Screen-Printed Carbon Electrodes with Macroporous Copper Film for Enhanced Amperometric Sensing of Saccharides.

A porous layer of copper was formed on the surface of screen-printed carbon electrodes via the colloidal crystal templating technique. An aqueous suspension of monodisperse polystyrene spheres of 500 nm particle diameter was drop-casted on the carbon tracks printed on the substrate made of alumina ceramic. After evaporation, the electrode was carefully dipped in copper plating solution for a certain time to achieve a sufficient penetration of solution within the polystyrene spheres. The metal was then electrodeposited galvanostatically over the self-assembled colloidal crystal. Finally, the polystyrene template was dissolved in toluene to expose the porous structure of copper deposit. The morphology of porous structures was investigated using scanning electron microscopy. Electroanalytical properties of porous copper film electrodes were evaluated in amperometric detection of selected saccharides, namely glucose, fructose, sucrose, and galactose. Using hydrodynamic amperometry in stirred alkaline solution, a current response at +0.6 V vs. Ag/AgCl was recorded after addition of the selected saccharide. These saccharides could be quantified in two linear ranges (0.2-1.0 µmol L-1 and 4.0-100 µmol L-1) with detection limits of 0.1 µmol L-1 glucose, 0.03 µmol L-1 fructose, and 0.05 µmol L-1 sucrose or galactose. In addition, analytical performance of porous copper electrodes was ascertained and compared to that of copper film screen-printed carbon electrodes, prepared ex-situ by the galvanostatic deposition of metal in the plating solution. After calculating the current densities with respect to the geometric area of working electrodes, the porous electrodes exhibited much higher sensitivity to changes in concentration of analytes, presumably due to the larger surface of the porous copper deposit. In the future, they could be incorporated in detectors of flow injection systems due to their long-term mechanical stability.

Analytical Performance of Clay Paste Electrode and Graphene Paste Electrode-Comparative Study.

The analytical performance of the clay paste electrode and graphene paste electrode was compared using square wave voltammetry (SWV) and cyclic voltammetry (CV). The comparison was made on the basis of a paracetamol (PA) determination on both working electrodes. The influence of pH and SWV parameters was investigated. The linear concentration ranges were found to be 6.0 × 10-7-3.0 × 10-5 and 2.0 × 10-6-8.0 × 10-5 mol L-1 for clay paste electrode (ClPE) and graphene paste electrode (GrPE), respectively. The detection and quantification limits were calculated as 1.4 × 10-7 and 4.7 ×10-7 mol L-1 for ClPE and 3.7 × 10-7 and 1.2 × 10-6 mol L-1 for GrPE, respectively. Developed methods were successfully applied to pharmaceutical formulations analyses. Scanning electron microscopy and energy-dispersive X-ray spectroscopy were used to characterize ClPE and GrPE surfaces. Clay composition was examined with wavelength dispersive X-ray (WDXRF).

Highly Sensitive Determination of Tenofovir in Pharmaceutical Formulations and Patients Urine-Comparative Electroanalytical Studies Using Different Sensing Methods.

This paper discusses the electrochemical behavior of antiviral drug Tenofovir (TFV) and its possible applicability towards electroanalytical determination with diverse detection strategies using square-wave voltammetry. Namely, oxidation processes were investigated using glassy carbon electrode with graphene oxide surface modification (GO/GCE), while the reduction processes, related to the studied analyte, were analyzed at a renewable silver amalgam electrode (Hg(Ag)FE). Scanning electron microscopy imaging confirmed the successful deposition of GO at the electrode surface. Catalytic properties of graphene oxide were exposed while being compared with those of bare GCE. The resultant modification of GCE with GO enhanced the electroactive surface area by 50% in comparison to the bare one. At both electrodes, i.e., GO/GCE and Hg(Ag)FE, the TFV response was used to examine and optimize the influence of square-wave excitation parameters, i.e., square wave frequency, step potential and amplitude, and supporting electrolyte composition and its pH. Broad selectivity studies were performed with miscellaneous interfering agents influence, including ascorbic acid, selected saccharides and aminoacids, metal ions, non-opioid analgesic metamizole, non-steroidal anti-inflammatory drug omeprazole, and several drugs used along with TFV treatment. The linear concentration range for TFV determination at GO/GCE and Hg(Ag)FE was found to be 0.3-30.0 µmol L-1 and 0.5-7.0 µmol L-1, respectively. The lowest LOD was calculated for GO/GCE and was equal to 48.6 nmol L-1. The developed procedure was used to detect TFV in pharmaceutical formulations and patient urine samples and has referenced utilization in HPLC studies.

