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Keywords = µ-FTIR mapping

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23 pages, 28828 KB  
Article
Evaluation of Starch-Derived Hydrogel Systems for Artifact-Cleaning Applications
by Nicola Razza, Maduka L. Weththimuni, Matteo Ferretti, Alessandro Girella, Barbara Vigani, Pietro Galinetto and Maurizio Licchelli
Gels 2026, 12(6), 557; https://doi.org/10.3390/gels12060557 (registering DOI) - 20 Jun 2026
Viewed by 65
Abstract
The demand for sustainable, high-performance biomaterials has driven intense research towards natural polysaccharide hydrogels. Accordingly, this study aimed to synthesize novel starch-based hydrogel materials, considering their inherent hydrogel-forming capabilities together with diverse potential applications (e.g., pharmaceuticals, medicine, and the cleaning application for the [...] Read more.
The demand for sustainable, high-performance biomaterials has driven intense research towards natural polysaccharide hydrogels. Accordingly, this study aimed to synthesize novel starch-based hydrogel materials, considering their inherent hydrogel-forming capabilities together with diverse potential applications (e.g., pharmaceuticals, medicine, and the cleaning application for the artifacts). To obtain hydrogels with enhanced mechanical and physico-chemical properties, starch was combined with other polymeric species (i.e., alginate, polyvinyl alcohol, and polyvinylpyrrolidone), and a gelling process was induced by using calcium cations or borate anions. Two distinct hydrogels (named S-Ca and S-SB, respectively) were prepared and characterized by a range of instrumental and experimental techniques. The assessed properties included water and solvent resistance, equilibrium water content, water-releasing capacity, morphology and microstructural features with their composition by SEM-EDS analysis, and mechanical properties (tensile strength, elasticity, Young’s modulus, and hardness). The results indicated that the investigated hydrogels exhibited suitable properties for a variety of applications, including surface cleaning processes in the field of cultural heritage conservation. For instance, they showed equilibrium water content (between 80 and 90%) comparable with other hydrogels commonly used as cleaning tools (e.g., agar and p(HEMA)/PVP) and quite low water-releasing capacity (between 10 and 17 mgcm−2). Moreover, the S-SB hydrogel displayed distinctly better tensile strength and elongation at break than hydrogel prepared in the presence of Ca2+ (S-Ca). Notably, S-SB experienced considerable elasticity improvement after freezing–thawing cycles, as indicated by a decrease in tensile strength (from 275 to 102 kPa) and an increase in elongation at break (from 121 to 275%). However, it should be noted that the hydrogel selection depends on the requirements of the target application, as different processes demand materials with distinct characteristics. Hence, both S-Ca and S-SB hydrogels were tested as cleaning tools for the removal of artificially aged acrylic coating (i.e., Paraloid B-72) from the surface of marble and wood specimens, respectively. The tests provided positive results, as aged coating was satisfactorily removed by applying the hydrogels loaded with a nanostructured emulsion (NSE). These novel starch-based hydrogels demonstrate significant potential as high-performance alternatives to conventional hydrogel systems currently used in conservation science as well as in other industrial applications. Full article
(This article belongs to the Special Issue Innovative Gels: Structure, Properties, and Emerging Applications)
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20 pages, 11845 KB  
Article
Development of an Electrochemical Platform Based on Zinc Oxide Nanoparticles Embedded onto Montmorillonite Clay Functionalized with Phenylalanine for the Nano-Sensing of Acetaminophen in Pharmaceutical Tablets
by Gildas Calice Wabo, Alex Vincent Somba, Sengor Gabou Fogang, Cyrille Ghislain Fotsop, Astree Lottie Djuffo Yemene, Léopoldine Sonfack Guenang, Marcel Cédric Deussi Ngaha, Gullit Deffo and Evangeline Njanja
Biosensors 2026, 16(5), 244; https://doi.org/10.3390/bios16050244 - 26 Apr 2026
Viewed by 1030
Abstract
This study describes the development of an electrochemical sensor for quantitatively measuring acetaminophen (ACOP) in drug tablets. The sensor design is based on the modification of glassy carbon electrode (GCE) using zinc oxide nanoparticles (ZnONPs) embedded in a naturally occurring clay matrix (Sa) [...] Read more.
