Irina Atkinson

@icf.ro

Institute of Physical Chemistry of the Romanian Academy

RESEARCH, TEACHING, or OTHER INTERESTS

Materials Science, Biomaterials, Ceramics and Composites, Surfaces, Coatings and Films

117

Scopus Publications

Scopus Publications

  • Comparison between Two Different Synthesis Methods of Strontium-Doped Hydroxyapatite Designed for Osteoporotic Bone Restoration
    Cosmin Iulian Codrea, Daniel Lincu, Irina Atkinson, Daniela C. Culita, Alexa-Maria Croitoru, Georgiana Dolete, Roxana Trusca, Bogdan Stefan Vasile, Miruna Silvia Stan, Denisa Ficai,et al.

    MDPI AG
    Development of efficient controlled local release of drugs that prevent systemic side effects is a challenge for anti-osteoporotic treatments. Research for new bone-regeneration materials is of high importance. Strontium (Sr) is known as an anti-resorptive and anabolic agent useful in treating osteoporosis. In this study, we compared two different types of synthesis used for obtaining nano hydroxyapatite (HA) and Sr-containing nano hydroxyapatite (SrHA) for bone tissue engineering. Synthesis of HA and SrHA was performed using co-precipitation and hydrothermal methods. Regardless of the synthesis route for the SrHA, the intended content of Sr was 1, 5, 10, 20, and 30 molar %. The chemical, morphological, and biocompatibility properties of HA and SrHA were investigated. Based on our results, it was shown that HA and SrHA exhibited low cytotoxicity and demonstrated toxic behavior only at higher Sr concentrations.

  • Hybrid Materials Obtained by Immobilization of Biosynthesized Ag Nanoparticles with Antioxidant and Antimicrobial Activity
    Gabriela Petcu, Elena Madalina Ciobanu, Gabriela Paun, Elena Neagu, Adriana Baran, Bogdan Trica, Andreea Neacsu, Irina Atkinson, Razvan Bucuresteanu, Alexandra Badaluta,et al.

    MDPI AG
    Ag nanoparticles (AgNPs) were biosynthesized using sage (Salvia officinalis L.) extract. The obtained nanoparticles were supported on SBA-15 mesoporous silica (S), before and after immobilization of 10% TiO2 (Degussa-P25, STp; commercial rutile, STr; and silica synthesized from Ti butoxide, STb). The formation of AgNPs was confirmed by X-ray diffraction. The plasmon resonance effect, evidenced by UV-Vis spectra, was preserved after immobilization only for the sample supported on STb. The immobilization and dispersion properties of AgNPs on supports were evidenced by TEM microscopy, energy-dispersive X-rays, dynamic light scattering, photoluminescence and FT-IR spectroscopy. The antioxidant activity of the supported samples significantly exceeded that of the sage extract or AgNPs. Antimicrobial tests were carried out, in conditions of darkness and white light, on Staphylococcus aureus, Pseudomonas aeruginosa, Escherichia coli and Candida albicans. Higher antimicrobial activity was evident for SAg and STbAg samples. White light increased antibacterial activity in the case of Escherichia coli (E. coli) and Pseudomonas aeruginosa (P. aeruginosa). In the first case, antibacterial activity increased for both supported and unsupported AgNPs, while in the second one, the activity increased only for SAg and STbAg samples. The proposed antibacterial mechanism shows the effect of AgNPs and Ag+ ions on bacteria in dark and light conditions.

  • Bioinspired 3D scaffolds with antimicrobial, drug delivery, and osteogenic functions for bone regeneration
    Irina Atkinson, Ana-Maria Seciu-Grama, Andrada Serafim, Simona Petrescu, Mariana Voicescu, Elena Maria Anghel, Cornelia Marinescu, Raul Augustin Mitran, Oana Catalina Mocioiu, Jeanina Pandele Cusu,et al.

    Springer Science and Business Media LLC

  • Hydrophobic and Transparent Tantalum Pentoxide-Based Coatings for Photovoltaic (PV) Solar Panels
    Oana Cătălina Mocioiu, Irina Atkinson, Ludmila Aricov, Veronica Bratan, Ana-Maria Mocioiu, Ioan Albert Tudor, and Diana Irinel Băilă