Comparative Electroanalytical Studies of Graphite Flake and Multilayer Graphene Paste Electrodes.

In this paper, the fabrication, surface characterisation and electrochemical properties of graphite flake (GFPE) and multilayer graphene (MLGPE) paste electrodes are described. The Raman investigations and scanning electron microscopy were used to analyze and compare structure of both carbon materials. The electroanalytical performance of both electrodes was examined and compared on the basis of the square-wave and cyclic voltammetric behavior of acetaminophen and model redox systems. Results of those studies revealed that GFPE has a larger electroactive surface area and better conductive properties, whilst MLGPE demonstrate better analytical characteristic in case of acetaminophen (AC) determination. AC determination was developed using square wave voltammetry (SWV) and square wave stripping voltammetry (SWSV). For both working electrodes, the process of accumulation enabled us to obtain an extended linear range and to lower the detection limit. In pharmaceutical formulations, AC was determined with good recovery.

Electrochemical study of the fungicide acibenzolar-s-methyl and its voltammetric determination in environmental samples.

The electrochemical behavior of new generation fungicide acibenzolar-s-methyl (S-methyl 1,2,3-benzothiadiazole-7-carbothioate, ASM) on the hanging mercury drop electrode (HMDE) was investigated using square wave adsorptive stripping voltammetry. This method of determination is based on the irreversible reduction of ASM at the HMDE. The well-defined ASM peak was observed at -0.4 V (vs. Ag/AgCl) in BR buffer at pH 2.2. The reduction peak current was proportional to concentration of ASM from 1.0 × 10(-8) to 6.0 × 10(-8) mol L(-1) with detection and quantification limit 3.0 × 10(-9) and 1.0 × 10(-8) mol L(-1), respectively. The applicability of the developed method for analysis of spiked samples of tap water, river water, and soil is illustrated. The effect of adsorption on the mercury electrode was studied in detail using the AC impedance method. Possible interferences with other common pesticides and heavy metal ions were examined. Clarification of the electrode mechanism was made using cyclic voltammetry (CV) technique.

Electrochemical and theoretical studies of the interaction between anticancer drug ponatinib and dsDNA.

In this study, electrochemical and theoretical studies were performed to explain the interaction mechanism between ponatinib (PNT), a third generation tyrosine kinase inhibitor, and dsDNA. The electrochemical part was conducted in phosphate-buffered saline (PBS) at physiological pH of 7.4 and in acetate buffer with a pH of 4.7, using square wave voltammetry. A boron-doped diamond electrode was used in a bulk-incubated solution. The theoretical part was investigated using computational methods, such as the semiempirical method PM7 and density functional theory (DFT). Significant differences in the electrochemical behavior of PNT in the presence of DNA confirmed the occurrence of interactions. The results obtained in the acetate buffer strongly suggested the preferential interaction of PNT with guanine residues. However, at physiological pH, it can be concluded that PNT interacts with dGua and dAdo in the dsDNA molecule. These results are consistent with outcomes from the theoretical studies, where quantum-chemical calculations showed that both electrochemically detectable nucleobases form hydrogen bonds with the drug. These bonds appeared to be stronger with guanine than with adenine. According to the computational studies, the dsDNA major groove is the energetically preferred site for the complexation of PNT.

Reviewing neonicotinoid detection with electroanalytical methods.

