CN109589448B - 一种氧气监测凝胶纤维伤口敷料及其制备方法 - Google Patents
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Abstract
本发明涉及氧气监测的凝胶纤维伤口敷料及其制备方法。依据本发明所制备的氧敏感凝胶纤维伤口敷料，其所需的特性物质组分及质量分数如下：有机硅烷95份，硅烷碳点5份，乏氧探针0.01−0.1份，PH为2.5的醋酸水溶液45份。本发明所提供的氧气监测凝胶纤维伤口敷料原料广泛、无毒，成本低廉。制备工艺简单，操作方便。硅烷碳点通过溶胶凝胶过程以化学键接的方式接枝到有机硅烷凝胶纤维中，实现分子级别的均匀分散，避免出现团聚、相分离等缺陷。凝胶纳米纤维伤口敷料即具有纳米纤维本身的高孔隙率和比表面积，以及较好的透气性能和机械性能，同时具有凝胶材料本身的微孔结构，具有优异的氧渗透性能，可实现实时原位地对伤口的氧气浓度进行监测，并且检测方法简单快速，灵敏度高。
Description
技术领域
本发明涉及利用溶液静电纺丝与溶胶凝胶纺丝相结合的方法，将硅烷碳点与乏氧探针负载在凝胶纤维中，制备有氧气监测功能的凝胶纤维形成的伤口敷料，使其具有高效快速检测氧气浓度的性能，属于医用耗材领域。
背景技术
氧气在伤口愈合过程中扮演着十分重要的作用，如细胞增殖、抗菌、新血管生成、胶原生成等过程都需要氧气的参与。在伤口愈合初期，由于血管破裂和血管收缩引起的供氧不足，以及由代谢活性细胞引起的耗氧量增加，使伤口处于乏氧环境中。氧气浓度的变化自然成为监测伤口愈合程度的一个重要参考指标。在伤口愈合过程中，如果能实时原位地对伤口的氧气浓度进行监测，将对医生进行诊断并及时提出合理准确的治疗方案提供非常大的帮助。
当前关于伤口成像的研究可以分为侵入式和非侵入式。非侵入式氧监测的方法由于伤害少、对病人友好的特点被研究者广泛采用。当前伤口成像的方法主要是将乏氧探针以液态的形式涂敷在伤口上，通过乏氧探针在不同氧气浓度下荧光强度不同的特点，对伤口进行荧光伤口成像，测得伤口处的氧气浓度。尽管液态形式的乏氧探针能较准确地监测出伤口的氧气浓度大小及分布情况，但每次检测前都需要重新涂覆上溶液，操作繁琐，并且无法实现实时原位检测的目的。同时，涂敷在伤口上的溶液会阻碍伤口与空气的正常接触，从而影响伤口的愈合。目前，许多研究者开始探索将乏氧探针引入到固体载体，来改变其液态的单一存在形式。其中，静电纺丝技术由于其制得的纤维膜具有孔隙率高、比表面积大、纤维直径小等特点，很早就被人们应用于伤口敷料领域。聚合物纤维膜由于具有多孔的纤维结构以及较小的纤维直径这两方面的因素，使得氧气在纤维膜中扩散并渗透进纤维内部的阻力很小。然而，不同的聚合物其氧透气性是不同的，并且大多数的聚合物透氧性较差，如聚乙烯吡络烷酮（PVP）、聚乳酸（PLA）等，因此能够用于生物体上作为氧传感器基体的聚合物非常少，目前许多研究主要基于聚己内酯（PCL）等材料。
溶胶凝胶法是制备有机无机杂化材料的主要方法，同时溶胶凝胶法制备的凝胶玻璃是一种天然的微孔材料，其光学性能和透氧性十分优异。因此，利用溶液静电纺丝技术与溶胶凝胶相结合的方法，制备出的凝胶纳米纤维伤口敷料，即具有纳米纤维本身的透气性能和一定的机械性能，同时也具有凝胶材料本身稳定的光学性能以及优异的氧渗透性能。由此将无氧响应性的硅烷碳点与具有氧敏感性能的乏氧探针负载在这种凝胶纤维伤口敷料中，通过紫外灯照射荧光成像的方法，计算碳点与乏氧探针的荧光强度比值，即可以实现实时原位地对伤口的氧气浓度进行监测，并且检测快速，灵敏度高。
