CN113798506A - 一种罗望子多糖纳米银的制备方法 - Google Patents
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Abstract
本发明公开了一种罗望子多糖纳米银的制备方法，该方法包含：将浓度为4～10mg/mL罗望子多糖和浓度为0.08～0.10mol/L硝酸银于水中，混合均匀，将混合溶液在微波炉中反应，微波频率为50Hz，控制微波辐射时间为4～7min，得到罗望子多糖纳米银。本发明的方法采用罗望子多糖作为还原剂和稳定剂，能够在纳米尺度上形成了具有球形颗粒的立方体银相，该方法绿色、可再现、生态友好、反应时间更短、成本低，形成具有更好抗菌活性的高度稳定的纳米粒子。
Description
技术领域
本发明涉及一种纳米银的制备方法，具体涉及一种罗望子多糖纳米银的制备方法。
背景技术
金属纳米粒子因其独特的尺寸、形状和表面体积比而得到广泛应用。贵金属纳米粒子，如银、金、铂和钯纳米粒子常被应用于物理、化学和生物方面。纳米银是一种无毒、安全的抗菌剂，对微生物有很高的毒性，对许多种类的细菌有很强的杀菌作用，但对动物细胞的毒性很低。因此，纳米银可作为抗菌和抗癌应用的纳米结构部分的良好候选物，在医学、水处理和催化方面应用较为广泛，尤其是在预防感染、伤口愈合、抗炎和作为抗生素的抗菌剂等生物应用方面具有较大的潜力。
目前，合成纳米银的方法主要包括：化学还原法、乳液聚合法、射线照射法、激光化学气相沉积法、物理吸附法、电化学方法、高压釜法、超声波法和光化学还原法等。在这些方法中，化学还原法被广泛研究，因为它具有产生纳米粒子而不聚集、产率高和制备成本低的优点，通常利用硼氢化钠、肼、甲酰胺等还原剂还原银离子，但是这些还原剂作为有毒的化学物质或不可生物降解的试剂，对环境和生物系统存在潜在的威胁，且在没有还原剂或稳定剂的条件下无法制备银纳米粒子。因此，采用绿色合成方法来制备环境友好型纳米银粒子具有一定的意义。
发明内容
本发明的目的是提供一种罗望子多糖纳米银的制备方法，解决了现有纳米银合成方法的试剂对环境有害的问题，该方法能够绿色、环保、简单、快速地合成罗望子多糖纳米银。
为了达到上述目的，本发明提供了一种罗望子多糖纳米银的制备方法，该方法包含：将浓度为4～10mg/mL罗望子多糖和浓度为0.08～0.10mol/L硝酸银于水中，混合均匀，将混合溶液在微波炉中反应，微波频率为50Hz，控制微波辐射时间为4～7min，得到罗望子多糖纳米银。
优选地，所述罗望子多糖的浓度为10mg/mL，所述硝酸银的浓度为0.08mol/L，微波辐射时间为6min。
本发明的罗望子多糖纳米银的制备方法，具有以下优点：
本发明的方法，采用罗望子多糖作为还原剂和稳定剂，能够在纳米尺度上形成了具有球形颗粒的立方体银相，该方法绿色、可再现、生态友好、反应时间更短(几分钟)、成本低，形成具有更好抗菌活性的高度稳定的纳米粒子，本发明中合成的银纳米粒子可用于医药、食品工业和传感器领域。
附图说明
图1为本发明实施例1不同微波辐射时间下反应液颜色的变化。
图2为本发明不同条件下罗望子多糖纳米银的紫外-可见吸收光谱。
图3为本发明实施例4制备的罗望子多糖纳米银的动态光散射图片。
图4为本发明实施例4制备的罗望子多糖纳米银的扫描电镜图片。
图5为本发明实施例4制备的罗望子多糖纳米银、罗望子多糖的傅里叶变换红外光谱。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
一种罗望子多糖纳米银的制备方法，以罗望子多糖为还原剂和稳定剂，在水溶液中，利用微波辐射法合成罗望子多糖纳米银，具体包含以下步骤：
将罗望子多糖和硝酸银于超纯水中，控制罗望子多糖的浓度为4mg/mL，硝酸银的浓度为0.08mol/L，利用旋涡混匀器混合均匀，将混合溶液在微波炉(型号：MS-2049UW，输入功率230V)中反应，微波频率为50Hz，控制微波辐射时间分别为30s、60s、90s、120s、150s、180s、210s、240s、270s、300s、310s、330s和360s，得到罗望子多糖纳米银，图1中产品1-产品13。
如图1所示，为本发明实施例1不同微波辐射时间下反应液颜色的变化，随着反应的进行，透明无色的溶液转化为特征性的浅黄色，最终显示黄褐色，表明形成了银纳米粒子。
实施例2
一种罗望子多糖纳米银的制备方法，与实施例1的基本相同，区别在于：微波辐射时间为7min，控制硝酸银的浓度分别为0.04mol/L、0.06mol/L、0.08mol/L、0.10mol/L和0.12mol/L。
实施例3
