Determination of Sulfide by Hematoxylin Multiwalled Carbon Nanotubes Modified Carbon Paste Electrode

This study investigates a new approach for the amperometric determination of sulfide using a hematoxylin multiwalled carbon nanotubes modified carbon paste electrode (HM‐MWCNTs/CPE). The experimental results show that HM‐MWCNTs/CPE significantly enhances the electrocatalytic activity towards sulfide oxidation. Cyclic voltammetric studies show that the peak potential of sulfide shifted from +400 mV at unmodified CPE to +175 mV at HM‐MWCNTs/CPE. The currents obtained from amperometric measurements at optimum conditions were linearly correlated with the concentration of sulfide. The calibration curve was obtained for sulfide concentrations in the range of 0.5–150×10^?6 mol L^?1. The detection limit was found to be 0.2×10^?6 mol L^?1 for the amperometric method. The proposed method was successfully applied to a river water sample in Pardubice, Czech Republic.     

碳纳米管碳糊电极吸附伏安法测定西沙必利

用循环伏安法和差分脉冲伏安法研究了西沙必利在多壁碳纳米管碳糊电极上的伏安行为和反应机理。在pH6.09Britton-Robinson缓冲液中,西沙必利在 0.89V(vs.SCE)处产生一灵敏的氧化峰。该氧化峰是由吸附控制的两电子一质子不可逆过程。其峰电流与浓度在4.0×10?8~2.0×10?5mol/L范围内呈线性关系(r=0.997),检出限为1.0×10?8mol/L。对5×10?6mol/L西沙必利平行测定10次的相对标准偏差为3.68%。用本法测定了片剂中西沙必利的含量,加标回收率为94.0%~104%。     

Electrochemistry and Adsorptive Stripping Voltammetric Determination of Amoxicillin on a Multiwalled Carbon Nanotubes Modified Glassy Carbon Electrode

The study of electrochemical behavior of amoxicillin (AMX), a β‐lactam antibiotic, is described on a multiwalled carbon nanotubes (MWCNTs) modified electrode by electrochemical impedance spectroscopy (EIS) and adsorptive stripping voltammetry for sensitive determination of AMX in pharmaceutical and human urine samples within a wide pH range from 2.0 to 10.0. Also, studies by Fe₂O₃ nanoparticles modified carbon paste electrode show that iron oxide impurities in the MWCNTs are not active sites for sensing of amoxicillin. Under optimized conditions, the oxidation peak has two linear dynamic ranges of 0.6–8.0 and 10.0–80.0 μM with a detection limit of 0.2 μM and a precision of <4%.     

Voltammetric Determination of Marbofloxacin at Carbon Paste Sensor Integrated with Copper Oxide Nanoparticles

The present work introduced copper oxide nanoparticles as an efficient electrode modifier for sensitive adsorptive differential pulse voltammetric assaying of marbofloxacin (MRB) in pharmaceutical formulations and surface water samples. In the presence of sodium dodecyl sulphate (SDS) at pH 4.0, the marbofloxacin molecule was irreversibly oxidized at the electrode surface showing an anodic oxidation peak at 0.954 V. The electrode reaction mechanism was assumed as adsorption-reaction controlled accompanied by the transferring of two electrons and proton exchange in agreement with the molecular orbital calculations performed on MRB molecule suggesting the oxidation of the amino group in the piperazinyl ring. At the optimized measuring conditions, the recorded peak heights were linearly correlated with the MRB concentration within the range from 6.67 to 360 ng mL⁻¹, and the estimated LOD value was 2.2 ng mL⁻¹. The integrated sensor showed a prolonged operational lifetime with good reproducibility of measurements. Based on the selectivity and sensitivity of the proposed method, MRB was successfully assayed in pharmaceutical formulations and surface water samples with mean average recoveries agreeable with the official method.     

Electrochemical Morphine Sensor Based on Gold Nanoparticles Metalphthalocyanine Modified Carbon Paste Electrode

Composites of gold nanoparticles (Au) electrochemically deposited and different metal phthalocyanines (Co, Ni, Cu, and Fe) were chemically prepared. The composites were used as modifiers for carbon paste electrodes and were used for the determination of morphine in presence of ascorbic acid and uric acid. Central metal atoms of phthalocyanine moiety affected the rate of electron transfer. Thus, the electroactivity of different modifiers were evaluated towards morphine oxidation. Au‐CoPcM‐CPE possessed the highest rate for charge transfer rate in all studied pH electrolytes. Limit of detection was 5.48×10^?9 mol L^?1 in the range of 4.0×10^?7 to 9.0×10^?4 mol L^?1.     

