甲酸溶液;然后将步骤(2)制备的复合抗菌剂与所述羊毛角蛋白/PVA甲酸溶液混合,在80℃的条件下搅拌1.5h,得到纺丝液,最后经过静电纺丝技术得到所述羊毛角蛋白/PVA抗菌纳米纤维膜。
优选的,步骤(1)所述二水合乙酸锌溶液的浓度为0.75mol/L。
优选的,步骤(1)所述煅烧的温度为350~450℃,煅烧时间为1.5~2.5h。
优选的,步骤(3)所述羊毛角蛋白、PVA粉末和甲酸的比例为0.3~0.4g:1.3~1.4g:10~12mL。
优选的,步骤(3)所述复合抗菌剂的添加量按照复合抗菌剂与甲酸的质量体积比例为0.25g:10~12mL添加。
本发明的另一个目的在于提供一种纳米纤维抗菌敷料的制备方法,包括以下步骤:
S1:将羊毛角蛋白/PVA抗菌纳米纤维膜、间隔织物与吸液无纺布裁剪成5cm×5cm的正方形,医用压敏胶带裁剪成10cm×10cm的正方形;
S2:使用粘合剂将羊毛角蛋白/PVA抗菌纳米纤维膜的背面与间隔织物的上层面进行粘合,将吸液无纺布的一面与间隔织物的下层粘合,最后将医用压敏胶带具有粘附性的一面与吸液无纺布的另一面进行粘贴,形成四层结构的抗菌敷料。
与现有技术相比,本发明具有以下有益效果:
本发明提供了一种纳米纤维抗菌敷料及其制备方法,制备的纳米纤维抗菌敷料以羊毛角蛋白/PVA纳米抗菌纤维膜为载体,结合间隔织物、吸液无纺布和医用压敏胶带,具有吸收性、透气性、无创性、保护性、安全性以及功能性。
本发明制备的抗菌敷料中的羊毛角蛋白是一种天然活性物质,富含酰胺、羧基、羟基以及巯基等多种活性基团,具有止血、促进伤口修复的功能;PVA是一种安全的高分子聚合物,对人体无毒无害,且具有良好的生物相容性;金银花提取物绿色合成的纳米氧化锌以及有机硅季铵盐作为抗菌剂,具有良好的抗菌活性,对抗生素没有耐药性,无毒且与皮肤相容。抗菌敷料生物相容性好,具有很好的吸液性和透湿性,并能够很好的阻隔外界液体,制备过程也较为简捷。
附图说明
图1为本发明纳米纤维抗菌敷料的制备方法示意图;
图2为羊毛角蛋白/PVA抗菌纳米纤维膜在SE溶液中质量随时间的变化情况;
图3为间隔织物和抗菌敷料的压缩应力-应变曲线;
图4为羊毛角蛋白/PVA抗菌纳米纤维膜、间隔织物、吸液无纺布和医用压敏胶带的动态接触角。
具体实施方式
本发明提拱了一种纳米纤维抗菌敷料及其制备方法,所述纳米纤维抗菌敷料从上至下依次包括羊毛角蛋白/PVA纳米纤维膜、间隔织物、吸液无纺布和医用压敏胶带。
在本发明的实施例中,所述羊毛角蛋白/PVA纳米纤维膜的厚度为0.2mm,所述间隔织物的厚度为3.8mm,所述吸液无纺布的厚度为1.2mm,所述医用压敏胶带的厚度为0.2mm。
本发明实施例中采用的羊毛角蛋白的制备方法如下:
分别称量5.0g亚硫酸氢钠、30.0g尿素和1.5g十二烷基硫酸钠置于烧杯中,倒入100mL去离子水进行搅拌至固体完全溶解;然后称取5.0g羊毛纤维,将其剪碎至长度为1cm置于上述溶液中,在95℃的条件下加热搅拌4h,冷却,使用循环水式多用真空泵对其进行抽滤,以滤去未溶解的羊毛纤维,所得淡黄色滤液即为羊毛溶解液。
然后采用去离子水作为透析液对所述羊毛溶解液进行透析,透析时间为72h,期间每8h换水一次,以除去溶液中的盐和小分子物质;透析完成后,向溶液中滴加1.0mol/L盐酸溶液,至溶液pH值达到蛋白质等电点4.8,滴加时,可观察到溶液中产生白色沉淀,溶液颜色逐渐变为乳白色,将滴定后的溶液与沉淀再次进行透析,步骤同上,所得固体即为羊毛角蛋白。
下面结合实施例对本发明作进一步说明。
实施例1
一种纳米纤维抗菌敷料的制备方法,步骤如下:
(一)制备羊毛角蛋白/PVA抗菌纳米纤维膜:
(1)制备纳米氧化锌颗粒:称量5.0g金银花,之后使用去离子水清洗称量的金银花。将清洗后的金银花放入烧杯中,加入50mL去离子水,使用保鲜膜对烧杯口进行密封,并用橡皮筋扎紧,浸泡24h,之后对烧杯中的液体进行过滤,滤掉烧杯中的叶片,保留所得液体。将50mL银花提取液与83.3mL浓度为0.75mol/L的二水合乙酸锌溶液混合,在80℃的磁力搅拌机中搅拌,边搅拌边滴加NaOH溶液来调整PH值为8,搅拌完成后进行抽滤,抽滤后煅烧得到纳米氧化锌颗粒,所述煅烧的温度为400℃,煅烧时间为2h;
(2)制备纳米氧化锌/有机硅季铵盐复合抗菌剂:按照纳米氧化锌质量占比为1.2%,将有机硅季铵盐和步骤(1)制备的纳米氧化锌颗粒混合,搅拌15分钟后升温至60℃,继续搅拌2.5h,最后采用超声震荡处理,得到所述纳米氧化锌/有机硅季铵盐复合抗菌剂;
(3)制备羊毛角蛋白/PVA抗菌纳米纤维膜:将0.332g羊毛角蛋白和1.331gPVA粉末置于10mL甲酸中,得到羊毛角蛋白/PVA甲酸溶液;然后将0.25g步骤(2)制备的复合抗菌剂与所述羊毛角蛋白/PVA甲酸溶液混合,在80℃的条件下搅拌1.5h,得到纺丝液,最后经过静电纺丝技术(温度为20℃,湿度为40%)得到所述羊毛角蛋白/PVA抗菌纳米纤维膜;
(二)制备纳米纤维抗菌敷料:
S1:将羊毛角蛋白/PVA抗菌纳米纤维膜、间隔织物与吸液无纺布裁剪成5cm×5cm的正方形,医用压敏胶带裁剪成10cm×10cm的正方形;
S2:使用粘合剂(购自深圳市奥信达胶业有限公司,型号为奥信达6061塑料专用胶)将羊毛角蛋白/PVA抗菌纳米纤维膜的背面与间隔织物的上层面进行粘合,将吸液无纺布的一面与间隔织物的下层粘合,最后将医用压敏胶带具有粘附性的一面与吸液无纺布的另一面进行粘贴,形成四层结构的抗菌敷料。纳米纤维抗菌敷料的制备方法示意图如图1。
实施例2
一种纳米纤维抗菌敷料的制备方法,步骤同实施例1,区别在于步骤(2)中纳米氧化锌质量占比为1.0%。
实施例3
一种纳米纤维抗菌敷料的制备方法,步骤同实施例1,区别在于步骤(2)中纳米氧化锌质量占比为1.4%。
性能测试
(1)对实施例1~3制备的纳米氧化锌/有机硅季铵盐复合抗菌剂进行测试,静置七天后,当纳米氧化锌质量占比为1.2%时,该复合抗菌剂没有出现白色沉淀物,分布均匀且能保证更好的抗菌性能,因此复合抗菌剂的性能最优。
(2)对实施例1制备的纳米氧化锌/有机硅季铵盐复合抗菌剂进行质量变化测试,将其浸泡于SE溶液(142mmol/L氯化钠和2.5mmol/L氯化钙)中,记录损失质量有时间的关系,羊毛角蛋白/PVA抗菌纳米纤维膜在SE溶液中质量随时间的变化情况如图2。由图2可见,纳米纤维膜的质量在浸泡于SE溶液24h之后质量有所下降,损失质量为7.14%,72h后损失质量为14.29%,120h后损失质量为28.57%,168h后损失质量为28.60%,质量变化较小,质量损失达到稳定。因此,在伤口渗出液较多时,为减少伤口处异物残留、避免伤口粘连和保持伤口处环境卫生,敷料的最佳使用更换时间为72h以内。
(3)对实施例1制备的纳米纤维抗菌敷料中间隔织物和抗菌敷料的抗压缩性能进行测试,具体试验方法为:
新型抗菌敷料相较于其它敷料的不同之处便是具有缓压功能,避免伤口遭受外力伤害,也可起到衬垫作用,分散和减轻压力。压缩性能测试的目的是探究新型抗菌敷料的压缩性能,由于敷料中起到压缩作用的部分为间隔织物,因此本测试的对象为间隔织物与组合后的新型抗菌敷料整体,之后对比分析组合前后材料压缩性能的变化。
本次测试使用INSTRON 5900系列型号的电子万能试验机进行测试,应变设定为样品厚度的60%,压头移动速度和回复速度5mm/min。测试步骤为首先从间隔织物上裁剪下5cm×5cm的样品,之后依次将间隔织物样品与新型抗菌敷料放置于压盘上,调整初始固定距离为样品的厚度,初始位移和载荷值调零后,开始测试。每个样品测试三次,之后对三组数据进行加权平均处理,所得值即为测试结果。间隔织物和抗菌敷料的压缩应力应变曲线如图3。
