Photodegradation of orange II dye using p-n junction NiO/TiO2 composite,and assessment of its biological activities

The chemical reduction method was used to synthesize nickel oxide particles (NiO) and NiO supported on titanium dioxide (NiO/TiO₂ nanocomposite). The composites were characterized through scanning electron microscopy (SEM), energy dispersive X-ray (EDX), X-ray diffraction (XRD) and Fourier transform infrared (FTIR) analysis. The morphological investigation showed that pseudocubic NiO are present in dispersed as well as agglomerated forms. Whereas NiO particles (<200 nm) are evenly deposited over the surface of TiO₂ in NiO/TiO₂ composite. The formation of NiO and NiO/TiO₂ was also verified by XRD analysis. The synthesized NiO and NiO/TiO₂ were used as photocatalysts for the degradation of Orange II (OII) dye. According to the degradation investigation, both NiO and NiO/TiO₂ composite degraded OII dye more efficiently when exposed to UV light. The results indicated that NiO degraded 93% and NiO/TiO₂ composites degraded approximately 96% of OII dye within 30 min. Both photocatalysts are highly sustainable and have significant OII dye degradation recyclability. Moreover, NiO and NiO/TiO₂ exhibited promising bioactivities (antioxidant activity of 80%) against the pathogenic bacteria Citrobacter and Providencia, which is comparable with the standard ascorbic acid (88%).     

Effect of hydrogen reduction temperature on the microstructure and magnetic properties of Fe–Ni powders

The effect of hydrogen reduction temperature on the properties of Fe–Ni powders was described. The mixed powders of Fe-oxide and NiO were prepared by chemical solution mixing of nitrates powders and calcination at 350 °C for 2 h in air. The calcined powders formed small agglomeration with an average particle size of 100 nm. The microstructure and magnetic properties were investigated by using X-ray diffractometry, thermogravimetry, differential thermal analyzer, and vibrating sample magnetometer. Microstructure and thermal analysis revealed that the Fe-oxide and NiO phase were changed to FeNi₃ phase in the temperature range of 245–310 °C, and by heat-up to 690 °C the FeNi₃ phase was transformed to γ-FeNi phase. The reduced powder at 350 °C showed saturation magnetization of 76.3 emu/g and coercivity of 205.5 Oe, while the reduced powders at 690 °C exhibited saturation magnetization of 84.0 emu/g and coercivity of 14.0 Oe. The change of magnetic properties was discussed by the observed microstructural features.

     

Preparation and adsorption performance of a NiO/MgF2 composite adsorbent

Fluoride adsorbents have been applied for the purification of UF₆ product from fluorination process. A MgF₂-based adsorbent, NiO/MgF₂, was prepared using NiF₂ as doping agent. The specific surface area of NiO/MgF₂ was 5 times larger than that of MgF₂, its porosity was also larger than that of MgF₂. The saturated adsorption capacity of NiO/MgF₂ for MoF₆ was 21.4?±?1.9 mg g^?1. The desorption behavior was examined by thermogravimetric analysis (TG). The NiO/MgF₂ with adsorbed MoF₆ was investigated using extended X-ray absorption fine structure spectroscopy (EXAFS), which showed no bonding interactions between NiO and MoF₆, while the adsorption of MoF₆ on NiO/MgF₂ was chemisorption via a Mo–F–Mg bond.

     

Direct synthesis of porous NiO nanowall arrays on conductive substrates for supercapacitor application

Porous NiO nanowall arrays (NWAs) grown on flexible Fe-Co-Ni alloy have been successfully synthesized by using nullaginite (Ni₂(OH)₂CO₃) as precursor and investigated as supercapacitor electrodes. In details, we adopted a simple hydrothermal method to realize Ni₂(OH)₂CO₃ NWAs and examined their robust mechanical adhesion to substrate via a long-time ultrasonication test. Porous NiO NWAs were then obtained by a post-calcination towards precursors at 500 °C in nitrogen atmosphere. Electrochemical properties of as-synthesized NiO NWAs were evaluated by cyclic voltammetry and galvanostatic charge/discharge; porous NiO NWAs electrode delivered a specific capacitance of 270 F/g (0.67 A/g); even at high current densities, the electrode could still deliver a high capacitance up to 236 F/g (13.35 A/g). Meanwhile, it exhibited excellent cycle lifetime with ∼93% specific capacitance kept after 4000 cycles. These results suggest that as-made porous NiO NWAs electrode is a promising candidate for future thin-film supercapacitors and other microelectronic systems.     

