Selective Simultaneous Determination of Paracetamol and Uric Acid Using a Glassy Carbon Electrode Modified with Multiwalled Carbon Nanotube/Chitosan Composite

A multiwalled carbon nanotube/chitosan modified glassy carbon electrode (MWCNTs‐CHT/GCE) has been used for simultaneous determination of paracetamol (PAR) and uric acid (UA). The measurements were carried out using differential pulse voltammetry (DPV), cyclic voltammetry (CV) and chronoamperometry (CA). DPV measurements showed a linear relationship between oxidation peak current and concentration of PAR and UA in phosphate buffer (pH 7) over the concentration range 2 µM to 250 µM, and 10 µM to 400 µM, respectively. The analytical performance of this sensor has been evaluated for detection of PAR and UA in human serum and human urine with satisfactory results.     

Development of Electrochemical Biosensor Based on Nanostructured Carbon Materials for Paracetamol Determination

This work describes the development of a biosensor for paracetamol (PAR) determination based on a glassy carbon electrode (GCE) modified with multiwalled carbon nanotubes (MWCNT) and laccase enzyme (LAC), which was immobilized by means of covalent crosslinking using glutaraldehyde. Voltammetric investigations were carried out by cyclic voltammetry (CV), differential pulse voltammetry (DPV) and square wave voltammetry (SWV). The biosensor was characterized by Scanning Electron Microscope (SEM) and Fourier Transform Infrared Spectroscopy (FT‐IR). The results showed that the use of MWCNT/LAC composite increased the sensor sensitivity, compared to bare glassy carbon electrode. Factors affecting the voltammetric signals such as pH, ionic strength, scan rate and interferents were assessed. Linear range, limit of detection (LOD) and limit of quantitation (LOQ) obtained were 10–320 μmol L^?1, 7 μmol L^?1 and 10 μmol L^{? 1}, respectively. The developed biosensor was successfully applied to PAR determination in urine and pharmaceutical formulations samples, with recovery varying from 99.96 to 106.20 % in urine samples and a relative standard deviation less than 1.04 % for PAR determination in pharmaceutical formulations. Therefore, the MWCNT‐LAC/GCE exhibits excellent sensitivity and can be used to PAR determination as a viable alternative in clinical analyzes and quality control of pharmaceutical formulations, through a simple, fast and inexpensive methodology.     

A Glassy Carbon Electrode Modified with Multiwalled Carbon Nanotube/Chitosan Composite as a New Sensor for Simultaneous Determination of Acetaminophen and Mefenamic Acid in Pharmaceutical Preparations and Biological Samples

A new chemically modified electrode is constructed based on multiwalled carbon nanotube/chitosan modified glassy carbon electrode (MWCNTs‐CHT/GCE) for simultaneous determination of acetaminophen (ACT) and mefenamic acid (MEF) in aqueous buffered media. The measurements were carried out by application of differential pulse voltammetry (DPV), cyclic voltammetry (CV) and chronoamperometry (CA) methods. Application of DPV method showed that the linear relationship between oxidation peak current and concentration of ACT and MEF were 1 μM to 145 μM, and 4 μM to 200 μM, respectively. The analytical performance of this sensor has been evaluated for detection of ACT and MEF in human serum, human urine and a pharmaceutical preparation with satisfactory results.     

Direct Electrochemical Determination of Glyphosate at Copper Phthalocyanine/Multiwalled Carbon Nanotube Film Electrodes

A copper phthalocyanine/multiwalled carbon nanotube film‐modified glassy carbon electrode has been used for the determination of the herbicide glyphosate (Gly) at ?50 mV vs. SCE by electrochemical oxidation using differential pulse voltammetry (DPV). Cyclic voltammetry and electrochemical impedance spectroscopy showed that Gly is adsorbed on the metallic centre of the copper phthalocyanine molecule, with formation of Gly‐copper ion complexes. An analytical method was developed using DPV in pH 7.4 phosphate buffer solution, without any pretreatment steps: Gly was determined in the concentration range of 0.83–9.90 μmol L^?1, with detection limit 12.2 nmol L^?1 (2.02 μg L^?1).     

