CN113069587B - 一种透湿、止血、抗菌伤口敷料及其制备方法 - Google Patents
一种透湿、止血、抗菌伤口敷料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种透湿、止血、抗菌伤口敷料及其制备方法,属于医疗技术领域。本发明首先合成了新型季铵盐抗菌剂QAS18,然后将该季铵盐抗菌剂接枝到ZnO纳米颗粒表面,制备成ZnO‑QAS18颗粒,之后通过静电纺丝以及喷涂zein蛋白和ZnO‑QAS18颗粒方式制备得到了伤口敷料。本发明的伤口敷料透湿性良好、具有一定的止血能力且抗菌效果显著,生物相容性良好,制备过程便捷、无污染。
Description
技术领域
本发明涉及一种透湿、止血、抗菌伤口敷料及其制备方法,属于医疗技术领域。
背景技术
微生物引起的伤口感染问题一直威胁着人类的健康,由于细菌等病原体引起的伤口感染常导致化脓、炎症等问题,伤口处细菌感染严重时如果得不到及时有效的处理甚至会造成机体死亡。在自然环境中,皮肤受损后很容易受到细菌等微生物的入侵,因此及时的处理伤口可以很大程度的避免感染。
Zein是玉米中的主要贮藏蛋白,储量丰富且来源广泛,作为一种天然的植物蛋白质,zein具有良好的生物相容性和可降解特性。Zein分子链中富含含硫氨基酸和疏水性氨基酸,所以zein分子链间容易形成二硫键和疏水键,这也使得zein分子具有一定的自组装(self-assembly)特性。Zein已经被证明有利于促进细胞生长和组织再生,因此在生物医用领域中受到了越来越多的关注。
ZnO颗粒和季铵盐抗菌剂目前在临床上已经得到了广泛的应用,但是也存在着部分问题,比如ZnO颗粒抗菌效果较弱,季铵盐类抗菌剂抗菌能力显著但是对生物具有一定的细胞毒性。此外,研究表明ZnO颗粒具有一定的体外凝血效果,可以作为伤口处的止血材料,而季铵盐抗菌剂由于具有带正电荷的季铵基团,对血浆中的红细胞具有一定的吸附作用,因此可以促进血液的凝固。
因此,作为伤口敷料,应该首先具有抗菌、止血的效果,同时,敷料的透湿特性也尤为重要,具有良好透湿特性的敷料可以保持伤口处干燥的微环境,有助于伤口组织的愈合、防止细菌等微生物的滋生和防止伤口细胞脱水。
总之,伤口敷料应该具备多项特征保护受损的皮肤,促进伤口的愈合。
发明内容
为了解决上述透湿、止血、抗菌的问题,本发明提供了一种以纳米纤维为基材的伤口敷料的制备方法。本发明合成了新型季铵盐抗菌剂QAS18,然后将该季铵盐抗菌剂接枝到ZnO纳米颗粒表面,制备成ZnO-QAS18颗粒,之后通过静电纺丝以及喷涂zein蛋白的方式制备得到了伤口敷料。本发明的伤口敷料透湿性良好、具有一定的止血能力且抗菌效果显著,生物相容性良好,制备过程便捷、无污染。
具体的,本发明首先提供了一种透湿、止血、抗菌伤口敷料的制备方法,所述方法包括以下步骤:
(1)制备季铵盐抗菌剂QAS18:将N,N-二甲基乙醇胺(DMEA)、异氰酸丙基三乙氧基硅烷(IPTS)、二月桂酸二丁基锡(DBEU)以及溶剂DMF加入到反应容器中,惰性氛围下80~100℃反应18~24h,之后加入1-溴十八烷和碘化钾(KI),惰性氛围下升温至110~120℃继续反应18~24h,之后过滤、旋蒸、提纯、干燥后即制备得到季铵盐抗菌剂QAS18;
(2)制备ZnO-QAS18颗粒:将ZnO分散在乙醇中制得ZnO悬浮液,将同等质量的步骤(1)制备得到的QAS18溶解于乙醇中制得QAS18溶液,再将两者混合,然后加水后95~105℃冷凝回流18~24h,之后抽滤、提取、干燥即可得到ZnO-QAS18颗粒;
