CN107372600B - 光驱动型纳米抗菌剂及其制备方法 - Google Patents
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Abstract
本发明涉及光驱动型纳米抗菌剂及其制备方法，步骤为：将柠檬酸加热反应得到橙色固体；加入NaOH水溶液超声处理至固体溶全部溶解后，调节溶液pH为7；将所得液体在超纯水中透析得石墨烯量子点溶液；干燥后加入二甘醇中超声处理；加入硬脂酸锌反应得到深棕色液体；产物用甲苯离心洗涤，在超纯水中透析，过滤去除悬浮物得纳米抗菌剂。与传统抗菌剂相比，本发明所制备的纳米抗菌剂具有安全环保、抗菌效果好，耐药性强等优点，采用本发明所制备的纳米抗菌剂在100w的紫外光下照射1min，即可杀死99.78%的大肠杆菌。
Description
技术领域
本发明涉及一种新型高效抗菌剂，具体涉及光驱动型纳米抗菌剂及其制备方法。
背景技术
随着经济、工业的发展，能源危机和环境污染成为当今科技领域的两大主题。2013年“雾霾”成为年度关键词，该年1月北京仅有5天不是雾霾天。2016年，“雾霾”已经从“雾锁京城”发展为“十面埋伏”，全国17个省区市均受到雾霾的影响。瑞典哥德堡大学的研究人员发现北京雾霾天气中含耐药基因的细菌群落可达64.4种。各类细菌感染，特别是一些耐药细菌的产生，对人类健康带来了极大的威胁。因此，新型高效抗菌剂的研究迫在眉睫。
近年来，随着纳米技术的不断发展，出现了一批包括纳米Ag、纳米TiO2、纳米ZnO在内的无机纳米抗菌材料。与传统抗菌材料相比，纳米材料具有安全可靠、无毒、无污染，不产生耐药性、耐热性强等优点。其中，纳米ZnO因具有氧化还原电位高、激子结合能大(～60meV)、物理化学稳定性较好、廉价无毒等特点，成为目前研究最多和应用最广的抗菌材料之一。相关研究表明：纳米ZnO对革兰氏阴性菌和革兰氏阳性菌都有较强的抗菌性能，且其抗菌性能与形貌尺寸有较大的关系。但是，作为一种光催化型抗菌剂，ZnO本身存在禁带宽度大、光生电子-空穴对易复合等问题，制约了其应用范围。
发明内容
本发明的目的是提供光驱动型纳米抗菌剂及其制备方法，避免各类细菌感染，特别是一些耐药细菌的产生。
本发明所采用的技术方案为：
光驱动型纳米抗菌剂的制备方法，其特征在于：
包括以下步骤：
步骤一：称取3～6g柠檬酸加入三口烧瓶中，加热到200℃反应20～50min，得到橙色固体；
接着，在搅拌状态下缓慢加入NaOH水溶液，NaOH加入量为1g，超声处理至固体全部溶解后，逐渐滴加HCl水溶液调节溶液 pH为7；
最后，将所得液体在超纯水中透析1天，即得石墨烯量子点溶液；
步骤二：将步骤一所得石墨烯量子点溶液干燥后，称取0.05～0.3g 石墨烯量子点加入二甘醇中超声处理20～60min，二甘醇含量为120-360mL；
接着，将其转移至带有回流冷凝管和电动搅拌器的三口烧瓶中，缓慢加入 0.5～0.9 g硬脂酸锌， 160～220℃温度下反应时间1～3h，得到深棕色液体；
产物用甲苯离心洗涤3次后，在超纯水中透析2天，过滤去除悬浮物，即得纳米抗菌剂。
所得纳米抗菌剂的尺寸为20～50nm。
所得纳米抗菌剂使用时，与所需处理的菌液混合，在光源下光照1-30min，即可完成杀菌处理；
所述光源的功率为30-1000w，激发波长为300-500nm。
所述菌液种类为大肠杆菌、金黄色葡萄球菌、白色念珠菌或霉菌。
步骤一中：
NaOH水溶液的质量体积分数为10-40 mg/mL；
HCl水溶液的摩尔体积分数为2 -4mol/L。
如所述的制备方法制得的光驱动型纳米抗菌剂。
本发明具有以下优点：
与传统抗菌剂相比，本发明所制备的纳米抗菌剂具有安全环保、抗菌效果好、耐药性强等优点，采用本发明所制备的纳米抗菌剂在100w的紫外光下照射1min，即可杀死99.78%的大肠杆菌。
