Search Results (130)

Herein, we propose an ultrasensitive electrochemical immunosensor based on glucose oxidase labeling and enzyme-catalyzed Au staining. In brief, the primary antibody (Ab₁), bovine serum albumin, an antigen and then a bionanocomposite that contains a second antibody (Ab₂), poly(3-anilineboronic acid) (PABA), Au nanoparticles (AuNPs) and glucose oxidase (GOx) are modified on a glassy carbon electrode coated with multiwalled carbon nanotubes, yielding a corresponding sandwich-type immunoelectrode. In the presence of glucose, a chemical reduction of NaAuCl₄ by enzymatically generated H₂O₂ can precipitate a lot of gold on the Ab₂-PABA-AuNPs-GOx immobilized immunoelectrode. In situ anodic stripping voltammetry (ASV) detection of gold in 8 μL 1.0 M aqueous HBr-Br₂ is conducted for the antigen assay, and the ASV detection process takes approximately 6 min. This method is employed for the assay of human immunoglobulin G (IgG) and human carbohydrate antigen 125 (CA125), which demonstrates exceptional sensitivity, high selectivity and fewer required reagents/samples. The achieved limits of detection (S/N = 3) by the method are 0.25 fg mL⁻¹ for IgG (approximately equivalent to containing 1 IgG molecule in the 1 microlitre of the analytical solution) and 0.1 nU mL⁻¹ for CA125, which outperforms many previously reported results. Full article

In this work, we designed a novel and simple electrochemical approach for the determination of daidzein antioxidant (Dz) in peanut oil samples. The Dz determination was based on anodic stripping linear voltammetry using screen-printed graphene electrodes (SPGEs) activated in acidic media, where a strong adsorption of Dz on activated graphene was obtained. In this regard, electroanalytical parameters such as the scan rate, supporting electrolyte, pH, and accumulation step were optimized to ensure the best conditions for the selective and sensitive Dz quantification. The electrochemical method developed for the determination of Dz exhibits a linear behavior of the anodic peak current in the concentration range from 0.05 to 1 μM, with a limit of detection of 0.012 μM. The electrochemical sensor demonstrated to the capacity to quantify Dz in peanut oil samples at low concentrations without the necessity of an extensive sample pretreatment. Therefore, the electrochemical method proposed can be used as a new portable analytical tool for the in situ quality control of peanut oil samples. Full article

Lead (Pb) and cadmium (Cd) ions have serious negative impacts on human health and the ecological environment due to toxicity, persistence and nonbiodegradability. Among various trace Pb and Cd ions detection technologies, electrochemical analysis is considered as one of the most promising methods. The deposition of Bi nanoparticles on delaminated Ti₃C₂T_x (DL-Ti₃C₂T_x) develops a sensor with good conductivity and performance. Square wave anodic stripping voltammetry (SWASV) technology was applied to simultaneously deposit Bi on DL-Ti₃C₂T_x/GCE and achieve the rapid detection of Pb and Cd ions. The Bi nanoparticles effectively improved the sensitivity of Bi/DL-Ti₃C₂T_x/GCE sensors to detect Pb and Cd ions. The preparation conditions of the Bi/DL-Ti₃C₂T_x/GCE were optimized, including DL-Ti₃C₂T_x droplet amount, solution pH, Bi³⁺ concentration, deposition time and deposition potential, to improve the detection ability. The Bi/DL-Ti₃C₂T_x/GCE sensor has detection limits of 1.73 and 1.06 μg/L for Pb and Cd ions, respectively (S/N > 3). This electrochemical sensor is easy, sensitive and selective to apply in actual water samples for trace Pb and Cd ions detection. Full article

Excessive levels of heavy metal pollutants in the environment pose significant threats to human health and ecosystem stability. Consequently, the accurate and rapid detection of heavy metal ions is critically important. A AgNPs@CeO₂/Nafion composite was prepared by dispersing nano-ceria (CeO₂) in a Nafion solution and incorporating silver nanoparticles (AgNPs). The morphology, microstructure, and electrochemical properties of the modified electrode materials were systematically characterized using scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), and cyclic voltammetry (CV). By leveraging the oxygen vacancies and high electron transfer efficiency of CeO₂, the strong adsorption capacity of Nafion, and the superior conductivity of AgNPs, an AgNPs@CeO₂/Nafion/GCE electrochemical sensor was developed. Under optimized conditions, trace Pb²⁺ in water was detected using square wave anodic stripping voltammetry (SWASV). The sensor demonstrated a linear response for Pb²⁺ within the concentration range of 1–100 μg·L⁻¹, with a detection limit of 0.17 μg·L⁻¹ (S/N = 3). When applied to real water samples, the method achieved recovery rates between 93.7% and 110.3%, validating its reliability and practical applicability. Full article

