CN112706477A - 一种蒲公英绒毛基抗菌止血敷料 - Google Patents
一种蒲公英绒毛基抗菌止血敷料 Download PDFInfo
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Abstract
本发明公开了一种蒲公英绒毛基抗菌止血敷料及其制备方法，首先以醛基化的蒲公英绒毛和粘胶纤维为原料制成了无纺布，再利用壳聚糖和魔芋葡甘露聚糖混合液作为整理液进行后整理获得，整理液采用化学交联的的方式稳定负载于醛基化的蒲公英绒毛/粘胶纤维无纺上；使本发明的敷料不仅具有良好的机械强度、透气性、吸液性；还具有抗菌止血和促伤口愈合作用，在医用敷料应用领域具有广泛的应用前景。
Description
技术领域
本发明属于医疗用品领域，具体涉及一种蒲公英绒毛基抗菌止血敷料。
背景技术
皮肤为人体提供保护作用，一旦皮肤受伤后，会对身体机能造成很大影响；因此皮肤受伤后，需要及时对伤口进行保护处理，避免伤口受到感染；医用敷料作为一种对伤口进行临时处理的医用材料，其主要作用是控制伤口的渗出液加速伤口止血、保护创面防止细菌和微尘污染创口、促进伤口愈合；目前常用的创面修复用品包括天然纤维类敷料(纱布)、合成纤维类敷料、凝胶类敷料以及海绵类敷料；天然纤维素类如纱布、棉垫等，多是由棉花、软麻布等加工而成，该类敷料属于惰性敷料，主要对创口起到物理阻隔的作用，不具有抗菌和促进伤口愈合的作用，且与创口的亲和性较差；随着对创面修复研究的不断进展，此种敷料的应用日益凸显出局限性；
蒲公英属于多年生草本药食兼用植物，植物体中含有多种健康营养成分，有研究表明蒲公英提取物对金黄色葡萄球菌、溶血性链球菌、肺炎双球菌、脑膜炎球菌、白喉杆菌、绿脓杆菌、痢疾杆菌、伤寒杆菌等具有杀菌作用；现有技术中公开了将蒲公英提取物作为药用成分添加于敷料中而起到一定杀菌消炎的作用；而蒲公英绒毛作为蒲公英植株的一部分，其作为一种天然的植物纤维应用于制作医用无纺布敷料尚未见报道；
发明内容
针对现有技术的不足，本发明提供了一种蒲公英绒毛基抗菌止血敷料，该抗菌止血敷料是以蒲公英绒毛、粘胶纤维作为无纺布基材，以壳聚糖、魔芋葡甘聚糖混合溶液作为整理液制备获得；该无纺布敷料具有良好的机械强度、透气性、吸液性以及抗菌止血性能。
为了实现上述目的，本发明采用以下技术方案：
一种蒲公英绒毛基抗菌止血敷料，是以蒲公英绒毛、粘胶纤维作为无纺布基材，以壳聚糖/魔芋葡甘聚糖混合溶液作为整理液制备获得；其制备方法具体包括以下步骤：
(1)前处理：将采集的蒲公英绒毛在避光条件下浸入高碘酸钾水溶液中，搅拌反应结束后清洗，得到醛基化蒲公英绒毛；
(2)蒲公英绒毛/粘胶纤维无纺布的制备；
(3)采用壳聚糖/魔芋葡甘聚糖混合溶液作为整理液对蒲公英绒毛/粘胶纤维无纺布进行二浸二轧的后整理；
(4)将整理后的蒲公英绒毛/粘胶纤维无纺布置于60-80℃干燥后获得蒲公英绒毛基抗菌止血敷料；
