基于铜/氧化铜纳米材料的非酶葡萄糖传感器研究
摘要
糖尿病（Diabetes）是一种代谢紊乱综合症，是世界公共健康问题。患病率在全球以惊人速度增加的糖尿病仍然是受到人们日益关注的疾病。该疾病是导致世界上死亡和残疾的主要原因之一。糖尿病一旦控制不好会引起多种并发症。这些并发症通过严格的控制个人血糖浓度水平是能够被大大地减少发病的程度，甚至不发病。因此，严格监测血糖水平对糖尿病的诊断和管理密不可分，它的检测具有重要的临床意义。
时至今，葡萄糖传感器已经经历了基于酶的和非酶的传感器的发展。虽然基于酶的葡萄糖传感器经历了三代的演变发展，但是它们都摆脱不了酶所固有的不稳定性的缺点。此外，酶的应用还受其他条件的制约，如pH、温度、湿度和对氧气的依赖性等。加之，酶的昂贵价格，使得传感器始终面临着构建成本的问题。基于以上因素，非酶葡萄糖传感器的研究受到了极大的关注。为了发展灵敏的非酶葡萄糖传感器，已有大量文献报道了已经探索的一系列各种金属和金属氧化物、双金属纳米材料或者合金、以及金属/金属氧化物-碳纳米管复合材料也已提出。尽管粒径大的材料和纳米尺度的材料都已经用于探索电催化葡萄糖的氧化作用，但是纳米结构的金属氧化物带或不带其他掺杂物质（如贵金属或导电金属氧化物）在非酶葡萄糖的检测方面还没有被系统地研究。一般认为纳米尺度的金属氧化物的性质不同于块体材料，这是由于纳米材料非常小的尺寸，大的表面积与体积比，更大程度的结晶度和德拜长度（λD）的原因。因此推测，纳米结构的金属氧化物或者金属氧化物复合材料，大大提高了灵敏度和/或者选择性，并且在电化学传感器的应用上（如葡萄糖的检测）也可能最大限度的减少毒性中间体的吸附，这将在本论文中进行证明。本研究以基于铜/氧化铜的纳米材料构建非酶葡萄糖传感器，并应用这种传感器在碱性条件和中性条件下均成功实现了对葡萄糖的检测，有望成为在医疗诊断、
生物过程和食品工业方面具有潜在应用的理想材料。开展主要研究工作如下：（1）由一种简易、尺寸可控的湿化学法合成一种能实现超灵敏的和选择性好的非酶葡萄糖传感器的Cu纳米线（CuNWs）催化剂。对所制备的CuNWs的形态、
结晶度和表面性质分别通过SEM、XRD和XPS等手段进行表征。结果表明，CuNWs粒度分布均匀，并具有大的比表面积（＞200）。CuNWs对葡萄糖的电氧化反应作用的电化学性质通过循环伏安法进行了充分研究。其优越的导电性和突出的催化性能，对葡萄糖的计时安培检测，由CuNWs修饰的玻碳电极展现出非凡的检测限（可低至35nM（S/N=3）），和伴随优良灵敏度（420.3μAcm-2mM-1）的宽泛的动态范围（线性响应可达3mM）。灵敏度比对照电极高出10,000多倍。所开发的葡萄糖传感器的性能也不受氧气的制约和氯离子的毒化。此外，在干扰物的正常生理水平的浓度下，来自尿酸（UA）、抗坏血酸（AA）、醋氨酚（AP）、果糖和蔗糖的干扰可以忽略不计，证明了CuNWs修饰的玻碳电极的优异的选择性。最后，对人血清样本中葡萄糖浓度的定量检测的准确度好和精密度高，意味着CuNWs在发展具有灵敏性和选择性的非酶葡萄糖传感器的成功应用。
（2）以CuNWs和单壁碳钠米管（SWCNTs）组成的电催化剂构建成的一种新杂交复合材料为研究对象，进一步研究纳米结构的CuNWs掺杂其他物质在非酶葡萄糖的传感检测方面的应用。通过SEM、EDX和XRD分别对所制备的CuNWs-SWCNTs杂交复合材料的形态、化学组成和晶体结构进行了表征。通过循环伏安法研究了CuNWs-SWCNTs对葡萄糖电氧化反应的电催化性能，并且观察到由于CuNWs与SWCNTs之间的协同效应所增强的电化学性能。杂交复合材料对葡萄糖监测的进一步应用展现出其对血糖检测的宽泛的动态范围（89nM的检测限（S/N=3）），极好的灵敏度（637.3μAcm~(-2)mM~(-1)）以及对常规干扰物的良好的选择性。这些结果表明，CuNWs-SWCNTs杂交复合材料在多种应用中，是一种很有前途的材料。
（3）基于金属铜表面易被氧化成氧化铜，故进一步研究了氧化铜（CuO）纳米材料对检测葡萄糖的应用，并探究了分别在最大电流响应的峰电位和初始氧化过程的电位下的检测响应。CuO纳米线（CuONWs）由一个简易的反应过程制得。在CuNWs的合成方法基础上，直接将CuNWs进行高温锻烧即得CuONWs。SEM和TEM用以表征所制备的CuONWs的形态、表面性质和晶体结构。此外，XRD研究了黑色终产物的成分组成。用CuONWs构建的非酶传感器在0.05MNaOH溶液中对葡萄糖的检测表现出极好的电化学性能。该传感器在两个不同的工作电位下对葡萄糖均表现出快速的检测响应（＜5s）和宽泛的动态范围（在+0.55V工作电位下，灵敏度为556.2μA·cm~(-2)·mM~(-1)（R2=0.995）；在+0.3V工作电位下，灵敏度为107.2μA·cm~(-2)·mM~(-1)（R2=0.984））。Langmuir等温吸附理论用于拟合校准曲线。在+0.55V的峰电位下对CuONWs促进的葡萄糖的氧化反应机制和对AA、UA和AP的良好的选择性也进行了研究。此外，来自生理浓度水平的果糖和蔗糖的干扰微不足道，进一步证明了CuONWs优良的选择性。这些结果证明，CuONWs在用于葡萄糖非酶检测的具有灵敏性和选择性的传感器的发展具有巨大的潜在应用。