This study describes the development of an electrochemical sensor for quantitatively measuring acetaminophen (ACOP) in drug tablets. The sensor design is based on the modification of glassy carbon electrode (GCE) using zinc oxide nanoparticles (ZnONPs) embedded in a naturally occurring clay matrix (Sa) functionalized with phenylalanine (Phe). To ensure that the ZnONPs are homogeneously dispersed on the clay surface, the nanocomposite was synthesized using an impregnation approach and low-temperature heat treatment. The amino acid promotes specific interactions with ACOP through hydrogen bonding and π-π stacking, acting as both a stabilizing agent and a molecular recognition moiety. FTIR, UV-Vis, XRD, and FESEM/EDX mapping were employed to fully characterize the developed material (ZnONPs-Sa/Phe). Cyclic voltammetry (CV) and differential pulse voltammetry (DPV) were used for the electrochemical determination of ACOP using the modified electrode GCE/ZnONPs-Sa/Phe. Parameters susceptible to affecting the sensitivity of the developed sensor were optimized, revealing that 5 µL of the suspension ZnONPs-Sa/Phe immobilized on GCE was ideal for the sensing of ACOP in a phosphate buffer solution at pH 2.0. The calibration curve obtained by plotting peak current intensity against ACOP concentration exhibited linear behavior within the concentration range between 0.02 µM and 0.28 µM, enabling determination of the limits of detection (LOD) and quantitation (LOQ) at 8.54 × 10−9 M and 2.84 × 10−8 M, respectively. The reproducibility, stability, and selectivity of the sensor were evaluated, followed by its application to the nano-sensing of ACOP in Africure and Doliprane tablets, yielding satisfactory results. The simplicity, affordability, and high analytical sensitivity of the developed sensor make this sensing platform a promising tool for pharmaceutical quality control applications. Full article
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11 pages, 3142 KB  
Article
Processing Maps and Nano-IR Diagnostics of Type I Modifications in Mid-IR Germanate-Based Optical Glass
by Paul Mathieu, Nadezhda Shchedrina, Florence De La Barrière, Guillaume Druart and Matthieu Lancry
Photonics 2026, 13(2), 197; https://doi.org/10.3390/photonics13020197 - 16 Feb 2026
Viewed by 802
Abstract
Mid-IR flat/integrated optics require low-loss, programmable phase control. We investigate femtosecond laser direct writing (FLDW) in aluminogermanate glass (Corning 9754), first mapping the processing landscape to delineate no modification, Type I index increase, and spatial broadening regimes. We then operate in a non-accumulating [...] Read more.
