Irreversible Oxidation Research Articles

Triosmium cluster bearing a metalated dibenzylideneacetone ligand: Synthesis, structure, redox and electronic properties

Dibenzylideneacetone (DBA) reacts with [Os3(CO)10(NCMe)2] in boiling benzene to afford the triosmium cluster [Os3(CO)10{κ2-(C,O)-C17H13O}(µ-H)] (1) formed through activation of one of the β-C–H bonds of the DBA ligand after initial coordination of the ketonic oxygen. The molecular structure of 1 has been determined unequivocally by single crystal X-ray diffraction analysis which reveals that the metalated DBA ligand formed a five-membered osmacycle by coordinating to a single osmium atom using its both donor atoms. Cluster 1 exhibits two closely spaced irreversible reduction peaks at –1.20 V and –1.30 V, respectively, together with an irreversible oxidation peak at 0.57 V. DFT calculations reveals the frontier orbitals are primarily either metal-based (HOMO) or ligand-based (LUMO) which suggests that the oxidation occurs from the metallic core while the first reduction is ligand-centered. Cluster 1 displays two absorption peaks at 337 nm and 477 nm in the UV-visible absorption spectrum. The lowest energy absorption at 477 nm can be attributed to the transition from HOMO to LUMO (MLCT) based on its frontier orbitals.

Chemometric-assisted eMIP-modified screen-printed sensor for robust herbicide MCPA determination

The paper describes the development and application of a screen-printed electrode cell with a graphite-ink working electrode modified by a molecularly imprinted electropolymerized polypyrrole for the voltammetric determination of the herbicide 4‑chloro-2-methylphenoxyacetic acid (MCPA). The method exploits the direct measurement of the analyte by applying the differential pulse voltammetry (DPV) technique, taking advantage of the irreversible oxidation peak at about +1.0 V vs. Ag/AgCl pseudo reference electrode. The presence of the molecularly imprinted polypyrrole enhances the sensor's selectivity and sensitivity. A chemometric approach has been crucial for quantitative analysis because of the peak's broad and not well-defined shape. Firstly, a proper pretreatment of the voltammetric signals is identified, proving the most effective is the first-derivative function transformation of the signal. The Partial Least Square regression (PLS) is the tool applied for MCPA quantification. A preliminary PLS model has been developed and validated in dihydrogen phosphate solution at pH 5.5, aiming to optimize the data treatment approach. Then, the same approach is used to develop a PLS model analyzing tap water samples fortified with MCPA and other pesticides as possible interferents to simulate contaminated natural waters. The model correctly predicted the analyte concentration in the range of 2.5–75 μM, assuring the reliability and robustness of the sensor for the possible quantification of MCPA in wastewater samples.

Oxygen Reaction of Nonlayered Tetrahedral KFeO2 Positive Electrode for Potassium-Ion Battery Using an FSA-based Ionic Liquid Electrolyte

K-ion batteries (KIBs) that use ionic liquid (IL) electrolytes are promising candidates for post-Li-ion batteries because of the abundance of potassium resources and safety of ILs. We successfully synthesized stoichiometric KFeO2 using a solid-state method and evaluated its charge–discharge performance as a KIB positive electrode material, with an amide-based IL electrolyte at 298 K. Transmission electron microscopy, X-ray photoelectron spectroscopy, synchrotron soft X-ray absorption spectroscopy, and energy-dispersive X-ray spectroscopy data showed that the bulk redox and surface oxidation of oxygen, rather than those of iron, contribute to the reversible and irreversible capacities, respectively. Capacity decay occurred upon repeated cycling, owing to the surface irreversible oxidation of oxygen ions to form O2 and K1−x FeO2−x/2, which blocks the pathways of K+ transfer to KFeO2 particles. This study provides a vital platform for constructing novel KIBs and elucidates the important role of oxygen in KFeO2 positive electrode.

Harnessing Graphene-Modified Electrode Sensitivity for Enhanced Ciprofloxacin 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.

Surface Extraction Process During Initial Oxidation of Pt(111): Effect of Hydrophilic/Hydrophobic Cations in Alkaline Media.

