CN103550816A - Preparation method for chitosan-based electrostatic spinning combined wound dressing - Google Patents
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- 229920001661 Chitosan Polymers 0.000 title claims abstract description 88
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000010041 electrostatic spinning Methods 0.000 title abstract description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 48
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 34
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Abstract
Description
技术领域technical field
本发明属于医用材料领域,具体涉及一种壳聚糖基静电纺丝复合伤口敷料的制备方法。The invention belongs to the field of medical materials, and in particular relates to a preparation method of a chitosan-based electrostatic spinning composite wound dressing.
背景技术Background technique
壳聚糖是天然高分子生物多糖甲壳素脱乙酰化产物,具有优良的耐溶剂性和耐碱性,良好的生物相容性与皮肤亲和性,抑菌性、成膜性、透气性、吸水性、保湿性好,可止血、促进伤口愈合等优点,可用作医学材料。但由于壳聚糖脆性大,力学性能差,使其单独使用受到限制。目前,有大量文献报道壳聚糖与其它高分子共混改性制得性能优良的敷料膜。引入其它高分子较纯壳聚糖膜而言,某些性能会受到影响。静电纺丝技术是实现壳聚糖在医药领域中应用的主要途径之一。但是由于壳聚糖的溶解性小,仅能溶于稀酸水溶液,溶液黏性很高并呈聚阳离子电解质的特性,壳聚糖溶液具有很高的粘度,增加了电纺制备纯壳聚糖纳米纤维膜的难度。纯壳聚糖纳米纤维直径一般在数十纳米到数百纳米之间,其膜具有很高的比表面积,适合做缓释材料。Chitosan is a natural macromolecule biological polysaccharide chitin deacetylation product, has excellent solvent resistance and alkali resistance, good biocompatibility and skin affinity, antibacterial, film-forming, breathable, It has good water absorption and moisturizing properties, can stop bleeding, promote wound healing, etc., and can be used as a medical material. However, due to the high brittleness and poor mechanical properties of chitosan, its use alone is limited. At present, there are a large number of literature reports that chitosan and other polymers are blended and modified to prepare dressing films with excellent properties. The introduction of other polymers will affect some properties compared to the pure chitosan film. Electrospinning technology is one of the main ways to realize the application of chitosan in the field of medicine. However, due to the low solubility of chitosan, it can only be dissolved in dilute acid aqueous solution, and the viscosity of the solution is very high and has the characteristics of polycation electrolyte. Difficulty of nanofibrous membranes. The diameter of pure chitosan nanofibers is generally between tens of nanometers and hundreds of nanometers, and its membrane has a high specific surface area, which is suitable for slow-release materials.
茶树精油,是澳洲互叶白千层叶片经水蒸气蒸馏获得的油性提取物,具有特殊的芳香气味。茶树精油具有显著的抑菌活性和广泛的抗菌谱范围,对常见的革兰氏阳性菌、革兰氏阴性菌和真菌都具有强烈的抑制作用,与化学抑菌剂相比副作用和残留毒性小的独特优势,对皮肤无刺激作用。茶树精油具有净化空气、杀菌、免疫、防腐、提供细胞营养等用途,可以作为安全有效的医用敷料抗菌剂。Tea tree essential oil is an oily extract obtained from the leaves of Melaleuca alternifolia through steam distillation, and has a special aromatic smell. Tea tree essential oil has significant antibacterial activity and a wide range of antibacterial spectrum. It has strong inhibitory effect on common Gram-positive bacteria, Gram-negative bacteria and fungi. Compared with chemical antibacterial agents, the side effects and residual toxicity are small Unique advantage, no irritation to the skin. Tea tree essential oil has the functions of purifying air, sterilizing, immunizing, antisepsis, providing cell nutrition, etc. It can be used as a safe and effective antibacterial agent for medical dressings.