    MDPI AG
    Photovoltaic (PV) solar panels suffer from efficiency losses due to the accumulation of dust on their surface during operation, as well as the loss of transparency in the top glass. The efficiency can be increased when hydrophobic films are deposited on the top glass of the solar cells. The top glass of solar cells must have three characteristics: high transmittance in the 380–750 nm range, a band gap greater than 3.2 eV and a refractive index higher than 1.23. So, the films require the same characteristics. This work presents an increase in the contact angle (related to an increase in the hydrophobic character) when Ta2O5 is partially substituted with ZnO. The studied films, physically deposited on glass by e-gun technology, present a non-crystalline state in the form of the X-ray patterns shown. The films have a transmission of 75%–80% in the visible range. The morphology and roughness of the coatings were evaluated by atomic force microscopy. All films show the values of the Millipore water contact angle higher than 91 degrees, leading to the acquisition of hydrophobic properties on the surface. In comparison, the substrate is hydrophilic, with an average contact angle of 53.81 ± 2.16. The hydrophobic properties and self-cleaning ability make the films recommendable for application. The band gap of the coatings was calculated with the Tauc method, and they have values of 4.5–4.6 eV.

  • Composite Photocatalysts with Fe, Co, and Ni Oxides on Supports with Tetracoordinated Ti Embedded into Aluminosilicate Gel during Zeolite Y Synthesis
    Gabriela Petcu, Elena Maria Anghel, Irina Atkinson, Daniela C. Culita, Nicoleta G. Apostol, Andrei Kuncser, Florica Papa, Adriana Baran, Jean-Luc Blin, and Viorica Parvulescu

    MDPI AG
    Ti-aluminosilicate gels were used as supports for the immobilization of Fe, Co, and Ni oxides (5%) by impregnation and synthesis of efficient photocatalysts for the degradation of β-lactam antibiotics from water. Titanium oxide (1 and 2%) was incorporated into the zeolite network by modifying the gel during the zeolitization process. The formation of the zeolite Y structure and its microporous structure were evidenced by X-ray diffraction and N2 physisorption. The structure, composition, reduction, and optical properties were studied by X-ray diffraction, H2-TPR, XPS, Raman, photoluminescence, and UV–Vis spectroscopy. The obtained results indicated a zeolite Y structure for all photocatalysts with tetracoordinated Ti4+ sites. The second transitional metals supported by the post-synthesis method were obtained in various forms, such as oxides and/or in the metallic state. A red shift of the absorption edge was observed in the UV–Vis spectra of photocatalysts upon the addition of Fe, Co, or Ni species. The photocatalytic performances were evaluated for the degradation of cefuroxime in water under visible light irradiation. The best results were obtained for iron-immobilized photocatalysts. Scavenger experiments explained the photocatalytic results and their mechanisms. A different contribution of the active species to the photocatalytic reactions was evidenced.

  • Continuous Supercritical Water Impregnation Method for the Preparation of Metal Oxide on Activated Carbon Composite Materials
    Florentina Maxim, Elena-Ecaterina Toma, Giuseppe-Stefan Stoian, Cristian Contescu, Irina Atkinson, Christian Ludwig, and Speranta Tanasescu

    MDPI AG
    Metal oxide (MexOy) nanomaterials are used as catalysts and/or sorbents in processes taking place in supercritical water (scH2O), which is the “green” solvent needed to obtain energy-relevant products. Their properties are significantly influenced by the synthesis method used to prepare active MexOy. In addition, the use of supported MexOy nanoparticles is more practical and cost-effective in terms of their performance maintenance. Within this context, the present study reports on the preparation of carbon-supported ZnO and CuO composites using an innovative scH2O impregnation method. Metal oxides were impregnated on a carbon (C) support using a continuous-flow tubular reactor. The results show that impregnation in scH2O is a promising approach for the preparation of ZnO/C and CuO/C composite materials. This one-step synthesis method, in a continuous flow, uses neither a seed layer nor a mineralizer, and it needs substantially lower preparation times than conventional impregnation methods.

  • Interplay of the hydroxyapatite structure and morphology with the thermodynamic parameters at hydroxyapatite/protein interface
    Adriana Serban, Florina Teodorescu, Ancuta M. Sofronia, Irina Atkinson, Cornelia A. Marinescu, Alina Botea-Petcu, Florentina Maxim, and Speranta Tanasescu

    Elsevier BV

  • Co- and Ni-Doped TiO<inf>2</inf> Nanoparticles Supported on Zeolite Y with Photocatalytic Properties
    Gabriela Petcu, Florica Papa, Irina Atkinson, Adriana Baran, Nicoleta G. Apostol, Simona Petrescu, Lionel Richaudeau, Jean-Luc Blin, and Viorica Parvulescu

