聚苏木精修饰玻碳电极测定酪氨酸

通过在玻碳电极上电聚合聚苏木精的方法制备了聚苏木精修饰电极,研究了酪氨酸在修饰电极上的电化学行为。在0.1 mol/L磷酸盐缓冲溶液(pH3.0)中,富集电位为-0.3 V,富集时间为180 s,氧化峰电流与酪氨酸的浓度在5.0×10-6～1.0×10-4mol/L的范围内呈良好的线性关系,检出限为3.0×10-7mo...     

Quantification of methyldopa in pharmaceuticals using a glassy carbon electrode modified with carbon nanotubes

The quantification of methyldopa in pharmaceuticals has been carried out using a glassy carbon electrode(GCE) modified with multi-walled carbon nanotubes(MWCNTs). Methyldopa exhibited a quasi-reversible response with a peak potential separation of 473 m V on a bare GCE. However, the cyclic voltammetric behaviour of methyldopa was improved with the increase of the amount of MWCNTs. It was also shown that the electrocatalytic activity of the electrode towards the response of methyldopa was higher with larger amount of film on the surface. The results showed that the peak current was proportional to the concentration of methyldopa with a linear dynamic range of 0.005–0.388 mmol/L and a detection limit of 1.0 nmol/L was obtained using square wave voltammetry. The experimental data showed that the detection limit of methyldopa and peak separation from interfering compounds such as ascorbic acid(AA) and uric acid(UA) were improved using the proposed procedure. The method was successfully applied for the determination of methyldopa in pharmaceuticals.     

Studies on the electrochemistry of rutin and its interaction with bovine serum albumin using a glassy carbon electrode modified with carbon-coated nickel nanoparticles

We report on a glassy carbon electrode modified with carbon-coated nickel nanoparticles (C-Ni/GCE) that can be used to study the electrochemical properties of rutin and its interaction with bovine serum albumin (BSA) via cyclic voltammetry and differential pulse voltammetry. The effects of pH value, accumulation potential, accumulation time and reaction time were optimized. A pair of reversible peaks is found in the potential range of 0 to around 0.6 V at pH?5.0. Two linear response ranges (with different slopes) are found, one in the 2 to 210 nM concentration range, the other between 0.21 and 1.72 μM. The detection limit is as low as 0.6 nM. On addition of BSA to the rutin solution, a decrease of the current is observed that is proportional to the concentration of BSA. The binding constant and stoichiometric ratio were calculated.

Determination of nitrite with a nano-gold modified glassy carbon electrode by cyclic voltammetry

Abstract

Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) was employed to determine the concentration of rare earth elements (REEs) in plants and soils. Sample preparation and analytical conditions were investigated to set up a simple routine procedure for measuring rare earth elements. For prompt sample decomposition, a microwave digestion technique was successfully used with an acid mixture of HCl+HNO₃+HF. Detection limits, reproducibility, accuracy and possible interference were also studied. ICP-MS provided extremely low detection limits for REEs (0.6–6ng/l). Precision was typically better than 6% RSD (relative standard deviation) for soil and 10% for plant. The potential of the method was evaluated by analysis of standard reference materials of soils and plants. A good agreement between the experimental results and certified values was observed. The spectroscopic interference of Ba with Eu and light REEs(LREEs, La-Eu) with heavy REEs(HREEs, Gd-Lu) were eliminated by the algebra correction.

The results suggested that REEs in soil samples existed mainly as light REEs, and the same concentration distribution patterns of Oddo-Hakins law were observed, showing negative gradient from La to Lu concentrations. The REE contents in plants were very low, less than 20μg/g and varied with plant species. Apart from rape leaf(Brassica juncea), the REE distribution patterns in other plant leaves were consistent with soils, indicating that these plants generally absorbed REEs from soil without selectivity. Rape leaf showed selective absorption for LREEs, especially for La. The REE concentration distribution in parts of hot pepper(Capsicum annuum) was characteriaed by root>leaf>stem>fruit. The REEs absorbed by hot pepper concentrated mainly in roots and leaves, very little migrated into fruit. Transfer factors(TFs) of REEs in plants were very low. Although the contents of LREEs were relatively more than those of HREEs, no distinct difference of TFs between LREEs and HREEs was observed, meaning that LREEs and HREEs have the same abilities of transportation. However, for rape leaf, the TFs of LREEs were one or two orders of magnitude higher than those of HREEs.     