Mid-IR flat/integrated optics require low-loss, programmable phase control. We investigate femtosecond laser direct writing (FLDW) in aluminogermanate glass (Corning 9754), first mapping the processing landscape to delineate no modification, Type I index increase, and spatial broadening regimes. We then operate in a non-accumulating regime that provides a broad, stable writing window. Quantitative-phase microscopy yields Δφ and a monotonic Δn with optically limited cross-sections compatible with low loss. Transmission spectroscopy shows high values (about 90% up to 4 µm) and no additional absorptions across the near-IR and mid-IR range. FTIR reveals a redshift of the Ge–O–(Ge/Al) stretching envelope from ≈1 µJ, correlating with the high Δn onset. s-SNOM at 925 cm−1 resolves the written line as reduced near-field amplitude and decreased phase, confirming a local complex permittivity change consistent with densification-driven Type I tracks. Together, these results define practical conditions for on-demand mid-IR flat/GRIN/Fresnel optics by FLDW in this commercial mid-IR transparent glass. Full article
(This article belongs to the Special Issue Advances in Micro-Nano Optical Manufacturing)
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17 pages, 28048 KB  
Article
Spectroscopic and Geochemical Characterization of NWA 11421: Insights into Lunar Crust–Mantle Composition and Implications for Remote Sensing and Moon Exploration
by Andrew Alberini, Francesco Renzi, Giovanni Poggiali, Fernándo Alberquilla, Sole Biancalani, Cristina García-Florentino, Anaïs Roussel, Mariano Battistuzzi, Julene Aramendia, Juan Manuel Madariaga, Teresa Fornaro and John Robert Brucato
Remote Sens. 2026, 18(4), 576; https://doi.org/10.3390/rs18040576 - 12 Feb 2026
Viewed by 837
Abstract
Lunar meteorites provide access to a geographically unconstrained record of the Moon, offering key insights into crustal diversity and interior evolution beyond the Apollo and Luna landing sites. Among them, the feldspathic breccia NWA 11421 is of particular interest because of its complex [...] Read more.
Lunar meteorites provide access to a geographically unconstrained record of the Moon, offering key insights into crustal diversity and interior evolution beyond the Apollo and Luna landing sites. Among them, the feldspathic breccia NWA 11421 is of particular interest because of its complex mineralogy and the presence of a dunite clast interpreted as a fragment of the lunar mantle. We present a non-destructive, multi-scale characterization of NWA 11421 using VIS–IR spectroscopy, µ-FTIR mapping, and µ-EDXRF. Results identify a polymict feldspathic breccia dominated by an anorthite matrix, with significant low-Ca pyroxene and olivine occurring as discrete mafic microdomains at the micro-scale. Near-infrared pyroxene band positions and Christiansen Feature (CF) value further indicate relatively mafic and primitive components. In addition, NWA 11421 CF value match with lunar crater-ejecta regions observed by the Diviner radiometer (LRO). These findings are consistent with a deep crustal or shallow mantle origin for NWA 11421 and may provide useful constraints for the selection of future landing sites, particularly in the context of ISRU-oriented human exploration, where mafic components are key sources of Fe and Mg. Full article
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17 pages, 3386 KB  
Article
MoS2/MWCNT Nanostructure: Enhanced Performance of Screen-Printed Carbon Electrode for Voltammetric Determination of 4-Nitrophenol in Water Samples
by Hadi Beitollahi and Somayeh Tajik
Micromachines 2025, 16(4), 366; https://doi.org/10.3390/mi16040366 - 23 Mar 2025
Cited by 8 | Viewed by 2074
Abstract
In the present work, we designed a straightforward and disposable voltammetric sensor utilizing a molybdenum disulfide/multi-walled carbon nanotube nanostructure-modified screen-printed carbon electrode (MoS2/MWCNTs/SPCE) for 4-nitrophenol (4-NP) determination. The successful synthesis of the MoS2/MWCNT nanostructure was characterized using Fourier transform [...] Read more.
