CN105606676A - 掺氮还原石墨烯-AuAg双金属纳米复合物的制备及其在电化学检测盐酸柔红霉素中的应用 - Google Patents
掺氮还原石墨烯-AuAg双金属纳米复合物的制备及其在电化学检测盐酸柔红霉素中的应用 Download PDFInfo
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Abstract
本发明公开了一种掺氮还原石墨烯-AuAg双金属纳米复合材料（NG-AuAg）的制备方法及其应用，包括如下步骤：制备掺氮石墨烯-Au（NG-Au）悬浮液。向上述NG-Au悬浮液中加入60？μL？0.1M？AgNO3和120？μL？0.1M？AA，然后移入25mL圆底烧瓶中110℃加热回流1h。最后用超纯水离心洗涤3次。得到的沉淀在60℃下真空干燥一夜，即制得产物。
Description
技术领域
本发明属于纳米复合材料的领域，具体涉及一种掺氮还原石墨烯-AuAg双金属纳米复合材料的制备方法及其应用。
背景技术
石墨烯因其独特的2维（2D）结构、优异的机械性能、卓越的电化学性能和大的比表面积，已经应用于许多领域，比如传感器、光催化、电池和超级电容器。用化学元素掺杂石墨烯可以调节石墨烯的能带结构、改变其电化学性质、调整其表面化学性质和改变石墨烯的带隙宽度。在众多的掺杂原子中，N具有理想的原子大小并含有5个共价键可以和C形成强共价键，是非常优秀的化学掺杂元素。目前，掺氮石墨烯主要有以下合成方法，氮等离子体处理法、化学气相沉积法（CVD）、电焦耳热法、热退火法和在N2H4或NH3存在的条件下水热还原GO法。但是这些方法复杂、昂贵、难以大规模生产。而且，在还原过程中，GO的还原程度也会影响石墨烯材料的电子传导。除了掺氮，石墨烯复合材料也是现在的研究热门。在石墨烯上引入纳米贵金属可以增加石墨烯的电化学性能。而且，独特的核壳双金属纳米颗粒因其更好的催化性能和选择性能也吸引了越来越多研究者的关注。目前为止，简单的一步水热法合成掺氮石墨烯-纳米贵金属复合材料还没有文献报道。
目前癌症是世界上死亡率第二的疾病，严重的影响人们的健康，对癌症的提前预防以及治疗是一项十分艰巨的任务。药物治疗是治疗癌症的三大治疗法之一，虽然药物治疗法已有很久的历史，但化学药物治疗法仅有四十年的历史。虽然药物治疗比放射治疗和手术治疗的历史要短得多，科学家们已经发现了多种疗效较好的抗癌药物。小分子抗癌药物不仅能够深入到传统癌症治疗方法难以攻克的皮肤癌、淋巴癌和血癌等领域，而且减轻了患者的痛苦。人们致力于研究各种小分子抗癌药物的药理，在基因和蛋白质层次上可以专属性地识别正常细胞和癌细胞，进一步推进了对癌症病发的了解。盐酸柔红霉素（Daunorubicinhydrochloride）作为一种小分子的抗癌药物，其制剂主要用于恶性淋巴瘤、乳腺癌和急性白血病的治疗。它的药理作用是通过和DNA分子结合，抑制核酸合成而导致癌细胞死亡。
发明内容
为克服现有技术中的不足，本发明的目的是提供一种掺氮还原石墨烯-AuAg双金属纳米复合材料（NG-AuAg）的制备制备方法及其应用，致力于结合核壳结构AuAg与石墨烯的诸多优点，构建一种检测抗癌药物盐酸柔红霉素（DNR）的新型高性能电化学传感器。本专利采用简单的一步水热法、环境友好的(NH4)2CO3作为还原剂和氮掺杂剂，合成了掺氮石墨烯-纳米金复合物（NG-Au）。在这一步中，(NH4)2CO3不仅掺杂还原了GO，同时还将HAuCl4还原为AuNPs。然后在水热条件下使用环境友好型还原剂AA制得了掺氮还原石墨烯-AuAg双金属纳米复合物(NG-AuAg)。而且，掺氮还原石墨烯-AuAg双金属纳米复合物对抗癌药物盐酸柔红霉素（DNR）有很好的电化学响应效果。从而为DNR的临床用药提供了一种简单有效的检测方法。
