CN113274539A - 一种自供电伤口贴片及其制备方法 - Google Patents
一种自供电伤口贴片及其制备方法 Download PDFInfo
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- CN113274539A CN113274539A CN202110476569.5A CN202110476569A CN113274539A CN 113274539 A CN113274539 A CN 113274539A CN 202110476569 A CN202110476569 A CN 202110476569A CN 113274539 A CN113274539 A CN 113274539A
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Abstract
本发明公开了一种自供电伤口贴片,包括PVDF/CNTs纤维贴片,PVDF/CNTs纤维贴片上涂敷有载药PDA‑CS水凝胶;载药PDA‑CS水凝胶包括以下成分:盐酸多巴胺DA、壳聚糖、姜黄素或表皮生长因子或积雪草苷,过硫酸铵APS、N,N‑亚甲基双丙烯酰胺MBA、偶氮二异丁腈AIBN、去离子水、醋酸溶液。本发明通过水凝胶吸水特性达到止血和吸收渗出液的目的,在炎症期,壳聚糖水凝胶不仅能够通过自身的抗炎抗菌及湿润特性为伤口愈合提高良好的微环境,还可以触发人体巨噬细胞产生坏死因子α,从而引发炎症信号触发巨噬细胞活动并使伤口中的细胞因子水平增加,促进伤口愈合。本发明还公开了一种自供电伤口贴片的制备方法。
Description
技术领域
本发明属于医用生物材料技术领域,涉及一种自供电伤口贴片,本发明还涉及上述自供电伤口贴片的制备方法。
背景技术
全球范围内,急性和慢性伤口,例如战创伤,烧伤和糖尿病性足溃疡,分别给患者和医疗保健***带来了显著的负担。为了减轻患者和社会的经济负担,目前正在进行广泛的研究,以开发能够在短时间内有效治疗创伤的技术。其中适当的治疗策略包括使用高愈合率的伤口敷料,这不仅可以防止感染,防止长期伤口不愈带来的不良后果,并降低成本,减轻患者痛苦。创面敷料是世界创面护理工业和贸易的重要组成部分。而且伤口敷料是治疗糖尿病足溃疡等难愈合伤口的关键部分,广泛用于伤口护理,既能保护伤口又能促进伤口愈合。
临床上广泛应用着纱布,棉花,绷带,水凝胶等传统的敷料虽然具有生物相容性好,创面吸收能力强及可提高湿润的环境有利于修复伤口细胞生长的优势,但仍存在透气性差、抑菌效果较差等缺点,除此之外最重要的是,伤口的愈合也全依赖于患者自身的恢复能力,无法起到促进伤口加速愈合的作用。为了加快伤口愈合,研究表明,伤口修复与伤口内源性电场(wound endogenous electric field,EF)密切相关,创面形成后由于跨上皮电势差的消失产生内源性的直流电场,此电场是创面愈合过程中指导表皮细胞向创面中心迁移的最重要的方向信号,这种电场可增强细胞迁移和增殖,对许多皮肤再生活动(如胶原沉积、血管生成、再上皮化)至关重要。电刺激(ES)疗法通过在创面部位应用外膜来模拟并增强创面内源性EF的作用,并被用于加速皮肤创面愈合;但其在临床操作中的应用往往受到设备体积大的限制,且难以实现实时治疗。综上所述,不仅需要制备出一种能够在创面部位应用的外膜,来模拟并增强创面内源性电场来加速皮肤创面愈合,而且该材料还应具备传统敷料该有的生物相容性好、保湿抗菌的特点,为伤口愈合提高较好的微环境,进一步加速伤口的愈合速率。
因此,一方面为了满足伤口愈合的外环境需求(湿润,透气),另一方面,为了增强细胞有效增殖和迁移加速皮肤创面愈合且便于临床操作。本专利想要通过将压电材料与天然水凝胶材料结合,以达到既能为伤口愈合提供良好的微环境,还能有效增强细胞迁移和增殖速率,进而达到提高伤口愈合速率的目的。
