CN106620813A - Preparation method of medical antibacterial nano dressing - Google Patents
Preparation method of medical antibacterial nano dressing Download PDFInfo
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- CN106620813A CN106620813A CN201611219438.4A CN201611219438A CN106620813A CN 106620813 A CN106620813 A CN 106620813A CN 201611219438 A CN201611219438 A CN 201611219438A CN 106620813 A CN106620813 A CN 106620813A
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 104
- 229920000747 poly(lactic acid) Polymers 0.000 claims abstract description 44
- 239000004626 polylactic acid Substances 0.000 claims abstract description 44
- 229920001661 Chitosan Polymers 0.000 claims abstract description 43
- 238000001523 electrospinning Methods 0.000 claims abstract description 36
- 239000002121 nanofiber Substances 0.000 claims abstract description 32
- 239000009306 yunnan baiyao Substances 0.000 claims abstract description 24
- 239000011259 mixed solution Substances 0.000 claims abstract description 21
- 239000012528 membrane Substances 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 13
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 6
- 239000003960 organic solvent Substances 0.000 claims abstract description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 22
- 239000002904 solvent Substances 0.000 claims description 19
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical group ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 16
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 16
- 238000009987 spinning Methods 0.000 claims description 10
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 8
- JKFYKCYQEWQPTM-UHFFFAOYSA-N 2-azaniumyl-2-(4-fluorophenyl)acetate Chemical compound OC(=O)C(N)C1=CC=C(F)C=C1 JKFYKCYQEWQPTM-UHFFFAOYSA-N 0.000 claims description 6
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 6
- 229910021612 Silver iodide Inorganic materials 0.000 claims description 6
- 229940045105 silver iodide Drugs 0.000 claims description 6
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 claims description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- YVHPHQBRUPLYOS-UHFFFAOYSA-N dichloromethane;methane Chemical compound C.ClCCl YVHPHQBRUPLYOS-UHFFFAOYSA-N 0.000 claims 1
- 230000005611 electricity Effects 0.000 claims 1
- 238000000465 moulding Methods 0.000 claims 1
- 230000003068 static effect Effects 0.000 claims 1
- 229910052709 silver Inorganic materials 0.000 abstract description 12
- 239000004332 silver Substances 0.000 abstract description 12
- 229940079593 drug Drugs 0.000 abstract description 11
- 239000003814 drug Substances 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 description 26
- 239000002184 metal Substances 0.000 description 26
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 21
- 229920000742 Cotton Polymers 0.000 description 16
- 239000004744 fabric Substances 0.000 description 16
- 239000012046 mixed solvent Substances 0.000 description 16
- 206010052428 Wound Diseases 0.000 description 9
- 208000027418 Wounds and injury Diseases 0.000 description 9
- 229960000583 acetic acid Drugs 0.000 description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 8
- 239000011888 foil Substances 0.000 description 8
- 239000012362 glacial acetic acid Substances 0.000 description 8
- 230000000740 bleeding effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000001737 promoting effect Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- -1 silver ions Chemical class 0.000 description 3
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 230000003110 anti-inflammatory effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 230000017531 blood circulation Effects 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 230000035876 healing Effects 0.000 description 2
- 239000012567 medical material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000029663 wound healing Effects 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 208000007536 Thrombosis Diseases 0.000 description 1
- 206010048038 Wound infection Diseases 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229940121363 anti-inflammatory agent Drugs 0.000 description 1
- 239000002260 anti-inflammatory agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 229940030225 antihemorrhagics Drugs 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000023597 hemostasis Effects 0.000 description 1
- 239000002874 hemostatic agent Substances 0.000 description 1
- 230000002439 hemostatic effect Effects 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004089 microcirculation Effects 0.000 description 1
- 230000037257 muscle growth Effects 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- ANOBYBYXJXCGBS-UHFFFAOYSA-L stannous fluoride Chemical compound F[Sn]F ANOBYBYXJXCGBS-UHFFFAOYSA-L 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229940099259 vaseline Drugs 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/26—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/18—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing inorganic materials
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/28—Polysaccharides or their derivatives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/40—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing ingredients of undetermined constitution or reaction products thereof, e.g. plant or animal extracts
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/46—Deodorants or malodour counteractants, e.g. to inhibit the formation of ammonia or bacteria
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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Abstract
本发明涉及一种医用抗菌纳米敷料的制备方法,包括以下步骤:将聚乳酸溶于有机溶剂,得到浓度为6wt%‑10wt%的聚乳酸溶液;将壳聚糖溶于酸,得到质量分数为2wt%‑5wt%的壳聚糖溶液;混合聚乳酸溶液与壳聚糖溶液,然后向混合溶液中加入云南白药和银盐,避光条件下搅拌均匀,得到静电纺丝溶液;将静电纺丝溶液进行静电纺丝,得到医用抗菌纳米敷料。本发明采用静电纺丝技术制备纳米级别的载药纳米纤维膜,采用生物相容性好的聚乳酸和本身具有杀菌性能壳聚糖作为基础材料,以云南白药和银作为添加成分,结合四者的优势,提供了一种疗效更好的新型医用纳米抗菌敷料。
The invention relates to a preparation method of a medical antibacterial nano dressing, which comprises the following steps: dissolving polylactic acid in an organic solvent to obtain a polylactic acid solution with a concentration of 6wt%-10wt%; dissolving chitosan in acid to obtain a mass fraction of 2wt%-5wt% chitosan solution; mix polylactic acid solution and chitosan solution, then add Yunnan Baiyao and silver salt to the mixed solution, and stir evenly under dark conditions to obtain an electrospinning solution; electrospinning The solution is electrospun to obtain a medical antibacterial nano dressing. The invention adopts electrospinning technology to prepare nano-scale drug-loaded nanofiber membranes, uses polylactic acid with good biocompatibility and chitosan with bactericidal properties as basic materials, and uses Yunnan Baiyao and silver as additional components, combining the four Advantages, providing a new type of medical nano antibacterial dressing with better curative effect.
Description
技术领域technical field
本发明涉及医用材料制备技术领域,尤其涉及一种医用抗菌纳米敷料的制备方法。The invention relates to the technical field of preparation of medical materials, in particular to a preparation method of a medical antibacterial nanometer dressing.
背景技术Background technique
静电纺丝是一种简单低成本的连续制作纳米纤维的方法。静电纺丝制得的纳米纤维有很大的比表面积,而多孔纳米纤维以其更高的比表面积和良好的性能,在生物医药等方面应用广泛,包括伤口敷料、药物缓释载体、组织工程等。Electrospinning is a simple and low-cost method for continuous fabrication of nanofibers. Nanofibers prepared by electrospinning have a large specific surface area, and porous nanofibers are widely used in biomedicine due to their higher specific surface area and good performance, including wound dressings, drug sustained release carriers, tissue engineering, etc. Wait.