因此,采用含有茶树精油乳滴的壳聚糖乳液作为纺丝液进行静电纺丝,制得精油壳聚糖纤维颗粒膜层,并将其夹于两张高舒适性的壳聚糖膜间制得壳聚糖基静电纺丝复合伤口敷料,具有重要的应用价值和发展前景。Therefore, the chitosan emulsion containing the tea tree essential oil emulsion was used as the spinning solution to carry out electrospinning to obtain the essential oil chitosan fiber particle film layer, which was sandwiched between two high-comfort chitosan films. The obtained chitosan-based electrospun composite wound dressing has important application value and development prospect.
发明内容Contents of the invention
本发明所要解决的技术问题是提供一种壳聚糖基静电纺丝复合伤口敷料的制备方法。The technical problem to be solved by the present invention is to provide a preparation method of chitosan-based electrospun composite wound dressing.
为解决上述技术问题,本发明采用的技术方案如下:In order to solve the problems of the technologies described above, the technical scheme adopted in the present invention is as follows:
一种壳聚糖基静电纺丝复合伤口敷料的制备方法,包括如下步骤:A preparation method of chitosan-based electrospinning composite wound dressing, comprising the steps of:
(1)将茶树精油和卵磷脂在水中混合搅拌均匀,超声分散脱气,制得精油乳液;(1) Mix and stir tea tree essential oil and lecithin in water evenly, and ultrasonically disperse and degas to obtain essential oil emulsion;
(2)将壳聚糖溶于90%的乙酸溶液中,加入甘油作为增塑剂,加入精油乳液,室温搅拌至完全溶解,制得纺丝液;(2) Dissolve chitosan in 90% acetic acid solution, add glycerin as a plasticizer, add essential oil emulsion, stir at room temperature until completely dissolved, and obtain a spinning solution;
(3)将壳聚糖溶于2%的乙酸溶液中,加入甘油作为增塑剂,室温搅拌至完全溶解,制得成膜液,利用流延成膜法制得壳聚糖膜;(3) Dissolve chitosan in 2% acetic acid solution, add glycerin as a plasticizer, stir at room temperature until completely dissolved to obtain a film-forming solution, and use a cast film-forming method to prepare a chitosan film;
(4)将壳聚糖膜包覆在静电纺丝接收板上,利用纺丝液进行静电纺丝,得到精油壳聚糖纤维颗粒层。(4) Coating the chitosan film on the electrospinning receiving plate, and performing electrospinning by using the spinning solution to obtain the chitosan fiber particle layer of essential oil.
(5)静电纺丝完成后,再将一层壳聚糖膜覆盖在精油壳聚糖纤维颗粒层上,在一定温度下压制成型得到壳聚糖基静电纺丝复合伤口敷料。(5) After the electrospinning is completed, a layer of chitosan film is covered on the layer of essential oil chitosan fiber particles, and pressed at a certain temperature to obtain a chitosan-based electrospinning composite wound dressing.
步骤(1)中,茶树精油(ml)、卵磷脂(g)和水(ml)的比例为0.5~1:0.1~0.2:0.5~1.0。In step (1), the ratio of tea tree essential oil (ml), lecithin (g) and water (ml) is 0.5-1:0.1-0.2:0.5-1.0.
步骤(2)和(3)中,壳聚糖的规格为粘均分子量为5.0×105,脱乙酰度为80~85%。In steps (2) and (3), the chitosan has a viscosity-average molecular weight of 5.0×10 5 and a deacetylation degree of 80-85%.
步骤(2)中,壳聚糖的90%乙酸溶液质量浓度为1.5~3%。甘油的加入量为2~4%,精油乳液的加入量为2~4%。In step (2), the mass concentration of chitosan in 90% acetic acid solution is 1.5-3%. The addition amount of glycerin is 2-4%, and the addition amount of essential oil emulsion is 2-4%.
步骤(3)中,壳聚糖的2%乙酸溶液质量浓度为1.5~2.5%。甘油的加入量为2~4%。In step (3), the mass concentration of chitosan in 2% acetic acid solution is 1.5-2.5%. The amount of glycerin added is 2 to 4%.