The surface oxidation states of the metal electrodes affect the activity, selectivity, and stability of the electrocatalysts. Oxide formation and reduction on such electrodes must be comprehensively understood to achieve next-generation electrocatalysts with outstanding performance and stability. Herein, the initial electrochemical oxidation of Pt(111) in alkaline media containing hydrophilic and hydrophobic cations is investigated by X-ray crystal truncation rod (CTR) scattering, infrared (IR) spectroscopy, and nanoparticle-based surface-enhanced Raman spectroscopy (SERS). Structural determination using X-ray CTR revealed surface buckling and Pt extraction at the initial stage of surface oxidation, depending on the cationic species. Vibrational spectroscopy is performed to identify the potential- and cation-dependent formation of three oxide species (IR-active OHad, Raman-active OHad/Oad(H2O), and Raman-active Oad). Hydrophilic alkali metal cations (Li+) inhibit surface roughening via irreversible oxide formation. Hydrophilic Li+ can strongly stabilize IR-active OHad, hindering the extraction of Pt surface atoms. Interestingly, bulky hydrophobic cations such as tetramethylammonium (TMA+) cation also reduce the extent of irreversible oxidation despite the absence of IR-active OHad. Hydrophobic TMA+ inhibits the formation of Raman-active OHad/Oad(H2O) associated with Pt extraction. In contrast, the moderate hydrophilicity of K+ has no protective effect against irreversible oxidation. Moderate hydrophilicity enables the coadsorption of Raman-active OHad/Oad(H2O) and Raman-active Oad. The electrostatic repulsion between Raman-active OHad/Oad(H2O) and neighboring Raman-active Oad promotes Pt extraction. These results provide insights into controlling the surface structures of electrocatalysts using cationic species during the oxide formation and reduction processes.

NaSn2F5 nanocluster composed of nanoparticles with matched lattices induced by dislocations: Accelerated sodium-ion transport via in situ oxidation in solid-state sodium metal battery

Na metal batteries using inorganic solid-state electrolytes (SSEs) have attracted extensive attention due to their superior safety and high energy density. However, their development is plagued by the unclear structural/volumetric evolution of SSEs and the corresponding Na+ migration mechanisms. In this work, NaSn2F5 (NSF) clusters are composed of nanoparticles (NPs) with matched lattices induced by dislocations, which can mitigate the volume swelling/shrinkage of the NPs. NSF behaves like a single ion conductor with a high Na+ transference number (tNa+) of 0.79. Specially, the ionic conductivity (σ) of NSF is increased from 7.64 × 10-6 to 5.42 × 10-5 S cm−1 after partial irreversible oxidation of Sn2+ (0.118 Å) → Sn4+ (0.069 Å) with the shrunk ionic radius during the charge process, giving more spaces for Na+ migration. Furthermore, a poly(acrylonitrile)-NaSn2F5-NaPF6 composite polymer electrolyte (NSF CPE) was fabricated with a σ of 4.13 × 10-4 S cm−1 and a tNa+ of 0.60. The NSF CPE-based symmetric cell can operate over 3000 h due to the couplings between the different components in NSF CPE, which is beneficial for ion transfer and the construction of stable solid electrolyte interface. And the quasi-solid-state Na|NSF CPE|Na3V2(PO4)3 full cell displays excellent electrochemical performance.

Disposable and Sensitive Electrochemical Determination of Isoliquiritigenin in Licorice Using Screen-Printed Carbon Electrode Modified With Multi-Walled Carbon Nanotubes

Herein, a high-sensitive electrochemical sensor based upon a multi-walled carbon nanotubes modified screen-printed carbon electrode (MWCNTs-SPCE) was constructed for the determination of isoliquiritigenin (ISL). The electrochemical properties of ISL on the MWCNTs-SPCE were investigated systematically and a fast and cost-effective method for the determination of ISL was successfully established. A clear irreversible oxidation peak of the ISL was observed at 0.3 V (versus Ag/AgCl) on the MWCNTs-SPCE. The oxidation of ISL on MWCNTs-SPCE was an adsorption reaction accompanied by diffusion. Using differential pulse voltammetry (DPV), we observed that the oxidation peak current of the ISL in phosphate buffer (pH 7) showed a linear relationship from 0.50 to 100 µg/mL and a detection limit of 0.10 µg/mL. This method displayed good repeatability and stability, as well as exhibited excellent selectivity for ISL. Also, we successfully applied the method to determine ISL in Chinese herbal medicine licorice. Validation of the analyses via spike assays showed a recovery rate ranging from 95.39 to 101.00%, which was consistent with high performance liquid chromatography (HPLC).