聚乳酸具有良好的生物相容性及生物可降解性,其降解产物可被机体吸收,且具有较好的力学性能,在生物医学领域有着广泛的应用。但聚乳酸结构中含有大量的酯键,对细胞的粘附性较弱,其降解过程中的酸性环境会导致无菌性炎症反应。壳聚糖的止血、抑菌、抗菌性、生物相容性、促进伤口愈合以及易于形成凝胶的性质,都赋予了它用作止血敷料或止血剂的良好性能,其本身具有抑菌、抗菌作用。但纯壳聚糖膜脆性大,力学性能欠佳。结合聚乳酸优异的力学性能,将两者混纺作为基础材料可以优势互补。Polylactic acid has good biocompatibility and biodegradability, its degradation products can be absorbed by the body, and has good mechanical properties, so it has a wide range of applications in the field of biomedicine. However, the polylactic acid structure contains a large number of ester bonds, which has weak adhesion to cells, and the acidic environment during its degradation process will lead to sterile inflammatory reactions. Chitosan's properties of hemostasis, antibacterial, antibacterial, biocompatibility, promotion of wound healing, and easy gel formation all endow it with good performance as a hemostatic dressing or hemostatic agent. effect. However, the pure chitosan film is brittle and has poor mechanical properties. Combined with the excellent mechanical properties of polylactic acid, the blending of the two as the basic material can complement each other.
云南白药由多种名贵药材组方而成,具有化疲止血、活血化瘀、抗炎愈伤、化腐生肌的神奇功效。现代药理学研究表明,云南白药不仅可以增强血小板活化率,加速血小板向创面的聚集速度,缩短出血及凝血时间,抑制创面渗血;还能降低血私稠度,加速微循环,防止血栓形成。因此云南白药在敷料领域有广阔的应用前景。Yunnan Baiyao is composed of a variety of precious medicinal materials, which has the miraculous effects of reducing fatigue and stopping bleeding, promoting blood circulation and removing blood stasis, anti-inflammatory and healing wounds, reducing putrefaction and promoting muscle growth. Modern pharmacological studies have shown that Yunnan Baiyao can not only enhance the activation rate of platelets, accelerate the aggregation of platelets to the wound surface, shorten the bleeding and coagulation time, and inhibit the bleeding from the wound surface; it can also reduce blood density, accelerate microcirculation, and prevent thrombus formation. Therefore, Yunnan Baiyao has broad application prospects in the dressing field.
此外,银具有优异的广谱抗菌能力,同时对人无毒副作用,可被广泛用作抗菌消炎剂使用。通过静电纺丝方法制备含银的纳米纤维,可达到均匀缓慢释放银离子,从而达到持久杀菌效果。通过缓慢释放敷料中的银离子,可有望达到对创口的持续杀菌消炎效果。In addition, silver has excellent broad-spectrum antibacterial ability and has no toxic side effects to humans, so it can be widely used as an antibacterial and anti-inflammatory agent. The preparation of silver-containing nanofibers by electrospinning can achieve uniform and slow release of silver ions, thereby achieving a long-lasting bactericidal effect. By slowly releasing the silver ions in the dressing, it is expected to achieve a continuous sterilization and anti-inflammatory effect on the wound.
敷料是一类可以起到暂时保护伤口、防止外界病菌侵入、促进愈合的医用材料。传统的敷料如纱布、海绵垫等在临床使用中也存在着一些问题,比如,现有的敷料只能对伤口进行包扎,不含药物成分,吸湿性和透气性较差,而目前临床使用的创口敷料多为凡士林纱布、碘伏纱布和无纺布等材料,用于清洁和保护创面。但这些材料在高效抑菌、减少伤口感染、促进创口愈合等方面仍然无法满足临床治疗的需求。Dressings are a class of medical materials that can temporarily protect wounds, prevent external germs from invading, and promote healing. Traditional dressings such as gauze, sponge pads, etc. also have some problems in clinical use. For example, the existing dressings can only bandage the wound, do not contain pharmaceutical ingredients, and have poor hygroscopicity and air permeability. Wound dressings are mostly materials such as vaseline gauze, iodophor gauze and non-woven fabrics, which are used to clean and protect the wound surface. However, these materials still cannot meet the needs of clinical treatment in terms of efficient antibacterial, reducing wound infection, and promoting wound healing.
发明内容Contents of the invention
为解决上述技术问题,本发明的目的是提供一种医用抗菌纳米敷料的制备方法,采用静电纺丝技术制备纳米级别的载药纳米纤维膜,采用生物相容性好的聚乳酸和本身具有杀菌性能壳聚糖作为基础材料,以云南白药和银作为添加成分,结合四者的优点,提供了一种疗效更好的新型医用纳米抗菌敷料。In order to solve the above-mentioned technical problems, the purpose of the present invention is to provide a preparation method of medical antibacterial nano dressing, which uses electrospinning technology to prepare nano-scale drug-loaded nanofiber membranes, adopts polylactic acid with good biocompatibility and has bactericidal properties. Performance Chitosan is used as the basic material, and Yunnan Baiyao and silver are used as the added components. Combining the advantages of the four, a new type of medical nano-antibacterial dressing with better curative effect is provided.
本发明的医用抗菌纳米敷料的制备方法,包括以下步骤:The preparation method of medical antibacterial nanometer dressing of the present invention, comprises the following steps:
(1)将聚乳酸溶于有机溶剂,得到浓度为6wt%-10wt%的聚乳酸溶液;(1) dissolving polylactic acid in an organic solvent to obtain a polylactic acid solution with a concentration of 6wt%-10wt%;
(2)将壳聚糖溶于酸,得到质量分数为2wt%-5wt%的壳聚糖溶液;(2) chitosan is dissolved in acid to obtain a chitosan solution whose mass fraction is 2wt%-5wt%;
(3)混合步骤(1)得到的聚乳酸溶液与步骤(2)得到的壳聚糖溶液,然后向混合溶液中加入云南白药和银盐,避光条件下搅拌均匀,得到静电纺丝溶液;(3) mixing the polylactic acid solution obtained in step (1) and the chitosan solution obtained in step (2), then adding Yunnan Baiyao and silver salt to the mixed solution, stirring evenly under dark conditions to obtain an electrospinning solution;
(4)将静电纺丝溶液进行静电纺丝,得到医用抗菌纳米敷料。(4) Electrospinning the electrospinning solution to obtain a medical antibacterial nano dressing.
进一步地,在步骤(1)中,将聚乳酸在有机溶剂中搅拌2-4h以使其完全溶解。Further, in step (1), the polylactic acid is stirred in an organic solvent for 2-4 hours to completely dissolve it.
进一步地,在步骤(1)中,有机溶剂包括主溶剂和辅助溶剂,主溶剂为三氯甲烷或二氯甲烷,辅助溶剂为N,N-二甲基甲酰胺或乙醇。Further, in step (1), the organic solvent includes a main solvent and an auxiliary solvent, the main solvent is chloroform or dichloromethane, and the auxiliary solvent is N,N-dimethylformamide or ethanol.
进一步地,当辅助溶剂为N,N-二甲基甲酰胺时,主溶剂与N,N-二甲基甲酰胺的质量比为5:1-9:1;当辅助溶剂为乙醇时,主溶剂与乙醇的质量比为1:1-3:1。Further, when the auxiliary solvent is N,N-dimethylformamide, the mass ratio of the main solvent to N,N-dimethylformamide is 5:1-9:1; when the auxiliary solvent is ethanol, the main solvent The mass ratio of solvent to ethanol is 1:1-3:1.