A Selective Simultaneous Determination of Levodopa and Serotonin Using a Glassy Carbon Electrode Modified with Multiwalled Carbon Nanotube/Chitosan Composite

A glassy carbon electrode (GCE) modified with carbon nanotube/chitosan (MWCNTs‐CHT/GCE) was used for the sensitive voltammetric determination of levodopa (Lev) and serotonin (Ser). The measurements were carried out using cyclic voltammetry (CV), differential pulse voltammetry (DPV) and chronoamperometry (CA). Under the optimum conditions the electrode provides a linear response versus Lev and Ser concentrations in the range of 2.0–220.0 µM and 0.5–130.0 µM, respectively, using DPV. The modified electrode was satisfactorily used for determination of Lev and Ser in human serum and urine with satisfactory results.     

Glassy Carbon Electrode Modified with Layering of Carbon Black/Poly(Allylamine Hydrochloride) Composite for Multianalyte Determination

An electrochemical sensor using glassy carbon electrode modified with carbon black within a poly(allylamine hydrochloride) film is proposed in this work. The novel sensor was characterized by scanning electron microscopy, electrochemical impedance spectroscopy, and cyclic voltammetry using the redox probe Fe(CN)6^3−/4−. The sensor was applied for the simultaneous determination of dopamine (DA), paracetamol (PAR), amlodipine (AML), and rosuvastatin (RSV). The quantification of all four analytes was carried out by linear sweep voltammetry and presented a linear concentration range for all analytes from 1.0 to 90 μmol L⁻¹, with limit of detection of 0.55, 1.3, 5.7, and 3.0 μmol L⁻¹ for DA, PAR, AML, and RSV, respectively. This sensor was successfully applied in the simultaneous determination of these analytes in environmental, pharmaceutical, and biological samples.     

Direct Electrocatalytic Oxidation and Simultaneous Determination of 5‐Methylcytosine and Cytosine at Electrochemically Reduced Graphene Modified Glassy Carbon Electrode

Direct electrocatalytic oxidation and simultaneous determination of 5‐methylcytosine (5‐mC) and cytosine(C) were realized in alkaline solutions by differential pulse voltammetry (DPV) based on an electrochemically reduced graphene oxide (er‐GO) modified glassy carbon electrode (er‐GO/GCE). The as‐prepared er‐GO/GCE exhibited good electrocatalytic activity towards the oxidation of 5‐mC and C. Under optimum conditions, the er‐GO/GCE was applied to the simultaneous determination of 5‐mC and C with a significantly improved peak potential resolution (about 150 mV), and a linear relationship can be obtained in the range of 6–200.0 µmol/L and 8–250.0 µmol/L, respectively. In addition, the proposed method was further successfully applied to the analysis of methylation status in short CpG oligonucleotides with satisfactory results.     

Electrocatalytic Oxidation and Determination of Nitrite at Multi‐walled Carbon Nanotubes Modified Carbon Ceramic Electrode

In the present work, the electrochemical oxidation of nitrite on carbon ceramic electrode (CCE) modified with multi‐walled carbon nanotubes (MWCNTs) was investigated. The modified electrode exhibited catalytic activity toward the electrooxidation of nitrite. Experimental parameters such as solution pH, scan rate, concentration of nitrite and nanotubes amount were studied. It was shown nitrite can be determined by differential pulse voltammetry (DPV) and hydrodynamic amperometry (HA) using the modified electrode. Under the optimized conditions the calibration plots are linear in the concentration ranges of 15‐220 and 50‐3000 μM with limit of detections of 4.74 and 35.8 μM for DPV and HA, respectively. The modified electrode was successfully applied for analysis of nitrite in spinach sample. The results were favorbly compared to those obtained by UV‐Visible spectrophotometric method. The results of the analysis suggest that the proposed method has promise for the routine determination of nitrite in the examined products.     

