二氧化硅/金复合膜修饰玻碳电极用于双酚A的检测

该文制备了二氧化硅/金复合膜修饰玻碳电极(SiO_2/Au/GCE),提出了一种简便检测双酚A(BPA)的电化学分析方法。采用扫描电镜(SEM)和红外光谱(FT-IR)对SiO_2和SiO_2/Au的形貌和结构进行了表征,循环伏安法(CV)和交流阻抗法(EIS)研究了SiO_2/Au/GCE的表面电化学特性,同时用CV、计时库仑法(CC)、控制电位电解库仑法、线性扫描伏安法(LSV)和差分脉冲伏安法(DPV)等研究了BPA在SiO_2/Au/GCE上的电化学行为,优化了实验参数,并得到电化学动力参数。实验发现:SiO_2/Au/GCE对BPA具有良好的电催化活性,BPA在该修饰电极上的氧化峰电流为GCE上的3倍,且BPA在SiO_2/Au/GCE上的氧化过程为2电子2质子的完全不可逆电极过程。在最佳条件下,BPA的氧化峰电流分别在0.01~0.50μmol/L和0.50~25μmol/L浓度范围内呈良好的线性关系,检出限为1.9×10-8mol/L。用于一次性手套中BPA含量的测定,回收率为98.9%~105.3%,与高效液相色谱法(HPLC)进行对照,结果满意。     

碳纳米管负载纳米金-石墨烯量子点修饰电极电化学检测过氧化氢

采用过氧化氢刻蚀法制备石墨烯量子点(GQDs),再采用原位化学还原法制备金纳米粒子-石墨烯量子点纳米复合物(Au NPs-GQDs),最后以聚二甲基二烯丙基氯化铵(PDDA)为交联剂将上述纳米复合物组装于多壁碳纳米管表面,制得金纳米粒子-石墨烯量子点-PDDA-多壁碳纳米管复合材料(Au NPs-GQDsPDDA-MWCNTs)。通过荧光光谱法、紫外-可见吸收光谱法和透射电子显微镜对上述复合材料进行表征。采用滴涂法制得该复合材料修饰的玻碳电极,研究了过氧化氢在该电极上的电化学行为。结果表明:在石墨烯量子点、金纳米粒子和多壁碳纳米管三者的协同作用下,该电极对过氧化氢的电氧化表现出强的催化活性。在优化条件下,安培法检测H_2O_2的线性范围为2.0×10~(-8)~1.5×10~(-3)mol/L,检出限(3sb)为8.0×10~(-9)mol/L,灵敏度为61.6μA/(mmol·L~(-1))。     

基于多壁碳纳米管负载金纳米粒子修饰的甲基对硫磷分子印迹电化学传感器的研制

本文以四氨基苯硫酚作为功能单体、甲基对硫磷(MP)作为模板分子,通过电聚合的方法在多壁碳纳米管负载金纳米粒子修饰的玻碳电极表面成功构建了MP分子印迹电化学传感器。借助循环伏安、电化学阻抗和差示脉冲等方法对传感器的电化学性能、选择性、稳定性以及重现性进行了研究。并将所建立的方法应用于黄河水中MP的加标回收检测,结果令人满意。该方法无需进行预处理,选择性好、灵敏度高、重现性好,为分析检测MP分子提供了一种非常有效的方法。     

基于聚对氨基苯磺酸、功能化石墨烯和纳米金修饰电极的构筑及用于双酚A的测定

通过电聚合方法制备聚对氨基苯磺酸修饰的玻碳电极（GCE/pABSA）,然后把带有正电荷的超支化聚乙烯亚胺功能化还原氧化石墨烯（BPEIGr）和带有负电荷的金纳米粒子（AuNPs）依次修饰到电极上,制得GCE/pABSA/BPEIGr/AuNPs修饰电极。研究了双酚A在GCE/pABSA/BPEIGr/AuNPs修饰电极上的电化学行为。结果表明,所制备的修饰电极对双酚A有良好的电催化效果,在pH 7.0的PBS溶液中进行循环伏安扫描,双酚A在0.2～0.8 V范围内出现1个不可逆的氧化还原峰。采用差分脉冲伏安法（DPV）对双酚A进行了检测,在优化的条件下,双酚A的浓度在0.05～10μmol/L范围内与氧化峰电流呈线性关系,检出限为0.02μmol/L(3σ)。将基于此修饰电极的传感器用于浑河水和自来水中双酚A含量的测定,加标回收率在97.0%～105.0%之间。     