    MDPI AG
    Zeolite Y samples with microporous and hierarchical structures containing Ti–Ni and Ti–Co oxides were obtained as active photocatalysts. Different Ti amounts (5, 10% TiO2) were supported, followed by the loading of Ni or Co oxides (5%). X-ray diffraction evidenced the presence of TiO2 as an anatase. N2 adsorption–desorption results showed type IV isotherms for hierarchical zeolite Y samples, and a combination of type IV and I isotherms for zeolite Y samples. UV–Vis diffuse reflectance spectra showed a shift in the absorption band to visible with increasing Ti loading and especially after Co and Ni addition. A significant effect of the support was evidenced for Ti and its interaction with Co/Ni species. The zeolite Y support stabilized Ti in the 4+ oxidation state while hierarchical zeolite Y support favored the formation of Ti3+ species, Ni0 and Ni2+ and the oxidation of Co to 3+ oxidation state. Photocatalytic activity, under UV and visible light irradiation, was evaluated by the degradation of amoxicillin, used as a model test. The photocatalytic mechanism was investigated using ethanol, p-benzoquinone and KI as ·OH and ·O2− radicals and hole (h+) scavengers. The best results were obtained for the immobilized Ni-Ti species on the hierarchical zeolite Y support.

  • Novel PEG<inf>6000</inf>–Silica-MWCNTs Shape-Stabilized Composite Phase-Change Materials (ssCPCMs) for Thermal-Energy Storage
    Cristina Lavinia Nistor, Ioana Catalina Gifu, Elena Maria Anghel, Raluca Ianchis, Cristiana-Diana Cirstea, Cristian Andi Nicolae, Augusta Raluca Gabor, Irina Atkinson, and Cristian Petcu

    MDPI AG
    This paper describes the preparation of new PEG6000–silica-MWCNTs composites as shape-stabilized phase change materials (ssPCMs) for application in latent heat storage. An innovative method was employed to obtain the new organic–inorganic hybrid materials, in which both a part of the PEG chains, used as the phase change material, and a part of the hydroxyl functionalized multiwall carbon nanotubes (MWCNTs-OH), used as thermo-conductive fillers, were covalently connected by newly formed urethane bonds to the in-situ-generated silica matrix. The study’s main aim was to investigate the optimal amount of PEG6000 that can be added to the fixed sol–gel reaction mixture so that no leakage of PEG occurs after repeated heating–cooling cycles. The findings show that the optimum PEG6000/NCOTEOS molar ratio was 2/1 (~91.5% PEG6000), because both the connected and free PEG chains interacted strongly with the in-situ-generated silica matrix to form a shape-stabilized material while preserving high phase-transition enthalpies (~153 J/G). Morphological and structural findings obtained by SEM, X-ray and Raman techniques indicated a distribution of the silica component in the amorphous phase (~27% for the optimum composition) located among the crystalline lamellae built by the folded chains of the PEG component. This composite maintained good chemical stability after a 450-cycle thermal test and had a good storage efficiency (~84%).

  • Influence of the Deposition Parameters on the Properties of TiO<inf>2</inf> Thin Films on Spherical Substrates
    Maria Covei, Cristina Bogatu, Silvioara Gheorghita, Anca Duta, Hermine Stroescu, Madalina Nicolescu, Jose Maria Calderon-Moreno, Irina Atkinson, Veronica Bratan, and Mariuca Gartner

    MDPI AG
    Wastewater treatment targeting reuse may limit water scarcity. Photocatalysis is an advanced oxidation process that may be employed in the removal of traces of organic pollutants, where the material choice is important. Titanium dioxide (TiO2) is a highly efficient photocatalyst with good aqueous stability. TiO2 powder has a high surface area, thus allowing good pollutant adsorption, but it is difficult to filter for reuse. Thin films have a significantly lower surface area but are easier to regenerate and reuse. In this paper, we report on obtaining sol-gel TiO2 thin films on spherical beads (2 mm diameter) with high surface area and easy recovery from wastewater. The complex influence of the substrate morphology (etched up to 48 h in concentrated H2SO4), of the sol dilution with ethanol (1:0 or 1:1), and the number of layers (1 or 2) on the structure, morphology, chemical composition, and photocatalytic performance of the TiO2 thin films is investigated. Etching the substrate for 2 h in H2SO4 leads to uniform, smooth surfaces on which crystalline, homogeneous TiO2 thin films are grown. Films deposited using an undiluted sol are stable in water, with some surface reorganization of the TiO2 aggregates occurring, while the films obtained using diluted sol are partially washed out. By increasing the film thickness through the deposition of a second layer, the roughness increases (from ~50 nm to ~100 nm), but this increase is not high enough to promote higher adsorption or overall photocatalytic efficiency in methylene blue photodegradation (both about 40% after 8 h of UV-Vis irradiation at 55 W/m2). The most promising thin film, deposited on spherical bead substrates (etched for 2 h in H2SO4) using the undiluted sol, with one layer, is highly crystalline, uniform, water-stable, and proves to have good photocatalytic activity.