优选地，步骤(1)中所述的高碘酸钾水溶液的浓度为2-3wt％；所述的搅拌反应是在室温下搅拌反应时间4-6h；
优选地，步骤(2)中所述的蒲公英绒毛/粘胶纤维无纺布的制备过程为：
(2.1)将醛基化蒲公英绒毛纤维(QR)和粘胶纤维(VF)开松处理；
(2.2)将开松后的纤维经梳理机梳理后形成经纬均匀分布的短纤维；
(2.3)将短纤维经铺网机铺成纤维网；
(2.4)将纤维网放入水刺机中水刺获得蒲公英绒毛/粘胶纤维无纺布基材；
优选地，所述的水刺为正反两面各水刺复合2-4次；水刺的压力为2-3MPa，进出料速度14-16m/min；
优选地，步骤(3)中所述的混合整理液的制备方法如下：
(3.1)壳聚糖溶液配制：取壳聚糖加入10倍重量份的醋酸，常温水浴搅拌均匀，完全溶解后，制成壳聚糖溶液，备用；
(3.2)魔芋葡甘聚糖溶液配制：向魔芋葡甘聚糖中加入去离子水，搅拌溶解，制成魔芋葡甘聚糖溶液；
(3.3)制备混合整理液：取壳聚糖溶液加入到魔芋葡甘聚糖溶液中，搅拌，超声乳化获得混合整理液；
优选地，所述的壳聚糖为脱乙酰度为65％-85％的壳聚糖和羧甲基壳聚糖以重量比1-3∶1的混合物；
优选地，所述的魔芋葡甘聚糖溶液的质量浓度为2-6wt％；所述的壳聚糖溶液与魔芋葡甘聚糖溶液的重量比为20∶80-60∶40；
优选地，步骤(3.3)中所述的搅拌速度为300-400r/min；所述的超声乳化条件为30-40℃超声乳化30-60min；
魔芋葡甘聚糖作为一种天然水溶性植物高分子多糖，是由葡萄糖和甘露糖按一定的摩尔比通过β-1,4糖苷键和β-1,3糖苷键键合形成具有空隙的双螺旋结构，其结构中存在着大量亲水的乙酰基团，使魔芋葡甘聚糖具有很好的结合水的能力和保湿性，且生物相容性好，无毒副作用，其还可以促进成纤维细胞的繁殖，使其具有促进创口愈合的作用，在医用敷料领域受到广泛研究。
有益效果：
本发明提供了一种蒲公英绒毛基抗菌止血敷料的制备方法，首先以醛基化的蒲公英绒毛和粘胶纤维为原料制成了无纺布，再利用壳聚糖和魔芋葡甘露聚糖混合液作为整理液进行后整理获得了一种抗菌止血敷料；该敷料不仅具有良好的机械强度、透气性、吸液性；还具有抗菌和促伤口愈合作用；
本发明选用蒲公英绒毛纤维作为基材，蒲公英绒毛是由自身生长出的种子上的纤维，作为一种可再生的绿色植物纤维，具有可降解性，绿色环保；其纤维是由成千上万微小的中空鳞片叠加而成，表面结构粗糙，且具有蓬松性能，可为后期整理液提供充足的负载空间，提高了整理液在纤维表面存在的稳定性；同时蒲公英绒毛具有良好的吸水性，且其纤维中富含清凉消炎止痛的成分，对创口愈合具有促进作用；
本发明选择壳聚糖与魔芋葡甘聚糖的混合液作为整理液，壳聚糖与魔芋葡甘聚糖具有良好的协同抗菌性，同时魔芋葡甘聚糖还具有促进成纤维细胞繁殖的作用而促进创口愈合，提高了敷料对创口的促愈合作用；另外，壳聚糖与魔芋葡甘聚糖以合适比例混合后获得的整理液采用化学交联的的方式负载于醛基化的蒲公英绒毛/粘胶纤维无纺布上，醛基化的蒲公英绒毛以及魔芋葡甘聚糖与壳聚糖上的氨基发生席夫碱反应而提高了整理液在无纺布层的存在稳定性，同时提高了无纺布敷料的机械强度以及吸液抗菌性；