Non-enzymatic sensing of glucose at neutral pH values using a glassy carbon electrode modified with carbon supported Co@Pt core-shell nanoparticles

Co@Pt core-shell nanoparticles (NPs) were synthetized by a two-step reductive method using carbon (Vulcan XC-72) as a solid support. The NPs were characterized by X-ray diffraction, field emission gun scanning electron microscopy, energy dispersive X-ray spectroscopy, and transmission electron microscopy. Their electrochemical performance was evaluated by cyclic voltammetry, electrochemical impedance spectroscopy and chronoamperometry, and these showed that the Co@Pt NPs display an electrocatalytic activity towards the oxidation of glucose that is much better than that of plain Pt NPs. Under optimized conditions and at pH 7.0, the oxidation current of glucose at a working potential of −50 mV (vs. SCE) is linearly related to its concentration in the 1.0 to 30 mM range, and the detection limit is 0.3 mM (S/N = 3). It therefore covers the clinical range. The sensor also exhibits excellent stability and repeatability.

Co@Pt core-shell nanoparticles (NPs) display an electrocatalytic activity towards the oxidation of glucose that is much better than that of plain Pt NPs. The oxidation current for glucose is linearly related to its concentration in the 1.0 to 30 mM range, and the detection limit is 0.3 mM (S/N =3).

     

多壁碳纳米管-Nafion修饰电极测定左旋氧氟沙星

本文报道了用多壁碳纳米管-Nafion修饰玻碳电极测定痕量左旋氧氟沙星的方法。详细研究了左旋氧氟沙星在修饰电极上的电化学行为。实验表明,该电极对左旋氧氟沙星具有良好的电催化作用。在伏安图中,+1.73V处出现一灵敏氧化峰,利用该峰可进行左旋氧氟沙星的测定。在优化条件下,氧化峰电流与左旋氧氟沙星的浓度在0.001~0.5 mg.mL-1范围内成良好的线性关系。信噪比等于3时,检出限为1×10-4mg.mL-1。用于实际样品中左旋氧氟沙星的测定,加标回收率为97.32~102.82。     

Sensitive and selective determination of hydrazine using glassy carbon electrode modified with Pd nanoparticles decorated multiwalled carbon nanotubes

A glassy carbon electrode modified with palladium nanoparticles decorated multiwalled carbon nanotubes (GCE/nanoPd-MWCNTs) was fabricated. Incorporation of palladium nanoparticles onto the carbon nantube surface by thermal decomposition of palladium acetate led to the fabrication of a sensor with a significant decrease in hydrazine electrooxidation potential. The sensor exhibited low detection limits, high sensitivity and selectivity, rapid response, and good stability toward hydrazine detection.     

Simultaneous sensing of L-tyrosine and epinephrine using a glassy carbon electrode modified with nafion and CeO2 nanoparticles

