Voltammetric sensing of sulfamethoxazole using a glassy carbon electrode modified with a graphitic carbon nitride and zinc oxide nanocomposite

A voltammetric sensor is described for the determination the antibiotic sulfamethoxazole (SMZ). It is based on the use of a glassy carbon electrode (GCE) modified with a nanocomposite prepared from graphitic carbon nitride and zinc oxide (g-C₃N₄/ZnO). The nanorod-like ZnO nanostructure were synthesized sonochemically. The g-C₃N₄/ZnO nanocomposite was then prepared by mixing g-C₃N₄ with ZnO, followed by ultrasonication. The morphology and structure of the nanocomposite were characterized by X-ray diffraction, Fourier-transform infrared spectroscopy and transmission electron microscopy. Under the optimal conditions, the response of the electrode, typically measured between 0.8 and 0.9 V (vs. Ag/AgCl), increases linearly in the 20 nM to 1.1 mM SMZ concentration range, and the lower detection limit is 6.6 nM. This is better than that of many previously reported sensors for SMZ. The modified electrode is highly selective, well reproducible and maintains its activity for at least 4 weeks. It was applied to the determination of SMZ in spiked human blood serum samples in with satisfactory results.

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Graphical abstract Schematic presentation of the voltammetric sensor for sulfamethoxazole. It consists of a glassy carbon electrode modified with a nanocomposite prepared from graphitic carbon nitride (g-C₃N₄/ZnO) that was supported with zinc oxide nanorods.

     

Approximation of continuous functions by generalized karamata means

A sufficient condition for the order of approximation of a continuous 2π periodic function with a given majorant for the modulus of continuity by the [F, d_n] means of its Fourier series to be of Jackson order is obtained. This sufficient condition is shown to be not enough for the order of approximation by partial sums of their Fourier series to be of Jackson order. The error estimate is shown to be the best possible.     

Preparation of nitrogen-doped reduced graphene oxide and its use in a glassy carbon electrode for sensing 4-nitrophenol at nanomolar levels

We describe a novel procedure for the synthesis of nitrogen-doped reduced graphene oxide (N-rGO). It is based on the thermal reduction of GO (dispersed in water) with sodium diethyldithiocarbamate that acts as both the reducing agent and the source for nitrogen. The surface morphology of the N-rGO is characterized using high resolution transmission electron microscopy. X-ray photoelectron spectroscopy was carried out to study the composition of their surface, and Raman spectroscopy was performed to study the level of doping with nitrogen and the structural order. The N-rGO was deposited on a glassy carbon electrode (GCE), and the resulting electrode utilized as a sensing platform for 4-nitrophenol (4-NP). The modified GCE exhibits a well-defined oxidation peak current that is about ten times larger when compared to that of a bare GCE. The electron transfer number, proton transfer number and electron transfer rate constant (k_s 1.046 s^?1) were determined. At optimized conditions, the oxidation peak current is linearly related to the concentration of 4-NP in the 20–500 nM range, with a correlation coefficient of 0.9917. The detection limit (at an SNR of 3) is 7 nM. The method was successfully applied to the analysis of waters spiked with 4-NP. Recoveries range from 97.8 to 102.6 %, and no interferences are found for common inorganic cations and anions. Figure

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Vibrational spectra and assignments of 5-amino-2-chlorobenzoic acid by ab initio Hartree-Fock and density functional methods

The Fourier transform Raman and Fourier transform infrared spectra of 5-amino-2-chlorobenzoic acid (5A2CBA) were recorded in the solid phase. Geometry opitimizations were done without any constraint and harmonic-vibrational wavenumber and several thermodynamic parameters were calculated for the minimum energy conformer at ab initio and DFT levels invoking 6-311G(d,p) basis set and the results are compared with the experimental values with the help of three specific scaling procedures, the observed vibrational wavenumbers in FTIR and FT-Raman spectra were analyzed and assigned to different normal modes of the molecule. Most of the modes have wavenumbers in the expected range, the error obtained was in general very low. The appropriate theoretical spectrograms for the FTIR spectra of the title molecule were also constructed.     

