One-dimensional NiFe2O4 nanorods modified with sulfur-rich spherical carbon nanoparticles for simultaneous voltammetric determination of ascorbic acid, dopamine and uric acid.

The work reports an easy way to prepare sulfur doped-carbon nanoparticles on a NiFe2O4 support. By placing the nanocomposite on a glassy carbon electrode (GCE), a sensor is obtained for simultaneous determination of ascorbic acid (AA), dopamine (DA) and uric acid (UA). The morphology, structural and chemical composition of the nanocomposite was characterized by various surface and physicochemical techniques, and its electrochemical properties were also examined. Modified GCE showed resolved electrocatalytic oxidation activity of AA, DA and UA with well separated peaks at 242 mV, 111 mV and 353 mV (vs. SCE). Under optimized conditions, the sensor has wide linear ranges and detection limits as low as 45, 25 and 17 nM for AA, DA and UA, respectively. The outstanding electrocatalytic performance of this GCE is attributed to the synergistic effect, defined size and unique morphology of the nanocomposite. This provides a benign micro-environment for convenient conjugation of biomolecules and improved charge transfer between the electrode and biomolecules for effective oxidation. The sensor was applied to the determination of AA in commercial vitamin C tablets, DA in injections, and UA in human urine. It showed recoveries in the range of 99.7-102.2%. Graphical abstract Schematic presentation of a method for synthesis of NiFe2O4-SDCNPs hybrid nanocomposite and its application for the electrochemical individual and simultaneous determination of ascorbic acid (AA), dopamine (DA) and uric acid (UA).

Quantification of Neuronal Cell-Released Hydrogen Peroxide Using 3D Mesoporous Copper-Enriched Prussian Blue Microcubes Nanozymes: A Colorimetric Approach in Real Time and Anticancer Effect.

Despite the effectiveness and selectivity of natural enzymes, their instability has paved the way for developing nanozymes with high peroxidase activity using a straightforward technique, thereby expanding their potential for multifunctional applications. Herein, meso-copper-Prussian blue microcubes (Meso-Cu-PBMCs) nanozymes were successfully prepared via a cost-effective hydrothermal route. It was found that the Cu-PBMCs nanozymes, with three-dimensional (3D) mesoporous cubic morphologies, exhibited an excellent peroxidase-like property. Based on the high affinity of Meso-Cu-PBMCs toward H2O2 (Km = 0.226 µM) and TMB (Km = 0.407 mM), a colorimetric sensor for in situ H2O2 detection was constructed. On account of the high catalytic activity, affinity, and cascade strategy, the Meso-Cu-PBMCs nanozyme generated rapid multicolor displays at varying H2O2 concentrations. Under optimized conditions, the proposed sensor exhibits a preferable sensitivity of 18.14 µA µM-1, a linear range of 10 nM-25 mM, and a detection limit of 6.36 nM (S/N = 10). The reliability of the sensor was verified by detecting H2O2 in spiked human blood serum and milk samples, as well as by detecting in situ H2O2 generated from the neuron cell SH-SY5Y. Besides, the Meso-Cu-PBMCs nanozyme facilitated the catalysis of H2O2 in cancer cells, generating •OH radicals that induce the death of cancer cells (HCT-116 colon cancer cells), which holds substantial potential for application in chemodynamic therapy (CDT). This proposed strategy holds promise for simple, rapid, inexpensive, and effective intracellular biosensing and offers a novel approach to improve CDT efficacy.

Laser-scribed Graphene Electrodes Functionalized with Nafion/Fe3O4 Nanohybrids for the Ultrasensitive Detection of Neurotoxin Drug Clioquinol.

