CN115531603A - 一种多功能聚合物水凝胶敷料及其制备方法 - Google Patents
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Abstract
本发明提供了一种多功能聚合物水凝胶敷料及其制备方法,属于聚合物水凝胶技术领域。本发明通过将酰肼化合物在碳二亚胺的作用下接枝于含羧基的多糖聚合物上,得到改性多糖聚合物;将改性多糖聚合物配制成改性多糖聚合物水溶液,将磺酸基甜菜碱甲基丙烯酸酯和改性多糖聚合物水溶液混合后进行交联反应,得到聚合物水凝胶;将天然抗菌剂与聚合物水凝胶混合后进行多次冷冻‑解冻,即得到多功能聚合物水凝胶敷料。本发明先对多糖聚合物进行接枝改性,在酰肼基团的作用下可原位与磺酸基甜菜碱甲基丙烯酸酯进行交联反应,显著提高了聚合物水凝胶敷料的透氧性能和伤口的愈合速率。
Description
技术领域
本发明涉及聚合物水凝胶技术领域,尤其涉及一种多功能聚合物水凝胶敷料及其制备方法。
背景技术
伤口细菌感染是临床常见的疾病,其主要治疗手段是抗生素治疗。近年来,由于抗生素滥用而导致的严重细菌耐药,已经成为威胁全球人类健康的重大医疗问题。因此,需要不断开发新型抗生素,消耗大量人力、物力,还无法从根本上解决问题。频繁更换敷料会增加患者的痛苦和治疗费用。
相比于传统的医用敷料,水凝胶医用敷料是近年来发展起来的一种新型的创伤敷料。与其它类型的敷料相比,其优点包括:水凝胶基质可以提供湿润的组织接触环境,具有良好的细胞相容性,能够吸收伤口渗出液,不与组织粘连从而避免更换敷料时带来的二次损伤等。
然而,目前的水凝胶医用敷料的含水率低、透氧性能差、抗蛋白吸附能力低,在实际应用中,水凝胶敷料的透氧性能差,使创口不能及时的接触空气,导致创口渗液严重,愈合效果不好。
因此,如何改进现有的水凝胶敷料,得到一种透氧性好、抗蛋白吸附能力好、伤口愈合快的多功能聚合物水凝胶敷料,是目前需要解决的技术问题。
发明内容
本发明的目的在于提供一种多功能聚合物水凝胶敷料及其制备方法,以解决现有水凝胶敷料透氧性能差、伤口愈合效果不佳的技术问题。
为了实现上述发明目的,本发明提供以下技术方案:
本发明提供了一种多功能聚合物水凝胶敷料的制备方法,包括以下步骤:
1)将酰肼化合物在碳二亚胺的作用下接枝于含羧基的多糖聚合物上,得到改性多糖聚合物;
2)将改性多糖聚合物配制成改性多糖聚合物水溶液,将磺酸基甜菜碱甲基丙烯酸酯和改性多糖聚合物水溶液混合后进行交联反应,得到聚合物水凝胶;
3)将天然抗菌剂与聚合物水凝胶混合后进行多次冷冻-解冻,即得到多功能聚合物水凝胶敷料。
进一步的,所述步骤1)中,所述酰肼化合物包含3,3'-二硫代二丙酰肼、2,2'-二硫代二乙酰肼、4,4'-二硫代二丁酰肼、己二酸二酰肼、丙二酸二酰肼、丁二酸二酰肼和癸二酸二酰肼中的一种或几种;
所述含羧基的多糖聚合物包含透明质酸、海藻酸钠、羧甲基纤维素钠和羧甲基壳聚糖中的一种或几种。
进一步的,所述酰肼化合物、碳二亚胺和含羧基的多糖聚合物中的羧基的摩尔比为5~20:0.2~0.5:1。
进一步的,所述步骤2)中,改性多糖聚合物水溶液的质量浓度为1~10%。
进一步的,所述磺酸基甜菜碱甲基丙烯酸酯和含羧基的多糖聚合物中的羧基的摩尔比为5~10:1。
进一步的,所述交联反应在溶剂中进行,所述溶剂为去离子水或乙二醇。
进一步的,所述交联反应的温度为60~90℃,交联反应的时间为5~8h。