  • Effects of Aluminosilicate Gel Treatment and TiO<inf>2</inf> Loading on Photocatalytic Properties of Au–TiO<inf>2</inf>/Zeolite Y
    Gabriela Petcu, Florica Papa, Elena Maria Anghel, Irina Atkinson, Silviu Preda, Simona Somacescu, Daniela C. Culita, Adriana Baran, Elena Madalina Ciobanu, Luiza Maria Jecu,et al.

    MDPI AG
    The present work reports the synthesis of efficient Ti–Au/zeolite Y photocatalysts by different processing of aluminosilicate gel and studies the effect of titania content on the structural, morphological, textural, and optical properties of the materials. The best characteristics of zeolite Y were obtained by aging the synthesis gel in static conditions and mixing the precursors under magnetic stirring. Titania (5, 10, 20%) and gold (1%) species were incorporated in zeolite Y support by the post-synthesis method. The samples were characterized by X-ray diffraction, N2-physisorption, SEM, Raman, UV–Vis and photoluminescence spectroscopy, XPS, H2-TPR, and CO2-TPD. The photocatalyst with the lowest TiO2 loading shows only metallic Au on the outermost surface layer, while a higher content favors the formation of additional species such as: cluster type Au, Au1+, and Au3+. A high TiO2 content contributes to increasing the lifetime of photogenerated charge careers, and the adsorption capacity of the pollutant. Therefore, an increase in the photocatalytic performances (evaluated in degradation of amoxicillin in water under UV and visible light) was evidenced with the titania content. The effect is more significant in visible light due to the surface plasmon resonance (SPR) effect of gold interacting with the supported titania.

  • Effect of Al Incorporation on the Structural and Optical Properties of Sol–Gel AZO Thin Films
    Hermine Stroescu, Madalina Nicolescu, Daiana Mitrea, Ecaterina Tenea, Irina Atkinson, Mihai Anastasescu, Jose Maria Calderon-Moreno, and Mariuca Gartner

    MDPI AG
    ZnO and Al-doped ZnO (AZO) thin films were prepared using the sol–gel method and deposited on a Silicon (Si(100)) substrate using the dipping technique. The structure, morphology, thickness, optical constants in the spectral range 300–1700 nm, bandgap (Eg) and photoluminescence (PL) properties of the films were analyzed using X-ray diffractometry (XRD), X-ray fluorescence (XRF), atomic force microscopy (AFM), scanning electron microscopy (SEM), spectroscopic ellipsometry (SE), Raman analysis and PL spectroscopy. The results of the structure and morphology analyses showed that the thin films are polycrystalline with a hexagonal wurtzite structure, as well as continuous and homogeneous. The PL background and broader peaks observable in the Raman spectra of the AZO film and the slight increase in the optical band gap of the AZO thin film, compared to undoped ZnO, highlight the effect of defects introduced into the ZnO lattice and an increase in the charge carrier density in the AZO film. The PL emission spectra of the AZO thin film showed a strong UV line corresponding to near-band-edge ZnO emission along with weak green and red emission bands due to deep-level defects, attributed to the oxygen-occupied zinc vacancies (OZn lattice defects).

  • Transition metal-containing MgFe ex-LDH mixed oxides, effective catalysts in the hydrodeoxygenation of benzyl alcohol
    Alexandru-Tudor Toderaşc, Irina Atkinson, Daniela Cristina Culiţă, Paul Emil Mereuţă, Florica Papa, Adriana Urdă, and Ioan-Cezar Marcu

    Elsevier BV


  • Brij 58–activated carbon assisted synthesis of Ag/Ag<inf>2</inf>O/TiO<inf>2</inf>-AC photocatalysts for efficient organic pollutants degradation
    Daniela Negoescu, Irina Atkinson, Mihaela Gherendi, Daniela C. Culita, Adriana Baran, Simona Petrescu, Bogdan Trica, Diana Pelinescu, Robertina Ionescu, Veronica Bratan,et al.

    Elsevier BV

  • Ag-Decorated Iron Oxides-Silica Magnetic Nanocomposites with Antimicrobial and Photocatalytic Activity
    Viorica Muşat, Lenuța Crintea (Căpăţână), Elena-Maria Anghel, Nicolae Stănică, Irina Atkinson, Daniela Cristina Culiţă, Liliana Baroiu, Nicolae Țigău, Alina Cantaragiu Ceoromila, Andreea-Veronica Botezatu (Dediu),et al.