附图说明
图1：本发明所制备的纳米抗菌剂。(a) 为TEM照片，(b)为粒径分布图。
图2：本发明所制备的纳米抗菌剂在100w紫外灯照射不同时间下对大肠杆菌的抗菌性能测试结果。
具体实施方式
下面结合具体实施方式对本发明进行详细的说明。
本发明涉及的光驱动型纳米抗菌剂的制备方法，包括以下步骤：
步骤一：称取3～6g柠檬酸加入三口烧瓶中，加热到200℃反应20～50min，得到橙色固体；
接着，在搅拌状态下缓慢加入NaOH水溶液，NaOH加入量为1g，超声处理至固体溶全部溶解后，逐渐滴加HCl水溶液调节溶液 pH为7； NaOH水溶液的质量体积分数为10-40 mg/mL；HCl水溶液的摩尔体积分数为2 -4mol/L；
最后，将所得液体在超纯水中透析1天，即得石墨烯量子点（GQD）溶液。
步骤二：将步骤一所得石墨烯量子点溶液干燥后，称取0.05～0.3g 石墨烯量子点加入二甘醇中超声处理20～60min，二甘醇含量为120-360mL；
接着，将其转移至带有回流冷凝管和电动搅拌器的三口烧瓶中，缓慢加入 0.5～0.9 g硬脂酸锌， 160～220℃温度下反应时间1～3h，得到深棕色液体；
产物用甲苯离心洗涤3次后，在超纯水中透析2天，过滤去除悬浮物，即得纳米抗菌剂，所得纳米抗菌剂的尺寸为20～50nm。
所得纳米抗菌剂使用时，与所需处理的菌液混合，在光源下光照1-30min，即可完成杀菌处理；所述光源的功率为30-1000w，激发波长为300-500nm。所述菌液种类为大肠杆菌、金黄色葡萄球菌、白色念珠菌、霉菌等。
采用本发明所制备的纳米抗菌剂在100w的紫外光下照射1min，即可杀死99.78%的大肠杆菌。
实施例1：
步骤一：称取4g柠檬酸加入三口烧瓶中，加热到200℃反应一定时间，得到橙色固体；接着，在搅拌状态下缓慢加入100mL 10 mg/mL NaOH水溶液，超声处理一段时间至固体溶全部溶解后，逐渐滴加2 mol/L HCl调节溶液 pH为7；最后，将所得液体在超纯水中透析1天，即得GQD 溶液；
步骤二：将上述所得GQD溶液干燥后，称取0.1g GQD加入120mL二甘醇中超声处理30min；接着，将其转移至带有回流冷凝管和电动搅拌器的三口烧瓶中，缓慢加入 0.768 g的硬脂酸锌，200℃反应2h得到深棕色液体，产物用甲苯离心洗涤3次后，用超纯水透析2天，并过滤出去悬浮物，即得所述的纳米抗菌剂 。
步骤三：取1mg/mL上述纳米抗菌剂90μL，与10μL大肠杆菌菌悬液混合(菌悬液浓度：600 nm处OD值为0.1)，混合液在100w的紫外灯下光照2min ，即可完成杀菌处理。
实施例2：
步骤一：称取5g柠檬酸加入三口烧瓶中，加热到200℃反应35min，得到橙色固体；接着，在搅拌状态下缓慢加入50mL 20 mg/mL NaOH水溶液，超声处理30min至固体溶全部溶解后，逐渐滴加4 mol/L HCl调节溶液 pH为7；最后，将所得液体在超纯水中透析1天，即得GQD 溶液；
步骤二：将上述所得GQD溶液干燥后，称取0.2g GQD加入200mL二甘醇中超声处理40min；接着，将其转移至带有回流冷凝管和电动搅拌器的三口烧瓶中，缓慢加入1.536g硬脂酸锌，180 ℃反应2h得到深棕色液体，产物用甲苯离心洗涤3次后，用超纯水透析2天，并过滤出去悬浮物，即得所述的纳米抗菌剂 。
步骤三：取2mg/mL上述纳米抗菌剂90 μL，与10μL金黄色葡萄球菌 (菌悬液在 600nm的OD值为0.1)，在200w、激发波长为365nm 光源下，光照5min，即可完成杀菌处理。
实施例3：