Preparation of nitrogen-doped reduced graphene oxide and its use in a glassy carbon electrode for sensing 4-nitrophenol at nanomolar levels

We describe a novel procedure for the synthesis of nitrogen-doped reduced graphene oxide (N-rGO). It is based on the thermal reduction of GO (dispersed in water) with sodium diethyldithiocarbamate that acts as both the reducing agent and the source for nitrogen. The surface morphology of the N-rGO is characterized using high resolution transmission electron microscopy. X-ray photoelectron spectroscopy was carried out to study the composition of their surface, and Raman spectroscopy was performed to study the level of doping with nitrogen and the structural order. The N-rGO was deposited on a glassy carbon electrode (GCE), and the resulting electrode utilized as a sensing platform for 4-nitrophenol (4-NP). The modified GCE exhibits a well-defined oxidation peak current that is about ten times larger when compared to that of a bare GCE. The electron transfer number, proton transfer number and electron transfer rate constant (k_s 1.046 s⁻¹) were determined. At optimized conditions, the oxidation peak current is linearly related to the concentration of 4-NP in the 20–500 nM range, with a correlation coefficient of 0.9917. The detection limit (at an SNR of 3) is 7 nM. The method was successfully applied to the analysis of waters spiked with 4-NP. Recoveries range from 97.8 to 102.6 %, and no interferences are found for common inorganic cations and anions.

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Phytosynthesis of Silver Nanoparticle (AgNPs) Using Aqueous Leaf Extract of Knoxia sumatrensis (Retz.) DC. and Their Multi-Potent Biological Activity: An Eco-Friendly Approach

Green synthesis of silver nanoparticles (AgNPs) has gained greater interest among chemists and researchers in this current scenario. The present research investigates the larvicidal and anti-proliferation activity of AgNPs derived from Knoxia sumatrensis aqueous leaf extract (K. sumatrensis-ALE) as a potential capping and reducing candidate. The synthesized AgNPs were characterized through-UV-spectra absorption peak at 425 nm. The XRD and FT-IR studied displayed the crystalline nature and presence of functional groups in prepared samples. FE-SEM showed the hexagonal shape of NPs with the size of 7.73 to 32.84 nm. The synthesized AgNPs displayed superior antioxidant and anti-proliferative activity (IC₅₀ 53.29 µg/mL) of breast cancer cell line (MCF-7). Additionally, larvicidal activity against mosquito vector Culex quinquefasciatus larvae delivered (LC₅₀-0.40, mg/L, and LC₉₀-15.83) significant mortality rate post treatment with synthesized AgNPs. Overall, the present research illustrates that the synthesized AgNPs have high biological potential and present a perfect contender in the pharmacological and mosquitocidal arena.     

Sensing of picric acid with a glassy carbon electrode modified with CuS nanoparticles deposited on nitrogen-doped reduced graphene oxide

We describe the preparation of a nanohybrid consisting of nitrogen doped reduced graphene oxide and CuS nanoparticles (N-rGO/CuS) by in-situ microwave irradiation at weight ratios of 25/75, 50/50, and 75/25. The resulting nanohybrids were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, FTIR, spectroscopy, scanning electron and transmission electron microscopy, electrochemically by cyclic voltammetry and electrochemical impedance analysis. It is shown that the CuS nanoparticles are evenly decorated onto the N-rGO surface. The nanohybrids was placed on glassy carbon electrode (GCE) where they showed electro-reductive activity towards picric acid, typically at working voltages between ?0.2 and ?0.8 V (vs. SCE). Effects of pH value and scan rate were evaluated, and it is shown that two electrons are involved in electro-reduction. The detection limits of the GCE modified with various N-rGO/CuS hybrids (with 25/75, 50/50, and 75/25 wt%) are 6.2, 3.2, and 0.069 μM respectively. The method demonstrates its applicability in sensing of picric acid with good reproducibility.

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Graphical abstract Nitrogen doped reduced graphene oxide nanohybrids was synthesized for the detection of picric acid. A straightforward and preconcentration free analysis of picric acid was successfully demonstrated at nanomolar levels using the nanohybrids.