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Innovative MOF-enhanced electroanalytical approach for sensitive sunitinib malate detection in renal carcinoma patients using CuO/lanthanum MOF-modified carbon paste electrode

Research Abstract

This study uniquely emphasizes the crucial role of MOF synthesis techniques in optimizing electrocatalytic properties and enhancing electroanalytical performance. The main aim of this work is to develop a highly sensitive, selective, and cost-effective electrochemical sensor for detecting sunitinib malate (SUN) in serum samples collected from renal cancer patients. The designed sensor was based on using CuO nanoparticles/lanthanum 1,4-napthalene dicarboxylic acid (NDC) MOF-modified carbon paste electrode (CuO NPs/LaNDC-MOF/CPE) coupled with square-wave adsorptive anodic stripping voltammetry (SW-AdASV) as the electrochemical technique. Two MOF synthetic approaches were utilized i.e. conventional (Conv.) and solvothermal (Solvo.). The synthesized La-MOFs were characterized using X-ray Diffraction analysis (XRD), Fourier transform IR spectroscopy (FTIR), Scanning electron microscopy (SEM), Transmission electron microscopy (TEM) and Nitrogen adsorption/desorption isotherm (BET). LaNDC-MOF (Conv.) has a higher surface area (four times) than LaNDC-MOF (Solvo.). Moreover, the modified electrode based on LaNDC-MOF (Conv.) exhibited better electrocatalytic activity and improved sensitivity towards the oxidation of SUN than that prepared through solvothermal route. Various experimental parameters, including accumulation potential, accumulation time, and pH of the supporting electrolyte, were optimized to obtain the best analytical performance. The fabricated sensor based on CuO NPs/LaNDC-MOF/CPE showed an oxidation peak of SUN at 0.66 V vs Ag/AgCl. Under the optimized conditions, SW-AdASV method exhibited a linear response over a concentration range of 0.01–1.0 μmol l-1 with a detection limit of 0.002 μmol l-1 for SUN. The proposed method was successfully applied for the determination of SUN in pharmaceutical formulations and serum samples of renal cancer patients. Moreover, the proposed methodology via modification of CPE with the synthesized MOFs tailors them to be applied for clinical analysis and therapeutic drug monitoring of SUN, providing a valuable tool for personalized medicine and improving the treatment outcomes for renal cancer patients.

Research Authors
Azza H. Rageh, Mohamed I. Said, Asmaa Abdeltawab, Fatma A.M. Abdel-aal
Research Date
Research Department
Research Journal
Talanta Open
Research Pages
100404
Research Publisher
ELSEVIER
Research Vol
11
Research Website
https://www.sciencedirect.com/science/article/pii/S2666831925000074
Research Year
2025

From complex to cleanup: PMA-modified zirconium ceftriaxone complex as a novel precursor to ZrMo₂O₈ nanoparticles for Rhodamine B adsorption

Research Abstract

Global environmental problems are one of the biggest threats to humanity today. These problems include water contamination, which is made worse by the economy's and industry's rapid growth. We describe in this work a new method for synthesis of ZrMo2O8 nanoparticles (NPs) by employing a phosphomolybdic acid (PMA)-modified zirconium ceftriaxone complex as a precursor. The precursor was thermally decomposed for 2 h at 600 °C, producing ZrMo2O8 NPs. Using transmission electron microscopy (TEM) and X-ray diffraction (XRD), the structural and morphological characteristics of the produced NPs were described. ZrMo2O8 NPs had a dense spherical structure with an average diameter of 25.2 nm. The surface characteristics of the modified complex and the resulting ZrMo2O8 NPs were investigated via nitrogen adsorption-desorption. Their specific surface areas were determined using the BET method to be 22.4 m2/g and 21.7 m2/g, respectively. Remarkably, ZrMo2O8 NPs showed a greater pore volume of 0.041 cm³/g and a larger pore width of 2.26 nm. Conversely, the modified complex had a pore volume of 0.023 cm³/g and a pore width of 2.06 nm. The adsorption efficiency of the ZrMo2O8 NPs was tested for the removal of Rhodamine B dye (RhB) from aqueous solutions. The adsorption studies indicated that the ZrMo2O8 NPs (50 mg) show rapid RhB adsorption (50 mL of 5.0 ppm), 95 % removal efficiency was attained in 180 min at pH 7. The highest adsorption capacity of 9.5 mg/g was observed when using 15 mg of ZrMo2O8 and 50 mL of 10.0 ppm RhB dye at pH 7. The studies of linear and non-linear kinetics showed that the adsorption mechanism is best described by pseudo-second-order model. The reusability of ZrMo2O8 NPs was examined over several cycles. Only a slight decrease in removal efficiency was observed, with removal efficacy reached 90 % after four cycles. Our results showed that the PMA-modified zirconium ceftriaxone complex is an effective precursor for producing ZrMo2O8 NPs. Furthermore, the nanoparticles are highly efficient adsorbents for the dye removal applications.

