CN115252885A - 一种多重氢键交联的水凝胶敷料及其制备和应用 - Google Patents
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Abstract
本发明公开了一种多重氢键交联的水凝胶敷料及其制备和应用,所述水凝胶敷料的原料包括明胶溶液和聚乙二醇,其中明胶与聚乙二醇的质量比为1:(1.2~2.2);进一步地,其原料还包括蛋白核小球藻提取物。该水凝胶敷料能够有效避免交联剂的使用故其生物相容性高,而且具有优异的力学性能和自粘附性能,即使在在极低温度下也可以保持柔软,在创面愈合领域具备应用潜力。
Description
技术领域
本发明属于水凝胶敷料技术领域,具体涉及一种多重氢键交联的水凝胶敷料及其制备和应用。
背景技术
水凝胶敷料是由非水溶性多聚体组成的一种含有大量水分的网状高分子溶胀体,具有良好的吸水性,水凝胶与创面接触时可发生反复水合作用,具有向创面提供水分与吸收渗液的双重功能,是目前临床常用的一种新型医用敷料。
明胶是一种胶原蛋白衍生物,由于其生物相容性好、免疫原性低、能诱导细胞粘附等能力,被广泛应用于水凝胶敷料的制备中。但明胶具有易降解、力学性能差、失水快、零度以下结冰、37℃不能凝胶等缺点,极大地限制了明胶水凝胶的临床应用。
目前,主要采用以下技术手段来解决明胶的缺陷:利用化学交联剂(如戊二醛,1-(3-二甲氨基丙基)-3-乙基碳二亚胺盐酸盐等)改善明胶易降解和力学性能差的缺点,但这些交联剂都具有一定的毒性成分的化学物质;或用甲基丙烯酸酐和半胱胺改性明胶,形成甲基丙烯酸酰化明胶水凝胶,但其在合成过程中又需要在去离子水中透析5-7天,以完全去除潜在小分子杂质,这限制了明胶基水凝胶的工业化生产和应用。因此开发一款制备简单、绿色合成且具有良好力学性能的明胶基水凝胶变得极为迫切。
发明内容
有鉴于此,本发明的目的在于提供一种无外加交联剂的明胶基水凝胶敷料,其具有优异得生物相容性和力学性能,适用于创面的愈合修复。
为了实现上述目的,本发明的技术方案具体如下:
一种多重氢键交联的水凝胶敷料,包括明胶溶液和聚乙二醇,其中明胶与聚乙二醇的质量比为1:(1.2~2.2)。
进一步地,在上述技术方案中,聚乙二醇的分子量为200,明胶溶液的溶剂为PBS缓冲液或水,且溶剂与聚乙二醇的体积比为1:(0.7~2.0)。
进一步地,在上述技术方案中,水凝胶敷料中还包括蛋白核小球藻提取物。
本发明还进一步提供了上述水凝胶敷料的制备方法,当水凝胶敷料中不含有蛋白核小球藻提取物时,其具体为:将明胶溶于溶剂中制备明胶溶液,再加入聚乙二醇,搅拌混合后注入模具,待充分交联后得到水凝胶敷料。
当水凝胶敷料中含有蛋白核小球藻提取物时,其制备方法为:先将蛋白核小球藻分别置于提取剂A和提取剂B中进行提取,待提取反应结束后,离心取上清,分别得到提取液A和提取液B;其中提取剂A为明胶溶液的溶剂,提取剂B为聚乙二醇;再将明胶溶于提取剂A,然后加入提取液B,搅拌混合后注入模具,待充分交联后得到水凝胶敷料。
进一步地,在上述技术方案中,步骤S1中的提取反应的温度为60~100℃且反应时间为2~6h;另外,蛋白核小球藻与提取剂A或提取剂B的质量体积比为(80~140)mg:1mL。
本发明的有益效果为:
1)本发明利用明胶与聚乙二醇之间多重氢键的交联作用,通过调节二者比例控制凝胶强度,避免了有毒交联剂的使用;
2)分别不同的提取剂提取蛋白核小球藻,不仅可以充分提取蛋白核小球藻中的活性成分,并通过两种提取液的合理配比,利用明胶与提取物中的羧基、氨基、羟基等官能团的相互作用,进一步提高水凝胶的力学性能和自粘附性能;
3)本发明的水凝胶不含有毒交联剂,且包含来自于蛋白核小球藻的活性成分,故具备良好的生物相容性,能有效促进创面的愈合;
4)本发明制备的水凝胶敷料在极低温度下也可以保持柔软,具备抗冻性,故可在极端低温下使用。
附图说明
图1为实施例2和实施例4制备的水凝胶敷料的成胶检测结果图;
图2为实施例1制备的水凝胶敷料的SEM图;
图3为各实施例制备的水凝胶敷料的粘附强度对比图;
图4为实施例3制备的水凝胶敷料的皮肤粘附性效果图;
图5为各实施例制备的水凝胶敷料的DSC抗冻曲线图;
图6为各实施例制备的水凝胶敷料的的拉力曲线图。
具体实施方式
下面结合附图及具体实施例,对本发明进行详细说明。应当说明,此处描述的具体实施例仅用于解释本发明,并不用于限定于本发明。
下述实施例中,若无特殊说明,均为常规方法;所用试剂和材料,若无特殊说明,均可从商业途径获得。
实施例1
本实施的水凝胶敷料通过以下过程制备:
取明胶溶于PBS缓冲液中,再加入聚乙二醇200,于60℃下混合后注入模具中,得到水凝胶敷料,记为PGel-1。其中PBS缓冲液与聚乙二醇200的体积比为1:0.88,明胶与聚乙二醇的质量比为1:1.3。
实施例2
与实施例1不同的是,PBS缓冲液与聚乙二醇200的体积比1:1.3,明胶与聚乙二醇的质量比为1:1.6,所得水凝胶敷料记为PGel-2。
