CN115094573B - 一种抗菌纳米敷料及其制备方法 - Google Patents
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Abstract
本发明属于生物医用材料领域，公开了一种抗菌纳米敷料及其制备方法，包括将溴代COF有机单体转化为格氏试剂，进而在TPU纳米纤维膜表面与多元醛基COF单体反应，得到COFs‑TPU纳米纤维膜，用硝酸银溶液处理后，水洗冻干制得抗菌纳米敷料。本发明制备的敷料具有强效抗菌效果。经回收后，硝酸银利用率大幅提高。
Description
技术领域
本发明属于生物医用材料领域，具体涉及一种抗菌纳米敷料及其制备方法。
背景技术
超级细菌是用尽所有抗生素都无法杀死的细菌，这一类细菌几乎能对各类抗菌药物都表现出耐药性，甚至对碳青霉烯类抗生素、万古霉素等强力抗生素也可能呈现出耐药性，有的还表现为多重抗药性。由于患者感染后往往无法从自身体内产生对抗细菌的抗体，致使死亡率大幅提高。
含银敷料是广谱抗菌作用的伤口敷料，其主要成分是银离子或银纳米粒子，通过干扰微生物呼吸链，损伤微生物的细胞膜，抑制基因的复制，转录，翻译，从而对各种微生物产生杀伤力，近年来被广泛应用于各类感染伤口。通过特殊工艺将银与新型敷料相结合制成的含银敷料能够持续而有效的控制伤口微环境中的微生物负荷，从而促进伤口的愈合。但是这些含银敷料不可避免会渗漏和释放，在伤口水洗过程中，敷料的抗菌性会下降。
发明内容
有鉴于此，本发明的目的在于提供一种抗菌纳米敷料及其制备方法，该敷料具有良好的抗菌效果。
为了解决上述技术问题，本发明提供了一种抗菌纳米敷料及其制备方法，包括如下步骤：
S1.将溴代COF有机单体溶于有机溶剂，加入镁粉，制得COF格氏试剂；
S2.以TPU的DMF溶液为纺丝液，通过溶液电纺制得TPU纳米纤维膜，将所述TPU纳米纤维膜预处理后，用所述COF格氏试剂浸轧，再经4',4”',4””'-氮三[([1,1'-联苯]-3,5-二甲醛)]溶液浸轧，水洗烘干；
S3.将步骤S2处理得到的TPU纳米纤维膜在硝酸银溶液中浸轧，水洗，得到抗菌纳米敷料。
优选的，上述制备方法中，所述4',4”',4””'-氮三[([1,1'-联苯]-3,5-二甲醛)]溶液的浓度为6.42g/L；所述TPU的DMF溶液的浓度为200g/L；所述硝酸银溶液的浓度为0.17g/L。
优选的，上述制备方法中，步骤S1中，所述溴代COF有机单体为5,10,15,20-四(4-溴苯基)卟啉、三(4-溴苯基)胺和2,4,6-三(4-(溴甲基)苯基)-1,3,5-三嗪中的一种。
优选的，上述制备方法中，步骤S1中，所述有机溶剂为乙醚或四氢呋喃。
优选的，上述制备方法中，步骤S1中，所述溴代COF有机单体、有机溶剂、镁粉的比例为1.0g：(100-220)ml：(0.5-2)g。
优选的，上述制备方法中，步骤S2中，所述溶液电纺条件为电压15-20kv、距离15-20cm，注射速率1-2ml/h。
优选的，上述制备方法中，步骤S2中，所述预处理具体指TPU纳米纤维膜用乙醚除去表面的灰尘和杂质，水洗后晾干。
优选的，上述制备方法中，所述浸轧采用二浸二轧，每次浸渍浴比为1:30-1:50，时间为10-20min。
优选的，上述制备方法中，步骤S3中，所述水洗还包括：回收水洗液，将所述水洗液经减压蒸馏浓缩后，得到可用于对TPU纳米纤维膜浸轧的硝酸银溶液。
本发明还提供了一种上述制备方法制备得到抗菌纳米敷料。
与现有技术相比，本发明具有以下有益效果：
本发明在TPU纳米纤维表面构建了COF膜，通过膜分子中的氮原子的孤对电子络合银离子，实现了TPU的表面功能化修饰。Ag-COF膜具有多孔晶体结构，耐磨，耐水洗，化学稳定性好。银的结合力强，不易释放。
具体实施方式
为了进一步理解本发明，下面结合实施例对本发明优选实施方案进行描述，但是应当理解，这些描述只是为了进一步说明本发明的特征和优点，而不是对本发明权利要求的限制。
实施例1
一种抗菌纳米敷料及其制备方法，包括如下步骤：
1.将1.0g三(4-溴苯基)胺溶于180ml乙醚，加入1.2g镁粉，制得COF格氏试剂；
2.利用200g/L TPU的DMF溶液，采用溶液电纺，条件为电压18kV、距离16cm，注射速率1.2ml/h制得TPU纳米纤维膜，经乙醚清洁，水洗晾干后，取1g TPU纳米纤维膜用40ml步骤1制得的COF格氏试剂二浸二轧，每次浸渍时间为18min，再经45ml 6.42g/L 4',4”',4””'-氮三[([1,1'-联苯]-3,5-二甲醛)]溶液二浸二轧，每次浸渍时间为11min，水洗烘干；
3.将1g步骤2处理的TPU纳米纤维膜在42ml 0.17g/L硝酸银溶液中二浸二轧，每次浸渍时间为15min，水洗，回收水洗液，得到抗菌纳米敷料A；
4.将步骤3回收的水洗液，经减压蒸馏浓缩后，可用作步骤3的硝酸银溶液用于浸轧。
实施例2
一种抗菌纳米敷料及其制备方法，包括如下步骤：
1.将1.0g 5,10,15,20-四(4-溴苯基)卟啉溶于100ml四氢呋喃，加入0.5g镁粉，制得COF格氏试剂；
