نشریه شیمی کاربردی روز
پیاپی 71 (تابستان 1403)

In this work, A novel novel cadmium (II) co-crystal binary coordination compound with 3- FBINH ligand and nitrate anionic ligand were synthesized and characterized. The structure of co-crystal (3- FBINH is the abbreviation of 3- flouro benzylidene iso nicotine hydrazide) ([Cd (3-FBINH)2 (NO3)2 (H2O)] [Cd (3-FBINH)2 (NO3) (C2H6O) (H2O)].NO3 (1) was characterized by single-crystal X-ray analysis. The X-ray structure revealed that the compound has two Cd (II) metal centers with 7 and 6 coordination numbers. The adjacent frameworks connected by labile interactions like strong hydrogen -bonding interactions, CH …π interactions CH …CH interactions that the self-assembly occurs in the structure. Consequently, the labile interactions also allow the structure to form a 3D supramolecular coordination system. Cd O nanoparticles were obtained by thermolysis of 1 at 550 °C. The morphology and size of the prepared Cd O nanoparticles were further studied using SEM and

Eco-friendly copper nanoparticles (NPs) were prepared from the interaction of a cheap and accessible precursor, blue alum with biomolecules (polyphenols, flavonoids, proteins, terpenoids and organic sulfur compounds) in the garlic extract as the reducing of copper(II) ions, and its protector and stabilizer. As-synthesized Cu NPs were characterized by conventional methods such as XRD, UV-Vis, FT-IR, SEM, TEM, TGA and EDX. Observing the absorption maximum at the wavelength of 580 nm in the UV-Vis spectrum of the suspension solution indicated the formation of copper nanoparticles due to its surface plasma resonance. The results of the XRD diffraction pattern showed that the average size of copper crystallite was 65 nm. The morphology of the synthesized sample by scanning electron microscope (SEM) showed that copper NPs were irregular spherical. Transmission electron microscopy (TEM) estimated the average size of copper particles to be 70 nm. The as-synthesized copper NPs were used as a nano-catalyst in the reduction process of methylene blue (MB) by sodium borohydride (NaBH4). The results showed that by increasing the amount of copper NPs, the rate of methylene blue reduction reaction increased. By adding 0.0010 g of as-synthesized copper NPs to a solution containing 25 mL of methylene blue 20 ppm and 25 mL of sodium borohydride 200 ppm, it reduced time of the reaction from 4 hours to 2 minutes and its efficiency was 77%. The complete reaction time of 25 mL of methylene blue solution with concentrations of 30, 40 and 50 ppm by 25 mL of sodium borohydride 200 ppm in the presence of 0.0010 g of copper NPs took 15, 25 and 28 minutes, respectively. The effect of solution pH showed that in a certain amount of nanoparticles, the reduction rate of methylene blue was higher in an alkaline environment.

The production of pure H2 for polymer fuel cells was studied by the chemical loop reforming of methanol in the presence of 0.3CoFe2O4-0.4ZrO2 as an oxygen carrier in a micro-channel reactor. The results of this study showed that the production of pure H2 is possible only if the coke deposition is controlled. By optimizing the reduction time to 7 minutes, the coke deposition controlled and pure H2 flow was produced with an average yield of 2.6%, which was an interesting result and so far this degree of purity of H2 has not been reported by the chemical loop reforming of methanol. To increase the yield of pure H2 in this study, a two-layer catalyst concept is proposed in the form of an additional layer coating with high resistance to coke and suitable reactivity with methanol from NiO/MgAl2O4 to 10% on 0.3CoFe2O4-0.4ZrO2 layer. Optimization of various parameters using the concept of double-layer oxygen carrier showed that the use of 20% nickel concentration with a reduction time of 11 minutes increased the yield of H2 with 100% purity, which increased by 42% in the double-layer arrangement compared to the single-layer state, and it is a promising result for the concept of bi-layer oxygen carrier in this process.

The objective of this research was to explore targeted drug delivery of ibuprofen, a nonsteroidal anti-inflammatory drug, in order to minimize its side effects for patients requiring long-term and continuous use. To achieve this, a ZnO/NiO nanocomposite was synthesized as a carrier for the drug using a simple co-precipitation method. The structural and morphological properties of the nanocomposite were analyzed using XRD, SEM, and EDS techniques, revealing an average diameter of approximately 65 nm. Subsequently, ibuprofen was successfully loaded onto the nanocomposite with the assistance of mint extract as a covering agent. The presence of ibuprofen in the prepared drug-composite sample was confirmed by FT-IR analysis. In vitro investigations were conducted to determine the release of the loaded drug from the brush nanocomposite, which was found to be 20.4%. This research introduces a new green nanostructure in the drug delivery process.