(3)配制得到浓度为15wt%的聚己内酯(PCL)纺丝液,溶剂为甲酸,进行静电纺丝,干燥后得到PCL纤维膜;
(4)喷涂zein和ZnO-QAS18:配制得到5wt%的zein溶液,溶剂为75wt%的乙醇溶液,利用喷雾瓶将溶解好的zein溶液均匀喷涂在步骤(3)得到的PCL纤维膜表面,之后干燥得到PCL/zein膜;再配制5mg/mL的ZnO-QAS18乙醇分散液,利用喷雾瓶将ZnO-QAS18乙醇分散液均匀喷涂在PCL/zein膜表面,干燥即可。
在本发明的一种实施方式中,步骤(1)中,所述N,N-二甲基乙醇胺(DMEA)、异氰酸丙基三乙氧基硅烷(IPTS)和1-溴十八烷的摩尔比为5:6:5。
在本发明的一种实施方式中,步骤(1)中,所述二月桂酸二丁基锡(DBEU)的加入量为反应体系中DMEA摩尔量的0.5~1%,所述碘化钾(KI)的加入量为反应体系中DMEA摩尔量的0.5~1%。
在本发明的一种实施方式中,步骤(1)中,所述提纯是利用乙酸乙酯进行提纯。
在本发明的一种实施方式中,步骤(1)中,所述惰性氛围是指氮气、氩气氛围的任一种或两种。
在本发明的一种实施方式中,步骤(2)中,加入的水的量为反应体系体积的1~2%。
在本发明的一种实施方式中,步骤(2)中,所述提取是利用索氏提取器进行提取,乙醇作为溶剂,回流8~12h。
在本发明的一种实施方式中,步骤(3)中,配制聚己内酯(PCL)纺丝液的具体过程为:将聚己内酯PCL颗粒加入到甲酸中,水浴下超声溶解0.5~1.5h后室温下搅拌4~6h即得到PCL纺丝液。
在本发明的一种实施方式中,步骤(3)中,静电纺丝的工艺参数为:电压20kV,注射速率0.5mL/h,环境温度20~25℃,相对湿度40-50%,纺丝距离15cm,滚筒转速100rpm/min。
在本发明的一种实施方式中,步骤(3)中,所述干燥优选在45℃真空干燥24h。
在本发明的一种实施方式中,步骤(4)中,喷涂的操作参数为:氮气出口压力为0.2MPa,持续时间30s。
本发明还提供了上述制备方法制备得到的透湿、止血、抗菌伤口敷料。
本发明还提供了包含上述透湿、止血、抗菌伤口敷料的医疗器械。
本发明的有益效果:
(1)本发明合成了新型季铵盐抗菌剂QAS18,并将其成功接枝到ZnO纳米颗粒表面,采用氮气载流喷雾的方式将zein和ZnO-QAS18均匀喷涂于PCL纳米纤维垫表面,制备过程简单、环保。
(2)该敷料以静电纺纳米纤维垫为基材,表面喷涂一层zein薄膜和功能性纳米颗粒,透湿性良好。
(3)该敷料可以吸附血液中的纤连蛋白和红细胞,刺激血小板响应,且血细胞相容性良好,具有良好的止血能力。
(4)该敷料可以在30min内杀灭6.01log的金黄色葡萄球菌,1h内杀灭6.04log的大肠肝菌,具有良好的抗菌能力。
(5)该敷料在使用过程中没有生物毒性,且zein的引入有利于受损皮肤处的细胞生长。
(6)该敷料轻薄,外侧表面是多孔PCL纳米纤维,有一定的疏水、抵御外部细菌黏附的能力。
附图说明
图1为季铵盐QAS18的合成路线。
图2为ZnO-QAS18合成路线。
图3为静电纺装置示意图。
图4为zein溶液喷雾涂覆和纳米颗粒分散液喷雾涂覆示意图。
图5为水蒸气透过率结果,A,B,C,D分别表示实施例2制备得到的样品PCL,PCL/zein,PCL/zein/ZnO以及实施例3制备得到的PCL/zein/ZnO-QAS18。