    MDPI AG
    Nanotechnology offers unlimited possibilities for creating effective hybrid materials, which combine functional performance in environment depollution and antimicrobial defense with a lack of toxicity, biocompatibility, biodegradability, and natural availability. This paper presents the silver effect on photocatalytic and antibacterial activities of double-coated iron oxide nanoparticles (NPs), Fe3O4@SiO2/ZnO-Ag. The structural, morphological, and textural information of the, core–shell iron oxides-based superparamagnetic nanoparticles (IOMNPs) decorated with 5% Ag by ultrasound-assisted synthesis were evaluated by scanning electron microscopy with energy dispersive spectroscopy (SEM-EDX), X-ray diffraction, Raman spectroscopy, and Brunauer–Emmett–Teller physisorption measurements. Although two synthesis temperatures of 95 and 80 °C were used for the co-precipitated iron oxide cores, the XRD patterns revealed the formation of a single magnetite, Fe3O4, phase. The sorption–photocatalytic activities under dark and UV irradiation encountered a maximum removal efficiency of the MB (90.47%) for the Fe3O4@SiO2/ZnO-Ag sample with iron oxide core obtained at 80 °C. The rate constant for the second-order kinetics was 0.0711 min−1 for 2 h, and the correlation coefficient R2 closed to unity. Two samples with Ag-decorated hybrid SiO2/ZnO shell and hierarchically interconnected porous structure with large surface area (328.8 and 342.5 m2g−1) exhibited the best disk diffusion antimicrobial activity against four microorganisms, especially gram-positive Staphylococcus aureus.

  • Band-Gap Engineering of Layered Perovskites by Cu Spacer Insertion as Photocatalysts for Depollution Reaction
    Monica Raciulete, Crina Anastasescu, Florica Papa, Irina Atkinson, Corina Bradu, Catalin Negrila, Diana-Ioana Eftemie, Daniela C. Culita, Akane Miyazaki, Veronica Bratan,et al.

    MDPI AG
    A multi-step ion-exchange methodology was developed for the fabrication of Cu(LaTa2O7)2 lamellar architectures capable of wastewater depollution. The (001) diffraction line of RbLaTa2O7 depended on the guest species hosted by the starting material. SEM and TEM images confirmed the well-preserved lamellar structure for all intercalated layered perovskites. The UV–Vis, XPS, and photocurrent spectroscopies proved that Cu intercalation induces a red-shift band gap compared to the perovskite host. Moreover, the UV–Vis spectroscopy elucidated the copper ions environment in the Cu-modified layered perovskites. H2-TPR results confirmed that Cu species located on the surface are reduced at a lower temperature while those from the interlayer occur at higher temperature ranges. The photocatalytic degradation of phenol under simulated solar irradiation was used as a model reaction to assess the performances of the studied catalysts. Increased photocatalytic activity was observed for Cu-modified layered perovskites compared to RbLaTa2O7 pristine. This behavior resulted from the efficient separation of photogenerated charge carriers and light absorption induced by copper spacer insertion.

  • Evolution of Morphology, Fractal Dimensions, and Structure of (Titanium) Aluminosilicate Gel during Synthesis of Zeolites Y and Ti-Y
    Gabriela Petcu, Gianina Dobrescu, Irina Atkinson, Madalina Ciobanu, Jean-Luc Blin, and Viorica Parvulescu

    MDPI AG
    Zeolite Y and Ti-containing zeolite Y (1%, 2% and 5% TiO2) were synthesized by a hydrothermal seed-assisted method. In order to evidence the evolution of morphology, structure, and fractal dimensions during the zeolitization process at certain time intervals, a small volume from the reaction medium was isolated and frozen by lyophilization. The obtained samples were characterized by scanning electron microscopy (SEM), wide-angle X-ray diffraction (XRD), and small-angle X-ray scattering (SAXS). The fractal dimension values of the isolated samples, calculated from SAXS data, evidenced a transition from small particles with a smooth surface (2.021) to compact structures represented by zeolite crystallites with rough surfaces (2.498) and specific organization for zeolite Y. The formation of new structures during hydrothermal treatment, the increase in crystallite size and roughness due to the continuous growth were suggested by variation of fractal dimensions values, SEM microscopy images and X-ray diffractograms. The incorporation of titanium in low concentration into the zeolite Y framework led to the obtaining of low fractal dimensions of 2.034–2.275 (smooth surfaces and compact structures). On the other hand, higher titanium concentration (2%) led to an increase in fractal dimensions indicating structures with rougher surfaces and well-defined self-similarity properties. A mechanism for zeolite synthesis was proposed by correlation of the results obtained through morphological, structural, and fractal analysis.


