نشریه شیمی کاربردی روز
پیاپی 69 (Winter 2024)

A novel, bis-salophen schiff base ligand anchored magnetic Fe3O4@SiO2 nanoparticles was prepared and applied for removal of Cu(II) from aqueous solutions. The obtained Fe3O4@SiO2/Schiff base MNPs was characterized by fourier transform infrared (FT-IR), X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray analysis (EDX) and vibration sample magnetometry (VSM). Then, the adsorption activity for copper ions was studied by nonmagnetic, in terms of effect of adsorbent dosage on the adsorption and kinetics behavior. Furthermore, the adsorption and regeneration experiment showed there was about 5% loss in the adsorption capacity of the prepared Fe3O4@SiO2/Schiff base MNPs for copper ions after 6 times reuse. Finally, our results suggested that the Fe3O4@SiO2/Schiff base composites have a great potential to be employed for treatment of wastewater containing Cu(II).

Herein, SnO2-NiO nanocomposite was prepared via a hydrothermal method and characterized by various techniques consisting X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and energy-dispersive X-ray spectroscopy (EDS). The FESEM image showed particles with the size at about 20–130 nm in diameters. The electrochemical oxidation of hydrochlorothiazide (HCTZ) at a carbon paste electrode modified with SnO2-NiO nanocomposite and an ionic liquid (1-butyl-3-methylimidazolium hexafluorophosphate (BMIM-PF6)) (SnO2-NiO/IL/CPE) was evaluated in phosphate buffer (PB) pH 8, by using cyclic voltammetry, linear sweep voltammetry, differential pulse voltammetry and chronoamperometry. The SnO2-NiO/IL/CPE indicated a good electrocatalytic behavior towards to oxidation of hydrochlorothiazide. The anodic peak currents were increased with the HCTZ concentration and indicated two linear dynamic range from 0.01 to 0.1 µM and 0.1 to 100 µM and a detection limit of 0.002 µM (S/N = 5) under the optimized conditions. The introduced electrochemical sensor was utilized for the determination of HCTZ in the pharmaceutical formulations and biological sample.

In this study CO2 absorption into aqueous droplets of N-methyl-diethanolamine (MDEA) in water-in-oil (w/o) and oil-in-water (o/w) emulsions were investigated in batch-stirred reactor at 298 K and different CO2 partial pressure in the range of 0.1-0.5 bar. The effects of the aqueous phase concentration, emulsion type, CO2 partial pressure and the amount of piperazine as a promoter on absorption percentage and loading amount of CO2 (mole of absorbed CO2/mole of amines) were studied. All microemulsion samples were prepared by titration method. The CO2 loading amounts of all experiments were calculated and the results showed that water in oil samples have better absorption performance and higher CO2 loading values. The loading values in samples were improved in both emulsion types with increasing CO2 partial pressure. The results also showed that in water-in-oil samples with different concentrations of piperazine or MDEA, CO2 absorption and loading improves with increasing amine concentration.

In this study, an attempt was made to synthesize a new sorbent based on the second generation of silica coated magnetic poly(amidoamine) (Fe3O4@SiO2@PAMAM) to improve the performance of magnetic solid phase extraction (MSPE) of some antifungal drugs including miconazole, clotrimazole and ticonazole in various real samples such as urine and human plasma. The extracted analytes were measured by high performance liquid chromatography equipped with ultraviolet detection (HPLC-UV). Field emission-scanning electron microscopy (FE-SEM), X-ray diffraction analysis (XRD), Thermogravimetric analysis (TGA), Transmission electron microscopy (TEM) and Fourier transform-infrared spectroscopy (FT-IR) were used to study the morphology and structure of the prepared sorbent. The various factors such as: extraction time, sorbent amount, solvent desorption volume, desorption time, ionic strength and pH were studied and optimized. The method is validated according to ICH guidelines with respect to precision, accuracy, linearity, specificity, robustness, and limits of detection and quantification. Under the optimized condition, the linearity of the method was in the range of 1–500 µg L-1 (miconazole= 1-200 µg L-1, clotrimazole = 1-500 µg L-1 and ticonazole = 1-200 µg L-1). The obtained correlation coefficients (r^2) were between 0.9871-0.9977. The limits of detection (LODs) were also calculated to be 0.14-0.18 µg L-1 (miconazole= 0.16 µg L-1, clotrimazole = 0.18 µg L-1 and ticonazole=0.14 µg L-1). The limits of quantification (LOQs) were also in the range of 0.46-0.60 µg L-1 for the selected analytes. The relative standard deviations (RSDs%), were obtained in the range of 4.6 to 5.9%. Moreover, the calculated enrichment factors were between 85 and 93. The proposed method was also employed for the analysis of various real samples such as urine and plasma samples. The obtained recoveries indicated that the method was useful and applicable in complicated real samples