Research Authors
Mohamed I. Said , Fatma Sayed , Mohamed A. El Gahami
Research Date
Research Department
Research Journal
Journal of Physics and Chemistry of Solids
Research Pages
112609
Research Publisher
ELSEVIER
Research Vol
200
Research Website
https://www.sciencedirect.com/science/article/abs/pii/S0022369725000605
Research Year
2025

Synthesis and Biological Utility of Binary and Mixed Metal Complexes Based on Ceftriaxone

Research Abstract

Binary ceftriaxone metal complex of Cr (III) and five mixed metal complexes of [CrM(ceft.)2Cl(H2O)3], where M = Co(II), Mn(II), Ni(II), Cu(II), and Cd(II) were synthesized by a 1:1:2 molar ratio. FT-IR and UV-Vis spectroscopies, magnetic measurements, molar conductance, and microanalytical (C, H, and N) analysis were all used to describe the complexes. The shape, morphology, and size calculations have been examined using TEM and thermogravimetric analysis (TGA). The electronic absorption spectra and the magnetic moment values indicated the Oh geometry of the metal ions in the complexes. The ceftriaxone drug as a tetradentate ligand towards five metal ions through N (amino group) and O (triazine, βlactam carbonyl, and carboxylate groups). Several microorganisms have been tested for the complexes antibacterial activity, and the outcomes are contrasted with ceftriaxone's activity. From the results, all complexes show higher activity against Bacillus cereus and Escherichia coli except [CrCd(ceft)2Cl(H2O)3], which has nearly the same activity compared to ceftriaxone. All complexes show higher activity against pseudomonas aeruginosa than the activity of ceftriaxone. Moreover, they have lower activity against Micrococcus luteus, Sarratia marcescens, and Staphylococcus aureus.

Research Authors
Fatma Hashem, Mohamed Said , mohamed elgahami
Research Department
Research Journal
Assiut University Journal of Multidisciplinary Scientific Research
Research Pages
68-85
Research Vol
2
Research Website
https://aunj.journals.ekb.eg/article_406218.html
Research Year
2025

FeBTC MOF-Derived Fe3O4@C Nanocomposite: Controlled Synthesis and Application as Potential Adsorbent for Rhodamine Dye Elimination From Wastewater