具体实施方式
实施例1
蒲公英绒毛/粘胶纤维无纺布的制备：
(1)采集500g蒲公英绒毛在避光条件下，置于2-3wt％高碘酸钾溶液中于室温下在300-400r/min搅拌反应4-6h后，用去离子水清洗至洗涤液中无钾离子存在，烘干后获得醛基化蒲公英绒毛；
(2)将醛基化蒲公英绒毛纤维(QR)和粘胶纤维(VF)开松处理；
(3)将开松后的纤维梳理机梳理后形成经纬均匀分布的短纤维；
(4)将短纤维经铺网机铺成纤维网；
(5)将纤维网放入水刺机中正反两面各水刺复合2-4次；使蒲公英纤维和粘胶纤维缠结在一起获得蒲公英绒毛/粘胶纤维无纺布基材；其中，水刺的压力为2-3MPa，进出料速度为14-16m/min；
所述的粘胶纤维是以农作物秸秆为原料采用熔融纺丝制备获得，干断裂伸长率为17％～23％，干断裂强度2.65～3.88cN/dtex，湿断裂强度1.7-2.5cN/dtex，回潮率16％以上；吸湿性好，手感柔软，符合人体皮肤的生理需求；
调整醛基化蒲公英绒毛纤维与粘胶纤维的比例获得不同系列无纺布基材，并对其性能进行测试，结果如表1所示。
表1.
由表1数据可知，随着无纺布层中蒲公英绒毛纤维量的增加，无纺布的断裂强度逐渐降低，透气率先升高后降低，吸液率降低；在QR∶VR的比例大于3∶7时，无纺布的强度急剧降低，综合考虑机械强度、透气性以及吸液率的因素，本发明优选QR∶VR为3∶7的无纺布(J-7)作为基材。
实施例2
(1)壳聚糖溶液配制：取壳聚糖(脱乙酰度为65％壳聚糖与羧甲基壳聚糖的重量比为2:1)加入10倍重量份的醋酸，常温水浴搅拌均匀，完全溶解后，制成壳聚糖溶液，备用；
(2)魔芋葡甘聚糖溶液配制：向魔芋葡甘聚糖中加入去离子水，搅拌溶解，制成质量浓度为4wt％魔芋葡甘聚糖溶液；
(3)制备混合整理液：取壳聚糖溶液加入到魔芋葡甘聚糖溶液中，搅拌，超声乳化获得混合整理液；所述的搅拌速度为300-400r/min；所述的超声乳化条件为30-40℃超声乳化30-60min；
(4)将实施例1制备获得蒲公英绒毛/粘胶纤维无纺布(J-7)置于壳聚糖/魔芋葡甘聚糖混合整理液中，通过搅拌，使整理液均匀覆盖于无纺布上，在60℃下浸渍60min后，进行第一次压轧；
(5)将第一次压轧的蒲公英绒毛/粘胶纤维无纺布置于壳聚糖/魔芋葡甘聚糖混合整理液中，通过搅拌，使整理液均匀覆盖于无纺布上，在60℃下浸渍30min后，进行第二次压轧；
(6)将二次压轧后的蒲公英绒毛/粘胶纤维无纺布于60-80℃下干燥后，灭菌即可获得蒲公英绒毛基抗菌止血敷料。
调整壳聚糖溶液(CS)与魔芋葡甘聚糖溶液(KGM)的比例获得不同种类的整理液，采用不同种类的整理液对无纺布基材(J-7)进行整理获得止血敷料，并对敷料的性能进行了测试，结果如表2所示。
表2.