步骤(4)中,静电纺丝注射器规格为10ml,针头规格为平头,7号针。In step (4), the specification of the electrospinning syringe is 10ml, the specification of the needle is flat head, and the needle is No. 7.
步骤(4)中,静电纺丝条件为,电压12~20KV,距离7~10cm,进样速率0.3~1.0ml/h,温度25~35℃。In step (4), the electrospinning conditions are: voltage 12-20KV, distance 7-10cm, sampling rate 0.3-1.0ml/h, temperature 25-35°C.
步骤(5)中,先用40~50℃压制10s,再用100~120℃压制10s。In step (5), press at 40-50°C for 10s first, and then press at 100-120°C for 10s.
本发明得到的壳聚糖基静电纺丝复合伤口敷料的制备方法,可以作为医用材料、纺织服装材料、抗菌材料等广泛应用于纺织工业、医药保健、生物医学等领域。The preparation method of the chitosan-based electrospinning composite wound dressing obtained in the present invention can be widely used in the fields of textile industry, medicine and health care, biomedicine and the like as medical materials, textile and clothing materials, antibacterial materials, and the like.
有益效果:本发明制备方法与现有技术相比,具有以下优点:Beneficial effect: compared with the prior art, the preparation method of the present invention has the following advantages:
1、本发明的方法操作简单,原材料廉价易得,耗时较少,可在短时间内获得包覆精油乳滴的直径和孔径在纳米级的壳聚糖膜材料;1. The method of the present invention is simple to operate, cheap and easy to get raw materials, less time-consuming, and can obtain the chitosan membrane material with the diameter and aperture of the coated essential oil emulsion droplet in nanoscale in a short time;
2、本发明采用的两大主材均为天然材料:壳聚糖和茶树精油。与其他合成的伤口敷料相比,其生物相容性好,环境友好,不添加过多的助剂、有机溶剂,对人体皮肤也无刺激性。2. The two main materials used in the present invention are natural materials: chitosan and tea tree essential oil. Compared with other synthetic wound dressings, it has good biocompatibility, is environmentally friendly, does not add too many additives, organic solvents, and is non-irritating to human skin.
3、制备的壳聚糖基静电纺丝复合伤口敷料具有一定的植物芳香味,能够一定程度遮盖伤口化脓产生的异味,还能加速消除患者的神经紧张,缓解压力,愉悦心情,满足人们精神上的享受;3. The prepared chitosan-based electrospinning composite wound dressing has a certain plant aroma, which can cover the peculiar smell produced by wound suppuration to a certain extent, and can also accelerate the elimination of nervous tension of patients, relieve pressure, delight the mood, and satisfy people's spiritual needs. enjoyment;
4、壳聚糖基静电纺丝复合伤口敷料外层采用经过塑化处理的壳聚糖膜,在支持精油壳聚糖纤维颗粒层的同时,其舒适性也大大提高,使敷料更加贴合皮肤。4. The outer layer of chitosan-based electrospun composite wound dressing adopts the plasticized chitosan film, which not only supports the chitosan fiber particle layer of essential oil, but also greatly improves its comfort, making the dressing more suitable for the skin .
附图说明Description of drawings
图1是本发明的原理示意图。Fig. 1 is a schematic diagram of the principle of the present invention.
具体实施方式Detailed ways
根据下述实施例,可以更好地理解本发明。然而,本领域的技术人员容易理解,实施例所描述的内容仅用于说明本发明,而不应当也不会限制权利要求书中所详细描述的本发明。The present invention can be better understood from the following examples. However, those skilled in the art can easily understand that the content described in the embodiments is only for illustrating the present invention, and should not and will not limit the present invention described in the claims.
