Ranolazine (RZ) is an anti-anginal drug with a distinct mechanism of action and widely employed in patients with chronic angina. Its measurement is essential in clinical environment to ensure adequate drug level and understand the redox mechanism which gives an idea of in-vivo fate of the drug. In view of this, an exemplary voltammetric approach is proposed here for determination of RZ utilizing glassy carbon electrode (GCE) fabricated with WO3 decorated graphene nanocomposite. The structural and morphological characterizations of modifier were made by employing XRD, FESEM, EDAX, HRTEM, XPS, Raman and FT-IR spectroscopy which revealed successful formation of the nanocomposite. As a result of high electrical conductivity and large effective surface area of WO3 nanoparticles and graphene nanosheets, the developed sensor WO3/Graphene/GCE displayed effectual and unrelenting electron interceding behavior exhibiting higher peak currents at lower potentials for RZ oxidation. Using square wave voltammetry, the drug showcased well-defined voltammetric response in Britton-Robinson buffer at pH 4.5 in concentration range from 0.2-1.4 μM and 1.4-14 μM with the low detection limit of 0.13 μM. The developed protocol was then implemented successfully to quantify RZ in commercially accessible pharmaceutical tablets with satisfactory recovery (99.8%-100.2%). The experimental results illustrated the applicability of the fabricated sensor for drug quality control and clinical analysis along with pharmacokinetic studies.
Chemical synthesis of Ag-NPs was carried out using reduction method. The reduction mechanistic approach of silver ions was found to be a basic clue for the formation of the Ag-NPs. The nanoparticles were characterized by UV-vis, FT-IR and TEM analysis. We had designed some experiments in support of our hypothesis, "low concentrations of novel nanoparticles (silver and gold) increases the activity of plant peroxidases and alter their structure also", we had used Ag-NPs and HRP as models. The immobilization/interaction experiment had demonstrated the specific concentration range of the Ag-NPs and within this range, an increase in HRP activity was reported. At 0.08 mM concentration of Ag-NPs, 50% increase in the activity yield was found. The U.V-vis spectra had demonstrated the increase in the absorbance of HRP within the reported concentration range (0.06-0.12 mM). Above and below this concentration range there was a decrease in the activity of HRP. The results that we had found from the fluorescence spectra were also in favor of our hypothesis. There was a maximum increase in ellipticity and α-helix contents in the presence of 0.08 mM concentration of Ag-NPs, demonstrated by circular dichroism (CD) spectra. Finally, incubation of a plant peroxidase, HRP with Ag-NPs, within the reported concentration range not only enhances the activity but also alter the structure.
In present work, we demonstrate a single step environmentally benign approach to synthesize Au/Ag bimetallic nanoparticles (BMNPs) using aqueous extract of Clove buds for the first time. Clove bud's (CB) extract has proficiency to act as a reducing and stabilizing agent for the formation of Au/Ag BMNPs. In presence of extract, AuIII and AgI are reduced competitively within same solution and produce Au/Ag alloy NPs. The kinetics besides the formation of NPs was studied using UV-visible spectroscopy and efficiency of the extract was monitored by varying contact time, temperature, pH and extract concentration. The electron microscopic studies revealed the presence of NPs with peculiar morphology at alkaline pH. Further, the existence of Au and Ag atoms was investigated using energy dispersive X-ray (EDX), X-ray diffraction (XRD) and cyclic voltammetry (CV) techniques. Fourier transform infrared spectroscopy (FTIR) showed that Eugenol in the extract is mainly responsible for the production of NPs which are also surrounded by various phytochemicals. Zeta potential of all the NPs is found to be negative which prevents their agglomeration due to inter-repulsion and the biosynthesized Au/Ag BMNPs revealed greater catalytic efficiency for the degradation of methyl orange (MO), methylene blue (MB) and reduction of p-nitrophenol (p-NP). Significant enhancement induced by BMNPs compared to individual monometallic nanoparticles (MMNPs) was assigned to the synergistic effect of MMNPs and coating of phytochemicals present in the CB extract.
In the present work, a chemically modified electrode has been fabricated utilizing Bi2O3/ZnO nanocomposite. The nanocomposite was synthesized by simple sonochemical method and characterized for its structural and morphological properties by using XRD, FESEM, EDAX, HRTEM and XPS techniques. The results clearly indicated co-existence of Bi2O3 and ZnO in the nanocomposite with chemical interaction between them. Bi2O3/ZnO nanocomposite based glassy carbon electrode (GCE) was utilized for sensitive voltammetric detection of an anti-biotic drug (balofloxacin). The modification amplified the electroactive surface area of the sensor, thus providing more sites for oxidation of analyte. Cyclic and square wave voltammograms revealed that Bi2O3/ZnO modified electrode provides excellent electrocatalytic action towards balofloxacin oxidation. The current exhibited a wide linear response in concentration range of 150-1000 nM and detection limit of 40.5 nM was attained. The modified electrode offered advantages in terms of simplicity of preparation, fair stability (RSD 1.45%), appreciable reproducibility (RSD 2.03%) and selectivity. The proposed sensor was applied for determining balofloxacin in commercial pharmaceutical formulations and blood serum samples with the mean recoveries of 99.09% and 99.5%, respectively.
The authors describe a method for solvent-free mechano-chemical synthesis of a bioinspired sorbent. A 2D ultra-thin carbon sheet similar to graphene oxide was prepared using a natural waste (onion sheet). The formation of 2D carbon sheets was confirmed by Raman spectroscopy, X-ray photoelectron spectroscopy and ATR-IR. The surface morphology was characterized by field emission scanning electron microscopy and high-resolution tunneling electron microscopy. The carbon sheets were decorated with crystalline MnFe2O4 nanoparticles by solid-state reaction at room temperature. The presence of magnetic particles in the final product was confirmed by vibrating sample magnetometry and electron microscopy. The synergistic effect of carbon sheets and MnFe2O4 led to an enhanced sorption of arsenic species compared to bare carbon sheets or to MnFe2O4 nanoparticles. A column was prepared for the simultaneous preconcentration and determination of trace levels of As(III) and As(V) from water samples. The preconcentration factors are between 900 and 833 for As(III) and As(V) species, respectively. The linearity of the calibration plot ranges from 0.4-10 ng mL-1. The detection limits (at 3σ) for both As(III) and As(V) are 30 pg mL-1. The Student's t values for the analysis of spiked samples are lower than the critical Student's t values at a 95% confidence level. The recoveries from spiked water samples range between 99 and 102.8%. Graphical abstract Schematic representation of the preparation of carbon sheets similar to graphene oxide from onion sheaths after pyrolysis at 800 °C. The prepared carbon sheet-MnFe2O4 composite shows excellent arsenic sorption and preconcentration down to the pg mL-1 concentration.