2.利用200g/L TPU的DMF溶液，采用溶液电纺，条件为电压20kV、距离15cm，注射速率2ml/h制得TPU纳米纤维膜，经乙醚清洁，水洗晾干后，取1g TPU纳米纤维膜用30ml步骤1制得的COF格氏试剂二浸二轧，每次浸渍时间为10min，再经50ml 6.42g/L 4',4”',4””'-氮三[([1,1'-联苯]-3,5-二甲醛)]溶液二浸二轧，每次浸渍时间为20min，水洗烘干；
3.将1g步骤2处理的TPU纳米纤维膜在30ml 0.17g/L硝酸银溶液中二浸二轧，每次浸渍时间为10min，水洗，回收水洗液，得到抗菌纳米敷料B；
4.将步骤3回收的水洗液，经减压蒸馏浓缩后，可用作步骤3的硝酸银溶液用于浸轧。
实施例3
一种抗菌纳米敷料及其制备方法，包括如下步骤：
1.将1.0g 2,4,6-三(4-(溴甲基)苯基)-1,3,5-三嗪溶于220ml乙醚，加入2g镁粉，制得COF格氏试剂；
2.利用200g/L TPU的DMF溶液，采用溶液电纺，条件为电压15kV、距离20cm，注射速率1ml/h制得TPU纳米纤维膜，经乙醚清洁，水洗晾干后，取1g TPU纳米纤维膜用50ml步骤1制得的COF格氏试剂二浸二轧，每次浸渍时间为20min，再经30ml 6.42g/L 4',4”',4””'-氮三[([1,1'-联苯]-3,5-二甲醛)]溶液二浸二轧，每次浸渍时间为10min，水洗烘干；
3.将1g步骤2处理的TPU纳米纤维膜在50ml 0.17g/L硝酸银溶液中二浸二轧，每次浸渍时间为20min，水洗，回收水洗液，得到抗菌纳米敷料C；
4.将步骤3回收的水洗液，经减压蒸馏浓缩后，可用作步骤3的硝酸银溶液用于浸轧。
抗菌性能测试
将供试菌种铜绿假单胞菌(ATCC 9027)在营养琼脂面上连续培养3代37±0.5℃恒温箱中培养18～20h，放置在4℃保存备用，作为实验菌种。用无菌棉蘸取浓度为5×105cfu/ml试验菌悬液，在营养琼脂培养基平板表面均匀涂抹。盖好平皿，置室温干燥5min。用打孔器取直径10mm的实施例1-3样品和两款市售聚氨酯敷料(市售1：3M防水透气透明敷料和市售2：CaduMedi防水透气敷贴)分别放在培养基中，置于37±0.5℃恒温箱中培养24h，测量抑菌环的大小，每组3个平行样，以抑菌环直径的平均值作为评价材料抗菌性能的依据。抑菌环越大，抑菌效果越好。
耐洗性测试：标准合成洗涤剂4g/L，浴比1:50，37℃浸渍10min；取出敷料，冷水冲洗，晾干，为1次洗涤。重复上述方法n次，测试洗涤后敷料的抗菌效果。
表1抗菌性能测试
根据表1可知，本发明制备的抗菌纳米敷料具有良好的抑制铜绿假单胞菌生长的作用，而且敷料经数次洗涤后，依然具有明显的抑制效果，与市售的敷料相比，其抗菌作用显著。
本发明提供了一种抗菌纳米敷料及其制备方法的思路及方法，具体实现该技术方案的方法和途径很多，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。本实施例中未明确的各组成部分均可用现有技术加以实现。
Claims (9)
1.一种抗菌纳米敷料的制备方法，其特征在于，包括如下步骤：
S1.将溴代COF有机单体溶于有机溶剂，加入镁粉，制得COF格氏试剂；所述溴代COF有机单体为5,10,15,20-四(4-溴苯基)卟啉、三(4-溴苯基)胺和2,4,6-三(4-(溴甲基)苯基)-1,3,5-三嗪中的一种；
S2.以TPU的DMF溶液为纺丝液，通过溶液电纺制得TPU纳米纤维膜，将所述TPU纳米纤维膜预处理后，用所述COF格氏试剂浸轧，再经4',4''',4'''''-氮三[([1,1'-联苯]-3,5-二甲醛)]溶液浸轧，水洗烘干；
S3.将步骤S2处理得到的TPU纳米纤维膜在硝酸银溶液中浸轧，水洗，得到抗菌纳米敷料。
2.根据权利要求1所述的制备方法，其特征在于，所述4',4''',4'''''-氮三[([1,1'-联苯]-3,5-二甲醛)]溶液的浓度为6.42g/L；所述TPU的DMF溶液的浓度为200g/L；所述硝酸银溶液的浓度为0.17g/L。
3.根据权利要求1所述的制备方法，其特征在于，步骤S1中，所述有机溶剂为乙醚或四氢呋喃。
4.根据权利要求1所述的制备方法，其特征在于，步骤S1中，所述溴代COF有机单体、有机溶剂、镁粉的比例为1.0g：（100-220）ml：（0.5-2）g。
5.根据权利要求1所述的制备方法，其特征在于，步骤S2中，所述溶液电纺条件为电压15-20kv、距离15-20cm，注射速率1-2ml/h。
6.根据权利要求1所述的制备方法，其特征在于，步骤S2中，所述预处理具体指TPU纳米纤维膜用乙醚除去表面的灰尘和杂质，水洗后晾干。
7.根据权利要求1所述的制备方法，其特征在于，所述浸轧采用二浸二轧，每次浸渍浴比为1:30-1:50，时间为10-20min。
8.根据权利要求1所述的制备方法，其特征在于，步骤S3中，所述水洗还包括：回收水洗液，将所述水洗液经减压蒸馏浓缩后，得到可用于对TPU纳米纤维膜浸轧的硝酸银溶液。
9.根据权利要求1~8任一项所述制备方法制备得到抗菌纳米敷料。