由图3可见,当压缩应变设定为样品厚度的60%时,间隔织物的压缩应力大于抗菌敷料的压缩应力。结果表明,间隔织物的抗压缩性能优于结合后的抗菌敷料,主要原因为结合后的抗菌敷料相较于单一的间隔织物,上下两层均被不具有抗压缩性能的材料覆盖,当受到外力时,表面不具备压缩性能的材料将力向四周分散,使得间隔织物各部位均可受到压力作用,因此压缩形变较为明显,但仍具备较好的抗压缩性能。
(4)对实施例1制备的纳米纤维抗菌敷料的各层结构进行接触角测试,羊毛角蛋白/PVA抗菌纳米纤维膜、间隔织物、吸液无纺布和医用压敏胶带的动态接触角如图4。
新型抗菌敷料各部分的功能不同,因此对于材料的亲疏液性能要求也不同。接触角性能测试的目的是探究新型抗菌敷料各部分材料的亲疏液性能,本测试的对象为羊毛角蛋白/PVA抗菌纳米纤维膜、间隔织物、吸液无纺布以及医用压敏胶带,由于敷料接触的液体主要为伤口渗出液,因此测试使用的液体为SE溶液。
本次测试使用Dataphysics OCA15pro型视频光学接触角测量仪进行测试,仪器参数设置为滴加液滴量2μL,滴液速率0.1μL/s,平衡时间5s。测试步骤为首先从各材料上裁剪2cm×2cm的样品,之后将样品放置于微量注射器针头下的载物台上,进行调焦调光,直至图像清晰后开始测试。仪器通过样品表面液滴轮廓的图像拟合技术进行接触角自动分析,可获得接触角度数据。
由图4可见,1s时羊毛角蛋白/PVA抗菌纳米纤维膜、间隔织物和吸液无纺布的接触角分别为69.6°、32.3°和40.7°,接触角均小于90°,表明材料具有亲液性;平衡5s后,羊毛角蛋白/PVA抗菌纳米纤维膜接触角为53.3°,而间隔织物和吸液无纺布已经将液滴完全吸收,接触角为0°,表明间隔织物和吸液无纺布对液体的亲和力较强,且能够快速吸收,羊毛角蛋白/PVA抗菌纳米纤维膜对液体的吸收性能相对较弱。1s时医用PE胶布的接触角为112.8°,平衡5s后,接触角减小为99.6°,均大于90°,表明材料具有疏液性。依据各部分材料功能,羊毛角蛋白/PVA抗菌纳米纤维膜作为敷料中与伤口直接接触的部分,需要吸收伤口渗出液;间隔织物在敷料中主要作用为导液,将纳米纤维膜层吸收的伤口渗出液及时导出,保持伤口干爽;吸液无纺布在敷料中主要负责吸收存储伤口渗出液,上述三种材料应该具有亲液性。医用压敏胶带在敷料中主要作用为隔液、防止吸收的伤口渗出液外渗,应该具有疏液性。测试结果均与需求相符,适合用于制备新型抗菌敷料。
(5)对实施例1制备的抗菌敷料以及其中的羊毛角蛋白/PVA抗菌纳米纤维膜(纳米纤维膜)、间隔织物、吸液无纺布、医用压敏胶带进行水蒸气透过率测试,结果如表1。
表1
W1:初始离心管与溶液质量
W2:24h取出样品后离心管与溶液质量
S:离心管敞口面积
V:24h透过水蒸气的速率
由表1可见,其中羊毛角蛋白/PVA抗菌纳米纤维膜、间隔织物、吸液无纺布和医用压敏胶带在37℃条件下24h水蒸气透过率分别为0.110g(cm2·24h)-1、0.258g(cm2·24h)-1、0.332g(cm2·24h)-1和0.090g(cm2·24h)-1,四种材料的水蒸气透过率位于正常皮肤与裸露伤口之间,符合敷料材料的水蒸气透过率性能标准。结合后的抗菌敷料在37℃条件下24h水蒸气透过率为0.296g(cm2·24h)-1,透气率略低于间隔织物,但相较于另外三种材料有所提高。结果表明,将多种材料结合能够改善敷料的透气性能,水蒸气透过率比正常皮肤最高值高出54%,为裸露伤口的62%,敷料可以排出伤口处周围多余水蒸气而不会引起脱水,保持伤口处适宜的湿度和生理环境,符合伤口敷料的水蒸气透过率性能标准。
(6)对羊毛角蛋白/PVA抗菌纳米纤维膜(纳米纤维膜)以及吸液无纺布进行液体吸收量测试,结果如表2。
表2
测试参数 | 纳米纤维膜 | 吸液无纺布 |
M1(g) | 0.00315 | 0.0317 |
M2(g) | 0.0211 | 0.5829 |
M3(g) | 0.0034 | 0.2138 |