一种罗望子多糖纳米银的制备方法，与实施例1的基本相同，区别在于：微波辐射时间为7min，控制罗望子多糖的浓度分别为2mg/mL、4mg/mL、6mg/mL、8mg/mL和10mg/mL。
实施例4
一种罗望子多糖纳米银的制备方法，与实施例1的基本相同，区别在于：微波时间为360s，罗望子多糖的浓度为10mg/mL。
实验例1紫外可见吸收光谱(UV-Vis)的测定
将各实施例制备的罗望子多糖纳米银2mL溶液倒入5mm的石英比色池中，以蒸馏水为空白样品，利用紫外可见分光光度计测定罗望子多糖纳米银的紫外可见吸收光谱。
如图2的A所示，为本发明实施例1不同微波辐射时间下的紫外-可见吸收光谱，在425nm处出现一个强烈的峰值，证实了银纳米粒子的形成，相关文献报道在432nm处出现纳米银的吸收峰，根据米氏理论，球形银纳米粒子将显示单一的对称吸收峰，而各向异性银纳米粒子将给出两个或更多的波段。从图2的A可以看出，在240s形成足够多的峰，这又显示了在240s形成银纳米粒子。
如图2的B所示，为本发明实施例2在不同浓度硝酸银下罗望子多糖纳米银的紫外-可见吸收光谱，当硝酸银的浓度为0.04mol/L、0.06mol/L时，在432nm处未出现紫外吸收峰，当浓度达到0.08mol/L时，在432nm处出现紫外吸收峰，随着硝酸银的浓度逐渐增大，峰位越明显，当硝酸银的浓度升高至0.12mol/L时，在432nm处无吸收峰出现，说明当硝酸银的浓度较大时，会影响纳米银的产生。
如图2的C所示，为本发明实施例3在不同浓度罗望子多糖下罗望子多糖纳米银的紫外-可见吸收光谱，当浓度增大为4mg/mL时，开始出现432nm处的吸收峰，当浓度增大为10mg/mL时，纳米银的吸收峰最大。
由图2可知，微波时间为360s，硝酸银的浓度为0.08mol/L，且望子多糖的浓度为10mg/mL为制备罗望子多糖纳米银的最佳条件。
实验例2动态光散射(DLS)的测定
取一定量实施例4制备的罗望子多糖纳米银加入到石英比色皿中，设置相关参数后利用动态光散射仪测定罗望子多糖纳米银的粒径。
由图3可知，通过绿色合成得到的罗望子多糖纳米银的尺寸主要分布于100～200nm之间，表明利用这种绿色合成方法合成了高稳定、窄分布的纳米银金属颗粒。
实验例3场发射扫描电镜(SEM)的测定
利用扫描电镜观察银纳米粒子的形貌：实施例4制备的罗望子多糖纳米银样品经液氮冷冻干燥和喷金处理后，采用场发射扫描电子显微镜对样品的微观形态进行表征，加速电压设定为10kv。
银纳米粒子的高分辨率扫描电镜图像如图4所示，显示了合成银纳米粒子的扫描电镜图像，它证实了纳米银颗粒的直径相对均匀。
实验例4傅里叶变换红外光谱仪(FT-IR)的测定
将实施例4制备的罗望子多糖纳米银溶液真空干燥40h，变成粘稠状固体后，加入一定量的KBr进行压片，同理罗望子多糖固体粉末也进行压片，然后进行红外测试。
如图5所示，为本发明实施例4制备的罗望子多糖纳米银、罗望子多糖的傅里叶变换红外光谱，从傅里叶变换红外光谱可知，1394cm-1附近的峰表明存在二氧化氮基团的对称拉伸振动，证实了多糖封端的银纳米粒子的形成。红外光谱中其他突出的条带是纯多糖的特征，如1632cm-1、3433cm-1，分别对应于碳≡碳对称拉伸、–HC＝O拉伸和分子内氢键的存在。从合并的光谱来看，1394cm-1附近的较弱带收代表罗望子多糖纳米银的形成。
通过上述的紫外可见吸收光谱(UV-Vis)、动态光散射(DLS)、高分辨扫描电镜(SEM)、傅里叶变换红外光谱仪(FT-IR)表征方法证实了罗望子多糖纳米银的形成，罗望子多糖纳米银的尺寸主要分布于100～200nm之间，呈球形颗粒的立方体银相，红外光谱图中在1394cm-1附近的峰证明了罗望子多糖纳米银的形成。
尽管本发明的内容已经通过上述优选实施例作了详细介绍，但应当认识到上述的描述不应被认为是对本发明的限制。在本领域技术人员阅读了上述内容后，对于本发明的多种修改和替代都将是显而易见的。因此，本发明的保护范围应由所附的权利要求来限定。
Claims (2)
1.一种罗望子多糖纳米银的制备方法，其特征在于，该方法包含：
将浓度为4～10mg/mL罗望子多糖和浓度为0.08～0.10mol/L硝酸银于水中，混合均匀，将混合溶液在微波炉中反应，微波频率为50Hz，控制微波辐射时间为4～7min，得到罗望子多糖纳米银。
2.根据权利要求1所述的罗望子多糖纳米银的制备方法，其特征在于，所述罗望子多糖的浓度为10mg/mL，所述硝酸银的浓度为0.08mol/L，微波辐射时间为6min。
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