In this research, a nano polymer was fabricated via the molecular imprinted polymer (MINP) method to transport and control the release of the drug eptifibatide. N-isopropyl acrylamide (NIPAAM), N-vinylidene (NVP), and EGDMA have been used as a temperature-sensitive monomers and cross-linker, respectively. Moreover, by changing the percentage composition of monomers, the drug’s potential adsorption, and temperature sensitivity were evaluated and optimized. The sample was examined and confirmed using nuclear magnetic resonance (1HNMR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), scanning electron microscope (SEM), and Dynamic light scattering (DLS).The results related to the in vitro drug eptifibatide demonstrated that the optimization of the nanopolymer composition percentage (MINP4) with has a direct impact on some characteristics such as proper response to ambient temperature, the ability to control response time, adequate size, critical dissolution temperature (LCST), and hydrophilicity of the polymer network. Therefore, due to increasing the half-life of eptifibatide, it could be a suitable carrier to deliver the drug molecules to the desired tissue. also, target selection, mastery of drug distribution control, and sensitivity to temperature are the main factors to enhance the efficiency of nano polymer for drug delivery.

In recent years, numerous efforts have been made to synthesize new hole-transporting materials for perovskite solar cells with the aim of replacing spiro-OMeTAD. However, to improve the conductivity and mobility of these materials, chemical additives are mostly used, which not only increase the cost but also reduce the stability and efficiency of perovskite solar cells in the long term due to the moisture sensitivity of perovskite crystals. Therefore, small organic molecules 2 and 6 were synthesized using cost-effective raw materials to improve the synthesis route, solubility and morphology on the perovskite surface compared to spiro-OMeTAD for additive-free hole transport materials. The chemical properties, purity, and identification of these molecules were confirmed using electrochemical methods, UV-Vis spectroscopy, and NMR spectroscopy. Due to the donor-acceptor type π-system, the molecules used increase the charge transfer mobility and thus reduce the use of chemical additives. The photovoltaic parameters of the solar cell made from hole transport material 2 and 6 were determined by photovoltaic analysis, and the results showed that the performance of hole-transporting layer 6 was almost the same as of spiro-OMeTAD in additive-free conditions, with a current density of 14.68 mA/cm², an open-circuit voltage of 0.82 V, a fill factor of 0.65, and a power conversion efficiency of 7.88%.

The mixture of TiO2-Al-C with stoichiometric ratio was prepared then ball milling process was done in a planetary ball mill in different times. The evidence of a chemical reaction was not detected in the 1 h milled sample however, the sign of an exothermic peak was detected at ~690ºC in the DTA results for this mixture. The XRD results of the as-milled samples indicated that the chemical reaction progresses as MSR model in the mixture with stoichiometric ratio. The decreasing of the particles size and the traces of amorphization were observed after increasing the milling time to 7 hours. The products of rection (i.e., Al2O3 and TiC) were well crystallized after isothermal heating of the 5 h milled sample at 1000 ºC for 1 h under argon atmosphere. The signs of these phases were also observed in the XRD patterns of the solid residues after DTA analysis. The evolution of the microstructures indicated the decreasing in the particle size due to ball milling and the change of morphology of the microstructure due to occurrence of chemical reaction. The assessments of the lattice parameter of the TiC in the final products indicated that the lattice parameter changes and reaches to amount of the stoichiometric composition due to isothermal heating. Thermodynamics assessments were done for the mixture of TiO2-Al-C and the feasibility of the reactions was studied using HSC thermodynamics software. The XRD results of the milled and the isothermally heated samples were accordance with the thermodynamics assessments.

