Preparation and Characterization of a Novel Salicin-Cyclodextrin Complex.

Bioactive compounds extracted from plants can provide wide health benefits. However, some molecules have limited applications as pharmaceuticals due to their limited solubility, poor bioavailability, and low stability when exposed to environmental factors. Their integration in formulations that can deliver them to physiological targets while preserving their biological activity can enhance their usage in improving human health. This research provides a delivery system design to enhance the solubility, stability and to mask the bitter taste of salicin. Thus, a novel salicin-ß-cyclodextrin complex was prepared and analyzed by X-ray diffraction, scanning electron microscopy, thermogravimetric analysis, FTIR, Raman and UV-Vis spectroscopy. The analytical and computational methods provided clear and distinct evidence for inclusion of salicin within the ß-cyclodextrin cavity and brought important findings for the characterization of the inclusion complex. The present study showed that salicin and ß-cyclodextrin can form inclusion complexes, both in solution and in solid state, and that the inclusion of salicin in the cavity of ß-cyclodextrin leads to the improvement of its solubility and stability. Thus, the study communicates both qualitative and quantitative knowledge about the preparation of a new salicin-ß-cyclodextrin inclusion complex suggesting its potential applications in pharmaceutical industry and medical sciences, as formulations with better compliance for the patient, with increased bioavailability, and easier control of dosage.

One-Step Microwave-Assisted Hydrothermal Preparation of Zn-ZnO(Nw)-rGO Electrodes for Supercapacitor Applications.

Zn-ZnO(Nw)-rGO hybrid electrodes for supercapacitor applications were successfully prepared in situ by a one-step microwave-assisted hydrothermal method by deposition of reduced graphene oxide (rGO) on the structure of ZnO nanowires grown on the Zn foil. During the hydrothermal treatment, two processes occur the reduction of graphene oxide (GO) and the deposition of rGO on the Zn-ZnO(Nw) support. The growth of ZnO nanowires was achieved by thermal oxidation below the melting point of the Zn foil in a controlled atmosphere. The as-obtained electrodes were assessed for structural, optical, and morphological properties by X-ray diffraction, Raman spectroscopy, ultraviolet-visible spectroscopy, SEM microscopy, and EDX analysis. The supercapacitor properties of the Zn-ZnO(Nw)-rGO hybrid electrodes were investigated by cyclic voltammetry, electrochemical impedance spectroscopy, and galvanostatic charge-discharge analysis. The CV curve reveals that the Zn-ZnO(Nw)-rGO hybrid structures work as negative electrodes and exhibit a non-ideal rectangle-like shape, suggesting that the as-synthesized structure behaves as a pseudo-capacitor. A maximum capacitance was determined to be 395.79 mF cm-2 at a scan rate of 5 mV s-1. Based on GCD analysis, the maximum specific capacitance of 145.59 mF cm-2 was achieved at a low power density of 2 mA cm-2. The cycle life assessment of the Zn-ZnO(Nw)-rGO hybrid electrode over a 250-cycle number was performed by CV and GCD analysis. The maximum retention rate of 120.86% was achieved from GCD analysis over 250 cycles for the Zn-ZnO(Nw)-rGO hybrid electrode.

Fabrication of Flexible Supercapacitor Electrode Materials by Chemical Oxidation of Iron-Based Amorphous Ribbons.

A flexible electrode constructed from Fe-based amorphous ribbons decorated with nanostructured iron oxides, representing the novelty of this research, was successfully achieved in one-step via a chemical oxidation method, using a low concentration of NaOH solution. The growth of metal oxides on a conductive substrate, which forms some metal/oxide structure, has been demonstrated to be an efficient method for increasing the charge transfer efficiency. Through the control and variation of synthetic parameters, different structures and morphologies of iron oxide were obtained, including hexagonal structures with a hollow ball shape and rhombohedral structures with rhombus-like shapes. Structural and morphological characterization methods such as X-ray diffraction and SEM morphology were used on the as-synthesized composite materials. The supercapacitor properties of the as-developed amorphous ribbons decorated with Fe2O3 nanoparticles were investigated by cyclic voltammetry, galvanostatic charge discharge, and electrochemical impedance spectroscopy. The flexible supercapacitor negative electrode demonstrates a specific capacitance of 5.96 F g-1 for the 0.2 M NaOH treated sample and 8.94 Fg-1 for the 0.4 M NaOH treated sample. The 0.2 M treated negative electrodes deliver 0.48 Wh/kg at a power density of 20.11 W/kg, and the 0.4 M treated electrode delivers 0.61 Wh/kg at a power density of 20.85 W/kg. The above results show that these flexible electrodes are adequate for integration in supercapacitor devices, for example, as negative electrodes.

Self-Powered Photodetector Based on FTO/n-TiO2/p-CuMnO2 Transparent Thin Films.