The analysis of pharmaceutical active ingredients plays an important role in quality control and clinical trials because they have a significant physiological effect on the human body even at low concentrations. Herein, a flexible three-electrode system using laser-scribed graphene (LSG) technology, which consists of Nafion/Fe3O4 nanohybrids immobilized on LSG as the working electrode and LSG counter and reference electrodes on a single polyimide film, is presented. A Nafion/Fe3O4/LSG electrode is constructed by drop coating a solution of Nafion/Fe3O4, which is electrostatically self-assembled between positively charged Fe3O4 and negatively charged Nafion on the LSG electrode and is used for the first time to determine a neurotoxicity drug (clioquinol; CQL) in biological samples. Owing to their porous 3D structure, an enriched surface area at the active edges and polar groups (OH, COOH, and -SO3H) in Nafion/Fe3O4/LSG electrodes resulted in excellent wettability to facilitate electrolyte diffusion, which gave ∼twofold enhancement in electrocatalytic activity over LSG electrodes. The experimental parameters affecting the analytical performance were investigated. The quantification of clioquinol on the Nafion/Fe3O4/LSG electrode surface was examined using differential pulse voltammetry and chronoamperometry techniques. The fabricated sensor displays preferable sensitivity (17.4 µA µM-1 cm-2), a wide linear range (1 nM to 100 µM), a very low detection limit (0.73 nM), and acceptable selectivity toward quantitative analysis of CQL. Furthermore, the reliability of the sensor was checked by CQL detection in spiked human blood serum and urine samples, and satisfactory recoveries were obtained.

Glassy carbon electrodes modified with reduced graphene oxide-MoS2-poly (3, 4-ethylene dioxythiophene) nanocomposites for the non-enzymatic detection of nitrite in water and milk.

The detrimental effect of (NO2-) on environment, a sensitive and selective detection of nitrite (NO2-) ions with point-to-care device is need to be fabricated. Herein, we report the non-enzymatic nitrite sensor using a novel reduced graphene oxide/molybdenum disulfide/poly (3, 4-ethylene dioxythiophene) (rGO/MoS2/PEDOT) nanocomposite electrode. The rGO/MoS2/PEDOT nanocomposite was synthesized using facile and cost-effective hydrothermal and polymerization approaches. The characteristics of rGO-MoS2-PEDOT nanocomposite was investigated by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), Raman, transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and Brunauer-Emmett-Teller (BET) analyses. The rGO-MoS2-PEDOT nanocomposite modified glassy carbon electrode (GCE) was directly used for electrocatalytic detection of nitrite ions present in the solution. TEM images show the PEDOT nanoparticles with an average size of 100-120 nm are uniformly covered on the outer face of rGO-MoS2 nanosheets. The interaction between the PEDOT and rGO-MoS2 is evidenced in the FTIR, XRD and XPS studies, and they produced synergistic effect, resulting enhanced electrocatalytic performance activity towards oxidation of nitrite. Under optimized conditions, the fabricated electrode exhibited remarkably good sensitivity (874.19 µA µM-1 cm-2), low detection limit (LOD) (0.059 µM, S/N = 3), wide linear range (0.001-1 mM) of nitrite with desirable selectivity, long-term stability and reproducibility. Furthermore, the practical feasibility of the fabricated sensor is validated by the successful detection of nitrite ion in some water and milk samples with excellent correlation. Thus, feasible easier synthesis method was adopted first time to fabricate rGO-MoS2-PEDOT nanocomposite nitrite sensor in the milk and water samples with enhanced selectivity, sensitivity and LOD.

Ultra-stable Mn1-xNixCO3 nano/sub-microspheres positive electrodes for high-performance solid-state asymmetric supercapacitors.

Long-term cycling performance of electrodes for application in supercapcitor has received large research interest in recent years. Ultra-stable Mn1-xNixCO3 (x-0, 0.20, 0.25 and 0.30) nano/sub-microspheres were synthesized via simple co-precipitation method and the Mn1-xNixCO3 was confirmed by XRD, FT-IR, XPS and their morphology was studied by SEM and TEM analysis. Among the various Mn1-xNixCO3 electrodes, the Mn0.75Ni0.25CO3 electrode exhibited the higher specific capacitance (364 F g-1 at 1 A g-1) with capacity retention of 96% after 7500 cycles at 5 A g-1. Moreover, the assembled solid-state asymmetric supercapacitor based on Mn0.75Ni0.25CO3//graphene nanosheets performed a high specific capacity of 46 F g-1 and energy density of 25 Wh kg-1 at a power density of 499 W kg-1 along with high capacity retention of 87.7% after 7500 cycles. The improved electrochemical performances are mainly owing to the intrinsic conductivity and electrochemical activity of MnCO3 after Mn1-xNixCO3 (x-0.20, 0.25 and 0.30) with appropriate Ni concentration. This study highlights the potentiality of the Mn0.75Ni0.25CO3//GNS asymmetric supercapacitor device for promising energy storage applications.

Temperature-Controlled Synthesis of Li- and Mn-Rich Li1.2Mn0.54Ni0.13Co0.13O2 Hollow Nano/Sub-Microsphere Electrodes for High-Performance Lithium-Ion Battery.