中国专利《基于纳米纤维空间结构可控的复合细菌纤维素敷料及制法》(申请号:202011495354.X,公开日:2021.04.02,公开号:CN112587712 A)公开了一种基于纳米纤维空间结构可控的复合细菌纤维素敷料及其制备方法,该方法制得的非织造材料复合细菌纤维素敷料虽然具有良好的生物相容性、力学性能和吸收伤口渗出液性能,但是伤口的愈合仅是靠机体的自体愈合,不能在更有效的促进机体伤口愈合能力。
中国专利《一种隔菌聚乳酸超细纳米纤维伤口敷料的制备方法》(申请号:CN201910307469.2,公开号:CN 110067036 A,公开日:2019.07.30)公开了一种隔菌聚乳酸超细纳米纤维伤口敷料的制备方法,所述材料是通过聚乳酸超细纳米纤维伤口敷料纤维孔径小于菌体的直径,可有效地起到隔菌抗感染的作用;且聚乳酸超细纤维存在多孔小间隙可促进止血,高比表面积可促进液体吸收,增强药物或抗生素的释放,从而可在消除了传统敷料更换时不可避免的二次伤害的同时促进伤口的愈合。但是该方法制备的伤口敷料由于产量问题在大面积创伤及深层次创伤上受到了局限,且超细的孔隙也可能阻绝伤口所必需的氧分。
中国专利《一种单原子抗菌消毒止血水凝胶及其制备方法》(申请号:202011340886.6,公开日:2021.02.09,公开号:CN 112336912 A)公开了一种单原子抗菌消毒止血水凝胶的制备方法,该方法制备了是由40~75%羟甲基纤维素钠、5~10%单原子抗菌消毒剂和20~50%去离子水混合而成。与传统的抗菌消毒止血材料相比,单原子抗菌消毒止血水凝胶具有更为优异的抗菌消毒止血性能。但是,它仅能起到抗菌消毒止血的作用,对于多样化疾病不能起到根本的治疗作用。
中国专利《一种促进伤口愈合的纤维型伤口敷料及其制备方法》(申请号:CN202010886847.X,公开号:CN 111956858 A,公开日:2020.11.20)公开了一种促进伤口愈合的纤维型伤口敷料的制备方法,该方法以聚谷氨酸、***胶、阿魏酸、角蛋白、原花青素为主要原料按照合适的配比和加工方式制备出了一种方便携带的纤维型伤口敷料,具有抗菌消炎、促进愈合、修复皮肤、减少疤痕、方便使用的优点。但该方法制备的材料不能为材料提供伤口愈合的保湿的微环境,且促进伤口愈合的手段为被动促进,不能诱导细胞自动愈合。
发明内容
本发明的目的是提供一种自供电伤口贴片,通过水凝胶吸水特性达到止血和吸收渗出液的目的,在炎症期,壳聚糖水凝胶不仅能够通过自身的抗炎抗菌及湿润特性为伤口愈合提高良好的微环境,还可以触发人体巨噬细胞产生坏死因子α,从而引发炎症信号触发巨噬细胞活动并使伤口中的细胞因子水平增加,促进伤口愈合。
本发明的另一目的是提供一种自供电伤口贴片的制备方法。
本发明所采用的技术方案是,一种自供电伤口贴片,包括PVDF/CNTs纤维贴片,PVDF/CNTs纤维贴片上涂敷有载药PDA-CS水凝胶;
PVDF/CNTs纤维贴片包括以下成分:聚偏氟乙烯PVDF 4.5g~7.5g、改性碳纳米管CNTs 0.5g~3.21g、丙酮C3H6O 7.5ml~12ml,N,N-二甲基甲酰胺DMF 18ml~22.5ml;
载药PDA-CS水凝胶包括以下成分:酸多巴胺DA 0.01g~0.05g,壳聚糖CS 0.5g~2g,姜黄素或表皮生长因子或积雪草苷0.01g~0.05g,过硫酸铵APS 0.005g~0.02g,N,N-亚甲基双丙烯酰胺MBA 0.005g~0.02g,偶氮二异丁腈AIBN 0.005g~0.02g,去离子水5ml~15ml,1wt%~2wt%醋酸溶液15ml~50ml。
本发明第一种技术方案的特征还在于,
改性碳纳米管CNTs包括以下成分:碳纳米管CNT 2g~5g,浓硝酸50ml~100ml,浓硫酸10ml~30ml。
本发明的另一种技术方案是,一种自供电伤口贴片的制备方法,具体按照如下步骤实施:
步骤1,制备改性碳纳米管CNTs;
步骤2,制备PVDF/CNTs纤维,PVDF/CNTs纤维包括以下成分:聚偏氟乙烯PVDF 4.5g~7.5g、改性碳纳米管CNTs 0.5g~3.21g、丙酮C3H6O7.5ml~12ml、N,N-二甲基甲酰胺DMF18ml~22.5ml;
步骤3,将步骤2制备的PVDF/CNTs纤维通过织造工艺,织造具有一定纤维取向及孔隙率的贴片材料;
步骤4,制备载药PDA-CS水凝胶,载药PDA-CS水凝胶包括以下成分:酸多巴胺DA0.01g~0.05g,壳聚糖CS 0.5g~2g,姜黄素或表皮生长因子或积雪草苷0.01g~0.05g,过硫酸铵APS 0.005g~0.02g,N,N-亚甲基双丙烯酰胺MBA0.005g~0.02g,偶氮二异丁腈AIBN0.005g~0.02g,去离子水5ml~15ml、1wt%~2wt%醋酸溶液15ml~50ml;
步骤5,将步骤4制备的载药PDA-CS水凝胶涂敷在步骤3中的具有一定纤维取向及孔隙率的贴片材料上,得到自供电伤口贴片。
本发明另一种技术方案的特征还在于,
步骤1具体为:
步骤1.1,量取以下成分:碳纳米管CNT 2g~5g、浓硝酸50ml~100ml、浓硫酸10ml~30ml;
步骤1.2,将步骤1量取的浓硝酸和浓硫酸混合然后将量取的碳纳米管加入然后采用超声溶解;
步骤1.3,向步骤1.2经超声溶解后的溶液中加入去离子水进行离心洗涤至pH=6.5,将所得产物抽滤后在50℃真空炉中干燥12h~24h即可得到改性碳纳米管CNTs。
步骤1.2中的超声溶解是在20℃~40℃下超声溶解8h~12h。
步骤2具体为:
步骤2.1,量取以下成分:聚偏氟乙烯PVDF 4.5g~7.5g、改性碳纳米管CNTs 0.5g~3.21g、丙酮C3H6O 7.5ml~12ml、N,N-二甲基甲酰胺DMF18ml~22.5ml;
步骤2.2,将量取的改性碳纳米管均匀分散在丙酮C3H6O和N,N-二甲基甲酰胺溶液DMF的混合溶液中,在室温下进行搅拌均匀,然后将称取的聚偏氟乙烯PVDF加入,在50℃~80℃恒温下搅拌均匀,配制出纺丝液;
步骤2.3,将步骤2.2制备的纺丝液通过湿法纺丝装置,在40℃~70℃的凝固浴中,通过一定牵伸比制备出PVDF/CNTs纤维。
步骤2.2中丙酮C3H6O和N,N-二甲基甲酰胺溶液DMF的体积比为6:4或6:2。
步骤4具体为:
步骤4.1,量取以下成分:酸多巴胺DA 0.01g~0.05g,壳聚糖CS 0.5g~2g,姜黄素或表皮生长因子或积雪草苷0.01g~0.05g,过硫酸铵APS 0.005g~0.02g,N,N-亚甲基双丙烯酰胺MBA 0.005g~0.02g,偶氮二异丁腈AIBN0.005g~0.02g,去离子水5ml~15ml,1wt%~2wt%醋酸溶液15ml~50ml;
步骤4.2,将步骤4.1量取的壳聚糖CS加入醋酸溶液中,在30℃~60℃下搅拌溶解,得到淡黄色透明液体;
步骤4.3,将酸多巴胺DA加入到pH=11的去离子水中,并于室温搅拌使其自聚合为PDA溶液;
步骤4.4,将步骤4.2制备的淡黄色透明液体以及姜黄素或表皮生长因子或积雪草苷加入到步骤4.3制备的PDA溶液中,在常温下搅拌使其分散均匀,然后加入过硫酸铵APS、N,N-亚甲基双丙烯酰胺MBA、偶氮二异丁腈AIBN,然后在50℃~90℃恒温搅拌使其充分交联,得到载药PDA-CS水凝胶。
本发明的有益效果是:
本发明一种自供电伤口贴片材料,在伤口愈合止血期,通过水凝胶吸水特性达到止血和吸收渗出液的目的,在炎症期,壳聚糖水凝胶不仅能够通过自身的抗炎抗菌及湿润特性为伤口愈合提高良好的微环境,还可以触发人体巨噬细胞产生坏死因子α(TNF-α),从而引发炎症信号触发巨噬细胞活动并使伤口中的细胞因子水平增加,促进伤口愈合;另一方面在伤口愈合的增殖期,可以通过具有压电特性的PVDF/CNTs提供局部电场EFs,结合定向织造技术,它可使细胞定向有序生长,这是最终形成组织或修复组织的一个重要条件。并且本发明通过湿法纺丝制备定向超细纤维束与织造技术结合,一方面通过调控孔隙大小实现透气性能,另一方面,定向排列纤维有助于促进细胞迁移和增殖,一定程度上促进伤口愈合。压电修复功能是通过机械力转化为电信号,提供外源电场,刺激成纤细胞定向迁移、增殖和分化,进一步实现伤口加速愈合。因此,本发明通过对材料结构的调控及材料压电性能的调控,二者协同作用实现加快伤口愈合的目的,且生产成本低廉、对生产设备无特殊性要求,在生物医用材料领域具有良好的应用前景。
具体实施方式
下面结合具体实施方式对本发明进行详细说明。
本发明一种自供电伤口贴片,包括PVDF/CNTs纤维贴片,PVDF/CNTs纤维贴片上涂敷有载药PDA-CS水凝胶;
PVDF/CNTs纤维贴片包括以下成分:聚偏氟乙烯PVDF 4.5g~7.5g、改性碳纳米管CNTs 0.5g~3.21g、丙酮C3H6O 7.5ml~12ml,N,N-二甲基甲酰胺DMF 18ml~22.5ml,其中改性碳纳米管CNTs包括以下成分:碳纳米管CNT 2g~5g,浓硝酸50ml~100ml,浓硫酸10ml~30ml;
载药PDA-CS水凝胶包括以下成分:酸多巴胺DA 0.01g~0.05g,壳聚糖CS 0.5g~2g,姜黄素或表皮生长因子或积雪草苷0.01g~0.05g,过硫酸铵APS 0.005g~0.02g,N,N-亚甲基双丙烯酰胺MBA 0.005g~0.02g,偶氮二异丁腈AIBN 0.005g~0.02g,去离子水5ml~15ml,1wt%~2wt%醋酸溶液15ml~50ml。
本发明一种自供电伤口贴片的制备方法,具体按照如下步骤实施:
步骤1,制备改性碳纳米管CNTs;具体为:
步骤1.1,量取以下成分:碳纳米管CNT 2g~5g、浓硝酸50ml~100ml、浓硫酸10ml~30ml;
步骤1.2,将步骤1量取的浓硝酸和浓硫酸混合然后将量取的碳纳米管加入然后在20℃~40℃下超声溶解8h~12h;
步骤1.3,向步骤1.2经超声溶解后的溶液中加入去离子水进行离心洗涤至pH=6.5,将所得产物抽滤后在50℃真空炉中干燥12h~24h即可得到改性碳纳米管CNTs;
步骤2,制备PVDF/CNTs纤维,PVDF/CNTs纤维包括以下成分:聚偏氟乙烯PVDF 4.5g~7.5g、改性碳纳米管CNTs 0.5g~3.21g、丙酮C3H6O7.5ml~12ml、N,N-二甲基甲酰胺DMF18ml~22.5ml;具体为:
步骤2.1,量取以下成分:聚偏氟乙烯PVDF 4.5g~7.5g、改性碳纳米管CNTs 0.5g~3.21g、丙酮C3H6O 7.5ml~12ml、N,N-二甲基甲酰胺DMF18ml~22.5ml;
步骤2.2,将量取的改性碳纳米管均匀分散在丙酮C3H6O和N,N-二甲基甲酰胺溶液DMF的混合溶液中,在室温下进行搅拌均匀,然后将称取的聚偏氟乙烯PVDF加入,在50℃~80℃恒温下搅拌均匀,配制出纺丝液,其中,丙酮C3H6O和N,N-二甲基甲酰胺溶液DMF的体积比为6:4或6:2;
步骤2.3,将步骤2.2制备的纺丝液通过湿法纺丝装置,在40℃~70℃的凝固浴中,通过一定牵伸比制备出PVDF/CNTs纤维。
步骤3,将步骤2制备的PVDF/CNTs纤维通过织造工艺,织造具有一定纤维取向及孔隙率的贴片材料;
步骤4,制备载药PDA-CS水凝胶,载药PDA-CS水凝胶包括以下成分:酸多巴胺DA0.01g~0.05g,壳聚糖CS 0.5g~2g,姜黄素或表皮生长因子或积雪草苷0.01g~0.05g,过硫酸铵APS 0.005g~0.02g,N,N-亚甲基双丙烯酰胺MBA 0.005g~0.02g,偶氮二异丁腈AIBN 0.005g~0.02g,去离子水5ml~15ml、1wt%~2wt%醋酸溶液15ml~50ml;具体为:
步骤4.1,量取以下成分:酸多巴胺DA 0.01g~0.05g,壳聚糖CS 0.5g~2g,姜黄素或表皮生长因子或积雪草苷0.01g~0.05g,过硫酸铵APS 0.005g~0.02g,N,N-亚甲基双丙烯酰胺MBA 0.005g~0.02g,偶氮二异丁腈AIBN0.005g~0.02g,去离子水5ml~15ml,1wt%~2wt%醋酸溶液15ml~50ml;
步骤4.2,将步骤4.1量取的壳聚糖CS加入醋酸溶液中,在30℃~60℃下搅拌溶解,得到淡黄色透明液体;
步骤4.3,将酸多巴胺DA加入到ph=11的去离子水中,并于室温搅拌使其自聚合为PDA溶液;
步骤4.4,将步骤4.2制备的淡黄色透明液体以及姜黄素或表皮生长因子或积雪草苷加入到步骤4.3制备的PDA溶液中,在常温下搅拌使其分散均匀,然后加入过硫酸铵APS、N,N-亚甲基双丙烯酰胺MBA、偶氮二异丁腈AIBN,然后在50℃~90℃恒温搅拌使其充分交联,得到载药PDA-CS水凝胶;
步骤5,将步骤4制备的载药PDA-CS水凝胶涂敷在步骤3中的具有一定纤维取向及孔隙率的贴片材料上,得到自供电伤口贴片。
本发明将具有压电性能的PVDF与载药PDA-CS水凝胶结合,一方面可在伤口愈合止血期,通过水凝胶吸水特性达到止血和吸收渗出液的目的,在炎症期,壳聚糖水凝胶不仅能够通过自身的抗炎抗菌及湿润特性为伤口愈合提高良好的微环境,还可以触发人体巨噬细胞产生坏死因子α(TNF-α),从而引发炎症信号触发巨噬细胞活动并使伤口中的细胞因子水平增加,促进伤口愈合;另一方面在伤口愈合的增殖期通过具有压电特性的PVDF提供局部电场EFs,结合定向织造技术,它可使细胞定向有序生长,这是最终形成组织或修复组织的一个重要条件。并且本发明通过湿法纺丝制备定向超细纤维束与织造技术结合,一方面通过调控孔隙大小实现透气性能,另一方面,定向排列纤维有助于促进细胞迁移和增殖,一定程度上促进伤口愈合。压电修复功能是通过机械力转化为电信号,提供外源电场,刺激成纤细胞定向迁移、增殖和分化,进一步实现伤口加速愈合。因此,本发明通过对材料结构的调控及材料压电性能的调控,二者协同作用实现加快伤口愈合的目的。
实施例1
步骤1,改性的CNT的制备:
在容器中将2gCNT加入100ml的体积比为3:1的浓硝酸-硫酸溶液中,在20℃下超声溶解8h来除去杂质及无定形碳,引入亲水官能团后,用去离子水离心洗涤至pH=6.5,将所得产物,抽滤后在50℃真空炉中干燥12h即可得到改性的CNT,即CNTs。
步骤2,PVDF/CNTs纤维的制备:
将0.5gCNTs均匀分散在100ml体积比为6:4DMF C3H6O溶液中,在室温下辅助磁力搅拌或者机械搅拌均匀后,加入4.5gPVDF粉末,在60℃恒温下辅以磁力搅拌或机械搅拌使其分散均匀得到均匀的纺丝液前驱体后,通过湿法纺丝装置,在60℃的去离子水凝固浴中,牵伸比为4的条件下,制备出PVDF/CNTs纤维;
步骤3、将步骤2制备的PVDF/CNTs纤维通过织造工艺,织造具有一定纤维取向及孔隙率的贴片材料;
步骤4、制备载药PDA-CS水凝胶;
首先,在容器中将2.5g壳聚糖加入12.5ml1wt%醋酸溶液,在30℃恒温下辅以磁力搅拌搅拌溶解得到淡黄色透明液体后;其次,将0.02gDA加入到11.2ml的pH=11的去离子水中,并于室温下辅以磁力搅拌或机械搅拌使其自聚合为PDA;将0.0025g姜黄素加入到上述两种溶液的混合溶液中,搅拌30min后,加入0.01gAPS,0.01gMBA和0.01gAIBN,在60℃恒温下辅以磁力搅拌或机械搅拌使其充分交联,聚合更充分,即可得到自黏附载药PDA-CS水凝胶。
步骤5、将步骤4中的自黏附水凝胶涂敷在步骤3中的具有一定纤维取向及孔隙率的贴片材料上,从而获得一种自供电伤口贴片材料。