A self-powered photodetector with the FTO/n-TiO2/p-CuMnO2 configuration, representing the novelty of the work, was successfully achieved for the first time and presumes two steps: deposition of the n-type semiconductor (TiO2) by the doctor blade method and of the p-type semiconductor (CuMnO2) by the spin coating technique, respectively. Investigation techniques of the structural and morphological characteristics of the as-synthesized heterostructures, such as XRD, UV-VIS analysis, and SEM/EDX and AFM morphologies, were used. The I-t measurements of the photodetector showed that the responsivity in the self-powered mode was 2.84 × 107 A W-1 cm2 and in the 1 V bias mode it was 1.82 × 106 A W-1 cm2. Additionally, a self-powered current of 14.2 nA was generated under UV illumination with an intensity of 0.1 mW/cm2. Furthermore, under illumination conditions, the response time (tres) and the recovery time (trec) of the sensor exhibited a good response; thus, tres = 7.30 s and trec = 0.4 s for the self-powered mode, and in the 1 V bias mode, these were tres = 15.16 s and trec = 2.18 s. The above results show that the transparent heterojunction device of n-TiO2/p-CuMnO2 exhibited a self-powered ultraviolet photodetector with high sensitivity.

Graphene Oxide Electroreduced onto Boron-Doped Diamond and Electrodecorated with Silver (Ag/GO/BDD) Electrode for Tetracycline Detection in Aqueous Solution.

A new electrochemical sensor designed by modifying the commercial boron-doped diamond (BDD) electrode with graphene oxide (GO) reduced electrochemically and further electrodecorated with silver (Ag), named the Ag/GO/BDD electrode, was selected among a series of the BDD, GOelectroreduced onto BDD (GO/BDD) and silver electrodeposited onto BDD (Ag/BDD) electrodes for the detection of tetracycline (TC) in aqueous solution. The best results regarding the sensitivity of 46.6 µA·µM-1·cm-2 and the lowest limit of detection of 5 nM was achieved using square-wave voltammetry (SWV) operated at the step potential of 5 mV, modulation amplitude of 200 mV and the frequency of 10 Hz in alkaline medium. The application of the alkaline supporting electrolyte-based procedure is limited for water monitoring due to the presence of chloride that interferes with TC detection; however, it can be applied for quantitative determination of pharmaceutical formulations. 0.1 M Na2SO4 supporting electrolyte eliminated chloride interference and can be used for the application of Ag/GO/BDD in practical detection of TC in water.

Electrochemical Method for Ease Determination of Sodium Diclofenac Trace Levels in Water Using Graphene-Multi-Walled Carbon Nanotubes Paste Electrode.

Sodium diclofenac (DCF) presence reported in water use cycle at various concentrations including trace levels necessitates continuous development of advanced analytical method for its determination. In this work, ease electrochemical methods for DCF determination based on voltammetric and amperometric techniques were proposed using a simple combination of graphene with multi-walled carbon nanotubes as paste electrode. Integration of the graphene with multi-walled carbon nanotubes enlarged the electroactive surface area of the electrode and implicitly enhanced the electrochemical response for DCF determination. On the basis of the sorption autocatalytic effect manifested at low concentration of DCF, we found that the preconcentration step applied prior to differential-pulsed voltammetry (DPV) and multiple-pulsed amperometry (MPA) allowed for the enhancement of the electroanalytical performance of the DCF electrochemical detections, which were validated by testing in tap water. The lowest limit of detection (LOD) of 1.40 ng·L-1 was found using preconcentration prior to DPV under optimized operating conditions, which is better than that reached by other carbon-based electrodes reported in the literature.

Enhanced Electrochemical Response of Diclofenac at a Fullerene⁻Carbon Nanofiber Paste Electrode.

The requirements of the Water Framework Directive to monitor diclofenac (DCF) concentration in surface water impose the need to find advanced fast and simple analysis methods. Direct voltammetric/amperometric methods could represent efficient and practical solutions. Fullerene⁻carbon nanofibers in paraffin oil as a paste electrode (F⁻CNF) was easily obtained by simple mixing and tested for DCF detection using voltammetric and amperometric techniques. The lowest limit of detection of 0.9 nM was achieved by applying square-wave voltammetry operated under step potential (SP) of 2 mV, modulation amplitude (MA) of 10 mV, and frequency of 25 Hz, and the best sensitivity was achieved by four-level multiple pulsed amperometry (MPA) that allowed in situ reactivation of the F⁻CNF electrode. The selection of the method must take into account the environmental quality standard (EQS), imposed through the "watchlist" of the Water Framework Directive as 0.1 µg·L-1 DCF. A good improvement of the electroanalytical parameters for DCF detection on the F⁻CNF electrode was achieved by applying the preconcentration step for 30 min before the detection step, which assured about 30 times better sensitivity, recommending its application for the monitoring of trace levels of DCF. The electrochemical behavior of F⁻CNF as a pseudomicroelectrode array makes it suitable for practical application in the in situ and real-time monitoring of DCF concentrations in water.

Copper-decorated carbon nanotubes-based composite electrodes for nonenzymatic detection of glucose.

The aim of this study was to prepare three types of multiwall carbon nanotubes (CNT)-based composite electrodes and to modify their surface by copper electrodeposition for nonenzymatic oxidation and determination of glucose from aqueous solution. Copper-decorated multiwall carbon nanotubes composite electrode (Cu/CNT-epoxy) exhibited the highest sensitivity to glucose determination.