实施例3
与实施例1不同的是,PBS缓冲液与聚乙二醇200的体积比1:2,明胶与聚乙二醇的质量比为1:2,所得水凝胶敷料记为PGel-3。
实施例4
本实施的水凝胶敷料通过以下过程制备:
(1)分别称取1.25g蛋白核小球藻溶于10mLPBS缓冲液和10mL聚乙二醇200中,于80℃反应4h;然后以5000rpm离心5分钟,收集上清,分别得到PBS提取液和聚乙二醇提取液。
(2)称取明胶溶于PBS提取液中,再加入聚乙二醇提取液中,于60℃下混合,将混合溶液注入模具中,得到小球藻水凝胶,记为CPGel。其中,PBS提取液与聚乙二醇提取液的体积比为1:1.3,明胶与聚乙二醇的比例为1:1.6。
对比例1
与实施例2不同的是,未加入聚乙二醇200。明胶在PBS缓冲液中不会成胶,仍为溶液状态。
对上述制备的水凝胶敷料进行以下检测:
①成胶性试验:将实施例2和实施例4制备的水凝胶置于样品瓶底部,对照品为对比例1中的明胶溶液,结果如图1所示:对比例1(图1中a)中的明胶溶液在重力作用下自然由底部流动至瓶盖处,而实施例2(图1中b)和实施例4(图1中c)的样品依然留在底部,说明在没有外加交联剂的情况下,明胶与聚乙二醇、蛋白核小球藻提取物可以自组装成水凝胶,且具有良好的粘附性能。
②水凝胶SEM试验:将实施例1制备的水凝胶充分水洗后于冷冻干燥机中冻干,表面喷金后用SEM观察其结构形态,结果如图2所示:水凝胶呈现典型的蜂窝状结构。
③粘附性检测:按照GB/T 2791—1995评价实施例4制备的水凝胶敷料对基底的粘结能力,结果如图3所示:在温室条件下,各水凝胶与基底粘度强度适中,其中实施例3制备的水凝胶的粘结强度为16Kpa;实施例4的水凝胶粘结强度较实施例2高,说明蛋白核小球藻提取物能提高凝胶的粘结能力。
以手部皮肤为基底,进一步检测实施例4所得水凝胶敷料的粘结能力,如图4所示,与皮肤具有很好的贴合性,可随皮肤弯折拉伸。
④抗冻性:使用DSC仪器测量各实施例制备的水凝胶的抗冻范围,结果如图5所示:对比例1的在0℃,出现了相转变温度,说明低于0℃,水凝胶会不再柔软,而实施例1,在-56℃,出现了相转变温度,说明在在-56℃-0℃之间,水凝胶会依然柔软,实施例2和实施例3,在-100℃都没有出现结晶峰,说明水凝胶敷料具有极端的抗冻性能。
⑤使用万能拉力机测量抗拉伸和耐压试验,其中,抗拉伸试验时将水凝胶呈哑铃状,窄宽为4mm,窄长为20mm,宽为12mm,总长度为70mm,速度设置为50mm·min-1;而用于压缩测试的水凝胶样品直径为10毫米,高度为20毫米。结果如图6所示:对比例1的抗压强度只有0.52MPa,抗拉伸强度只有0.006MPa,0.285MPa,实例2在80%的应变下,抗压强度显著增加到3.17MP,抗拉伸强度提高为之前的50倍,实例4的抗压强度显著增加到5.50±0.012MP,抗拉伸强度为0.379±0.020Mpa。
本发明所列举的各原料,以及本发明各原料的上下限、区间取值,以及工艺参数(如温度、时间等)的上下限、区间取值都能实现本发明,在此不一一列举实施例。
综上所述,本发明提供的明胶水凝胶能够有效避免交联剂的使用且具有足够的强度和粘性能够满足医用敷料的需求。
以上所述是本发明的优选实施方式,不能以此来限定本发明之权利范围,应当指出,对于本技术领域的普通技术人员来说,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (7)
1.一种多重氢键交联的水凝胶敷料,其特征在于,所述水凝胶敷料的原料包括明胶溶液和聚乙二醇,其中明胶与聚乙二醇的质量比为1:(1.2~2.2)。
2.根据权利要求1所述的水凝胶敷料,其特征在于,所述聚乙二醇的分子量为200,所述明胶溶液的溶剂为PBS缓冲液或水,所述溶剂与聚乙二醇的体积比为1:(0.7~2.0)。
3.根据权利要求2所述的水凝胶敷料,其特征在于,还包括蛋白核小球藻提取物。
4.如权利要求1或2所述水凝胶敷料的制备方法,其特征在于,将明胶溶于溶剂中制备明胶溶液,再加入聚乙二醇,搅拌混合后注入模具,待充分交联后得到水凝胶敷料。
5.如权利要求3所述水凝胶敷料的制备方法,其特征在于,包括以下步骤:
S1、将蛋白核小球藻分别置于提取剂A和提取剂B中进行提取,待提取反应结束后,离心取上清,分别得到提取液A和提取液B;其中提取剂A为明胶溶液的溶剂,提取剂B为聚乙二醇;
S2、将明胶溶于提取剂A,在加入提取液B,搅拌混合后注入模具,待充分交联后得到水凝胶敷料。
6.根据权利要求5所述的制备方法,其特征在于,步骤S1所述提取反应的温度为60~100℃,时间为2~6 h;所述蛋白核小球藻与提取剂A或提取剂B的质量体积比为(80~140)mg:1 mL。
7.如权利要求1~3任一项所述的水凝胶敷料在制备创面愈合药物中的应用。
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