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Search Results (381)

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9 pages, 1081 KiB  
Brief Report
Shoots Regeneration in Brigitta and Duke Blueberry Cultivars from Different Encapsulated Vegetative Propagules
by Luca Regni, Arianna Cesarini, Silvia Calisti, Primo Proietti and Maurizio Micheli
Horticulturae 2025, 11(3), 259; https://doi.org/10.3390/horticulturae11030259 - 28 Feb 2025
Viewed by 163
Abstract
Synthetic seed technology, an advanced in vitro propagation method, combines the benefits of micropropagation with the practicality of zygotic seeds, offering an efficient solution for the handling, storage, and transportation of plant propagules. This study represents the first investigation of the role of [...] Read more.
Synthetic seed technology, an advanced in vitro propagation method, combines the benefits of micropropagation with the practicality of zygotic seeds, offering an efficient solution for the handling, storage, and transportation of plant propagules. This study represents the first investigation of the role of explant type in blueberry encapsulation. In particular, three non-embryogenic propagules (basal node, median node, and shoot tip) were evaluated in the Brigitta and Duke blueberry cultivars. The artificial endosperm consists of Woody Plant Medium (WPM) macro- and micro-nutrients and Murashige and Skoog vitamins at half concentration, inositol (5 g L−1), Indole-3-butyric acid (IBA) (0.005 mg L−1), zeatin (0.25 mg L−1), and sucrose (50 g L−1). Forty-five days after sowing in in vitro conditions, the encapsulated shoot tips showed better results than basal and median nodes in several parameters, including viability, shoot length, and fresh shoot weight, in both cultivars. In both cultivars, none of the encapsulated propagule types developed roots. These results underscore the advantages of using shoot tips in encapsulation technology for blueberries and provide valuable insights for optimizing encapsulation protocols to improve propagation efficiency. Full article
(This article belongs to the Special Issue In Vitro Culture for Small Fruits Plants: Challenges and Perspectives)
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Figure 1
<p>Shoots obtained from the encapsulated shoot tip (<b>a</b>,<b>d</b>), median node (<b>b</b>,<b>e</b>), and basal node (<b>c</b>,<b>f</b>) of the Brigitta cultivar.</p>
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<p>Shoots obtained from encapsulated shoot tip (<b>a</b>,<b>d</b>), median node (<b>b</b>,<b>e</b>), and basal node (<b>c</b>,<b>f</b>) of the Duke cultivar.</p>
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22 pages, 2751 KiB  
Article
Valorization of Banana Peel Waste into Advanced Adsorbent Beads for the Removal of Emerging Pollutants from Wastewater
by Olivia Boyle, Bo Xiao and Chirangano Mangwandi
Materials 2025, 18(5), 1084; https://doi.org/10.3390/ma18051084 - 28 Feb 2025
Viewed by 189
Abstract
This study addresses environmental concerns by utilizing banana peel waste to develop innovative adsorbent materials for wastewater treatment, aligning with circular economy principles. Spherical beads were synthesized from sodium alginate mixed with various banana peel-based materials, including pure powder (PBP), activated carbon (AC), [...] Read more.