步骤一：称取4g柠檬酸加入三口烧瓶中，加热到200℃反应33min，得到橙色固体；接着，在搅拌状态下缓慢加入100mL 10 mg/mL NaOH水溶液，超声处理35min至固体溶全部溶解后，逐渐滴加4 mol/L HCl调节溶液 pH为7；最后，将所得液体在超纯水中透析1天，即得GQD 溶液；
步骤二：将上述所得GQD溶液干燥后，称取0.1g GQD加入150mL二甘醇中超声处理30min；接着，将其转移至带有回流冷凝管和电动搅拌器的三口烧瓶中，缓慢加入0.768g硬脂酸锌，190 ℃反应2h得到深棕色液体，产物用甲苯离心洗涤3次后，用超纯水透析2天，并过滤出去悬浮物，即得所述的纳米抗菌剂 。
步骤三：取1mg/mL上述纳米抗菌剂90 μL，与10μL大肠杆菌 (菌悬液在 600 nm的OD值为0.1)，在200w紫外光下光照3min，即可完成杀菌处理。
实施例4：
步骤一：称取4.5g柠檬酸加入三口烧瓶中，加热到200℃反应40min，得到橙色固体；接着，在搅拌状态下缓慢加入25mL 40 mg/mL NaOH水溶液，超声处理30min至固体溶全部溶解后，逐渐滴加4 mol/L HCl调节溶液 pH为7； 最后，将所得液体在超纯水中透析1天，即得GQD 溶液；
步骤二：将上述所得GQD溶液干燥后，称取0.3g GQD加入360mL二甘醇中超声处理40min；接着，将其转移至带有回流冷凝管和电动搅拌器的三口烧瓶中，缓慢加入2.36g硬脂酸锌，205 ℃反应2h得到深棕色液体，产物用甲苯离心洗涤3次后，用超纯水透析2天，并过滤出去悬浮物，即得所述的纳米抗菌剂 。
步骤三：取1mg/mL上述纳米抗菌剂90 μL，与10μL白色念珠菌 (菌悬液在 600 nm的OD值为0.1)，在200w紫外光下光照5min，即可完成杀菌处理。
本发明的内容不限于实施例所列举，本领域普通技术人员通过阅读本发明说明书而对本发明技术方案采取的任何等效的变换，均为本发明的权利要求所涵盖。
Claims (6)
1.光驱动型纳米抗菌剂的制备方法，其特征在于：
包括以下步骤：
步骤一：称取3～6g柠檬酸加入三口烧瓶中，加热到200℃反应20～50min，得到橙色固体；
接着，在搅拌状态下缓慢加入NaOH水溶液，NaOH加入量为1g，超声处理至固体全部溶解后，逐渐滴加HCl水溶液调节溶液 pH为7；
最后，将所得液体在超纯水中透析1天，即得石墨烯量子点溶液；
步骤二：将步骤一所得石墨烯量子点溶液干燥后，称取0.05～0.3g 石墨烯量子点加入二甘醇中超声处理20～60min，二甘醇含量为120-360mL；
接着，将其转移至带有回流冷凝管和电动搅拌器的三口烧瓶中，缓慢加入 0.5～0.9 g硬脂酸锌， 160～220℃温度下反应时间1～3h，得到深棕色液体；
产物用甲苯离心洗涤3次后，在超纯水中透析2天，过滤去除悬浮物，即得纳米抗菌剂。
2.根据权利要求1所述的光驱动型纳米抗菌剂的制备方法，其特征在于：
所得纳米抗菌剂的尺寸为20～50nm。
3.根据权利要求1所述的光驱动型纳米抗菌剂的制备方法，其特征在于：
所得纳米抗菌剂使用时，与所需处理的菌液混合，在光源下光照1-30min，即可完成杀菌处理；
所述光源的功率为30-1000w，激发波长为300-500nm。
4.根据权利要求3所述的光驱动型纳米抗菌剂的制备方法，其特征在于：
所述菌液种类为大肠杆菌、金黄色葡萄球菌、白色念珠菌或霉菌。
5.根据权利要求1所述的光驱动型纳米抗菌剂的制备方法，其特征在于：
步骤一中：
NaOH水溶液的质量体积分数为10-40 mg/mL；
HCl水溶液的摩尔体积分数为2 -4mol/L。
6.如权利要求1所述的制备方法制得的光驱动型纳米抗菌剂。
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