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE721524A (zh) * | 1967-09-29 | 1969-03-27 | ||
| JPH01193349A (ja) * | 1988-01-29 | 1989-08-03 | Nippon Mektron Ltd | 含フッ素エラストマー組成物 |
| JP2004161632A (ja) * | 2002-11-11 | 2004-06-10 | Daiwa Fine Chemicals Co Ltd (Laboratory) | 銀コロイド抗菌性、殺菌性又は防黴性組成物及び該組成物を利用した製品 |
| WO2015096611A1 (zh) * | 2013-12-25 | 2015-07-02 | 重庆医药工业研究院有限责任公司 | 一种喹啉衍生物、其制备方法和应用 |
| CN110352071A (zh) * | 2016-10-26 | 2019-10-18 | 库瑞瓦格股份公司 | 脂质纳米颗粒mRNA疫苗 |
| AU2020101584A4 (en) * | 2019-07-31 | 2020-09-10 | Hefei University Of Technology | Preparation method of metal monatomic composite loaded with covalent organic framework (COF)-derived carbon skeleton |
| CN113089185A (zh) * | 2021-04-02 | 2021-07-09 | 南通大学 | 一种具有杀菌功能的导电性纳米纤维膜及制备方法与应用 |
| CN113527676A (zh) * | 2021-07-05 | 2021-10-22 | 山东师范大学 | 一种共价有机框架材料及其制备方法与应用 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111440253B (zh) * | 2019-01-17 | 2021-08-27 | 中国科学院上海药物研究所 | 立方形环糊精骨架-rgd组合物及其制备方法 |
-
2022
- 2022-07-18 CN CN202210844018.4A patent/CN115094573B/zh active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE721524A (zh) * | 1967-09-29 | 1969-03-27 | ||
| JPH01193349A (ja) * | 1988-01-29 | 1989-08-03 | Nippon Mektron Ltd | 含フッ素エラストマー組成物 |
| JP2004161632A (ja) * | 2002-11-11 | 2004-06-10 | Daiwa Fine Chemicals Co Ltd (Laboratory) | 銀コロイド抗菌性、殺菌性又は防黴性組成物及び該組成物を利用した製品 |
| WO2015096611A1 (zh) * | 2013-12-25 | 2015-07-02 | 重庆医药工业研究院有限责任公司 | 一种喹啉衍生物、其制备方法和应用 |
| CN110352071A (zh) * | 2016-10-26 | 2019-10-18 | 库瑞瓦格股份公司 | 脂质纳米颗粒mRNA疫苗 |
| AU2020101584A4 (en) * | 2019-07-31 | 2020-09-10 | Hefei University Of Technology | Preparation method of metal monatomic composite loaded with covalent organic framework (COF)-derived carbon skeleton |
| CN113089185A (zh) * | 2021-04-02 | 2021-07-09 | 南通大学 | 一种具有杀菌功能的导电性纳米纤维膜及制备方法与应用 |
| CN113527676A (zh) * | 2021-07-05 | 2021-10-22 | 山东师范大学 | 一种共价有机框架材料及其制备方法与应用 |
Non-Patent Citations (1)
| Title |
|---|
| Jia Chen.Novel Quaternary Ammonium-Functionalized Covalent Organic Frameworks/Poly (2,6-dimethyl-1,4-phenylene oxide) Hybrid Anion Exchange Membranes with Enhanced Ion Conductivity and Stability.交流应用材料.2020,1-17. * |
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