This study addresses environmental concerns by utilizing banana peel waste to develop innovative adsorbent materials for wastewater treatment, aligning with circular economy principles. Spherical beads were synthesized from sodium alginate mixed with various banana peel-based materials, including pure powder (PBP), activated carbon (AC), and magnetic activated carbon (MAC). These beads were evaluated for their efficiency in removing tetracycline (TC) and hexavalent chromium (Cr(VI)) as model pollutants representing antibiotics and heavy metals, respectively. Characterization of the beads revealed functional groups and thermal stability conducive to effective adsorption. Adsorption trials demonstrated that MAC beads achieved the highest removal efficiencies, up to 92% for TC and 79% for Cr(VI). The adsorption process followed pseudo-second-order kinetics and Langmuir isotherms. Remarkably, the beads retained a significant adsorption capacity across reuse cycles, indicating their regenerative potential. Comparisons with other adsorbents highlight the competitive performance of these banana peel-based materials. The results emphasize the potential of banana peel-derived adsorbents as cost-effective, sustainable solutions for mitigating emerging pollutants in water systems, promoting waste valorization and environmental protection. The research demonstrates a novel approach to sequential adsorption without intermediate regeneration, showing that the beads can effectively remove both tetracycline and chromium (VI) in successive cycles. This finding is particularly significant because it reveals that the presence of previously adsorbed chromium actually enhanced the beads’ capacity for tetracycline removal in the second cycle, suggesting a synergistic effect that had not been previously reported in the literature. These innovations contribute meaningfully to both waste valorization and water treatment technologies, offering new insights into the development of multi-functional adsorbents from agricultural waste materials. Full article
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Figure 1
<p>FTIR spectra for (<b>a</b>) banana peel powder and (<b>b</b>) magnetic activated carbon beads.</p>
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<p>TGA thermograph of the MAC@NaAlg beads.</p>
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<p>Comparison of the (<b>a</b>) TC removal efficiency and (<b>b</b>) TC adsorption capacity of the different materials.</p>
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<p>Comparison of the (<b>a</b>) Cr (VI) removal efficiency and (<b>b</b>) Cr(VI) adsorption capacity of the different materials.</p>
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<p>Effect of initial concentration of Cr(VI) on its removal by various beads. Study performed at room temperature with dosage of adsorbent beads of 2.5 g/L.</p>
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<p>Effect of initial concentration of tetracycline on its removal by various beads. Study performed at room temperature with dosage of adsorbent beads of 2.5 g/L.</p>
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<p>Freundlich model fit to the Cr adsorption experimental data for the different types of beads.</p>
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<p>Freundlich model fit to the TC adsorption experimental data for the different types of beads.</p>
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<p>Removal efficiency of various beads in the 2nd cycle after adsorption of another pollutant (<b>a</b>) Cr(VI) followed by TC (<b>b</b>) TC followed by Cr(VI).</p>
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22 pages, 8422 KiB  
Article
Alginate Microbeads for Trapping Phenolic Antioxidants in Rosemary (Rosmarinus officinalis L.): Multivariate Optimization Based on Bioactive Properties and Morphological Measurements
by Gizem Toprakçı, İrem Toprakçı and Selin Şahin
Gels 2025, 11(3), 172; https://doi.org/10.3390/gels11030172 - 27 Feb 2025
Viewed by 220
Abstract
Medical and aromatic plant extracts are often very sensitive to environmental, gastrointestinal, and processing conditions despite their health benefits. Therefore, they can be rapidly inactivated. Microencapsulation is used to overcome such challenges. In this study, phenolic antioxidants from rosemary (Rosmarinus officinalis L.) [...] Read more.
Medical and aromatic plant extracts are often very sensitive to environmental, gastrointestinal, and processing conditions despite their health benefits. Therefore, they can be rapidly inactivated. Microencapsulation is used to overcome such challenges. In this study, phenolic antioxidants from rosemary (Rosmarinus officinalis L.) were encapsulated in alginate beads by means of ionic gelation. A Box–Behnken design with response surface methodology (BBD–RSM) was used with three numeric factors (calcium chloride concentration, alginate concentration, and hardening time) to achieve the best formulation in terms of encapsulation efficiency, antioxidant activity, and morphological characteristics. Generally, the sodium alginate concentration of the microbeads was the most critical factor (p < 0.0001) for the quality of the products. The optimal encapsulation conditions were accessed using concentrations with almost 6% calcium chloride and 2% alginate, and a time of 10 min for bead hardening in order to obtain the highest responses (30.01% encapsulation efficiency, 7.55 mg-TEAC/g-DM of antioxidant activity value as measured by the DPPH method, a sphericity factor of 0.05, and a roundness of 0.78). At the optimum point, the microbeads were determined to be spherical in shape, and the bulk density value was measured as 0.34 ± 0.01 g/mL. Full article