图6为血液测试结果,PCL,其中,图a为实施例2制备得到的PCL/zein,PCL/zein/ZnO以及实施例3制备得到的PCL/zein/ZnO-QAS18敷料的BCI值以及血液凝固的实际图片;图b为PCL/zein/ZnO-QAS18样品表面的红细胞观察;图c为PCL/zein/ZnO-QAS18样品的血小板黏附测试;图d为PCL,PCL/zein,PCL/zein/ZnO,PCL/zein/ZnO-QAS18敷料的血细胞相容性。
图7为抗菌测试和细胞相容性测试结果,其中,图a为实施例2制备得到的PCL/zein,PCL/zein/ZnO以及实施例3制备得到的PCL/zein/ZnO-QAS18敷料的抗菌测试结果,测试菌种为S.aureus和E.coli O157:H7;图b为细胞毒性测试,A为对照组,B,C,D,E分别为实施例2制备得到的PCL,PCL/zein,PCL/zein/ZnO以及实施例3制备得到的PCL/zein/ZnO-QAS18样品。
具体实施方式
各种测试方法如下:
水蒸气透过率测试:样品的水蒸气透过率(WVTR)根据ASTM E96标准方法测定。准备4个圆柱型玻璃瓶,瓶口面积为1.44cm2,瓶中装有10mL去离子水,用不同的样品将每个玻璃瓶的瓶口密封,边缘用封口膜封住防止水分的流失。样品为实施例制备得到的膜。将所用玻璃瓶放置于37℃恒温培养箱中。定时测量玻璃瓶的重量,重量变化代表了水分的流失,水蒸气透过率(WVTR)按公式(1)计算:
其中Wloss表示24h水分的减少量,A表示玻璃瓶瓶口的面积。
全血凝固测试:样品的凝血效果根据血液凝固指数(BCI)作为测定标准。将样品裁剪成1cm×1cm的正方形并放入培养皿中,于37℃恒温振荡箱中预热5min,取100μL小兔全血缓慢滴加到预热后的样品表面,随后滴加10mL CaCl2溶液(0.2N)中和血液中的抗凝剂。5min后沿培养皿的边缘缓慢加入25mL去离子水,以30rpm的速度摇晃10min,此时没有被凝固的血红细胞会发生溶血现象。所得的血红蛋白溶液于540nm处测定其紫外吸光度(ABSsample)。全血溶于去离子水中的紫外吸光度作为对照样(ABSblank)。所得样品的BCI按公式(2)计算:
为了进一步观察血红细胞在样品表面的附着情况,将测试后的样品在2.5wt%戊二醛/PBS溶液中浸泡2h以固定,然后采用不同浓度梯度的乙醇/PBS溶液(25%,50%,75,85%,90%,95%,100%)对样品上的血细胞进行脱水。45℃干燥24h用于SEM观察。
血小板黏附测试:取40mL抗凝兔全血进行离心(1500rpm,20min)分离得到富含血小板的血浆(PRP)。将1cm×1cm的正方形样品于37℃下预热5min,然后在3mL 37℃的PRP中浸泡1h。浸泡后的样品用PBS溶液冲洗3次并在2.5wt%戊二醛/PBS溶液中浸泡2h。采用不同浓度梯度的乙醇/PBS溶液(25%,50%,75,85%,90%,95%,100%)对血小板进行脱水。随后将样品放置于45℃干燥24h用于SEM观察。
溶血测试:根据文献中报道的方法进行溶血测试。取抗凝小兔全血与PBS溶液以4:5的体积比混合稀释。将1cm×1cm的样品放置于装有10mL PBS溶液的离心管中,37℃恒温培养30min,然后加入0.2mL稀释的抗凝血液,继续培养1h。培育完成后先倒置离心管使内部混合均匀,然后以3000rpm的速率离心5min。收集上清液测量其在540nm处的吸光度,根据公式(3)计算溶血率:
式中A1表示样品组上清液的吸光度,A2表示PBS溶液的吸光度,A3表示去离子水的吸光度。