调整壳聚糖和魔芋葡甘聚糖的的添加比例获得的整理液对蒲公英绒毛/粘胶纤维无纺布进行整理获得不同种类敷料(表2所示)。
由表2数据可知，随着壳聚糖溶液添加比例的增加，相对应的魔芋葡甘聚糖添加量降低，敷料的机械强度先增加后降低，透气率增大，吸液率逐渐降低，且在溶液配比大于50∶50时，吸液率降低幅度明显；整理液中的壳聚糖作为一种交联剂存在，其中的氨基分别与魔芋葡甘聚糖以及醛基化蒲公英绒毛中醛基发生席夫碱反应，提高了整理液中的高分子网状结构与无纺布基材的结合强度，而随着壳聚糖含量的增加，可交联魔芋葡甘聚糖的量降低，生物高分子网状结构致密性降低而使敷料的机械强度降低；由于魔芋葡甘聚糖具有较强的吸水能力，其含量降低使敷料的吸液率降低；综合考虑机械强度、透气率以及吸液率，优选壳聚糖溶液与魔芋葡甘聚糖溶液配比为20∶80-60∶40；更优选50∶50；
实施例3
蒲公英绒毛基抗菌止血敷料的制备
(1)壳聚糖溶液配制：
取10g壳聚糖(脱乙酰度为65％的壳聚糖与羧甲基壳聚糖的重量比为1∶1)，向其中加入10倍重量份的醋酸，常温水浴搅拌均匀，完全溶解后，制成壳聚糖溶液(CS-1)，备用；
取10g壳聚糖(脱乙酰度为65％的壳聚糖与羧甲基壳聚糖的重量比为2∶1)，向其中加入10倍重量份的醋酸，常温水浴搅拌均匀，完全溶解后，制成壳聚糖溶液(CS-2)，备用；
取10g壳聚糖(脱乙酰度为65％的壳聚糖与羧甲基壳聚糖的重量比为3∶1)，向其中加入10倍重量份的醋酸，常温水浴搅拌均匀，完全溶解后，制成壳聚糖溶液(CS-3)，备用；
(2)魔芋葡甘聚糖溶液配制：向魔芋葡甘聚糖中加入去离子水，搅拌溶解，分别配制质量浓度为2wt％、4wt％、6wt％的魔芋葡甘聚糖溶液(依次记为KGM-1、KGM-2、KGM-3)，备用；
(3)制备混合整理液：取壳聚糖溶液加入到等质量魔芋葡甘聚糖溶液中，于300-400r/min搅拌，再于30-40℃超声乳化30-60min获得混合整理液；
(4)将实施例1制备获得蒲公英绒毛/粘胶纤维无纺布(J-7)置于壳聚糖/魔芋葡甘聚糖混合整理液中，通过搅拌，使整理液均匀覆盖于无纺布上，在60℃下浸渍60min后，进行第一次压轧；
(5)将第一次压轧的蒲公英绒毛/粘胶纤维无纺布置于壳聚糖/魔芋葡甘聚糖混合整理液中，通过搅拌，使整理液均匀覆盖于无纺布上，在60℃下浸渍30min后，进行第二次压轧；
(6)将第二次压轧后的蒲公英绒毛/粘胶纤维无纺布于60-80℃下干燥后，灭菌即可获得蒲公英绒毛基抗菌止血敷料。
调整壳聚糖溶液(CS)和魔芋葡甘聚糖溶液(KGM)的浓度，混合后获得不同整理液，采用上述方法对无纺布基材进行整理后获得蒲公英绒毛基敷料；依次记为F-1～F-9，并对敷料的性能进行了测试，结果如表3所示。
实施例4
粘胶纤维基抗菌止血敷料的制备
(1)壳聚糖溶液配制：取壳聚糖(脱乙酰度为65％的壳聚糖与羧甲基壳聚糖的重量比为2∶1)加入10倍重量份的醋酸，常温水浴搅拌均匀，完全溶解后，制成壳聚糖溶液，备用；
(2)魔芋葡甘聚糖溶液配制：向魔芋葡甘聚糖中加入去离子水，搅拌溶解，制成质量浓度为4wt％魔芋葡甘聚糖溶液；
(3)制备混合整理液：取壳聚糖溶液加入到等质量的魔芋葡甘聚糖溶液中，于300-400r/min搅拌后，于30-40℃超声乳化30-60min后获得混合整理液；
(4)将实施例1制备获得蒲公英绒毛/粘胶纤维无纺布(J-1)置于壳聚糖/魔芋葡甘聚糖混合整理液中，通过搅拌，使整理液均匀覆盖于无纺布上，在60℃下浸渍60min后，进行第一次压轧；
(5)将第一次压轧的蒲公英绒毛/粘胶纤维无纺布置于壳聚糖/魔芋葡甘聚糖混合整理液中，通过搅拌，使整理液均匀覆盖于无纺布上，在60℃下浸渍30min后，进行第二次压轧；
(6)将二次压轧后的蒲公英绒毛/粘胶纤维无纺布于60-80℃下干燥后，灭菌即可获得蒲公英绒毛基抗菌止血敷料(F-0)。
表3.