In this research, nylon 6 nanofiber/chitosan nanoparticles (CS/N6NFs) adsorbent was fabricated by combining electrospinning and electrospraying methods. First, the nylon 6 nanofibrous substrate was made by electrospinning method, and then chitosan nanoparticles were electrosprayed on this substrate to make a adsorbent. The adsorbent was characterized by, field emission scanning electron microscopy (FESEM), contact angle and tensile test. FESEM studies showed that chitosan nanoparticles are uniformly distributed on the surface of nylon 6 electrospun nanofibers and are well connected to the fibers. The production of chitosan nanoparticles by electrospraying showed an almost uniform particle size distribution with an average size of about 110 nm. The role of chitosan in improving wettability was observed by reducing the contact angle from 64.06 to 53.80. Young's modulus values were obtained for N6NFs and Cs/N6NFs equal to 4.82 and 5.28 MPa, respectively. The performance of Cs/N6NFs adsorbent in removing acid red 8 (AR8) dye from aqueous solutions was investigated. Experiments showed that the value of 0.015 g of Cs/N6NFs adsorbent has the ability to remove more than 95% of AR8. Adsorption tests in batch mode indicate that the adsorbent designed to absorb AR8 after 5 times of reduction by NaOH still has a high absorption efficiency of 70%. The adsorption capacity of the adsorbent was calculated to be 195.16 mg.g-1 for AR8. The Langmuir model had a good fit with the experimental data of the adsorption isotherm. Kinetic studies showed that the adsorption data followed a pseudo-quadratic model.

In this paper, by combining ultraviolet spectroscopy and Chemometrics method, the acid dissociation constant of 4- (2-thiazole azo) rososinol was measured. The absorption spectra of the 4- (2-thiazole azo) rososinol solution have a large spectral overlap, so it will be difficult to determine its acid dissociation constant using conventional spectroscopy. Using ultraviolet-visible spectroscopy and two rank annihilation factor analysis (TRAFA), acid constants, number of species, molar fraction, relative standard deviation (RSD) and net species spectrum acid dissociation of 4- (2-thiazole azo) rososinol in 20 to 80% v/v of acetonitrile in water and dioxane in water was calculated. The results obtained by the two rank annihilation factor analysis method show the efficiency of this method in determining the solution with high spectral overlap. As the percentage of solvents increases, the acid constant becomes smaller, which can be explained by the fact that the solubility and dielectric constant of water, acetonitrile and dioxane are different. The value of these variables depends on the physical parameters (dielectric constant and induction number).

In this study, a simple and efficient online preconcentration method based on headspace in-tube microextraction was used to simultaneously extract and preconcentrate small amounts of six trichlorophenols in aqueous samples. After extraction, the analytes were quantified by capillary electrophoresis and using the calibration curve of standard solutions. The effect of effective factors on the extraction process such as the pH of the donor phase, the type of the acceptor phase, the temperature and time of extraction, and the addition of organic solvent to the donor phase were investigated and optimized. Under optimal conditions, the linear dynamic range for the proposed technique was 15 to 1000 nM with a correlation coefficient of 0.99, and relative standard deviations were obtained with seven repetitions of the experiment and a concentration of 500 nM of analytes in the range of 4.78-7.63%. The detection limit of the method was 5-6 nM. The preconcentration factor for six trichlorophenols was obtained in the range of 310 to 661 times. Finally, this method was used to preconcentrate and measure six trichlorophenols in environmental water samples. The relative recoveries for the spiked samples were within the 82-92% range, indicating good accuracies and the absence of matrix effects.

Pyrazolophthalazines and their derivatives are known as a substance with diverse chemical and biological activity. These compounds have various medicinal properties such as anti-bacterial, anti-viral, anti-coagulant and anti-cancer. In this research synthesis of Pyrazolo-phthalazine derivatives by reaction of aromatic aldehyde derivatives, Phthalic hydrazide and malononitrile in the presence of Hercynite as nano-catalyst were studied and the products were obtained in 45-90 minutes with yield of 90-97%. The structure of Hercynite nanocatalyst was investigated using FT-IR and SEM methods and X-ray diffraction pattern. The results of the morphology of the nanocatalyst surface show that the nanoparticles are spherical and the size of the particles is between 49-80 nm. Investigating the magnetic property of the catalyst with VSM analysis shows the favorable magnetic property of Hercynite nanocatalyst for its separation with an external magnetic field. Easy operation, high efficiency, reuse of the catalyst for several times, short reaction time and easy separation of the catalyst using an external magnet are the most important advantages of the presented method.