电化学还原氧化石墨烯/纳米金-壳聚糖复合膜修饰玻碳电极对尿酸的灵敏测定

将氧化石墨烯(GO)在玻碳电极(GCE)表面进行直接电化学还原,再组装上纳米金-壳聚糖(AuNPCS)聚阳离子,形成了电化学还原氧化石墨烯/纳米金-壳聚糖(ERGO/AuNP-CS)复合膜修饰的玻碳电极。采用扫描电子显微镜(SEM)表征了不同修饰膜表面的形貌,探讨了其对尿酸(UA)分子的差分脉冲伏安(DPV)行为,发现ERGO/AuNP-CS复合膜对UA分子表现出显著的电催化氧化活性。在0.10 mol/L磷酸盐缓冲溶液(pH=6.5)中,扫速为100 mV/s时,此复合膜修饰电极的DPV响应与UA的浓度在0.05~110μmol/L范围内呈性关系,检测限为12.4 nmol/L(S/N=3)。此修饰电极具有良好的选择性、重现性和稳定性,可应用于人体血清和尿液样品中UA的测定,回收率达到93.8%~104.1%。结果与分光光度法和尿酸酶试剂盒法相符。     

金纳米粒子/碳纳米管复合修饰玻碳电极对对苯二酚氧化还原反应的电催化性能

以对苯二酚为目标化合物比较研究了金纳米粒子、碳纳米管、金纳米粒子/碳纳米管3种纳米粒子修饰电极的电催化性能,结果发现:3种纳米粒子修饰电极均对对苯二酚的电化学信号具有增强作用。电化学阻抗谱和修饰层数试验表明:金纳米粒子的增强效果来自于金纳米粒子的电催化作用,碳纳米管的增强作用来自于电催化作用与大的电极表面积,金纳米粒子/碳纳米管复合修饰电极综合利用了两种纳米粒子的特性,表现出了更为优良的电催化行为。对苯二酚在修饰电极上的电化学过程均为扩散控制过程。     

纳米金/Nafion/石墨烯修饰玻碳电极检测对苯二酚的研究

采用一步电化学共还原的方法将纳米金(AuNPs)、Nafion、电化学还原石墨烯(ERGO)修饰到玻碳电极(GCE)表面,制成修饰电极AuNPs/Nafion/ERGO/GCE。以扫描电镜对其进行表征,用循环伏安法和微分脉冲伏安法研究对苯二酚在该修饰电极上的电催化行为。优化了实验参数,对苯二酚在2.0～100μmol/L及100～800μmol/L浓度范围内与其氧化峰电流呈良好的线性关系,检出限为0.3μmol/L。用该修饰电极成功地进行了实际水样中对苯二酚含量的测定。     

金纳米粒子/聚多巴胺/碳纳米管修饰玻碳电极对核黄素的测定

采用原位还原法制备金纳米粒子/聚多巴胺/碳纳米管（Au-PDA-MWNTs）复合材料,并将其用于建立高灵敏检测核黄素的电化学方法.采用紫外–可见光谱、扫描电镜、x-射线能谱对Au-PDA-MWNTs复合材料进行表征,采用循环伏安法和差示脉冲伏安法探讨核黄素（RF）在Au-PDA-MWNTs修饰的玻碳电极上的电化学行为,并对RF含量进行测定.该方法对核黄素的检测在5×10^-9 mol·L^-1～1×10^-5 mol·L^-1的范围内呈良好的线性关系（R=0.9906）,检测限为1.7×10^-9 mol·L^-1.本方法操作简便、抗干扰能力强,方法可行,因此该方法成功实现了维生素药片中RF含量的测定.     

金-石墨烯修饰电极电化学检测塑料瓶中双酚A

在离子液体碳糊电极(CILE)表面上采用一步电还原法制备了纳米金(nAu)-石墨烯(GR)复合膜修饰电极(nAu-GR/CILE).研究了双酚A(BPA)在nAu-GR/CILE上的电化学行为,BPA的电极反应过程为受吸附控制的不可逆过程;采用示差脉冲伏安法研究了BPA氧化峰电流和浓度之间的关系,在0.08～400.0...     

金纳米粒子-石墨烯修饰玻碳电极的制备及对多巴胺、抗坏血酸和尿酸的同时检测

采用三步法制备了金纳米粒子-石墨烯层层组装的复合材料,并将其修饰在玻碳电极上,制备成一种新型的同时检测抗坏血酸(AA)、多巴胺(DA)和尿酸(UA)的电化学传感器。采用扫描电子显微镜(SEM)对复合材料进行了表征,并研究了传感器对AA、DA、UA电催化性能。结果表明:该传感器对AA、DA和UA的氧化具有很好的催化和分离效果,可实现AA、DA和UA的同时测定。在三者共存体系中,AA-DA、DA-UA、AA-UA的氧化峰电位差分别为152mV、161mV和313mV。线性范围分别为1.996×10-5~5.580×10-3、1.996×10-6~5.478×10-3和1.000×10-6~1.000×10-3 mol/L,检出限分别为1.200×10-5、1.030×10-7和4.100×10-7 mol/L。该修饰电极选择性好、稳定性高,有望用于实际样品中AA、DA和UA的同时检测。     