Preparation of thiazolidin-4-one derivatives using ZnO–NiO–NiFe2O4 nano-composite system

The hydrothermal synthesis of ZnO–NiO–NiFe₂O₄ nano-composite is reported. The sample was utilized to characterize via XRD, FE-SEM, EDS, FT-IR, UV–Vis, and BET techniques. The sample consisted of three different phases as ZnO (hexagonal), NiO (cubic), and NiFe₂O₄ (cubic) with the average particle size as 34 nm and specific surface area, average pore diameter, and pore volume as 64.35 m² g^?1, 13.02 nm, and 0.201 cm³ g^?1, respectively. Catalytic behavior of the nano-composite was investigated on the synthesis of thiazolidin-4-one derivatives under thermal and ultrasonic irradiation condition. Our results show that the catalytic activity of ZnO–NiO–NiFe₂O₄ nano-composite is much higher than ZnO, NiO, and NiFe₂O₄ metal oxides. All products were prepared in high yields with short reaction times. In addition, the catalyst was recovered for at least five times.

     

Biogenic Synthesis of NiO Nanoparticles Using Areca catechu Leaf Extract and Their Antidiabetic and Cytotoxic Effects

Nanoworld is an attractive sphere with the potential to explore novel nanomaterials with valuable applications in medicinal science. Herein, we report an efficient and ecofriendly approach for the synthesis of Nickel oxide nanoparticles (NiO NPs) via a solution combustion method using Areca catechu leaf extract. As-prepared NiO NPs were characterized using various analytical tools such as powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and UV-Visible spectroscopy (UV-Vis). XRD analysis illustrates that synthesized NiO NPs are hexagonal structured crystallites with an average size of 5.46 nm and a hexagonal-shaped morphology with slight agglomeration. The morphology, size, and shape of the obtained material was further confirmed using SEM and TEM analysis. In addition, as-prepared NiO NPs have shown potential antidiabetic and anticancer properties. Our results suggest that the inhibition of α-amylase enzyme with IC 50 value 268.13 µg/mL may be one of the feasible ways through which the NiO NPs exert their hypoglycemic effect. Furthermore, cytotoxic activity performed using NiO NPs exhibited against human lung cancer cell line (A549) proved that the prepared NiO NPs have significant anticancer activity with 93.349 μg/mL at 50% inhibition concentration. The biological assay results revealed that NiO NPs exhibited significant cytotoxicity against human lung cancer cell line (A549) in a dose-dependent manner from 0–100 μg/mL, showing considerable cell viability. Further, the systematic approach deliberates the NiO NPs as a function of phenolic extracts of A. catechu with vast potential for many biological and biomedical applications.     

Novel visible-light-driven photocatalyst of NiO/Cd/g-C3N4 for enhanced degradation of methylene blue

Novel NiO/Cd/g-C₃N₄ photocatalysts were synthesized using a green and straightforward microwave-assisted method and characterized by X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), the Brunauer–Emmett–Teller (BET) method, transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and ultraviolet–visible spectroscopy (UV–Vis). The ternary NiO/Cd/g-C₃N₄ nanocomposites were evaluated for the degradation of methylene blue (MB) at room temperature under the visible light irradiation. Experimental results revealed that the weight percent of cadmium had a remarkable effect on the photodegradation efficiency. The NiO/Cd/g-C₃N₄ (0.1%) sample exhibited superior activity in the degradation reaction. The activity of this nanocomposite was about 4.5 and 3.25 fold higher than those of the pure g-C₃N₄ and NiO/g-C₃N₄ samples in the degradation of MB, respectively. The enhanced photocatalytic activity was attributed to the low energy gap, increased absorption capacity of the visible light, and efficient suppression of the recombination of photogenerated electron-hole pairs. A detailed photocatalytic mechanism over the nanocomposite of NiO/Cd/g-C₃N₄ (0.1%) was proposed with superoxide radical anion O₂^– as the main reactive species. The stability of the nanocomposite was confirmed after four consecutive runs as well.     