一种掺氮还原石墨烯-AuAg双金属纳米复合材料（NG-AuAg）的制备制备方法，包括以下步骤：步骤一：首先根据现有技术合成GO，然后将制备的GO分散到超纯水中，得到GO水溶液，后向得到的GO水溶液中加入质量分数为1%的HAuCl4超声搅拌0.5h，再加入(NH4)2CO3搅拌使其溶解，然后将混合液移入高压反应釜中130℃反应10h，最后用超纯水离心洗涤多次，直至上层清夜的pH为7左右，向沉淀中加入超纯水，得到1mgmL-1NG-Au悬浮液。
步骤二：向上述NG-Au悬浮液中加入60μL0.1MAgNO3和120μL0.1MAA，然后在110℃下加热回流1h，自然冷却后用超纯水离心洗涤3次，得到的沉淀在60℃下真空干燥一夜，即制得掺氮还原石墨烯-AuAg双金属纳米复合材料。
一种掺氮还原石墨烯-AuAg双金属纳米复合材料的应用，用于检测抗癌药物盐酸柔红霉素。
一种掺氮还原石墨烯-AuAg双金属纳米复合材料用于检测抗癌药物盐酸柔红霉素的方法，包括以下步骤：
步骤一、以5μL1mg/mLNG-Au-Ag纳米复合材料修饰的玻碳电极为工作电极，Ag/AgCl为参比电极，铂电极为对电极，用差分脉冲伏安法测定0.1MpH6.5PBS中含有的不同的DNR标准浓度；
步骤二、根据步骤一得到的检测结果，作出DNR浓度与响应电流的线性关系图，得到线性范围；
步骤三、在相同检测条件下，测出待测DNR溶液的电流响应值，带入步骤二得到的线性方程中，计算待测DNR浓度。
所述检测抗癌药物盐酸柔红霉素的方法，检测抗癌药物盐酸柔红霉素的线性范围为0.01-15μgmL-1。
本发明的有益技术效果为：首次一步法合成了掺氮石墨烯-Au纳米复合物，之后又在此基础上制备了掺氮石墨烯-AuAg核壳双金属纳米复合物。
与现有电化学方法检测盐酸柔红霉素的技术相比，本发明的检测效果更好，且操作简单，成本低，应用前景广阔。
附图说明
图1为GO(A)的TEM图；
图2为NG-Au的TEM图；
图3为NG-AuAg的TEM图；
图4为bare/GCE，(b)NG/GCE，(c)NG-Au/GCE和(d)NG-AuAg/GCE在含有4μgmL-1DNR的0.1MpH6.5PBS中的CVs图，扫速：100mVs-1；
图5为NG-AuAg/GCE修饰电极在含有0（a），2(b)，4(c)，6(d)，8(e)和10（f）μgmL-1DNR的0.1MpH7PBS电解液中的CVs图，扫速：100mVs-1。
具体实施方式
实施例1
首先根据文献合成GO，然后将5mg制备的GO分散到5mL超纯水中，得到GO水溶液。之后向得到的GO水溶液中加入250μL1%(w/w)HAuCl4超声搅拌0.5h，之后加入500mg(NH4)2CO3搅拌使其溶解，然后将混合液移入高压反应釜中130℃反应10h。最后用超纯水离心洗涤多次，直至上层清夜的pH为7左右。向沉淀中加入5mL超纯水，得到1mgmL-1NG-Au悬浮液。向上述NG-Au悬浮液中加入60μL0.1MAgNO3和120μL0.1MAA，然后移入25mL圆底烧瓶中110℃加热回流1h。最后用超纯水离心洗涤3次。得到的沉淀在60℃下真空干燥一夜，即制得产物(NG-AuAg)。如图1表明，制备的GO呈现出褶皱的薄片状结构。图2表明，AuNPs均匀的分散在掺氮还原石墨烯的表面。从图3可以看出，掺氮还原石墨烯上的纳米颗粒明显比单独的纳米金颗粒尺寸大。以上TEM图证明在掺氮石墨烯表面成功制备了AuAg核壳结构纳米颗粒。