(This article belongs to the Special Issue Functional Gels Loaded with Natural Products)
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<p>Influence of calcium chloride (<b>a</b>), sodium alginate (<b>b</b>), and time (<b>c</b>) on encapsulation efficiency.</p>
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<p>Influence of calcium chloride (<b>a</b>), sodium alginate (<b>b</b>), and time (<b>c</b>) on antioxidant activity.</p>
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<p>Influence of calcium chloride (<b>a</b>), sodium alginate, (<b>b</b>) and time (<b>c</b>) on the sphericity factor.</p>
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<p>Influence of calcium chloride (<b>a</b>), sodium alginate, (<b>b</b>) and time (<b>c</b>) on roundness.</p>
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<p>Effects of calcium chloride concentration and sodium alginate concentration on the (<b>a</b>) encapsulation efficiency, (<b>b</b>) antioxidant activity, (<b>c</b>) sphericity factor (SF), and (<b>d</b>) roundness (Rn) values of the microcapsules, including the phenolic antioxidant-rich extract from rosemary (<span class="html-italic">Rosmarinus officinalis</span> L.).</p>
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<p>Effects of calcium chloride concentration and sodium alginate concentration on the (<b>a</b>) encapsulation efficiency, (<b>b</b>) antioxidant activity, (<b>c</b>) sphericity factor (SF), and (<b>d</b>) roundness (Rn) values of the microcapsules, including the phenolic antioxidant-rich extract from rosemary (<span class="html-italic">Rosmarinus officinalis</span> L.).</p>
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<p>Effects of the calcium chloride concentration and hardening time on the (<b>a</b>) encapsulation efficiency, (<b>b</b>) antioxidant activity, (<b>c</b>) sphericity factor (SF), and (<b>d</b>) roundness (Rn) values of the microcapsules, including the phenolic antioxidant-rich extract from rosemary (<span class="html-italic">Rosmarinus officinalis</span> L.).</p>
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<p>Effects of the calcium chloride concentration and hardening time on the (<b>a</b>) encapsulation efficiency, (<b>b</b>) antioxidant activity, (<b>c</b>) sphericity factor (SF), and (<b>d</b>) roundness (Rn) values of the microcapsules, including the phenolic antioxidant-rich extract from rosemary (<span class="html-italic">Rosmarinus officinalis</span> L.).</p>
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<p>Effects of the sodium alginate concentration and hardening time on the (<b>a</b>) encapsulation efficiency, (<b>b</b>) antioxidant activity, (<b>c</b>) sphericity factor (SF), and (<b>d</b>) roundness (Rn) values of the microcapsules, including the phenolic antioxidant-rich extract from rosemary (<span class="html-italic">Rosmarinus officinalis</span> L.).</p>
Full article ">Figure 7 Cont.
<p>Effects of the sodium alginate concentration and hardening time on the (<b>a</b>) encapsulation efficiency, (<b>b</b>) antioxidant activity, (<b>c</b>) sphericity factor (SF), and (<b>d</b>) roundness (Rn) values of the microcapsules, including the phenolic antioxidant-rich extract from rosemary (<span class="html-italic">Rosmarinus officinalis</span> L.).</p>
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<p>Perturbation plot for the (<b>a</b>) encapsulation efficiency, (<b>b</b>) antioxidant activity, (<b>c</b>) sphericity factor (SF), and (<b>d</b>) roundness (Rn) values of the microcapsules, including a phenolic antioxidant-rich extract from rosemary (<span class="html-italic">Rosmarinus officinalis</span> L.).</p>
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<p>Perturbation plot for the (<b>a</b>) encapsulation efficiency, (<b>b</b>) antioxidant activity, (<b>c</b>) sphericity factor (SF), and (<b>d</b>) roundness (Rn) values of the microcapsules, including a phenolic antioxidant-rich extract from rosemary (<span class="html-italic">Rosmarinus officinalis</span> L.).</p>
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<p>Pareto chart for the (<b>a</b>) encapsulation efficiency, (<b>b</b>) antioxidant activity, (<b>c</b>) sphericity factor (SF), and (<b>d</b>) roundness (Rn) values of the microcapsules, including a phenolic antioxidant-rich extract from rosemary (<span class="html-italic">Rosmarinus officinalis</span> L.).</p>
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<p>Pareto chart for the (<b>a</b>) encapsulation efficiency, (<b>b</b>) antioxidant activity, (<b>c</b>) sphericity factor (SF), and (<b>d</b>) roundness (Rn) values of the microcapsules, including a phenolic antioxidant-rich extract from rosemary (<span class="html-italic">Rosmarinus officinalis</span> L.).</p>
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15 pages, 4231 KiB  
Article
Microstructure and Release Behavior of Alginate–Natural Hydrocolloid Composites: A Comparative Study
by Hatice Sıçramaz, Ali Baran Dönmez, Buse Güven, Derya Ünal and Elif Aşbay
Polymers 2025, 17(4), 531; https://doi.org/10.3390/polym17040531 - 18 Feb 2025
Viewed by 292
Abstract
This study investigated the effects of combining sodium alginate (ALG) with various natural hydrocolloids on the microstructure and release behaviors of microbeads. The encapsulation solutions were prepared at a 1:1 (w/w) ratio with ALG as the control and carrageenan [...] Read more.