Highly efficient sorption of U(VI) from aqueous solution using amino/amine-functionalized magnetic mesoporous silica nanospheres

The amino/amine-functionalized magnetic mesoporous silica nanospheres (MSN-DETA) exhibited relatively high sorption capacity (q_m?=?153.68 mg/g) as well as excellent selectivity for U(VI). The U4f_7/2 X-ray photoelectron spectrometry revealed two binding energies at 380.8?±?0.3 eV (with the proportion of 75.2%) and 382.3?±?0.3 eV, which indicated the inner-surface complexation mechanism. The sorption isotherms fitted well with the Langmuir model, whereas the sorption kinetics could be fitted by pseudo-second-order model. The U(VI)-loaded MSN-DETA could be efficiently regenerated by acidified EDTA (0.4 M). These findings indicated that MSN-DETA could be used as a potential material for the efficient sorption/separation of U(VI) from wastewater.

     

Improved pechini sol-gel fabrication of Li2B4O7/NiO/Ni3(BO3)2 nanocomposites to advanced photocatalytic performance

In current research, nano-scaled Li₂B₄O₇/NiO/Ni₃(BO₃)₂ (LiBNi) composites were fabricated through improved pechini sol–gel method for advanced photocatalytic applications to remove dye contaminations of drinking water under UV/Visible irradiation. To optimize LiBNi nanocomposites properties, different complexing agents including ethylenediaminetetraacetic acid (EDTA), citric acid, tannic acid, tartaric acid and phthalic acid were utilized in pechini sol–gel process. Various sizes and morphologies of Li₂B₄O₇/NiO/Ni₃(BO₃)₂ nanocomposites obtained that were characterized by SEM and TEM techniques. Also, to confirm crystalline and structural features of nano-sized LiBNi samples, analyses of X-ray diffraction (XRD), Fourier transform infrared (FT-IR) and energy dispersive X-ray (EDX) were performed. By consideration of UV–Vis data, band-gap of LiBNi nanocomposites premeditated is 3.35 eV. Moreover, photocatalytic degradation of Li₂B₄O₇/NiO/Ni₃(BO₃)₂ nanocomposites was examined via UV/visible waves in aqueous solution for degradation acid red 88 pollutant after 90 min. Some operative factors such as nanocatalyst concentration and irradiation type for optimized LiBNi nanocomposites were assessed for removal of drinking water contaminant.     

Honey-mediated synthesis of Cr2O3 nanoparticles and their potent anti-bacterial,anti-oxidant and anti-inflammatory activities

Green synthesis of nanoparticles has gained tremendous attention in recent era which is pertinent to their unique properties and broad applications. This approach is cost-effective, environment-friendly as well as highly biocompatible. In this research, chromium oxide nanoparticles (Cr₂O₃-NPs) were synthesized by using Apis mellifera honey as a reducing and capping agent and their anti-bacterial, anti-biofilm, anti-oxidant and anti-inflammatory abilities were explored. Ultra Violet-visible double beam spectroscopy revealed that chromium underwent d-d transition during synthesis of nanoparticles. X-ray diffraction (XRD) analysis verified that Cr₂O₃-NPs were crystalline in nature and average crystal size was 24 nm. Energy-dispersive X-ray (EDX) analysis confirmed that chromium and oxygen formed nano-composites in solution which possessed a stable form. Scanning electron microscopy (SEM) provided morphological characteristics of nanoparticles and proved that their average size was 20 nm. Cr₂O₃-NPs displayed excellent anti-bacterial activity (minimum inhibition zone, 20 mm; maximum inhibition zone, 26 mm) against 30 selected clinical isolates of Klebsiella pneumoniae as determined by agar well-diffusion method. Their antibacterial activity was considerably superior to that of three selected antibiotics including Gentamicin, Ciprofloxacin and Cefepime. However, no synergism was observed between nanoparticles and these antibiotics as calculated from fractional inhibitory concentration index (FICI) values all of which were  > 1. The synthesized nanoparticles possessed good biofilm inhibition potential (60 % to 73 %) at all concentrations (20 µg/ml to 50 µg/ml) tested. Cr₂O₃-NPs exhibited excellent anti-oxidant activity (IC₅₀ = 128 µg/ml) which was nearly equivalent to that of ascorbic acid. Anti-inflammatory effect of Cr₂O₃-NPs was also significant (IC₅₀ = 549 µg/ml) and comparable to that of standard. Both anti-oxidant and anti-inflammatory capacities were found to increase with an increase in the concentration of Cr₂O₃-NPs. In conclusion, this work revealed that Apis mellifera honey-mediated synthesis of Cr₂O₃-NPs could be investigated for future biomedical applications.     

