Pt基微纳结构无酶葡萄糖传感器的构建和性能研究
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摘要
葡萄糖酶传感器由于稳定性、重复性、灵敏度、选择性较差及外径较大的缺点使其应用受到限制，无酶葡萄糖传感器利用葡萄糖在电极表面直接发生电催化氧化对其进行检测，能够避免酶传感器的不足。因此，可植入式无酶葡萄糖传感器的发展为血糖监测提供了新的途径。
采用恒电位沉积法制备Pt纳米花电极，Pt纳米花电极对葡萄糖具有很好的电催化性能，在含有氯离子的溶液中不会失活。构建的无酶葡萄糖传感器的线性响应范围为1mM–16mM，响应灵敏度为1.87μAcm~(-2)mM~(-1)（R=0.9993），最低检测限为48μM（S/N=3）。传感器具有很好的重现性、重复性、稳定性和选择性，表明纳米花结构能够改善裸Pt电极的不足，提高传感器的选择性、灵敏度、重复性以及稳定性。
采用恒电流沉积法制备松树花状Pt–Pb纳米锥电极，该电极对葡萄糖具有很好的电催化性能，在含有氯离子的溶液中不会失活。对葡萄糖的电催化氧化过程遵守葡萄糖在Pt电极表面的反应机理，Pb对葡萄糖没有直接的电催化氧化活性，但是能够提高Pt电极的电催化性能。构建的无酶传感器对葡萄糖的线性检测范围为0.5mM–12mM，灵敏度为10.71μAcm~(-2)mM~(-1)（R=0.9997），最低检测限为8.4μM。传感器具有很好的选择性、稳定性和重复性。此外，在20oC到70oC的范围内，松树花状Pt–Pb纳米锥电极对葡萄糖的电催化活性随温度的升高而增大，当温度超过70oC之后，活性趋于稳定。因此，该无酶葡萄糖传感器的工作温度范围宽，相比酶传感器将有更加广泛的应用。
采用电流置换反应制备Pt–Ag和Pt–Cu中空纳米颗粒电极，研究表明添加Ag与Cu能够提高Pt电极对葡萄糖的电催化氧化活性，同时会提高葡萄糖在电极表面的电催化氧化电位。Pt–Ag和Pt–Cu中空纳米颗粒修饰电极构建的无酶葡萄糖传感器的线性检测范围分别为0.5mM–16mM和0.5mM–14mM，响应灵敏度分别为7.64μAcm~(-2)mM~(-1)和8.04μAcm~(-2)mM~(-1)，最低检测限分别为11.78μM和11.19μM，传感器对抗坏血酸和尿酸的响应电流是葡萄糖响应电流的15%和9%。
用直径为0.35mm的不锈钢针灸针作为工作电极，基于Pt-Pb纳米颗粒电活性面积高、壳聚糖易成膜及生物相容性好的优势，用恒电流沉积法结合苯醌还原诱导壳聚糖沉积的方法构建针式酶葡萄糖传感器。针电极对葡萄糖具有很好的电催化氧化性能，说明苯醌电还原诱导壳聚糖与葡萄糖氧化酶共沉积制备针式酶电极的方法是可行的。构建的针式酶葡萄糖传感器的线性检测范围为0.03–9mM，响应灵敏度为0.4485μAcm~(-2)mM~(-1)（R=0.9995），最低检测限为200μM。
用直径为0.35mm的不锈钢针灸针作为工作电极，用恒电流沉积法构建Pt-Pb纳米颗粒修饰不锈钢针式无酶葡萄糖传感器。构建的针式无酶传感器对葡萄糖的线性检测范围为1.5mM–24mM，响应灵敏度为3.33μAcm~(-2)mM~(-1)（R=0.9997），最低检测限为27μM。传感器具有很好的选择性、稳定性以及重复性。与针式酶葡萄糖传感器相比，针式无酶葡萄糖传感器具有高的稳定性、选择性和灵敏度。
The poor sensitivity, repeatability and stability of the enzymatic sensors remainas problems for real sensor applications. Direct electrocatalytic oxidation of glucose atan enzyme-free electrode would exhibit conveniences and advantages to avoid thedrawbacks of the enzymatic electrode. Therefore, the development of needle-typenonenzymatic glucose biosensor provides a promising method for glucose detection.
Pt nanofowers were fabricated by using template-free ultrasonicelectrodeposition method. The Pt nanofowers electrode exhibited excellent catalyticactivity towards glucose oxidation in the present and in the absence of chloride ions.The results showed that the sensitivity of the electrode to glucose oxidation was1.87μAcm~(-2)mM~(-1)with a linear range from1mM to16mM and detection limit of48μM.In addition, the nonenzymatic glucose sensors exhibited excellent selectivity, stabilityand repeatability. This indicated that nanoflower structure exhibit advantages to avoidthe drawbacks of bare Pt electrode, and thus selectivilty, sensitivity, stability andrepeatability of the sensors can be improved.