An electrochemical sensor was developed and tested for detection of L-tyrosine in the presence of epinephrine by surface modification of a glassy carbon electrode (GCE) with Nafion and cerium dioxide nanoparticles. Fabrication parameters of a surfactant-assisted precipitation method were optimized to produce 2–3 nm CeO₂ nanoparticles with very high surface-to-volume ratio. The resulting nanocrystals were characterized structurally and morphologically by X-ray diffractometery (XRD), scanning and high resolution transmission electron microscopy (SEM and HR-TEM). The nanopowder is sonochemically dispersed in a Nafion solution which is then used to modify the surface of a GCE electrode. The electrochemical activity of L-tyrosine and epinephrine was investigated using both a Nafion-CeO₂ coated and a bare GCE. The modified electrode exhibits a significant electrochemical oxidation effect of L-tyrosine in a 0.2 M Britton-Robinson (B-R) buffer solution of pH 2. The electro-oxidation peak current increases linearly with the L-tyrosine concentration in the molar concentration range of 2 to 160 μM. By employing differential pulse voltammetry (DPV) for simultaneous measurements, we detected two reproducible peaks for L-tyrosine and epinephrine in the same solution with a peak separation of about 443 mV. The detection limit of the sensor (signal to noise ratio of 3) for L-tyrosine is ~90 nM and the sensitivity is 0.20 μA μM⁻¹, while for epinephrine these values are ~60 nM and 0.19 μA μM⁻¹. The sensor exhibited excellent selectivity, sensitivity, reproducibility and stability as well as a very good recovery time in real human blood serum samples.

Simultaneous electrochemical determination of L-tyrosine and epinephrine in blood plasma with Nafion-CeO₂/GCE modified electrode showing a 443 mV peak-to-peak potential difference between species oxidation peak currents.

     

Simultaneous sensing of L-tyrosine and epinephrine using a glassy carbon electrode modified with nafion and CeO2 nanoparticles

An electrochemical sensor was developed and tested for detection of L-tyrosine in the presence of epinephrine by surface modification of a glassy carbon electrode (GCE) with Nafion and cerium dioxide nanoparticles. Fabrication parameters of a surfactant-assisted precipitation method were optimized to produce 2–3 nm CeO₂ nanoparticles with very high surface-to-volume ratio. The resulting nanocrystals were characterized structurally and morphologically by X-ray diffractometery (XRD), scanning and high resolution transmission electron microscopy (SEM and HR-TEM). The nanopowder is sonochemically dispersed in a Nafion solution which is then used to modify the surface of a GCE electrode. The electrochemical activity of L-tyrosine and epinephrine was investigated using both a Nafion-CeO₂ coated and a bare GCE. The modified electrode exhibits a significant electrochemical oxidation effect of L-tyrosine in a 0.2 M Britton-Robinson (B-R) buffer solution of pH 2. The electro-oxidation peak current increases linearly with the L-tyrosine concentration in the molar concentration range of 2 to 160 μM. By employing differential pulse voltammetry (DPV) for simultaneous measurements, we detected two reproducible peaks for L-tyrosine and epinephrine in the same solution with a peak separation of about 443 mV. The detection limit of the sensor (signal to noise ratio of 3) for L-tyrosine is ~90 nM and the sensitivity is 0.20 μA μM^?1, while for epinephrine these values are ~60 nM and 0.19 μA μM^?1. The sensor exhibited excellent selectivity, sensitivity, reproducibility and stability as well as a very good recovery time in real human blood serum samples.

Simultaneous electrochemical determination of L-tyrosine and epinephrine in blood plasma with Nafion-CeO₂/GCE modified electrode showing a 443 mV peak-to-peak potential difference between species oxidation peak currents.     

Electrooxidation of insulin at silicon carbide nanoparticles modified glassy carbon electrode

For the first time silicon carbide nanoparticles (SiC) was used for electrode modification and electrocatalytic oxidation of insulin. In comparison to bare glassy carbon (GC) electrode, the oxidation of insulin at GC electrode modified with SiC nanoparticles occurred at reduced overpotentials. The modified electrode was applied for insulin detection using cyclic voltammetry, differential pulse voltammetry (DPV) and flow injection analysis (FIA). Flow injection amperometric determination of insulin at this modified electrode yielded a calibration curve with the following characteristics; linear dynamic range up to 600 pM, sensitivity of 710 pA pM^?1 cm^?2 and detection limit of 3.3 pM. In addition interference effect of the electroactive existing species (uric acid, glucose, lactic acid, l-cysteine and cholesterol) was diminished and for ascorbic acid eliminated by covering the surface of modified electrode with nafion film. This electrode shows many advantages as an insulin sensor such as simple preparation method without using any specific electron transfer mediator or specific reagent, high sensitivity, excellent catalytic activity, short response time, long term stability and remarkable antifouling property toward insulin and its oxidation product. Sensitivity, detection limit and antifouling properties of this insulin sensor are better than all of the reports in the literature for insulin detection at physiological pH solutions.     

