Highly Sensitive and Selective Voltammetric Sensor Fullerene Modified Glassy Carbon Electrode for Determination of Cefitizoxime in Solubilized System

The usefulness of fullerene modified glassy carbon electrode in mediating the reduction of cefitizoxime in solubilized system has been demonstrated. Due to the unique structure and extraordinary properties, fullerene shows higher catalytic efficiency towards cefitizoxime reduction. The kinetic parameters, electron transfer coefficient (α) and rate constant (K₀) across the modified electrode are 0.37 and 0.1081/s respectively. The proposed square‐wave voltammetric method is linear over the concentration range 1.2–10.3 µg/mL. The limit of detection (LOD) is found 0.27 ng/mL. High sensitivity and selectivity together with low detection limit of the electrode response make it suitable for the determination of cefitizoxime.     

Nafion修饰碳纤维微电极在抗坏血酸共存下选择性测定去甲肾上腺素

制备了碳纤维微电极,将洁净的碳纤维微电极浸入Nafion溶液中,采用电沉积的方法制得Nafion修饰碳纤维微电极。采用循环伏安法(CV)、差分脉冲伏安法(DPV)研究了去甲肾上腺素(NE)和抗坏血酸(AA)在电极上的电化学行为。结果表明:在最优条件下制备的Nafion修饰电极能完全屏蔽AA的电化学响应,而对NE仍表现出良好的电化学响应。修饰电极能在1.0 mmol/L AA的共存下选择性地测定NE,采用DPV进行检测,NE的氧化峰电流与其浓度在1.0×10~(-6)~1.0×10~(-4)mol/L范围内呈良好的线性关系,相关系数(r~2)为0.991 2,检出限(S/N=3)为8.6×10~(-7)mol/L。利用该方法测定了模拟样品中NE的含量,平均加标回收率为101.6%。该电极的重现性和稳定性良好,且具有良好的灵敏度和选择性,有望用于复杂生物环境中NE浓度的检测。     

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.     

Voltammetric determination of cefpirome at multiwalled carbon nanotube modified glassy carbon sensor based electrode in bulk form and pharmaceutical formulation

A new, simple and low cost voltammetric method for the determination of cefpirome in pharmaceutical preparations has been developed using multiwalled carbon nanotube modified glassy carbon electrode (MWCNT), which showed stable response with enhanced selectivity and sensitivity over the bare glassy carbon electrode. A multiwalled carbon nanotube (MWCNT) modified glassy carbon electrode (GCE) is used for the simultaneous determination of cefpirome by differential pulse voltammetry and square wave voltammetry. Results indicated that cathodic peak of cefpirome is greatly improved at MWCNT modified GC electrode as compared with the bare GC electrode showing excellent electrocatalytic activity towards cefpirome reduction. Linear calibration curves are obtained over the concentration range 100-600 μg mL(-1) in Britton Robinson buffer at pH 4.51 with limit of detection (LOD) and limit of quantification (LOQ) are 0.647 μg mL(-1) and 2.159 μg mL(-1) using SWV and 5.540 μg mL(-1) and 18.489 μg mL(-1) using DPV, respectively. The described method is rapid and can be successfully applied for the determination of cefpirome in bulk form and pharmaceutical formulations.     

亚硝酸根在纳米金修饰玻碳电极上的电催化氧化行为及其测定

采用直接电化学沉积法制备出纳米金修饰玻碳电极,研究了其对亚硝酸根的电催化氧化作用。结果表明,亚硝酸根在该修饰电极上于0.8 V处出现了一个良好的氧化峰。在最优实验条件下,亚硝酸根的峰电流与其浓度在2×10-6～2×10-3mol/L范围内呈一定的线性关系,检出限为6.0×10-7(S/N=3),提出了用循环伏安法测定亚硝酸根的方法。纳米金修饰电极用于东莞自来水水样中亚硝酸根的测定,回收率在98.1%～101.4%之间。对比本方法,用分光光度法对东莞自来水样中亚硝酸根进行了测定,结果满意。     