Electroanalytical Determination of Trimetazidine in Pharmaceuticals and Synthetic Urine Using an Anodically Treated Boron-Doped Diamond (BDD) Electrode and Square Wave Voltammetry (SWV)

Trimetazidine dihydrochloride is an anti-ischemic agent widely used in the treatment of coronary artery disease, more specifically in the treatment of angina. Here is reported a simple and sensitive electroanalytical methodology for quantifying trimetazidine in pharmaceutical and synthetic urine samples using square-wave voltammetry. The influence of anodic and cathodic treatments on boron-doped diamond (BDD) was evaluated. The best results for trimetazidine were obtained using a BDD treated anodically at +3.0 V versus Ag(s)/AgCl(s)/Cl-(aq., saturated KCl) for 300 s in 0.1 mol L−1 H2SO4. The determination of trimetazidine was carried out in Britton-Robinson buffer at pH 3. Trimetazidine oxidation reveals two well-defined irreversible oxidation peaks. A calibration relationship was obtained from 0.35 mg L-1 to 2.6 mg L−1 (R2 = 0.997). Limits of detection and quantification for trimetazidine were 5.63 x 10−9 and 1.88 x 10−8 mol L−1, respectively. Recovery values were between 97 and 101 % and 96.8 and 99.8 % in pharmaceutical and synthetic urine.

Ca-MOF-Polymer Modified Thin-Film Electrode for Detection of Toxic Cadmium (Cd2+) in Biofluid and Environmental Fluid

Abstract Competitive adsorption of Cd2+ on the cell leads to different diseases like kidney damage and osteoporosis. It is crucial for Cd2+ intake that ambient and biofluid supplies of Cd2+ be contained. For this, a calcium-based metal organic framework (Ca-MOF) was developed by hydrothermal methods using bidendate 1,4-benzene dicarboxylic acid and Calcium derived from biowaste chicken egg shells. Lower binding efficiency of Cd2+ with the undoped MOF is improved by complexing it with polyaniline (PANI) to generate Ca-MOF-PANI which provide amine functional groups. These are characterized by cyclic voltammetry (CV), ultra-violet visible spectroscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction and Fourier transform infrared spectroscopy spectroscopy. Electrochemical sensing showed an irreversible oxidation peak for Cd2+ at -0.75 V. The Ca-MOF-PANI showed higher Cd2+ sensing than the CaCO3, Ca-MOF, and PANI modified electrodes and confirmed by UV-Vis studies. The sensor showed lowest detection limit of 138 nM (25.3 ppb) with linearity range 0.1-2000 μM, respectively, high selectivity in presence of potential interferences, good reproducibility, stability, and repeatability features. Real sample analysis using urine and water samples indicates good signal recoveries ranged from 93.0 % to 112.0 %.

Fe single atoms encapsulated in N, P-codoped carbon nanosheets with enhanced peroxidase-like activity for colorimetric detection of methimazole

Excessive use of antithyroid drug methimazole (MMI) in pharmaceutical samples can cause hypothyroidism and symptoms of metabolic decline. Hence, it is urgent to develop rapid, low cost and accurate colorimetric method with peroxidase-like nanozymes for determination of MMI in medical, nutrition and pharmaceutical studies. Herein, Fe single atoms were facilely encapsulated into N, P-codoped carbon nanosheets (Fe SAs/NP-CSs) by a simple pyrolysis strategy, as certified by a series of characterizations. UV–vis absorption spectroscopy was employed to illustrate the high peroxidase-mimicking activity of the resultant Fe SAs/NP-CSs nanozyme through the typical catalysis of 3,3′,5,5′-tetramethylbenzidine (TMB) oxidation. The catalytic mechanism was scrutionously investigated by the fluorescence spectroscopy and electron paramagnetic resonance (EPR) tests. Additionally, the introduced MMI had the ability to reduce the oxidation of TMB (termed oxTMB) as a peroxidase inhibitor, coupled by fading the blue color. By virtue of the above findings, a visual colorimetric sensor was established for dual detection of methimazole (MMI) with a linear scope of 5–50 mM and a LOD of 1.57 mM, coupled by assay of H2O2 at a linear range of 3–50 mM. According to the irreversible oxidation of the drug, its screening with acceptable results was achieved on the sensing platform even in commercial tablets The Fe SAs/NP-CSs nanozyme holds great potential for clinical diagnosis and drug analysis.