金纳米粒子/碳纳米管修饰电极对4 壬基酚的电催化氧化及检测研究

制备了金纳米粒子/碳纳米管修饰玻碳电极(AuNPs-CNTs/GCE),采用循环伏安法和线性扫描伏安法研究了4-壬基酚在修饰电极上的电化学行为,并建立了一种灵敏简便地检测4-壬基酚的电化学方法。优化了pH值、扫描速率、富集时间等测定参数,并计算出pH值与氧化峰电压、扫描速率与氧化峰电流之间的数量关系。在pH 10.0的BR缓冲溶液中,4-壬基酚在AuNPs-CNTs/GCE上出现灵敏的氧化峰,氧化电位为0.51 V。与裸玻碳电极(GCE)和单一碳纳米管修饰电极(CNTs/GCE)相比,AuNPs-CNTs/GCE明显提高了4-壬基酚的氧化电流。在优化实验条件下,4-壬基酚的浓度分别在0.05～4μmol/L和6～14μmol/L范围内与氧化峰电流呈良好的线性关系,检出限为0.023μmol/L,对于实际样品测定的回收率为95%～104%。该修饰电极具有良好的重现性和稳定性,可用于环境样品中4-壬基酚的直接检测。     

基于还原石墨烯/纳米银复合材料的电化学传感器测定双酚A

石墨烯特有的褶皱层状结构以及银纳米粒子良好的催化性能,使其在电化学方面具有良好的应用潜能.本研究以柠檬酸钠为还原剂,通过水热反应原位制备出还原石墨烯/纳米银复合材料(rGO/AgNPs),用于修饰玻碳电极,研究了双酚A的电化学行为.循环伏安法(CV)和方波伏安法(SWV)的实验结果表明,双酚A可以在rGO/AgNPs修饰电极表面发生快速的氧化还原反应,基于此实现了对双酚A的高灵敏检测.在最优条件下,双酚A的氧化峰电流与其浓度在0.1~40.0μmol/L范围内呈良好的线性关系(r2=0.996),检出限为50.7 nmol/L(S/N=3).将其用于实际环境和塑料样品中双酚A的检测,回收率为91.7%~102.9%.     

碳纳米纤维修饰碳糊电极用于双酚A的电化学检测

制备了碳纳米纤维修饰碳糊电极,并用于双酚A的高灵敏和高选择性电化学检测。碳纳米纤维材料经静电纺丝和碳化过程相结合制备而成,采用滴涂的方法修饰于碳糊电极表面制成电化学传感器。利用循环伏安法、交流阻抗法以及微分脉冲伏安法考察了传感器的性质及双酚A的电化学行为。结果表明,双酚A的峰电流响应与其浓度在0.8~50μmol/L之间呈良好的线性关系,检测限为0.1μmol/L。构建的电化学传感器用于环境水样中双酚A的检测具有较高的回收率。     

Sensitive Electrochemical Detection of Bisphenol A Using Molybdenum Disulfide/Au Nanorod Composites Modified Glassy Carbon Electrode

Bisphenol A, an important compound that is classified as an environmental hormone, has been proven to have harmful effects on human health and ecology. A molybdenum disulfide/Au nanorod‐modified glassy carbon electrode was prepared as an electrochemical sensor for the detection of bisphenol A using a simple and convenient approach. UV–Vis spectrophotometry and transmission electron microscopy were employed to characterize the composite. The electrochemical behavior of bisphenol A at the modified electrode was investigated via differential pulse voltammetry and cyclic voltammetry. The results show that bisphenol A exhibits a good electrochemical signal at the modified electrode under optimized conditions, and a good linear relationship was observed between the bisphenol A concentration and peak current within the range of 0.01–50 μM, with a detection limit of 3.4 nM. Furthermore, the fabricated electrodes showed good anti‐interference, reproducibility and stability. The proposed electrochemical method was successfully applied for the detection of bisphenol A in milk and water samples, and its potential for applications in pollutant detection was demonstrated.     

Electrochemical Determination of Tetracycline Using Molecularly Imprinted Polymer Modified Carbon Nanotube‐Gold Nanoparticles Electrode

This paper reports the use of a tetracycline (TC) sensor constructed from a combination of molecularly imprinted polymer (MIP) and gold nanoparticles modified multiwall carbon nanotubes (MWNTs‐GNPs). The results demonstrated that the amount of recognition sites in the polymer was significantly increased and the electron transfer ability of the sensor was improved. The relationship between the peak current and the TC concentration was linear in the range from 0.1 to 40 mg L^?1, and the detection limit was 0.04 mg L^?1 (S/N=3). The peak current to TC was 4.3, 6.2 and 6.8 times larger than that of oxytetracycline, chloramphenicol and nafcillin, respectively. Thus, the combination of MIP and MWNTs‐GNPs provides a sensitive and selective electrochemical detection method for tetracycline.     