A Sensitive Simultaneous Determination of Epinephrine and Piroxicam Using a Glassy Carbon Electrode Modified with a Nickel Hydroxide Nanoparticles/Multiwalled Carbon Nanotubes Composite

The electrooxidation of epinephrine (EPI) and piroxicam (PRX) has been investigated by application of nickel hydroxide nanoparticles/multiwalled carbon nanotubes composite electrode (MWCNTs‐NHNPs/GCE) using cyclic voltammetry (CV), differential pulse voltammetry (DPV) and chronoamperometry (CA) methods. The modified electrode showed suitable electrochemical responses for EPI and PRX determination. Under the optimum conditions the electrode provides a linear response versus EPI and PRX concentrations in the range of 1–220 µM and 0.7–75 µM, respectively using the DPV method. Linear responses versus EPI and PRX concentrations in the range of 1–1000 µM and 1–800 µM, respectively, were obtained using the CA method. The modified electrode was used for determination of EPI and PRX in human urine with satisfactory results.     

Simultaneous Determination of Rosmarinic Acid and Protocatechuic Acid at Poly(o‐Phenylenediamine)/Pt Nanoparticles Modified Glassy Carbon Electrode

A system of Pt nanoparticles and poly(ortho‐phenylenediamine) film electrochemically deposited onto a glassy carbon electrode (GCE/PoPD/Pt) was fabricated. Scanning electron microscopy, Fourier‐transform infrared spectroscopy, and atomic force microscopy techniques were used to identify the surface characteristics of the composite electrode. The conductive polymers and Pt nanoparticles together resulted in a synergistic effect, and the new formed surface was highly active against polyphenolic structures. Rosmarinic acid (RA) and protocatechuic acid (PCA) are phenolic compounds found in plants, and they are used in many applications, particularly as pharmaceuticals. The GCE/PoPD/Pt was used for the simultaneous determination of RA and PCA in a pH 2.0 H₂SO₄ solution for the first time. The RA and PCA concentrations were determined using differential pulse voltammetry (DPV) and chronoamperometry. By the amperometry measurement, for RA and PCA, a linear relation was observed in the concentration ranges of 1–55 μmol L^?1 and 1–60 μmol L^?1, with detection limits of 0.5 μmol L^?1 and 0.6 μmol L^?1, respectively. In the simultaneous determination with DPV, the detection limits for both RA and PCA were calculated as 0.7 μmol L^?1. The GCE/PoPD/Pt was successfully used for the simultaneous determination of RA and PCA in a real sample, and its accuracy was verified by high‐performance liquid chromatography studies.     

Nanostructured Conducting Polymer/Copper Oxide as a Modifier for Fabrication of L‐DOPA and Uric Acid Electrochemical Sensor

A modified electrode was prepared by modification of the carbon paste electrode (CPE) with a nanostructured material. This nanostructure with electrocatalytic activity was synthesized by combination of poly pyrrole and copper oxide nanoparticles (PPy/CuO). The structure and morphology of PPy/CuO was studied. The fabricated modified electrode (CPE‐PPy/CuO) exhibited an excellent electrocatalytic activity toward levodopa (L‐DOPA) and uric acid (UA) oxidation because of high conductivity, low electron transfer resistance and catalytic effect. The CPE‐PPy/CuO had a lower overvoltage and enhanced electrical current with respect to the bare CPE for both L‐DOPA and UA. Also, the modified electrode showed a good resolution for the overlapped anodic peaks of L‐DOPA and UA. This electrode was used for the successful simultaneous determination of L‐DOPA and UA. The electrochemical sensor responded to L‐DOPA and UA in the concentration range of 0.050–1200 μM and 0.040–2000 μM, respectively. The detection limits were obtained by differential pulse voltammetry as 15 nM for L‐DOPA and 20 nM for UA. Finally, the proposed electrode was used for determination of L‐DOPA and UA in real samples using standard addition method.     

