CN108744013B - 纳米银-葛根纤维敷料的制备方法及应用 - Google Patents
纳米银-葛根纤维敷料的制备方法及应用 Download PDFInfo
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Abstract
本发明提供的纳米银‑葛根纤维敷料的制备方法，包括以下步骤：利用Ag2SO4溶液对葛根纤维进行脱胶处理，并生成银‑葛根纤维沉淀物；对银‑葛根纤维沉淀物表面进行中性化处理；用75％的乙醇溶液溶解处理后的银‑葛根纤维沉淀物，超声震荡直至溶液变为稳定的黄色溶液，形成葛根纤维‑纳米银混合剂；在葛根纤维‑纳米银混合剂中加入聚偏二氟乙烯、二甲亚砜、脂肪酸聚乙二醇酯、表面活性剂，超声震荡至均匀，制成静电纺丝液；使用静电纺丝溶液纺丝，制成纳米银‑葛根纤维敷料。本发明的制备方法，使葛根中的类黄酮物质成份大比例地保留在葛根纤维素中，使制成的敷料止血迅速、透气性好、抗菌能力强。
Description
技术领域
本发明属于生物制造技术领域，特别涉及纳米银-葛根纤维敷料的制备方法及应用。
背景技术
由于失血是战伤伤员死亡最重要的原因之一，因此多功能性高端快速止血敷料是在战场和日常各种创伤发生情况下进行急救的重要工具。战伤失血通常分为体内出血和体外出血，体内出血大部分是因为脏器破裂，体外出血基本是由于动静脉损伤。如果能及时有效地止血，对挽救伤员生命，稳定伤情，为后续治疗创造条件十分重要。敷料作为止血材料，是指盖在伤口上、有保护作用的覆盖物，可以协助控制出血，防止感染并吸收分泌物，止血敷料对于及时止血有着重要的意义。
葛根，为豆科植物野葛，是中国南方一些省区的一种常食蔬菜，其味甘凉可口，常作煲汤之用。现代医学表明：葛根中含有大量的葛根素，能增加冠状动脉血流量、降低血管阻力、调节血液循环、降低心肌耗氧等，是一种较为常见的心肌保护物质，能解痉止痛，防治高血压、头晕头痛、冠心病、心绞痛、神经性头痛等。但事实上，除葛根素外，葛根中因品种不同至少还含有12～18％的类黄酮物质，黄酮类物质具有扩张外周血管、改善微循环,祛腐生肌,解热收敛的作用，是上等的止血材料，再加上葛根纤维经特殊处理后，具有组织疏松、吸附力强等特性，二者结合其实具有成为高端快速止血材料的可能，但国内对此方面却鲜有研究。
发明内容
本发明的目的是为解决以上问题，本发明提供纳米银-葛根纤维敷料的制备方法及应用。本发明的技术方案是通过以下实现的。
根据本发明的一个方面提供纳米银-葛根纤维敷料的制备方法，包括以下步骤：
(1)利用Ag2SO4溶液对葛根纤维进行脱胶处理，并生成银-葛根纤维沉淀物；
(2)对银-葛根纤维沉淀物表面进行中性化处理；
(3)用75％的乙醇溶液溶解处理后的银-葛根纤维沉淀物，超声震荡直至溶液变为稳定的黄色溶液，形成葛根纤维-纳米银混合剂；
(4)在葛根纤维-纳米银混合剂中加入聚偏二氟乙烯、二甲亚砜、脂肪酸聚乙二醇酯、表面活性剂，超声震荡至均匀，制成静电纺丝液；
(5)使用静电纺丝溶液纺丝，生成纳米银-葛根纤维敷料。
其中，步骤(1)包括：
使用浓度为1～1.5mL/L的H2SO4溶解葛根粉末，置于40℃的水浴锅中30～60min，用自来水冲洗至中性；再加入由浓度为30mL/L的Na2SiO3溶液、质量浓度为12.75g/L的MgSO4溶液、质量浓度为40g/mL的NaOH溶液和H2O2混合形成的混合液，并置于85℃的水浴锅中60～80min，搅拌；然后加入浓度为0.8～1.6g/L的Ag2SO4溶液将溶液调节至中性；过滤得到银-葛根纤维沉淀物。
其中，步骤(1)包括：H2SO4和葛根粉末的浴比为5:1，混合液和葛根粉末的浴比为4:1。
