CN113713167A - 一种新型光热敏感复合水凝胶敷料的制备与应用 - Google Patents

一种新型光热敏感复合水凝胶敷料的制备与应用 Download PDF

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CN113713167A
CN113713167A CN202111141497.5A CN202111141497A CN113713167A CN 113713167 A CN113713167 A CN 113713167A CN 202111141497 A CN202111141497 A CN 202111141497A CN 113713167 A CN113713167 A CN 113713167A
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composite hydrogel
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agarose
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谭志勇
孙婕
徐晨
邓宏玲
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Changchun University of Technology
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Abstract

本发明公开了一种新型光热敏感复合水凝胶敷料，我们以琼脂糖为水凝胶基质，包裹单宁酸铁纳米粒子，并加入抗生素药物，赋予其抗菌能力。该复合水凝胶能够在低强度近红外光照射下表现出优异的光热杀菌性能，而且能够通过低强度的近红外光控制抗生素释放，使其与热疗结合协同用于抗菌治疗。药物可控释放的能力能够避免有效药物在局部积累，使得光毒性副作用最小化。这种光热敏感复合水凝胶有望实现细菌感染伤口的快速愈合，并广泛应用于生物、医药及组织工程领域。

Description

一种新型光热敏感复合水凝胶敷料的制备与应用
技术领域
本发明属于高分子材料领域，具体涉及一种新型光热敏感复合水凝胶敷料制备与应用。
背景技术
在处理皮肤屏障等软组织受损时，为防止微生物和化学物质入侵，伤口敷料起到重要作用。然而传统的敷料功能单一，甚至在更换过程中有可能导致二次伤害并引发炎症。在实际应用中，理想的伤口敷料除了需要保持伤口湿润洁净以外，还应避免伤口部位遭受细菌侵害，同时在更换敷料时能够减弱粘附力以达到轻松揭除的效果。因此，多功能水凝胶作为伤口敷料用于软组织修复目前受到广泛关注。在这些伤口敷料中，高分子凝胶理化特性相比于其他人工合成材料更接近活体组织[1]，如光热水凝胶伤口敷料通常具有近红外(NIR)光吸收剂，可以通过精确控制光源的辐照强度、辐照时间及照射位点实现多方面的响应目的[2]。除此之外，采用物理化学交联方式设计水凝胶结构并赋予其相应功能，可以实现水凝胶结构功能一体化，不但可以有效的改善水凝胶的各项性能[3]，而且可以实现凝胶的功能性应用，从而广泛应用于生物、医药及组织工程领域。
然而，开发一种具有良好生物相容性温、光热敏性且有抗菌性能的复合水凝胶仍然是一个挑战。目前水凝胶敷料可以填充伤口，粘在伤口上并保护伤口，但很多水凝胶敷料在设计时只考虑生物相容性及力学性能问题，没有引入一种能促进伤口愈合且协同抗菌物质，而且此类敷料制备过程繁杂且成本过高、反应条件过高和促愈合效果不佳等问题，限制了其使用。
参考文献：
[1] Li W, Wang J, Ren J, et al. 3D graphene oxide-polymer hydrogel:near-infrared light-triggered active scaffold for reversible cell capture andon-demand release.[J]. Advanced Materials, 2013, 25(46):6737-6743.
[2]Kurapati, R, Raichur, et al. Near-infrared light-responsivegraphene oxide composite multilayer capsules: A novel route for remotecontrolled drug delivery[J]. Chemical communications, 2013, 49:734-736.
[3]刘晟, 夏梦阁, 张燕,等. 具有物理/化学双重交联结构可调的mZnO/PAAm纳米抗菌复合水凝胶的合成及性能[J]. 高分子学报, 2013(10):45-51.。
发明内容
为解决现有技术的缺点和不足之处，本发明的首要目的在于提供一种新型光热敏感复合水凝胶敷料的制备方法与应用。该复合水凝胶以琼脂糖（AG）作为高分子骨架包裹单宁酸铁（TA-Fe）纳米粒子和抗生素药物，低强度近红外光照射不仅能诱导单宁酸铁纳米粒子产生局部热疗作用还可以时空可控地促进抗生素的释放，除了良好的光热抗菌性能，该复合水凝胶还具有优异的力学性能。
本发明目的通过以下技术方案实现：
一种新型光热敏感复合水凝胶敷料的制备方法，包括以下步骤：
（1）将一定量琼脂糖和一定量单宁酸加入去离子水中，加热并搅拌至完全溶解。
（2）将上述溶液转移至油浴锅中继续搅拌，待其温度稳定后加入三氯化铁溶液和抗生素溶液，搅拌30min。
（3）再将碳酸氢钠溶液缓慢滴入上述溶液中，搅拌均匀。
（4）将所得溶液用注射器注入到成型模具中，存放于4℃冰箱中静置数小时。