石墨烯修饰玻碳电极测定邻苯二酚

制备了用于测定邻苯二酚(CAT)的石墨烯修饰电极,并应用循环伏安法研究了CAT在该修饰电极上的电化学行为;用差分脉冲伏安法研究了测试底液的pH值对该修饰电极性能的影响,结果表明,此修饰电极在含不同浓度CAT的PBS溶液(pH=7.0)中测定,响应电流与CAT浓度在5.0×10-8～5.6×10-4mol/L范围内有良好的线性关系,相关系数r=0.9919,检出限为6.68×10-9mol/L(S/N=3)。与其它几种修饰电极相比,石墨烯修饰电极制备简单、响应时间快、操作简便,稳定性和重现性良好,有应用价值。     

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。     

Selective Voltammetric Detection of Uric Acid in the Presence of Ascorbic Acid at Well‐Aligned Carbon Nanotube Electrode

The voltammetric behaviors of uric acid (UA) and L ‐ascorbic acid (L ‐AA) were studied at well‐aligned carbon nanotube electrode. Compared to glassy carbon, carbon nanotube electrode catalyzes oxidation of UA and L ‐AA, reducing the overpotentials by about 0.028 V and 0.416 V, respectively. Based on its differential catalytic function toward the oxidation of UA and L ‐AA, the carbon nanotube electrode resolved the overlapping voltammetric response of UA and L ‐AA into two well‐defined voltammetric peaks in applying both cyclic voltammetry (CV) and differential pulse voltammetry (DPV), which can be used for a selective determination of UA in the presence of L ‐AA. The peak current obtained from DPV was linearly dependent on the UA concentration in the range of 0.2 μM to 80 μM with a correlation coefficient of 0.997. The detection limit (3δ) for UA was found to be 0.1 μM. Finally, the carbon nanotube electrode was successfully demonstrated as a electrochemical sensor to the determination of UA in human urine samples by simple dilution without further pretreatment.     

Platinum Nanoparticles/Poly(isoleucine) Modified Glassy Carbon Electrode for the Simultaneous Determination of Hydroquinone and Catechol

A new electrochemical sensor based on Poly(Isoleucine) modified glassy carbon electrode decorated with platinum nanoparticles (Pt/Poly(Isoleucine)/GCE) was developed for sensitive individual and simultaneous determination of hydroquinone (HQ) and catechol (CC). Scanning electron microscopy (SEM), Electrochemical impedance spectroscopy (EIS), Cyclic voltammetry (CV) and Differential pulse voltammetry (DPV) were performed in order to characterize the Pt/Poly(Isoleucine)/GCE nanocomposite. For simultaneous determination of HQ and CC, Pt/Poly(Isoleucine)/GCE showed wide linear range between the 0.01–100.0 μM. The detection limits were 0.006 μM for HQ and 0.005 μM for CC. The Pt/Poly(Isoleucine)/GC electrode exhibited good sensitivity and reliability in the simultaneous electroanalysis of two isomers in PBS of pH 7.5. The modified electrode was used to detect the isomers in naturel samples.     

Chitosan Incorporating Cetyltrimethylammonium Bromide Modified Glassy Carbon Electrode for Simultaneous Determination of Ascorbic Acid and Dopamine

Simultaneous determination of a neurotransmitter, dopamine (DA), and ascorbic acid (AA) is achieved at neutral pH on a chitosan incorporating cetyltrimethylammonium bromide (CTAB) modified glassy carbon (GC) electrode. Differential pulse voltammetry (DPV) technique was used to investigate the electrochemical response of DA and AA at a glassy carbon electrode modified with chitosan incorporating CTAB. An optimum 6.0 mmol L^?1 of CTAB together with 0.5 wt% of chitosan was used to improve the resolution and the determination sensitivity. In 0.1 mol L^?1 aqueous phosphate buffer solution of pH 6.8, the chitosan‐CTAB modified electrode showed a good electrocatalytic response towards DA and AA. The anodic peak potential of DA shifted positively, while that of AA shifted negatively. Thus, the difference of the anodic peaks of DA and AA reached 0.23 V, which was enough to separate the two anodic peaks very well. The presented method herein could be applied to the direct simultaneous determination of DA and AA without prior treatment. The anodic peak currents (I_pa) of DPV are proportional to DA in the concentration range of 8 μM to 1000 μM, to that of AA 10 μM to 2000 μM, with correlation coefficients of 0.9930 and 0.9945, respectively. The linear range is much wider than previously reported.     