（4）探索了基于铜的纳米材料在中性条件下对葡萄糖的非酶传感检测。参考一种大规模的回流合成技术合成了具有明确纳米结构的氧化铜纳米花材料（CuONFs）。用CuONFs构建的非酶葡萄糖传感器实现了在中性溶液中对葡萄糖及其他碳水化合物的检测。各种技术被用来表征CuONFs的结构和组成。SEM研究所制备材料的形态；XRD研究所得终产物的晶体结构；FTIR用以确认合成过程中硝酸铜向氧化铜的完全转化。CuONFs对葡萄糖检测的电化学性能通过循环伏安法、电化学阻抗谱法和差分脉冲伏安法进行研究。研究结果显示，CuONFs对葡萄糖的检测表现出较宽的线性响应范围（可至10mM（R2=0.997）），以及良好的选择性（对干扰物UA和AA）。CuONFs所增强的传感性能也体现在对其他碳水化合物的检测上。这些结果表明CuONFs在生物传感器的发展向生理条件下对非酶碳水化合物的检测的潜在适用性。
Diabetes is a metabolic disorder and a major world health problem. As stated by International Diabetes Federation, there are over285million diabetics worldwide in2010. Due to the financial burden caused by diabetes and its serious health complications, glucose detection is incredibly important in reducing the costs of diabetes management.
Glucose sensor has already experienced the development of sensors based on enzymatic catalysts and non-enzymatic catalysts. In the past decades, three generation enzymatic glucose sensors have been developed, but they suffer from the inherent instability of the enzyme due to its pH and temperature sensitivity, and sensor performance variation due to oxygen concentration fluctuation. Additionally, the high cost of enzyme also limits the wide application of enzymatic glucose biosensors in developing countries. Due to aforementioned factors, considerable research efforts have been focused on the development of non-enzymatic glucose sensors with high sensitivity and selectivity. In order to develop sensitive non-enzymatic glucose sensors, a variety of metals and metal oxides, bimetallic nanomaterials or alloys and metals/metal oxides-CNTs composites have been explored. Although both bulk and nanoscale noble materials have been extensively explored for electrocatalyzing glucose oxidation, the nanostructured non-precious metal or metal oxides with or without dopants (e.g. noble metals or conductive metal oxide) have not been systematically investigated in the non-enzymatic glucose detection, which triggers our considerable research interests. It is generally believed that the properties of nanoscale metal or metal oxides can be very different from bulk materials, due to the extremely reduced size, large surface-to-volume ratio, greater level of crystal and the Debye length (λD) comparable to the dimensions of nanomaterials. Therefore, we hypothesize that nanostructured non-precious metal, metal oxide or metal oxide composites could greatly promote the glucose oxidation/adsorption, and thus improve the sensitivity and/or selectivity in glucose sensing, which will be demonstrated in this dissertation.