Neonicotinoids, as the fastest-growing class of insecticides, currently account for over 25% of the global pesticide market. Their effectiveness in controlling a wide range of pests that pose a threat to croplands, home yards/gardens, and golf course greens cannot be denied. However, the extensive use of neonicotinoids has resulted in significant declines in nontarget organisms such as pollinators, insects, and birds. Furthermore, the potential chronic, sublethal effects of these compounds on human health remain largely unknown. To address these pressing issues, it is crucial to explore and understand the capabilities of electrochemical sensors in detecting neonicotinoid residues. Surprisingly, despite the increasing importance of this topic, no comprehensive review article currently exists in the literature. Therefore, our proposed review aims to bridge this gap by providing a thorough analysis of the use of electrochemical methods for neonicotinoid determination. In this review article, we will delve into various aspects of electrochemical analysis, including the influence of electrode materials, employed techniques, and the different types of electrode mechanisms utilized. By synthesizing and analysing the existing research in this field, our review will offer valuable insights and guidance to researchers, scientists, and policymakers alike.

The Influence of Graphene Oxide Composition on Properties of Surface-Modified Metal Electrodes.

The present paper describes the effect of the concentration of two graphene oxides (with different oxygen content) in the modifier layer on the electrochemical and structural properties of noble metal disk electrodes used as working electrodes in voltammetry. The chemistry of graphene oxides was tested using EDS, FTIR, UV-Vis spectroscopy, and combustion analysis. The structural properties of the obtained modifier layers were examined by means of scanning electron and atomic force microscopy. Cyclic voltammetry was employed for comparative electrochemical studies.

Interactions of lamotrigine with single- and double-stranded DNA under physiological conditions.

This study presents evaluation of the possible mechanisms of interaction between the antiepileptic drug lamotrigine (LMT) and single- and double-stranded DNA (ssDNA and dsDNA, respectively). These interactions were studied in phosphate-buffered saline (PBS) at physiological pH 7.4 by cyclic voltammetry (CV) and square wave voltammetry (SWV) using a glassy carbon electrode (GCE) in a bulk incubated solution. The addition of both types of DNA to LMT solution decreased peak currents and led to a negative shift in peak potentials, thus indicating the dominance of electrostatic interactions. UV-Vis absorption spectroscopy was also used to assess the interaction between ds/ssDNA and LMT. The data obtained from spectroscopic analysis confirmed that electrostatic interaction is the predominant interaction between LMT and both types of DNA. The calculated binding constants for LMT-dsDNA and LMT-ssDNA complexes as determined by SWV were 6.46 × 105 and 1.81 × 106, respectively, while the values obtained from UV-Vis spectroscopy were 6.93 × 105 and 1.19 × 106, respectively. The obtained results indicated a higher affinity of LMT for ssDNA than for dsDNA.

Rapid electroanalytical procedure for sesamol determination in real samples.

In this study, the development of an electroanalytical assay based on square wave voltammetry technique for determining sesamol (Ses) in sesame oil samples is described. The influence of various factors such as pH of the supporting electrolyte, its composition, and SW (square wave) parameters was studied. Linearity of the peak current depended on the concentration of Ses in the range from 3.0 to 140.0 µmol L-1 with a limit of detection of 0.71 µmol L-1. Furthermore, the cyclic voltammetric behavior of Ses and the effects of scan rate and pH on the peak current and peak potential of Ses were determined. Moreover, the electrode process was found to be diffusion-controlled. The proposed methodology was successfully applied for determining Ses in commercial sesame oil samples. The obtained results were in good agreement with the results from the HPLC-UV reference method.

Recent Applications of Silver Amalgam Electrodes for Analysis of Pharmaceuticals and Vitamins.

The features and applications of silver amalgam electrodes in electroanalysis of pharmaceuticals and vitamins are summarized in this review. The state-of-the-art in the preparation and construction of solid silver amalgam electrodes for prolonged and userfriendly use is presented. Although not as widely spread as other electrode materials, silver amalgam possesses a unique and viable combination of favorable electrochemical properties, which are close to ideal mercury electrodes, non-toxic character, high durability and mechanical stability, if properly prepared. Its capability of conducting the redox processes at highly negative potentials is essential for the analysis of large number of bioactive organic compounds. The review features also overview information for each application in drug or vitamin analysis divided to the sections according to the construction variants of silver amalgam electrodes.

Electrochemical and spectroscopic studies of the interaction of antiviral drug Tenofovir with single and double stranded DNA.