由表3可知，本发明的敷料具有良好的机械强度，较高的透气率和吸液率，满足医用敷料的要求。
抑菌实验
将实施例3和实施例4所制备获得的止血敷料F-0、F-1、F-2、F-3、F-4、F-5、F-6、F-7、F-8、F-9对金黄色酿脓葡萄球菌、大肠杆菌和白色念珠菌的抗菌性进行测试；
测试方法为抑菌圈法，具体为：将敷料剪裁为直径为2cm的圆形，分别配制金黄色酿脓葡萄球菌、大肠杆菌和白色念珠菌菌液，将菌液滴加到蛋白胨培养基上，用玻璃棒涂布均匀后，将敷料置于培养基上，分别在恒温箱中培养24h后，观察记录抑菌圈的大小；为了使数据更准确，测试了每隔90°四个方向的抑菌圈宽度，取平均值作为抑菌圈大小记录于表4中。
表4.
由表4数据可知，本发明制备获得止血敷料具有良好的抑菌性；且敷料对不同菌种的抑菌性能不同，抑菌性能为：金黄色酿侬葡萄球菌＞大肠杆菌＞白色念珠菌；
由本发明制备获得的敷料F-1～F-9与F-0对比还可以看出，本发明制备获得的敷料F-
1～F-9对三种菌种的抑菌圈大于F-0；且蒲公英绒毛基无纺布中蒲公英绒毛的添加显著提高了敷料对大肠杆菌、白色念珠菌的抑菌性。
蒲公英绒毛基抗菌止血敷料对伤口的止血实验
将本发明实施例3和实施例4制备的抗菌止血敷料用于家兔的伤口止血，探究敷料对家兔伤口的止血促愈合情况；实验方法如下：
将本发明实施例3和4制备获得的抗菌止血敷料(F-0～F-9)剪裁为5cm×5cm的大小，取家兔50只(健康状况良好，体重为2-3kg)分为10组，每组5只，将兔子背部预留5cm×5cm的去除背毛的部位，消毒后，用手术刀在其背部作1cm×1cm的伤口，将伤口自由出血液10s后，将上述的敷料贴敷于伤口表面，并对伤口施加0.5N的力，以后每24h更换两次敷料，统计家兔的创面愈合情况，记录结果如表5所示。
表5.
