CN113059176A - 一种钴-银纳米微粒的制备方法及其应用 - Google Patents
一种钴-银纳米微粒的制备方法及其应用 Download PDFInfo
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Abstract
本发明属于纳米材料技术领域，具体涉及一种钴‑银纳米微粒的制备方法及其应用，所述的钴‑银纳米微粒由47.2‑141.6mg纳米钴和含272mg硝酸银的水溶液中制备而成，制备方法简单，钴‑银纳米微粒呈“树枝状”分布，粒径均一，平均粒径约为100nm，比表面积大，具有超顺磁性等优点，且具有良好的抑菌性能，可以用于水处理，且回收方法简单，不会造成银中毒，具有良好的应用前景。
Description
技术领域
本发明属于纳米材料技术领域，具体涉及一种钴-银纳米微粒的制备方法及其应用。
背景技术
纳米生物技术是一个新兴领域，在医学方面由于纳米材料研究而获得新生的药物比比皆是并且应用广泛，已经为人类生命健康做出了重大贡献。致病菌的感染和蔓延一直以来都严重威胁着人类的生存和健康。抗菌素的出现使人类在与致病菌的斗争中处于有利地位，然而过度使用抗菌素又给我们带来了耐药菌、新的致病菌以及基因突变的超级细菌。近年来，纳米杀菌材料以自身理化性质对细菌的杀灭作用使其有望成为新型抗菌物质。目前所报道的纳米杀菌材料包括TiO2、ZnO、CuO、Ca(HO)2、MgO、壳聚糖、银等。
在这些杀菌材料中，银及其复合物能够广泛地杀死细菌、病毒等微生物，是较为有效的抑菌剂，并且它具有较小的毒副作用优点，在局部的抑菌治疗中发挥着重要的作用。临床上使用载银医用敷料可以杀灭伤口上的细菌，避免伤口的感染，且可以促进慢性伤口的愈合。与无涂层的外科缝线相比，涂有载银生物活性的外科缝线抑制细菌粘附能力更强。此外，载银系抗菌材料还用于导尿管、纤维织物、抗菌塑料等银抗菌剂具有广谱抗菌性，对大量的病原微生物都有杀灭作用，且不会导致微生物产生耐药性。在水处理方面，TiO2很早被用于废水处理系统，然而银及其含银复合物在机体中累积过多会导致严重的银中毒，处理这些化学材料会增加额外的时间和成本，因此，含银复合物在水处理方面的应用研究较少。
钴是一种两性金属，有着良好的磁性，在硬度、抗拉强度、机械加工性能、热力学性质以及电化学行为方面的特性与铁、镍相似，尤其在磁性方面钴有着明显的优势，是少数能够磁化一次后就保持磁性的金属，但是钴本身不具有抑菌活性。
针对上述技术问题，本发明利用以钴纳米微粒为载体，在硝酸银水溶液中制备了表面载银的钴-银复合纳米材料，并对其进行的抗菌实验，结果表明这种磁性钴-银复合纳米材料具有良好的抗菌效果，可以作为一种新型的抗菌剂。
发明内容
针对上述技术问题，本发明提供了一种钴-银纳米微粒，所述的钴-银纳米微粒由47.2-141.6mg纳米钴和272mg硝酸银制备而成。
本发明还公开了所述的钴-银纳米微粒的制备方法，所述的方法包括如下步骤：称取钴纳米颗粒47.2-141.6mg，硝酸银272mg，分别溶于硝酸银水溶液中，混合，室温条件下搅拌，离心得到钴-银纳米沉淀，用去离子水和无水乙醇超声、离心，冷冻干燥，即得。
优选地，所述的搅拌转速为800rmp，搅拌时间为4h。
优选地，离心时的转速为5000rmp。
本发明还公开了所述的钴-银纳米微粒在抑制细菌生长中的应用。
优选地，所述的细菌包括大肠杆菌、铜绿假单胞菌、白色念珠菌和金黄色葡萄球菌。
本发明还公开了所述的钴-银纳米微粒在抑制水中细菌生长的应用。
本发明的有益效果是：本发明所述的钴-银纳米微粒，制备方法简单，呈“树枝状”分布，粒径均一，平均粒径约为100nm，比表面积大，具有超顺磁性等优点，且具有良好的抑菌性能，可以用于水处理，且回收方法简单，减少环境污染，可以循环利用，降低处置成本，也不会造成银中毒，具有良好的应用前景。