This study investigated the effects of combining sodium alginate (ALG) with various natural hydrocolloids on the microstructure and release behaviors of microbeads. The encapsulation solutions were prepared at a 1:1 (w/w) ratio with ALG as the control and carrageenan (CAR), locust bean gum (LBG), acacia gum (ACA), pectin (PEC), and carboxymethyl cellulose (CMC) as experimental groups. Each formulation contained 0.2% (w/v) tartrazine and was extruded into a CaCl2 solution for bead production. Encapsulation efficiency varied across formulations, with the lowest in the control (ALG-ALG) and highest in ALG-CAR and ALG-CMC, reaching 74% and 78%, respectively. The microbead sizes ranged from 2.07 to 3.48 mm, with the lowest particle diameter observed in ALG-ACA composites. Surface analysis showed smooth and uniform microbeads in the control (ALG-ALG), while ALG-LBG microbeads were rougher. Release kinetics were assessed using various models, with the Higuchi model best describing the release for most formulations (highest R2 values). Tartrazine release followed pseudo-Fickian behavior in all formulations, with slower release in ALG-ACA and faster release in ALG-LBG microbeads. This study fills a gap in understanding how the incorporation of different natural hydrocolloids influences both the encapsulation efficiency and release dynamics of alginate-based microbeads, providing valuable insights for applications in food and pharmaceutical industries. Full article
(This article belongs to the Special Issue Development of Polymer Materials as Functional Coatings)
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Graphical abstract

Graphical abstract
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<p>The optical microscopic images of alginate microparticles at a magnification of 4×.</p>
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<p>SEM images of microbeads at (<b>a</b>) 100× (except ALG-ACA, which was monitored at 250×), (<b>b</b>) 2000×, (<b>c</b>) 8000×.</p>
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<p>SEM images of microbeads at (<b>a</b>) 100× (except ALG-ACA, which was monitored at 250×), (<b>b</b>) 2000×, (<b>c</b>) 8000×.</p>
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<p>FTIR spectra of microbeads at (<b>a</b>) 1500–3900 and (<b>b</b>) 500–1500 cm<sup>−1</sup>.</p>
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<p>Chemical structure of tartrazine.</p>
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<p>DSC curves of microbeads.</p>
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<p>Encapsulation efficiencies (EEs%) of microbeads. Different letters “a–c” represent statistical differences according to Tukey’s test (<span class="html-italic">p</span> &lt; 0.05).</p>
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<p>Release profiles of tartrazine from microbeads.</p>
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21 pages, 9468 KiB  
Article
Development and Evaluation of Magnetite Loaded Alginate Beads Based Nanocomposite for Enhanced Targeted Analgesic Drug Delivery
by Amrita Das, Prateep Sengupta, Shreya Chatterjee, Jasmina Khanam, Pranab Kumar Mondal, Eder Lilia Romero, Anton M. Manakhov, Sabu Thomas, Syed Mahmood and Kajal Ghosal
Magnetochemistry 2025, 11(2), 14; https://doi.org/10.3390/magnetochemistry11020014 - 13 Feb 2025
Viewed by 514
Abstract
Iron oxide-based nanoparticles, such as magnetic nanoparticles (MNPs), have gained significant attention in the area of drug delivery due to their unique magnetic properties, allowing for precise targeting and controlled release of therapeutic agents. Several successful research studies were reported with combinations of [...] Read more.