进一步地,辅助溶剂为N,N-二甲基甲酰胺时,主溶剂与N,N-二甲基甲酰胺的质量比为9:1,8:1,7:1,6:1或5:1。辅助溶剂为乙醇时,主溶剂与乙醇的质量比为8:1,7:1或6:1。Further, when the auxiliary solvent is N,N-dimethylformamide, the mass ratio of the main solvent to N,N-dimethylformamide is 9:1, 8:1, 7:1, 6:1 or 5 :1. When the auxiliary solvent is ethanol, the mass ratio of the main solvent to ethanol is 8:1, 7:1 or 6:1.
优选地,按质量比,三氯甲烷:乙醇=1:1;二氯甲烷:酒精=1:1;三氯甲烷:N,N-二甲基甲酰胺=9:1;二氯甲烷:N,N-二甲基甲酰胺=9:1。Preferably, by mass ratio, chloroform: ethanol = 1:1; dichloromethane: alcohol = 1:1; chloroform: N,N-dimethylformamide = 9:1; dichloromethane: N , N-dimethylformamide = 9:1.
进一步地,在步骤(2)中,酸为甲酸或乙酸。Further, in step (2), the acid is formic acid or acetic acid.
进一步地,在步骤(2)中,将壳聚糖在酸中搅拌4-6h,使其完全溶解。Further, in step (2), stir the chitosan in acid for 4-6 hours to dissolve it completely.
进一步地,在步骤(3)中,聚乳酸溶液与壳聚糖溶液的质量比为1-2:1-3。Further, in step (3), the mass ratio of the polylactic acid solution to the chitosan solution is 1-2:1-3.
进一步地,在步骤(3)中,聚乳酸溶液与壳聚糖溶液的质量比为1:1,2:1,1:2或1:3。优选的,聚乳酸溶液与壳聚糖溶液的质量比为1:1。Further, in step (3), the mass ratio of the polylactic acid solution to the chitosan solution is 1:1, 2:1, 1:2 or 1:3. Preferably, the mass ratio of the polylactic acid solution to the chitosan solution is 1:1.
进一步地,在步骤(3)中,云南白药占混合溶液总质量的8%-10%。Further, in step (3), Yunnan Baiyao accounts for 8%-10% of the total mass of the mixed solution.
进一步地,在步骤(3)中,银盐为硝酸银、氯化银、溴化银和碘化银中的一种或几种。Further, in step (3), the silver salt is one or more of silver nitrate, silver chloride, silver bromide and silver iodide.
进一步地,在步骤(3)中,银盐占混合溶液质量的4%-6%。Further, in step (3), the silver salt accounts for 4%-6% of the mass of the mixed solution.
进一步地,在步骤(3)中,避光条件下搅拌1-2h。Further, in step (3), stir for 1-2 h under the condition of avoiding light.
进一步地,在步骤(4)中,在20-30℃,45%-65%相对湿度下进行静电纺丝。Further, in step (4), electrospinning is carried out at 20-30° C. and 45%-65% relative humidity.
进一步地,所述步骤(4)包括以下步骤:Further, the step (4) includes the following steps:
(S1)将静电纺丝溶液倒入注射器中,并连接高压电源,在接收板上覆盖基层后,在10-20kV下进行静电纺丝得到一层纳米纤维膜;;(S1) Pour the electrospinning solution into a syringe, connect a high-voltage power supply, cover the base layer on the receiving plate, and perform electrospinning at 10-20kV to obtain a layer of nanofiber film;
(S2)在步骤(S1)得到的所述纳米纤维膜上再附上一层基层,在10-20kV下进行静电纺丝,形成第二层纳米纤维膜,待第二层纳米纤维膜成型后再覆盖一层基层,得到医用抗菌纳米敷料;(S2) Attach a base layer on the nanofiber membrane obtained in step (S1), and carry out electrospinning at 10-20kV to form a second nanofiber membrane, after the second nanofiber membrane is formed Then cover a base layer to obtain a medical antibacterial nano dressing;
其中,注射器的喷头与接收板的距离为10-20cm,静电纺丝溶液的流速为0.4-1.0ml/h。Wherein, the distance between the nozzle of the injector and the receiving plate is 10-20 cm, and the flow rate of the electrospinning solution is 0.4-1.0 ml/h.
进一步地,在步骤(S1)中,接收板为金属板。在金属板上覆盖三层纱布作为基层。Further, in the step (S1), the receiving plate is a metal plate. Cover the metal plate with three layers of gauze as a base layer.
进一步地,在步骤(S2)中,在步骤(S1)得到的纳米纤维膜上再附上两层纱布作为基层。待第二层纳米纤维膜成型后,再覆盖三层纱布。Further, in step (S2), attach two layers of gauze as the base layer on the nanofiber membrane obtained in step (S1). After the second layer of nanofiber membrane is formed, it is covered with three layers of gauze.
借由上述方案,本发明至少具有以下优点:By means of the above solution, the present invention has at least the following advantages:
采用本发明的技术方案,制备出直径为60nm左右的纳米纤维,这些纳米纤维构成了抗菌纳米敷料,由纳米纤维聚集成膜所制得的敷料拥有更好的药物释放效果,因静电纺丝的纳米纤维膜比表面积远大于普通敷料,比表面积越大,吸附性能越强,因此可以吸附更多的药物,后期释放的药物也越多;选用壳聚糖和聚乳酸所制备的敷料具有优异的力学性质,强度好;选用云南白药制备敷料,其同时具备抗菌和活血化瘀消肿止痛的作用;选用跟抗生素抗菌效果接近的银离子作为抗菌物质,同时结合云南白药和纳米纤维的优势获得了纳米敷料,其对金黄葡萄球菌可达到97%的抑菌率,对大肠杆菌可达到99%的抑菌率;本发明提供了最适宜制备新型医用敷料的原料配比和实验条件,然后利用静电纺丝技术直接制备一种医用抗菌纳米敷料,结构简单、操作方便、控制简单、工艺流程短。Adopting the technical solution of the present invention, nanofibers with a diameter of about 60nm are prepared, and these nanofibers constitute an antibacterial nano dressing. The specific surface area of the nanofiber membrane is much larger than that of ordinary dressings. The larger the specific surface area, the stronger the adsorption performance, so it can absorb more drugs and release more drugs in the later stage; the dressing prepared by using chitosan and polylactic acid has excellent The mechanical properties and strength are good; Yunnan Baiyao is used to prepare the dressing, which has the functions of antibacterial, blood circulation, stasis, swelling and pain relief; silver ions, which are close to the antibacterial effect of antibiotics, are used as antibacterial substances, and combined with the advantages of Yunnan Baiyao and nanofibers Nano dressing, which can reach 97% antibacterial rate to Staphylococcus aureus, and can reach 99% antibacterial rate to Escherichia coli; the invention provides the most suitable raw material ratio and experimental conditions for preparing new medical dressings, and then uses electrostatic A medical antibacterial nano dressing is directly prepared by spinning technology, which has simple structure, convenient operation, simple control and short process flow.
上述说明仅是本发明技术方案的概述,为了能够更清楚了解本发明的技术手段,并可依照说明书的内容予以实施,以下以本发明的较佳实施例并配合附图详细说明如后。The above description is only an overview of the technical solutions of the present invention. In order to understand the technical means of the present invention more clearly and implement them according to the contents of the description, the preferred embodiments of the present invention and accompanying drawings are described in detail below.