In the present work, we designed a straightforward and disposable voltammetric sensor utilizing a molybdenum disulfide/multi-walled carbon nanotube nanostructure-modified screen-printed carbon electrode (MoS2/MWCNTs/SPCE) for 4-nitrophenol (4-NP) determination. The successful synthesis of the MoS2/MWCNT nanostructure was characterized using Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), transmission electron microscopy (TEM), and energy-dispersive X-ray spectroscopy (EXD) mapping. The electrochemical behavior of 4-NP at the MoS2/MWCNTs/SPCE was examined using differential pulse voltammetry (DPV), cyclic voltammetry (CV), and chronoamperometry techniques. The MoS2/MWCNTs/SPCE exhibited outstanding electro-catalytic activity for the voltammetric detection of 4-NP. Under optimized conditions, the reduction peak current showed a linear dependence with the concentration of 4-NP in the range of 0.05 to 800.0 µM, and a detection limit (LOD) of 0.01 µM was determined. In addition, the MoS2/MWCNTs/SPCE sensor has advantages including repeatability, reproducibility, stability, inexpensiveness, and practical application. The MoS2/MWCNTs/SPCE-based sensor was also utilized for the determination of 4-NP in real water specimens. Full article
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25 pages, 6758 KB  
Article
Comprehensive Advanced Physicochemical Characterization and In Vitro Human Cell Culture Assessment of BMS-202: A Novel Inhibitor of Programmed Cell Death Ligand
by Hasham Shafi, Andrea J. Lora, Haley M. Donow, Sally E. Dickinson, Georg T. Wondrak, H.-H. Sherry Chow, Clara Curiel-Lewandrowski and Heidi M. Mansour
Pharmaceutics 2024, 16(11), 1409; https://doi.org/10.3390/pharmaceutics16111409 - 1 Nov 2024
Cited by 3 | Viewed by 2927
Abstract
Background/Objectives: BMS-202, is a potent small molecule with demonstrated antitumor activity. The study aimed to comprehensively characterize the physical and chemical properties of BMS-202 and evaluate its suitability for topical formulation, focusing on uniformity, stability and safety profiles. Methods: A range of analytical [...] Read more.
Background/Objectives: BMS-202, is a potent small molecule with demonstrated antitumor activity. The study aimed to comprehensively characterize the physical and chemical properties of BMS-202 and evaluate its suitability for topical formulation, focusing on uniformity, stability and safety profiles. Methods: A range of analytical techniques were employed to characterize BMS-202. Scanning Electron Microscopy (SEM) was used to assess morphology, Differential Scanning Calorimetry (DSC) provided insights of thermal behavior, and Hot-Stage Microscopy (HSM) corroborated these thermal behaviors. Molecular fingerprinting was conducted using Raman spectroscopy and Fourier Transform Infrared (FTIR) spectroscopy, with chemical uniformity of the batch further validated by mapping through FTIR and Raman microscopies. The residual water content was measured using Karl Fisher Coulometric titration, and vapor sorption isotherms examined moisture uptake across varying relative humidity levels. In vitro safety assessments involved testing with skin epithelial cell lines, such as HaCaT and NHEK, and Transepithelial Electrical Resistance (TEER) to evaluate barrier integrity. Results: SEM revealed a distinctive needle-like morphology, while DSC indicated a sharp melting point at 110.90 ± 0.54 ℃ with a high enthalpy of 84.41 ± 0.38 J/g. HSM confirmed the crystalline-to-amorphous transition at the melting point. Raman and FTIR spectroscopy, alongside chemical imaging, confirmed chemical uniformity as well as validated the batch consistency. A residual water content of 2.76 ± 1.37 % (w/w) and minimal moisture uptake across relative humidity levels demonstrated its low hygroscopicity and suitability for topical formulations. Cytotoxicity testing showed dose-dependent reduction in skin epithelial cell viability at high concentrations (100 µM and 500 µM), with lower doses (0.1 µM to 10 µM) demonstrating acceptable safety. TEER studies indicated that BMS-202 does not disrupt the HaCaT cell barrier function. Conclusions: The findings from this study establish that BMS-202 has promising physicochemical and in vitro characteristics at therapeutic concentrations for topical applications, providing a foundation for future formulation development focused on skin-related cancers or localized immune modulation. Full article
(This article belongs to the Special Issue Dosage Form Design and Delivery Therapy for Skin Disorders)
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16 pages, 2206 KB  
Article
Synthesis, Spectroscopic Characterization, Antibacterial Activity, and Computational Studies of Novel Pyridazinone Derivatives
by Said Daoui, Şahin Direkel, Munjed M. Ibrahim, Burak Tüzün, Tarik Chelfi, Mohammed Al-Ghorbani, Mustapha Bouatia, Miloud El Karbane, Anass Doukkali, Noureddine Benchat and Khalid Karrouchi
Molecules 2023, 28(2), 678; https://doi.org/10.3390/molecules28020678 - 9 Jan 2023
Cited by 28 | Viewed by 6874
Abstract
In this work, a novel series of pyridazinone derivatives (317) were synthesized and characterized by NMR (1H and 13C), FT-IR spectroscopies, and ESI-MS methods. All synthesized compounds were screened for their antibacterial activities against Staphylococcus aureus [...] Read more.
