聚钙羧酸膜修饰电极对亚甲基蓝的检测研究

制备了聚钙羧酸膜修饰玻碳电极,采用循环伏安法和方波伏安法研究了亚甲基蓝在修饰电极上的电化学行为,优化了包括支持电解质、缓冲液p H等测定条件。建立了亚甲基蓝测定的新方法。结果表明:该方法灵敏度高、检测范围宽,可用于水产品中亚甲基蓝残留的测定。     

自组装壳聚糖接枝聚苯胺/葡萄糖氧化酶生物传感器的研究

合成了壳聚糖接枝聚苯胺，并采用静电自组装法制备了壳聚糖接枝聚苯胺／葡萄糖氧化酶生物传感器。讨论了温度、pH值、离子强度以及自组装膜层数对传感器电流响应的影响。制备的葡萄糖生物传感器检测范围为0．5mmol／L～16mmol／L，电流响应时间仅为5．2s。     

一种基于静电纺碳纳米纤维的酚醛传感器

采用静电纺制备纳米纤维膜,接着通过高温碳化技术处理得到碳纳米纤维膜(ECNFs),再通过共混得到漆酶-全氟磺酸聚四氟乙烯共聚物-纳米碳纤维玻碳电极(laccase-Nafion-ECNFs/GCE)并制备新酚醛传感器。采用拉曼荧光显微分光计和Nicolet iS10傅里叶红外光谱仪对ECNFs进行分析;用循环伏安法对laccase-Nafion/GCE、laccase/GCE、laccase-Nafion-ECNFs/GCE进行了检测并测试扫描速率对laccase-Nafion-ECNFs/GCE效果的影响;采用方波伏安法对laccase-Nafion/GCE、laccase/GCE、laccase-Nafion-ECNFs/GCE进行了检测并测试对苯二酚浓度对laccase-Nafion-ECNFs/GCE效果的影响。结果表明:实验获得了ECNFs,且ECNFs的表面存在大量的羧基基团,有利于提高ECNFs的电催化性能和生物相容性;ECNFs的添加,提高了复合材料的导电率并增加了玻碳电极表面到漆酶中心的电子转移速率;漆酶在laccase-Nafion-ECNFs复合材料和玻碳电极表面很容易发生电子传输;ECNFs的修饰强烈地增加了玻碳电极对对苯二酚的电催化作用;该生物传感器的检测限为0.32μmol/L,线性范围为1~20μmol/L,可满足环境监测的要求。这种基于电纺纳米碳纤维的新型生物传感器装置具有很大的应用潜力。     

Acetylcholinesterase Biosensor Based on Poly (diallyldimethylammonium chloride)-multi-walled Carbon Nanotubes-graphene Hybrid Film

Nano-Micro Letters - In this paper, an amperometric acetylcholinesterase (AChE) biosensor for quantitative determination of carbaryl was developed. Firstly, the poly (diallyldimethy-lammonium...     

PVP-GR/GCE电化学检测塑料制品中双酚A的研究

针对塑料制品中双酚A(BPA)检测问题,制备了聚乙烯吡咯烷酮-石墨烯复合膜修饰玻碳电极(PVP-GR/GCE)并建立了BPA的电化学检测方法。通过扫描电子显微镜对PVP-GR的形貌进行了表征;以循环伏安法分别对GCE、PVP/GCE、GR/GCE以及PVP-GR/GCE进行了电化学表征;采用二阶导数线性扫描伏安法研究了PVP-GR/GCE对BPA的电化学性能;对检测条件进行了优化,并在最佳检测条件下对该电化学检测方法的线性范围、检测限、重现性、再现性、稳定性、选择性以及样品加标回收率进行了研究。实验结果表明:PVP-GR仍具有GR的特有性能,且其在水溶液中的分散性优于GR;K3[Fe(CN)6]在PVP-GR/GCE上的氧化峰电流最大,即PVP的引入改善了GR的水溶性,使PVP-GR/GCE的电化学性能增强;BPA在PVPGR/GCE的电化学响应较裸GCE明显增强;在最佳检测条件下,BPA的氧化峰电流与其浓度在0.01~0.40μmol/L和0.40~60.00μmol/L范围内呈良好的线性关系,检测限为8.0 nmol/L(信噪比为3),且该方法具有良好的选择性、灵敏度、重现性和稳定性,并成功被用于塑料制品中BPA的检测,回收率为97.3%~105.2%。     

基于二氧化硅球腔阵列的葡萄糖传感器研究

在二氧化硅球腔阵列电极上,通过电沉积普鲁士蓝和直接吸附葡萄糖氧化酶,制备了一种新型葡萄糖生物传感器。该传感器对酶催化反应产物过氧化氢的选择性催化还原特性可实现对葡萄糖的检测,实验结果表明,传感器的最佳工作电位是－0．3V,测试溶液的最佳pH值为6．0。在选定的工作条件下,传感器的线性范围为2．49×10-5－2．42×10-3mol／L,检测极限值为7．2×10-6mol／L（S／N=3）,米氏常数为1．136mmol／L。该方法制备的生物传感器能有效降低干扰,具有潜在的应用价值。     