Insight into role of Co species on NiCo/CeMgAl for ethanol steam reforming: Enhanced activity and resistance to coke

Bimetallic catalysts with unique geometric and electronic structure exhibit high performance compared to that of monometallic counterparts in the ethanol steam reforming (ESR). Herein, NiCo bimetals supported on CeO2 doped MgAl2O4 (NiCo/CeMgAl) with different ratio of Ni/Co were prepared for ESR. The synergies between Ni and Co in catalytic activities and ability to anti-coking were focused. The results demonstrate Co atoms trend to segregate toward the surface and are oxidized synchronously, forming the Ni-CoO hybrid surface. The reduced Ni particles are beneficial to maintain a stable catalytic activity for the C-C bonds scission, and the CoO particles formed by segregation and irreversible oxidation of Co0 are more conducive to activation of H2O, the resulting OH promotes the transformation of CHx species, which significantly reduces the selectivity of CH4 and prevents the formation of filamentous carbon. Controlling Co content and maintaining a stable M/Mδ+ are critical to balance the C-C bond scission reaction and the CH3* conversion reaction on the NiCo bimetallic catalysts. The optimal catalyst 9Ni1Co/CeMgAl shows the ethanol conversion of 93.9 % at TOS of 100 h, and the average rate of coke formation is 0.50 mgc·gcat-1·h−1.

Rational design and synthesis of triazene-amonafide derivatives as novel potential antitumor agents causing oxidative damage towards DNA through intercalation mode

In this work, we rationally designed and synthesized two novel triazene-amonafide derivatives 2-(2-(diisopropylamino)ethyl)-5-(3,3-dimethyltriaz-1-en-1-yl)-1H-benzo[de]isoquinoline-1,3(2H)-dione (D-11) and 5-(3,3-diethyltriaz-1-en-1-yl)-2-(2-(diisopropylamino)ethyl)-1H-benzo[de]isoquinoline-1,3(2H)-dione (D-12) as potential antitumor agents. The DNA damage induced by the intercalation mode of D-11 (D-12) towards DNA was electrochemically detected through the construction of efficient biosensors. The consecutive processes of reversible redox of naphthylimide ring and irreversible oxidation of triazene moiety were elucidated on the surface of glassy carbon electrode (GCE) by CV, SWV, and DPV methods. Electrochemical biosensors were obtained through the immobilization of ctDNA, G-quadruplexes, poly(dG), and poly(dA), respectively, on the clean surface of GCE. After the incubation of biosensors with D-11 or D-12, the peaks of dGuo and dAdo decreased prominently, and the peak of 8-oxoGua appeared at +0.50 V, suggesting that the interaction between D-11 (D-12) and DNA could result in the oxidative damage of guanine. Unexpected, the as-prepared DNA biosensor possessed satisfactory anti-interference property and good practicability in real samples. UV–vis and fluorescence spectra, and gel electrophoresis assays were employed to further confirm the intercalation mode of D-11 (D-12) towards DNA base pairs. Moreover, D-11 was proved to exhibit stronger anti-proliferation activity than mitionafide and amonafide against both A549 and HeLa cell lines.

Oxidative Post-translational Protein Modifications upon Ischemia/Reperfusion Injury.

While reperfusion, or restoration of coronary blood flow in acute myocardial infarction, is a requisite for myocardial salvage, it can paradoxically induce a specific damage known as ischemia/reperfusion (I/R) injury. Our understanding of the precise pathophysiological molecular alterations leading to I/R remains limited. In this study, we conducted a comprehensive and unbiased time-course analysis of post-translational modifications (PTMs) in the post-reperfused myocardium of two different animal models (pig and mouse) and evaluated the effect of two different cardioprotective therapies (ischemic preconditioning and neutrophil depletion). In pigs, a first wave of irreversible oxidative damage was observed at the earliest reperfusion time (20 min), impacting proteins essential for cardiac contraction. A second wave, characterized by irreversible oxidation on different residues and reversible Cys oxidation, occurred at late stages (6-12 h), affecting mitochondrial, sarcomere, and inflammation-related proteins. Ischemic preconditioning mitigated the I/R damage caused by the late oxidative wave. In the mouse model, the two-phase pattern of oxidative damage was replicated, and neutrophil depletion mitigated the late wave of I/R-related damage by preventing both Cys reversible oxidation and irreversible oxidation. Altogether, these data identify protein PTMs occurring late after reperfusion as an actionable therapeutic target to reduce the impact of I/R injury.