Syngas production from pyrolysis–catalytic steam reforming of waste biomass in a continuous screw kiln reactor

A two-stage continuous screw-kiln reactor was investigated for the production of synthesis gas (syngas) from the pyrolysis of biomass in the form of waste wood and subsequent catalytic steam reforming of the pyrolysis oils and gases. Four nickel based catalysts; NiO/Al₂O₃, NiO/CeO₂/Al₂O₃, NiO/SiO₂ (prepared by an incipient wetness method) and another NiO/SiO₂ (prepared by a sol–gel method), were synthesized and used in the catalytic steam reforming process. Pyrolysis of the biomass at a rapid heating rate of approximately 40 °C/s, was carried out at a pyrolysis temperature of 500 °C and the second stage reforming of the evolved pyrolysis gases was carried out with a catalytic bed kept at a temperature of 760 °C. Gases were analysed using gas chromatography while the fresh and reacted catalyst was analysed by scanning electron microscopy, thermogravimetric analysis, transmission electron microscopy with energy dispersive X-ray and X-ray photoelectron spectroscopy. The reactor design was shown to be effective for the pyrolysis and catalytic steam reforming of biomass with a maximum syngas yield of 54.0 wt.% produced when the sol–gel prepared NiO/SiO₂ catalyst was used, which had the highest surface area of 765 m² g⁻¹. The maximum H₂ production of 44.4 vol.% was obtained when the NiO/Al₂O₃ catalyst was used.     

Nanoflower-like composites of ZnO/SiO2 synthesized using bamboo leaves ash as reusable photocatalyst

In this study, the synthesis of ZnO/SiO₂ nanocomposites using bamboo leaf ash (BLA) and tested their photocatalytic activity for rhodamine B decolorization have been conducted. The nanocomposites were prepared by the sol–gel reaction of zinc acetate dihydrate, which was used as a zinc oxide precursor, with silica gel obtained from the caustic extraction of BLA. The effect of the Zn content (5, 10, and 20 wt%) on the physicochemical characteristics and photocatalytic activity of the nanocomposites was investigated. The results of X-ray diffraction, scanning electron microscopy, gas sorption, and transmission electron microscopy characterization confirmed the mesoporous structure of the composites containing nanoflower-like ZnO (wurtzite) nanoparticles of 10–30 nm in size dispersed on the silica support. Further, the nanocomposites were confirmed to be composed of ZnO/SiO₂ by X-ray photoelectron spectroscopy analysis. Meanwhile, diffuse-reflectance UV–visible spectrophotometry analysis of the nanocomposites revealed band gap energies of 3.38–3.39 eV. Of the tested nanocomposites, that containing 10 wt% Zn exhibited the highest decolorization efficiency (99%) and fastest decolorization rate. In addition, the degradation efficiencies were not reduced significantly after five repeated runs, demonstrating the reusability of the nanocomposite catalysts. Therefore, the ZnO/SiO₂ nanocomposite obtained from BLA is a promising reusable photocatalyst for the degradation of dye-polluted water.     