抗菌测试:根据改良的AATCC 100-2004方法测试了样品对革兰氏阳性金黄色葡萄球菌(ATCC 6538)和革兰氏阴性大肠杆菌(ATCC 43895)的抗菌性能。取25μL细菌悬浮液(1×106CFU/mL)滴加在两块样品膜(2.54cm×2.54cm)之间,并用无菌砝码压紧以确保良好接触。在接触5min、10min、30和60min后,将样品转移到无菌试管中涡旋250s洗脱细菌。随后,取上述洗脱液连续稀释10、100、1000倍,并将每种稀释液100μL均匀滴加在胰蛋白酶琼脂平板上,于37℃恒温培养24h,计算杀菌率。
生物相容性测试:根据ISO 10993-5的XTT细胞相容性测试方法评估了样品对小鼠成纤细胞(L 929)存活率的影响。将L-929细胞置于含10%FBS和1%青霉素-链霉素溶液的DMEM培养基中,5%CO2分为中37℃复苏细胞。将复苏的细胞用胰蛋白酶消化,然后将细胞悬液接种到96孔板中,培养24h。24h后将培养基替换为样品的液体提取物并继续培养24h。之后向每个孔中加入50μL XTT/PMS试剂,并于黑暗中于37℃培养4h。测量每个孔在450nm处的OD值来显示细胞活力,空白培养基作为对照。
原料来源:N,N-二甲基乙醇胺(DMEA,98%),3-异氰酸根合丙基三乙氧基硅烷(IPTS,95%),二月桂酸二丁锡(DBDU,95%)购自上海阿拉丁试剂公司,聚己内酯(PCL,Mn=80kDa)购自美国圣路易斯Sigma-Aldrich公司,ZnO(OD=80nm,99.9%)购自北京德科道金科技有限公司,玉米蛋白Zein,购自1-溴十八烷购自百灵威科技有限公司。其他化学试剂购自国药控股化学试剂有限公司。以上所有试剂按原样使用,无需进一步纯化。
下面结合实施例对本发明作进一步的描述,但本发明的实施方式不限于此。
实施例1
QAS18的制备:称取20mmol的N,N-二甲基乙醇胺(DMEA),24mmol异氰酸丙基三乙氧基硅烷(IPTS)以及DMEA摩尔量的1%的二月桂酸二丁基锡(DBEU)在室温下加入三口烧瓶,溶剂为DMF,在氮气氛围下90℃反应24h。24h后向体系中加入20mmol的1-溴十八烷和DMEA摩尔量的1%碘化钾(KI)升温至120℃继续反应24h,保持氮气氛围。反应后混合物经布氏漏斗过滤,将滤液旋蒸得到粗产物。经乙酸乙酯提纯、干燥得到季铵盐产物QAS18。
QAS18的化学反应方程式及其结构式见图1。
ZnO-QAS18颗粒的制备:称取1g的ZnO粉末在乙醇中超声分散30min,称取等质量制备的QAS18溶解于乙醇中,然后将分散好的ZnO悬浮液和QAS18溶液混合,滴加少量去离子水,100℃冷凝回流24h。24h后抽滤,将所得固体用滤纸包裹,置于索氏提取器中,选择乙醇作为溶剂回流12h,干燥,得到产物ZnO-QAS18。
ZnO-QAS18的合成步骤见图2。
实施例2
(1)称取1.5g PCL固体加入到8.5g甲酸中,超声溶解1h后室温下搅拌6h得到15wt%的PCL纺丝液,静电纺工艺参数:电压20kV,注射速率0.5mL/h,室温,相对湿度40-50%,纺丝距离15cm,滚筒转速100rpm/min。纺丝完成后放入45℃真空干燥箱干燥24h,得到纯的PCL纳米纤维垫,标记为PCL。
(2)称取2g zein粉末超声溶解于38g 75wt%的乙醇/水溶液中,配置成5wt%的zein溶液,利用喷雾瓶将溶解好的zein溶液均匀喷涂在PCL纤维膜表面,氮气瓶出口压力设置为0.2Mpa,持续时间为30s,干燥12h,该敷料标记为PCL/zein。