Research Abstract

This study explores the controlled synthesis of a novel Fe3O4@C magnetic nanocomposite derived from FeBTC metal–organic framework (MOF) and its application as an efficient adsorbent for the removal of rhodamine dye from wastewater. The FeBTC MOF was first synthesized and then thermally decomposed in a controlled oxygen atmosphere at 375°C (1 h) to form the Fe3O4@C nanocomposite with a magnetic Fe3O4 core embedded in a porous carbon matrix. A comprehensive characterization of the nanocomposite was performed using x-ray diffraction (XRD), transmission electron microscopy (TEM), and x-ray photoelectron spectroscopy (XPS) to confirm the successful formation and to evaluate its structural and morphological properties. The morphological investigation revealed that the particles of Fe3O4 had a spherical shape with diameter of 10–15 nm. The carbon coating appeared as a thin amorphous layer surrounding the Fe3O4 nanoparticles. The adsorption capacity of Fe3O4@C for rhodamine B (RhB) dye was assessed under various conditions, including different pH values, contact times, initial dye concentrations, and temperatures. Complete dye removal was attained in 45 min using 50 mg of the nanocomposite and 50 mL of 5.0 ppm RhB at the optimum pH of 9.1. Under the same experimental conditions, the highest adsorption capacity of 13.0 mg/g was obtained, but using 15.0 mg of the nanocomposite. Fe3O4@C nanocomposite exhibits high adsorption efficiency, with a maximum removal capacity of 100%, which is clearly superior to many conventional adsorbents. This performance can be attributed to the synergistic effects of the magnetic Fe3O4 and the large surface area of the carbon matrix. Kinetic models were employed to understand the adsorption mechanism. The adsorption kinetics followed a pseudo-second-order model. The reusability of the adsorbent was tested over multiple cycles and showed a minimal loss of performance (drops to 93.0% after five removal cycles). The study demonstrates that the Fe3O4@C nanocomposite is a promising candidate for the effective removal of organic dyes from wastewater, offering potential benefits for environmental remediation and sustainable water management.

Research Authors
Mohamed I. Said, Mohamed M. Abd EL-Wahab, Alshimaa M. Sadek
Research Date
Research Department
Research Journal
Applied Organometallic Chemistry
Research Pages
e7869
Research Publisher
WILEY
Research Vol
39
Research Website
https://onlinelibrary.wiley.com/doi/abs/10.1002/aoc.7869
Research Year
2024

Zirconium-based hydrophobic-MOFs as innovative electrode modifiers for flibanserin determination: Exploring the electrooxidation mechanism using a comprehensive spectroelectrochemical study

Research Abstract

Three different types of Zr-based MOFs derived from benzene dicarboxylic acid (BDC) and naphthalene dicarboxylic acid as organic linkers (ZrBDC, 2,6-ZrNDC, and 1,4-ZrNDC) were synthesized. They were characterized using X-ray diffraction analysis (XRD), X-ray photoelectron spectroscopy (XPS), Fourier-transform IR spectroscopy (FT-IR), and Transmission electron microscopy (TEM). Their hydrophilic/hydrophobic nature was investigated via contact angle measurements; ZrBDC MOF was hydrophilic and the other two (ZrNDC) MOFs were hydrophobic. The three MOFs were combined with MWCNTs as electrode modifiers for the determination of a hydrophobic analyte, flibanserin (FLB), as a proof-of-concept analyte. Under the optimized experimental conditions, a significant enhancement in the oxidation peak current of FLB was observed when utilizing 2,6-ZrNDC and 1,4-ZrNDC, being the highest when using 1,4-ZrNDC. Furthermore, a thorough investigation of the complex oxidation pathway of FLB was performed by carrying out simultaneous spectroelectrochemical measurements. Based on the obtained results, it was verified that the piperazine moiety of FLB is the primary site for electrochemical oxidation. The fabricated sensor based on 1,4-ZrNDC/MW/CPE showed an oxidation peak of FLB at 0.8 V vs Ag/AgCl. Moreover, it showed excellent linearity for the determination of FLB in the range 0.05 to 0.80 μmol L−1 with a correlation coefficient (r) = 0.9973 and limit of detection of 3.0 nmol L−1. The applicability of the developed approach was demonstrated by determination of FLB in pharmaceutical tablets and human urine samples with acceptable repeatability (% RSD values were below 1.9% and 2.1%, respectively) and reasonable recovery values (ranged between 97 and 103% for pharmaceutical tablets and between 96 and 102% for human urine samples). The outcomes of the suggested methodology can be utilized for the determination of other hydrophobic compounds of pharmaceutical or biological interest with the aim of achieving low detection limits of these compounds in various matrices.