附图说明
图1钴-银纳米微粒的TEM图
图2钴-银纳米微粒的XRD/XPS谱图：
(a)钴-银纳米微粒的XRD谱；(b)钴-银纳米微粒的XPS全谱；(c)Ag 3d轨道的XPS窄谱；(d)Co 2p轨道的XPS窄谱
图3钴-银纳米微粒的磁学性能示意图。
(a)磁铁对钴-银纳米微粒的磁场作用。(b)/(c)室温条件下测量的钴、钴-银纳米微粒磁化曲线。
图4钴-银纳米微粒对标准菌株的抑菌检测图
M-H培养基上的种植菌依次为(a)铜绿假单胞菌、(b)大肠杆菌、(c)金黄色葡萄球菌、(d)白色念珠菌；位置0的药敏纸片含有钴纳米微粒，位置1的药敏纸片含有钴-银纳米微粒
具体实施方式
为使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体实施方式，进一步阐述本发明。以下实施例仅用以说明本发明的技术方案而非限制，尽管参照较佳实施例对本发明进行了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的宗旨和范围，其均应涵盖在本发明的权利要求范围当中。
实施例一、钴-银纳米微粒的制备
1.试剂来源：
钴纳米颗粒(粒径100nm)购自上海允复科技有限公司，无水乙醇(C2H5OH)购自天津市百世化工有限公司，硝酸银(AgNO3)购自国药集团试剂公司。
2.钴-银纳米微粒的制备
精密称取钴纳米颗粒47.2-141.6mg，AgNO3粉末272mg各自溶于50ml去离子水中，配置的两种溶液加到三口烧瓶中，将反应体系增加至200ml；室温条件下800rmp转速搅拌4h，5000rmp离心得到钴-银纳米沉淀；依次用去离子水和无水乙醇超声、离心洗涤数次，冷冻干燥，以备进一步表征和应用。
3.钴-银纳米微粒的表征
采用透射电子显微镜(TEM,Kevex JSM-6701F,Japan)对合成的钴-银纳米微粒样品的表观形貌进行观察。通过X射线光电子能谱仪(XPS,ESCALAB 250型，美国赛默飞世尔科技)确定了钴-银纳米微粒的元素种类、原子价态以及质量占比并用X射线衍射仪(XRD,Bruker D8 Advance型)进一步确定了复合材料的物相组成。室温利用振荡样品磁力计(VSM，Lake Shore Cryotronics Inc.,Ohio,USA)检测钴-银纳米微粒的磁学性能。
4.结果分析
钴-银纳米微粒的TEM形貌如图1-(a)所示，钴纳米微粒外表面包裹了一层银，并且构成“树枝状”。如图1-(b)所示，组成“树枝状”钴-银纳米微粒尺寸较为均匀，平均粒径约为100nm。
图2为材料的X射线衍射仪(XRD)图以及X射线光电子能谱(XPS)图，从图2-(a)可知，复合材料包含银单质和钴单质的特征峰，证明两种单质成功的复合到一起。图2-(b)为XPS全谱图，从元素分布可知钴-银纳米微粒表面含有O，Ag，Co 3种元素，通过图中Co、Ag波峰下的面积计算出产物中Co、Ag的含量分别为9.04％、10.03％。X射线光电子能谱仪测试的是材料表层极薄的区域，而纳米微粒在空气中表层会被氧化，所以测试结果中会存在氧元素。XRD测试结果表明材料整体由银单质和钴单质构成。图2-(c)为材料中Ag的价态分布图，Ag表现出3d5/2和3d3/2价态，其结合能分别为368.4和374.4eV，与金属Ag单质在3d5/2和3d3/2处的标准电子结合能相符，另外位置为374.43eV和368.43eV对应Ag2O中Ag+的峰位。图2-(d)为材料中钴元素的价态分布图，其中780.88eV、796.9eV处分别对应Co3O4中Co的2p3/2和2p1/2价态，786.58eV和803.79eV为Co3O4中Co的卫星振动峰，778.39eV、793.49eV处对应钴单质中Co0价态的峰位。