  • Au/Ti Synergistically Modified Supports Based on SiO<inf>2</inf> with Different Pore Geometries and Architectures
    Gabriela Petcu, Elena Maria Anghel, Elena Buixaderas, Irina Atkinson, Simona Somacescu, Adriana Baran, Daniela Cristina Culita, Bogdan Trica, Corina Bradu, Madalina Ciobanu,et al.

    MDPI AG
    New photocatalysts were obtained by immobilization of titanium and gold species on zeolite Y, hierarchical zeolite Y, MCM-48 and KIT-6 supports with microporous, hierarchical and mesoporous cubic structure. The obtained samples were characterized by X-ray diffraction (XRD), N2-physisorption, scanning and transmission electron microscopy (SEM/TEM), diffuse reflectance UV–Vis spectroscopy (DRUV-Vis), X-ray photoelectron spectroscopy (XPS), Raman and photoluminescence spectroscopy. The photocatalytic properties were evaluated in degradation of amoxicillin (AMX) from water, under UV (254 nm) and visible light (532 nm) irradiation. The higher degradation efficiency and best apparent rate constant were obtained under UV irradiation for Au-TiO2-KIT-6, while in the visible condition for the Au-TiO2-MCM-48 sample containing anatase, rutile and the greatest percent of Au metallic clusters were found (evidenced by XPS). Although significant values of amoxicillin degradation were obtained, total mineralization was not achieved. These results were explained by different reaction mechanisms, in which Au species act as e− trap in UV and e− generator in visible light.

  • In Vitro Anticancer Activity of Mucoadhesive Oral Films Loaded with Usnea barbata (L.) F. H. Wigg Dry Acetone Extract, with Potential Applications in Oral Squamous Cell Carcinoma Complementary Therapy
    Violeta Popovici, Elena Matei, Georgeta Camelia Cozaru, Laura Bucur, Cerasela Elena Gîrd, Verginica Schröder, Emma Adriana Ozon, Adina Magdalena Musuc, Mirela Adriana Mitu, Irina Atkinson,et al.

    MDPI AG
    Oral squamous cell carcinoma (OSCC) is the most frequent oral malignancy, with a high death rate and an inadequate response to conventional chemotherapeutic drugs. Medical research explores plant extracts’ properties to obtain potential nanomaterial-based anticancer drugs. The present study aims to formulate, develop, and characterize mucoadhesive oral films loaded with Usnea barbata (L.) dry acetone extract (F-UBA) and to investigate their anticancer potential for possible use in oral cancer therapy. U. barbata dry acetone extract (UBA) was solubilized in ethanol: isopropanol mixture and loaded in a formulation containing hydroxypropyl methylcellulose (HPMC) K100 and polyethylene glycol 400 (PEG 400). The UBA influence on the F-UBA pharmaceutical characteristics was evidenced compared with the references, i.e., mucoadhesive oral films containing suitable excipients but no active ingredient loaded. Both films were subjected to a complex analysis using standard methods to evaluate their suitability for topical administration on the oral mucosa. Physico-chemical and structural characterization was achieved by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), and atomic force microscopy (AFM). Pharmacotechnical evaluation (consisting of the measurement of specific parameters: weight uniformity, thickness, folding endurance, tensile strength, elongation, moisture content, pH, disintegration time, swelling rate, and ex vivo mucoadhesion time) proved that F-UBAs are suitable for oral mucosal administration. The brine shrimp lethality (BSL) assay was the F-UBA cytotoxicity prescreen. Cellular oxidative stress, caspase 3/7 activity, nuclear condensation, lysosomal activity, and DNA synthesis induced by F-UBA in blood cell cultures and oral epithelial squamous cell carcinoma (CLS-354) cell line were investigated through complex flow cytometry analyses. Moreover, F-UBA influence on both cell type division and proliferation was determined. Finally, using the resazurin-based 96-well plate microdilution method, the F-UBA antimicrobial potential was explored against Staphylococcus aureus ATCC 25923, Pseudomonas aeruginosa ATCC 27353, Candida albicans ATCC 10231, and Candida parapsilosis ATCC 22019. The results revealed that each UBA-loaded film contains 175 µg dry extract with a usnic acid (UA) content of 42.32 µg. F-UBAs are very thin (0.060 ± 0.002 mm), report a neutral pH (7.01 ± 0.01), a disintegration time of 146 ± 5.09 s, and an ex vivo mucoadhesion time of 85 ± 2.33 min, and they show a swelling ratio after 6 h of 211 ± 4.31%. They are suitable for topical administration on the oral mucosa. Like UA, they act on CLS-354 tumor cells, considerably increasing cellular oxidative stress, nuclear condensation, and autophagy and inducing cell cycle arrest in G0/G1. The F-UBAs inhibited the bacterial and fungal strains in a dose-dependent manner; they showed similar effects on both Candida sp. and higher inhibitory activity against P. aeruginosa than S. aureus. All these properties lead to considering the UBA-loaded mucoadhesive oral films suitable for potential application as a complementary therapy in OSCC.