Graphene oxide nanosheets (GONs) are ideally suited for implementation in electrochemical applications due to their large electrical conductivity, large surface area and low production costs. In this research, electrochemical exfoliated graphene oxide-modified graphite electrode was developed for voltammetric determination of clozapine (CLZ). The dependence of oxidation peak current on the pH of the solution, scan rate and concentration of analyte were studied to optimize the experimental conditions for electrochemical determination of CLZ. The experimental results suggested that the modified electrode promoted electron transfer reaction for the oxidation of CLZ. The modified electrode exhibited high effective surface area, more reactive sites and excellent electrocatalytic activity toward the oxidation of CLZ. In the concentration range of 0.75–100 µM of CLZ in citrate buffer solution (CBS, pH 6), the anodic peak currents, measured via differential pulse voltammetry (DPV), presented good linear relationship with limit of detection (LOD) of 2.15 nM and good sensitivity of 0.0477 µA µM−1. The proposed method was successfully applied to quantify the amount of CLZ in the blood serum and plasma of schizophrenia patient.

In analytical chemistry, the use of the simplest tool that provides the possibility of on-site measurement, low cost, and simple equipment has always been an area of interest for researchers. In recent years, the use of smartphones as an available tool can have these features. In this study, Bi2O3/ZnO/Pd adsorbent was used for preconcentration and measurement of Sudan IV color as one of the azo family colors in food and water samples, exploiting ultrasonic-assisted dispersive micro solid phase extraction (UA-d-μ-SPE) method along with a smartphone. The structure of this adsorbent was examined by XRD, SEM, and EDS analyses. Factors such as the amount of adsorbent (5.1 mg), sample solution pH (7.1), washing solvent volume (430.0 μL), and adsorption time (65 seconds) were optimized, utilizing central composite design (CCD) method. The type of washing solvent (methanol) and desorption time (45 seconds) were also optimized using the one-parameter-at-a-time method. In the best conditions, the limit of detection (LOD) was 5.58 ng mL-1, and the linear detection range (LDR) for this color was 20-1100 ng mL-1. The enrichment factor (EF) was also computed as 22.87. In addition, the relative standard deviation (RSD%) was acquired as 3.91 with n=5.

One of the biggest challenges to the expansion of photochemical processes has been the creation of effective visible light photocatalysts for organic synthesis. Heterogeneous photocatalysts present a favorable procedure to realize green and eco-friendly organic reactions. we fabricated the heterogenous catalyst CuFe2O4/CuO-rGO@EosinY (EY) by immobilizing eosin on the substrate CuFe2O4/CuO-rGO. The substrate of eosin was fabricated from the calcination of basil seed hydrogel (BSH) impregnated with copper and iron. The prepared heterogeneous catalyst as photocatalyst was applied in a green one-pot multi-component protocol for the production of biologically important xanthene derivatives via condensation of aromatic aldehydes and dimedone under the condition of visible light irradiation. The synthesized photocatalyst was characterized using various techniques such as FT-IR, XRD, and TGA. The significant advantages of the present methodology include remarkable yield, cost-effectiveness, easy work-up, broad substrate scope, and significant reusability. The prepared catalyst was used four times without a significant decrease in reaction efficiency.

This study presents an innovative approach to eliminating the pharmaceutical pollutant diclofenac sodium (DFS) by combining nanofiltration membrane technology with an electrochemical oxidation process. The nanofiltration membrane was prepared by phase inversion, and modified with cetyltrimethylammonium chloride (CTAC) to improve surface properties and pore structure. The concentrate from the nanofiltration treatment has been utilized as the input feed for the electrochemical section, employing Ti/SnO2-α-Fe2O3 electrodes. The PES/CTAC membrane exhibits a more uniform and stable pore structure, leading to increased permeability and antifouling properties. Additionally, the inclusion of CTAC through the surface adsorption mechanism improved the DFS rejection performance, achieving a maximum rejection rate of 65.2% for the membrane with a composition of 0.1 wt% CTAC. The obtained results show that the titanium electrode coated with SnO2 and α-Fe2O3 nanoparticles removed the DFS pollutant by 56%. In total, both membrane and electrochemical process removed 80.5% of the primary Diclofenac pollutant. According to the low energy consumption of this process (EEC=0.014144 US$/m3) and other results, the combination of the PES/CTAC membrane and Ti/SnO2-α-Fe2O3 electrode is an efficient method for diclofenac sodium pollutant removal.