We report the first synthesis of zwitterionic thiacalixarenes featuring imidazolium and sulfonate groups on the upper rim and alkyl (butyl or octyl) fragments on the lower rim of the platform. Despite their amphiphilic structure, these macrocycles exhibit limited water solubility. However, dynamic light scattering detected the formation of associates for derivatives with octyl moieties at a concentration of 0.1 mM. To develop stable materials for aqueous environments and to investigate the functionality of zwitterionic sulfonate-imidazolium groups along with the thiacalixarene platform, mixed organo-organic systems based on polydiacetylene polymer were created. Characterization of the modified polydiacetylene systems through various analytical methods revealed a significant colorimetric response to lead ions in aqueous media, surpassing that of the unmodified polydiacetylene polymer. Additionally, the modified polymers demonstrated efficacy in purifying aqueous media from lead ions, as evidenced by anodic stripping voltammetry (ASV) and microwave plasma atomic emission spectroscopy (MP AES). Full article

This paper shows the fabrication of a new environmentally friendly sensor, an activated glassy carbon electrode with an in situ deposited bismuth film (aGCE/BiF), to determine Cd(II) and Pb(II) at the nanotrace level. The electrochemical activation of the GCE surface was achieved in a solution of 0.1 M phosphate-buffered saline (PBS) of pH = 7 by performing five cyclic voltammetric scans in the range of −1.5–2.5 V at ν of 100 mV/s. The newly developed electrode provides several advantages, such as an increased electron active surface (compared to the glassy carbon electrode) and improved electron transfer kinetics. As a result, the new voltammetric procedure (square-wave anodic stripping voltammetry, SWASV) was established and optimized. With the SWASV method, the following calibration curves and low detection limits (LODs) were obtained for Cd(II) and Pb(II), respectively: 5–100 nM, 0.62 nM, 2–200 nM, and 0.18 nM. The newly prepared method was used to determine the amounts of Pb(II) and Cd(II) in the certified reference material, and the results agreed with the certified values. Moreover, the procedure was successfully applied to determine the Cd(II) and Pb(II) in river samples. The official and standard addition methods validated the measurement results. Full article

The bioavailability of dissolved copper (Cu) in seawater is influenced by the presence of natural organic matter. Changes in physicochemical conditions, such as pH, temperature, and salinity, can significantly affect the solubility and speciation of copper, thereby impacting the complexation of Cu(II)-binding organic ligands. The concentration of dissolved Cu in the coastal water of Mersing, Malaysia, was detected by anodic stripping voltammetry (ASV). The natural organic copper(II)-binding ligands (CuL) and their conditional stability constants (log K′) were determined by using the competitive ligand exchange–adsorptive cathodic stripping voltammetry method (CLE–AdCSV) in our samples. The in situ parameters, such as pH, temperature, salinity, and dissolved oxygen (DO), were found to be significantly different between sampling periods and indicated the different physical chemical conditions between the sampling periods. However, we found a consistent concentration of dissolved Cu throughout the water column between sampling periods. This suggests that the presence of a strong class of natural organic ligands (L₁) in Mersing’s coastal water maintains the dissolved Cu(II) ions in the water column and prevents the scavenging and precipitation processes under the seasonal variations. Full article

Heavy metal contamination of water has become a global environmental problem in recent years, which is caused by the rapid development of economies and industries. Gallium is of enduring interest because of its wide range of applications in technology and industry. In its pure form or as a component of alloys, gallium is used in devices such as high-current switches, pressure gauges, and thermometers. Gallium compounds also play an important role in electronics and optoelectronics, particularly in devices that operate in the infrared range. Gallium isotopes are also used in medical diagnostics. The increasing demand for gallium emphasizes the need for accurate methods for its determination in different matrices. One method used for this purpose is stripping voltammetry. The working electrodes, complexing agents, and the influence of interferences on the accuracy of the measurement are discussed in detail, highlighting their crucial role in obtaining the analytical signal of gallium in procedures based on stripping voltammetry. Voltammetric procedures for the simultaneous determination of gallium and other metal ions are also described. The application of the developed procedures to the analysis of real samples is emphasized as crucial for environmental monitoring and the accurate determination of trace concentrations of gallium. A summary of the results is presented in the form of a table which provides detailed information on the stripping voltammetry methods, including the types of working electrodes, characteristics of the substrate electrolytes used, complexing agents, linear ranges, and detection limits. The table also includes accumulation times, interferences investigated, and practical applications of the methods discussed, making it a valuable resource for researchers and analysts involved in environmental analysis. The review highlights the importance of this technique as an accurate and sensitive tool for the analysis of gallium in environmental samples. Full article