The calcination temperature plays a significant role in the structural, textural, and energy-storage performance of metal oxide nanomaterials in Li-ion battery application. Here, we report the formation of well-crystallized homogeneously dispersed Li1.2Mn0.54Ni0.13Co0.13O2 hollow nano/sub-microsphere architectures through a simple cost-effective coprecipitation and chemical mixing route without surface modification for improving the efficiency of energy storage devices. The synthesized Li1.2Mn0.54Ni0.13Co0.13O2 hollow nano/sub-microsphere cathode materials are calcined at 800, 900, 950, and 1000 °C. Among them, Li1.2Mn0.54Ni0.13Co0.13O2 calcined at 950 °C exhibits a high discharge capacity (277 mAh g-1 at 0.1C rate) and excellent capacity retention (88%) after 50 cycles and also delivers an excellent discharge capacity of >172 mAh g-1 at 5C rate. Good electrochemical performance of Li1.2Mn0.54Ni0.13Co0.13O2-950 is directly related to the optimized size of its primary particles (85 nm) (which constitute the spherical secondary particle, ∼720 nm) and homogeneous cation mixing. Higher calcination temperature (≥950 °C) leads to an increase of the primary particle size, poor cycling stability, and inferior rate capacity of Li1.2Mn0.54Ni0.13Co0.13O2 due to smashing of quasi-hollow spheres upon repeated lithium ion intercalations/deintercalations. Therefore, Li1.2Mn0.54Ni0.13Co0.13O2-950 is a promising electrode for the next-generation high-voltage and high-capacity Li-ion battery application.

Sensitive and selective non-enzymatic detection of glucose by monodispersed NiO @ S-doped hollow carbon sphere hybrid nanostructures.

Development of selective, sensitive and non-enzymatic sensor for glucose determination is highly important for the diagnosis and management of diabetes. Herein, we have reported the novel ultra sensitive and non-enzymatic sensor development by in-situ wraped NiO nanostructures (∼10-15 nm) on the sulfur-doped hollow carbon nanospheres (SDHCNSs) through hydrothermal-assisted process. The structural and morphological properties of the nanocomposites were characterized by X-ray diffraction (XRD), Raman spectroscopy, field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS) techniques. The prepared NiO@SDHCNSs was directly used as an electrochemical sensor for glucose determination, and its performance was evaluated by cyclic voltammetry and amperometric techniques. The fabricated non-enzymatic biosensor was exhibited remarkably good sensitivity (1697 µA mM-1cm-2), low detection limit (LOD) (52 nM), a wide linear range (up to 13 mM) of glucose with desirable selectivity, stability and reproducibility. Further, the constructed sensor has demonstrated an excellent anti-interference property in the presence of common interferences such as dopamine (DA), uric acid (UA) and ascorbic acid (AA). Most interestingly, the fabricated electrode is applicable for the practical analysis of glucose in the real blood serum and urine samples. The excellent electrochemical performances of NiO@SDHCNSs towards the oxidation of glucose are attributed to the increased electron transfer passage through unique hollow spherical morphology with increased redox couple of Ni(OH)2/NiOOH derived from NiO. Thus, the improved electrochemical performances of NiO@SDHCNSs can be adopted as a potential electrode for the real sample analysis.

Biodiesel synthesis by TiO2-ZnO mixed oxide nanocatalyst catalyzed palm oil transesterification process.

Biodiesel is a promising alternating environmentally benign fuel to mineral diesel. For the development of easier transesterification process, stable and active heterogeneous mixed metal oxide of TiO2-ZnO and ZnO nanocatalysts were synthesized and exploited for the palm oil transesterification process. The synthesized catalysts were characterized by XRD, FT-IR, and FE-SEM studies for their structural and morphological characteristics. It was found that TiO2-ZnO nanocatalyst exhibits good catalytic activity and the catalytic performance was greatly depends on (i) catalyst concentration (ii) methanol to oil molar ratio (iii) reaction temperature and (iv) reaction time. A highest 98% of conversion was obtained at the optimum reaction parameters with 200 mg of catalyst loading and the biodiesel was analyzed by TLC and (1)H NMR techniques. The TiO2-ZnO nanocatalyst shows good catalytic performance over the ZnO catalyst, which could be a potential candidate for the large-scale biodiesel production from palm oil at the reduced temperature and time.