Research Authors
Azza H. Rageh, Mohamed I. Said & Fatma A. M. Abdel-aal
Research Date
Research Department
Research Journal
Microchimica Acta
Research Pages
236
Research Publisher
SPRINGER NATURE
Research Vol
191
Research Website
https://link.springer.com/article/10.1007/s00604-024-06297-1
Research Year
2024

MnO2@Al-BDC nanocomposite as adsorbent of remarkable high efficiency toward iron remediation from wastewaters

Research Abstract

Global environmental problems, especially those related to water contamination brought on by rapid industrialization and economic growth, are among the most dangerous threats facing humanity today. In this research work, Al3+ based metal–organic framework with 1,4-benzenedicarboxylic acid (H2BDC) linker has been synthesized by a simple and economic coprecipitation method. The obtained Al-BDC MOF was utilized as an adsorbent for sequestering iron from wastewater, but only 54.0% of iron concentration was eliminated after 120 min. To boost the removal efficiency, modification of the Al-BDC MOF was carried out. MnO2@Al-BDC nanocomposite was prepared and applied as a nanoadsorbent for iron remediation from water. The adsorption capability of Al-BDC MOF was greatly enhanced by facile modification. The adsorption efficiency reached 97.0% using 35.0 mg of the nanocomposite after 120 min compared to 54.0% iron removal using the un-modified MOF. The effect of pH of the medium was then studied using MnO2@Al-BDC nanocomposite. The best elimination efficacy of iron was accomplished at pH ~ 2.2. The adsorption of iron on the surface of MnO2@Al-BDC nanocomposite attains 97.0% (120 min) using a 35.0 mg dose of adsorbent and reaches 98.7% utilizing a 50.0 mg dose of adsorbent. In contrast, at pH = 9.2, the removal efficiency drops to 90.0% (after 120 min, 35.0 mg adsorbent). The adsorption capability was examined also using a variety of iron concentrations, i.e., 2.5, 5.0, and 7.5 mg/L where the adsorption efficiency dropped notably upon increasing the concentration. It dropped from 96.3% to 87.0% using 35.0 mg of MnO2@Al-BDC nanocomposite at 90 min. The newly developed adsorbent showed a pronounced efficiency for Fe3+ removal against real samples collected from different water sources. Ultimately, this research introduces a novel MnO2@Al-BDC nanocomposite, synthesized through a simple and economical coprecipitation method, to address water contamination by iron. The innovation lies in the significant enhancement of iron elimination efficiency, from 54.0% with unmodified Al-BDC MOF to 97.0% with the MnO2@Al-BDC nanocomposite.

Research Authors
Mohamed I. Said, Marwa Sayed, Aref A. M. Aly, Muhammad Atef
Research Date
Research Department
Research Journal
Applied Organometallic Chemistry
Research Pages
e7639
Research Publisher
Wiley
Research Vol
38
Research Website
https://onlinelibrary.wiley.com/doi/abs/10.1002/aoc.7639
Research Year
2024

