There are no documented electroanalytical methods for quantifying the anti-inflammatory drug bumadizone (BUM) in pharmaceutical or biological matrices. So, a new voltammetric method was developed to determine BUM at nano concentrations in pharmaceutical forms, in the presence of its alkaline degradant, and in biological fluids. Five electrodes were tested, including three nano-reduced graphene oxide (nRGO) electrodes (5%, 15%, and 20%), a carbon paste electrode (CPE), and a 10% nRGO-modified CPE. The 10% nRGO-modified electrode showed the best performance, offering high selectivity and low detection limits, with good linearity in the concentration range of 0.9 × 102 to 15 × 102 ng mL-1. Differential pulse voltammetry successfully applied this electrode for BUM determination in various samples, achieving excellent recovery without preliminary separation. The method was validated according to ICH guidelines and compared favorably to the reference method. Its environmental impact was assessed using AGREE and Eco-scale metrics in addition to the RGB algorithm, showing superior greenness and whiteness profiles due to safer solvents and lower energy consumption, along with high practical effectiveness using the BAGI metric.

Aquatic selenium (Se) oxyanions have profound ecosystem and human health impacts, necessitating their conversion and immobilization into elemental Se(0) to mitigate the aquatic Se pollution. While thermodynamically favorable, this transformation encounters kinetic limitations, especially for selenate (SeO42-) or Se(VI). To lower the activation barrier, we investigated the electrocatalytic Se(VI) transformation using five affordable catalysts on graphite cathodes, including TiO2, underpotentially deposited Cu (UPD Cu), underpotentially deposited Cd (UPD Cd), Co, and CuFe. Among these five catalysts, we identified characteristic Se(VI) reduction peaks for TiO2 through cyclic voltammetry. Other catalysts removed less than 5% of 1-mM Se(VI) in 24-h chronoamperometry tests while leaching ppm-level metal cations in the treated water. In contrast, TiO2 as the electrocatalyst could remove more than 80% of 1-mM Se(VI) with negligible catalyst dissolution. Mechanistic investigations revealed a six-electron Se(VI)/Se(0) reduction pathway at -0.30 V (vs. Ag/AgCl), resulting in red Se(0) deposits on the TiO2-coated graphite cathode. Further potential decrease to more negative than -0.45 V led to Se(-II) formation, triggering cathodic Se(0) dissolution and surface regeneration. Electrochemical impedance spectroscopy indicated that Se(VI) reduction was optimal with a moderate TiO2 loading of 0.55 mg cm-2 and acidic environments (pH=1.0∼2.5), achieving an optimized removal of 88.7 ± 2.3% under -0.70 V and an energy input of 3.6 kWh kg-1 Se. These findings lay the foundation for efficient selenate removal from impaired waters. Future efforts should evaluate catalyst performance over time and refine electrode and reactor designs to improve efficiency.

An electrochemical sensor was developed for the detection of hydrogen peroxide (H2O2), utilizing the synergistic effects of graphene (Gr) and MOF-on-MOF nanozymes (FeCu-NZs). Initially, Fe-MOF with peroxide-like activity is synthesized using a solvothermal method. Subsequently, the organic ligand on its surface binds Cu2+, enhancing the enzyme-like activity further. The resulting FeCu-NZs exhibit a distinctive electrochemical signal in response to H2O2. Moreover, integrating FeCu-NZs with Gr significantly amplifies the electrochemical signal and effectively reduces the sensor\'s detection limit. The developed sensor exhibited linear ranges of 0.1-3800 μM, with a limit of detection (LOD) of 0.06 μM. Additionally, FeCu-NZs catalyze H2O2 to generate abundant •OH radicals, and colorimetric detection of H2O2 is facilitated using the color rendering principle of 3,3\',5,5\'-tetramethylbenzidine (TMB). Notably, this detection method was applied to determine  H2O2 concentrations in real samples, achieving a recovery exceeding 95.7%. In summary, this research provides a practical platform for the construction of traditional nanozymes and the integration of electrochemical systems, which have broad applications in food analysis, environmental monitoring, and medical diagnosis.