  • Antibiofilm Activity of Biocide Metal Ions Containing Bioactive Glasses (BGs): A Mini Review
    Irina Atkinson

    MDPI AG
    One of the major clinical issues during the implantation procedure is the bacterial infections linked to biofilms. Due to their tissue localization and the type of bacteria involved, bacterial infections at implant sites are usually difficult to treat, which increases patient morbidity and even mortality. The difficulty of treating biofilm-associated infections and the emergence of multidrug-resistant bacteria are further challenges for the scientific community to develop novel biomaterials with excellent biocompatibility and antibacterial properties. Given their ability to stimulate bone formation and have antibacterial properties, metal ion-doped bioactive glasses (BGs) have received considerable research. This mini review aims to be successful in presenting the developments made about the role of biocide metal ions incorporated into BGs against the development of bacterial biofilms and the spread of nosocomial diseases.

  • The Influence of the Polymer Type on the Quality of Newly Developed Oral Immediate-Release Tablets Containing Amiodarone Solid Dispersions Obtained by Hot-Melt Extrusion
    Ancuța Cătălina Fița, Ana Andreea Secăreanu, Adina Magdalena Musuc, Emma Adriana Ozon, Iulian Sarbu, Irina Atkinson, Adriana Rusu, Erand Mati, Valentina Anuta, and Anca Lucia Pop

    MDPI AG
    The present study aims to demonstrate the influence of the polymer-carrier type and proportion on the quality performance of newly developed oral immediate-release tablets containing amiodarone solid dispersions obtained by hot-melt extrusion. Twelve solid dispersions including amiodarone and different polymers (PEG 1500, PEG 4000; PEG 8000, Soluplus®, and Kolliphor® 188) were developed and prepared by hot-melt extrusion using a horizontal extruder realized by the authors in their own laboratory. Only eleven of the dispersions presented suitable physical characteristics and they were used as active ingredients in eleven tablet formulations that contain the same amounts of the same excipients, varying only in solid dispersion type. The solid dispersions’ properties were established by optical microscopy with reflected light, volumetric controls and particle size evaluation. In order to prove that the complex powders have appropriate physical characteristics for the direct compression process, they were subjected to different analyses regarding their flowability and compressibility behavior. Additionally, the Fourier transform infrared spectroscopy and X-ray diffraction analysis were performed on the obtained solid dispersions. After confirming the proper physical attributes for all blends, they were processed into the form of tablets by direct compression technology. The manufactured tablets were evaluated for pharmacotechnical (dimensions–diameter and thickness, mass uniformity, hardness and friability) and in vitro biopharmaceutical (disintegration time and drug release) performances. Furthermore, the influence of the polymer matrix on their quality was determined. The high differences in flow and compression performances of the solid dispersions prove the relevant influence of the polymer type and their concentration-dependent plasticizing properties. The increase in flowability and compressibility characteristics of the solid dispersions could be noticed after combining them with direct compression excipients owning superior mechanical qualities. The influence of the polymer type is best detected in the disintegration test, where the obtained values are quite different between the studied formulations. The use of PEG 1500 alone or combined in various proportions with Soluplus® leads to rapid disintegration. In contrast, the mixture of PEG 4000 and Poloxamer 188 in equal proportions determined the increase in disintegration time to 120 s. The use of Poloxamer 188 alone and a 3:1 combination of PEG 4000 and Soluplus® also generates a prolonged disintegration time for the tablets.

  • Design, Characterization, and Anticancer and Antimicrobial Activities of Mucoadhesive Oral Patches Loaded with Usnea barbata (L.) F. H. Wigg Ethanol Extract F-UBE-HPMC
    Violeta Popovici, Elena Matei, Georgeta Camelia Cozaru, Laura Bucur, Cerasela Elena Gîrd, Verginica Schröder, Emma Adriana Ozon, Mirela Adriana Mitu, Adina Magdalena Musuc, Simona Petrescu,et al.

