CN108498851A - 一种水凝胶材料及其制备方法 - Google Patents

一种水凝胶材料及其制备方法 Download PDF

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CN108498851A
CN108498851A CN201810353552.9A CN201810353552A CN108498851A CN 108498851 A CN108498851 A CN 108498851A CN 201810353552 A CN201810353552 A CN 201810353552A CN 108498851 A CN108498851 A CN 108498851A
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chitosan
hydrogel
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汪斌
贺沁婷
舒莉
唐新璐
叶招莲
刘维桥
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Jiangsu University of Technology
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Abstract

本发明提供一种水凝胶材料，本发明所述水凝胶材料由以下重量份的原料组成：改性壳聚糖1‑5份、聚乙烯醇4‑20份、水60‑80份，改性壳聚糖是由氯乙酸、乙二酸酐或丁二酸酐改性壳聚糖所得中的一种，改性壳聚糖的取代度20％‑85％。本发明还提供一种水凝胶敷料，由水凝胶材料加上功能性成分组成，该水凝胶敷料的制备方法为将水凝胶材料浸入功能性成分溶液中，以该水凝胶材料作为功能性成分的载体，功能性成分在水凝胶材料中均匀吸附在水凝胶三维网络中，制得水凝胶敷料。

Description

一种水凝胶材料及其制备方法
技术领域
本发明涉及一种医用水凝胶材料,具体涉及一种水凝胶敷料及其制备方法。
背景技术
传统的医用敷料主要采用棉纱布等进行护理，能保持创面干燥透气、控制感染，但棉制品的空隙不足以阻止大多数微生物进入伤口愈合环境，容易与伤口阻止发生粘连而造成痛苦，造成二次创伤。
壳聚糖广泛存在于天然界中，具有良好的生物相容性、生物降解性及成膜性，还具有止血止痛，抗菌消炎，缓释药物等生物活性，是制备医用敷料的理想材料。为了进一步提高壳聚糖缓释性能，将壳聚糖改性制备成海绵状。中国发明专利申请(申请号201510785249.2)提供了一种羧乙基壳聚糖海绵敷料的制备方法，步骤包括将羧乙基壳聚糖采用等离子体处理进行活化得到活化羧乙基壳聚糖海绵；将活化羧乙基壳聚糖海绵在温度50-200℃，湿度20-70％条件下处理得到羧乙基壳聚糖海绵敷料。该发明羧乙基壳聚糖海绵敷料亲水性较强，容易与新生表皮细胞粘黏，造成敷料更换困难。中国发明专利申请(201510528208.5)将羧甲基壳聚糖与阴离子聚电解质或两性聚电解质混合，利用库仑力相互作用形成复合物凝胶，复合物凝胶经冷冻干燥得到海绵状创伤敷料。该发明中和了羧甲基壳聚糖表面电荷，降低了其与细菌表面电荷作用，降低了其抗菌性。
发明内容
本发明提供一种水凝胶材料，所述水凝胶材料由以下原料组成：改性壳聚糖、聚乙烯醇和水。
优选的本发明所述水凝胶材料由以下重量份的原料组成：改性壳聚糖1-5份、聚乙烯醇4-20份、水60-80份。所述改性壳聚糖是由氯乙酸、乙二酸酐或丁二酸酐改性壳聚糖所得中的一种。所述改性壳聚糖的取代度20％-85％。
本发明所述的水凝胶材料的制备方法为将改性壳聚糖、聚乙烯醇和水先混合均匀，再冷冻干燥后得到的水凝胶材料具有微米多孔结构。
本发明还提供一种水凝胶敷料，所述水凝胶敷料是由上述方法制备的水凝胶材料加上功能性成分组成。该水凝胶敷料的制备方法为将水凝胶材料浸入功能性成分溶液中，以该水凝胶材料作为功能性成分的载体，功能性成分在水凝胶材料中均匀吸附在水凝胶三维网络中，制得水凝胶敷料。
优选的本发明所述的功能性成分为药物或生长因子。
本发明还提供了一种水凝胶敷料在制备治疗伤口愈合的药物中的应用。
本发明利用氯乙酸、乙二酸酐或丁二酸酐改性壳聚糖，利用其表面电荷，提高壳聚糖抗菌性；利用聚乙烯醇成膜性，降低改性壳聚糖与新生细胞的粘黏；将敷料制备成海绵状，负载药物或者成长因子，拓展敷料的功能。
为了解决现有技术问题，本发明提供了一种具有对创面无粘连、吸水性能良好、生物相容性能佳，同时具有可以负载药物或生长因子的空间微结构，可负载各类功能性成分，如药物或生长因子，实现敷料的功能化治疗，实现创面治疗中抗菌、促进伤口愈合等功能的医用防粘水凝胶敷料及其制备方法。