In this work, a novel series of pyridazinone derivatives (317) were synthesized and characterized by NMR (1H and 13C), FT-IR spectroscopies, and ESI-MS methods. All synthesized compounds were screened for their antibacterial activities against Staphylococcus aureus (Methicillin-resistant), Escherichia coli, Salmonella typhimurium, Pseudomonas aeruginosa, and Acinetobacter baumannii. Among the series, compounds 7 and 13 were found to be active against S. aureus (MRSA), P. aeruginosa, and A. baumannii with the lowest MIC value range of 3.74–8.92 µM. Afterwards, DFT calculations of B3LYP/6-31++G(d,p) level were carried out to investigate geometry structures, frontier molecular orbital, molecular electrostatic potential maps, and gap energies of the synthesized compounds. In addition, the activities of these compounds against various bacterial proteins were compared with molecular-docking calculations. Finally, ADMET studies were performed to investigate the possibility of using of the target compounds as drugs. Full article
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13 pages, 3253 KB  
Article
A Novel Nanocomposite of Zn(II)-Protoporphyrin-Chitosan-Multi Walled Carbon Nanotubes and the Application to Caffeic Acid Sensing
by Bingkai Han, Xin Wen, Jinneng Wang and Yingrui Sun
Nanomaterials 2022, 12(19), 3412; https://doi.org/10.3390/nano12193412 - 29 Sep 2022
Cited by 7 | Viewed by 2533
Abstract
Caffeic acid is an antioxidant that has been widely been related to the health benefits of people in recent years. In this paper, the amino side chains of chitosan (CS) were modified with protoporphyrin IX by amide cross-linking, and then Zn ions were [...] Read more.
Caffeic acid is an antioxidant that has been widely been related to the health benefits of people in recent years. In this paper, the amino side chains of chitosan (CS) were modified with protoporphyrin IX by amide cross-linking, and then Zn ions were chelated. The properties of metalloporphyrin-preparing functionalized multi-walled carbon nanotubes (MWCNTs) and Zn ions chelated by protoporphyrin IX composites were used as sensitive-selective electrochemical biosensors for the determination of caffeic acid. The morphology and structure of nanocomposite Zn–PPIX–CS–MWCNTs were observed by X-ray spectroscopy mapping (EDX mapping), transmission electron microscopy (TEM), and Fourier-transform infrared spectroscopy (FTIR). The electrochemical behaviors of Zn–PPIX–CS–MWCNT-modified glassy carbon (GC) electrodes were evaluated by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The results show that the modified electrode had good electrocatalytic activity towards caffeic acid with a wide linear range of 0.0008–1.6 mM, an excellent sensitivity of 886.90 µAmM−1cm−1, and a detection limit of 0.022 µM. In addition, the caffeic acid sensor had excellent reproducibility, stability, and selectivity to various interfering substances. Therefore, the modified electrode prepared by this experiment can also be applied to electrochemical sensors of other substances. Full article
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16 pages, 4066 KB  
Article
Neovascularization Effects of Carbon Monoxide Releasing Drugs Chemisorbed on Coscinodiscus Diatoms Carriers Characterized by Spectromicroscopy Imaging
by Joachim Delasoie, Natasa Radakovic, Aleksandar Pavic and Fabio Zobi
Appl. Sci. 2020, 10(20), 7380; https://doi.org/10.3390/app10207380 - 21 Oct 2020
Cited by 10 | Viewed by 3495
Abstract
Silica microparticles made of diatomaceous earth have become particularly attractive materials for designing drug delivery systems. In order to investigate the use of natural diatoms as drug scaffolds for carbon monoxide releasing molecules (CORMs), we evaluated the chemisorption of the cis-[Re(CO)2Br [...] Read more.