In this study, the copper-or copper oxide-based nanomaterials were used to fabricate non-enzymatic glucose sensors, which successfully detected glucose in alkaline or neutral conditions. The developed non-enzymatic glucose sensors have potential applications in medical diagnostics, biological processes and food Industry. In this dissertation, we focused on following researches:
(1) In the pursuit of more economical electrocatalysts for non-enzymatic glucose sensors, one-dimensional Cu nanowires (Cu NWs) with uniform size distribution and a large aspect ratio (>200) were synthesized by a facile, scalable, wet-chemistry approach. The morphology, crystallinity, and surface property of the as-prepared Cu NWs were examined by SEM, XRD, and XPS, respectively. The electrochemical property of Cu NWs for glucose electrooxidation was thoroughly investigated by cyclic voltammetry. In the amperometric detection of glucose, the Cu NWs modified glassy carbon electrode exhibits an extraordinary limit of detection of35nM (S/N=3) and a wide dynamic range with excellent sensitivity of420.3μA·cm-2·mM-1, which is more than10,000times higher than that of the control electrode without Cu NWs. The performance of the developed glucose sensor is also independent to oxygen concentration and free from chloride poisoning. Furthermore, the interference from uric acid, ascorbic acid, acetaminophen, fructose, and sucrose at the level of their physiological concentration were insignificant, indicating excellent selectivity. Finally, good accuracy and high precision for the quantification of glucose concentration in human serum samples implicate the applicability of Cu NWs in sensitive and selective non-enzymatic glucose detection.
(2) A novel hybrid composite based electrocatalyst consisting of copper nanowires (Cu NWs) and single-walled carbon nanotubes (SWCNTs) was introduced for glucose electrooxidation and detection in alkaline medium. The morphology, chemical composition, and crystalline structure of the as-prepared Cu NWs-SWCNTs hybrid composite were examined by SEM, EDX, and XRD, respectively. The electrocatalytic property of Cu NWs-SWNTs for glucose electrooxidation was investigated by cyclic voltammetry and enhanced performance was observed due to the synergistic effect between Cu NWs and SWCNTs. Further application of the hybrid composite for glucose monitoring shows a wide dynamic range with a limit of detection of89nM (S/N=3), an excellent sensitivity (637.3μA-cm-2·mM-1), and good selectivity against commonly interfering species. These results indicate that Cu NWs-SWCNTs hybrid composite is a promising material in various applications.
(3) Copper oxide nanowires (CuO NWs) were fabricated by a facile two-step procedure consisting of wet-chemistry synthesis and subsequent thermal treatment in air. SEM and TEM were employed to characterize the morphology, surface property, and crystal structure of the as-prepared CuO NWs, while the composition of the as-prepared CuO nanowires was investigated using XRD. The CuO NWs were further employed to construct an enzyme-free sensor with excellent performance towards the glucose detection in0.05M NaOH solution. The developed sensor showed a fast response time (less than5s), a wide dynamic range with excellent sensitivity of556.2μA-cm-2·mM-1(R2=0.995) and107.2μA-cm-2·mM-1(R2=0.984) at the working potential of+0.55V and+0.3V, respectively. The Langmuir isothermal theory was employed to fit the obtained calibration curve. The mechanisms for the glucose oxidation promoted by CuO NWs and the good selectivity against ascorbic acid, uric acid and acetaminophen at an applied potential of+0.55V were also discussed. Furthermore, the interference from fructose, and sucrose at the level of their physiological concentration were insignificant, indicating excellent selectivity. These results implicate that CuO NWs have great potential applications in the development of sensitive and selective sensors for enzyme-free detection of glucose.
(4) A reflux synthesis technique was used to synthesize CuO materials with well-defined nanostructures in large scale, which were further applied to construct an enzyme-free sensor for the detection of glucose and carbohydrates in a neutral pH solution. A variety of techniques were used to characterize these materials. Specially, scanning electron microscopy was employed to study the morphology of the as-prepared materials; X-ray diffraction was used to investigate the crystal structure of the final product; and Fourier transform infrared spectroscopy was applied to confirm the complete conversion of copper nitrate to copper oxide in the synthetic process. The electrochemical property of CuO nanoflowers for glucose detection in a neutral pH solution was investigated by cyclic voltammetry, electrochemical impedance spectroscopy, and differential pulse voltammetry, showing a wide linear range up to10mM (R2=0.997) and good selectivity against uric acid and ascorbic acid. The enhanced sensing performance of CuO nanoflowers was also observed on other carbohydrates. This is the first report to detect glucose in neutral pH using CuO. These results implicate the potential applicability of CuO nanoflowers in the development of biosensors for enzyme-free carbohydrates detection in physiological condition.