CuMOF@Faujasite nanocomposite as a novel catalyst for hydrogen production

Research Abstract

Energy production is one of the most crucial issues presently attracting global attention. In this work, a CuMOF@Faujasite nanocomposite was synthesized and utilized as a novel efficient catalyst for hydrogen production. The produced composite was first characterized using X-ray diffraction (XRD), Fourier- transform infrared (FT-IR), thermogravimetric analysis (TGA), and differential scanning calorimetry. Surface properties were analyzed via nitrogen adsorption–desorption isotherms. All characterization results revealed the formation of a pure and well-defined crystalline phase, with a high specific surface area (SBET) of 286 m2/g (SBET of Faujasite is 35 m2/g). Moreover, the morphology and compositional analysis of the nanocomposite were assured through the scanning (SEM) and transmission (TEM) electron microscope and X-ray photospectroscopy (XPS). SEM and TEM images revealed sponge-like spheres that are related to Faujasite besides small spherical particles related to CuBDC MOF. XPS analysis revealed a low content of CuMOF in the nanocomposite. The catalytic activity of the nanocomposite was tested for the dehydrogenation of NaBH4. The impact of NaBH4 concentration, weight of the catalyst, and the reaction temperature on NaBH4 hydrolysis was investigated. A hydrogen generation rate (HGR) of 484 mLmin−1 g−1 at 30 °C was achieved using 50 mg of the catalyst and 0.05 mol/l of NaBH4 owing to the high specific area and the selective active sites for such hydrolytic reaction. The kinetic analysis of the activity data indicates the first-order behavior at low concentrations of NaBH4. Furthermore, at concentrations ≥0.065 mol L−1, zero-order kinetics was predominant. The time needed for completion of the hydrolysis reaction was found to be decreased (~20 min) by increasing the catalyst mass as well as NaBH4 concentration or even by elevating the reaction temperature (~4 min at 60 °C). The activation energy was estimated; it was found to be 70.5 KJ mol−1. Ultimately, our catalyst showed a reasonable rate of hydrogen production, as compared to others reported earlier.

Research Authors
Mohamed I. Said, Fatma M. Dardir, Rabei M. Gabr, Ezzat A. Ahmed, Mamdouh F. Soliman, Mostafa R. Abukhadra
Research Date
Research Department
Research Journal
Applied Organometallic Chemsitry
Research Pages
e7455
Research Publisher
Wiley
Research Vol
38
Research Website
https://onlinelibrary.wiley.com/doi/abs/10.1002/aoc.7455
Research Year
2024

Synthesis of porous MnO@ C nanocomposite via controlled heat-treatment of malonate precursor for the potential remediation of dye-contaminated water

Research Abstract

Remediation of the dye-contaminated water has received a broad interest due to the health problems and defects in the ecological system originating from the presence of such toxic materials in water. Herein, MnO@C nanocomposites as efficient adsorbent/photocatalyst materials for the removal of cationic and anionic dyes were synthesized via a simple and new precursor-assisted method. Manganese malonate was prepared and calcined at 350 °C for 1 h under air, argon, and H2 atmospheres. Pristine MnO was obtained under argon and H2. The obtained nanocomposites are highly crystalline and have sphere-like shapes as evidenced by TEM, HRTEM, and SAED. EDX analysis demonstrated the presence of C in the prepared samples. The study of the surface texture via the BJH method and Va-t plots has revealed the presence of both microporous and mesoporous pores. BET surface areas of 22.7 and 50.1 m2/g were found for MnO@C nanocomposites prepared under Ar and H2, respectively. Removal of MB as a cationic dye from water was explored via adsorption of the dye over the surface of MnO@C nanocomposites. The MnO@C sample prepared under H2 exhibited the largest removal efficacy, removal of 97% of the dye occurs in 6 h. Furthermore, the MnO@C nanocomposite was utilized as a photocatalyst for removal of the anionic dye, eosin Y. Complete removal of eosin Y color was achieved after exposure to sunlight for 2 h. The mechanism of the photocatalytic degradation of eosin Y was investigated. The possible degradation products were detected through HPLC-UV analysis. The prepared nanocomposite showed good recyclability and even preserving its structure after 4 cycles.

Research Authors
Mohamed Abdel-megeed Ibrahim Said
Research Date
Research Department
Research Journal
Solid State Sciences
Research Pages
106383
Research Publisher
ELSEVIER
Research Vol
108
Research Website
https://www.sciencedirect.com/science/article/abs/pii/S1293255820312553
Research Year
2020

Enhanced biological activity of chitinase immobilized on cobalt metal-organic framework: Isolation, characterization, and potential applications