Sustainable fabrication of silver-titania nanocomposites using goji berry (Lycium barbarum L.) fruit extract and their photocatalytic and antibacterial applications

Silver-titania nanocomposites (Ag-TiO₂ NCs) have unique functional attributes due to their photocatalytic and antibacterial properties. In this study, titania nanoparticles (TiO₂-NPs) were successfully in-situ decorated with silver nanoparticles (Ag-NPs) using the aqueous extract of goji berries (Lycium barbarum L.) as a bioreducing and stabilizing agent. Different Ag-TiO₂ NCs were synthesized by treating different concentrations of silver nitrate with a specific concentration of TiO₂-NPs in the presence of fruit extract. The green-synthesized NCs were characterized using several techniques viz., ultraviolet–visible spectrophotometry, X-ray diffractometry (XRD), scanning electron microscopy, field-emission transmission electron microscopy (FE-TEM), Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy. XRD analysis revealed the formation of face-centered cubic (fcc) crystals, and FE-TEM analysis revealed the embedment of Ag-NPs throughout the surface of TiO₂-NPs. The average size of Ag-NPs on TiO₂-NPs increased from 11.2 ± 3.05 nm to 16.4 ± 4.5 nm with an increase in the concentration of silver ions, and the morphology of Ag-NPs was predominantly quasi-spherical and hexagonal. These NCs exhibited an excellent photocatalytic degradation of an azo dye, methylene blue (MB). The synthesized Ag-TiO₂ NCs (3:1) showed higher photocatalytic degradation efficiency of ∼ 93.4% for MB in 130 min under visible light irradiation. Ag-TiO₂ NC_S also exhibited good antibacterial activities towards Staphylococcus aureus (Gram-positive) and Escherichia coli (Gram-negative). Therefore, the formation of Ag-NPs on the surface of TiO₂-NPs to form Ag-TiO₂ NCs exhibits eco-friendly photocatalytic degradation of azo dye contaminants as well as antibacterial activity.     

Facile synthesis and characterization of copper oxalate/cobalt oxalate/manganese oxalate and copper oxide/cobalt manganese oxide/manganese oxide as new nanocomposites for efficient photocatalytic degradation of malachite green dye

Scientists seek to synthesize new catalysts with simple methods to treat water pollution from organic dyes using photocatalytic degradation technology. In this technology, when light falls on the catalyst, the produced hydroxyl free radicals convert the dye into non-toxic gases such as CO₂ and H₂O. So, in this work, copper oxalate/cobalt oxalate/manganese oxalate (Abbreviated as P₁) and copper oxide/cobalt manganese oxide/manganese oxide (Abbreviated as P₂) new nanocomposites were fabricated via precipitation of Cu²⁺/Co²⁺/Mn²⁺ solution using oxalic acid and ignition of precipitate at 550 °C for 4 hrs, respectively. Some tools, involving X-ray diffraction (XRD), UV–vis spectrophotometer, energy dispersive X-ray spectroscopy (EDX), nitrogen gas sorption analyzer, transmission electron microscope (TEM), and field emission scanning electron microscope (FE-SEM), were used for characterizing the fabricated nanocomposites. The EDX spectra confirmed that the P₁ composite consist of C (26.28 %), oxygen (46.66 %), manganese (7.27 %), cobalt (7.59 %), and copper (12.20 %). Also, the P₂ composite consist of oxygen (8.23 %), manganese (31.34 %), cobalt (27.19 %), and copper (33.24 %). A transmission electron microscope shows that the P₁ and P₂ composites consist of polyhedral and spherical shapes with an average diameter of 28.13 and 14.37 nm, respectively. The BET surface area, average pore size, and total pore volume of the P₁ composite are 29.0725 m²/g, 2.0749 nm, and 0.0302 cc/g, respectively. Besides, the BET surface area, average pore size, and total pore volume of the P₂ composite are 58.1088 m²/g, 1.6087 nm, 0.0467 cc/g, respectively. 60 mg of the synthesized nanocomposites completely decompose 60 mL of 15 mg/L of malachite green dye solution within 20 min in the presence of hydrogen peroxide and UV light. The synthesized catalysts outperformed many other catalysts published in previous studies.     