Heavy metal pollution has become an increasingly serious environmental issue, making the detection of heavy metals essential for safeguarding public health and the environment. This review aims to highlight the commonly used methods for detecting heavy metals (such as atomic absorption spectroscopy (AAS), atomic emission spectroscopy (AES), inductively coupled plasma–mass spectrometry (ICP-MS), square-wave anodic stripping voltammetry (SWASV), etc.), with a particular focus on electrochemical detection and electrode modification materials. Metal nanomaterials (such as titanium dioxide (TiO₂), copper oxide (CuO), ZIF-8, MXene, etc.) are emphasized as promising candidates for enhancing the performance of sensors due to their high surface area and excellent catalytic properties. However, challenges such as interference from non-target heavy metal ions and the formation of organometallic complexes with organic compounds can complicate the detection process. To address these issues, two potential solutions have been proposed: the development of advanced algorithms (such as machine learning (ML), back-propagation neural network (BPNN), support vector machines (SVM), random forests (RF), etc.) for signal processing and the use of pretreatment methods (such as Fenton oxidation (FO), ozone oxidation, and photochemical oxidation) to suppress such interferences. This paper aims to review commonly used methods for detecting heavy metals, with a particular emphasis on electrochemical techniques. It will also highlight the challenges faced in these methods, such as interference and sensitivity limitations, and propose innovative solutions, including the use of metal nanomaterials for improved sensor performance and the integration of advanced algorithms and pretreatment techniques to address interference and enhance detection accuracy. Full article

The monitoring of heavy metals in aquatic ecosystems is of critical importance due to the toxic effects that these elements can have on wildlife and the potential risks that they pose to human health. Rivers situated in close proximity to agricultural regions are particularly susceptible to contamination from a combination of natural and anthropogenic sources. The study of bioaccumulation is of great importance for the early detection of environmental stressors. The combination of electrochemical techniques, such as square-wave anodic stripping voltammetry (SWASV), with automated flow-batch systems represents an efficient and cost-effective approach for the detection of trace metals in environmental samples. This study examines the bioaccumulation of cadmium and lead in Cyprinus carpio, a bioindicator of contamination in the Colorado River, Argentina. The fish were exposed to sublethal metal concentrations for 24, 48, and 96 h. Metal quantification was conducted using a novel automatic flow-batch system with SWASV and a bismuth film electrode. To the best of our knowledge, this constitutes the first application of this methodology on aquatic bioindicators for the assessment of metal accumulation in a natural environment. The technique demonstrated enhanced sensitivity and selectivity for the detection of trace metals. The bioaccumulation results demonstrated an increase in cadmium and lead concentrations in fish liver tissue after 96 h, reaching 10.5 µg g⁻¹ and 11.9 µg g⁻¹, respectively. Validation with inductively coupled plasma–atomic emission spectrometry (ICP-AES) demonstrated a satisfactory correlation, confirming the reliability of the method. This novel electrochemical approach offers enhanced accuracy and efficiency, making it a promising tool for environmental monitoring. The results indicate that Colorado River water is within safe levels for aquatic life regarding these metals. However, continuous monitoring is recommended to detect changes in contamination levels and protect ecosystem health, especially during water crises and under climate change. Full article

Cadmium is one of the most dangerous pollutants found in the environment, where it exists mainly due to human activities. High cadmium concentrations can cause serious problems, which is why the detection and determination of Cd is one of the most important tasks. Electroanalytical methods provide rapid and accurate results in the detection of cadmium in various solutions. In this study, the possibility of using a bismuth film electrode deposited on a brass surface and electroanalytical techniques for the detection of cadmium is investigated. The bismuth film was deposited on the surface of the brass electrode using a chronoamperometric technique. Cyclic voltammetry and electrochemical impedance spectroscopy were used to characterize the synthesized bismuth film electrode. The current peaks obtained by anodic square-wave stripping voltammetry under optimized conditions showed a linear relationship in the investigated concentration range of cadmium. The study of the interference of different cations (Cr³⁺, Mn²⁺, Zn²⁺, Ca²⁺, K⁺, Mg²⁺ and Na⁺) showed that the tested cations have no influence on the determination of Cd²⁺ ions in the investigated solution. This finding provides a good opportunity for the use of the synthesized electrode in real samples. Full article