实施例1:Example 1:
一种壳聚糖基静电纺丝复合伤口敷料的制备方法,包括如下步骤:A preparation method of chitosan-based electrospinning composite wound dressing, comprising the steps of:
(1)将0.5ml茶树精油和0.1g卵磷脂在0.5ml水中混合搅拌均匀,超声分散脱气,制得精油乳液;(1) Mix 0.5ml tea tree essential oil and 0.1g lecithin in 0.5ml water and stir evenly, and ultrasonically disperse and degas to obtain an essential oil emulsion;
(2)将0.75g壳聚糖(粘均分子量为5.0×105,脱乙酰度为80~85%)溶于50ml90%的乙酸溶液中,加入1ml甘油作为增塑剂,加入1ml精油乳液,室温搅拌至完全溶解,制得纺丝液;(2) Dissolve 0.75g chitosan (viscosity average molecular weight 5.0×10 5 , deacetylation degree 80-85%) in 50ml 90% acetic acid solution, add 1ml glycerin as plasticizer, add 1ml essential oil emulsion, Stir at room temperature until completely dissolved to obtain a spinning solution;
(3)将1g壳聚糖溶于50ml2%的乙酸溶液中,加入1ml甘油作为增塑剂,室温搅拌至完全溶解,制得成膜液,利用流延成膜法制得壳聚糖膜,揭下备用;(3) Dissolve 1g of chitosan in 50ml of 2% acetic acid solution, add 1ml of glycerin as a plasticizer, stir at room temperature until completely dissolved to obtain a film-forming liquid, and use the cast film-forming method to prepare a chitosan film, uncover next standby;
(4)将壳聚糖膜包覆在静电纺丝接收板上,用10ml注射器(7#平头针)抽取纺丝液,固定在静电纺丝装置上,固定静电压20KV,接收距离为7cm,进样速率为0.3ml/h,在温度25℃下进行电纺,得到精油壳聚糖纤维颗粒层。(4) Coat the chitosan film on the electrospinning receiving plate, extract the spinning solution with a 10ml syringe (7# flat needle), and fix it on the electrospinning device with a fixed static voltage of 20KV and a receiving distance of 7cm. The injection rate was 0.3ml/h, and the electrospinning was carried out at a temperature of 25°C to obtain the chitosan fiber particle layer of essential oil.
(5)静电纺丝完成后,再将一层壳聚糖膜覆盖在精油壳聚糖纤维颗粒层上,先用50℃压制10s,再用120℃压制10s,得到壳聚糖基静电纺丝复合伤口敷料。(5) After the electrospinning is completed, a layer of chitosan film is covered on the chitosan fiber particle layer of essential oil, first pressed at 50°C for 10s, and then pressed at 120°C for 10s to obtain chitosan-based electrospinning Composite wound dressing.
实施例2:Example 2:
一种壳聚糖基静电纺丝复合伤口敷料的制备方法,包括如下步骤:A preparation method of chitosan-based electrospinning composite wound dressing, comprising the steps of:
(1)将1ml茶树精油和0.2g卵磷脂在1ml水中混合搅拌均匀,超声分散脱气,制得精油乳液;(1) Mix 1ml of tea tree essential oil and 0.2g of lecithin in 1ml of water and stir evenly, and ultrasonically disperse and degas to obtain an essential oil emulsion;
(2)将1.5g壳聚糖(粘均分子量为5.0×105,脱乙酰度为80~85%)溶于50ml90%的乙酸溶液中,加入2ml甘油作为增塑剂,加入2ml精油乳液,室温搅拌至完全溶解,制得纺丝液;(2) Dissolve 1.5g chitosan (viscosity average molecular weight 5.0×10 5 , deacetylation degree 80-85%) in 50ml 90% acetic acid solution, add 2ml glycerin as plasticizer, add 2ml essential oil emulsion, Stir at room temperature until completely dissolved to obtain a spinning solution;
(3)将1.25g壳聚糖溶于50ml2%的乙酸溶液中,加入2ml甘油作为增塑剂,室温搅拌至完全溶解,制得成膜液,利用流延成膜法制得壳聚糖膜,揭下备用;(3) Dissolve 1.25g of chitosan in 50ml of 2% acetic acid solution, add 2ml of glycerin as a plasticizer, stir at room temperature until completely dissolved to obtain a film-forming liquid, and use the cast film-forming method to prepare a chitosan film. Take off the spare;
(4)将壳聚糖膜包覆在静电纺丝接收板上,用10ml注射器(7#平头针)抽取纺丝液,固定在静电纺丝装置上,固定静电压12KV,接收距离为10cm,进样速率为1ml/h,在温度35℃下进行电纺,得到精油壳聚糖纤维颗粒层。(4) Coat the chitosan film on the electrospinning receiving plate, extract the spinning solution with a 10ml syringe (7# flat needle), and fix it on the electrospinning device with a fixed static voltage of 12KV and a receiving distance of 10cm. The injection rate was 1ml/h, and the electrospinning was performed at a temperature of 35°C to obtain the chitosan fiber particle layer of essential oil.