Aging Effect of Plasma-Treated Carbon Fiber Surface: From an Engineering Point

Dielectric barrier discharge (DBD) plasma surface modification has certain aging effect. This article studies the aging effect of plasma (DBD) on the surface modification of carbon fibers. The test results show that plasma (DBD) treatment reduces the impurity particles on the surface of carbon fibers and makes the surface texture coarser. In addition, there is no significant change. After plasma (DBD) treatment, the content of C–O–C, C–O and C=O on the surface of carbon fibers increased from 3.20%, 7.76% and 1.64% to 7.06%, 21.50 and 6.08%, respectively. This is due to the high-energy particle bombardment of the fiber surface, which forms activated carbon atoms on the surface. The free electrons of these activated carbon atoms combine with ionized oxygen in the air. However, with the passage of time, the content of C–O–C, C–O and C=O gradually decreases to 3.31%, 8.57% and 1.77%, respectively. This is because some functional groups formed on the treated carbon fiber surface are not firmly bound, and some of these functional groups containing O2 groups will combine with surrounding substances through irreversible chemical oxidation reactions to produce CO2, which leaves the carbon fiber surface as a gas. The treated carbon fibers will immediately become hydrophilic, and the water contact angle decreases from 148.71° to 0°. With the passage of time, the water contact angle gradually increases to 118.16°, and the hydrophobicity recovers.

Oxidation of Methanesulfinate by Hexachloroiridate(IV) and the Standard Electrode Potential of the Aqueous Methanesulfonyl Radical.

The aqueous reaction of [IrCl6]2- with CH3SO2- is biphasic and yields a 1:1 mixture of [IrCl6]3- and [IrCl5(H2O)]2- and CH3SO2Cl in the initial rapid phase. The next slow phase corresponds to the hydrolysis of CH3SO2Cl to yield CH3SO3- and Cl-. The initial phase shows kinetic inhibition by [IrCl6]3- that can be minimized by the addition of the radical scavenger propiolic acid. A detailed analysis of the kinetics indicates a mechanism with reversible outer-sphere electron transfer from CH3SO2- to [IrCl6]2- as the first step, followed by the irreversible inner-sphere oxidation of CH3SO2• by [IrCl6]2- to yield [IrCl5(H2O)]2- and CH3SO2Cl. Analysis of the inhibition by [IrCl6]3- and the kinetic effects of propiolic acid enable the determination of the equilibrium constant for the first electron-transfer step. This equilibrium constant then yields E° (CH3SO2•/CH3SO2-) = 1.01 V vs NHE at 25 °C. This is the first report of a standard potential for an alkanesulfonyl radical.

3D grape string-like heterostructures enable high-efficiency sodium ion capture in Ti3C2Tx MXene/fungi-derived carbon nanoribbon hybrids.

2D transition metal carbides and carbonitrides (MXenes) have emerged as promising electrode materials for electrochemistry ion capture but always suffer from severe layer-restacking and irreversible oxidation that restrains their electrochemical performance. Here we design a dual strategy of microstructure tailoring and heterostructure construction to synthesize a unique 3D grape string-like heterostructure consisting of Ti3C2Tx MXene hollow microspheres wrapped by fungi-derived N-doping carbon nanoribbons (denoted as GMNC). The 3D grape string-like heterostructure effectively avoids the aggregation of Ti3C2Tx MXene sheets and enhances the stability of MXenes, providing abundant active sites for ion capture, and an interconnected conductive bionic nanofiber network for high-rate electron transport. In consequence, GMNC achieves a superior adsorption capacity for sodium ions (Na+) in capacitive deionization (CDI) (162.37 mg gNaCl-1) with an ultra-high instantaneous adsorption rate (30.52 mg g-1 min-1) at an applied voltage of 1.6 V and satisfactory cycle stability over 100 cycles, which is a strong performer among the state-of-the-art values for MXene-based CDI electrodes. In addition, in situ electrochemical quartz crystal microbalance with dissipation monitoring (EQCM-D) measurement combined with density functional theory (DFT) reveals the mechanisms of the Na+ capture process in the GMNC heterostructure. This work opens a new avenue for designing high-performance MXenes with a 3D hierarchical heterostructure for advanced electrochemical applications.