CTAB存在下双酚A在纳米氧化锌/碳纳米管复合材料修饰电极上的电化学行为及测定

利用水热法合成了纳米氧化锌/碳纳米管复合材料,将该复合材料滴涂在玻碳电极表面,制得纳米氧化锌-碳纳米管复合材料修饰电极(ZnO-MWCNTs/GCE)。在阳离子表面活性剂十六烷基三甲基溴化铵(CTAB)存在下,利用循环伏安法研究了双酚A在修饰电极上的电化学行为。考察了溶液pH值、CTAB浓度和富集时间等对测定的影响。结果表明,在pH 7.0的含8.0×10-5mol/L CTAB的磷酸盐缓冲液中,该修饰电极对双酚A具有良好的电化学响应,双酚A在修饰电极上的氧化峰电流为裸电极上的7倍。在优化条件下,采用差分脉冲伏安法对双酚A进行测定。双酚A的峰电流在5.0×10-8~1.5×10-5mol/L浓度范围内呈良好的线性关系,检出限(S/N=3)为1.0×10-8mol/L。对1.0×10-5mol/L双酚A平行测定8次的相对标准偏差为4.6%。该法用于塑料制品中溶出双酚A的测定,回收率为99%~107%,结果满意。     

Synthesis and application of a natural-based nanocomposite with carbon nanotubes for sensitive voltammetric determination of lead (II) ions

ABSTRACT

A modified carbon paste electrode has been developed for the determination of Pb(ΙΙ) ions based on Fe₃O₄/eggshell magnetic nanocomposite. The structure and morphology of Fe₃O₄/eggshell were analysed by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The prepared nanocomposite was also characterized by Fourier transform infrared spectroscopy (FT-IR) and vibrating sample magnetometer (VSM). The electrochemical procedure was based on the accumulation and determination of Pb(ΙΙ) ions at the surface of the modified carbon paste electrode with Fe₃O₄/eggshell nanocomposites and carbon nanotubes by differential pulse anodic stripping voltammetry (DPASV). Various experimental parameters involved in the preconcentration of Pb(ΙΙ) ions and voltammetric stripping step were studied. Under the optimum conditions, the voltammetric peak current of Pb(ΙΙ) occurs at a potential about ?0.5 V. Also, the voltammetric peak current increased linearly with Pb(ΙΙ) concentration in the range of 0.5–200 ng mL^?1 and a detection limit of 0.15 ng mL^?1 was obtained for Pb(ΙΙ). The selectivity of the proposed electrode for Pb(ΙΙ) ions in the presence of some cations was also examined. The practical application of the proposed modified electrode was evaluated by the determination of Pb(ΙΙ) ions in human hair and water samples. The results were satisfactory for the spiked samples.     

Electrooxidative behavior and determination of trifluoperazine at multiwalled carbon nanotube-modified glassy carbon electrode

The mechanism of electrochemical oxidation of trifluoperazine has been proposed on the basis of cyclic and differential pulse voltammetry at a multiwalled carbon nanotube-modified glassy carbon electrode. The modified electrode exhibits catalytic activity, high sensitivity, and stability. The oxidation process exhibited an adsorption-controlled behavior. Also, depending on this adsorption control, a sensitive electroanalytical method for the determination of trifluoperazine has been investigated by adsorptive stripping differential pulse voltammetry. Under the optional conditions, the anodic peak current was linear to the trifluoperazine concentration over the range of 2.08 10^?8?M to 1.67 10^?6?M, and the limit of detection was 7.49 10^?10?M. The modified electrode had good stability and repeatability, and it was successfully applied to the determination of trifluoperazine in pharmaceuticals.     

双酚A在纳米金-离子液体复合修饰电极上的电化学行为及测定

该文制备了纳米金-离子液体修饰电极(GNP-[BMIM]PF6/GCE),用红外光谱对GNP和[BMIM]PF6进行了表征.采用交流阻抗法研究了GNP-[BMIM]PF6/GCE的表面电化学特性,同时研究了双酚A(BPA)在该修饰电极上的循环伏安行为.结果表明,BPA在该修饰电极上出现1个氧化峰,无还原峰,为不可逆电化...     

Electrochemical behavior and voltammetric determination of norfloxacin at glassy carbon electrode modified with multi walled carbon nanotubes/Nafion

A simple and rapid electrochemical method is developed for the determination of trace-level norfloxacin, based on the excellent properties of multi-walled carbon nanotubes (MWCNTs). The MWCNTs/Nafion film-coated glassy carbon electrode (GCE) is constructed and the electrochemical behavior of norfloxacin at the electrode is investigated in detail. The results indicate that MWCNTs modified glassy carbon electrode exhibited efficiently electrocatalytic oxidation for norfloxacin (NFX) with relatively high sensitivity, stability and life time. Under conditions of cyclic voltammetry, the current for oxidation of selected analyte is enhanced significantly in comparison to the bare GCE. The electrocatalytic behavior is further exploited as a sensitive detection scheme for the analyte determinations by linear sweep voltammetry (LSV). Under optimized condition in voltammetric method the concentration calibration range and detection limit (S/N=3) are 0.1-100 micromol/L and 5 x 10(-8)mol/L for NFX. The proposed method was successfully applied to NFX determination in tablets. The analytical performance of this sensor has been evaluated for detection of the analyte in urine as a real sample.     