Four polyoxomolybdated compounds based on Tetp (Tetp = 4-[4-(2-Thiophen-2-yl-ethyl)-4H-[1, 2, 4]triazole-3-yl]-pyridine), namely [Zn(Tetp)2(H2O)2][(β-Mo8O26)0.5] (Zn-Mo8), [Co(Tetp)2(H2O)2][(β-Mo8O26)0.5] (Co-Mo8), [Cu4(Tetp)6(H2O)2]{H3[K(H2O)3](θ-Mo8O26)(Mo12O40)}·8H2O (Cu-Mo20) and [Cu3(Tetp)3][PMo12O40]·H2O (Cu-PMo12) are synthesized by hydrothermal methods and are used as electrode materials for supercapacitors(SCs) and electrochemical sensors. Inserting polyoxometalates (POMs) with redox active sites into transition metal compounds (TMCs) can improve the internal ion/electron transfer rate, thus effectively enhancing the electrochemical performance. Compared with the parent POMs, four compounds exhibit excellent electrochemical properties. In particular, Cu-PMo12 shows an excellent specific capacitance (812.3 F g-1 at 1 A g-1) and stability (94.42%), as well as a wide detection range (0.05 to 1250 µM) and a low detection limit (0.057 µM) for NO2- sensing.

Chlorambucil (CML) cures chronic lymphatic leukemia (white blood cell cancer). A high dose of CML can cause several side effects like bone marrow suppression, anemia, peripheral neuropathy, and infertility in the human body. In this research, we have synthesized a nanocomposite based on copper-doped titanium dioxide (CuTiO2) adorned with 2D hexagonal boron nitride (CuTiO2@BN) for the efficient electrochemical detection of CML. A series of characterization techniques FT-IR, XRD, Raman spectroscopy, SEM, TEM, EDAX XPS, and electrochemical characterization were used to analyze the CuTiO2@BN nanocomposite structural and morphological compositions. The sensing performance of the CuTiO2@BN modified GCE for CML detection has been assessed using voltammetry methods. The chronoamperometry technique analyzed the kinetics of the electrochemical oxidation of CML at CuTiO2@BN/GCE. The CuTiO2@BN-based glassy carbon electrode (GCE) has a synergetic electro-catalytic effect on CML oxidation due to its many active sites, enhanced surface area, fast charge transfer, and numerous defects. For the detection of CML, the suggested electrochemical sensor exhibits excellent selectivity, low limit of detection (LOD) as found 5.0 nM, wide linear ranges (0.02-8000 µM), and quick reaction times.

Tetrahedral DNA nanostructure (TDN) is highly promising in developing electrochemical aptamer-based (E-AB) sensors for biomolecular detection, owing to its inherit programmability, spatial orientation and structural robustness. However, current interrogation strategies applied for TDN-based E-AB sensors, including enzyme-based amperometry, voltammetry, and electrochemical impedance spectroscopy, either require complicated probe design or suffer from limited applicability or selectivity. In this study, a TDN pendulum-empowered E-AB sensor interrogated by chronoamperometry for reagent-free and continuous monitoring of a blood clotting enzyme, thrombin, was developed. TDN pendulums with extended aptamer sequences at three vertices were immobilized on a gold electrode via a thiolated double-stranded DNA (dsDNA) at the fourth vertex, and their motion is modulated by the bonding of target thrombin to aptamers. We observed a significantly amplified signalling output on our sensor based on the TDN pendulum compared to E-AB sensors modified with linear pendulums. Moreover, our sensor achieved highly selective and rapidly responsive measurement of thrombin in both PBS and artificial urine, with a wide dynamic range from 1 pM to 10 nM. This study shows chronoamperometry-enabled continuous biomarker monitoring on a sub-second timescale with a drift-free baseline, demonstrating a novel approach to accurately detect molecular dynamics in real time.

Glypican-3 (GPC3) is an essential reference target for hepatocellular carcinoma detection, follow-up and prediction. Herein, a dual-signal electrochemical aptasensor based on reduced graphene oxide-cuprous oxide (RGO-Cu2O) nanozyme was developed for GPC3 detection. The RGO-Cu2O nanoenzyme displayed excellent electron transport effect, large specific surface area and outstanding peroxidase-like ability. The differential pulse voltammetry (DPV) signal of Cu2O oxidation fraction and the chronoamperometry (i-t) signal of H2O2 decomposition catalyzed by RGO-Cu2O nanozyme were used as dual-signal detection. Under optimal conditions, the log-linear response ranges were 0.1 to 500.0 ng/mL with the limit of detection 0.064 ng/mL for DPV technique, and 0.1-50.0 ng/mL for i-t technique (detection limit of 0.0177 ng/mL). The electrochemical aptasensor has remarkably analytical performance with wide response range, low detection limit, excellent repeatability and specificity, good recovery in human serum samples. The two output signals of one sample achieve self-calibration of the results, effectively avoiding the occurrence of possible leakage and misdiagnosis of a single detection signal, suggesting that it will be a promising method in the early biomarker detection.