In the present study, the electrochemical behavior of the antiviral drug tenofovir (tnf) on a boron-doped diamond electrode (BDDE) has been studied using square-wave voltammetry (SWV). The experimental conditions such as the supporting electrolyte composition and the SWV parameters were optimized. Under the optimized conditions, a simple and sensitive SWV procedure for tnf determination was developed in the concentration range of 5.0 × 10-6 to 1.0 × 10-4 mol L-1. The calculated limit of detection and limit of quantification were equal to 5.6 × 10-7 and 1.9 × 10-6 mol L-1, respectively. The biological significance of the developed method was demonstrated by a quantitative analysis of the pharmaceutical formulations Viread and Tenofovir disoproxil Teva. Moreover, both voltammetric and spectroscopic techniques were used to study the interaction between tnf and DNA. Changes in the electrochemical and spectroscopic behavior of tnf in the presence of DNA were used to calculate the binding constants of the formed complexes. The estimated values of Gibbs free energy revealed that the formation of the drug-DNA complexes was a spontaneous and favorable process. Moreover, for free and bound tenofovir, kinetic parameters such as heterogeneous rate constant, electron transfer coefficient, and diffusion coefficient were determined.

Graphene oxide activation with a constant magnetic field.

The effect of constant magnetic field strength on activation of sensors modified with graphene oxide monolayers was investigated. The use of constant magnetic field resulted in improved electroanalytical properties of the sensors. It was proven that level of GO activation is clearly related to constant magnetic field strength. Moreover, it was demonstrated that observed phenomenon is stable in time.

Improved electroanalytical characteristics for flumetralin determination in the presence of surface active compound.

ABSTRACT: The use of square wave voltammetry (SWV) and square wave adsorptive stripping voltammetry (SWAdSV) in conjunction with a cyclic renewable silver amalgam film electrode for the determination of flumetralin is presented. Poor separation of two overlapped reduction peaks is significantly improved when hexadecyltrimethylammonium bromide is used as a component of the supporting electrolyte solution (together with BR buffer pH 9.5). The SW technique parameters were investigated and found optimal as follows: frequency 50 Hz, amplitude 40 mV, and step potential 5 mV. Accumulation time and potential were studied to select the optimal conditions in adsorptive voltammetry. The analytical curve was linear for the flumetralin concentration range from 1.0 × 10-6 to 1.0 × 10-5 mol dm-3 and from 5.0 × 10-9 to 1.0 × 10-7 mol dm-3 for SWV and SWAdSV, respectively. Detection limit of 6.5 × 10-10 mol dm-3 was calculated for accumulation time 60 s at -0.2 V. The repeatability of the method was determined at a flumetralin concentration level equal to 5.0 × 10-9 mol dm-3 and expressed as %RSD = 5.0% (n = 6). The proposed method was applied and validated successfully by studying the recovery of herbicide content in spiked environmental samples.

Rapid and Sensitive Voltammetric Determination of Aclonifen in Water Samples.

This paper presents the use of square wave voltammetry (SWV) and square wave adsorptive stripping voltammetry (SWAdSV) in conjunction with a cyclic renewable silver amalgam film electrode (Hg(Ag)FE) for the determination of aclonifen in spiked water samples. A reduction peak at -0.65 V versus Ag/AgCl was obtained in the selected buffer (borax buffer with pH 9.2), exhibiting the characteristics of an irreversible reaction. The effect of square wave (SW) frequency, SW amplitude and step potential, as well as accumulation parameters (time and potential) were studied to select the optimal experimental conditions. The calibration curve was linear in the aclonifen concentration range from 1.0×10(-7) to 1.0×10(-6) mol L(-1) and from 1.0×10(-8) to1.0×10(-7) mol L(-1) for SWV and SWAdSV, respectively. The detection and quantification limits were found to be 3.1×10(-8) mol L(-1); 1.0×10(-7) mol L(-1) and 2.9×10(-9) mol L(-1); 9.6×10(-9) mol L-1 for SWV and SWAdSV, respectively. The proposed method was applied successfully in the determination of aclonifen in spiked water samples. The developed procedure can be adequate at least for screening purposes, where positive results should be confirmed by more selective method.