Pinecone–shaped Pt–Pb nanocone electrode was prepared on the bare Auelectrodes by electrochemical deposition. The synthesized pinecone–shaped Pt–Pbnanocone electrode exhibited strong and sensitive current responses to glucose at anegative potential in the present and in the absence of chloride ions. In the Pt–Pbbinary system, Pb can considerably accelerate glucose electrooxidation at Ptelectrodes but it exhibited no direct catalytic effect towards glucose. Therefore,glucose oxidation at the Pt–Pb mainly followed the reaction pathway of glucoseoxidation at Pt electrode. The sensitivity of the sensor was10.71μAmM1cm2withlinearity up to12mM and a detection limit of8.4μM. In addition, the as–preparednonenzyme glucose sensor exhibited acceptable repeatability, stability andreproducibility for determination of glucose. The response current increased with thetemperature in the range from20oC to70oC, and became stable when thetemperature was above70oC. Therefore, the sensor exhibited a wide range ofapplications compared with enzymatic biosensor.
Pt–Ag and Pt–Cu hollow nanoparticles were fabricated by galvanic replacement.Electrochemical results showed that Cu and Ag can considerably accelerate glucoseelectrooxidation at Pt electrodes, but the electrooxidation potential increased. Thesensitivity of the sensor based on Pt–Ag hollow nanoparticles was7.64μAmM1cm2 with linear range from0.5mM to16mM and a detection limit of11.78μM. Thesensitivity of the sensor based on Pt–Cu hollow nanoparticles was8.04μAmM1cm2with linear range from0.5mM to14mM and a detection limit of11.19μM. Thenonenzymatic sensors based on Pt–Ag and Pt–Cu hollow nanoparticles showedacceptable stability and repeatability.
An enzymatic glucose biosensor was fabricated by electrodepositing chitosan–glucose oxidase biocomposite onto the stainless steel needle electrode modifed byPt–Pb nanoparticles. The linear range of the proposed biosensor was from0.03to9mM with a current sensitivity of0.4485μAmM1and a detection limit of200μM.This work confirmed that the fabrication method of the needle-type glucose biosensorwas feasible.
A nonenzymatic glucose biosensor was fabricated by electrodepositing Pt–Pbnanoparticles onto the stainless steel needle electrode. The results showed that thesensitivity of the electrodes to glucose was3.33μAcm~(-2)mM~(-1)with liner range from1.5mM–24mM and detection limit of27μM. In addition, the nonenzymatic glucosesensors exhibited excellent selectivity, stability and repeatability. Compared with theenzymatic glucose biosensors, the nonenzyme sensors exhibited high stability,sensitility and repeatability.
采用恒电位沉积法制备Pt纳米花电极，Pt纳米花电极对葡萄糖具有很好的电催化性能，在含有氯离子的溶液中不会失活。构建的无酶葡萄糖传感器的线性响应范围为1mM–16mM，响应灵敏度为1.87μAcm~(-2)mM~(-1)（R=0.9993），最低检测限为48μM（S/N=3）。传感器具有很好的重现性、重复性、稳定性和选择性，表明纳米花结构能够改善裸Pt电极的不足，提高传感器的选择性、灵敏度、重复性以及稳定性。
采用恒电流沉积法制备松树花状Pt–Pb纳米锥电极，该电极对葡萄糖具有很好的电催化性能，在含有氯离子的溶液中不会失活。对葡萄糖的电催化氧化过程遵守葡萄糖在Pt电极表面的反应机理，Pb对葡萄糖没有直接的电催化氧化活性，但是能够提高Pt电极的电催化性能。构建的无酶传感器对葡萄糖的线性检测范围为0.5mM–12mM，灵敏度为10.71μAcm~(-2)mM~(-1)（R=0.9997），最低检测限为8.4μM。传感器具有很好的选择性、稳定性和重复性。此外，在20oC到70oC的范围内，松树花状Pt–Pb纳米锥电极对葡萄糖的电催化活性随温度的升高而增大，当温度超过70oC之后，活性趋于稳定。因此，该无酶葡萄糖传感器的工作温度范围宽，相比酶传感器将有更加广泛的应用。
采用电流置换反应制备Pt–Ag和Pt–Cu中空纳米颗粒电极，研究表明添加Ag与Cu能够提高Pt电极对葡萄糖的电催化氧化活性，同时会提高葡萄糖在电极表面的电催化氧化电位。Pt–Ag和Pt–Cu中空纳米颗粒修饰电极构建的无酶葡萄糖传感器的线性检测范围分别为0.5mM–16mM和0.5mM–14mM，响应灵敏度分别为7.64μAcm~(-2)mM~(-1)和8.04μAcm~(-2)mM~(-1)，最低检测限分别为11.78μM和11.19μM，传感器对抗坏血酸和尿酸的响应电流是葡萄糖响应电流的15%和9%。
用直径为0.35mm的不锈钢针灸针作为工作电极，基于Pt-Pb纳米颗粒电活性面积高、壳聚糖易成膜及生物相容性好的优势，用恒电流沉积法结合苯醌还原诱导壳聚糖沉积的方法构建针式酶葡萄糖传感器。针电极对葡萄糖具有很好的电催化氧化性能，说明苯醌电还原诱导壳聚糖与葡萄糖氧化酶共沉积制备针式酶电极的方法是可行的。构建的针式酶葡萄糖传感器的线性检测范围为0.03–9mM，响应灵敏度为0.4485μAcm~(-2)mM~(-1)（R=0.9995），最低检测限为200μM。
用直径为0.35mm的不锈钢针灸针作为工作电极，用恒电流沉积法构建Pt-Pb纳米颗粒修饰不锈钢针式无酶葡萄糖传感器。构建的针式无酶传感器对葡萄糖的线性检测范围为1.5mM–24mM，响应灵敏度为3.33μAcm~(-2)mM~(-1)（R=0.9997），最低检测限为27μM。传感器具有很好的选择性、稳定性以及重复性。与针式酶葡萄糖传感器相比，针式无酶葡萄糖传感器具有高的稳定性、选择性和灵敏度。