附图说明Description of drawings
图1是本发明制备的医用抗菌纳米敷料的剖面结构示意图;Fig. 1 is the sectional structure schematic diagram of the medical antibacterial nano dressing prepared by the present invention;
图2是本发明制备的医用抗菌纳米敷料中纳米纤维膜整体形貌的扫描电镜图;Fig. 2 is the scanning electron micrograph of the overall appearance of nanofiber membrane in the medical antibacterial nano dressing prepared by the present invention;
图3是本发明制备的医用抗菌纳米敷料中纳米纤维膜的局部扫描电镜图;Fig. 3 is the partial scanning electron micrograph of nanofiber film in the medical antibacterial nano dressing prepared by the present invention;
图4是本发明制备的医用抗菌纳米敷料在台式电镜能谱仪下扫描银的示意图;Fig. 4 is the schematic diagram that the medical antibacterial nano dressing prepared by the present invention scans silver under the desktop electron microscope energy spectrometer;
图5是本发明医用抗菌纳米敷料中纳米纤维膜的元素分析结果;Fig. 5 is the elemental analysis result of the nanofibrous film in the medical antibacterial nano dressing of the present invention;
图6是云南白药的红外光谱图;Fig. 6 is the infrared spectrogram of Yunnan Baiyao;
图7是载药纳米纤维膜的红外光谱图;Fig. 7 is the infrared spectrogram of drug-loaded nanofiber membrane;
附图标记说明:1-医用纱布;2-载药纳米纤维膜。Explanation of reference numerals: 1 - medical gauze; 2 - drug-loaded nanofiber membrane.
具体实施方式detailed description
下面结合附图和实施例,对本发明的具体实施方式作进一步详细描述。以下实施例用于说明本发明,但不用来限制本发明的范围。The specific implementation manners of the present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments. The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention.
实施例1Example 1
在棕色磨口瓶中将质量比为9:1的二氯甲烷和N,N-二甲基甲酰胺相互混合,得到混合溶剂。然后将聚乳酸溶于上述混合溶剂,在磁力搅拌器上匀速搅拌3h,使其完全溶解,配制出浓度为8wt%的聚乳酸溶液,溶液呈澄清透明状。Mix dichloromethane and N,N-dimethylformamide at a mass ratio of 9:1 in a brown ground-mouth bottle to obtain a mixed solvent. Then polylactic acid was dissolved in the above mixed solvent, stirred at a constant speed on a magnetic stirrer for 3 hours to completely dissolve, and a polylactic acid solution with a concentration of 8 wt% was prepared, and the solution was clear and transparent.
在烧杯中将壳聚糖溶于冰乙酸,然后在磁力搅拌器上匀速搅拌6h,使其完全溶解,得到乳白色的壳聚糖溶液,壳聚糖溶液的浓度为3wt%。Chitosan was dissolved in glacial acetic acid in a beaker, and then stirred at a constant speed on a magnetic stirrer for 6 hours to completely dissolve to obtain a milky white chitosan solution with a concentration of 3 wt%.
将上述聚乳酸溶液与壳聚糖溶液案1:1的质量比在棕色磨口瓶中混合,然后向溶液中加入相对于混合溶液质量10%的云南白药溶液,并加入相对于混合溶液溶质质量5%的硝酸银。用铝箔包裹棕色磨口瓶,保证完全避光,然后在磁力搅拌器上匀速搅拌2h,待硝酸银完全溶解,得到淡黄色的静电纺丝溶液。Mix the above-mentioned polylactic acid solution and chitosan solution at a mass ratio of 1:1 in a brown ground-mouth bottle, then add 10% Yunnan Baiyao solution relative to the quality of the mixed solution, and add 10% of the solute quality relative to the mixed solution 5% silver nitrate. Wrap the brown ground bottle with aluminum foil to ensure that it is completely protected from light, and then stir it on a magnetic stirrer at a constant speed for 2 hours until the silver nitrate is completely dissolved to obtain a light yellow electrospinning solution.
控制实验环境温度在20℃-30℃,相对湿度在45%-65%。将配置好的静电纺丝溶液倒入喷射口内径为0.7mm,容量为10ml的注射器中并将注射器固定在注射泵上,注射器喷射口和实验接收板分别连接直流高压电源的正负极,接收板为金属板,在金属接收板上覆盖三层纱布作为基层,接收板和喷丝头之间的距离调节为15cm。实验装置检查无误后打开注射泵调节流速为0.6ml/h,待溶液缓慢流出后打开高压电源并调节电压为15kV,开始纺丝实验。待在接收板棉织物上形成一层膜后,调低关闭电压装置,在接收板上再贴附大小相等的两层纱布,重启电压装置,在第二层膜成型后,调零高压电源并切断电源,然后取下金属接收板上的棉织物并在第二层膜上面覆盖三层纱布,得到医用抗菌纳米敷料。The temperature of the experimental environment is controlled at 20°C-30°C, and the relative humidity is at 45%-65%. Pour the prepared electrospinning solution into a syringe with an inner diameter of 0.7mm and a capacity of 10ml and fix the syringe on the syringe pump. The plate is a metal plate, covered with three layers of gauze on the metal receiving plate as the base layer, and the distance between the receiving plate and the spinneret is adjusted to 15cm. After the experimental device is checked correctly, turn on the syringe pump and adjust the flow rate to 0.6ml/h. After the solution flows out slowly, turn on the high voltage power supply and adjust the voltage to 15kV to start the spinning experiment. After a layer of film is formed on the cotton fabric of the receiving plate, turn down the voltage device, attach two layers of gauze of equal size to the receiving plate, restart the voltage device, and after the second layer of film is formed, adjust the high-voltage power supply to zero and Cut off the power supply, then remove the cotton fabric on the metal receiving plate and cover three layers of gauze on the second layer of film to obtain a medical antibacterial nano dressing.
实施例2Example 2
在棕色磨口瓶中将质量比为8:1的三氯甲烷和无水乙醇相互混合,得到混合溶剂。然后将聚乳酸溶于上述混合溶剂,在磁力搅拌器上匀速搅拌3h,使其完全溶解,配制出浓度为10wt%的聚乳酸溶液,溶液呈澄清透明状。Mix chloroform and absolute ethanol with a mass ratio of 8:1 in a brown ground-mouth bottle to obtain a mixed solvent. Then polylactic acid was dissolved in the above mixed solvent, stirred at a constant speed on a magnetic stirrer for 3 hours to completely dissolve, and a polylactic acid solution with a concentration of 10 wt% was prepared, and the solution was clear and transparent.
在烧杯中将壳聚糖溶于冰乙酸,然后在磁力搅拌器上匀速搅拌6h,使其完全溶解,得到乳白色的壳聚糖溶液,壳聚糖溶液的浓度为3wt%。Chitosan was dissolved in glacial acetic acid in a beaker, and then stirred at a constant speed on a magnetic stirrer for 6 hours to completely dissolve to obtain a milky white chitosan solution with a concentration of 3 wt%.