Electrochemical behavior of phenol at acetylene black-dihexadecyl hydrogen phosphate composite modified glassy carbon electrode in the presence of cetyltrimethylammonium bromide

The electrochemical response of phenol at acetylene black (AB)-dihexadecyl hydrogen phosphate (DHP) composite modified glassy carbon electrode in the presence of cetyltrimethylammonium bromide (CTAB) was investigated. In this system, a sensitive oxidation peak at 0.62 V (SCE) was obtained. The electrode process and the influence of CTAB on the oxidation of phenol were explored by chronocoulometry and linear sweep voltammetry (LSV). Experimental conditions for the determination of phenol were optimized. In the range of 5.0 × 10⁻⁷ to 1.2 × 10⁻⁵ M, the phenol concentration was linear with the oxidation peak current and the detection limit was found to be 1.0 × 10⁻⁷ M for 3 min accumulation. The method was applied for the determination of phenol in lake water and the results were satisfactory. Published in Russian in Elektrokhimiya, 2008, Vol. 44, No. 2, pp. 222–229. The text was submitted by the authors in English.     

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。     

Sensitive determination of phenols in environmental water samples with SPE packed with bamboo carbon prior to HPLC

Bamboo carbon, an inexpensive, readily available material, has attracted great attention in recent years because of adsorptive properties. In this paper, the potential of bamboo carbon as a SPE adsorbent for the determination of phenols, was investigated. Phenols are important environmental contaminants that may adversely affect human health. Parameters influencing extraction efficiency, including type of eluent, eluent volume, amount of adsorbent, as well as sample pH, volume, and flow rate were investigated and optimized. The optimized results exhibited excellent linear relationships between peak area and phenol concentrations over the range of 2.0–100 ng/mL, with precision between 2.2–7.2%. The LODs were 0.06–0.4 ng/mL for the eight phenols tested. The proposed method has been successfully applied to the analysis of several real‐world environmental water samples. These results indicate that bamboo carbon may be used as a novel SPE adsorbent for the concentration and determination of phenols in real environmental water samples.     

A Disposable Carbon Nanotubes‐screen Printed Electrode (CNTs‐SPE) for Determination of the Antifungal Agent Posaconazole in Biological Samples

For the first time, the use of carbon nanotubes was exploited for the development of a sensitive electrochemical method for determination of the newly antifungal posaconazole (POS). The electrochemical activity of POS was investigated at the surface of multi‐walled nanotubes (MWNTs) modified electrode. The cyclic voltammograms showed a sharp oxidation peak at potential around 671 mV vs. Ag/AgCl. To reach the assay optimization, factors affecting the method sensitivity have been investigated, such as types of carbon nanotubes and its concentration in the electrode matrix, type of supporting electrolyte, pH, accumulation time and scan rate. A good linear relationship was obtained within the concentration range from 32–1280 ng/ml with the limit of detection and quantification of 11 ng/ml and 33 ng/ml, respectively. The proposed method was successfully applied for the determination of POS in its commercial dosage form, spiked human plasma samples, and dried blood spots. The in vivo results obtained were also used to study the pharmacokinetics of POS in human plasma. The results obtained were validated and found to be in accordance with those obtained by the reference methods.     

多巴胺和抗坏血酸在十六烷基三甲基溴化铵/碳纳米管电极上的检测

研究了十六烷基三甲基溴化铵(CTMAB)/多壁碳纳米管修饰玻碳电极的制备以及多巴胺和抗坏血酸在该修饰电极上的电化学行为。在CTMAB和多壁碳纳米管的协同作用下,该修饰电极对多巴胺和抗坏血酸均具有显著的催化氧化作用,多巴胺和抗坏血酸的氧化峰电位分别为223mV和15mV,实现了在抗坏血酸共存时测定多巴胺。在pH7.0的磷酸盐缓冲溶液中,多巴胺和抗坏血酸的线性范围分别为2.0×10-6～2.0×10-3mol/L和4.0×10-5～1.0×10-2mol/L,检出限分别为6.0×10-7mol/L和1.0×10-5mol/L。     

Electrochemical determination of dipyridamole at a carbon paste electrode using cetyltrimethyl ammonium bromide as enhancing element