其中，步骤(1)包括：葛根为250g，H2SO4为1L，Na2SiO3溶液为30mL，MgSO4溶液为100mL，NaOH为210mL，H2O2为660mL，Ag2SO4溶液为400mL。
其中，步骤(4)包括：葛根纤维-纳米银混合剂：聚偏二氟乙烯：二甲亚砜：脂肪酸聚乙二醇酯：表面活性剂＝270～290：35～45：12～15：1～1.5：1～1.5，超声震荡时间为30～50min。
其中，步骤(5)包括：静电纺丝电压为6～8kV，针头与接收板之间的距离为10～12cm，推进泵的推进速度为0.30～0.40mm/h，纺丝环境温度为30～35℃。
其中，步骤(2)包括：用温水冲洗银-葛根纤维沉淀物，使银-葛根纤维沉淀物的表面为中性。
其中，步骤(3)包括：超声震荡60～90min。
根据本发明的另一方面提供该制备方法制备的纳米银-葛根纤维敷料在止血方面的应用。
本发明具有以下有益效果：
1.本发明的制备方法，使葛根中类黄酮物质大比例地保留在葛根纤维素中，因此使制成的敷料具有良好的止血功能。
2.本方法制备的敷料主要成份为天然葛根纤维，对血液的吸收能力和材料自身透气性均优于普通的止血功能材料。
3.本发明将葛根纤维、纳米银和高分子聚合物通过静电纺丝技术结合，使形成的敷料具有较大的比表面积和微孔结构，一方面能够引导纤维迅速深入至伤口深处，修复受伤组织，另一方面使材料具备良好的抗菌能力，能够避免二次感染。
具体实施方式
下面将更详细地描述本公开的示例性实施方式。虽然本说明书中显示了本公开的示例性实施方式，然而应当理解，可以以各种形式实现本公开而不应被这里阐述的实施方式所限制。相反，提供这些实施方式是为了能够更透彻地理解本公开，并且能够将本公开的范围完整的传达给本领域的技术人员。
实施例1纳米银-葛根纤维敷料X1的制备方法及应用
包括以下步骤：
使用1L浓度为1mL/L的H2SO4溶解250g葛根粉末，置于40℃的水浴锅中45min，用自来水冲洗至溶液的PH至为7；再加入由30mL浓度为30mL/L的Na2SiO3溶液、100mL质量浓度为12.75g/L的MgSO4溶液、210mL质量浓度为40g/mL的NaOH溶液和660mL的H2O2混合形成的混合液，并置于85℃的水浴锅中80min，搅拌10min；然后加入400mL浓度为1.5g/L的Ag2SO4溶液使得溶液的PH至为7；。用布氏漏斗过滤得到银-葛根纤维沉淀物；使用30℃的温水冲洗银-葛根纤维沉淀物，至银-葛根纤维沉淀物的表面的PH值为7.2；用75％的乙醇溶液溶解处理后的银-葛根纤维沉淀物，超声震荡90min至溶液变为稳定的黄色溶液，形成葛根纤维-纳米银混合剂；在葛根纤维-纳米银混合剂中加入聚偏二氟乙烯、二甲亚砜、脂肪酸聚乙二醇酯、表面活性剂，超声震荡30min至均匀，制成静电纺丝液，其中，葛根纤维-纳米银混合剂：聚偏二氟乙烯：二甲亚砜：脂肪酸聚乙二醇酯：表面活性剂＝270：40：12：1.5：1.5；使用静电纺丝溶液纺丝，制成纳米银-葛根纤维敷料X1，其中静电纺丝电压为6kV，针头与接收板之间的距离为10cm，推进泵的推进速度为0.40mm/h，纺丝环境温度为30℃。
使用高效液相色谱法(HPLC)对纳米银-葛根纤维敷料X1的类黄酮物质含量进行测定，经检测X1中类黄酮物质含量为15g，因此实施例1的制备方法黄酮的提取率为6％。
实施例2纳米银-葛根纤维敷料X2的制备方法及应用
包括以下步骤：