聚邻苯二胺负载纳米铜氧化物修饰玻碳电极的制备及表征

在磷酸盐缓冲溶液中于玻碳电极表面聚合邻苯二胺,再负载纳米铜氧化物,成功制备了邻苯二胺负载纳米铜氧化物修饰玻碳电极(CuO/P-oPD/GC).探讨了聚合和负载机理,用电化学交流阻抗谱表征了修饰电极界面的阻抗变化,用扫描电镜表征了聚邻苯二胺膜和负载铜氧化物后的表面形态,发现CuO/P-oPD/GC电极对H2O2有显著的电催化氧化、还原双重活性,并呈现"协同增敏"效应.考察了制备条件对CuO/P-oPD/GC电极电催化活性的影响,最佳CoO负载扫描次数为20,Cu2+的质量浓度为1.67mmol/L.对H2O2电催化氧化的线性方程为△ip8(μA)=0.08+5.64c(mmol/L)(R=0.9982),线性范围为2.4×10-2～48mmol/L,检测限为2.8×10-3mmol/L(3S/k);电催化还原的线性方程为△ipc(μA)=0.11-2.45c(mmol/L)(R=0.9820),线性范围为2.4×10-3～38.4mmol/L,检测限为2.0×10-4mmol/L(3S/k).该复合材料修饰电极的灵敏度高、稳定性好,用于实际水样中H2O2测定结果满意.     

纳米硫化铜修饰玻碳电极的原位制备及分析应用

采用镀膜/循环伏安法原位制备了纳米CuS/GC电极,研究了其制备机理,探讨了具有最大电催化活性的制备及测试条件。通过SEM、EIS对修饰膜进行了表征,表明纳米CuS粒子均匀附着于电极表面,具有较高的导电性。采用电流-时间曲线法研究了CuS/GC电极的分析性能,结果表明,电极对H2O2浓度的响应时间短于0.1s,在0.67～20.5μmol.L-1及0.033～2.93mmol.L-1范围内,电流变化和H2O2浓度的线性方程分别为Δi(μA)=-0.0081+0.0267c(R=0.9998)及Δi(μA)=0.7378+22.17c(R=0.9930),检出限为6.0×10-8 mol.L-1(S/N=3)。该修饰电极具有较高的电化学及贮存稳定性,实际水样测试结果表明回收率为92%～98%,相对标准偏差小于3.6%。     

掺磷四面体非晶碳薄膜电极的电化学伏安特性

采用过滤阴极真空电弧技术, 以高纯磷烷气体为掺杂源制备掺磷四面体非晶碳(ta-C:P)薄膜. 利用X射线光电子能谱和激光拉曼光谱表征薄膜的成分和结构, 采用循环伏安和微分脉冲伏安分析薄膜的电化学行为. 结果表明, 磷的掺入没有引起薄膜非晶结构的明显变化, 只是促进了sp²杂化碳原子的团簇. 经过酸预处理的ta-C:P薄膜在硫酸溶液中有宽的电势窗口和低的背景电流; 对Cl^-有催化活性; 薄膜表面电子传输速度快; 对水溶液中Cu²⁺和Cd²⁺有检测活性. 因此具有良好导电性的ta-C:P薄膜适于作为电极并有望用于污水中重金属离子的分析检测等领域.     

基于花状MoS2微米材料的葡萄糖生物传感器的制备及其性能研究

本研究采用水热法制备了花状MoS₂微米材料, 将其作为电极构建葡萄糖生物传感器, 并研究了相关性能。结果表明: 水热法制备的MoS₂呈花状, 具有较好的结晶质量, 尺寸约为3.6 μm, 比表面积约为9.646 m²/g; MoS₂电极具有优良的电催化活性, 且电阻抗较小, 使得传感器对葡萄糖具有较好的响应。葡萄糖检测结果表明, 该传感器在0~20 mmol/L范围内, 氧化峰电流与葡萄糖浓度呈良好的线性关系, 相关系数(R)为0.9653, 灵敏度为262 μA•L/mmol。     

New Composite Electrode Material Based on Glassy Carbone/Polythiophene/MnO2

In this paper, it presents the work which consists to develop and characterize a modified electrode with a conductive polymer film, poly [3-methyl thiophene] then incorporating manganese dioxide MnO2 into the film. The deposition of the polymer film on the surface of the glassy carbon electrode is realized by the electrochemical oxidation of the monomer [3-methyl thiophene] in an organic medium. Then the electrode obtained was immersed in a solution containing ions Mn4~ to introduce into the polymeric film. The technique of insertion of manganese ions is performed by interaction with the polymer film. The electrochemical oxidation of the modified electrode in an aqueous medium will precipitate the manganese dioxide in the form of particles in the polymer film. In this study, it was found that several parameters affect the amount of manganese dioxide introduced as the pH of the medium and the thickness of the polymer film.     