Electrochemical behaviors of dipyridamole (DIP) at a carbon paste electrode in the presence of cetyltrimethyl ammonium bromide (CTAB) were investigated by voltammetry, chronocoulometry and electrochemical impedance spectroscopy (EIS). The results indicated that the electrochemical responses of DIP are apparently improved by CTAB, due to the enhanced accumulation of dipyridamole at the carbon paste electrode surface. Electrochemical parameters for the oxidation of DIP were explored by chronocoulometry. Under optimal conditions, the oxidation peak current at 0.53 V was proportional to DIP concentration in the range of 0.03-12 microg mL-1, with a detection limit of 0.01 microg mL-1 for 120 s accumulation by different pulse voltammetry (DPV). This method was applied to the determination of DIP in the tablet samples. The results were satisfying compared with that obtained by standardized method of high performance liquid chromatography (HPLC).     

多壁碳纳米管修饰电极检测盐酸氯丙嗪的研究

制备了多壁碳纳米管修饰玻碳电极,采用循环伏安法(CV)研究了盐酸氯丙嗪在修饰电极上的电化学特性,发展了一种新的检测盐酸氯丙嗪的电化学分析方法。在最佳实验条件下,用循环伏安法检测盐酸氯丙嗪,其响应电流与盐酸氯丙嗪的浓度在8.0×10-5~1.0×10-3mol/L范围内有很好的线性关系,线性方程为Ip(A)=0.0106c(mol/L)-8×10-8(R2=0.999,n=6),检出限为6.2×10-6mol/L(S/N=3)。方法可用于盐酸氯丙嗪片的测定。     

Voltammetric determination of tinidazole using a glassy carbon electrode modified with single-wall carbon nanotubes.

An electrochemical method based on a single-wall carbon nanotubes (SWNTs) film-coated glassy carbon electrode (GCE) was described for the determination of tinidazole. In a 0.1 M Britton-Robinson buffer with a pH of 10.0, tinidazole yields a very sensitive and well-defined reduction peak at -0.78 V (vs. SCE) on a SWNTs-modified GCE. Compared with that on a bare GCE, the reduction peak of tinidazole increases significantly on the modified GCE. Thus, all of the experimental parameters were optimized and a sensitive voltammetric method is proposed for tinidazole determination. It is found that the reduction peak current is proportional to the concentration of tinidazole over the range from 5 x 10(-8) to 4 x 10(-5) M, and that the detection limit is 1 x 10(-8) M at 3 min open-circuit accumulation. This new analysis method was demonstrated with tinidazole drugs.     

γ-Oryzanol-loaded calcium pectinate microparticles reinforced with chitosan: Optimization and release characteristics

The cationic surfactant, cetyltrimethyl ammonium bromide (CTAB) effect on accurate determination of dopamine in the presence of ascorbic acid (as natural obtrusive in determination of dopamine) using chemically modified electrode based on tin hexacyanoferrate (SnHCF) as a modifier at carbon paste electrode (CPE) is described. The electrochemical response of bare CPE and SnHCF modified electrode (ME) examined in different pHs, in absence and presence of different concentration of dopamine (DA) and ascorbic acid (AA). In addition a simple and reliable method for simultaneous electrochemical determination of AA and DA was presented. It was based on the use of the cationic surfactant CTAB that enables the separation of the oxidation peaks potential of AA and DA. The experimental results showed that DA and AA have two separate peaks. In pH 3 and at presence of 3 mM of CTAB the separation of DA and AA peaks and the eminence of them increased evidently. Good linear response to AA and DA was observed in the range of 0.4–50 and 0.2–25 mM with the correlation of 0.9912 and 0.9955, respectively.     

在3,4-二羟基肉桂酸介质中以多壁碳纳米管为传感器电催化检测L-半胱氨酸(英文)

A highly sensitive electrochemical sensor was prepared for the determination of L-cysteine using a modified multiwall carbon nanotubes paste electrode in the presence of 3,4-dihydroxycinnamic acid(3,4-DHCA) as a mediator, based on an electrocatalytic process. The results indicate that the electrode is electrocatalytically efficient for the oxidation of L-cysteine in the presence of 3,4-DHCA. The interaction between the mediator and L-cysteine can be used for its sensitive and selective determination. Using chronoamperometry, the catalytic reaction rate constant was calculated to be 2.37 × 102 mol–1 L s–1. The catalytic peak current was linearly dependent on the L-cysteine concentration in the range of 0.4–115 μmol/L. The detection limit obtained by linear sweep voltammetry was 0.25 μmol/L. Finally, the modified electrode was examined as a selective, simple, and precise new electrochemical sensor for the determination of L-cysteine in real samples.