使用0.4L浓度为1mL/L的H2SO4溶解100g葛根粉末，置于40℃的水浴锅中45min，用自来水冲洗至溶液的PH至为7.3；再加入由12mL浓度为30mL/L的Na2SiO3溶液、40mL质量浓度为12.75g/L的MgSO4溶液、84mL质量浓度为40g/mL的NaOH溶液和264mL的H2O2混合形成的混合液，并置于85℃的水浴锅中80min，搅拌5min；然后加入160mL浓度为1.5g/L的Ag2SO4溶液使得溶液的PH至为7.4；。用布氏漏斗过滤得到银-葛根纤维沉淀物；使用50℃的温水冲洗银-葛根纤维沉淀物，至银-葛根纤维沉淀物的表面的PH值为7.5；用75％的乙醇溶液溶解处理后的银-葛根纤维沉淀物，超声震荡60min至溶液变为稳定的黄色溶液，形成葛根纤维-纳米银混合剂；在葛根纤维-纳米银混合剂中加入聚偏二氟乙烯、二甲亚砜、脂肪酸聚乙二醇酯、表面活性剂，超声震荡35min至均匀，制成静电纺丝液，其中，葛根纤维-纳米银混合剂：聚偏二氟乙烯：二甲亚砜：脂肪酸聚乙二醇酯：表面活性剂＝290：45：15：1.2：1.5；使用静电纺丝溶液纺丝，制成纳米银-葛根纤维敷料X3，其中静电纺丝电压为8kV，针头与接收板之间的距离为10cm，推进泵的推进速度为0.30mm/h，纺丝环境温度为35℃。
使用高效液相色谱法(HPLC)对纳米银-葛根纤维敷料X2的类黄酮物质含量进行测定，经检测X2中类黄酮物质含量为6.2g，因此实施例2的制备方法黄酮的提取率为6.2％。
实施例3纳米银-葛根纤维敷料X3的制备方法及应用
使用0.1L浓度为1mL/L的H2SO4溶解25g葛根粉末，置于40℃的水浴锅中45min，用自来水冲洗至溶液的PH至为6.8；再加入由3mL浓度为30mL/L的Na2SiO3溶液、10mL质量浓度为12.75g/L的MgSO4溶液、21mL质量浓度为40g/mL的NaOH溶液和66mL的H2O2混合形成的混合液，并置于85℃的水浴锅中80min，搅拌7min；然后加入40mL浓度为1.5g/L的Ag2SO4溶液使得溶液的PH至为7.1；。用布氏漏斗过滤得到银-葛根纤维沉淀物；使用50℃的温水冲洗银-葛根纤维沉淀物，至银-葛根纤维沉淀物的表面的PH值为7.1；用75％的乙醇溶液溶解处理后的银-葛根纤维沉淀物，超声震荡80min至溶液变为稳定的黄色溶液，形成葛根纤维-纳米银混合剂；在葛根纤维-纳米银混合剂中加入聚偏二氟乙烯、二甲亚砜、脂肪酸聚乙二醇酯、表面活性剂，超声震荡45min至均匀，制成静电纺丝液，其中，葛根纤维-纳米银混合剂：聚偏二氟乙烯：二甲亚砜：脂肪酸聚乙二醇酯：表面活性剂＝270：35：14：1：1；使用静电纺丝溶液纺丝，制成纳米银-葛根纤维敷料X2，其中静电纺丝电压为8kV，针头与接收板之间的距离为12cm，推进泵的推进速度为0.40mm/h，纺丝环境温度为32℃。
使用高效液相色谱法(HPLC)对纳米银-葛根纤维敷料X3的类黄酮物质含量进行测定，经检测X2中类黄酮物质含量为1.38g，因此实施例2的制备方法黄酮的提取率为5.52％。
实验例1血液吸收实验
①.实验步骤：称取20ml血液置于烧杯中，分别裁切出1cm*1cm尺寸的纳米银-葛根纤维敷料X1～X3投入烧杯中，其中纳米银-葛根纤维敷料X1～X3的厚度均为0.3毫米，记录吸附全部血液所需时间，如不能完成吸附，记录最大吸附时间。
②.实验结果：
纳米银-葛根纤维敷料X1～X3均顺利完成吸附，其中纳米银-葛根纤维敷料X1所需时间为8s，纳米银-葛根纤维敷料X2所需时间为10s，蜂胶-纳米银敷料X3所需时间为10s。
实验例2止血实验
①.实验步骤：选取30只体重为6.0～6.3kg的比利时长耳兔，随机分为3组，每组10只，进行止血测试实验。按40mg/kg剂量静脉缓慢注射戊巴比妥钠溶液麻醉后，将其中央耳动脉区域备皮、消毒，沿耳动脉方向切开皮肤，钝性分离出耳动脉、静脉和神经，再用手术刀横向切断动脉，待血液涌出后立即用1层尺寸为1*1cm的待测试材料并使用推拉力计施加3N的压力，每隔10s观察止血情况，直至最终完全止血后记录止血时间，计算每组所用平均时间。其中每组使用一种实施例1～3中的纳米银-葛根纤维敷料作为待测试材料。