时至今，葡萄糖传感器已经经历了基于酶的和非酶的传感器的发展。虽然基于酶的葡萄糖传感器经历了三代的演变发展，但是它们都摆脱不了酶所固有的不稳定性的缺点。此外，酶的应用还受其他条件的制约，如pH、温度、湿度和对氧气的依赖性等。加之，酶的昂贵价格，使得传感器始终面临着构建成本的问题。基于以上因素，非酶葡萄糖传感器的研究受到了极大的关注。为了发展灵敏的非酶葡萄糖传感器，已有大量文献报道了已经探索的一系列各种金属和金属氧化物、双金属纳米材料或者合金、以及金属/金属氧化物-碳纳米管复合材料也已提出。尽管粒径大的材料和纳米尺度的材料都已经用于探索电催化葡萄糖的氧化作用，但是纳米结构的金属氧化物带或不带其他掺杂物质（如贵金属或导电金属氧化物）在非酶葡萄糖的检测方面还没有被系统地研究。一般认为纳米尺度的金属氧化物的性质不同于块体材料，这是由于纳米材料非常小的尺寸，大的表面积与体积比，更大程度的结晶度和德拜长度（λD）的原因。因此推测，纳米结构的金属氧化物或者金属氧化物复合材料，大大提高了灵敏度和/或者选择性，并且在电化学传感器的应用上（如葡萄糖的检测）也可能最大限度的减少毒性中间体的吸附，这将在本论文中进行证明。本研究以基于铜/氧化铜的纳米材料构建非酶葡萄糖传感器，并应用这种传感器在碱性条件和中性条件下均成功实现了对葡萄糖的检测，有望成为在医疗诊断、
生物过程和食品工业方面具有潜在应用的理想材料。开展主要研究工作如下：（1）由一种简易、尺寸可控的湿化学法合成一种能实现超灵敏的和选择性好的非酶葡萄糖传感器的Cu纳米线（CuNWs）催化剂。对所制备的CuNWs的形态、
结晶度和表面性质分别通过SEM、XRD和XPS等手段进行表征。结果表明，CuNWs粒度分布均匀，并具有大的比表面积（＞200）。CuNWs对葡萄糖的电氧化反应作用的电化学性质通过循环伏安法进行了充分研究。其优越的导电性和突出的催化性能，对葡萄糖的计时安培检测，由CuNWs修饰的玻碳电极展现出非凡的检测限（可低至35nM（S/N=3）），和伴随优良灵敏度（420.3μAcm-2mM-1）的宽泛的动态范围（线性响应可达3mM）。灵敏度比对照电极高出10,000多倍。所开发的葡萄糖传感器的性能也不受氧气的制约和氯离子的毒化。此外，在干扰物的正常生理水平的浓度下，来自尿酸（UA）、抗坏血酸（AA）、醋氨酚（AP）、果糖和蔗糖的干扰可以忽略不计，证明了CuNWs修饰的玻碳电极的优异的选择性。最后，对人血清样本中葡萄糖浓度的定量检测的准确度好和精密度高，意味着CuNWs在发展具有灵敏性和选择性的非酶葡萄糖传感器的成功应用。
（2）以CuNWs和单壁碳钠米管（SWCNTs）组成的电催化剂构建成的一种新杂交复合材料为研究对象，进一步研究纳米结构的CuNWs掺杂其他物质在非酶葡萄糖的传感检测方面的应用。通过SEM、EDX和XRD分别对所制备的CuNWs-SWCNTs杂交复合材料的形态、化学组成和晶体结构进行了表征。通过循环伏安法研究了CuNWs-SWCNTs对葡萄糖电氧化反应的电催化性能，并且观察到由于CuNWs与SWCNTs之间的协同效应所增强的电化学性能。杂交复合材料对葡萄糖监测的进一步应用展现出其对血糖检测的宽泛的动态范围（89nM的检测限（S/N=3）），极好的灵敏度（637.3μAcm~(-2)mM~(-1)）以及对常规干扰物的良好的选择性。这些结果表明，CuNWs-SWCNTs杂交复合材料在多种应用中，是一种很有前途的材料。
（3）基于金属铜表面易被氧化成氧化铜，故进一步研究了氧化铜（CuO）纳米材料对检测葡萄糖的应用，并探究了分别在最大电流响应的峰电位和初始氧化过程的电位下的检测响应。CuO纳米线（CuONWs）由一个简易的反应过程制得。在CuNWs的合成方法基础上，直接将CuNWs进行高温锻烧即得CuONWs。SEM和TEM用以表征所制备的CuONWs的形态、表面性质和晶体结构。此外，XRD研究了黑色终产物的成分组成。用CuONWs构建的非酶传感器在0.05MNaOH溶液中对葡萄糖的检测表现出极好的电化学性能。该传感器在两个不同的工作电位下对葡萄糖均表现出快速的检测响应（＜5s）和宽泛的动态范围（在+0.55V工作电位下，灵敏度为556.2μA·cm~(-2)·mM~(-1)（R2=0.995）；在+0.3V工作电位下，灵敏度为107.2μA·cm~(-2)·mM~(-1)（R2=0.984））。Langmuir等温吸附理论用于拟合校准曲线。在+0.55V的峰电位下对CuONWs促进的葡萄糖的氧化反应机制和对AA、UA和AP的良好的选择性也进行了研究。此外，来自生理浓度水平的果糖和蔗糖的干扰微不足道，进一步证明了CuONWs优良的选择性。这些结果证明，CuONWs在用于葡萄糖非酶检测的具有灵敏性和选择性的传感器的发展具有巨大的潜在应用。
（4）探索了基于铜的纳米材料在中性条件下对葡萄糖的非酶传感检测。参考一种大规模的回流合成技术合成了具有明确纳米结构的氧化铜纳米花材料（CuONFs）。用CuONFs构建的非酶葡萄糖传感器实现了在中性溶液中对葡萄糖及其他碳水化合物的检测。各种技术被用来表征CuONFs的结构和组成。SEM研究所制备材料的形态；XRD研究所得终产物的晶体结构；FTIR用以确认合成过程中硝酸铜向氧化铜的完全转化。CuONFs对葡萄糖检测的电化学性能通过循环伏安法、电化学阻抗谱法和差分脉冲伏安法进行研究。研究结果显示，CuONFs对葡萄糖的检测表现出较宽的线性响应范围（可至10mM（R2=0.997）），以及良好的选择性（对干扰物UA和AA）。CuONFs所增强的传感性能也体现在对其他碳水化合物的检测上。这些结果表明CuONFs在生物传感器的发展向生理条件下对非酶碳水化合物的检测的潜在适用性。