附图说明
图1：为本发明实施例1所制备的水凝胶敷料显微结构；
图2：为本发明实施例2所制备的水凝胶敷料显微结构。
图3：为本发明实施例3所制备的水凝胶敷料显微结构。
具体实施方式
实施例1
将10g聚乙烯醇粉末溶于100mL蒸馏水中，90℃条件下加热溶解2h，制得10％的聚乙烯醇水溶液。将制得的丁二酰化壳聚糖溶于冷水中得5％的丁二酰化壳聚糖溶液。将100mL聚乙烯醇水溶液与50mL5％的丁二酰化壳聚糖溶液混合，60℃条件下磁力搅拌反应完全。将混合液预冷冻后冷冻干燥24h取出得到水凝胶产品。
制备得到的水凝胶经实验测试不粘连伤口，平均溶胀率为542％，保持伤口湿润性，并且具有较好的弹性，具有丰富的微米多孔结构，如图1所示。
实施例2
将10g聚乙烯醇粉末溶于100mL蒸馏水中，90℃条件下加热溶解2h，制得10％的聚乙烯醇水溶液。将制得的丁二酰化壳聚糖溶于冷水中得5％的丁二酰化壳聚糖溶液。将100mL聚乙烯醇水溶液与100mL5％的丁二酰化壳聚糖溶液混合，60℃条件下磁力搅拌反应完全。将混合液预冷冻后冷冻干燥24h取出得到水凝胶产品。
制备得到的水凝胶经实验测试不粘连伤口，平均溶胀率为876％，保持伤口湿润性，并且具有较好的弹性，具有丰富的微米多孔结构，如图2所示。
实施例3
将10g聚乙烯醇粉末溶于100mL蒸馏水中，90℃条件下加热溶解2h，制得10％的聚乙烯醇水溶液。将制得的羧甲基壳聚糖溶于冷水中得5％的羧甲基壳聚糖。将100mL聚乙烯醇水溶液与75mL5％的羧甲基壳聚糖溶液混合，60℃条件下磁力搅拌反应完全。将混合液预冷冻后冷冻干燥24h取出得到水凝胶产品。
制备得到的水凝胶经实验测试不粘连伤口，平均溶胀率为712％，保持伤口湿润性，并且具有较好的弹性，具有丰富的微米多孔结构，如图3所示。
试验例：实验测试，C1～C3分别代表实施例1、2、3配方制得的水凝胶，并作为测试样品：
(1)水凝胶的平衡溶胀率
将制备水凝胶于-40℃冷冻干燥至恒重。在25温度下浸没与纯水中24h取出，轻轻用滤纸吸干表面水分，称量水凝胶溶胀后的重量，根据水凝胶溶胀前后计算水凝胶的平衡溶胀率。
表1水凝胶样品溶胀率
水凝胶样品 平衡溶胀率
C1 542％
C2 876％
C3 712％
由表1可看出水凝胶的平衡溶胀率，最大能达到876％。
(2)水凝胶细胞毒性检测
参照IS0 10993.5-2009的标准，对水凝胶进行细胞毒性研究。按材料重量与浸提介质体积为0.2g/ml的比例加入含10％血清的α-MEM(Hyclone)培养基，于37℃中浸提24小时。将此浸提原液与含10％血清的α-MEM培养基(V/V＝1：0，1：1，1：3)混合，得到100％、50％、25％浓度的浸提液。取100μl密度为50000个/ml的MC3T3-E1细胞悬浮液于96孔板培养24小时后，弃去培养液，用不同浓度的浸提稀释液继续培养1天。以含10％血清的α-MEM培养液培养的细胞作为空白对照(control组)。采用MTT法在490nm波长处，测得其吸光值(OD)。
表2：实施例1-3凝胶材料不同浸提液浓度的吸光值
所制备水凝胶的不同浓度浸提液与空白样比较，OD值相差不大，说明所制备水凝胶无明显毒性，生物相容性良好。
(3)水凝胶缓释性能检测
将0.5g实施例1-3所得水凝胶放入20ml硫酸庆大霉素溶液中(1500U/ml)浸泡24h，将水凝胶取出并用蒸馏水清洗其表面，冷冻干燥后得到载药水凝胶。将载药水凝胶放入200ml缓冲溶液中(pH＝7.2)，温度控制在37℃，每隔一段时间取出3ml溶液，并补充3ml缓冲溶液。用紫外分光光度计在232nm处测量取样的吸光度，计算硫酸庆大霉素累积释放率。表3为实施案例2凝胶材料硫酸庆大霉素累积释放率。
表3实施例1-3凝胶材料硫酸庆大霉素累积释放率
时间/h 3 5 10 20 40 60 80 100
C1的累积释放率/％ 4.2 6.7 10.5 15.7 22.5 46.6 51.4 53.1
C2的累积释放率/％ 5.4 7.2 11.7 18.5 27.6 52.7 54.6 57.9
C3的累积释放率/％ 4.8 6.8 11.2 17.6 25.4 50.7 52.8 54.9
由表3可看出水凝胶的硫酸庆大霉素累积释放率在60h后基本达到稳定，实施例1、实施例2、实施例3的60h累积释放率分别达到46.6％、52.7％、50.7％。
以上所述，仅为本发明的较佳实施例，并不用以限制本发明，凡是依据本发明的技术实质对以上实施例所作的任何细微修改、等同替换和改进，均应包含在本发明技术方案的保护范围内。