发明内容
本发明的目的是克服当前伤口氧气检测困难，无法实现实时原位监测的问题，利用溶液静电纺丝技术与溶胶凝胶相结合的方法，将硅烷碳点与乏氧探针负载在凝胶纤维中，制备出可实时原位对伤口氧气浓度进行快速监测的凝胶纤维伤口敷料。
本发明所提供的氧气监测凝胶纤维伤口敷料所需的特性物质组分及质量份数如下：
有机硅烷95份，硅烷碳点5份，乏氧探针0.01-0.1份，PH为1.5 − 2.5的醋酸水溶液45份。
本发明氧气监测凝胶纤维伤口敷料所提供的有机硅烷包括正硅酸乙酯、甲基三乙氧基硅烷等可以进行水解缩聚并溶液静电纺丝的各种有机硅烷。
本发明氧气监测凝胶纤维伤口敷料所提供的硅烷碳点是经有机硅烷（AEAPMS）表面修饰的碳点，粒径在10 nm左右，可以通过溶胶凝胶法以化学键接的方式接枝到有机硅烷凝胶基体中，并实现分子级别的均匀分散，避免出现团聚、相分离等缺陷。
发明氧气监测凝胶纤维伤口敷料所提供的乏氧探针为氧敏感的水或醇溶性的荧光探针，如金属配合物等氧敏感荧光材料。
本发明氧气监测凝胶纤维伤口敷料所提供的醋酸为未经提纯的冰醋酸。
本发明氧气监测凝胶纤维伤口敷料所提供的乙醇浓度为98%，未经进一步提纯。
本发明氧气监测凝胶纤维伤口敷料所提供的水为蒸馏水。
本实验所提供的氧气监测凝胶纤维伤口敷料制备方法如下：
第一步，将冰醋酸加入到蒸馏水中搅拌均匀，配制成PH为1.5 − 2.5的醋酸水溶液；将有机硅烷与无水乙醇混合均匀后，向其溶液中逐滴加入醋酸水溶液，制得有机硅烷溶胶溶液，并在密封条件下搅拌12小时；之后，将溶胶溶液在30oC的水浴锅中旋蒸至原2/3质量；向旋蒸后的溶胶溶液中加入无水乙醇与硅烷碳点和乏氧探针的混合液，制得复合凝胶溶液，并在室温下敞口搅拌，避光。
第二步，待凝胶溶液的粘度增大至一定值后，利用溶液静电纺丝技术纺丝，制得溶胶纳米纤维膜；溶液静电纺丝的参数设置，纺丝距离15 − 20 cm，件数金属针头电压-2.5 −-5 kV，接收板电压18 − 20 kV，供料速度0.5 − 2ml/h。
通过紫外灯照射荧光成像的方法，计算碳点与乏氧探针荧光强度的比值，继而得到氧气浓度，可实现实时原位地对伤口的氧气浓度进行监测。
本发明具有以下有益效果：
本发明所提供的氧气监测凝胶纤维伤口敷料原料广泛、无毒，成本低廉。制备工艺简单，操作方便。硅烷碳点通过溶胶凝胶法以化学键接的方式接枝到有机硅烷凝胶纤维中，实现分子级别的均匀分散，避免出现团聚、相分离等缺陷。凝胶纳米纤维伤口敷料即具有纳米纤维本身的高孔隙率和比表面积，以及较好的透气性能和一定的机械性能，同时又具有凝胶材料本身的微孔结构，具有优异的氧渗透性能，并且检测方法简单快速，灵敏度高。
具体实施方式
下列实施方式中所指的份数均指质量分数。浓度均为质量百分比浓度。
实施例1：
冰醋酸加入到蒸馏水中搅拌均匀，配制成PH为1.5的醋酸水溶液；将甲基三乙氧基硅烷95份与无水乙醇190份混合均匀后，向其溶液中逐滴加入醋酸水溶液45份，制得有机硅烷溶胶溶液，并在密封搅拌12小时；之后，将溶胶溶液在30oC的恒温水浴锅中旋蒸至原2/3质量；将无水乙醇95份、硅烷碳点5份、氧敏感荧光探针0.01份充分混合，并加入到旋蒸后的溶胶溶液中，制得凝胶溶液，并在室温下敞口搅拌，避光。
待凝胶溶液的粘度增大并达到一定值后，经溶液静电纺丝装置纺丝（纺丝距离15cm，金属针头电压-2.5 kV，接收板电压18 kV，供料速度0.5ml/h）。
实施例2：