Determination of Trace Copper by Adsorptive Voltammetry Using a Multiwalled Carbon Nanotube Modified Carbon Paste Electrode

A new method for the determination of trace copper was described. A multiwalled carbon nanotube modified carbon paste electrode was prepared and the adsorptive voltammetric behavior of copper‐alizarin red S (ARS) complex at the modified electrode was investigated. By use of the second‐order derivative linear sweep voltammetry, it was found that in 0.04 mol/L acetate buffer solution (pH 4.2) containing 4×10^?6 mol/L ARS, when accumulation potential is 0 mV, accumulation time is 60 s and scan rate is 100 mV/s, the complex can be adsorbed on the surface of the electrode, yielding one sensitive reduction peak at ?172 mV (vs. SCE). The peak current of the complex is proportional to the concentration of Cu(II) in the range of 2.0×10^?11–4.0×10^?7 mol L^?1 with a detection limit (S/N=3) of 8.0×10^?12 mol/L (4 min accumulation). The proposed method was successfully applied to the determination of copper in biological samples with satisfactory results, the recoveries were found to be 96%–102%.     

羧基化碳纳米管修饰碳糊电极伏安法测定食盐中碘酸根

应用羧基化多壁碳纳米管(c-MWCNT)修饰碳糊电极,测定食盐中的碘酸根含量.在0.1 mol/L的NaOH电解液中,当IO3-在羧基化多壁碳纳米管修饰碳糊电极表面富集60 s,电位扫速为300 mV/s时,该修饰电极在线性扫描伏安图上能出现一灵敏的阴极溶出峰,峰电位为-0.52 V,峰电流与IO3-浓度在8.0×10-10~5.0×10-8mol/L和1.0×10-7~3.0×10-6mol/L的范围内成良好线关系,相关系数分别为0.999和0.998,检出限可达1.0×10-11mol/L;该修饰电极无汞,稳定性较好,用于加碘食盐中碘酸根含量的测定灵敏度高,平均回收率为101.1%.循环伏安(CV)测试表明,碘酸根在修饰电极上电化学反应是一不可逆过程,其电极反应标准均相速率常数为0.0109 cm.s-1.     

Novel Lu3+ Carbon Paste Electrode Based on Functionalized Multiwalled Carbon Nanotubes

A novel carbon paste ion selective electrode for determination of trace amount of lutetium was prepared. Modified (functionalized) multiwalled carbon nanotubes (f‐MWCNTs) were used for improvement of a lutetium carbon paste sensor response. MWCNTs have a good conductivity which helps the transduction of the signal in carbon paste electrode. In this work it is shown that introducing certain functional groups on MWCNTs can improve the electrode signals. The electrode composition of 20 % paraffin oil, 56 % graphite powder, 18 % ionophore and 6 % f‐MWCNTs showed the stable potential response to Lu³⁺ ions with the Nernstian slope of 21.1 (±0.3) mV decade^?1 over a wide linear concentration range of 1.0×10^?6–1.0×10^?1 mol L^?1. The electrode has fast response time (<15 s) and long term stability (about one month).     

Voltammetric Determination of Uric Acid with a Glassy Carbon Electrode Coated by Paste of Multiwalled Carbon Nanotubes and Ionic Liquid

The voltammetric behavior of uric acid (UA) has been studied at a multiwalled carbon nanotube‐ionic liquid (i.e., 1‐butyl‐3‐methylimidazolium hexafluorophosphate, BMIMPF₆) paste coated glassy carbon electrode (MWNTs‐BMIMPF₆/GC). It is found that UA can effectively accumulate at this electrode and cause a sensitive anodic peak at about 0.49 V (vs. SCE) in pH 4.0 phosphate buffer solutions. Experimental parameters influencing the response of the electrode, such as solution pH and accumulation time, are optimized for uric acid determination. Under the optimum conditions, the anodic peak current is linear to UA concentration in the range of 1.0×10^?8 M to 1.0×10^?6 M and 2.0×10^?6 M to 2.0×10^?5 M. The detection limit is 5.0×10^?9 M for 180 s accumulation on open circuit. The electrode can be regenerated by successively cycling in a blank solution for about 3 min and exhibits good reproducibility. A 1.0×10^?6 M UA solution is measured for eight times using the same electrode regenerated after every determination, and the relative standard deviation (RSD) of the peak current is 3.2%. As for different electrodes fabricated by the same way the RSD (i.e., the electrode to electrode deviation) is 4.2%(n=9). This method has been applied to the determination of UA in human urine samples, and the recoveries are 99%–100.6%. In addition, comparison is made between MWNTs‐BMIMPF₆/GC and MWNTs/GC. Results show that the MWNTs‐BMIMPF₆/GC exhibits higher sensitivity, selectivity and ratio of peak current to background current.     