(5)静电纺丝完成后,再将一层壳聚糖膜覆盖在精油壳聚糖纤维颗粒层上,先用40℃压制10s,再用110℃压制10s,得到壳聚糖基静电纺丝复合伤口敷料。(5) After the electrospinning is completed, a layer of chitosan film is covered on the chitosan fiber particle layer of essential oil, first pressed at 40°C for 10s, and then pressed at 110°C for 10s to obtain chitosan-based electrospinning Composite wound dressing.
实施例3:Example 3:
一种壳聚糖基静电纺丝复合伤口敷料的制备方法,包括如下步骤:A preparation method of chitosan-based electrospinning composite wound dressing, comprising the steps of:
(1)将0.75ml茶树精油和0.15g卵磷脂在0.75ml水中混合搅拌均匀,超声分散脱气,制得精油乳液;(1) Mix 0.75ml tea tree essential oil and 0.15g lecithin in 0.75ml water and stir evenly, and ultrasonically disperse and degas to prepare essential oil emulsion;
(2)将1g壳聚糖(粘均分子量为5.0×105,脱乙酰度为80~85%)溶于50ml90%的乙酸溶液中,加入1.5ml甘油作为增塑剂,加入1.5ml精油乳液,室温搅拌至完全溶解,制得纺丝液;(2) Dissolve 1g chitosan (viscosity average molecular weight: 5.0×10 5 , deacetylation degree: 80-85%) in 50ml 90% acetic acid solution, add 1.5ml glycerin as plasticizer, add 1.5ml essential oil emulsion , stirred at room temperature until completely dissolved to obtain a spinning solution;
(3)将0.75g壳聚糖溶于50ml2%的乙酸溶液中,加入0.75ml甘油作为增塑剂,室温搅拌至完全溶解,制得成膜液,利用流延成膜法制得壳聚糖膜,揭下备用;(3) Dissolve 0.75g of chitosan in 50ml of 2% acetic acid solution, add 0.75ml of glycerin as a plasticizer, stir at room temperature until completely dissolved to obtain a film-forming solution, and use the cast film-forming method to prepare a chitosan film , take off the spare;
(4)将壳聚糖膜包覆在静电纺丝接收板上,用10ml注射器(7#平头针)抽取纺丝液,固定在静电纺丝装置上,固定静电压15KV,接收距离为8cm,进样速率为0.5ml/h,在温度30℃下进行电纺,得到精油壳聚糖纤维颗粒层。(4) Cover the chitosan film on the electrospinning receiving plate, draw the spinning solution with a 10ml syringe (7# flat needle), fix it on the electrospinning device, fix the static voltage at 15KV, and the receiving distance is 8cm, The injection rate was 0.5ml/h, and the electrospinning was carried out at a temperature of 30°C to obtain the chitosan fiber particle layer of essential oil.
(5)静电纺丝完成后,再将一层壳聚糖膜覆盖在精油壳聚糖纤维颗粒层上,先用45℃压制10s,再用100℃压制10s,得到壳聚糖基静电纺丝复合伤口敷料。(5) After the electrospinning is completed, a layer of chitosan film is covered on the chitosan fiber particle layer of essential oil, first pressed at 45°C for 10s, and then pressed at 100°C for 10s to obtain chitosan-based electrospinning Composite wound dressing.
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