聚(3-氨基-5-巯基-1,2,4-三唑)/多壁碳纳米管修饰的玻碳电极同时检测尿酸、黄嘌呤与次黄嘌呤

采用滴涂法得到多壁碳纳米管(MWCNTs)修饰的玻碳电极(GCE),通过电沉积方法将3-氨基-5-巯基-1,2,4-三唑(TA)沉积在MWCNTs/GCE表面,制备了聚(3-氨基-5-巯基-1,2,4-三唑)/多壁碳纳米管修饰电极(p TA/MWCNTs/GCE)。采用循环伏安法(CV)和示差脉冲伏安法(DPV),研究了尿酸(UA)、黄嘌呤(XA)和次黄嘌呤(HX)在该修饰电极上的电化学行为。结果表明,该修饰电极对UA、XA和HX均有较好的电催化活性作用,能实现对3种物质的同时测定。UA、XA和HX在该修饰电极上的线性范围分别为9.0~739.0、2.0~259.0、1.0~353.0μmol/L;检出限分别为0.67、0.17、0.33μmol/L。该修饰电极已成功用于尿液和血清实际样品中UA、XA和HX的同时测定,回收率为98.8%~105.5%。     

Highly Sensitive Nanostructured Electrochemical Sensor Based on Carbon Nanotubes-Pt Nanoparticles Paste Electrode for Simultaneous Determination of Levodopa and Tyramine

A multicomponent electrochemical sensor, with two nanometer-scale components in sensing matrix/electrode, was used to simultaneous determination of levodopa (LD) and tyramine (TR) in pharmaceutical and diet samples. Multiwall carbon nanotubes (MWCNTs) were used as carbonaceous materials in the electrode construction. 5-amino-3',4'-dimethoxy-biphenyl-2-ol (5ADMB) was used as electron mediator and Pt nanoparticles (nPt) as a catalyst. The 5ADMB catalyzes the oxidation of LD to the corresponding catecholamine, which is electrochemically reduced back to LD. Preparation of this electrode was very simple and modified electrode showed good properties at electrocatalytic oxidization of LD and TR. Using differential pulse voltammetry (DPV), a highly selective and simultaneous determination of LD and TR has been explored at the modified electrode. Differential pulse voltammetry peak currents of LD and TR increased linearly with their concentrations at the ranges of 0.50–100.0 μM and 0.60–100.0 μM, respectively. Also, the detection limits for LD and TR were 0.31 and 0.52 μM, respectively. The electrode exhibited an efficient catalytic response with good reproducibility and stability.     

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.     

还原氧化石墨烯-多壁碳纳米管复合膜负载金纳米粒子修饰玻碳电极检测双酚A

以水合肼为还原剂,采用均相还原法制备还原氧化石墨烯-多壁碳纳米管复合材料(rGO-MWCNTs),通过滴涂法将其修饰到玻碳电极(GCE)表面.以此复合材料为载体,采用电化学方法制备了金纳米粒子-还原氧化石墨烯-多壁碳纳米管复合膜修饰电极(AuNPs-rGO-MWCNTs/GCE).通过扫描电镜(SEM)、EDS能谱技术和电化学方法对此电极进行了表征.研究了双酚A在修饰电极上的电化学行为.结果表明,此电极对双酚A的电极过程具有良好的电化学活性,在0.10 mol/L PBS溶液(pH 7.0)中,微分脉冲伏安法测定双酚A的线性范围为5.0 × 10-9~1.0 × 10-7 mol/L和1.0 × 10-7~2.0 × 10-5 mol/L,检出限为1.0 ×10-9 mol/L(S/N=3). 将此电极用于模拟水样和超市购物小票样品中双酚A含量的测定,加标回收率分别为97%~110%和98%~104%.