钴-银纳米微粒的磁学性质对于后续的应用至关重要。在装有钴-银纳米微粒浊液的容器旁边放置一块磁铁，纳米微粒在磁场作用力下快速运动到靠近磁铁的一侧，我们可以清楚的看到钴-银纳米微粒有良好的磁响应性图3-(a)。室温条件下，利用VSM检测钴-银纳米微粒的磁学性能。磁场范围为-30-30kOe，从图3-(c)可以看出钴-银纳米微粒在外加磁场下具有磁响应性，磁饱和强度为70.1emu/g。在外磁场磁矩为0时，没有滞磁现象的存在，这说明合成的钴-银纳米微粒具有超顺磁性，因此可借助外部磁场从溶液中分离出来。而钴-银饱和磁强度低于钴纳米微粒3-(b)，可能归因于磁核钴纳米微粒表面上附着一层银单质增加了壳层厚度。
实施例二、钴-银纳米微粒的体外抗菌活性测定
1.菌株来源：
铜绿假单胞菌(ATCC 27853革兰氏阴性细菌)、大肠杆菌(ATCC 25922，革兰氏阴性细菌)、金黄色葡萄球菌(ATCC 25923，革兰氏阳性细菌)和白色念珠菌(ATTC 90029，酵母菌)，由西安市第九医院微生物实验室提供。
2.试剂来源
水解酪蛋白(M-H)购自琼脂培养基温州市康泰生物科技有限公司，LB液体培养基(干粉)购自北京索莱宝科技有限公司，黄河水取自黄河兰州段。
3.黄河水的处理
黄河水过200目筛去除较大杂物，静置沉淀，取上清液在无菌条件下，吸取100μl黄河水均匀的涂抹在LB固体培养基上，37℃、12h培养，测得黄河水浊度为6～7×103CFU/ML。兰州段黄河水主要细菌为粪大肠菌群。
4.最低抑菌浓度测定
选用铜绿假单胞菌、大肠杆菌、金黄色葡萄球菌和白色念珠菌标准菌株做为研究对象，利用纸片琼脂扩散法和肉汤稀释法测定钴-银纳米微粒的最小抑菌浓度(MIC)。分别取无菌钴、钴-银纳米微粒配成10mg/ml的悬浊液，各加入空白药敏纸片振荡过夜，制得分别含有钴、钴-银纳米微粒的药敏纸片；将制备好的药敏纸片粘贴在接种了以上四种标准菌的M-H琼脂培养基上，过夜，观察抑菌效果。
在无菌条件下，挑取单个铜绿假单胞菌、大肠杆菌、金黄色葡萄球菌和白色念珠菌用LB液体培养基稀释为1.0×105CFU/ML的稀释菌液，24孔板每孔中加入2ml稀释菌液，从第一孔开始加入一定量的钴-银纳米微粒抗菌液，抗菌液浓度依次为：0(阳性对照，即只加菌液不加钴-银纳米微粒)、100、200、300、400、500、600、700、900、1000、2000g/μl，最后一孔中加入2ml钴-银纳米微粒抗菌液作为阴性对照，37℃、180rmp、12h培养增菌；设置复孔。第二天观察钴-银纳米微粒抑菌效果，以无细菌生长的最低浓度为MIC。
钴-银纳米微粒对黄河水的最小抑菌浓度的测定：无菌条件下，将黄河水按照1:100稀释到LB液体培养基中，24孔板中每孔加入2ml稀释的黄河水LB液体培养基，从第一孔开始加入一定量的钴银纳米微粒抗菌液，每孔抗菌液浓度依次为：0(阳性对照，即只加菌液不加钴-银纳米微粒)、100、200、300、400、500、600、700、900、1000、2000g/μl，最后一孔中加入2ml钴-银纳米微粒抗菌液作为阴性对照，37℃、180rmp、12h培养增菌，设置复孔。第二天观察钴-银纳米微粒抑菌效果，以无细菌生长的最低浓度为MIC。
5.钴-银纳米微粒的二次利用
钴-银纳米微粒对铜绿假单胞菌、大肠杆菌、金黄色葡萄球菌和白色念珠菌的二次最小抑菌浓度的测定：确定钴-银纳米微粒对标准菌株的首次抑菌浓度后，将磁铁放到24孔板下方30min左右，钴-银纳米微粒被磁铁吸引到24孔板底部，然后缓慢弃掉24孔板中的细菌菌液，重新加入2ml稀释菌液，37℃、180rmp、12h培养增菌。第三天肉眼观察钴银纳米微粒抑菌效果，以无细菌生长的最低浓度为MIC。