电沉积羟基磷灰石修饰电极上的葡萄糖传感器的研制

在铂电极上电沉积羟基磷灰石（HAp）-聚乙烯醇（PVA）复合涂层,并将葡萄糖氧化酶（GOD）固定在羟基磷灰石HAp-PVA-Nafion复合膜,构建了高灵敏度、高选择性的葡萄糖传感器。固定在此电极上的GOD在pH 7.0的磷酸缓冲液（PBS）中展现出一对可逆性好的氧化还原峰,此电极对葡萄糖的氧化有良好的催化作用随葡萄糖浓度,在恒电位-0.92 V（相对于饱和甘汞电极）时测量溶解氧还原电流,结果显示,羟基磷灰石和Nafion良好的协同作用增强了GOD的电化学活性,促进了GOD与电极表面之间的电子转移,提高了传感器的穗定性与灵敏度,还原电流的衰减在浓度0.04-0.52 mmol dm~（-3）范围内与葡萄糖的浓度呈线性关系     

A Novel Urea Amperometric Biosensor Based on Secretion of Wild Winter Jasmine Petal Cells Modified on Graphite-Epoxy Composite Electrode

A new kind of amperometric biosensor was designed for detection of urea with a high selectivity, sensitivity and wide detection range based on the secretion of whole living cells of wild winter jasmine petals paste covered on a graphite-epoxy composite basic electrode surface. The petal paste from mashed fresh winter jasmine petals was tightly fixed on the basic electrode surface with teflon thin film to keep it contact with electrode surface. During the mashing process, the winter Jasmine petal cells secrete some species, which are electrochemical active and gives an oxidation peak at 0.316 V （vs. SCE） in differential pulse voltammetric curve. The interactions of secreted species with urea molecules, and results in the decrease the oxidation peak current. The oxidation peak current was decreased linearly with the logarithm of urea concentration in the range of 1.3×10^-16-4.57 ×10^-16 M with the detection limit of 1.3×10^-16 M.     

Preconcentration and Voltammetric Determination of Mercury(II) at a Chemically Modified Glassy Carbon Electrode

In this work, the organic compound 2-mercaptobenzimidazole was covalently bound on the surface of a glassy carbon rod, via silanization, yielding a material capable of selectively complexing Hg(2+) ions. This material was applied as an electrode for voltammetric determination of mercury(II) following its nonelectrolytic preconcentration. After exchanging the medium, the voltammetric measurements were carried out by anodic stripping in the differential pulse mode (pulse amplitude, 50 mV; scan rate, 1.25 mV s(-)(1)) using 10(-)(2) mol L(-)(1) NaSCN solution as supporting electrolyte. An anodic stripping peak was obtained at 0.06 V (vs SCE) by scanning the potential from -0.3 to +0.3 V. After a 5 min preconcentration period in a pH 4.0 Hg(2+) solution, this electrode shows increasing voltammetric response in the range 0.1-2.2 μg mL(-)(1), with a relative standard deviation of 5% and a practical detection limit of 0.1 μg mL(-)(1) (5.0 × 10(-)(7) mol dm(-)(3)). Compared with the conventional stripping approach, this chemically modified glassy carbon electrode procedure presented good discrimination against interference from Cu(II) in up to 10-fold molar excess.     

基于电化学共聚蛋白A固定抗体的安培型免疫微传感器

研究了共聚合吡咯和蛋白A（staphylococcal proteinA）修饰传感界面的新方法,用于安培型免疫微传感器检测人免疫球蛋白（immunoglobulin G,IgG）抗原．基于微机电系统（micro electro mechanical systems,MEMS）技术,在硅片上制备带有SU-8微反应池和微型两电极系统的传感芯片,利用电化学循环伏安法,将蛋白A与吡咯掺杂后共聚于工作电极表面,以此固定IgG抗体．优化蛋白A和抗体固定的实验条件,对聚合膜进行了扫描电镜（SEM）成像分析．实验结果表明,该方法操作简便、可控性强,在160S内能够有效固定蛋白A,改善抗体固定效果,与用聚吡咯修饰传感界面的方法相比,检测灵敏度提高约10％,以此实现的安培型免疫微传感器非特异性吸附小,具有较好的重复性和稳定性．     

Effect of Neutron Irradiation on Properties of Glassy Carbon

Experimental data are presented on the effect of neutron irradiation (90–750°C, 4 × 10²² n/cm², E > 0.18 MeV) on the dimensions and properties of glassy carbon. The irradiation leads to a linear shrinkage of up to 8–12%, without secondary swelling. The radiation effects are analyzed in terms of the microstructure and properties of glassy carbon.