将上述聚乳酸溶液与壳聚糖溶液案1:1的质量比在棕色磨口瓶中混合,然后向溶液中加入相对于混合溶液质量10%的云南白药溶液,并加入相对于混合溶液溶质质量6%的氯化银。用铝箔包裹棕色磨口瓶,保证完全避光,然后在磁力搅拌器上匀速搅拌2h,待氯化银完全溶解,得到淡黄色的静电纺丝溶液。Mix the above-mentioned polylactic acid solution and chitosan solution at a mass ratio of 1:1 in a brown ground-mouth bottle, then add 10% Yunnan Baiyao solution relative to the quality of the mixed solution, and add 10% of the solute quality relative to the mixed solution 6% silver chloride. Wrap the brown ground-mouth bottle with aluminum foil to ensure that it is completely protected from light, and then stir it on a magnetic stirrer at a constant speed for 2 hours until the silver chloride is completely dissolved to obtain a light yellow electrospinning solution.
控制实验环境温度在20℃-30℃,相对湿度在45%-65%。将配置好的静电纺丝溶液倒入喷射口内径为0.7mm,容量为10ml的注射器中并将注射器固定在注射泵上,注射器喷射口和实验接收板分别连接直流高压电源的正负极,接收板为金属板,在金属接收板上覆盖三层纱布作为基层,接收板和喷丝头之间的距离调节为13cm。实验装置检查无误后打开注射泵调节流速为0.8ml/h,待溶液缓慢流出后打开高压电源并调节电压为20kV,开始纺丝实验。待在接收板棉织物上形成一层膜后,调低关闭电压装置,在接收板上再贴附大小相等的两层纱布,重启电压装置,在第二层膜成型后,调零高压电源并切断电源,然后取下金属接收板上的棉织物并在第二层膜上面覆盖三层纱布,得到医用抗菌纳米敷料。The temperature of the experimental environment is controlled at 20°C-30°C, and the relative humidity is at 45%-65%. Pour the prepared electrospinning solution into a syringe with an inner diameter of 0.7mm and a capacity of 10ml and fix the syringe on the syringe pump. The plate is a metal plate, covered with three layers of gauze as the base layer on the metal receiving plate, and the distance between the receiving plate and the spinneret is adjusted to 13cm. After the experimental device is checked correctly, turn on the syringe pump and adjust the flow rate to 0.8ml/h. After the solution flows out slowly, turn on the high voltage power supply and adjust the voltage to 20kV to start the spinning experiment. After a layer of film is formed on the cotton fabric of the receiving plate, turn down the voltage device, attach two layers of gauze of equal size to the receiving plate, restart the voltage device, and after the second layer of film is formed, adjust the high-voltage power supply to zero and Cut off the power supply, then remove the cotton fabric on the metal receiving plate and cover three layers of gauze on the second layer of film to obtain a medical antibacterial nano dressing.
实施例3Example 3
在棕色磨口瓶中将质量比为5:1的二氯甲烷和N,N-二甲基甲酰胺相互混合,得到混合溶剂。然后将聚乳酸溶于上述混合溶剂,在磁力搅拌器上匀速搅拌3h,使其完全溶解,配制出浓度为8wt%的聚乳酸溶液,溶液呈澄清透明状。Mix dichloromethane and N,N-dimethylformamide at a mass ratio of 5:1 in a brown ground-mouth bottle to obtain a mixed solvent. Then polylactic acid was dissolved in the above mixed solvent, stirred at a constant speed on a magnetic stirrer for 3 hours to completely dissolve, and a polylactic acid solution with a concentration of 8 wt% was prepared, and the solution was clear and transparent.
在烧杯中将壳聚糖溶于冰乙酸,然后在磁力搅拌器上匀速搅拌6h,使其完全溶解,得到乳白色的壳聚糖溶液,壳聚糖溶液的浓度为3wt%。Chitosan was dissolved in glacial acetic acid in a beaker, and then stirred at a constant speed on a magnetic stirrer for 6 hours to completely dissolve to obtain a milky white chitosan solution with a concentration of 3 wt%.
将上述聚乳酸溶液与壳聚糖溶液按2:1的质量比在棕色磨口瓶中混合,然后向溶液中加入相对于混合溶液质量10%的云南白药溶液,并加入相对于混合溶液溶质质量6%的碘化银。用铝箔包裹棕色磨口瓶,保证完全避光,然后在磁力搅拌器上匀速搅拌2h,待碘化银完全溶解,得到淡黄色的静电纺丝溶液。Mix the above polylactic acid solution and chitosan solution in a brown ground-mouth bottle at a mass ratio of 2:1, then add 10% Yunnan Baiyao solution relative to the mass of the mixed solution, and add 10% of the solute mass relative to the mixed solution 6% silver iodide. Wrap the brown ground bottle with aluminum foil to ensure that it is completely protected from light, and then stir it on a magnetic stirrer at a constant speed for 2 hours until the silver iodide is completely dissolved to obtain a light yellow electrospinning solution.
控制实验环境温度在20℃-30℃,相对湿度在45%-65%。将配置好的静电纺丝溶液倒入喷射口内径为0.7mm,容量为10ml的注射器中并将注射器固定在注射泵上,注射器喷射口和实验接收板分别连接直流高压电源的正负极,接收板为金属板,在金属接收板上覆盖三层纱布作为基层,接收板和喷丝头之间的距离调节为15cm。实验装置检查无误后打开注射泵调节流速为1.0ml/h,待溶液缓慢流出后打开高压电源并调节电压为20kV,开始纺丝实验。待在接收板棉织物上形成一层膜后,调低关闭电压装置,在接收板上再贴附大小相等的两层纱布,重启电压装置,在第二层膜成型后,调零高压电源并切断电源,然后取下金属接收板上的棉织物并在第二层膜上面覆盖三层纱布,得到医用抗菌纳米敷料。The temperature of the experimental environment is controlled at 20°C-30°C, and the relative humidity is at 45%-65%. Pour the prepared electrospinning solution into a syringe with an inner diameter of 0.7mm and a capacity of 10ml and fix the syringe on the syringe pump. The plate is a metal plate, covered with three layers of gauze on the metal receiving plate as the base layer, and the distance between the receiving plate and the spinneret is adjusted to 15cm. After the experimental device is checked correctly, turn on the syringe pump and adjust the flow rate to 1.0ml/h. After the solution flows out slowly, turn on the high voltage power supply and adjust the voltage to 20kV to start the spinning experiment. After a layer of film is formed on the cotton fabric of the receiving plate, turn down the voltage device, attach two layers of gauze of equal size to the receiving plate, restart the voltage device, and after the second layer of film is formed, adjust the high-voltage power supply to zero and Cut off the power supply, then remove the cotton fabric on the metal receiving plate and cover three layers of gauze on the second layer of film to obtain a medical antibacterial nano dressing.
实施例4Example 4
在棕色磨口瓶中将质量比为7:1的三氯甲烷和乙醇相互混合,得到混合溶剂。然后将聚乳酸溶于上述混合溶剂,在磁力搅拌器上匀速搅拌3h,使其完全溶解,配制出浓度为9wt%的聚乳酸溶液,溶液呈澄清透明状。Mix chloroform and ethanol with a mass ratio of 7:1 in a brown grinding bottle to obtain a mixed solvent. Then polylactic acid was dissolved in the above mixed solvent, stirred at a constant speed on a magnetic stirrer for 3 hours to completely dissolve, and a polylactic acid solution with a concentration of 9 wt% was prepared, and the solution was clear and transparent.