钴-银纳米微粒对黄河水的二次最小抑菌浓度的测定：确定钴-银纳米微粒对黄河水首次抑菌浓度后，将磁铁放到24孔板下方30min左右，钴-银纳米微粒被磁铁吸引到24孔板底部，然后缓慢弃掉24孔板中的细菌菌液，重新加入2ml稀释菌液，37℃、180rmp、24h培养增菌。第三天肉眼观察钴银纳米微粒抑菌效果，以无细菌生长的最低浓度为MIC。
6.结果分析
通过定性和定量的方法评估钴-银纳米微粒对生活中常见菌的抑菌效果，结果如图4、表1所示：位置0是含有钴纳米微粒的药敏纸片，它对铜绿假单胞菌(a)、金黄色葡萄球菌(b)、大肠杆菌(c)和白色念珠菌(d)均没有抑菌效果；钴-银纳米微粒对铜绿假单胞菌、白色念珠菌和金黄色葡萄球菌的抑菌明显效果优于大肠杆菌，抑菌圈直径依次为12.8±0.4、15.2±0.4、12.6±0.5、10.2±0.4mm。
由表1可以看出，钴-银纳米微粒对于一般的标准菌株均能够达到优异的抑菌效果；二次回收的钴-银纳米微粒依然对细菌有很好抑菌效果。钴-银纳米微粒对于黄河水能够达到优异的抑菌效果；并且二次回收的钴-银纳米微粒依然对黄河水依然有抑菌效果。
表1钴-银纳米微粒对标准菌株的MIC(μg/ml)
实施例三、钴-银纳米微粒的回收
精密称取5mg钴-银纳米微粒，溶解到含有25ml细菌浓度为1.0×105CFU/ML的大肠杆菌稀释菌液的离心管中，37℃、180rmp、12h培养增菌。次日，将磁铁放到离心管下方30min左右，钴-银纳米微粒被磁铁吸引到试管底部，然后缓慢弃掉离心中的细菌菌液，60℃干燥至离心管恒重。对回收后钴-银纳米微粒进行称重。根据下面公式计算回收率：回收率＝回收量/投入量。
首次抑菌实验中加入的5mg钴-银纳米微粒利用磁铁吸附、去上清再经干燥后得到钴-银纳米微粒4.9mg，计算回收率，测得回收率为98％。
综上所述，本发明以钴纳米微粒为核心，将硝酸银溶液中的银离子还原成银单质包覆在钴纳米微粒表面，制备成的钴-银纳米微粒粒径均匀，约100nm，形状呈“树枝状”，比表面积大，抑菌效果好，对铜绿假单胞菌、大肠杆菌、金黄色葡萄球菌、白色念珠菌以及黄河水中的细菌均有良好的抑菌效果。并且制备方法简单，制备出的钴-银纳米微粒不仅具有金属银的抑菌性而且还具有金属钴的强磁性。在污水处理方面，钴-银纳米微粒抑制了细菌的生长，在磁场力的作用下，可以再次回收，并且具有较高的回收率，降低了金属银的毒性，回收后的复合材料还存在较好的抑菌效果，所述的钴-银纳米微粒不会对周边环境造成影响，减少环境污染，可循环利用，降低处置成本，具有良好的应用前景。
Claims (7)
1.一种钴-银纳米微粒，其特征在于，所述的钴-银纳米微粒由47.2-141.6mg纳米钴和272mg硝酸银制备而成。
2.一种如权利要求1所述的钴-银纳米微粒的制备方法，其特征在于，所述的方法包括如下步骤：称取钴纳米颗粒47.2-141.6mg，硝酸银272mg，分别溶于水中，混合，室温条件下搅拌，离心得到钴-银纳米微粒沉淀，用去离子水和无水乙醇超声、离心，冷冻干燥，即得。
3.如权利要求2所述的钴-银纳米微粒的制备方法，其特征在于，所述的搅拌转速为800rmp，搅拌时间为4h。
4.如权利要求2所述的钴-银纳米微粒的制备方法，其特征在于，离心时的转速为5000rmp。
5.如权利要求1所述的钴-银纳米微粒在抑制细菌生长中的应用。
6.如权利要求5所述的应用，其特征在于，所述的细菌包括大肠杆菌、铜绿假单胞菌、白色念珠菌和金黄色葡萄球菌的任一种或几种。
7.如权利要求1所述的钴-银纳米微粒在抑制水中细菌生长的应用。
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