Electrochemical Determination of Capsaicin and Silymarin Using a Glassy Carbon Electrode Modified by Gold Nanoparticle Decorated Multiwalled Carbon Nanotubes

The goal of this study was to develop a suitable electroanalytical method for the determination of primary compounds in the extracts of capsaicin and silymarin. For this purpose, a glassy carbon electrode immobilized with multiwalled carbon nanotubes decorated with gold nanoparticles was characterized by high resolution transmission electron microscopy and attenuated total reflectance infrared spectroscopy. The developed electrochemical sensor had a linear dynamic range from 0.15 to 35.0 µM. In addition, the limits of quantification for silymarin and capsaicin with the gold nanoparticle decorated multiwalled carbon nanotubes were 0.1564 and 0.2761 µg L^?1 with relative standard deviations (n = 3) of 1.65% and 2.09% and equivalent mass percentages of 93.33% and 62.02%, respectively. The methodology may be employed for the determination of capsaicin and silymarin in pharmaceutical and food products.     

多壁碳纳米管修饰玻碳电极伏安法测定香草醛

制备了羧基化多壁碳纳米管修饰玻碳电极(c-MWCNTs/GCE),采用循环伏安法在0.5 mol/L HCl中研究了食品添加剂香草醛的电化学行为。结果显示,该修饰电极对香草醛的电化学氧化具有良好的电催化作用,与裸玻碳电极相比电流响应显著增强。香草醛在该修饰电极上的氧化为不可逆的扩散控制过程。在最佳条件下,采用二阶导数线性扫描伏安法进行测定,香草醛的氧化峰电流与其浓度在0.1～6.0μmol/L和6.0～100μmol/L范围内呈良好的线性关系,检出限(S/N=3)为0.02μmol/L。该修饰电极具有良好的重现性(RSD=4.6%)和稳定性。方法应用于食品中香草醛的测定,回收率为96.3%～104%。     

Determination of Oxytetracycline with a Gold Electrode Modified by Chitosan-Multiwalled Carbon Nanotube Multilayer Films and Gold Nanoparticles

A molecularly imprinted electrochemical sensor was fabricated based on a gold electrode modified by chitosan-multiwalled carbon nanotube composite (CS-MWCNTs) multilayer films and gold nanoparticles (AuNPs) for convenient and sensitive determination of oxytetracycline (OTC). The multilayer of CS-MWCNTs composites and AuNPs were used to augment electronic transmission and sensitivity. The molecularly imprinted polymers (MIPs) were synthesized using OTC as the template molecule and o-phenylenediamine (OPD) as the functional monomer. They were modified on a gold electrode by electropolymerization. The electrochemical behavior of OTC at the imprinted sensor was characterized by cyclic voltammetry (CV), scanning electron microscopy (SEM), and amperometry. The molecularly imprinted sensor showed high selectivity and excellent stability toward OTC. The linear range was from 3.0 × 10^?8 to 8.0 × 10^?5 mol/L, with a limit of detection (LOD) of 2.7 × 10^?8 mol/L (S/N = 3). The developed sensor showed good recovery in spiked samples analysis.     

Simultaneous Electrochemical Determination of Hydroquinone and Bisphenol A using a Carbon Paste Electrode Modified with Silver Nanoparticles

In this paper, a rapid and sensitive modified electrode for the simultaneous determination of hydroquinone (HQ) and bisphenol A (BPA) is proposed. The simultaneous determination of these two compounds is extremely important since they can coexist in the same sample and are very harmful to plants, animals and the environment in general. A carbon paste electrode (CPE) was modified with silver nanoparticles (nAg) and polyvinylpyrrolidone (PVP). The PVP was used as a reducing and stabilizing agent of nAg from silver nitrate in aqueous media. The nAg‐PVP composite obtained was characterized by transmission electron microscopy and UV‐vis spectroscopy. The electrochemical behavior of HQ and BPA at the nAg‐PVP/CPE was investigated in 0.1 mol L⁻¹ B−R buffer (pH 6.0) using cyclic voltammetry (CV) and square wave voltammetry (SWV). The results indicate that the electrochemical responses are improved significantly with the use of the modified electrode. The calibration curves obtained by SWV, under the optimized conditions, showed linear ranges of 0.09–2.00 μmol L⁻¹ for HQ (limit of detection 0.088 μmol L⁻¹) and 0.04–1.00 μmol L⁻¹ for BPA (limit of detection 0.025 μmol L⁻¹). The modified electrode was successfully applied in the analysis of water samples and the results were comparable to those obtained using UV‐vis spectroscopy.