在烧杯中将壳聚糖溶于冰乙酸,然后在磁力搅拌器上匀速搅拌6h,使其完全溶解,得到乳白色的壳聚糖溶液,壳聚糖溶液的浓度为5wt%。Chitosan was dissolved in glacial acetic acid in a beaker, and then stirred at a constant speed on a magnetic stirrer for 6 hours to completely dissolve to obtain a milky white chitosan solution with a concentration of 5 wt%.
将上述聚乳酸溶液与壳聚糖溶液案1:1的质量比在棕色磨口瓶中混合,然后向溶液中加入相对于混合溶液质量10%的云南白药溶液,并加入相对于混合溶液溶质质量6%的碘化银。用铝箔包裹棕色磨口瓶,保证完全避光,然后在磁力搅拌器上匀速搅拌2h直至碘化银完全溶解。Mix the above-mentioned polylactic acid solution and chitosan solution at a mass ratio of 1:1 in a brown ground-mouth bottle, then add 10% Yunnan Baiyao solution relative to the quality of the mixed solution, and add 10% of the solute quality relative to the mixed solution 6% silver iodide. Wrap the brown ground bottle with aluminum foil to keep it completely protected from light, then stir it on a magnetic stirrer at a constant speed for 2 h until the silver iodide is completely dissolved.
控制实验环境温度在20℃-30℃,相对湿度在45%-65%。将配置好的静电纺丝溶液倒入喷射口内径为0.7mm,容量为10ml的注射器中并将注射器固定在注射泵上,注射器喷射口和实验接收板分别连接直流高压电源的正负极,接收板为金属板,在金属接收板上覆盖三层纱布作为基层,接收板和喷丝头之间的距离调节为15cm。实验装置检查无误后打开注射泵调节流速为0.6ml/h,待溶液缓慢流出后打开高压电源并调节电压为15kV,开始纺丝实验。待在接收板棉织物上形成一层膜后,调低关闭电压装置,在接收板上再贴附大小相等的两层纱布,重启电压装置,在第二层膜成型后,调零高压电源并切断电源,然后取下金属接收板上的棉织物并在第二层膜上面覆盖三层纱布,得到医用抗菌纳米敷料。The temperature of the experimental environment is controlled at 20°C-30°C, and the relative humidity is at 45%-65%. Pour the prepared electrospinning solution into a syringe with an inner diameter of 0.7mm and a capacity of 10ml and fix the syringe on the syringe pump. The plate is a metal plate, covered with three layers of gauze on the metal receiving plate as the base layer, and the distance between the receiving plate and the spinneret is adjusted to 15cm. After the experimental device is checked correctly, turn on the syringe pump and adjust the flow rate to 0.6ml/h. After the solution flows out slowly, turn on the high voltage power supply and adjust the voltage to 15kV to start the spinning experiment. After a layer of film is formed on the cotton fabric of the receiving plate, turn down the voltage device, attach two layers of gauze of equal size to the receiving plate, restart the voltage device, and after the second layer of film is formed, adjust the high-voltage power supply to zero and Cut off the power supply, then remove the cotton fabric on the metal receiving plate and cover three layers of gauze on the second layer of film to obtain a medical antibacterial nano dressing.
实施例5Example 5
在棕色磨口瓶中将质量比为6:1的三氯甲烷和N,N-二甲基甲酰胺相互混合,得到混合溶剂。然后将聚乳酸溶于上述混合溶剂,在磁力搅拌器上匀速搅拌3h,使其完全溶解,配制出浓度为10wt%的聚乳酸溶液,溶液呈澄清透明状。Mix chloroform and N,N-dimethylformamide with a mass ratio of 6:1 in a brown ground-mouth bottle to obtain a mixed solvent. Then polylactic acid was dissolved in the above mixed solvent, stirred at a constant speed on a magnetic stirrer for 3 hours to completely dissolve, and a polylactic acid solution with a concentration of 10 wt% was prepared, and the solution was clear and transparent.
在烧杯中将壳聚糖溶于冰乙酸,然后在磁力搅拌器上匀速搅拌6h,使其完全溶解,得到乳白色的壳聚糖溶液,壳聚糖溶液的浓度为3wt%。Chitosan was dissolved in glacial acetic acid in a beaker, and then stirred at a constant speed on a magnetic stirrer for 6 hours to completely dissolve to obtain a milky white chitosan solution with a concentration of 3 wt%.
将上述聚乳酸溶液与壳聚糖溶液案1:1的质量比在棕色磨口瓶中混合,然后向溶液中加入相对于混合溶液质量8%的云南白药溶液,并加入相对于混合溶液溶质质量6%的硝酸银。用铝箔包裹棕色磨口瓶,保证完全避光,然后在磁力搅拌器上匀速搅拌2h,待硝酸银完全溶解,得到淡黄色的静电纺丝溶液。Mix the above-mentioned polylactic acid solution and chitosan solution at a mass ratio of 1:1 in a brown ground-mouth bottle, then add 8% Yunnan Baiyao solution relative to the quality of the mixed solution, and add 6% silver nitrate. Wrap the brown ground bottle with aluminum foil to ensure that it is completely protected from light, and then stir it on a magnetic stirrer at a constant speed for 2 hours until the silver nitrate is completely dissolved to obtain a light yellow electrospinning solution.
控制实验环境温度在20℃-30℃,相对湿度在45%-65%。将配置好的静电纺丝溶液倒入喷射口内径为0.7mm,容量为10ml的注射器中并将注射器固定在注射泵上,注射器喷射口和实验接收板分别连接直流高压电源的正负极,接收板为金属板,在金属接收板上覆盖三层纱布作为基层,接收板和喷丝头之间的距离调节为15cm。实验装置检查无误后打开注射泵调节流速为0.4ml/h,待溶液缓慢流出后打开高压电源并调节电压为20kV,开始纺丝实验。待在接收板棉织物上形成一层膜后,调低关闭电压装置,在接收板上再贴附大小相等的两层纱布,重启电压装置,在第二层膜成型后,调零高压电源并切断电源,然后取下金属接收板上的棉织物并在第二层膜上面覆盖三层纱布,得到医用抗菌纳米敷料。The temperature of the experimental environment is controlled at 20°C-30°C, and the relative humidity is at 45%-65%. Pour the prepared electrospinning solution into a syringe with an inner diameter of 0.7mm and a capacity of 10ml and fix the syringe on the syringe pump. The plate is a metal plate, covered with three layers of gauze on the metal receiving plate as the base layer, and the distance between the receiving plate and the spinneret is adjusted to 15cm. After the experimental device is checked correctly, turn on the syringe pump and adjust the flow rate to 0.4ml/h. After the solution flows out slowly, turn on the high voltage power supply and adjust the voltage to 20kV to start the spinning experiment. After a layer of film is formed on the cotton fabric of the receiving plate, turn down the voltage device, attach two layers of gauze of equal size to the receiving plate, restart the voltage device, and after the second layer of film is formed, adjust the high-voltage power supply to zero and Cut off the power supply, then remove the cotton fabric on the metal receiving plate and cover three layers of gauze on the second layer of film to obtain a medical antibacterial nano dressing.