Increased evidence has documented a direct association between Ciprofloxacin (CFX) intake and significant disruption to the normal functions of connective tissues, leading to severe health conditions (such as tendonitis, tendon rupture and retinal detachment). Additionally, CFX is recognized as a potential emerging pollutant, as it seems to impact both animal and human food chains, resulting in severe health implications. Consequently, there is a compelling need for the precise, swift and selective detection of this fluoroquinolone-class antibiotic. Herein, we present a novel graphene-based electrochemical sensor designed for Ciprofloxacin (CFX) detection and discuss its practical utility. The graphene material was synthesized using a relatively straightforward and cost-effective approach involving the electrochemical exfoliation of graphite, through a pulsing current, in 0.05 M sodium sulphate (Na2SO4), 0.05 M boric acid (H3BO3) and 0.05 M sodium chloride (NaCl) solution. The resulting material underwent systematic characterization using scanning electron microscopy/energy dispersive X-ray analysis, X-ray powder diffraction and Raman spectroscopy. Subsequently, it was employed in the fabrication of modified glassy carbon surfaces (EGr/GC). Linear Sweep Voltammetry studies revealed that CFX experiences an irreversible oxidation process on the sensor surface at approximately 1.05 V. Under optimal conditions, the limit of quantification was found to be 0.33 × 10-8 M, with a corresponding limit of detection of 0.1 × 10-8 M. Additionally, the developed sensor\'s practical suitability was assessed using commercially available pharmaceutical products.

The present work evaluates the effect of Co content on the microstructure and corrosion performance of Al-Co alloys of various compositions (2-32 wt% Co), fabricated by flux-assisted stir casting. A preliminary investigation on the effect of heat treatment (600 °C, up to 72 h) on the microstructure and corrosion behavior of Al-20 wt% Co and Al-32 wt% Co was also conducted. The Al- (2-10) wt% Co alloys were composed of acicular Al9Co2 particles uniformly dispersed in an Al matrix. The Al-20 wt% Co and Al-32 wt% Co alloys additionally contained Al13Co4 blades enveloped in Al9Co2 wedges. Heat treatment of Al-20 wt% Co and Al-32 wt% Co led to a significant reduction in the volume fraction of Al13Co4 and a decrease in hardness. Al-Co alloys with high Co content (10-32 wt% Co) exhibited greater resistance to localized corrosion in 3.5 wt% NaCl, but lower resistance to general corrosion compared to the (0-5 wt% Co) alloys. Heat treatment led to a slight increase in the corrosion resistance of the Al-Co alloys. The microstructure of the produced alloys was analyzed and correlated with the corrosion performance. Finally, corrosion mechanisms were formulated.

A flow-through biosensor system for the determination of uric acid was developed on the platform of flow-through electrochemical cell manufactured by 3D printing from poly(lactic acid) and equipped with a modified screen-printed graphite electrode (SPE). Uricase was immobilized to the inner surface of a replaceable reactor chamber. Its working volume was reduced to 10 μL against a previously reported similar cell. SPE was modified independently of the enzyme reactor with carbon black, pillar[5]arene, poly(amidoamine) dendrimers based on the p-tert-butylthiacalix[4]arene (PAMAM-calix-dendrimers) platform and electropolymerized 3,7-bis(4-aminophenylamino) phenothiazin-5-ium chloride. Introduction of the PAMAM-calix-dendrimers into the electrode coating led to a fivefold increase in the redox currents of the electroactive polymer. It was found that higher generations of the PAMAM-calix-dendrimers led to a greater increase in the currents measured. Coatings consisted of products of the electropolymerization of the phenothiazine with implemented pillar[5]arene and PAMAM-calix-dendrimers showing high efficiency in the electrochemical reduction of hydrogen peroxide that was formed in the enzymatic oxidation of uric acid. The presence of PAMAM-calix-dendrimer G2 in the coating increased the redox signal related to the uric acid assay by more than 1.5 times. The biosensor system was successfully applied for the enzymatic determination of uric acid in chronoamperometric mode. The following optimal parameters for the chronoamperometric determination of uric acid in flow-through conditions were established: pH 8.0, flow rate 0.2 mL·min-1, 5 U of uricase per reactor. Under these conditions, the biosensor system made it possible to determine from 10 nM to 20 μM of uric acid with the limit of detection (LOD) of 4 nM. Glucose (up to 1 mM), dopamine (up to 0.5 mM), and ascorbic acid (up to 50 μM) did not affect the signal of the biosensor toward uric acid. The biosensor was tested on spiked artificial urine samples, and showed 101% recovery for tenfold diluted samples. The ease of assembly of the flow cell and the low cost of the replacement parts make for a promising future application of the biosensor system in routine clinical analyses.