The poor sensitivity, repeatability and stability of the enzymatic sensors remainas problems for real sensor applications. Direct electrocatalytic oxidation of glucose atan enzyme-free electrode would exhibit conveniences and advantages to avoid thedrawbacks of the enzymatic electrode. Therefore, the development of needle-typenonenzymatic glucose biosensor provides a promising method for glucose detection.
Pt nanofowers were fabricated by using template-free ultrasonicelectrodeposition method. The Pt nanofowers electrode exhibited excellent catalyticactivity towards glucose oxidation in the present and in the absence of chloride ions.The results showed that the sensitivity of the electrode to glucose oxidation was1.87μAcm~(-2)mM~(-1)with a linear range from1mM to16mM and detection limit of48μM.In addition, the nonenzymatic glucose sensors exhibited excellent selectivity, stabilityand repeatability. This indicated that nanoflower structure exhibit advantages to avoidthe drawbacks of bare Pt electrode, and thus selectivilty, sensitivity, stability andrepeatability of the sensors can be improved.
Pinecone–shaped Pt–Pb nanocone electrode was prepared on the bare Auelectrodes by electrochemical deposition. The synthesized pinecone–shaped Pt–Pbnanocone electrode exhibited strong and sensitive current responses to glucose at anegative potential in the present and in the absence of chloride ions. In the Pt–Pbbinary system, Pb can considerably accelerate glucose electrooxidation at Ptelectrodes but it exhibited no direct catalytic effect towards glucose. Therefore,glucose oxidation at the Pt–Pb mainly followed the reaction pathway of glucoseoxidation at Pt electrode. The sensitivity of the sensor was10.71μAmM1cm2withlinearity up to12mM and a detection limit of8.4μM. In addition, the as–preparednonenzyme glucose sensor exhibited acceptable repeatability, stability andreproducibility for determination of glucose. The response current increased with thetemperature in the range from20oC to70oC, and became stable when thetemperature was above70oC. Therefore, the sensor exhibited a wide range ofapplications compared with enzymatic biosensor.
Pt–Ag and Pt–Cu hollow nanoparticles were fabricated by galvanic replacement.Electrochemical results showed that Cu and Ag can considerably accelerate glucoseelectrooxidation at Pt electrodes, but the electrooxidation potential increased. Thesensitivity of the sensor based on Pt–Ag hollow nanoparticles was7.64μAmM1cm2 with linear range from0.5mM to16mM and a detection limit of11.78μM. Thesensitivity of the sensor based on Pt–Cu hollow nanoparticles was8.04μAmM1cm2with linear range from0.5mM to14mM and a detection limit of11.19μM. Thenonenzymatic sensors based on Pt–Ag and Pt–Cu hollow nanoparticles showedacceptable stability and repeatability.
An enzymatic glucose biosensor was fabricated by electrodepositing chitosan–glucose oxidase biocomposite onto the stainless steel needle electrode modifed byPt–Pb nanoparticles. The linear range of the proposed biosensor was from0.03to9mM with a current sensitivity of0.4485μAmM1and a detection limit of200μM.This work confirmed that the fabrication method of the needle-type glucose biosensorwas feasible.
A nonenzymatic glucose biosensor was fabricated by electrodepositing Pt–Pbnanoparticles onto the stainless steel needle electrode. The results showed that thesensitivity of the electrodes to glucose was3.33μAcm~(-2)mM~(-1)with liner range from1.5mM–24mM and detection limit of27μM. In addition, the nonenzymatic glucosesensors exhibited excellent selectivity, stability and repeatability. Compared with theenzymatic glucose biosensors, the nonenzyme sensors exhibited high stability,sensitility and repeatability.
引文
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