实施例6Example 6
在棕色磨口瓶中将质量比为8:1的三氯甲烷和乙醇相互混合,得到混合溶剂。然后将聚乳酸溶于上述混合溶剂,在磁力搅拌器上匀速搅拌3h,使其完全溶解,配制出浓度为8wt%的聚乳酸溶液,溶液呈澄清透明状。Mix chloroform and ethanol with a mass ratio of 8:1 in a brown ground bottle to obtain a mixed solvent. Then polylactic acid was dissolved in the above mixed solvent, stirred at a constant speed on a magnetic stirrer for 3 hours to completely dissolve, and a polylactic acid solution with a concentration of 8 wt% was prepared, and the solution was clear and transparent.
在烧杯中将壳聚糖溶于冰乙酸,然后在磁力搅拌器上匀速搅拌6h,使其完全溶解,得到乳白色的壳聚糖溶液,壳聚糖溶液的浓度为3wt%。Chitosan was dissolved in glacial acetic acid in a beaker, and then stirred at a constant speed on a magnetic stirrer for 6 hours to completely dissolve to obtain a milky white chitosan solution with a concentration of 3 wt%.
将上述聚乳酸溶液与壳聚糖溶液案1:1的质量比在棕色磨口瓶中混合,然后向溶液中加入相对于混合溶液质量12%的云南白药溶液,并加入相对于混合溶液溶质质量5%的溴化银。用铝箔包裹棕色磨口瓶,保证完全避光,然后在磁力搅拌器上匀速搅拌2h,直到溴化银完全溶解。Mix the above-mentioned polylactic acid solution and chitosan solution at a mass ratio of 1:1 in a brown ground-mouth bottle, then add 12% Yunnan Baiyao solution relative to the quality of the mixed solution to the solution, and add 5% silver bromide. Wrap the brown ground-mouth bottle with aluminum foil to ensure that it is completely protected from light, and then stir it on a magnetic stirrer at a constant speed for 2 hours until the silver bromide is completely dissolved.
控制实验环境温度在20℃-30℃,相对湿度在45%-65%。将配置好的静电纺丝溶液倒入喷射口内径为0.7mm,容量为10ml的注射器中并将注射器固定在注射泵上,注射器喷射口和实验接收板分别连接直流高压电源的正负极,接收板为金属板,在金属接收板上覆盖三层纱布作为基层,接收板和喷丝头之间的距离调节为13cm。实验装置检查无误后打开注射泵调节流速为0.8ml/h,待溶液缓慢流出后打开高压电源并调节电压为20kV,开始纺丝实验。待在接收板棉织物上形成一层膜后,调低关闭电压装置,在接收板上再贴附大小相等的两层纱布,重启电压装置,在第二层膜成型后,调零高压电源并切断电源,然后取下金属接收板上的棉织物并在第二层膜上面覆盖三层纱布,得到医用抗菌纳米敷料。The temperature of the experimental environment is controlled at 20°C-30°C, and the relative humidity is at 45%-65%. Pour the prepared electrospinning solution into a syringe with an inner diameter of 0.7mm and a capacity of 10ml and fix the syringe on the syringe pump. The plate is a metal plate, covered with three layers of gauze as the base layer on the metal receiving plate, and the distance between the receiving plate and the spinneret is adjusted to 13cm. After the experimental device is checked correctly, turn on the syringe pump and adjust the flow rate to 0.8ml/h. After the solution flows out slowly, turn on the high voltage power supply and adjust the voltage to 20kV to start the spinning experiment. After a layer of film is formed on the cotton fabric of the receiving plate, turn down the voltage device, attach two layers of gauze of equal size to the receiving plate, restart the voltage device, and after the second layer of film is formed, adjust the high-voltage power supply to zero and Cut off the power supply, then remove the cotton fabric on the metal receiving plate and cover three layers of gauze on the second layer of film to obtain a medical antibacterial nano dressing.
实施例7Example 7
在棕色磨口瓶中将质量比为7:1的二氯甲烷和N,N-二甲基甲酰胺相互混合,得到混合溶剂。然后将聚乳酸溶于上述混合溶剂,在磁力搅拌器上匀速搅拌3h,使其完全溶解,配制出浓度为9wt%的聚乳酸溶液,溶液呈澄清透明状。Mix dichloromethane and N,N-dimethylformamide with a mass ratio of 7:1 in a brown ground-mouth bottle to obtain a mixed solvent. Then polylactic acid was dissolved in the above mixed solvent, stirred at a constant speed on a magnetic stirrer for 3 hours to completely dissolve, and a polylactic acid solution with a concentration of 9 wt% was prepared, and the solution was clear and transparent.
在烧杯中将壳聚糖溶于冰乙酸,然后在磁力搅拌器上匀速搅拌6h,使其完全溶解,得到乳白色的壳聚糖溶液,壳聚糖溶液的浓度为3wt%。Chitosan was dissolved in glacial acetic acid in a beaker, and then stirred at a constant speed on a magnetic stirrer for 6 hours to completely dissolve to obtain a milky white chitosan solution with a concentration of 3 wt%.
将上述聚乳酸溶液与壳聚糖溶液案1:1的质量比在棕色磨口瓶中混合,然后向溶液中加入相对于混合溶液质量10%的云南白药溶液,并加入相对于混合溶液溶质质量5%的硝酸银。用铝箔包裹棕色磨口瓶,保证完全避光,然后在磁力搅拌器上匀速搅拌2h,待硝酸银完全溶解,得到淡黄色的静电纺丝溶液。Mix the above-mentioned polylactic acid solution and chitosan solution at a mass ratio of 1:1 in a brown ground-mouth bottle, then add 10% Yunnan Baiyao solution relative to the quality of the mixed solution, and add 10% of the solute quality relative to the mixed solution 5% silver nitrate. Wrap the brown ground bottle with aluminum foil to ensure that it is completely protected from light, and then stir it on a magnetic stirrer at a constant speed for 2 hours until the silver nitrate is completely dissolved to obtain a light yellow electrospinning solution.
控制实验环境温度在20℃-30℃,相对湿度在45%-65%。将配置好的静电纺丝溶液倒入喷射口内径为0.7mm,容量为10ml的注射器中并将注射器固定在注射泵上,注射器喷射口和实验接收板分别连接直流高压电源的正负极,接收板为金属板,在金属接收板上覆盖三层纱布作为基层,接收板和喷丝头之间的距离调节为20cm。实验装置检查无误后打开注射泵调节流速为0.6ml/h,待溶液缓慢流出后打开高压电源并调节电压为15kV,开始纺丝实验。待在接收板棉织物上形成一层膜后,调低关闭电压装置,在接收板上再贴附大小相等的两层纱布,重启电压装置,在第二层膜成型后,调零高压电源并切断电源,然后取下金属接收板上的棉织物并在第二层膜上面覆盖三层纱布,得到医用抗菌纳米敷料。The temperature of the experimental environment is controlled at 20°C-30°C, and the relative humidity is at 45%-65%. Pour the prepared electrospinning solution into a syringe with an inner diameter of 0.7mm and a capacity of 10ml and fix the syringe on the syringe pump. The plate is a metal plate, covered with three layers of gauze on the metal receiving plate as the base layer, and the distance between the receiving plate and the spinneret is adjusted to 20cm. After the experimental device is checked correctly, turn on the syringe pump and adjust the flow rate to 0.6ml/h. After the solution flows out slowly, turn on the high voltage power supply and adjust the voltage to 15kV to start the spinning experiment. After a layer of film is formed on the cotton fabric of the receiving plate, turn down the voltage device, attach two layers of gauze of equal size to the receiving plate, restart the voltage device, and after the second layer of film is formed, adjust the high-voltage power supply to zero and Cut off the power supply, then remove the cotton fabric on the metal receiving plate and cover three layers of gauze on the second layer of film to obtain a medical antibacterial nano dressing.