The aim of this study was to systematically analyze the influence of potential and the Co(II)–Ru(III) molar ratio on the electrochemical behavior of the Co–Ru system during codeposition from acidic chloride electrolytes. The equilibrium speciation of the baths was investigated spectrophotometrically and compared with theoretical calculations based on the stability constants of Co(II) and Ru(III) complexes. The codeposition of the metals was characterized using electroanalytical methods, including cyclic voltammetry, chronoamperometry, and anodic stripping linear voltammetry. The alloys obtained at different potentials were analyzed for their elemental composition (EDS, mapping), phase composition (XRD), and surface morphology (SEM). The morphology and composition of the alloys were mainly dependent on the deposition potential, which controlled the cobalt incorporation. Ruthenium–rich alloys were produced at potentials of −0.6 V and −0.7 V (vs. SCE). In these conditions, cobalt anomalously codeposited due to the formation of the CoOH⁺ intermediate, triggered by the intense hydrogen evolution on the ruthenium sublayer. Bulk cobalt electrodeposition began at a potential of around −0.8 V, resulting in the formation of cobalt-rich alloys. The early stages of the electrodeposition were investigated using different nucleation models. A transition from 2D progressive nucleation to 3D instantaneous nucleation at around −0.8 V was identified as being caused by cobalt incorporation. This was well correlated with electroanalytical data, partial polarization curves of alloy deposition, elemental mapping analysis, and the structure of the deposits. Full article

A new molecularly imprinted polymer (MIP)-based disposable electrochemical sensor for dipyridamole (DIP) determination was obtained. The sensor was rapidly prepared by potentiodynamic electrochemical polymerization on a pencil graphite electrode (PGE) using curcumin (CUR) as a functional monomer and DIP as a template molecule. After the optimization of the conditions (pH, monomer–template ratio, scan rate, number of cyclic voltammetric cycles applied in the electro-polymerization process and extraction time of the template molecule) for MIP formation, DIP voltammetric behavior at the modified electrode (MIP_PGE) was investigated. DIP oxidation took place in a pH-dependent, irreversible mixed diffusion-adsorption controlled process. Differential pulse voltammetry (DPV) and adsorptive stripping differential pulse voltammetry (AdSDPV) were used to quantify DIP from pharmaceutical and tap water samples. Under optimized conditions (Britton–Robinson buffer at pH = 3.29), the obtained linear ranges were 5.00 × 10⁻⁸–1.00 × 10⁻⁵ mol/L and 5.00 × 10⁻⁹–1.00 × 10⁻⁷ mol/L DIP for DPV and AdSDPV, respectively. The limits of detection of the methods were 1.47 × 10⁻⁸ mol/L for DPV and 3.96 × 10⁻⁹ mol/L DIP for AdSDPV. Full article

In this study, a new and simple glassy carbon electrode modified with carbon nanohorns (SWCNH/GCE) was used for the determination of Cr(VI) in aqueous matrices via adsorptive cathodic stripping voltammetry (AdCSV). The modified electrode was characterized via field emission scanning electron microscopy and cyclic voltammetry, which revealed a homogeneous distribution of spherical agglomerates of SWCNH on the electrode surface. The modification increased the electrochemically active area from 0.10 cm² ± 0.01 (GCE) to 0.16 cm² ± 0.01 (SWCNH/GCE). The optimized analytical conditions were as follows: a supporting electrolyte (0.15 mol L⁻¹ HCl), an accumulation potential of 0.8 V versus Ag/AgCl, and an accumulation time of 240 s. Validation of the analytical methodology was performed, obtaining a linear range between 20 and 100 µg L⁻¹, a limit of detection of 3.5 µg L⁻¹, and a limit of quantification of 11.6 µg L⁻¹ with good accuracy and precision. The method was applied to the analysis of spiked tap water samples, and the results were compared using a flame atomic absorption spectrophotometer (FAAS) with no significant statistical differences. Full article

In this study, nanoporous gold (NPG) was deposited on a screen-printed carbon electrode (SPCE) by the dynamic hydrogen bubble template (DHBT) method to prepare an electrochemical sensor for the simultaneous determination of Pb²⁺ and Cu²⁺ by square wave anodic stripping voltammetry (SWASV). The electrodeposition potential and electrodeposition time for NPG/SPCE preparation were investigated thoroughly. Scanning electron microscopy (SEM) and energy-dispersive X-ray diffraction (EDX) analysis confirmed successful fabrication of the NPG-modified electrode. Electrochemical characterization exhibits its superior electron transfer ability compared with bare and nanogold-modified electrodes. After a comprehensive optimization, Pb²⁺ and Cu²⁺ were simultaneously determined with linear range of 1–100 μg/L for Pb²⁺ and 10–100 μg/L for Cu²⁺, respectively. The limits of detection were determined to be 0.4 μg/L and 5.4 μg/L for Pb²⁺ and Cu²⁺, respectively. This method offers a broad linear detection range, a low detection limit, and good reliability for heavy metal determination in drinking water. These results suggest that NPG/SPCE holds great promise in environmental and food applications. Full article