优选地，步骤(1)所述的琼脂糖质量浓度为15-20g/L；单宁酸质量浓度为3-5g/L；在步骤(2) 所述的抗生素溶液质量浓度为1-2g/L。
优选地，步骤(1)所述的琼脂糖和单宁酸加入去离子水中的质量分别为0.5-0.7g、0.1-0.2g。
优选地，步骤(1)所述的琼脂糖和单宁酸加入去离子水中后加热至100-120℃。
优选地，步骤(2)所述的油浴锅温度为40-60℃。
优选地，步骤(2)所述的加入三氯化铁溶液应按此比例：TA：Fe的摩尔比为2-3：1。
优选地，步骤(2)所述抗生素为万古霉素、达托霉素、环丙沙星。
优选地，步骤(2)所述加入2mL抗生素溶液（1g/L）。
优选地，步骤(3)所述加入10mL碳酸氢钠溶液（0.05mol /L）。
优选地，步骤(4)所述溶液存放于4℃冰箱中静置2-4h。
上述方法制得了一种新型光热敏感复合水凝胶敷料。
上述新型光热敏感复合水凝胶敷料在生物、医药及组织工程领域应用。
与现有技术相比，本发明具有以下的有益技术效果：
本发明所提供的新型光热敏感复合水凝胶敷料，具有优异的光热及光热抗菌性能，良好的力学性能，同时，安全环保，且具有较好的稳定性，制备过程简便。
（1）本发明制备的新型光热敏感复合水凝胶敷料中琼脂糖分子上丰富的羟基提供了大量的氢键和静电吸引从而形成物理交联。单宁酸与Fe（III）螯合形成的单宁酸铁纳米粒子赋予了新型光热敏感复合水凝胶敷料光热转换性能。
（2）本发明中新型光热敏感复合水凝胶敷料拥有优良的光热抗菌性能，水凝胶原料中抗生素具有一定的抗菌效果，且效果显著，同时单宁酸铁作为一种NIR光吸收剂，能够将光能转化为热量，通过提高局部温度（>50℃）杀死微生物，当将光热伤口敷料置于近红外光照射下时，会导致细菌的物理损伤（热破坏），从而能够有效杀菌。
（3）该水凝胶具有稳定的流变学特性，与人体软组织接近的模量，可调控的成凝胶时间，良好的光热效应和时空可控的精确药物释放。
因此，这种对光热敏感的复合水凝胶作为伤口敷料有很大的发展前景。
附图说明
图1为实施例1制得的新型光热敏感复合水凝胶冻干样品在1000倍下的扫描电子显微镜图。图1中a观察到此复合水凝胶为多孔结构；图1中b表明在复合水凝胶中成功生成了单宁酸铁纳米粒子。
图2为实施例1制得的新型光热敏感复合水凝胶红外光谱图。
图3为实施例1制得的新型光热敏感复合水凝胶的应力-应变图。图中可以得出此复合水凝胶的拉伸强度比琼脂糖水凝胶更好。这说明制得的新型光热敏感复合水凝胶力学性能优良并能满足伤口敷料力学性能的要求。
图4为实施例1制得的新型光热敏感复合水凝胶和琼脂糖的流变学测量结果。图中，复合水凝胶的储存模量（G’）大于损耗模量（G”），这说明此复合水凝胶具有良好的弹性。
图5为实施例1制得的新型光热敏感复合水凝胶在808 nm近红外激光照射下(0.5W·cm-2, 10 min）的红外摄像照片和温度变化曲线。图中，在0~5min，复合水凝胶的温度由25.0℃上升至45.5℃，随后温度基本不变。因此，说明该复合水凝胶具有优异的光热性能。
图6为实施例1制得的新型光热敏感复合水凝胶近红外光照射组及无近红外光照射组的万古霉素释放曲线。图中，在近红外光激光照射下，复合水凝胶中抗生素释放量增加，而停止光照后，抗生素释放量降低。这表明近红外光能够远程的控制抗生素的释放。
图7为不同处理5天后的细菌活力统计图。图中，低强度近红外光照射组与对照组相比，细菌存活率在80%以上。而经复合水凝胶处理后的细菌存活率仅为30%。近红外光照射下的复合水凝胶能杀死约99%的细菌。由此可知，在低强度近红外照射下的复合水凝胶具有较强的协同杀菌能力。
具体实施方式
为了更好的理解本发明，下面结合实施例和附图对本发明作进一步详细的描述，但本发明的实施方式不限于此。
其中，以下实施例所用原料均为市售或自制。
实施例1
新型光热敏感复合水凝胶的制备
（1）将0.5g琼脂糖（20g/L）和0.1g 单宁酸（5g/L）加入去离子水中，加热至100℃并搅拌至完全溶解。
（2）将上述溶液转移至40℃的油浴锅中继续搅拌，待其温度稳定后加入三氯化铁溶液（TA：Fe的摩尔比为3：1）和2mL万古霉素溶液（1g/L），搅拌30 min。
（3）将10 mL碳酸氢钠溶液（0.05 mol/L）缓慢滴入上述溶液中，搅拌均匀。
（4）将此溶液用注射器注入到成型模具中，存放于4℃冰箱中静置2 h，即可得到琼脂糖/单宁酸铁@万古霉素水凝胶。
实施例2
（1）将0.6g琼脂糖（20g/L）和0.15g 单宁酸（5g/L）加入去离子水中，加热至110℃并搅拌至完全溶解。
（2）将上述溶液转移至50℃的油浴锅中继续搅拌，待其温度稳定后加入三氯化铁溶液（TA：Fe的摩尔比为2：1）和2 mL达托霉素溶液（1g/L），搅拌30 min。
（3）将10mL碳酸氢钠溶液（0.05 mol/L）缓慢滴入上述溶液中，搅拌均匀。
（4）将此溶液用注射器注入到成型模具中，存放于4℃冰箱中静置3 h，即可得到琼脂糖/单宁酸铁@达托霉素水凝胶。
实施例3
（1）将0.7g琼脂糖（20g/L）和0.2g 单宁酸（5g/L）加入去离子水中，加热至120℃并搅拌至完全溶解。
（2）将上述溶液转移至60℃的油浴锅中继续搅拌，待其温度稳定后加入三氯化铁溶液（TA：Fe的摩尔比为3：1）和2mL环丙沙星溶液（1g/L），搅拌30 min。
（3）将10mL碳酸氢钠溶液（0.05 mol/L）缓慢滴入上述溶液中，搅拌均匀。
（4）将此溶液用注射器注入到成型模具中，存放于4℃冰箱中静置4h，即可得到琼脂糖/单宁酸铁@环丙沙星水凝胶。
说明：以上实施例仅用以说明本发明而并非限制本发明所描述的技术方案；因此，尽管本说明书参照上述的实施例对本发明已进行了详细的说明，但是熟悉本领域的技术人员在不脱离本发明的精神和范围的技术方案及其改进，均应涵盖在本发明的权利要求范围内。