L-半胱氨酸在环糊精复合碳纳米管电极上的伏安测定

L-半胱氨酸(CySH)连同其氧化形式的胱氨酸(CySSCy)在生命活动中起重要作用,有关其分析测试和性质研究备受关注．由于CySH的摩尔消光系数低,须通过巯基衍生化才适合于各种光谱法测定。电分析具有简便和灵敏度高的优点,但巯基化合物的不可逆氧化在绝大多数传统电极表面需要较正的过电势,因此电极修饰和新的功能性电极的开发就成为CySH电分析的关键．迄今,已研发了用于电化学测定CySH的多种修饰电极,但所有的电极都有缺陷。最近,又报道了Nation／铅钌酸盐烧绿石化学修饰电极及硼沉积的金刚石电极对CySH的电催化,实现了CySH的痕量分析．由碳纳米管(CNT)构置的电极对多巴胺等生物分子具有催化作用。L-L-     

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%。     

多壁碳纳米管化学修饰电极测定替硝唑的研究

替硝唑(Tinidazole,TNZ)是继甲硝唑后新一代的抗厌氧菌和抗滴虫的国家级二类新药,可广泛应用于临床各种厌氧菌感染。其测定方法有紫外分光光度法、高效液相色谱法、光度法及电化学方法等。但用碳纳米管修饰电极测定TNZ还未见报道。     

Voltammetric Determination of Trace Antiepileptic Gabapentin with a Silver‐Nanoparticle Modified Multiwalled Carbon Nanotube Paste Electrode

For the first time, a novel carbon nanotube bed electrode impregnated with silver–nanoparticles (AgNPs) for the determination of trace amounts of gabapentin (GBP) is described. We synthesized the AgNPs via a new procedure. The voltammetric behavior of the electrode was investigated by cyclic voltammetry. There were linear relationships in the ranges from 3.1×10^?9 to 2.9×10^?2 M and from 1.0×10^?8 to 1.0×10^?2 GBP with square wave and differential pulse voltammetric peak currents, respectively. The detection limits were 5.6×10^?10 and 9.7×10^?9 M, respectively. The electrode showed excellent response over a period of 2 months and was successfully applied in human plasma and pharmaceutical capsular products.     

Amperometric Lactate Biosensor Based on Carbon Paste Electrode Modified with Benzo[c]cinnoline and Multiwalled Carbon Nanotubes

Amperometric lactate biosensor based on a carbon paste electrode modified with benzo[c]cinnoline and multiwalled carbon nanotubes is reported. Incorporation of benzo[c]cinnoline acting as a mediator and multiwalled carbon nanotubes providing a conduction pathway to accelerate electron transfer due to their excellent conductivity into carbon paste matrix resulted in a high performance lactate biosensor. The resulting biosensor exhibited a fast response, high selectivity, good repeatability and storage stability. Under the optimal conditions, the enzyme electrode showed the detection limit of 7.0×10^?8 M with a linear range of 2.0×10^?7 M–1.1×10^?4 M. The usefulness of the biosensor was demonstrated in serum samples.     

Glassy Carbon Electrode Modified via Molybdenum Disulfide Decorated Multiwalled Carbon Nanotubes for Sensitive Voltammetric Detection of Aristolochic Acids

In this study, a molybdenum disulfide/multiwalled carbon nanotubes (MoS₂@MWCNTs) nanocomposite was synthesized by employing a simple hydrothermal method. The flower‐like structure of the MoS₂@MWCNTs was characterized via scanning electron microscopy (SEM) and transmission electron microscopy (TEM), and the load of crystalline MoS₂ was verified via X‐ray diffraction (XRD) and energy‐dispersive spectroscopy (EDS). The as‐prepared MoS₂@MWCNTs nanocomposite was used to modify glassy carbon electrode (GCE) as an electrochemical sensor for detecting aristolochic acids (AAs). With the optimized parameters, the proposed electrochemical sensor exhibited good sensitivity and a broad linear concentration range for detecting AAs from 0.2 to 10 μ mol/L and 10 to 100 μ mol/L, with the sensitivity of ?3.10 μ A/(μ mol/L) and ?0.91 μ A/(μ mol/L), respectively. The detection limit was also calculated as 0.06 μ mol/L (S/N=3) based on the low background signal. Furthermore, the modified electrochemical sensor exhibited good selectivity, repeatability, reproducibility, and stability, thus showing potential application for detecting AA in chinese herbs with good mean recovery and accuracy. In other words, the MoS₂@MWCNTs/GCE can be used as an excellent platform to detect AAs.     