Protein Tyrosine Phosphatase regulation by Reactive Oxygen Species.

Protein Tyrosine Phosphatases (PTPs) help to maintain the balance of protein phosphorylation signals that drive cell division, proliferation, and differentiation. These enzymes are also well-suited to redox-dependent signaling and oxidative stress response due to their cysteine-based catalytic mechanism, which requires a deprotonated thiol group at the active site. This review focuses on PTP structural characteristics, active site chemical properties, and vulnerability to change by reactive oxygen species (ROS). PTPs can be oxidized and inactivated by H2O2 through three non-exclusive mechanisms. These pathways are dependent on the coordinated actions of other H2O2-sensitive proteins, such as peroxidases like Peroxiredoxins (Prx) and Thioredoxins (Trx). PTPs undergo reversible oxidation by converting their active site cysteine from thiol to sulfenic acid. This sulfenic acid can then react with adjacent cysteines to form disulfide bonds or with nearby amides to form sulfenyl-amide linkages. Further oxidation of the sulfenic acid form to the sulfonic or sulfinic acid forms causes irreversible deactivation. Understanding the structural changes involved in both reversible and irreversible PTP oxidation can help with their chemical manipulation for therapeutic intervention. Nonetheless, more information remains unidentified than is presently known about the precise dynamics of proteins participating in oxidation events, as well as the specific oxidation states that can be targeted for PTPs. This review summarizes current information on PTP-specific oxidation patterns and explains how ROS-mediated signal transmission interacts with phosphorylation-based signaling machinery controlled by growth factor receptors and PTPs.

Linear Scan Voltammetry of Two-Step Irreversible Electron Oxidation Enhanced by the Immobilization of an Intermediate (E E) on the Electrode Surface

Linear Scan Voltammetry of Two-Step Irreversible Electron Oxidation Enhanced by the Immobilization of an Intermediate (E E) on the Electrode Surface

First report on the electrooxidation of vinpocetine using a modification free sensing platform: application to pharmaceutical formulations.

This study presents the first insights into vinpocetine (VIN) behavior, a nootropic compound, on a glassy carbon electrode (GCE). Cyclic voltammetry (CV) revealed an irreversible oxidation peak at +1.0 V (vs. Ag/AgCl), with pH dependency indicating proton involvement in the electrochemical reaction. Density functional theory (DFT) optimized VIN's molecular geometry, while Fukui functions and dual descriptors elucidated its reactivity for a more straightforward exploration of the complete electrooxidation mechanism. Differential pulse voltammetry (DPV) demonstrated VIN sensing capabilities within a concentration range of 0.20 to 12.8 mg L-1, with a theoretical limit of detection (LOD) at 0.07 mg L-1, using optimized conditions of supporting electrolyte. The method showed selectivity in the presence of excipients and interfering species commonly found in pharmaceutical formulations. Recovery tests yielded 95.5% (n = 3), and quantification in pharmaceutical formulations showed no significant differences compared to the reference method based on HPLC DAD. This novel electroanalytical method holds promise for VIN nootropic sensing and routine pharmaceutical analysis.

Electrocatalytic Amplified Sensor For Determination of Ofloxacin Using Zn2SnO4/Reduced Graphene Oxide Composite As Surface-Modifying Agent

This study describes an electroanalytical approach for the quantification of ofloxacin (OFL) through an electrochemical sensor based on a glassy carbon electrode modified with composite material (Zn2SnO4-rGO/GCE) using square wave voltammetry. Zn2SnO4 was synthesized by hydrothermal treatment and characterized by X-ray diffraction, Fourier-transform infrared and Raman spectroscopy and scanning electron microscopy. The analysis suggests a synergistic effect between the composite material, indicating irreversible oxidation of OFL in its protonated form (OFL+), involving two electrons. The electroanalytical methodology was successfully applied to determine OFL in ophthalmic solutions samples, achieving recovery rates ranging from 98.03% to 104.91%. Furthermore, it demonstrated high stability in both repeatability (RSD = 3.20%, n = 12) and reproducibility (RSD = 4.64%, n = 7), with no observed interference when additional substances were added. These results suggest the potential electroanalytical application of Zn2SnO4 and recommend the developed methodology as an alternative tool for OFL determination in commercial pharmaceutical samples.