冰醋酸加入到蒸馏水中搅拌均匀，配制成PH为2.0的醋酸水溶液；将甲基三乙氧基硅烷95份与无水乙醇190份混合均匀后，向其溶液中逐滴加入醋酸水溶液45份，制得有机硅烷溶胶溶液，并在密封搅拌12小时；之后，将溶胶溶液在30oC的恒温水浴锅中旋蒸至原2/3质量；将无水乙醇95份、硅烷碳点5份、氧敏感荧光探针0.1份充分混合，并加入到旋蒸后的溶胶溶液中，制得凝胶溶液，并在室温下敞口搅拌，避光。
待凝胶溶液的粘度增大并达到一定值后，经溶液静电纺丝装置纺丝（纺丝距离15cm，金属针头电压-2.5 kV，接收板电压18 kV，供料速度0.5ml/h）。
实施例3：
冰醋酸加入到蒸馏水中搅拌均匀，配制成PH为2.5的醋酸水溶液；将正硅酸乙酯95份与无水乙醇190份混合均匀后，向其溶液中逐滴加入醋酸水溶液45份，制得有机硅烷溶胶溶液，并在密封搅拌12小时；之后，将溶胶溶液在30oC的恒温水浴锅中旋蒸至原2/3质量；将无水乙醇95份、硅烷碳点5份、氧敏感荧光探针0.01份充分混合，并加入到旋蒸后的溶胶溶液中，制得凝胶溶液，并在室温下敞口搅拌，避光。
待凝胶溶液的粘度增大并达到一定值后，经溶液静电纺丝装置纺丝（纺丝距离20cm，金属针头电压-5 kV，接收板电压20 kV，供料速度0.5 ml/h）。
实施例4：
冰醋酸加入到蒸馏水中搅拌均匀，配制成PH为2.0的醋酸水溶液；将正硅酸乙酯/35份、甲基三乙氧基硅烷65份与无水乙醇190份混合均匀后，向其溶液中逐滴加入醋酸水溶液45份，制得有机硅烷溶胶溶液，并在密封搅拌12小时；之后，将溶胶溶液在30oC的恒温水浴锅中旋蒸至原2/3质量；将无水乙醇95份、硅烷碳点5份、氧敏感荧光探针0.01份充分混合，并加入到旋蒸后的溶胶溶液中，制得凝胶溶液，并在室温下敞口搅拌，避光。
待凝胶溶液的粘度增大并达到一定值后，经溶液静电纺丝装置纺丝（纺丝距离20cm，金属针头电压-5 kV，接收板电压20 kV，供料速度0.5 ml/h）。
Claims (4)
1.一种氧气监测凝胶纤维伤口敷料及其制备方法，其特征在于，物质组分及质量分数为：
可以水解缩聚并进行溶液静电纺丝的有机硅烷95份，硅烷碳点5份，具有氧敏感的水或醇溶性的荧光探针0.01 − 0.1份；
其制作方法为
第一步，将冰醋酸加入到蒸馏水中搅拌均匀，配制成pH为2.5的醋酸水溶液；将有机硅烷与无水乙醇混合均匀后，向其溶液中逐滴加入醋酸水溶液，制得有机硅烷溶胶溶液，并在密封条件下搅拌12小时；之后，将溶胶溶液在30oC的水浴锅中旋蒸至原2/3质量；向旋蒸后的溶胶溶液中加入无水乙醇与硅烷碳点和乏氧探针的混合液，制得复合凝胶溶液，并在室温下敞口搅拌，避光；
第二步，待凝胶溶液的粘度增大并达到一定值后，利用溶液静电纺丝技术纺丝，制得溶胶微米-纳米纤维膜，溶液静电纺丝的参数设置，纺丝距离15 − 20 cm，件数金属针头电压-2.5 − -5 kV，接收板电压18 − 20 kV，供料速度0.5 − 2ml/h。
2.根据权利要求1所述的一种氧气监测凝胶纤维伤口敷料及其制备方法，其特征在于，有机硅烷为正硅酸乙酯、甲基三乙氧基硅烷或其混合物。
3.根据权利要求1所述的一种氧气监测凝胶纤维伤口敷料及其制备方法，其特征在于，硅烷碳点是经有机硅烷（AEAPMS）表面修饰的碳点，激发光波长为430 nm。
4.根据权利要求1所述的一种氧气监测凝胶纤维伤口敷料及其制备方法，其特征在于，乏氧探针为具有氧敏感的水或醇溶性的荧光金属配合物，激发波长为600 nm。
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