实施例2
步骤1,改性的CNT的制备:
在容器中将2gCNT加入100ml的体积比为3:1的浓硝酸-硫酸溶液中,在30℃下超声溶解10h来除去杂质及无定形碳,引入亲水官能团后,用去离子水离心洗涤至pH=6.5,将所得产物,抽滤后在50℃真空炉中干燥12h即可得到改性的CNT,即CNTs。
步骤2,PVDF/CNTs纤维的制备:
将1.125gCNTs均匀分散在100ml体积比为6:2DMF C3H6O溶液中,在室温下辅助磁力搅拌或者机械搅拌均匀后,加入4.5gPVDF粉末,在60℃恒温下辅以磁力搅拌或机械搅拌使其分散均匀得到均匀的纺丝液前驱体后,通过湿法纺丝装置,在60℃的去离子水凝固浴中,牵伸比为5的条件下,制备出PVDF/CNTs纤维;
步骤3、将步骤2制备的PVDF/CNTs纤维通过织造工艺,织造具有一定纤维取向及孔隙率的贴片材料;
步骤4、制备载药PDA-CS水凝胶;
首先,在容器中将2.5g壳聚糖加入12.5ml1wt%醋酸溶液,在40℃恒温下辅以磁力搅拌搅拌溶解得到淡黄色透明液体后;其次,将0.02gDA加入到11.2ml的pH=11的去离子水中,并于室温下辅以磁力搅拌或机械搅拌使其自聚合为PDA;将0.0025g表皮生长因子加入到上述两种溶液的混合溶液中,搅拌30min后,加入0.01gAPS,0.02gMBA和0.02gAIBN,在60℃恒温下辅以磁力搅拌或机械搅拌使其充分交联,聚合更充分,即可得到自黏附载药PDA-CS水凝胶。
步骤5、将步骤4中的自黏附水凝胶涂敷在步骤3中的具有一定纤维取向及孔隙率的贴片材料上,从而获得一种自供电伤口贴片材料。
实施例3
步骤1,改性的CNT的制备:
在容器中将2gCNT加入100ml的体积比为3:1的浓硝酸-硫酸溶液中,在30℃下超声溶解10h来除去杂质及无定形碳,引入亲水官能团后,用去离子水离心洗涤至pH=6.5,将所得产物,抽滤后在50℃真空炉中干燥24h即可得到改性的CNT,即CNTs。
步骤2,PVDF/CNTs纤维的制备:
将0.667gCNTs均匀分散在100ml体积比为6:4DMF C3H6O溶液中,在室温下辅助磁力搅拌或者机械搅拌均匀后,加入6gPVDF粉末,在60℃恒温下辅以磁力搅拌或机械搅拌使其分散均匀得到均匀的纺丝液前驱体后,通过湿法纺丝装置,在70℃的去离子水凝固浴中,牵伸比为4的条件下,制备出PVDF/CNTs纤维;
步骤3、将步骤2制备的PVDF/CNTs纤维通过织造工艺,织造具有一定纤维取向及孔隙率的贴片材料;
步骤4、制备载药PDA-CS水凝胶;
首先,在容器中将2.5g壳聚糖加入12.5ml1wt%醋酸溶液,在30℃恒温下辅以磁力搅拌搅拌溶解得到淡黄色透明液体后;其次,将0.02gDA加入到11.2ml的pH=11的去离子水中,并于室温下辅以磁力搅拌或机械搅拌使其自聚合为PDA;将0.0025g积雪草苷加入到上述两种溶液的混合溶液中,搅拌50min后,加入0.01gAPS,0.02gMBA和0.02gAIBN,在60℃恒温下辅以磁力搅拌或机械搅拌使其充分交联,聚合更充分,即可得到自黏附载药PDA-CS水凝胶。
步骤5、将步骤4中的自黏附水凝胶涂敷在步骤3中的具有一定纤维取向及孔隙率的贴片材料上,从而获得一种自供电伤口贴片材料。
实施例4
步骤1,改性的CNT的制备:
在容器中将2gCNT加入100ml的体积比为3:1的浓硝酸-硫酸溶液中,在30℃下超声溶解10h来除去杂质及无定形碳,引入亲水官能团后,用去离子水离心洗涤至pH=6.5,将所得产物,抽滤后在50℃真空炉中干燥24h即可得到改性的CNT,即CNTs。
步骤2,PVDF/CNTs纤维的制备:
将0.833gCNTs均匀分散在100ml体积比为6:4DMF C3H6O溶液中,在室温下辅助磁力搅拌或者机械搅拌均匀后,加入7.5gPVDF粉末,在60℃恒温下辅以磁力搅拌或机械搅拌使其分散均匀得到均匀的纺丝液前驱体后,通过湿法纺丝装置,在60℃的去离子水凝固浴中,牵伸比为6的条件下,制备出PVDF/CNTs纤维;