实施例2
分别用相同条件下制得的复合材料：掺氮石墨烯（NG）、掺氮石墨烯-Au（NG-Au）、NG-AuAg和裸电极修饰玻碳电极后，采用三电极体系（玻碳电极为工作电极，铂电极为对电极，Ag/AgCl电极为参比电极）在含有4μgmL-1DNR的0.1MpH6.5PBS溶液中进行循环伏安法测试，扫速为100mVs-1，电压范围为-0.2～-0.8V。如图4所示。发现：裸电极基本没有峰电流，说明裸电极不适合DNR的测定。掺氮石墨烯修饰电极明显比裸电极的电流大，说明掺氮可以增加石墨烯的电化学性能。而且曲线b、c的峰电流都没有曲线d中的峰电流大，进一步体现了石墨烯与核壳结构纳米颗粒AuAg之间的协同作用，使得NG-AuAg/GCE修饰电极对于测定DNR具有优越性。
实施例3
NG-AuAg/GCE修饰电极检测DNR的电化学行为：采用三电极体系（玻碳电极为工作电极，铂电极为对电极，Ag/AgCl电极为参比电极）在含有0(a)、2(b)、4(c)、6(d)、8(e)和10(f)μgmL-1DNR的0.1MpH7PBS溶液中进行循环伏安法测试，扫速为100mVs-1，电压范围为-0.2～-0.8V。如图5所示，比较曲线a、b可以发现，该修饰电极在空白的0.1MpH7PBS中没有出现氧化还原峰，但是添加了2μgmL-1DNR后，在-0.58V和-0.62V出现了一组氧化还原峰，而且，随着添加的DNR的浓度增大，这组氧化还原峰也逐渐增大，充分说明了该修饰电极对DNR有很好的电催化活性。
Claims (5)
1.一种掺氮还原石墨烯-AuAg双金属纳米复合材料的制备制备方法，包括以下步骤：
步骤一：首先根据现有技术合成GO，然后将制备的GO分散到超纯水中，得到GO水溶液，后向得到的GO水溶液中加入质量分数为1%的HAuCl4超声搅拌0.5h，再加入(NH4)2CO3搅拌使其溶解，然后将混合液移入高压反应釜中130℃反应10h，最后用超纯水离心洗涤多次，直至上层清夜的pH为7左右，向沉淀中加入超纯水，得到1mgmL-1NG-Au悬浮液。
2.步骤二：向上述NG-Au悬浮液中加入60μL0.1MAgNO3和120μL0.1MAA，然后在110℃下加热回流1h，自然冷却后用超纯水离心洗涤3次，得到的沉淀在60℃下真空干燥一夜，即制得掺氮还原石墨烯-AuAg双金属纳米复合材料。
3.一种根据权利要求1所述方法制得的掺氮还原石墨烯-AuAg双金属纳米复合材料的应用，用于检测抗癌药物盐酸柔红霉素。
4.一种根据权利要求1所述方法制得的掺氮还原石墨烯-AuAg双金属纳米复合材料用于检测抗癌药物盐酸柔红霉素的方法，包括以下步骤：
步骤一、以5μL1mg/mLNG-Au-Ag纳米复合材料修饰的玻碳电极为工作电极，Ag/AgCl为参比电极，铂电极为对电极，用差分脉冲伏安法测定0.1MpH6.5PBS中含有的不同的DNR标准浓度；
步骤二、根据步骤一得到的检测结果，作出DNR浓度与响应电流的线性关系图，得到线性范围；
步骤三、在相同检测条件下，测出待测DNR溶液的电流响应值，带入步骤二得到的线性方程中，计算待测DNR浓度。
5.根据权利要求4所述的检测抗癌药物盐酸柔红霉素的方法，其特征在于检测抗癌药物盐酸柔红霉素的线性范围为0.01-15μgmL-1。
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