(3)称取50mg ZnO超声分散在10mL乙醇中,利用喷雾瓶喷均匀涂在步骤(2)的PCL/zein表面,氮气出口压力为0.2MPa,持续时间30s,干燥12h,该敷料标记为PCL/zein/ZnO。
实施例3
步骤(1)和(2)同实施例2;
(3)称取50mg实施例1制备的ZnO-QAS18超声分散在10mL乙醇中,利用喷雾瓶喷均匀涂在步骤(2)的PCL/zein表面,氮气出口压力为0.2MPa,持续时间30s,干燥12h,该敷料标记为PCL/zein/ZnO-QAS18。
对实施例2和3制备得到的样品进行性能测试,结果如下:
实施例2制备得到的样品PCL,PCL/zein,PCL/zein/ZnO以及实施例3制备得到的PCL/zein/ZnO-QAS18敷料的水蒸气透过量如图5所示,分别对应水蒸气透过量为3683±28mL/m2/day,3589±52mL/m2/day,3561±42mL/m2/day,3533±93mL/m2/day。可以看出经过zein和ZnO-QAS18涂覆的纤维垫仍然具有良好的透湿性。通常正常皮肤的水蒸气透过率为204mL/m2/day,损伤的皮肤表面水蒸气透过量应该控制为279mL/m2/day到5138mL/m2/day,4类样品的水蒸气透过率均在此范围类,可以看出实施例3得到的PCL/zein/ZnO-QAS18敷料的透湿性既可以保持伤口处相对干燥的微环境,也可以防止伤口细胞脱水。
全血凝固指数(BCI)测试、血小板黏附测试、溶血测试结果如图6所示。图a表示实施例2制备得到的PCL,PCL/zein,PCL/zein/ZnO和实施例3制备得到的PCL/zein/ZnO-QAS18敷料的BCI值以及血液凝固的图片。BCI值是描述血液凝固特性的参数,BCI值越低表示材料的凝血性能越好,图a中PCL,PCL/zein,PCL/zein/ZnO,PCL/zein/ZnO-QAS18敷料的BCI值依次降低,经过zein喷涂后凝血性能提高,这是由于PCL纤维垫表面的zein膜可以吸附血液中的纤连蛋白和血小板,使纤连蛋白和血小板发生聚集从而促进血凝块的形成,ZnO的加入也可以提高材料的凝血性能,ZnO-QAS18颗粒表面带有含正电荷的季铵盐基团,也可以提高其对红细胞的吸附能力,使得凝血性能进一步提高,从凝血图片可以看出随着BCI值得降低,样品表面具有更加明显的血块凝集。
为了进一步探究止血机制,利用SEM对血凝块和血小板的形态进行了观察(图b,c),可以看出全血凝固后大量的血细胞被纤维蛋白固定,此时的红细胞由于在实验中吸水形态变成球型。图c中可以观察到黏附在敷料表面的血小板变得不规则,有多个方向的突起,证明此时的血小板处于激活状态,证明PCL/zein/ZnO-QAS18敷料可以促使血液中的血小板活化,达到凝血的效果。为了测试样品的学细胞相容性,对PCL,PCL/zein,PCL/zein/ZnO,PCL/zein/ZnO-QAS18敷料进行了溶血测试(图d),结果表明PCL/zein/ZnO-QAS18敷料具有最高的溶血百分率,为0.98%。一般生物医用材料的溶血百分率要求≤5%,因此可以认为PCL/zein/ZnO-QAS18敷料对血红细胞损害小,具有良好的血细胞相容性。以上测试结果表明,PCL/zein/ZnO-QAS18敷料可以激活血小板并促进血凝块的形成,因此该材料具有良好的止血性能。