Voltammetric Determinations of Thymol on an Electrode Modified by Coimmobilized Carboxylated Multiwalled Carbon Nanotubes and Surfactants

Thymol is oxidized at glassy carbon electrodes (GCEs) modified with coimmobilized carboxylated multiwalled carbon nanotubes (MWCNT-COOH) and surfactants of various nature in a Britton–Robinson buffer solution. The effect of the nature and concentration of surfactants in the composition of the electrode surface modifier on the amperometric response of thymol was evaluated. It was found that the best voltammetric characteristics are achieved in the case of an anionic 0.10 mM sodium dodecyl sulfate (SDS) (a decrease in oxidation potential by 50 mV and an increase in oxidation currents 2.2-fold in comparison with MWCNT-COOH/GCE). The electrooxidation of thymol at MWCNT-COOH–SDS/GCE proceeds irreversibly with the participation of one electron and one proton and is controlled by the adsorption of the analyte. The electrode response is linear in the ranges 0.500–17.0 and 17.0–150 μM of thymol with the limits of detection 0.14 μM and determination 0.48 μM. The developed method is tested on thymol-containing pharmaceutical preparations. The voltammetry data are compared with the results of an independent spectrophotometric determination.     

生物合成纳米金与MWCNTs/L-Cys复合修饰玻碳电极测定左旋多巴

利用荷叶萃取液生物合成纳米金,并与多壁碳纳米管/L-半胱氨酸复合成修饰电极材料,研究了左旋多巴在该修饰电极上的电化学行为.在0.2 mol/L乙酸-乙酸钠体系(pH=2.6)中,氧化峰电流与左旋多巴浓度在0.6~40μmol/L及60~120μmol/L范围内呈良好的线性关系,检出限达5.2×10-8mol/L.实验结果表明,生物合成纳米金复合多壁碳纳米管/L-半胱氨酸修饰电极具有良好的稳定性和高灵敏度,对实际样品测定的回收率在91.2%~102.5%之间.     

Carbon Paste Electrode Modified by Surfactant for Anodic Stripping Voltammetric Determination of Sulphadiazine

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多壁碳纳米管修饰玻碳电极伏安法测定氯霉素

研究了氯霉素(CAP)在多壁碳纳米管修饰玻碳电极上的电化学行为.发现在pH=2.0的0.1 mol/LKCl-HCl底液中,CAP在该修饰电极上有一灵敏的还原峰(Ep=-0.36 V vs.Ag/AgCl),峰电流与CAP浓度成正比,线性范围为6.0×10-6~2.7×10-4mol/L,检测限达3.0×10-6mol/L.该方法灵敏、准确,用于模拟样品和实际样品的测定,结果满意.     

Acetylferrocene Modified Carbon Paste Electrode; A Sensor for Electrocatalytic Determination of Hydrazine

The electrocatalytic oxidation of hydrazine at a carbon paste electrode spiked with acetylferrocene as a mediator was studied by cyclic voltammetry, differential pulse voltammetry, and chronoamperometry. In contrast to other ferrocenic compounds, acetylferrocene exhibits a chemical irreversible behavior, but it can act as an effective mediator for electrocatalytic oxidation of hydrazine, too. The heterogeneous electron transfer rate constant between acetylferrocene and the electrode substrate (carbon paste) and the diffusion coefficient of spiked acetylferrocene in silicon oil were estimated to be about 3.45×10^?4 cm s^?1 and 4.45×10^?9 cm² s^?1, respectively. It has been found that under the optimum conditions (pH 7.5) the oxidation of hydrazine occurs at a potential of about 228 mV less positive than that of an unmodified carbon paste electrode. The catalytic oxidation peak current of hydrazine was linearly dependent on its concentration and the obtained linear range was 3.09×10^?5 M–1.03×10^?3 M. The detection limit (2σ) has been determined as 2.7×10^?5 M by cyclic voltammetry. Also, the peak current was increased linearly with the concentration of hydrazine in the range of 1×10^?5 M–1×10^?3 M by differential pulse voltammetry with a detection limit of 1×10^?5 M. This catalytic oxidation of hydrazine has been applied as a selective, simple, and precise new method for the determination of hydrazine in water samples.