进一步的,所述天然抗菌剂包含甲壳素、壳聚糖、芥末和蓖麻油中的一种或几种,所述天然抗菌剂和聚合物水凝胶的质量比为0.1~0.5:1。
进一步的,所述步骤3)中,多次冷冻-解冻的次数为2~4次,所述冷冻的温度独立的为-30~-10℃,冷冻的时间独立的为2~8h。
本发明提供了一种多功能聚合物水凝胶敷料。
本发明的有益效果:
本发明通过采用酰肼化合物接枝改性含羧基的多糖聚合物,得到的改性多糖聚合物可直接与磺酸基甜菜碱甲基丙烯酸酯进行原位交联反应,无需额外添加交联剂,通过调控磺酸基甜菜碱甲基丙烯酸酯与羧基的含量,可得到多功能聚合物水凝胶敷料,提高了聚合物水凝胶敷料的透氧性能,明显提高了伤口的愈合速率。
具体实施方式
本发明提供了一种多功能聚合物水凝胶敷料的制备方法,包括以下步骤:
1)将酰肼化合物在碳二亚胺的作用下接枝于含羧基的多糖聚合物上,得到改性多糖聚合物;
2)将改性多糖聚合物配制成改性多糖聚合物水溶液,将磺酸基甜菜碱甲基丙烯酸酯和改性多糖聚合物水溶液混合后进行交联反应,得到聚合物水凝胶;
3)将天然抗菌剂与聚合物水凝胶混合后进行多次冷冻-解冻,即得到多功能聚合物水凝胶敷料。
在本发明中,所述步骤1)中,所述酰肼化合物包含3,3'-二硫代二丙酰肼、2,2'-二硫代二乙酰肼、4,4'-二硫代二丁酰肼、己二酸二酰肼、丙二酸二酰肼、丁二酸二酰肼和癸二酸二酰肼中的一种或几种,优选为3,3'-二硫代二丙酰肼、己二酸二酰肼和癸二酸二酰肼中的一种或几种。
在本发明中,所述含羧基的多糖聚合物包含透明质酸、海藻酸钠、羧甲基纤维素钠和羧甲基壳聚糖中的一种或几种,优选为海藻酸钠和/或羧甲基纤维素钠。
在本发明中,所述步骤1)中,改性多糖聚合物的取代度为10~50%,优选为20~40%,进一步优选为30%。
在本发明中,所述酰肼化合物、碳二亚胺和含羧基的多糖聚合物中的羧基的摩尔比为5~20:0.2~0.5:1,优选为8~18:0.3~0.4:1,进一步优选为10~15:0.35:1。
在本发明中,所述碳二亚胺优选为1-(3-二甲氨基丙基)-3-乙基碳二亚胺盐酸盐。
在本发明中,所述步骤2)中,改性多糖聚合物水溶液的质量浓度为1~10%,优选为2~8%,进一步优选为3~6%。
在本发明中,所述磺酸基甜菜碱甲基丙烯酸酯和含羧基的多糖聚合物中的羧基的摩尔比为5~10:1,优选为6~9:1,进一步优选为7~8:1。
在本发明中,所述交联反应在溶剂中进行,所述溶剂为去离子水或乙二醇,优选为去离子水。
在本发明中,所述交联反应的温度为60~90℃,优选为65~85℃,进一步优选为70~75℃;交联反应的时间为5~8h,优选为6~7h,进一步优选为6.5h。
在本发明中,所述天然抗菌剂包含甲壳素、壳聚糖、芥末和蓖麻油中的一种或几种,优选为甲壳素;所述天然抗菌剂和聚合物水凝胶的质量比为0.1~0.5:1,优选为0.2~0.4:1,进一步优选为0.3:1。
在本发明中,所述步骤3)中,多次冷冻-解冻的次数为2~4次,优选为3次;所述冷冻的温度独立的为-30~-10℃,优选为-25~-15℃,进一步优选为-20℃;冷冻的时间独立的为2~8h,优选为3~7h,进一步优选为4~6h。
本发明提供了一种多功能聚合物水凝胶敷料。
下面结合实施例对本发明提供的技术方案进行详细的说明,但是不能把它们理解为对本发明保护范围的限定。
实施例1
多功能聚合物水凝胶敷料的制备:
1)将分子量500kDa的海藻酸钠配制成质量浓度为2%的水溶液,加入海藻酸钠中羧基摩尔量0.5倍的1-(3-二甲氨基丙基)-3-乙基碳二亚胺盐酸盐和海藻酸钠中羧基摩尔量5倍的3,3'-二硫代二丙酰肼,经过室温反应5h后用截留分子量为2000Da的透析袋对水透析3天,再经零下20摄氏度冷冻干燥10小时,得到取代度为50%的改性海藻酸钠;
2)将步骤1)所得改性海藻酸钠溶于水中,配制成质量浓度为5%的水溶液,将海藻酸钠中羧基摩尔量2倍的磺酸基甜菜碱甲基丙烯酸酯与5%的水溶液混合,在60℃下交联反应8h,得到聚合物水凝胶;
3)取步骤2)所得聚合物水凝胶0.2倍的甲壳素和0.1倍的蓖麻油混合于聚合物水凝胶中,在-20℃下冷冻8h后解冻,进行3次冷冻-解冻,最后得到多功能聚合物水凝胶敷料。
实施例2
多功能聚合物水凝胶敷料的制备:
1)将分子量1000kDa的透明质酸配制成质量浓度为1%的水溶液,加入透明质酸中羧基摩尔量0.3倍的1-(3-二甲氨基丙基)-3-乙基碳二亚胺盐酸盐和透明质酸中羧基摩尔量10倍的2,2'-二硫代二乙酰肼,经过室温反应8h后用截留分子量为2000Da的透析袋对水透析3天,再经零下20摄氏度冷冻干燥10小时,得到取代度为30%的改性透明质酸;
2)将步骤1)所得改性透明质酸溶于水中,配制成质量浓度为8%的水溶液,将透明质酸中羧基摩尔量5倍的磺酸基甜菜碱甲基丙烯酸酯与8%的水溶液混合,在70℃下交联反应8h,得到聚合物水凝胶;
3)取步骤2)所得聚合物水凝胶0.2倍的壳聚糖和0.1倍的芥末混合于聚合物水凝胶中,在-30℃下冷冻5h后解冻,进行3次冷冻-解冻,最后得到多功能聚合物水凝胶敷料。
实施例3
多功能聚合物水凝胶敷料的制备:
1)将分子量800kDa的羧甲基纤维素钠配制成质量浓度为5%的水溶液,加入羧甲基纤维素钠中羧基摩尔量0.2倍的1-(3-二甲氨基丙基)-3-乙基碳二亚胺盐酸盐和羧甲基纤维素钠中羧基摩尔量15倍的己二酸二酰肼,经过室温反应8h后用截留分子量为2000Da的透析袋对水透析3天,再经零下20摄氏度冷冻干燥10小时,得到取代度为45%的改性羧甲基纤维素钠;
2)将步骤1)所得改性羧甲基纤维素钠溶于水中,配制成质量浓度为10%的水溶液,将羧甲基纤维素钠中羧基摩尔量8倍的磺酸基甜菜碱甲基丙烯酸酯与10%的水溶液混合,在75℃下交联反应8h,得到聚合物水凝胶;
3)取步骤2)所得聚合物水凝胶0.2倍的壳聚糖和0.1倍的芥末混合于聚合物水凝胶中,在-30℃下冷冻5h后解冻,进行2次冷冻-解冻,最后得到多功能聚合物水凝胶敷料。
实施例4
多功能聚合物水凝胶敷料的制备:
1)将分子量1000kDa的羧甲基壳聚糖配制成质量浓度为5%的水溶液,加入羧甲基壳聚糖中羧基摩尔量0.2倍的1-(3-二甲氨基丙基)-3-乙基碳二亚胺盐酸盐和羧甲基壳聚糖中羧基摩尔量20倍的丙二酸二酰肼,经过室温反应8h后用截留分子量为2000Da的透析袋对水透析3天,再经零下20摄氏度冷冻干燥10小时,得到取代度为50%的改性羧甲基壳聚糖;
2)将步骤1)所得改性羧甲基壳聚糖溶于水中,配制成质量浓度为2%的水溶液,将羧甲基壳聚糖中羧基摩尔量10倍的磺酸基甜菜碱甲基丙烯酸酯与2%的水溶液混合,在75℃下交联反应8h,得到聚合物水凝胶;
3)取步骤2)所得聚合物水凝胶0.5倍的壳聚糖混合于聚合物水凝胶中,在-30℃下冷冻5h后解冻,进行4次冷冻-解冻,最后得到多功能聚合物水凝胶敷料。
实验例1
对实施例1~4所得多功能聚合物水凝胶敷料进行性能测试,结果如下表1。
表1实施例1~4所得多功能聚合物水凝胶敷料的性能测试