抗菌测试、细胞相容性测试结果如图7所示。PCL/zein,PCL/zein/ZnO,PCL/zein/ZnO-QAS18敷料的抗菌测试结果如图7a所示,测试菌种为革兰氏阳性金黄色葡萄球菌S.aureus(ATCC 6538)和革兰氏阴性大肠肝菌E.coli O157:H7(ATCC 43895)。PCL/zein样品作为空白组,PCL/zein/ZnO,PCL/zein/ZnO-QAS18样品作为对照组,接种60min后,PCL/zein样品分别对S.aureus和E.coli O157:H7造成0.41log和0.2log的降低,导致这一数据的原因可能是样品表面对细菌的黏附而不是样品本身对细菌的杀灭作用。从PCL/zein/ZnO样品的杀菌数据图中可以看出,接种60min后PCL/zein/ZnO样品分别对S.aureus和E.coliO157:H7造成2.58log和1.14log的降低,与PCL/zein样品相比,它的抗菌性能提高,这是由于ZnO颗粒在中性条件下具有部分正电性,可以通过其表面的静电相互作用吸引带负电的细菌,破坏细菌的细胞膜结构,进而抑制细菌的增殖。从PCL/zein/ZnO-QAS18样品的测试数据图中可以看出,PCL/zein/ZnO-QAS18抗菌样可以在接种30min内全部杀死S.aureus,接种60min可以全部杀死E.coli O157:H7。与PCL/zein和PCL/zein/ZnO样品相比,PCL/zein/ZnO-QAS18样品的抗菌性能显著提高,这是由于表面接枝了季铵盐QAS18的纳米ZnO颗粒正电性变强,对细菌的吸附作用更明显,同时,由于季铵盐本身具有破坏细菌细胞膜的作用,从而使得表面接枝有QAS18的ZnO杂化颗粒抗菌效果更佳显著。从图a中还可以看出,与S.aureus相比,E.coli O157:H7更难被杀死,这可能是因为E.coli O157:H7具有更复杂的细胞壁结构,而S.aureus的细胞壁更为简单。以上数据表明,PCL/zein/ZnO-QAS18敷料具有优异的抗菌性能。
PCL/zein,PCL/zein/ZnO,PCL/zein/ZnO-QAS18敷料的细胞相容性测试如图7b所示,与对照组A相比,PCL样品的细胞存活率基本不变,而PCL/zein样品的细胞存活率提高,这是因为zein可以提高小鼠细胞的黏附能力,促进其增殖。ZnO颗粒和ZnO-QAS18颗粒喷涂在zein表面后,它们的细胞存活率分别降低为81%和74%,根据ISO/EN 10993-5:2009的最低细胞活力标准为70%,所以仍然可以认为PCL/zein/ZnO和PCL/zein/ZnO-QAS18样品不具有细胞毒性。因此,PCL/zein/ZnO-QAS18敷料可以作为生物相容性材料应用于医用领域。
实施例4
(1)称取1.5g PCL固体加入到8.5g甲酸中,超声溶解1h后室温下搅拌6h得到15wt%的PCL纺丝液,静电纺工艺参数:电压20kV,注射速率0.5mL/h,室温,相对湿度40-50%,纺丝距离15cm,滚筒转速100rpm/min。纺丝完成后放入45℃真空干燥箱干燥24h,得到纯的PCL纳米纤维垫,标记为PCL。
(2)称取50mg ZnO超声分散在10mL 5wt%的zein溶液中,利用喷雾瓶喷均匀涂在步骤(1)的PCL表面,氮气出口压力为0.2MPa,持续时间30s,干燥12h,该敷料标记为PCL/zein/ZnO*。
实施例5
步骤(1)同实施例4步骤(1);
(2)称取50mg实施例1制备的ZnO-QAS18超声分散在10mL 5wt%的zein溶液中,利用喷雾瓶喷均匀涂在步骤(1)的PCL表面,氮气出口压力为0.2MPa,持续时间30s,干燥12h,该敷料标记为PCL/zein/ZnO-QAS18*。
