Search Results (6)

This study centers on the development and characterization of an innovative electrochemical sensing probe composed of a sensing mesoporous functional sol–gel coating integrated onto a glassy carbon electrode (sol–gel/GCE) for the detection of NH₃ and/or NH₄⁺ in water. The main interest for integrating a functional sol–gel coating onto a GCE is to increase the selective and sensing properties of the GCE probe towards NH₃ and/or NH₄⁺ ions. The structure and surface morphology of the newly developed sol–gel/GCE probe were characterized employing scanning electron microscopy (SEM), atomic force microscopy (AFM), dynamic light scattering (DLS), and Fourier-transform infrared (FTIR), while the electrochemical sensing properties were evaluated by Berthelot’s reaction, cyclic voltammetry (CV), and adsorptive square wave–anodic striping voltammetry (Ads SW–ASV). It is shown that the newly developed sol–gel coating is homogeneously deposited on the GCE with a sub-micron and uniform thickness close to 630 nm and a surface roughness of 25 nm. The sensing testing of the sol–gel/GCE probe showed limits of detection and limits of quantitation of 1.7 and 5.56 nM of NH₄⁺, respectively, as well as a probe sensitivity of 5.74 × 10⁻¹ μA/μM cm⁻². The developed probe was fruitfully validated for the selective detection of NH₃/NH₄⁺ in fresh and sea water samples. Computed Student t_exp (0.45–1.25) and F_exp (1.69–1.78) (n = 5) tests were less than the theoretical t_tab (2.78) and F_tab (6.39) at 95% probability. Full article

The blood ammonia (NH₃) level is one of the most important hepatic biomarkers for the diagnosis and monitoring of liver pathologies and infections. In this work, we developed an optimized optical biosensing method to extract and quantify the ammonia contained in complex-matrix samples emulating the blood serum. First, the approach was tested with solutions of phosphate-buffered saline (PBS) and ammonia chloride. Then, further trials were carried out with solutions of fetal bovine serum (FBS). The ammonia was extracted from the tested samples through a customized cell, and it was optically quantified by exploiting the indophenol reaction. The extraction cell included a cation-exchange membrane in Nafion, which was chemically pre-treated through cleaning procedures of sulfuric acid and hydrogen peroxide to keep a basic pH in the ammonia solution and to avoid contaminants in the membrane. From the NH₃ solution, the indophenol reaction produced light-reactive indophenol dye molecules, which were used as colorimetric indicators. Through absorbance measurements of the indophenol dye solution at 670 nm wavelength, we were able to detect and quantify the ammonia level in the samples both with a spectrophotometer and a customized miniaturized read-out system, obtaining a detection limit of 0.029 µmol/mL. Full article

Nanotechnology is a burning field of scientific interest for researchers in current era. Diverse plant materials are considered as potential tool in green chemistry based technologies for the synthesis of metal nanoparticles (NPs) to cope with the hazardous effects of synthetic chemicals, leading to severe abiotic climate change issues in today’s agriculture. This study aimed to determine the synthesis and characterization of metal-based nanoparticles using extracts of the selected plant Calotropis gigantea and to evaluate the enzyme-inhibition activities and antibacterial and antifungal activity of extracts of metal-based zinc nanoparticles using C. gigantea extracts. The crystal structure and surface morphology were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). C. gigantea was examined for antimicrobial activity against clinical isolates of bacteria and fungi. The water, ethanolic, and acetone extracts of C. gigantea were studied for their antagonistic action against bacterial strains (E. coli, S. aureus, P. multocida, and B. subtilis) and selected fungal strains (A. paracistic, F. solani, A. niger, S. ferrugenium, and R. nigricans). In vitro antimicrobial activity was determined by the disc diffusion method, where C. gigantea was tested for AChE and BChE inhibitory activity using Ellman’s methodology. The kinetic analysis was performed by the proverbial Berthelot reaction for urease inhibition. The results showed that out of all the extracts tested, ethanolic and water extracts possessed zinc nanoparticles. These extracts showed the maximum zone of inhibition against F. solani and P. multocida and the lowest against S. ferrugenium and B. subtilis. A potential source of AChE inhibitors is certainly provided by the abundance of plants in nature. Numerous phyto-constituents, such as AChE and BChE inhibitors, have been reported in this communication. Water extract was active and has the potential for in vitro AChE and BChE inhibitory activity. The urease inhibition with flower extracts of C. gigantea revealed zinc nanoparticles in water extracts that competitively inhibited urease enzymes. In the case of cholinesterase enzymes, it was inferred that the water extract and zinc nanoparticles have more potential for inhibition of BChE than AChE and urease inhibition. Furthermore, zinc nanoparticles with water extract are active inthe inhibition of the bacterial strains E. coli, S. aureus, and P. multocida and the fungal strains A. paracistic, F. solani, and A. niger. Full article