实施例8Example 8
在棕色磨口瓶中将质量比为5:1的二氯甲烷和乙醇相互混合,得到混合溶剂。然后将聚乳酸溶于上述混合溶剂,在磁力搅拌器上匀速搅拌3h,使其完全溶解,配制出浓度为9wt%的聚乳酸溶液,溶液呈澄清透明状。Mix dichloromethane and ethanol with a mass ratio of 5:1 in a brown grinding bottle to obtain a mixed solvent. Then polylactic acid was dissolved in the above mixed solvent, stirred at a constant speed on a magnetic stirrer for 3 hours to completely dissolve, and a polylactic acid solution with a concentration of 9 wt% was prepared, and the solution was clear and transparent.
在烧杯中将壳聚糖溶于冰乙酸,然后在磁力搅拌器上匀速搅拌6h,使其完全溶解,得到乳白色的壳聚糖溶液,壳聚糖溶液的浓度为5wt%。Chitosan was dissolved in glacial acetic acid in a beaker, and then stirred at a constant speed on a magnetic stirrer for 6 hours to completely dissolve to obtain a milky white chitosan solution with a concentration of 5 wt%.
将上述聚乳酸溶液与壳聚糖溶液案1:1的质量比在棕色磨口瓶中混合,然后向溶液中加入相对于混合溶液质量10%的云南白药溶液,并加入相对于混合溶液溶质质量5%的氯化银。用铝箔包裹棕色磨口瓶,保证完全避光,然后在磁力搅拌器上匀速搅拌2h,待氯化银完全溶解,得到淡黄色的静电纺丝溶液。Mix the above-mentioned polylactic acid solution and chitosan solution at a mass ratio of 1:1 in a brown ground-mouth bottle, then add 10% Yunnan Baiyao solution relative to the quality of the mixed solution, and add 10% of the solute quality relative to the mixed solution 5% silver chloride. Wrap the brown ground-mouth bottle with aluminum foil to ensure that it is completely protected from light, and then stir it on a magnetic stirrer at a constant speed for 2 hours until the silver chloride is completely dissolved to obtain a light yellow electrospinning solution.
控制实验环境温度在20℃-30℃,相对湿度在45%-65%。将配置好的静电纺丝溶液倒入喷射口内径为0.7mm,容量为10ml的注射器中并将注射器固定在注射泵上,注射器喷射口和实验接收板分别连接直流高压电源的正负极,接收板为金属板,在金属接收板上覆盖三层纱布作为基层,接收板和喷丝头之间的距离调节为13cm。实验装置检查无误后打开注射泵调节流速为0.6ml/h,待溶液缓慢流出后打开高压电源并调节电压为15kV,开始纺丝实验。待在接收板棉织物上形成一层膜后,调低关闭电压装置,在接收板上再贴附大小相等的两层纱布,重启电压装置,在第二层膜成型后,调零高压电源并切断电源,然后取下金属接收板上的棉织物并在第二层膜上面覆盖三层纱布,得到医用抗菌纳米敷料。The temperature of the experimental environment is controlled at 20°C-30°C, and the relative humidity is at 45%-65%. Pour the prepared electrospinning solution into a syringe with an inner diameter of 0.7mm and a capacity of 10ml and fix the syringe on the syringe pump. The plate is a metal plate, covered with three layers of gauze as the base layer on the metal receiving plate, and the distance between the receiving plate and the spinneret is adjusted to 13cm. After the experimental device is checked correctly, turn on the syringe pump and adjust the flow rate to 0.6ml/h. After the solution flows out slowly, turn on the high voltage power supply and adjust the voltage to 15kV to start the spinning experiment. After a layer of film is formed on the cotton fabric of the receiving plate, turn down the voltage device, attach two layers of gauze of equal size to the receiving plate, restart the voltage device, and after the second layer of film is formed, adjust the high-voltage power supply to zero and Cut off the power supply, then remove the cotton fabric on the metal receiving plate and cover three layers of gauze on the second layer of film to obtain a medical antibacterial nano dressing.
图2-3是本发明制备的医用抗菌纳米敷料中纳米纤维膜的扫描电镜图,从图中可以看到呈纤维状的纳米纤维,且本发明制备的纳米纤维直径在60nm左右,这些纳米纤维构成了抗菌纳米敷料,由纳米纤维聚集成膜所制得的敷料拥有更好的药物释放效果。图4是本发明制备的医用抗菌纳米敷料在台式电镜能谱仪下扫描银的示意图,图中发光的部分为银,说明本发明的敷料中将银负载入其中,使得敷料的抗菌效果增强。图5是本发明医用抗菌纳米敷料中纳米纤维膜的元素分析结果,从图中可以看到银的峰。图6和图7分别为云南白药和本发明载药纳米纤维膜的红外光谱图,从图中可以看出云南白药在1747,1087,1185处的特征峰在载药纳米纤维膜上均有明显的峰值。证明云南白药存在于载药纳米纤维膜。Fig. 2-3 is the scanning electron micrograph of the nanofiber film in the medical antibacterial nano dressing prepared by the present invention, can see the nanofiber that is fibrous form from the figure, and the diameter of the nanofiber prepared by the present invention is about 60nm, these nanofibers An antibacterial nano dressing is formed, and the dressing made of nanofibers aggregated into a film has a better drug release effect. Fig. 4 is a schematic diagram of the medical antibacterial nano dressing prepared by the present invention scanning silver under a desktop electron microscope energy spectrometer. The luminescent part in the figure is silver, indicating that silver is loaded into the dressing of the present invention, so that the antibacterial effect of the dressing is enhanced. Fig. 5 is the elemental analysis result of the nanofibrous membrane in the medical antibacterial nano dressing of the present invention, and the peak of silver can be seen from the figure. Figure 6 and Figure 7 are the infrared spectrograms of Yunnan Baiyao and the drug-loaded nanofiber membrane of the present invention respectively. It can be seen from the figure that the characteristic peaks of Yunnan Baiyao at 1747, 1087, and 1185 are all obvious on the drug-loaded nanofiber membrane. Peak. It is proved that Yunnan Baiyao exists in the drug-loaded nanofiber membrane.
以上所述仅是本发明的优选实施方式,并不用于限制本发明,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明技术原理的前提下,还可以做出若干改进和变型,这些改进和变型也应视为本发明的保护范围。The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention. It should be pointed out that for those of ordinary skill in the art, some improvements can also be made without departing from the technical principle of the present invention. and modifications, these improvements and modifications should also be considered as the protection scope of the present invention.
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