经过实施例3的测试可以发现,实施例4和5制备得到的PCL/zein/ZnO*和PCL/zein/ZnO-QAS18*样品抗菌、止血效果较实施例2制备得到的PCL/zein/ZnO和实施例3制备得到的PCL/zein/ZnO-QAS18样品均明显减弱,但是其水蒸气通过率和生物相容性分别和实施例2制备得到的PCL/zein/ZnO和实施例3制备得到的PCL/zein/ZnO-QAS18样品基本一致。
虽然本发明已以较佳实施例公开如上,但其并非用以限定本发明,任何熟悉此技术的人,在不脱离本发明的精神和范围内,都可做各种的改动与修饰,因此本发明的保护范围应该以权利要求书所界定的为准。
Claims (10)
1.一种透湿、止血、抗菌伤口敷料的制备方法,其特征在于,所述方法包括以下步骤:
(1)制备季铵盐抗菌剂QAS18:将N,N-二甲基乙醇胺(DMEA)、异氰酸丙基三乙氧基硅烷(IPTS)、二月桂酸二丁基锡(DBEU)以及溶剂DMF加入到反应容器中,惰性氛围下80~100℃反应18~24h,之后加入1-溴十八烷和碘化钾(KI),惰性氛围下升温至110~120℃继续反应18~24h,之后过滤、旋蒸、提纯、干燥后即制备得到季铵盐抗菌剂QAS18;
(2)制备ZnO-QAS18颗粒:将ZnO分散在乙醇中制得ZnO悬浮液,将同等质量的步骤(1)制备得到的QAS18溶解于乙醇中制得QAS18溶液,再将两者混合,然后加水后95~105℃冷凝回流18~24h,之后抽滤、提取、干燥即可得到ZnO-QAS18颗粒;
(3)配制得到浓度为15wt%的聚己内酯(PCL)纺丝液,溶剂为甲酸,进行静电纺丝,干燥后得到PCL纤维膜;
(4)喷涂zein和ZnO-QAS18:配制得到5wt%的zein溶液,溶剂为75wt%的乙醇溶液,利用喷雾瓶将溶解好的zein溶液均匀喷涂在步骤(3)得到的PCL纤维膜表面,之后干燥得到PCL/zein膜;再配制5mg/mL的ZnO-QAS18乙醇分散液,利用喷雾瓶将ZnO-QAS18乙醇分散液均匀喷涂在PCL/zein膜表面,干燥即可。
2.根据权利要求1所述的制备方法,其特征在于,步骤(1)中,所述N,N-二甲基乙醇胺(DMEA)、异氰酸丙基三乙氧基硅烷(IPTS)和1-溴十八烷的摩尔比为5:6:5。
3.根据权利要求1所述的制备方法,其特征在于,步骤(1)中,所述二月桂酸二丁基锡(DBEU)的加入量为反应体系中DMEA摩尔量的0.5~1%,所述碘化钾(KI)的加入量为反应体系中DMEA摩尔量的0.5~1%。
4.根据权利要求1所述的制备方法,其特征在于,步骤(1)中,所述惰性氛围是指氮气、氩气氛围的任一种或两种。
5.根据权利要求1所述的制备方法,其特征在于,步骤(3)中,静电纺丝的工艺参数为:电压20kV,注射速率0.5mL/h,环境温度20~25℃,相对湿度40-50%,纺丝距离15cm,滚筒转速100rpm/min。
6.根据权利要求1所述的制备方法,其特征在于,喷涂的操作参数为:氮气出口压力为0.2MPa,持续时间30s。
7.根据权利要求1所述的制备方法,其特征在于,步骤(3)中,所述干燥为在45℃真空干燥24h。
8.权利要求1~7任一项所述的制备方法制备得到的透湿、止血、抗菌伤口敷料。
9.包含权利要求8所述的透湿、止血、抗菌伤口敷料的医疗器械。
10.权利要求8所述的透湿、止血、抗菌伤口敷料在医疗行业中的应用。
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