Research Abstract

Chitinase, an enzyme that hydrolyzes glycosidic bonds in chitin, holds significant potential for industrial applications, including biological control, antifungal treatments, and antibiofilm strategies. In this study, chitinase derived from Planomicrobium sp. (PP133202) was immobilized onto a cobalt metal-organic framework (Co-MOF), and its properties were extensively analyzed using various biological, chemical, and physical characterization techniques. The microbial source was identified via 16S rRNA sequencing, and enzyme activity was optimized under submerged conditions using Response Surface Methodology (RSM). Structural and morphological characterization of the chitinase/Co-MOF complex was conducted through FTIR, SEM, TEM, XPS, XRD, EDX, and surface area analyses. The encapsulation efficiency and loading capacity were determined to be 42 % and 20 %, respectively. Notably, the immobilized chitinase exhibited a threefold increase in enzymatic activity compared to its free form. Additionally, the chitinase/Co-MOF complex demonstrated enhanced biological control efficacy, effectively inhibiting Tribolium castaneum and multiple pathogenic microorganisms, including Pseudomonas aeruginosaAspergillus flavusAspergillus terreus, and Beauveria bassiana. These findings highlight the potential of chitinase/Co-MOF as a promising agent for antimicrobial and pest control applications.

Research Authors
Fatma M. Tawfiq, Fatma El-Zahraa A. Abd El-Aziz, Shimaa H. Salem, Abdelnaby M. Elshahawy, Ahmed M. Sayed, A.A. Abdel-Hafez
Research Date
Research Journal
International Journal of Biological Macromolecules
Research Publisher
Elsevier
Research Vol
308
Research Website
https://doi.org/10.1016/j.ijbiomac.2025.142538
Research Year
2025

Hydrothermal Synthesis of Microporous CuWO4 for Hydrogen Generation and Antibacterial Activity

Research Abstract

Hydrogen gas (H2) is an environmentally benign and sustainable energy fuel. Because of its high energy content, hydrogen presents a viable clean energy source alternative to fossil fuels and is regarded as a one of the most promising energy sources. In the current investigation, CuWO4 was applied, for the first time, as an efficient catalyst for the green generation of H2 from the hydrolysis of NaBH4. CuWO4 was fabricated via a co-precipitation assisted hydrothermal method. The synthesized catalyst was characterized by XRD, XPS, VSM, FTIR, SEM, TEM, and nitrogen sorption analyses. XRD and XPS analyses confirmed the successful formation of CuWO4. It was estimated that, values of hydrogen generation rate (HGR) 818, 1250, 2467, and 2920 ml min−1 g−1 were respectively obtained at reaction temperatures of 28, 35, 40, and 45 °C. According to the pseudo-first-order equation, CuWO4 have an estimated apparent activation energy of 59.2 kJ mol−1. Thermodynamic parameters like ∆H#, ∆S#, and ∆G# were also calculated. The antibacterial efficacy of CuWO4 was evaluated against four Gram positive pathogenic strains; Bacillus subtilis, Bacillus cereus, Staphylococcus aureus and Micrococcus luteus with concentration range 0–150 µg ml−1 comparing with chloramphenicol (CHL) antibacterial agent. Minimum inhibitory concentration (MIC) was determined for CuWO4 and CHL for the four strains. CuWO4 clear promising antibacterial properties with growth inhibition (%) of 82.79 (49.9 CHL) %, 73.56 (67.89 CHL) %, 61.38 (58.18 CHL) %, and 50.47 (43.4 CHL) % at 150 µg ml−1 of B. subtilis, S. aureus, B. cereus, and Micrococcus luteus, respectively.

Research Authors
Mohamed N. Goda · Laila S. Alqarni · Mohamed Khairy · Mortaga M. Abou-Krisha · Babiker Y. Abdulkhair· Ehab A. Abdelrahman · Ghada Abd-Elmonsef Mahmoud
Research Date
Research Journal
Journal of Inorganic and Organometallic Polymers and Materials
Research Member
Research Pages
1-15
Research Publisher
@ Springer
Research Rank
International
Research Website
https://link.springer.com/article/10.1007/s10904-025-03727-2
Research Year
2025
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