Non-enzymatic amperometric hydrogen peroxide sensor using a glassy carbon electrode modified with gold nanoparticles deposited on CVD-grown graphene

A glassy carbon electrode (GCE) was modified with gold nanoparticles (AuNPs) coated on monolayer graphene (AuNP/MG) by direct in situ sputtering of AuNPs on CVD-generated graphene. This process avoids complicated polymer transfer and polymer cleaning processes and affords AuNPs with a clean surface. The monolayer graphene is ductile and well dispersed. The clean surface of the AuNPs renders this sensor superior to GCEs modified with AuNPs on reduced graphene oxide in terms of the amperometric non-enzymatic determination of hydrogen peroxide. The detection limit is 10 nM (S/N = 3) at 0.55 V (vs. SCE), which is lower than that for similar methods, and the response time is as short as 2 s. Another attractive feature of the sensor is its feasibility for large-scale production via CVD and sputtering.

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Graphical abstract Gold nanoparticles deposited onto monolayered graphene generated by chemical vapor deposition (CVD) are used for electrochemical sensing of H₂O₂, with the detection limit of 10 nM (S/N = 3) and response time of less than 2 s.

     

Determination of zearalenone with a glassy carbon electrode modified with nanocomposite consisting of palladium nanoparticles and a conductive polymeric ionic liquid

A glassy carbon electrode (GCE) modified with polymeric nanocomposite consisting of palladium nanoparticles and a conductive polymeric ionic liquid was prepared. The modified GCE was applied to sensitive and fairly selective electrochemical determination of the mycotoxin zearalenone. Electrocatalytic oxidation is performed in a solution containing 20 % (V/V) acetonitrile and 80 % (V/V) of 1 M perchloric acid. Cyclic voltammetry and square wave voltammetry revealed a well-defined electrocatalytic peak current at overpotential of +0.69 V versus Ag/AgCl. Under optimized experimental conditions, there is a linear relationship between anodic peak current and zearalenone concentration in the range from 0.03 to 35 ng?mL￣¹, and the detection limit is 0.01 ng?mL￣¹. The method was successfully applied to the analysis of zearalenone in spiked food samples and gave recoveries between 95.6 and 104.0 %.

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Graphical abstract The nanocomposite (PdVC-PIL) was prepared by polymerization of ionic liquid monomer (PIL) in presence of Pd nanoparticles on Vulcan XC-72R carbon (PdVC). The solution containing nanocomposite was placed on the glassy carbon electrode (GCE). The voltammetry activity of modified electrode (PdVC-PIL/GCE) was compared to a bare GCE for zearalenone determination.

     

Determination of sulfonamides in milk samples by HPLC with amperometric detection using a glassy carbon electrode modified with multiwalled carbon nanotubes

A sensitive and accurate method for determining five sulfonamides based on HPLC with amperometric detection and using a glassy carbon electrode modified with multiwalled carbon nanotubes is proposed. Optimal conditions for the quantitative separation of selected sulfonamides were studied, and glassy carbon electrodes with and without modification with carbon nanotubes were systematically investigated as electrodic materials. Statistical analysis of the obtained results demonstrated that these modified electrodes achieved considerably better stability and sensitivity than the conventional unmodified ones. Detection limits were in the 1.2–6.0 ng/mL range. The usefulness of the method was demonstrated by the analysis of milk samples, taking into account the European legislation on residues in food products, following both a screening method to classify the samples and a confirmation method to provide more detailed information in the case of positive samples.     

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.