Iron oxide-based nanoparticles, such as magnetic nanoparticles (MNPs), have gained significant attention in the area of drug delivery due to their unique magnetic properties, allowing for precise targeting and controlled release of therapeutic agents. Several successful research studies were reported with combinations of magnetic nanoparticles and polysaccharides such as sodium alginate, chitosan, cellulose, etc. The presented research work is based on synthesising MNPs via the co-precipitation method and their successful encapsulation within alginate beads, serving as a promising drug delivery system for aceclofenac, a model drug. The physical and chemical characteristics of both the prepared magnetite nanoparticles and the aceclofenac-loaded MNPs alginate beads were thoroughly examined using scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), Fourier-transform infrared spectroscopy (FTIR), powder X-ray diffraction (PXRD), and vibrating sample magnetometry (VSM). Furthermore, a drug release study was conducted to evaluate the release kinetics of aceclofenac from the prepared MNP alginate beads. The magnetic characteristics of magnetite and MNP beads shed light on the potential application of novel drug delivery systems for magnetically targeted therapeutic interventions. The present research offers valuable insights into the development of magnetic nanoparticle-based drug carriers, paving the way for enhanced drug delivery strategies in the field of pharmaceutical sciences. Full article
(This article belongs to the Section Applications of Magnetism and Magnetic Materials)
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<p>Structure of sodium alginate.</p>
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<p>Procedure for preparing magnetic beads coated with sodium alginate.</p>
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<p>Standard calibration curve of aceclofenac in phosphate buffer solution of pH 6.8.</p>
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<p>Dried magnetic nanoparticle beads. (<b>A</b>) blank, (<b>B</b>) F1, (<b>C</b>) F2.</p>
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<p>Magnetic nanoparticles beads under the microscope. (<b>a</b>) Blank, (<b>b</b>) F1, (<b>c</b>) F2. The visible inner whitish circular objects v are magnetic nanoparticle beads.</p>
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<p>SEM images of MNP beads. (<b>a</b>) F1, (<b>b</b>) F2, (<b>c</b>) magnified surface of F1 and (<b>d</b>) magnified surface of F2.</p>
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<p>HRTEM images of F2.</p>
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<p>EDX analysis of F2 sample.</p>
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<p>AFM 3D image and height distribution of prepared formulations. (<b>a</b>) AFM 3D image of F1; (<b>b</b>) AFM 3D image of F2; (<b>c</b>) height distribution of F1; (<b>d</b>) height distribution of F2.</p>
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<p>pXRD spectra of aceclofenac, blank, F1, and F2.</p>
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<p>FTIR spectrum of aceclofenac (drug), blank, F1, and F2.</p>
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<p>Magnetite displayed magnetic characteristics by being attracted to an external magnet. (<b>a</b>) The magnetite solution in the absence of an external magnet. (<b>b</b>) The magnetite solution in the presence of an external magnet. (<b>c</b>) Dried magnetite is attracted to external magnetic beads.</p>
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<p>Variations in magnetisation property as a result of the applied magnetic field. Ms = Saturation magnetization, Mr = Remanence mag, Hc = Coercivity.</p>
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<p>% Cumulative drug release vs. Time of F1 and F2.</p>
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16 pages, 3545 KiB  
Article
Enhancing Viability of Lactobacillus rhamnosus GG and Total Polyphenol Content in Fermented Black Goji Berry Beverage Through Calcium–Alginate Encapsulation with Hydrocolloids
by Charoonsri Chusak, Vernabelle Balmori, Kritmongkhon Kamonsuwan, Phim on Suklaew and Sirichai Adisakwattana
Foods 2025, 14(3), 518; https://doi.org/10.3390/foods14030518 - 6 Feb 2025
Viewed by 915
Abstract
Encapsulation techniques play a crucial role in enhancing the stability and viability of probiotics in functional foods. This study investigates the efficacy of calcium–alginate encapsulation, combined with hydrocolloids such as carrageenan, agar, and gelatin, in improving the survival of Lactobacillus rhamnosus GG (LGG) [...] Read more.