步骤3、将步骤2制备的PVDF/CNTs纤维通过织造工艺,织造具有一定纤维取向及孔隙率的贴片材料;
步骤4、制备载药PDA-CS水凝胶;
首先,在容器中将2.5g壳聚糖加入12.5ml1wt%醋酸溶液,在30℃恒温下辅以磁力搅拌搅拌溶解得到淡黄色透明液体后;其次,将0.02gDA加入到11.2ml的pH=11的去离子水中,并于室温下辅以磁力搅拌或机械搅拌使其自聚合为PDA;将0.0025g姜黄素加入到上述两种溶液的混合溶液中,搅拌50min后,加入0.01gAPS,0.02gMBA和0.02gAIBN,在60℃恒温下辅以磁力搅拌或机械搅拌使其充分交联,聚合更充分,即可得到自黏附载药PDA-CS水凝胶。
步骤5、将步骤4中的自黏附水凝胶涂敷在步骤3中的具有一定纤维取向及孔隙率的贴片材料上,从而获得一种自供电伤口贴片材料。
实施例5
步骤1,改性的CNT的制备:
在容器中将2gCNT加入100ml的体积比为3:1的浓硝酸-硫酸溶液中,在30℃下超声溶解10h来除去杂质及无定形碳,引入亲水官能团后,用去离子水离心洗涤至pH=6.5,将所得产物,抽滤后在50℃真空炉中干燥24h即可得到改性的CNT,即CNTs。
步骤2,PVDF/CNTs纤维的制备:
将1.5gCNTs均匀分散在100ml体积比为6:4DMF C3H6O溶液中,在室温下辅助磁力搅拌或者机械搅拌均匀后,加入6gPVDF粉末,在60℃恒温下辅以磁力搅拌或机械搅拌使其分散均匀得到均匀的纺丝液前驱体后,通过湿法纺丝装置,在60℃的去离子水凝固浴中,牵伸比为5的条件下,制备出PVDF/CNTs纤维;
步骤3、将步骤2制备的PVDF/CNTs纤维通过织造工艺,织造具有一定纤维取向及孔隙率的贴片材料;
步骤4、制备载药PDA-CS水凝胶;
首先,在容器中将2.5g壳聚糖加入12.5ml1wt%醋酸溶液,在30℃恒温下辅以磁力搅拌搅拌溶解得到淡黄色透明液体后;其次,将0.02gDA加入到11.2ml的pH=11的去离子水中,并于室温下辅以磁力搅拌或机械搅拌使其自聚合为PDA;将0.0025g积雪草苷加入到上述两种溶液的混合溶液中,搅拌30min后,加入0.01gAPS,0.02gMBA和0.02gAIBN,在60℃恒温下辅以磁力搅拌或机械搅拌使其充分交联,聚合更充分,即可得到自黏附载药PDA-CS水凝胶。
步骤5、将步骤4中的自黏附水凝胶涂敷在步骤3中的具有一定纤维取向及孔隙率的贴片材料上,从而获得一种自供电伤口贴片材料。
Claims (8)
1.一种自供电伤口贴片,其特征在于,包括PVDF/CNTs纤维贴片,所述PVDF/CNTs纤维贴片上涂敷有载药PDA-CS水凝胶;
所述PVDF/CNTs纤维贴片包括以下成分:聚偏氟乙烯PVDF 4.5g~7.5g、改性碳纳米管CNTs 0.5g~3.21g、丙酮C3H6O 7.5ml~12ml,N,N-二甲基甲酰胺DMF 18ml~22.5ml;
所述载药PDA-CS水凝胶包括以下成分:酸多巴胺DA 0.01g~0.05g,壳聚糖CS 0.5g~2g,姜黄素或表皮生长因子或积雪草苷0.01g~0.05g,过硫酸铵APS 0.005g~0.02g,N,N-亚甲基双丙烯酰胺MBA 0.005g~0.02g,偶氮二异丁腈AIBN 0.005g~0.02g,去离子水5ml~15ml,1wt%l~2wt%醋酸溶液15ml l~50ml。
2.根据权利要求1所述的一种自供电伤口贴片,其特征在于,所述改性碳纳米管CNTs包括以下成分:碳纳米管CNT 2g~5g,浓硝酸50ml~100ml,浓硫酸10ml~30ml。
3.一种自供电伤口贴片的制备方法,其特征在于,具体按照如下步骤实施:
步骤1,制备改性碳纳米管CNTs;