Preconcentration and determination of boron in milk,infant formula,and honey samples by solid phase extraction-electrothermal atomic absorption spectrometry

This work presents alternative procedures for the electrothermal atomic absorption spectrometric determination of boron in milk, infant formulas, and honey samples. Honey samples (10% m/v) were diluted in a medium containing 1% v/v HNO₃ and 50% v/v H₂O₂ and introduced in the atomizer. A mixture of 20 µg Pd and 0.5 µg Mg was used for chemical modification. Calibration was carried out using aqueous solutions prepared in the same medium, in the presence of 10% m/v sucrose. The detection limit was 2 µg g^− 1, equivalent to three times the standard error of the estimate (s_y/x) of the regression line. For both infant formulas and milk samples, due to their very low boron content, we used a procedure based on preconcentration by solid phase extraction (Amberlite IRA 743), followed by elution with 2 mol L^− 1 hydrochloric acid. Detection limits were 0.03 µg g^− 1 for 4% m/v honey, 0.04 µg g^− 1 for 5% m/v infant formula and 0.08 µg mL^− 1 for 15% v/v cow milk. We confirmed the accuracy of the procedure by comparing the obtained results with those found via a comparable independent procedure, as well by the analysis of four certified reference materials.     

In situ growth of MnO2 on pDA-templated cotton fabric for degradation of formaldehyde

Degradation of formaldehyde (HCHO) in interior decoration has been an urgent issue due to its toxicity nature and potential threats to human health. In this work, manganese dioxide nanoparticles (MnO₂ NPs) were in situ grown on the polydopamine (pDA)-templated cotton fabrics for environmentally friendly HCHO degradation applications. The morphology, elemental composition, and crystal structure of the cotton/pDA/MnO₂ were characterized by scanning electron microscopy–energy dispersive X-ray spectrum, Fourier transform infrared, X-ray diffractometer and X-ray photoelectron spectroscopy, respectively. The degradation of HCHO by the as-developed cotton/pDA/MnO₂ was measured in a self-made quartz reactor, and the stability of adsorption was evaluated by cyclic experiments. The results showed that the HCHO removal efficiency reached to 100% within 20 min after three cycles, suggesting that the as-prepared fabrics exhibited good stability for the degradation of HCHO. The development of MnO₂ NPs coated fabrics provides new strategies in degradation HCHO in interior decoration.

     

Photo catalytic oxidation of TNT using TiO<Subscript>2</Subscript>-SiO<Subscript>2</Subscript> nano-composite aerogel catalyst prepared using sol–gel process

The degradation of nitro aromatics like trinitrotoluene (TNT) released in the waste water from explosive process plants is the serious problem due to toxic and explosive nature of TNT. The poor response of TNT to biodegradation enhanced the gravity of the problem. We have demonstrated that high specific surface area TiO₂–SiO₂ nano-composite aerogel is promising photo catalyst in successful treating of TNT contaminated aqueous solution. The TiO₂–SiO₂ composite aerogel with nominal content of 20 and 50% TiO₂, used as catalyst, were prepared by co-precursor sol–gel method using titanium isopropaxide and tetramethylorthosilicate as source of titania and silica, respectively. The XRD studies confirmed formation of anatase phase of crystalline TiO₂ with nano sized crystallites. The TiO₂–SiO₂ aerogel showed specific surface area of 1,107 and 485 m²/g for the aerogels containing 20 and 50% TiO₂, respectively. The 100 ppm TNT solution was treated, in 700 ml capacity reaction vessel, using H₂O₂ oxidizer and TiO₂–SiO₂ aerogel catalyst in presence of UV light (8 W UV lamp). Using TiO₂–SiO₂ (50/50) aerogel with surface area of 485 m²/g, we succeeded to reduce the TOC to 1 ppm within 3.5 h where as using TiO₂/SiO₂ (20/80) aerogel with surface area of 1,107 m²/g, the TOC was reduced to about only 7 ppm in the same time. It revealed that the combination of high TiO₂ content and high specific surface area is an important factor to achieve effective and faster degradation of TNT for complete mineralization.     