Encapsulation techniques play a crucial role in enhancing the stability and viability of probiotics in functional foods. This study investigates the efficacy of calcium–alginate encapsulation, combined with hydrocolloids such as carrageenan, agar, and gelatin, in improving the survival of Lactobacillus rhamnosus GG (LGG) and stabilizing the total phenolic content (TPC) in fermented black goji berry beverages. The results revealed that 1.5% alginate encapsulation, combined with 1% carrageenan, agar, or gelatin and 5% calcium, significantly enhanced the LGG viability and increased the TPC content in the fermented black goji berry beads when compared to calcium–alginate encapsulation alone. Fourier Transform Infrared Spectroscopy (FTIR) confirmed the successful incorporation and interaction of hydrocolloids within the encapsulation matrix. Among the formulations, calcium–alginate–gelatin beads exhibited the highest LGG survival rates after simulated gastric and intestinal digestion. Notably, calcium–alginate beads containing carrageenan preserved LGG viability during simulated gastric and intestinal conditions when co-digested with all tested milk types (high carbohydrate, high protein, and high fat). Co-ingestion with these milk types further improved TPC retention in all bead formulations, as the macronutrients in milk provided protective effects, stabilizing the encapsulated polyphenols and minimizing their degradation during simulated gastric and intestinal digestion. This study highlights the potential of calcium–alginate encapsulation, integrated with hydrocolloids such as carrageenan, agar, or gelatin, to improve probiotic viability and polyphenol stability, offering promising applications for enhancing the functional properties of non-dairy fermented beverages. Full article
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<p>A schematic representation of the encapsulation process for fermented black goji berry in a calcium–alginate system with hydrocolloids.</p>
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<p>(<b>A</b>) Viability of <span class="html-italic">Lactobacillus rhamnosus</span> GG (LGG) and (<b>B</b>) total polyphenol content (TPC) in the encapsulated beads, comparing 1.2% alginate (Ag) and 1.5% Ag with 1% hydrocolloids. Data are expressed as the mean ± standard error of the mean (SEM) (n = 3). Different letters indicate significant differences between 1.2% Ag and 1.5% Ag at <span class="html-italic">p</span> &lt; 0.05. C: carrageenan; A: agar; G: gelatin.</p>
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<p>(<b>A</b>) Scanning Electron Microscopy (SEM) images of 1.5% Ag (alginate), 1.5% Ag + 1% C (carrageenan), 1.5% Ag + 1% A (agar), and 1.5% Ag + 1% G (gelatin) encapsulated beads. The overall structure is shown at 30× magnification (left), surface morphology at 2000× magnification (middle), and cross-section at 10,000× magnification (right). (<b>B</b>) FT-IR spectra of 1.5% Ag, 1.5% Ag + 1% C, and C encapsulated beads. (<b>C</b>) FT-IR spectra of 1.5% Ag, 1.5% Ag + 1% A, and A encapsulated beads. (<b>D</b>) FT-IR spectra of 1.5% Ag, 1.5% Ag + 1% G, and G encapsulated beads.</p>
Full article ">Figure 3 Cont.