| 编号 | 创面愈合时间/天 |
| F-0 | 14.1 |
| F-1 | 11.2 |
| F-2 | 9.6 |
| F-3 | 8.3 |
| F-4 | 8.6 |
| F-5 | 7.5 |
| F-6 | 6.3 |
| F-7 | 6.5 |
| F-8 | 5.0 |
| F-9 | 5.0 |
由表5可以看出，实施例3制备获得的敷料F-1～F-9相较于F-0，其创面愈合时间明显缩短，且由F-1至F-9，创面愈合时间呈现下降趋势，且F-1至F-3、F-4至F-6以及F-7至F-9；创面愈合时间呈现下降趋势，是由于魔芋葡甘聚糖的促进表皮成纤维细胞的增殖作用使具有促创口愈合作用，因此随着敷料中魔芋葡甘聚糖含量的增加，创口的愈合时间缩短，但是，将敷料从创口移除时，敷料中魔芋葡甘聚糖含量较高时，敷料从创口移除较难。
最后说明的是，以上实施例仅用以说明本发明的技术方案而非限制，本领域普通技术人员对本发明的技术方案所做的其他修改或者等同替换，只要不脱离本发明技术方案的精神和范围，均应涵盖在本发明的权利要求范围当中。
Claims (8)
1.一种蒲公英绒毛基抗菌止血敷料，其特征在于，其是以蒲公英绒毛、粘胶纤维作为无纺布基材，以壳聚糖/魔芋葡甘聚糖混合溶液作为整理液制备获得；其制备方法具体包括以下步骤：
前处理：将采集的蒲公英绒毛在避光条件下浸入高碘酸钾水溶液中，搅拌反应结束后清洗，得到醛基化蒲公英绒毛；
蒲公英绒毛/粘胶纤维无纺布的制备；
采用壳聚糖/魔芋葡甘聚糖混合溶液作为整理液对蒲公英绒毛/粘胶纤维无纺布进行二浸二轧的后整理；
将整理后的蒲公英绒毛/粘胶纤维无纺布置于60-80℃干燥后获得蒲公英绒毛基抗菌止血敷料。
2.如权利要求1所述的蒲公英绒毛基抗菌止血敷料，其特征在于，步骤（1）中所述的高碘酸钾水溶液的浓度为2-3wt%；所述的搅拌反应是在室温下搅拌反应时间为4-6 h。
3.如权利要求1所述的蒲公英绒毛基抗菌止血敷料，其特征在于，步骤（2）中所述的蒲公英绒毛/粘胶纤维无纺布的制备过程为：
（2.1）将醛基化蒲公英绒毛纤维和粘胶纤维开松处理；
（2.2）将开松后的纤维经梳理机梳理后形成经纬均匀分布的短纤维；
（2.3）将短纤维经铺网机铺成纤维网；
（2.4）将纤维网放入水刺机中水刺获得蒲公英绒毛/粘胶纤维无纺布基材。
4. 如权利要求3所述的蒲公英绒毛基抗菌止血敷料，其特征在于，所述的水刺为正反两面各水刺复合2-4次；水刺的压力为2-3MPa，进出料速度14-16 m/min。
5.如权利要求1所述的蒲公英绒毛基抗菌止血敷料，其特征在于，步骤（3）中所述的混合整理液的制备方法如下：
（3.1）壳聚糖溶液配制：取壳聚糖加入10倍重量份的醋酸，常温水浴搅拌均匀，完全溶解后，制成壳聚糖溶液，备用；
（3.2）魔芋葡甘聚糖溶液配制：向魔芋葡甘聚糖中加入去离子水，搅拌溶解，制成魔芋葡甘聚糖溶液；
（3.3）制备混合整理液：取壳聚糖溶液加入到魔芋葡甘聚糖溶液中，搅拌，超声乳化获得混合溶液。
6.如权利要求1所述的蒲公英绒毛基抗菌止血敷料，其特征在于，所述的壳聚糖为脱乙酰度为65%-85%的壳聚糖和羧甲基壳聚糖以重量比1-3∶1的混合物。
7.如权利要求5所述的蒲公英绒毛基抗菌止血敷料，其特征在于，所述的魔芋葡甘聚糖溶液的质量浓度为2-6wt%；所述的壳聚糖溶液与魔芋葡甘聚糖溶液的重量比为20∶80-60∶40。
8. 如权利要求5所述的蒲公英绒毛基抗菌止血敷料，其特征在于，步骤（3.3）中所述的搅拌速度为300-400 r/min；所述的超声乳化条件为30-40℃超声乳化30-60 min。
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