Preparation and characteristics of NiO-coated nano-fibriform silica

NiO-coated nano-fibriform silica (NFS) was prepared by an excessive soakage method and was characterized using transmission electron microscopy, X-ray diffraction, and physical N₂ adsorption techniques under different conditions. The results demonstrate that the coated NiO is of a cubic crystal form. The best preparation conditions are incubation in a water bath at 95 °C for 2 h and drying at 45 °C for 17 h, which lead to a higher NFS utilization ratio and thus lower cost, and a well-distributed NiO coating on the carrier NFS. Nitrogen adsorption isotherms for NiO-coated NFS are similar to a type IV curve, with a specific surface area of 292.7 m²/g, adsorptive capacity of 379.2 cm³/g, and pore volume of 0.59 cm³/g. The average pore diameter of NiO-coated NFS is 8.01 nm, but most pore diameters are in the range 2.1–3.9 nm. Comparison of NiO-coated NFS and NiO(Ni)-coated sol–gel silica as catalysts reveals that NiO-coated NFS may be an effective catalyst and that NFS may be a good catalyst carrier.     

Green micellar stability-indicating high-performance liquid chromatography method for determination of rupatadine fumarate in the presence of its main impurity desloratadine: Oxidative degradation kinetics study

A green micellar stability-indicating high-performance liquid chromatography method was developed for rupatadine fumarate determination in existence with its main impurity desloratadine. Separation was attained using Hypersil ODS column (150 × 4.6 mm, 5 μm), the micellar mobile phase consisted of 0.13 M sodium dodecyl sulfate, 0.1 M disodium hydrogen phosphate adjusted by phosphoric acid to pH 2.8 and 10% n-butanol. The column was maintained at 45^◦C and detection was carried out at 267 nm. A linear response was achieved over the range of 2–160 μg/ml for rupatadine and 0.4–8 μg/ml for desloratadine. The method was applied for rupatadine determination in alergoliber tablets and alergoliber syrup without the interference of methyl paraben and propyl paraben present as main excipients. Rupatadine fumarate revealed pronounced susceptibility to oxidation; further study of oxidative degradation kinetics was carried out. Rupatadine was found to follow pseudo-first-order kinetics when exposed to 10% H₂O₂ at 60 and 80°C and the activation energy was found to be 15.69 Kcal/mol. At a lower temperature (40°C), degradation kinetics regression was best fitted as a polynomial quadratic relationship, thus rupatadine oxidation at a lower temperature tends to adopt a second-order kinetics rate. Oxidative degradation product structure was revealed using infrared and found to be rupatadine N-oxide at all temperature values.     

Biogenic synthesis of silver nanoparticles using Echium vulgare: Characterisation,quantitative analysis of bioactive compounds,antioxidant activity and catalytic degradation

Nanotechnology has a great significance owing to its large variety of applications. Silver nanoparticles (AgNPs@Ev) were produced using water extract of Echium vulgare aerial part by a simple, nontoxic, eco-friendly method. The spectroscopic study identified the structure of AgNPs@Ev. The absorption was detected as 460 nm by UV/Vis spectrophotometer. TEM analysis presented the morphology of nanostructures and particle size was calculated as 9.55 nm. XRD pattern showed the structure to be face-centered cubic unit cell. EDS analysis verified the presence of elemental silver. DLS and zeta potential analyses were executed by Zetasizer. The stability of nanostructures was revealed by the zeta potential analysis (−3.1 mV). The degradation performance of AgNPs@Ev on methylene blue was evaluated by UV/Vis spectrophotometer and 64% of methylene blue was degraded after 40 h. Quantitative analysis of natural compounds was performed by HPLC and isoquercitrin (1.32 mg/g extract), naringin (1.15 mg/g extract) were detected as major products. Antioxidant activity of extract and nanoparticles were achieved. AgNPs@Ev exhibited excellent DPPH, ABTS, and FRAP activities (IC₅₀, 6.8 μg/mL), (IC₅₀, 2.3 μg/mL), (5.3 μmol/g sample) respectively.