    MDPI AG
    The oral cavity’s common pathologies are tooth decay, periodontal disease, and oral cancer; oral squamous cell carcinoma (OSCC) is the most frequent oral malignancy, with a high mortality rate. Our study aims to formulate, develop, characterize, and pharmacologically investigate the oral mucoadhesive patches (F-UBE-HPMC) loaded with Usnea barbata (L.) F.H. Wigg dry ethanol extract (UBE), using HPMC K100 as a film-forming polymer. Each patch contains 312 µg UBE, with a total phenolic content (TPC) of 178.849 µg and 33.924 µg usnic acid. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) were performed for their morphological characterization, followed by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and thermogravimetric analysis (TGA). Pharmacotechnical evaluation involved the measurement of the specific parameters for mucoadhesive oral patches as follows: weight uniformity, thickness, folding endurance, tensile strength, elongation, moisture content, pH, disintegration time, swelling rate, and ex vivo mucoadhesion time. Thus, each F-UBE-HPMC has 104 ± 4.31 mg, a pH = 7.05 ± 0.04, a disintegration time of 130 ± 4.14 s, a swelling ratio of 272 ± 6.31% after 6 h, and a mucoadhesion time of 102 ± 3.22 min. Then, F-UBE-HPMCs pharmacological effects were investigated using brine shrimp lethality assay (BSL assay) as a cytotoxicity prescreening test, followed by complex flow cytometry analyses on blood cell cultures and oral epithelial squamous cell carcinoma CLS-354 cell line. The results revealed significant anticancer effects by considerably increasing oxidative stress and blocking DNA synthesis in CLS-354 cancer cells. The antimicrobial potential against Staphylococcus aureus ATCC 25923, Pseudomonas aeruginosa ATCC 27353, Candida albicans ATCC 10231, and Candida parapsilosis ATCC 22019 was assessed by a Resazurin-based 96-well plate microdilution method. The patches moderately inhibited both bacteria strains growing and displayed a significant antifungal effect, higher on C. albicans than on C. parapsilosis. All these properties lead to considering F-UBE-HPMC suitable for oral disease prevention and therapy.

  • Formulation and Development of Bioadhesive Oral Films Containing Usnea barbata (L.) F.H.Wigg Dry Ethanol Extract (F-UBE-HPC) with Antimicrobial and Anticancer Properties for Potential Use in Oral Cancer Complementary Therapy
    Violeta Popovici, Elena Matei, Georgeta-Camelia Cozaru, Laura Bucur, Cerasela Elena Gîrd, Verginica Schröder, Emma Adriana Ozon, Iulian Sarbu, Adina Magdalena Musuc, Irina Atkinson,et al.

    MDPI AG
    Medical research explores plant extracts’ properties to obtain potential anticancer drugs. The present study aims to formulate, develop, and characterize the bioadhesive oral films containing Usnea barbata (L.) dry ethanol extract (F-UBE-HPC) and to investigate their anticancer potential for possible use in oral cancer therapy. The physicochemical and morphological properties of the bioadhesive oral films were analyzed through Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), Atomic Force Microscopy (AFM), thermogravimetric analysis (TG), and X-ray diffraction techniques. Pharmacotechnical evaluation (consisting of the measurement of the specific parameters: weight uniformity, thickness, folding endurance, tensile strength, elongation, moisture content, pH, disintegration time, swelling rate, and ex vivo mucoadhesion time) completed the bioadhesive films’ analysis. Next, oxidative stress, caspase 3/7 activity, nuclear condensation, lysosomal activity, and DNA synthesis induced by F-UBE-HPC in normal blood cell cultures and oral epithelial squamous cell carcinoma (CLS-354) cell line and its influence on both cell types’ division and proliferation was evaluated. The results reveal that each F-UBE-HPC contains 0.330 mg dry extract with a usnic acid (UA) content of 0.036 mg. The bioadhesive oral films are thin (0.093 ± 0.002 mm), reveal a neutral pH (7.10 ± 0.02), a disintegration time of 118 ± 3.16 s, an ex vivo bioadhesion time of 98 ± 3.58 min, and show a swelling ratio after 6 h of 289 ± 5.82%, being suitable for application on the oral mucosa. They displayed in vitro anticancer activity on CLS-354 tumor cells. By considerably increasing cellular oxidative stress and caspase 3/7 activity, they triggered apoptotic processes in oral cancer cells, inducing high levels of nuclear condensation and lysosomal activity, cell cycle arrest in G0/G1, and blocking DNA synthesis. All these properties lead to considering the UBE-loaded bioadhesive oral films suitable for potential application as a complementary therapy in oral cancer.