Silica microparticles made of diatomaceous earth have become particularly attractive materials for designing drug delivery systems. In order to investigate the use of natural diatoms as drug scaffolds for carbon monoxide releasing molecules (CORMs), we evaluated the chemisorption of the cis-[Re(CO)2Br4]2− complex (ReCORM-2) and its vitamin B12 derivative (B12-ReCORM-2) on Coscinodiscus frustules by 3D FT-IR spectroscopic imaging, and the drugs’ neovascularization effects in vivo in the zebrafish (Danio rerio) model. By mapping the symmetric Re-C≡O υ(CO) stretching vibration of the CORMs in the 2000 cm−1 region, we found that the drugs are mostly localized at the girdle band of the diatom frustule. Both ReCORM-2 and B12-ReCORM-2 retain their CO-releasing ability when chemisorbed on the diatoms. When applied in vivo at doses ≥25 µM, the molecules markedly reduced intersegmental and subintestinal vessels development in zebrafish, revealing high anti-angiogenic potential. In addition, diatom frustules did not provoke any toxic in vivo response in the zebrafish embryos, including inflammation. Overall, our results indicate that: (1) CORMs chemisorbed on diatom frustules retain their CO-releasing abilities; (2) both CO-releasing molecules show a concentration-dependent effect on the neovascularization in developing zebrafish; (3) silicate frustules are not toxic and could be used as CORMs drug carriers. Full article
(This article belongs to the Special Issue New Frontiers in Diatom Nanotechnology)
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11 pages, 2212 KB  
Article
Non-Destructive In Situ Study of Plastic Deformations in Diamonds: X-ray Diffraction Topography and µFTIR Mapping of Two Super Deep Diamond Crystals from São Luiz (Juina, Brazil)
by Giovanna Agrosì, Gioacchino Tempesta, Giancarlo Della Ventura, Mariangela Cestelli Guidi, Mark Hutchison, Paolo Nimis and Fabrizio Nestola
Crystals 2017, 7(8), 233; https://doi.org/10.3390/cryst7080233 - 28 Jul 2017
Cited by 16 | Viewed by 6701
Abstract
Diamonds from Juina, Brazil, are well-known examples of superdeep diamond crystals formed under sublithospheric conditions and evidence would indicate their origins lie as deep as the Earth’s mantle transition zone and the Lower Mantle. Detailed characterization of these minerals and of inclusions trapped [...] Read more.
Diamonds from Juina, Brazil, are well-known examples of superdeep diamond crystals formed under sublithospheric conditions and evidence would indicate their origins lie as deep as the Earth’s mantle transition zone and the Lower Mantle. Detailed characterization of these minerals and of inclusions trapped within them may thus provide precious minero-petrogenetic information on their growth history in these inaccessible environments. With the aim of studying non-destructively the structural defects in the entire crystalline volume, two diamond samples from this locality, labelled JUc4 and BZ270, respectively, were studied in transmission mode by means of X-ray Diffraction Topography (XRDT) and micro Fourier Transform InfraRed Spectroscopy (µFTIR). The combined use of these methods shows a good fit between the mapping of spatial distribution of extended defects observed on the topographic images and the µFTIR maps corresponding to the concentration of N and H point defects. The results obtained show that both samples are affected by plastic deformation. In particular, BZ270 shows a lower content of nitrogen and higher deformation, and actually consists of different, slightly misoriented grains that contain sub-grains with a rounded-elongated shape. These features are commonly associated with deformation processes by solid-state diffusion creep under high pressure and high temperature. Full article
(This article belongs to the Special Issue Diamond Crystals)
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