In this study, the electrocatalytic activity of the functionalized graphene oxide (GO) using L-lysine (GO-Lys) as well as L-lysine and copper (GO-Lys-Cu) was investigated for oxygen and hydrogen evolution reactions. Identification and characterization of GO, GO-Lys and GO-Lys-Cu were done using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, field emission scanning electron microscopy (FESEM) and elemental mapping images. Also, electrochemical impedance spectroscopy (EIS) and linear sweep voltammetry (LSV) were used to investigate the electrochemical properties and electrocatalytic activities. The obtained results not only confirmed the decoration of the GO surface by Lys and Lys-Cu, but also revealed the reduction of graphene oxide (rGO) sheets. EIS results confirmed the lowest charge transfer resistance for Lys-rGO hybrid nanocomposite compared to other synthesized samples. The results obtained of LSV show that the functionalization of GO with Lys-Cu leads to efficient and stable electrocatalytic activity for the oxygen evolution reaction (OER) and hydrogen evolution reaction (HER) with the lowest overpotential (375 and 732 mV, respectively) at the current density of 10 mA/cm2 (1 M KOH) and the smallest Tafel slope is 346 and 160 mV/dec, respectively, compared to GO, L-Lys, GO-Lys and Lys-Cu samples.

MIL-101(Cr) stands as one of the extensively researched chromium-based metal–organic frameworks, comprised of chromium metal ions and terephthalic acid ligands. This study introduces an innovative approach to MIL-101(Cr) synthesis by employing ultrasound (UTS) irradiation. Our primary objective revolved around optimizing key operational parameters, namely time and temperature, using the central composite design method. Subsequently, we conducted an in-depth analysis using variance analysis to understand their respective impacts. To predict process behaviour, we developed quadratic equations under varying conditions, achieving a remarkable R2 value of 0.9998 to relate parameters and synthesis yield. Results revealed a more pronounced influence of time variation compared to temperature on the synthesis process. Moreover, we subjected the synthesized MIL-101(Cr) to rigorous characterization using FT-IR, XRD, SEM, TGA, and N2 physisorption techniques. Our findings showcased the synthesized MIL-101(Cr) possessing exceptional characteristics, including an ultra-high specific surface area (2143 m2. g-1), substantial pore size (0.8 cm3.g-1), and excellent thermal, chemical, and water stability. Further examination indicated the presence of microporous windows, mesoporous cages, and uniform octahedral particles ranging in size between 125-260 nm.Notably, our study emphasized the energy efficiency of UTS irradiation over conventional electric (CE) heating, highlighting its potential as a quicker, more efficient, and environmentally friendly alternative to conventional synthesis methods.

The cholinergic hypothesis is one of the hypotheses of Alzheimer's disease that shows the relationship between the onset and progression of the disease. One of the main ways to increase the level of acetylcholine is to inhibit cholinesterase enzymes. The benzimidazole core is very important in medicinal chemistry research due to its high affinity to various enzymes and protein receptors. The present study was conducted in the synthesis of benzimidazole derivatives with the aim of investigating butyrylcholinesterase (BuChE) and acetylcholinesterase (AChE) inhibitory activity. In the first step of experimental study, the product 2-(chloromethyl)benzimidazole (2) was obtained, then the final three benzimidazole derivatives 3, 4, and 5 were synthesized from the reaction of 1 mmol 2-(Chloromethyl)benzimidazole and 1 mmol of piperazine, N-phenylpiperazine, and 2-phenylethan-1-amine, respectively. The structure of the prepared compounds was confirmed by 1H-NMR, 13C-NMR, and FT-IR spectroscopic methods. The ability of the compounds to inhibit AChE and BuChE was evaluated using Ellman’s assay. The results of this test showed the significant inhibitory activities of these compounds. Compound 5 with IC50 = 0.28 µM showed the highest inhibition against BuChE enzyme. The inhibitory activity of compound 5 against BuChE was better than donepezil. In addition, the interaction of compound 5, galantamine, and rivastigmine with BuChE enzyme was investigated using docking studies. In these studies, compound 5 with an energy value of -8.88 kcal/mol showed the best interaction with the active site of the receptor. According to the obtained results, compound 5 is the most promising compound for the development of benzimidazole derivatives against Alzheimer's disease.

Sulfonamide compounds with functional group -SO2NH- show a wide range of biological activities and medicinal properties. The synthesis of sulfonamides has been of interest to medicinal chemists for a long time. In this article, the selective acylation of sulfanilamide with acetic anhydride was carried out using some catalysts with Lewis acid properties. In this research, the one-pot selective method of N-acylation of -SO2NH2 group in sulfanilamide molecule using stannous oxide nanoparticles as an efficient recyclable catalyst has been used. In this method, THF was replaced with expensive toxic amine solvents. The acylated product was identified by FTIR, 1HNMR, 13CNMR and MASS spectra. The best results with 85% efficiency, 95% selectivity were obtained using stannous oxide nanoparticles as catalyst (0.5 g) in tetrahydrofuran as solvent, at 60°C in 60 minutes. The catalyst was recycled three times and maintained its efficiency. Using this method is completely green and has economic and environmental benefits.

