CN114518393A - 一种gnp-cnt印刷电极及其制备方法和应用 - Google Patents
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Abstract
本案涉及一种GNP‑CNT印刷电极及其制备方法和应用，在碳印刷电极基础上，采用水性石墨烯纳米片/碳纳米管纳米传感涂料修饰得到GNP‑CNT印刷电极。本发明通过碳纳米技术简便地构建工作电极，CNT以单分散的状态分布在GNP纳米薄片之间，形成了由纳米管桥连纳米片的三维导电网络结构形貌，有利于形成高电子传输通道；具有大比表面，有效地增大电极反应速率；纳米涂料采用水性丙稀酸树脂作为粘结物质，具有亲水带负电特性，有利于多巴胺在电极表面进行静电吸附扩散；DA浓度为0.4～40μM范围呈现良好的线性关系，同时对其它神经介质如尿酸、抗坏血酸具有优异的抗干扰性，使准确、快速、简便测试多巴胺成为可能。
Description
技术领域
本发明涉及电化学和纳米分析检测技术领域，具体涉及一种GNP-CNT印刷电极及其制备方法和应用。
背景技术
多巴胺(DA)是人类和哺乳动物重要的神经递质，在肾脏、血管、消化系统、免疫系统和中枢神经系统中发挥着重要作用。低水平的DA与许多病理事件密切相关，如心力衰竭、帕金森病和神经肌肉紊乱。因此，迫切需要开发高效、快速、灵敏的DA检测方法有助于对疾病的早期诊断与治疗。目前测定DA的方法主要有荧光分析法、酶联法、气相色谱以及高效液相色谱法。但上述方法存在测试方法繁琐、所用仪器昂贵、重复性差等问题，因此，这些方法还未能推广到医院临床应用。电化学分析方法由于快速、灵敏已经引起科学研究与临床检测的广泛兴趣，但文献报道需要构建特殊的工作电极材料才能测定DA，复杂的电极制作限制了电化学传感方法的临床应用。
发明内容
针对现有技术中的不足之处，本发明提出了一种利用碳纳米技术简便地构建工作电极，制得的印刷电极能够快速测定血液中的多巴胺，很好的克服现有技术中存在的造价昂贵、灵敏度低等缺点。
为实现上述目的，本发明提供如下技术方案：
一种GNP-CNT印刷电极的制备方法，其特征在于，包括如下步骤：
1)取超分散剂DC-02加入水搅拌溶解后，加入碳纳米管(CNT)，以1500r/min的转速分散10-15分钟；砂磨6-7小时；根据体系粘度分步加入石墨烯纳米片(GNP)，加完后继续研磨10小时，得石墨烯/碳纳米管水性纳米悬浮液；
2)将82～85份的石墨烯/碳纳米管纳米悬浮液、18～15份的水性丙烯酸树脂、0.1～0.3份的流平剂和0.1～0.3份的润湿分散剂混合制得水性纳米涂料；
3)采用点胶机将所述纳米涂料涂布在碳印刷电极的工作电极上，湿膜厚度为9～13μm，于80℃烘干后得到石墨烯/碳纳米管纳米涂料修饰印刷电极，即GNP-CNT印刷电极。
优选地，所述步骤1)中各原料组成如下：水75～80份、超分散剂DC-022～5份、石墨烯纳米片16～18份、碳纳米管1.4～2.3份。
优选地，所述步骤3)的工作电极中参比电极为银/氯化银电极，对电极为碳电极。
本发明提供一种如上所述的制备方法制得的GNP-CNT印刷电极。
本发明进一步提供一种如上所述的GNP-CNT印刷电极的应用，是采用所述GNP-CNT印刷电极，以及电化学工作站测试人多巴胺浓度。
本发明制备的石墨烯纳米片与碳纳米管复合电极(印刷电极的工作电极)，具有超高导电性、与多巴胺强π-π相互作用以及良好的亲水性，结果使得DA浓度处于0.4～40μM范围呈现非常良好的线性关系，同时对其它神经介质如尿酸、抗坏血酸具有优异的抗干扰性，使准确测试DA浓度成为可能。
与现有技术相比，本发明的有益效果是：本发明通过碳纳米技术简便地构建工作电极，制备方法简单，原料易得，且具有如下特点：
1、CNT以单分散的状态分布在GNP纳米薄片之间，形成了由纳米管桥连纳米片的三维导电网络结构形貌，有利于形成高电子传输通道；
2、形成微纳米表面具有大比表面，有效地增大电极反应速率；
3、CNT与GNP具有大π结构与检测物质DA可以形成电子给体-电子受体相互作用，对多巴胺氧化具有催化作用；
4、纳米涂料采用水性丙稀酸树脂作为粘结物质，具有亲水带负电特性，有利于DA在电极表面进行静电吸附扩散。
附图说明
为了更清楚地说明本发明具体实施方式或现有技术中的技术方案，下面将对具体实施方式或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图是本发明的一些实施方式，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1为GNP-CNT分散液的TEM图。
图2为水性纳米GNP-CNT涂膜的SEM图。
图3为GNP-CNT印刷电极测试DA的DPV图。
图4为GNP-CNT印刷电极测试DA的线性拟合图。
图5为GNP-CNT印刷电极测试人血清111#与112#样的DA浓度的电流电位图。
图6为GNP-CNT印刷电极抗干扰性能的DPV测试图。