Claims (9)

1.一种水凝胶材料，其特征在于，所述水凝胶材料由以下原料组成：改性壳聚糖、聚乙烯醇和水。
2.根据权利要求1所述的水凝胶材料，其特征在于，所述水凝胶材料由以下重量份的原料组成：改性壳聚糖1-5份、聚乙烯醇4-20份、水60-80份。
3.根据权利要求1所述的水凝胶材料，其特征在于，所述改性壳聚糖是由氯乙酸、乙二酸酐或丁二酸酐改性壳聚糖所得中的一种。
4.根据权利要求3所述的水凝胶材料，其特征在于，所述改性壳聚糖的取代度20％-85％
5.根据权利要求1-4任一项所述的水凝胶材料的制备方法，其特征在于，该制备方法为将改性壳聚糖、聚乙烯醇和水先混合均匀，再冷冻干燥后得到的水凝胶材料具有微米多孔结构。
6.一种水凝胶敷料，其特征在于，所述水凝胶敷料是由权利要求5制备的水凝胶材料加上功能性成分组成。
7.根据权利要求6所述的水凝胶敷料的制备方法，其特征在于，该方法为将水凝胶材料浸入功能性成分溶液中，以该水凝胶材料作为功能性成分的载体，功能性成分在水凝胶材料中均匀吸附在水凝胶三维网络中，制得水凝胶敷料。
8.根据权利要求7所述的水凝胶敷料的制备方法，其特征在于，所述功能性成分为药物或生长因子。
9.根据权利要求8所制备的水凝胶敷料在制备治疗伤口愈合的药物中的应用。
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