Moringa plant with the scientific name Moringa oleifera L. has important medicinal chemical compounds including flavonoids, which have antioxidant and anticancer properties. In this research, the properties of metal nanoparticles such as Iron, Copper, Zinc and Silver biosynthesized from the aqueous extract of M. oleifera plant have been studied, and then the antioxidant and antibacterial properties of the aqueous extract obtained from the aerial parts of this plant and the nanoparticles have been studied. The resulting metal was treated. The size and structure of metal nanoparticles obtained from Moringa plant aqueous extract were confirmed by scanning electron microscope (SEM) and X-ray diffraction (XRD), respectively. The amount of antioxidant activity was measured using the DPPH method and the antibacterial properties of Moringa plant aqueous extract and metal nanoparticles obtained from it were measured with the help of disk diffusion and MIC method on two types of bacteria E. coli and S. aureus. The highest amount of antioxidant activity (89.23%) was related to copper nanoparticles at a concentration of 500 μg/ml. As well as E. coli bacteria were more sensitive than S. aureus to the same concentrations of the used treatments and had bigger inhibition zone. Additionally, the diameter of the inhibition zone (in millimeters) was also dependent on the concentration and grew with increasing concentration. The use of copper nanoparticles (especially in higher concentrations) has more antibacterial properties. In terms of survival rate and growth of cultured bacteria using the MIC method, the IC50 of E. coli bacteria compared to S. aureus bacteria in equal concentrations to the applied treatments was low, and the results demonstrated the high sensitivity of E. coli bacteria strain to S. aureus bacteria. According to the obtained results, a significant difference was observed between the aqueous extract obtained from the M. oleifera plant and the metal nanoparticles biosynthesized from it in terms of antioxidant and anticancer activity.

Gemcitabine (Gem), as a nucleoside analog, is chemotherapy agent for breast, bladder, and pancreatic cancers. Nanoparticles can cause fewer unwanted side effects by improving the accumulation of drugs in the target tissue. The present study aimed to develop and optimize Gem-MSLNs, gemcitabine-loaded magnetic solid lipid nanoparticles, to minimizing undesired side effects. Gem-MSLNs were synthesized by emulsification and solvent evaporation methods. A definitive screening design was used to optimize the formulation of Gem-MSLNs. Particle size, zeta potential, and the entrapment efficiency of Gem-MSLNs were examined as responses. Characterizing and assessing the optimized Gem-MSLNs was done. The optimal formulation for Gem-MSLNs had a particle size of 96.50 ± 4.36 nm, zeta potential of +72.1 ± 0.3 mV, and an entrapment efficiency of 21.10 ± 2.12%. These results show that the Gem-MSLNs have good colloidal stability in an aqueous environment, which preventing aggregation during the experimentation processes. Gem-MSLNs are hence excellent options for upcoming therapeutic uses.

In this research, carbon dots with high luminescence intensity were synthesized using pumpkin seed shell as a new and green source with hydrothermal method. The prepared carbon dots were characterized using X-ray diffraction, Fourier transform infrared spectroscopy and Scanning electron microscopy. The average size of the synthesized carbon dots was estimated about 59 nm. In addition, the luminescence property of the synthesized carbon dots was evaluated using photoluminescence analysis and according to their high luminescence property at excitation wavelength of 340 nm and emission wavelength of 425 nm, they were used as nanosensor for the determination of L-cysteine. By addition of L-cysteine, the emission intensity of carbon dots solution was reduced. In order to enhancement of the method sensitivity, the effective parameters on the quenching intensity of L-cysteine such as pH, interaction time and environment ionic strength were examined and optimized. Under the laboratory optimum conditions, linear range of 5-500 µM, limit of detection of 1.0 µM and relative standard deviation (at 10 µM of L-cysteine) of 3% was obtained. The accuracy of the proposed method was evaluated using spiking procedure and according to the recoveries percent (96-102), the proposed method is a reliable method for determination of L-cysteine in the examined samples. Finally, the prepared nanosensor was successfully used for the determination of L-cysteine in tap water samples.