Claims (10)

1.新型光热敏感复合水凝胶敷料，其特征在于，以天然琼脂糖（AG）为高分子骨架的光热响应型复合水凝胶，该复合水凝胶载有优异光热性能的单宁酸铁（TA-Fe）纳米粒子和抗生素药物。
2.根据权利要求1所述新型光热敏感复合水凝胶敷料，其特征在于，其步骤为：将一定量琼脂糖和一定量单宁酸加入去离子水中，加热至一定温度后，高速搅拌至完全溶解，将此溶液转移至一定温度的油浴锅中继续搅拌，待其温度稳定后加入一定量三氯化铁溶液和2mL抗生素溶液（1g/L）并再搅拌30min，然后将10mL碳酸氢钠溶液（0.05mol /L）缓慢滴入溶液中，最后，将此溶液用注射器注入成型模具中，存放于4℃冰箱中静置数小时。
3.根据权利要求2所述新型光热敏感复合水凝胶敷料的制备方法，其特征在于，所述加入琼脂糖和单宁酸的质量分别为0.5-0.7g、0.1-0.2g。
4.根据权利要求2所述新型光热敏感复合水凝胶敷料的制备方法，其特征在于，所述琼脂糖质量浓度为15-20g/L；单宁酸质量浓度为3-5g/L。
5.根据权利要求2所述新型光热敏感复合水凝胶敷料的制备方法，其特征在于，琼脂糖和单宁酸加入去离子水中后加热至100-120℃。
6.根据权利要求2所述新型光热敏感复合水凝胶敷料的制备方法，其特征在于，油浴锅温度为40-60℃。
7.根据权利要求2所述新型光热敏感复合水凝胶敷料的制备方法，其特征在于，加入三氯化铁溶液应按此比例：TA：Fe的摩尔比为2-3：1。
8.根据权利要求2所述新型光热敏感复合水凝胶敷料的制备方法，其特征在于，所述抗生素为万古霉素、达托霉素、环丙沙星。
9.根据权利要求2所述新型光热敏感复合水凝胶敷料的制备方法，其特征在于，所述溶液存放于4℃冰箱中静置2-4h。
10.权利要求2-9任一项所述的制备方法制得的一种新型光热敏感复合水凝胶敷料。
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CN114522271A (zh) * 2022-01-14 2022-05-24 江苏大学 一种可控杀菌的复合水凝胶及其制备方法和应用
CN114767935A (zh) * 2022-03-09 2022-07-22 上海市第十人民医院 一种镁基复合凝胶材料、制备方法及应用
CN115429927A (zh) * 2022-09-14 2022-12-06 广东省东莞市质量监督检测中心 海藻酸钠复合苹果多酚的光热抗菌敷料及制备方法与应用
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114522271A (zh) * 2022-01-14 2022-05-24 江苏大学 一种可控杀菌的复合水凝胶及其制备方法和应用
CN114767935A (zh) * 2022-03-09 2022-07-22 上海市第十人民医院 一种镁基复合凝胶材料、制备方法及应用
CN115429927A (zh) * 2022-09-14 2022-12-06 广东省东莞市质量监督检测中心 海藻酸钠复合苹果多酚的光热抗菌敷料及制备方法与应用
CN116694089A (zh) * 2022-09-19 2023-09-05 广州贝奥吉因生物科技股份有限公司 一种用于抑制瘢痕的水凝胶及其制备方法和应用
CN116694089B (zh) * 2022-09-19 2024-03-26 广州贝奥吉因生物科技股份有限公司 一种用于抑制瘢痕的水凝胶及其制备方法和应用

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