Gastrointestinal tract infection caused by Helicobacter pylori is a common virulent disease found worldwide, and the infection rate is much higher in developing countries than in developed ones. In the pathogenesis of H. pylori in the gastrointestinal tract, the secretion of the urease enzyme plays a major role. Therefore, inhibition of urease is a better approach against H. pylori infection. In the present study, a series of syn and anti isomers of N-substituted indole-3-carbaldehyde oxime derivatives was synthesized via Schiff base reaction of appropriate carbaldehyde derivatives with hydroxylamine hydrochloride. The in vitro urease inhibitory activities of those derivatives were evaluated against that of Macrotyloma uniflorum urease using the modified Berthelot reaction. Out of the tested compounds, compound 8 (IC₅₀ = 0.0516 ± 0.0035 mM) and compound 9 (IC₅₀ = 0.0345 ± 0.0008 mM) were identified as the derivatives with potent urease inhibitory activity with compared to thiourea (IC₅₀ = 0.2387 ± 0.0048 mM). Additionally, in silico studies for all oxime compounds were performed to investigate the binding interactions with the active site of the urease enzyme compared to thiourea. Furthermore, the drug-likeness of the synthesized oxime compounds was also predicted. Full article

The development of in situ analytical devices has gained outstanding scientific interest. A solid sensing membrane composed of 1,2-naphthoquinone-4-sulfonate (NQS) derivatizing reagent embedded into a polymeric polydimethylsiloxane (PDMS) composite was proposed for in situ ammonium (NH₄⁺) and urea (NH₂CONH₂) analysis in water and urine samples, respectively. Satisfactory strategies were also applied for urease-catalyzed hydrolysis of urea, either in solution or glass-supported urease immobilization. Using diffuse reflectance measurements combined with digital image processing of color intensity (RGB coordinates), qualitative and quantitative analyte detection was assessed after the colorimetric reaction took place inside the sensing membrane. A suitable linear relationship was found between the sensor response and analyte concentration, and the results were validated by a thymol-PDMS-based sensor based on the Berthelot reaction. The suggested sensing device offers advantages such as rapidity, versatility, portability, and employment of non-toxic reagents that facilitate in situ analysis in an energy-efficient manner. Full article

Analytical methods based on the Berthelot reaction were recently adapted for determining monochloramine (MCA: NH₂Cl) in freshwater. The specificity of the Berthelot reaction with regard to MCA is related to the need for two exchangeable hydrogen atoms to form indophenol blue. MCA can thus be distinguished from organic N-chloramines, which have only one exchangeable hydrogen atom. Monobromamine (MBA: NH₂Br) may be formed during chlorination of seawater containing ammonium ions. Quantifying MBA is quite challenging and no method has been reported for its specific determination in seawater. As MBA also has two exchangeable hydrogen atoms, its reactivity might be analogous to that of MCA, but this hypothesis has never been investigated. The aim of this study was to examine the applicability of the so-called “indophenol method” for the determination of the MBA in freshwater and seawater samples. The reaction between MBA and Berthelot reagents was studied in both ultrapure water and artificial seawater. The reaction products were characterized by using gas chromatography coupled to mass spectrometry (GC–MS), Fourier transform-ion cyclotron resonance mass spectrometry (FT–ICR MS), and UV–vis spectroscopy. Results showed that colorimetric methods based on the Berthelot reaction were not suitable for measuring MBA in freshwater or seawater, since NH₂Br reacts with alkaline phenol derivative via electrophilic substitution to form ortho- and para-brominated phenols instead of forming indophenol. Full article