In this work, a natural sodium-montmorillonite clay mineral (Mt-Na) was functionalized with amine groups, either by direct grafting (Mt-NH 2 ) or via acid activation followed by grafting (MtH-NH 2 ) of [3(2-aminoethyl)amino)]propyltrimethoxysilane (AEP-TMS). The morphology and structure of the resulting composite materials were characterized by scanning electron microscopy, X-ray diffraction, N 2 adsorption-desorption isotherms (BET method) infrared spectroscopy, CHN elemental analysis and thermogravimetric analyses (TGA). The obtained organoclays were then used to modify the surface of a glassy carbon electrode (GCE), and the permselectivity and accumulation properties of the resulting films were investigated by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS).The results indicated that MtH-NH 2 modified GCE (GCE/MtH-NH 2 ) exhibited some charge selectivity features and can be applied to the electrochemical oxidation of catechol (CT). By plotting the double logarithmic variation of anodic peak currents (Ipa) versus potential scan rate, the obtained slope value of 0.49 revealed a diffusion-controlled electron-transfer mechanisms for the redox process. The electrochemical behavior of CT on the modified electrode was also studied using differential pulse voltammetry (DPV). The sensitivities of GCE/MtH-NH 2 for CT were 1.71, 3.87 and 1.35-fold greater than signals obtained on the bare GCE, GCE/Mt-Na and GCE/Mt-NH 2 respectively, due to the ability of the aminated materials to strongly accumulate CT. After optimization, GCE/MtH-NH 2 was used for CT determination by differential pulse voltammetry that gave rise to a linear response in the concentration range from 5 µM to 80 µM (R 2 = 0.999), and to a detection limit of 0.65 µM.The proposed method was applied to CT detection in water samples and in a tea sample.
The coupling reactions of diazotized thienocoumarin derivatives with p-acetaminophen, salicylic acid and acetylsalicylic acid gave four products in which the benzene ring of the phenolic reagents were primarily substituted by two 3-diazenyl-4H-thieno[3,4-c]chromen-4-one or 3-diazenyl-4-imino-4H-thieno[3,4c]chromene moieties. The newly prepared azo dyes were fully characterized based on their analytical and spectroscopic data. The electrochemical analysis of the novel azo dyes carried out on a glassy carbon electrode unequivocally further confirmed the assigned structures. The synthesized compounds tested for their antimicrobial activity using broth microdilution method, showed good activities.
A talc-like magnesium phyllosilicate functionalized with amine groups (TalcNH2), useful as sensor material in voltammetry stripping analysis, was synthesized by a sol–gel-based processing method. The characterizations of the resulting synthetic organoclay by scanning electron microscopy (SEM), X-ray diffraction, N2 sorption isotherms (BET method), Fourier transform infrared spectroscopy (FTIR), CHN elemental analysis and UV–Vis diffuse reflectance spectroscopy (UV–Vis-DRS) demonstrated the effectiveness of the process used for grafting of amine functionality in the interlamellar clay. The results indicate the presence of organic moieties covalently bonded to the inorganic lattice of talc-like magnesium phyllosilicate silicon sheet, with interlayer distances of 1568.4 pm. In an effort to use a talc-like material as an electrode material without the addition of a dispersing agent and/or molecular glue, the TalcNH2 material was successfully dispersed in distilled water in contrast to natural talc. Then, it was used to modify a glassy carbon electrode (GCE) by drop coating. The characterization of the resulting modified electrode by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) revealed its charge selectivity ability. In addition, EIS results showed low charge transfer resistance (0.32 Ω) during the electro-oxidation of [Fe(CN)6]3−. Kinetics studies were also performed by EIS, which revealed that the standard heterogeneous electron transfer rate constant was (0.019 ± 0.001) cm.s−1, indicating a fast direct electron transfer rate of [Fe(CN)6]3− to the electrode. Using anodic adsorptive stripping differential pulse voltammetry (DPV), fast and highly sensitive determination of Pb(II) ions was achieved. The peak current of Pb2+ ions on TalcNH2/GCE was about three-fold more important than that obtained on bare GCE. The calculated detection and quantification limits were respectively 7.45 × 10−8 M (S/N = 3) and 24.84 × 10−8 M (S/N 10), for the determination of Pb2+ under optimized conditions. The method was successfully used to tap water with satisfactory results. The results highlight the efficient chelation of Pb2+ ions by the grafted NH2 groups and the potential of talc-like amino-functionalized magnesium phyllosilicate for application in electrochemical sensors.
In this work, an electrode modified with an amino-functionalized clay mineral was used for the electrochemical analysis and quantification of quercetin (QCT). The resulting amine laponite (LaNH2) was used as modifier for a glassy carbon electrode (GCE). The organic–inorganic hybrid material was structurally characterized using X-ray diffraction, Fourier transformed infrared spectroscopy (FTIR), scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and CHN elemental analysis. The covalent grafting of the organosilane to the clay backbone was confirmed. The charge on the aminated laponite, both without and with the protonation of NH2 groups, was evaluated via cyclic voltammetry. On the protonated amine (LaNH3+)-modified GCE, the cyclic voltammograms for QCT showed two oxidation peaks and one reduction peak in the range of −0.2 V to 1.2 V in a phosphate buffer–ethanol mixture at pH 3. By using the differential pulse voltammetry (DPV), the modification showed an increase in the electrode performance and a strong pH dependence. The experimental conditions were optimized, with the results showing that the peak current intensity of the DPV increased linearly with the QCT concentration in the range from 2 × 10−7 M to 2 × 10−6 M, leading to a detection limit of 2.63 × 10−8 M (S/N 3). The sensor selectivity was also evaluated in the presence of interfering species. Finally, the proposed aminated organoclay-modified electrode was successfully applied for the detection of QCT in human urine. The accuracy of the results achieved with the sensor was evaluated by comparing the results obtained using UV–visible spectrometry.
Epinephrine (EP, also called adrenaline) is a compound belonging to the catecholamine neurotransmitter family. It can cause neurodegenerative diseases such as Alzheimer’s disease, Parkinson’s disease, Huntington’s disease and amyotrophic lateral sclerosis. This work describes an amperometric sensor for the electroanalysis of EP, based on an inkjet-printed graphene electrode (IPGE), modified by a thin film of a laponite (La) clay mineral. The ion exchange properties and permeability of the prepared sensor (denoted La/IPGE) were evaluated using multi-sweep cyclic voltammetry while its charge transfer resistance was determined by electrochemical impedance spectroscopy. The results showed globally that La/IPGE exhibited more a sensitive response towards the detection of EP, in comparison with the bare IPGE. The developed sensor was directly applied for the determination of EP in aqueous solution using differential pulse voltammetry, and under optimized conditions, the calibration curve was plotted in the concentration range of 0.8 to 60 μM. The anodic peak current of EP was directly proportional to its concentration, leading to a detection limit of 0.29 μM. The sensor was successfully applied for the determination of EP in pharmaceutical preparation and best recovery rates were also obtained. The interfering effect of selected species was evaluated to highlight the selectivity of the elaborated sensor.
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