具体实施方式
下面将结合附图对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例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。
此外，下面所描述的本发明不同实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互结合。
实施例
1)制备稳定的GNP-CNT纳米悬浮液，其组成包括水重量组成百分比：80；超分散剂DC-02：5；GNP：17.78；CNT：2.22。制备工艺：取配方量水加入DC-02搅拌溶解后，加入CNT，高速分散(1500r/min)12分钟；砂磨6小时；分三次加入GNP砂磨，每次间隔2小时，加完GNP后进一步研磨10小时。
2)制备GNP-CNT纳米涂料，上述GNP-CNT纳米悬浮液(固含量20％)：84.11克；水性丙烯酸酯树脂(固含量35％)：15.89克；流平剂：0.2克；润湿分散剂：0.15克。
3)GNP-CNT纳米涂料修饰印刷电极，在碳印刷电极的工作电极上(参比电极为银/氯化银电极，对电极为碳电极)采用点胶机涂膜，湿膜厚度为9-13μm厚度，80℃烘干后得到GNP-CNT印刷电极。
其中超分散剂DC-02(购买于扬州市维纳复合材料科技有限公司)的结构式为：
R为芳香基，主链具有疏水性，侧链具有亲水性；水性丙烯酸酯树脂的结构式为
具有亲水带负电特性，而DA带正电荷，有利于DA在电极表面进行静电吸附扩散。
如图1显示了本发明GNP-CNT分散液的TEM图像；从图中可以看出CNT呈现良好的分散状态并与GNP纳米片形成三维网络结构分布。图2则显示了本发明水性纳米GNP-CNT涂膜的SEM图像；说明了GNP与CNT形成了均匀分散的微纳形貌分布。
验证制得的GNP-CNT印刷电极对DA的电催化性能：
检测DA浓度范围在0.4μM～40μM，峰值电流随浓度的DPV图(图3)，从图中可以看到峰值电流随浓度增大而增大。对其进行线性拟合得到图4，本发明制得的GNP-CNT印刷电极对DA具有很好的线性，检测限为3.14×10-7M，线性方程为IP(μA)＝0.33744C(μM)+0.11425。
应用：
将40μL的人血清，滴在上述制备的GNP-CNT印刷电极的工作电极上，采用电化学工作站测试人血清111#与112#样的DA浓度。测试结果如图5所示，根据图4模拟的线性方程：111#与112#样的DA浓度分别为7.71μM与5.78μM。
干扰性测试：
如图6显示了本发明制备的GNP-CNT印刷电极测试10μM DA，10μM AA以及10μM UA的DPV图。说明DA的检测对抗坏血酸与尿酸具有优异的抗干扰性能。
对比试验：
作为对比，本案同时进行了直接采用碳印刷电极测试人血清111#与112#样的DA浓度，但在DPV图上没有任何信号；以及在不加水性丙烯酸酯的情况下制备GNP-CNT印刷电极，在此情况下制得的电极膜不稳定，检测可靠性不能满足临床应用的要求。
尽管本发明的实施方案已公开如上，但其并不仅仅限于说明书和实施方式中所列运用，它完全可以被适用于各种适合本发明的领域，对于熟悉本领域的人员而言，可容易地实现另外的修改，因此在不背离权利要求及等同范围所限定的一般概念下，本发明并不限于特定的细节和这里示出与描述的图例。
Claims (4)
1.一种GNP-CNT印刷电极的制备方法，其特征在于，包括如下步骤：
1)将2～5份超分散剂DC-02加75～80份水搅拌溶解后，加入1.4～2.3份碳纳米管，以1500r/min的转速分散10-15分钟；砂磨6-7小时；分次加入16～18份石墨烯纳米片，加完后继续研磨10小时，得石墨烯/碳纳米管纳米悬浮液；
2)将82～85份的石墨烯/碳纳米管纳米悬浮液、15～18份的水性丙烯酸树脂、0.1～0.3份的流平剂和0.1～0.3份的润湿分散剂混合制得纳米涂料；
3)采用点胶机将所述纳米涂料涂布在碳印刷电极的工作电极上，湿膜厚度为9～13μm，烘干后得到石墨烯/碳纳米管纳米涂料修饰印刷电极，即GNP-CNT印刷电极。
2.如权利要求1所述的GNP-CNT印刷电极的制备方法，其特征在于，所述步骤3)的工作电极中参比电极为银/氯化银电极，对电极为碳电极。
3.一种如权利要求1或2所述的制备方法制得的GNP-CNT印刷电极。
4.一种如权利要求3所述的GNP-CNT印刷电极的应用，其特征在于，采用所述GNP-CNT印刷电极，通过电化学工作站测定多巴胺。
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| CN103308574A (zh) * | 2013-05-21 | 2013-09-18 | 上海师范大学 | 一种碳纳米管-石墨烯复合膜修饰的电化学传感器及其制备方法和应用 |
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