步骤2,制备PVDF/CNTs纤维,PVDF/CNTs纤维包括以下成分:聚偏氟乙烯PVDF 4.5g~7.5g、改性碳纳米管CNTs 0.5g~3.21g、丙酮C3H6O 7.5ml~12ml、N,N-二甲基甲酰胺DMF18ml~22.5ml;
步骤3,将步骤2制备的PVDF/CNTs纤维通过织造工艺,织造具有一定纤维取向及孔隙率的贴片材料;
步骤4,制备载药PDA-CS水凝胶,载药PDA-CS水凝胶包括以下成分:酸多巴胺DA 0.01g~0.05g,壳聚糖CS 0.5g~2g,姜黄素或表皮生长因子或积雪草苷0.01g~0.05g,过硫酸铵APS 0.005g~0.02g,N,N-亚甲基双丙烯酰胺MBA 0.005g~0.02g,偶氮二异丁腈AIBN0.005g~0.02g,去离子水5ml~15ml、1wt%-2wt%醋酸溶液15ml-50ml;
步骤5,将步骤4制备的载药PDA-CS水凝胶涂敷在步骤3中的具有一定纤维取向及孔隙率的贴片材料上,得到自供电伤口贴片。
4.根据权利要求3所述的一种自供电伤口贴片的制备方法,其特征在于,所述步骤1具体为:
步骤1.1,量取以下成分:碳纳米管CNT 2g~5g、浓硝酸50ml~100ml、浓硫酸10ml~30ml;
步骤1.2,将步骤1量取的浓硝酸和浓硫酸混合然后将量取的碳纳米管加入然后采用超声溶解;
步骤1.3,向步骤1.2经超声溶解后的溶液中加入去离子水进行离心洗涤至pH=6.5,将所得产物抽滤后在50℃真空炉中干燥12h~24h即可得到改性碳纳米管CNTs。
5.根据权利要求4所述的一种自供电伤口贴片的制备方法,其特征在于,所述步骤1.2中的超声溶解是在20℃~40℃下超声溶解8h~12h。
6.根据权利要求5所述的一种自供电伤口贴片的制备方法,其特征在于,所述步骤2具体为:
步骤2.1,量取以下成分:聚偏氟乙烯PVDF 4.5g~7.5g、改性碳纳米管CNTs 0.5g~3.21g、丙酮C3H6O 7.5ml~12ml、N,N-二甲基甲酰胺DMF 18ml~22.5ml;
步骤2.2,将量取的改性碳纳米管均匀分散在丙酮C3H6O和N,N-二甲基甲酰胺溶液DMF的混合溶液中,在室温下进行搅拌均匀,然后将称取的聚偏氟乙烯PVDF加入,在50℃~80℃恒温下搅拌均匀,配制出纺丝液;
步骤2.3,将步骤2.2制备的纺丝液通过湿法纺丝装置,在40℃~70℃的凝固浴中,通过一定牵伸比制备出PVDF/CNTs纤维。
7.根据权利要求6所述的一种自供电伤口贴片的制备方法,其特征在于,所述步骤2.2中丙酮C3H6O和N,N-二甲基甲酰胺溶液DMF的体积比为6:4或6:2。
8.根据权利要求6所述的一种自供电伤口贴片的制备方法,其特征在于,所述步骤4具体为:
步骤4.1,量取以下成分:酸多巴胺DA 0.01g~0.05g,壳聚糖CS 0.5g~2g,姜黄素或表皮生长因子或积雪草苷0.01g~0.05g,过硫酸铵APS 0.005g~0.02g,N,N-亚甲基双丙烯酰胺MBA 0.005g~0.02g,偶氮二异丁腈AIBN 0.005g~0.02g,去离子水5ml~15ml,1wt%~2wt%醋酸溶液15ml~50ml;
步骤4.2,将步骤4.1量取的壳聚糖CS加入醋酸溶液中,在30℃~60℃下搅拌溶解,得到淡黄色透明液体;
步骤4.3,将酸多巴胺DA加入到pH=11的去离子水中,并于室温搅拌使其自聚合为PDA溶液;
步骤4.4,将步骤4.2制备的淡黄色透明液体以及姜黄素或表皮生长因子或积雪草苷加入到步骤4.3制备的PDA溶液中,在常温下搅拌使其分散均匀,然后加入过硫酸铵APS、N,N-亚甲基双丙烯酰胺MBA、偶氮二异丁腈AIBN,然后在50℃~90℃恒温搅拌使其充分交联,得到载药PDA-CS水凝胶。
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