Diabetes is a metabolic disorder and a major world health problem. As stated by International Diabetes Federation, there are over285million diabetics worldwide in2010. Due to the financial burden caused by diabetes and its serious health complications, glucose detection is incredibly important in reducing the costs of diabetes management.
Glucose sensor has already experienced the development of sensors based on enzymatic catalysts and non-enzymatic catalysts. In the past decades, three generation enzymatic glucose sensors have been developed, but they suffer from the inherent instability of the enzyme due to its pH and temperature sensitivity, and sensor performance variation due to oxygen concentration fluctuation. Additionally, the high cost of enzyme also limits the wide application of enzymatic glucose biosensors in developing countries. Due to aforementioned factors, considerable research efforts have been focused on the development of non-enzymatic glucose sensors with high sensitivity and selectivity. In order to develop sensitive non-enzymatic glucose sensors, a variety of metals and metal oxides, bimetallic nanomaterials or alloys and metals/metal oxides-CNTs composites have been explored. Although both bulk and nanoscale noble materials have been extensively explored for electrocatalyzing glucose oxidation, the nanostructured non-precious metal or metal oxides with or without dopants (e.g. noble metals or conductive metal oxide) have not been systematically investigated in the non-enzymatic glucose detection, which triggers our considerable research interests. It is generally believed that the properties of nanoscale metal or metal oxides can be very different from bulk materials, due to the extremely reduced size, large surface-to-volume ratio, greater level of crystal and the Debye length (λD) comparable to the dimensions of nanomaterials. Therefore, we hypothesize that nanostructured non-precious metal, metal oxide or metal oxide composites could greatly promote the glucose oxidation/adsorption, and thus improve the sensitivity and/or selectivity in glucose sensing, which will be demonstrated in this dissertation.