MZ(g/g) | 5.70 | 17.39 |
MK(g/g) | 5.62 | 11.64 |
MX(g/g) | 0.08 | 5.75 |
M1:初始样品质量
M2:置于10mL 37℃的SE溶液中浸泡30min后样品质量
M3:以1200rpm的速度离心15min后样品质量
MZ:材料对液体的总吸收量
MK:材料孔隙对液体的吸收量
MX:材料纤维对液体的吸收量
由表2可见,羊毛角蛋白/PVA抗菌纳米纤维膜纤维可吸收自身重量0.08倍的渗出液,纤维孔隙可吸收自身重量5.62倍的渗出液,总共吸收自身重量5.7倍的渗出液;吸液无纺布纤维可吸收自身重量5.75倍的渗出液,纤维孔隙可吸收自身重量11.64倍的渗出液,总共吸收自身重量17.39倍的渗出液。结果表明,二者均具有良好的吸液性,但其纤维吸收量均低于孔隙吸收量。主要原因是吸液无纺布和制备纳米纤维膜的羊毛角蛋白和PVA均为亲水性材料,纤维内含有较多羟基和羧基等亲水基团,这些亲水基团能够通过氢键与水分子结合,但其纤维直径较小,孔隙率较高,因此液体更易被纤维孔隙吸收。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (7)
1.一种纳米纤维抗菌敷料,其特征在于,从上至下依次包括羊毛角蛋白/PVA纳米纤维膜、间隔织物、吸液无纺布和医用压敏胶带;所述羊毛角蛋白/PVA纳米纤维膜的厚度为0.2mm,所述间隔织物的厚度为3.8mm,所述吸液无纺布的厚度为1.2mm,所述医用压敏胶带的厚度为0.2mm。
2.根据权利要求1所述的纳米纤维抗菌敷料,其特征在于,所述羊毛角蛋白/PVA纳米纤维膜的制备方法,包括以下步骤:
(1)制备纳米氧化锌颗粒:将金银花提取液与二水合乙酸锌溶液按照50~55:80~85的体积比进行混合,在80℃的磁力搅拌机中搅拌,边搅拌边滴加NaOH溶液来调整PH值为8,搅拌完成后进行抽滤,抽滤后煅烧得到纳米氧化锌颗粒;
(2)制备纳米氧化锌/有机硅季铵盐复合抗菌剂:按照纳米氧化锌质量占比为1.0%~1.4%,将有机硅季铵盐和步骤(1)制备的纳米氧化锌颗粒混合,搅拌15~20分钟后升温至55~65℃,继续搅拌2~3h,最后采用超声震荡处理,得到所述纳米氧化锌/有机硅季铵盐复合抗菌剂;
(3)制备羊毛角蛋白/PVA抗菌纳米纤维膜:将羊毛角蛋白和PVA粉末置于甲酸中,得到羊毛角蛋白/PVA甲酸溶液;然后将步骤(2)制备的复合抗菌剂与所述羊毛角蛋白/PVA甲酸溶液混合,在80℃的条件下搅拌1.5h,得到纺丝液,最后经过静电纺丝技术得到所述羊毛角蛋白/PVA抗菌纳米纤维膜。
3.根据权利要求1所述的纳米纤维抗菌敷料,其特征在于,步骤(1)所述二水合乙酸锌溶液的浓度为0.75mol/L。
4.根据权利要求1所述的纳米纤维抗菌敷料,其特征在于,步骤(1)所述煅烧的温度为350~450℃,煅烧时间为1.5~2.5h。
5.根据权利要求1所述的纳米纤维抗菌敷料,其特征在于,步骤(3)所述羊毛角蛋白、PVA粉末和甲酸的比例为0.3~0.4g:1.3~1.4g:10~12mL。
6.根据权利要求1所述的纳米纤维抗菌敷料,其特征在于,步骤(3)所述复合抗菌剂的添加量按照复合抗菌剂与甲酸的质量体积比例为0.25g:10~12mL添加。
7.根据权利要求1~6任一所述的纳米纤维抗菌敷料的制备方法,包括以下步骤:
S1:将羊毛角蛋白/PVA抗菌纳米纤维膜、间隔织物与吸液无纺布裁剪成5cm×5cm的正方形,医用压敏胶带裁剪成10cm×10cm的正方形;
S2:使用粘合剂将羊毛角蛋白/PVA抗菌纳米纤维膜的背面与间隔织物的上层面进行粘合,将吸液无纺布的一面与间隔织物的下层粘合,最后将医用压敏胶带具有粘附性的一面与吸液无纺布的另一面进行粘贴,形成四层结构的抗菌敷料。
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