②.实验结果：
纳米银-葛根纤维X1～X3的平均止血时间分别为100s，105s和111s。
实验例3
实验材料：厚度均为0.620mm的纳米银-葛根纤维敷料X1～X3和纯棉织物Y，其中纯棉织物Y的规格见表1所示。
实验步骤：使用GELLOWEN透气性测试仪依次对敷料X1～X3和纯棉织物Y进行透气度测试，每种材料测试10次，取均值即为该种材料的透气度。
实验结果：经检测纳米银-葛根纤维敷料X1～X3的平均透气度分别为38.7L/min、32.9L/min和35.7L/min，而纯棉织物Y的平均透气度为15.1L/min。
综上所述，本发明制备的纳米银-葛根纤维敷料除具有优异的吸收和止血能力外，其透气性更加优于相同厚度的纯棉织物。
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，可轻易想到的变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应以所述权利要求的保护范围为准。
Claims (8)
1.纳米银-葛根纤维敷料的制备方法，其特征在于，包括以下步骤：
(1)利用Ag2SO4溶液对葛根纤维进行脱胶处理，并生成银-葛根纤维沉淀物；
(2)对银-葛根纤维沉淀物表面进行中性化处理；
(3)用75％的乙醇溶液溶解处理后的银-葛根纤维沉淀物，超声震荡直至溶液变为稳定的黄色溶液，形成葛根纤维-纳米银混合剂；
(4)在葛根纤维-纳米银混合剂中加入聚偏二氟乙烯、二甲亚砜、脂肪酸聚乙二醇酯、表面活性剂，超声震荡至均匀，制成静电纺丝液；
(5)使用静电纺丝溶液纺丝，制成纳米银-葛根纤维敷料。
2.如权利要求1所述的制备方法，其特征在于，所述步骤(1)包括：
使用浓度为1～1.5mL/L的H2SO4溶解葛根粉末，置于40℃的水浴锅中30～60min，用自来水冲洗至中性；再加入由浓度为30mL/L的Na2SiO3溶液、质量浓度为12.75g/L的MgSO4溶液、质量浓度为40g/mL的NaOH溶液和H2O2混合形成的混合液，并置于85℃的水浴锅中60～80min，搅拌；然后加入浓度为0.8～1.6g/L的Ag2SO4溶液将溶液调节至中性；过滤得到银-葛根纤维沉淀物。
3.如权利要求2所述的制备方法，其特征在于，所述步骤(1)包括：
其中，H2SO4和葛根粉末的浴比为5:1，混合液和葛根粉末的浴比为4:1。
4.如权利要求2所述的制备方法，其特征在于，所述步骤(1)包括：
其中，葛根为250g，H2SO4为1L，Na2SiO3溶液为30mL，MgSO4溶液为100mL，NaOH为210mL，H2O2为660mL，Ag2SO4溶液为400mL。
5.如权利要求1所述的制备方法，其特征在于，所述步骤(4)包括：
葛根纤维-纳米银混合剂：聚偏二氟乙烯：二甲亚砜：脂肪酸聚乙二醇酯：表面活性剂＝270～290：35～45：12～15：1～1.5：1～1.5，超声震荡时间为30～50min。
6.如权利要求1所述的制备方法，其特征在于，所述步骤(5)包括：
静电纺丝电压为6～8kV，针头与接收板之间的距离为10～12cm，推进泵的推进速度为0.30～0.40mm/h，纺丝环境温度为30～35℃。
7.如权利要求1所述的制备方法，其特征在于，所述步骤(2)包括：
用温水冲洗银-葛根纤维沉淀物，使银-葛根纤维沉淀物的表面为中性。
8.如权利要求1所述的制备方法，其特征在于，所述步骤(3)包括：
超声震荡60～90min。
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