In this study, the copper-or copper oxide-based nanomaterials were used to fabricate non-enzymatic glucose sensors, which successfully detected glucose in alkaline or neutral conditions. The developed non-enzymatic glucose sensors have potential applications in medical diagnostics, biological processes and food Industry. In this dissertation, we focused on following researches:
(1) In the pursuit of more economical electrocatalysts for non-enzymatic glucose sensors, one-dimensional Cu nanowires (Cu NWs) with uniform size distribution and a large aspect ratio (>200) were synthesized by a facile, scalable, wet-chemistry approach. The morphology, crystallinity, and surface property of the as-prepared Cu NWs were examined by SEM, XRD, and XPS, respectively. The electrochemical property of Cu NWs for glucose electrooxidation was thoroughly investigated by cyclic voltammetry. In the amperometric detection of glucose, the Cu NWs modified glassy carbon electrode exhibits an extraordinary limit of detection of35nM (S/N=3) and a wide dynamic range with excellent sensitivity of420.3μA·cm-2·mM-1, which is more than10,000times higher than that of the control electrode without Cu NWs. The performance of the developed glucose sensor is also independent to oxygen concentration and free from chloride poisoning. Furthermore, the interference from uric acid, ascorbic acid, acetaminophen, fructose, and sucrose at the level of their physiological concentration were insignificant, indicating excellent selectivity. Finally, good accuracy and high precision for the quantification of glucose concentration in human serum samples implicate the applicability of Cu NWs in sensitive and selective non-enzymatic glucose detection.
(2) A novel hybrid composite based electrocatalyst consisting of copper nanowires (Cu NWs) and single-walled carbon nanotubes (SWCNTs) was introduced for glucose electrooxidation and detection in alkaline medium. The morphology, chemical composition, and crystalline structure of the as-prepared Cu NWs-SWCNTs hybrid composite were examined by SEM, EDX, and XRD, respectively. The electrocatalytic property of Cu NWs-SWNTs for glucose electrooxidation was investigated by cyclic voltammetry and enhanced performance was observed due to the synergistic effect between Cu NWs and SWCNTs. Further application of the hybrid composite for glucose monitoring shows a wide dynamic range with a limit of detection of89nM (S/N=3), an excellent sensitivity (637.3μA-cm-2·mM-1), and good selectivity against commonly interfering species. These results indicate that Cu NWs-SWCNTs hybrid composite is a promising material in various applications.
(3) Copper oxide nanowires (CuO NWs) were fabricated by a facile two-step procedure consisting of wet-chemistry synthesis and subsequent thermal treatment in air. SEM and TEM were employed to characterize the morphology, surface property, and crystal structure of the as-prepared CuO NWs, while the composition of the as-prepared CuO nanowires was investigated using XRD. The CuO NWs were further employed to construct an enzyme-free sensor with excellent performance towards the glucose detection in0.05M NaOH solution. The developed sensor showed a fast response time (less than5s), a wide dynamic range with excellent sensitivity of556.2μA-cm-2·mM-1(R2=0.995) and107.2μA-cm-2·mM-1(R2=0.984) at the working potential of+0.55V and+0.3V, respectively. The Langmuir isothermal theory was employed to fit the obtained calibration curve. The mechanisms for the glucose oxidation promoted by CuO NWs and the good selectivity against ascorbic acid, uric acid and acetaminophen at an applied potential of+0.55V were also discussed. Furthermore, the interference from fructose, and sucrose at the level of their physiological concentration were insignificant, indicating excellent selectivity. These results implicate that CuO NWs have great potential applications in the development of sensitive and selective sensors for enzyme-free detection of glucose.
(4) A reflux synthesis technique was used to synthesize CuO materials with well-defined nanostructures in large scale, which were further applied to construct an enzyme-free sensor for the detection of glucose and carbohydrates in a neutral pH solution. A variety of techniques were used to characterize these materials. Specially, scanning electron microscopy was employed to study the morphology of the as-prepared materials; X-ray diffraction was used to investigate the crystal structure of the final product; and Fourier transform infrared spectroscopy was applied to confirm the complete conversion of copper nitrate to copper oxide in the synthetic process. The electrochemical property of CuO nanoflowers for glucose detection in a neutral pH solution was investigated by cyclic voltammetry, electrochemical impedance spectroscopy, and differential pulse voltammetry, showing a wide linear range up to10mM (R2=0.997) and good selectivity against uric acid and ascorbic acid. The enhanced sensing performance of CuO nanoflowers was also observed on other carbohydrates. This is the first report to detect glucose in neutral pH using CuO. These results implicate the potential applicability of CuO nanoflowers in the development of biosensors for enzyme-free carbohydrates detection in physiological condition.
引文
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