项目 | 氧渗透率/barrer | 抗压强度/MPa | 含水率/% |
实施例1 | 55.6 | 21.5 | 67 |
实施例2 | 60.1 | 20.2 | 65 |
实施例3 | 63.2 | 22.5 | 66 |
实施例4 | 68.7 | 23.1 | 69 |
实验例2
测试多功能聚合物水凝胶敷料对SD大鼠深Ⅱ度烧伤创面的愈合效率,结果见下表2。
表2SD大鼠深Ⅱ度烧伤后创面面积统计结果
由以上实施例可知,本发明提供了一种多功能聚合物水凝胶敷料及其制备方法。本发明的多功能聚合物水凝胶敷料具备高氧渗透性和含水率,用于患者皮肤创伤的治疗,可改善患者皮肤的不适感,减少积液的产生,有助于创口的愈合。经过测试发现,使用本发明的多功能聚合物水凝胶敷料创伤愈合速率快,可在10天左右愈合,效果显著,使用过程中无需换药,吸收伤口产生的积液,愈合后伤口表面干燥。可见,本发明的多功能对于伤口的愈合作用显著。
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 (10)
1.一种多功能聚合物水凝胶敷料的制备方法,其特征在于,包括以下步骤:
1)将酰肼化合物在碳二亚胺的作用下接枝于含羧基的多糖聚合物上,得到改性多糖聚合物;
2)将改性多糖聚合物配制成改性多糖聚合物水溶液,将磺酸基甜菜碱甲基丙烯酸酯和改性多糖聚合物水溶液混合后进行交联反应,得到聚合物水凝胶;
3)将天然抗菌剂与聚合物水凝胶混合后进行多次冷冻-解冻,即得到多功能聚合物水凝胶敷料。
2.根据权利要求1所述的多功能聚合物水凝胶敷料的制备方法,其特征在于,所述步骤1)中,所述酰肼化合物包含3,3'-二硫代二丙酰肼、2,2'-二硫代二乙酰肼、4,4'-二硫代二丁酰肼、己二酸二酰肼、丙二酸二酰肼、丁二酸二酰肼和癸二酸二酰肼中的一种或几种;
所述含羧基的多糖聚合物包含透明质酸、海藻酸钠、羧甲基纤维素钠和羧甲基壳聚糖中的一种或几种。
3.根据权利要求2所述的多功能聚合物水凝胶敷料的制备方法,其特征在于,所述酰肼化合物、碳二亚胺和含羧基的多糖聚合物中的羧基的摩尔比为5~20:0.2~0.5:1。
4.根据权利要求1~3任意一项所述的多功能聚合物水凝胶敷料的制备方法,其特征在于,所述步骤2)中,改性多糖聚合物水溶液的质量浓度为1~10%。
5.根据权利要求4所述的多功能聚合物水凝胶敷料的制备方法,其特征在于,所述磺酸基甜菜碱甲基丙烯酸酯和含羧基的多糖聚合物中的羧基的摩尔比为5~10:1。
6.根据权利要求1或2或5所述的多功能聚合物水凝胶敷料的制备方法,其特征在于,所述交联反应在溶剂中进行,所述溶剂为去离子水或乙二醇。
7.根据权利要求6所述的多功能聚合物水凝胶敷料的制备方法,其特征在于,所述交联反应的温度为60~90℃,交联反应的时间为5~8h。
8.根据权利要求1或5或7所述的多功能聚合物水凝胶敷料的制备方法,其特征在于,所述天然抗菌剂包含甲壳素、壳聚糖、芥末和蓖麻油中的一种或几种,所述天然抗菌剂和聚合物水凝胶的质量比为0.1~0.5:1。
9.根据权利要求8所述的多功能聚合物水凝胶敷料的制备方法,其特征在于,所述步骤3)中,多次冷冻-解冻的次数为2~4次,所述冷冻的温度独立的为-30~-10℃,冷冻的时间独立的为2~8h。
10.权利要求1~9任意一项所述制备方法得到的多功能聚合物水凝胶敷料。
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