<p>(<b>A</b>) Scanning Electron Microscopy (SEM) images of 1.5% Ag (alginate), 1.5% Ag + 1% C (carrageenan), 1.5% Ag + 1% A (agar), and 1.5% Ag + 1% G (gelatin) encapsulated beads. The overall structure is shown at 30× magnification (left), surface morphology at 2000× magnification (middle), and cross-section at 10,000× magnification (right). (<b>B</b>) FT-IR spectra of 1.5% Ag, 1.5% Ag + 1% C, and C encapsulated beads. (<b>C</b>) FT-IR spectra of 1.5% Ag, 1.5% Ag + 1% A, and A encapsulated beads. (<b>D</b>) FT-IR spectra of 1.5% Ag, 1.5% Ag + 1% G, and G encapsulated beads.</p>
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<p>(<b>A</b>) Viability of <span class="html-italic">Lactobacillus rhamnosus</span> GG (LGG) and (<b>B</b>) total polyphenol content (TPC) in the encapsulated beads before and after 180 min of in vitro simulated gastric and intestinal digestion. Data are expressed as the mean ± SEM (n = 3). Different letters indicate statistically significant differences at <span class="html-italic">p</span> &lt; 0.05. Uppercase letters (A–C) indicate comparisons between 1.5% Ag, 1.5% Ag + 1% C, 1.5% Ag + 1% A, and 1.5% Ag + 1% G before or after digestion. Lowercase letters (a,b) represent comparisons between before and after digestion within the same sample.</p>
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<p>Effect of co-ingestion with different milk types (high carbohydrate (HC), high protein (HP), and high fat (HF)) on (<b>A</b>) the viability of <span class="html-italic">Lactobacillus rhamnosus</span> GG (LGG) and (<b>B</b>) total polyphenol content (TPC) in the encapsulated beads after in vitro simulated gastric and intestinal digestion. Control refers to beads in water. Data are presented as the mean ± standard error of the mean (SEM) (n = 3). Statistical differences are denoted by different superscript letters (<span class="html-italic">p</span> &lt; 0.05).</p>
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20 pages, 4307 KiB  
Article
Preparation and Biochemical Characterization of Penicillium crustosum Thom P22 Lipase Immobilization Using Adsorption, Encapsulation, and Adsorption–Encapsulation Approaches
by Ismail Hasnaoui, Sondes Mechri, Ahlem Dab, Nour Eddine Bentouhami, Houssam Abouloifa, Reda Bellaouchi, Fawzi Allala, Ennouamane Saalaoui, Bassem Jaouadi, Alexandre Noiriel, Abdeslam Asehraou and Abdelkarim Abousalham
Molecules 2025, 30(3), 434; https://doi.org/10.3390/molecules30030434 - 21 Jan 2025
Viewed by 867
Abstract
This work describes the immobilization and the characterization of purified Penicillium crustosum Thom P22 lipase (PCrL) using adsorption, encapsulation, and adsorption–encapsulation approaches. The maximum activity of the immobilized PCrL on CaCO3 microspheres and sodium alginate beads was shifted from 37 to 45 [...] Read more.
This work describes the immobilization and the characterization of purified Penicillium crustosum Thom P22 lipase (PCrL) using adsorption, encapsulation, and adsorption–encapsulation approaches. The maximum activity of the immobilized PCrL on CaCO3 microspheres and sodium alginate beads was shifted from 37 to 45 °C, compared with that of the free enzyme. When sodium alginate was coupled with zeolite or chitosan, the immobilization yield reached 100% and the immobilized PCrL showed improved stability over a wide temperature range, retaining all of its initial activity after a one-hour incubation at 60 °C. The immobilization of PCrL significantly improves its catalytic performance in organic solvents, its pH tolerance value, and its thermal stability. Interestingly, 95% and almost 50% of PCrL’s initial activity was retained after 6 and 12 cycles, respectively. The characteristics of all PCrL forms were analyzed by X-ray diffraction and scanning electron microscopy combined with energy dispersive spectroscopy. The maximum conversion efficiency of oleic acid and methanol to methyl esters (biodiesel), by PCrL immobilized on CaCO3, was 65% after a 12 h incubation at 40 °C, while free PCrL generated only 30% conversion, under the same conditions. Full article
(This article belongs to the Section Macromolecular Chemistry)
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Figure 1
<p>Adsorption kinetics of PCrL on CaCO<sub>3</sub> and Celite 545. PCrL adsorbed on CaCO<sub>3</sub> leads to the highest yield of 90% after 30 min of incubation (4500 U) at 4 °C. The lipase activity was measured with the pH-STAT technique using TC8 as the substrate.</p>
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<p>Identification of the PCrL-SA-ZE, PCrL-SA-CS, and PCrL-CaCO<sub>3</sub> beads. (<b>a</b>) The XRD patterns of the support beads alone (SA, SA-ZE, or SA-CS) or complexed with PCrL (PCrL-SA, PCrL-SA-ZE, and PCrL-SA-CS). The XRD patterns were generated using Match! software (version 3.10.2.173); (<b>b</b>) Identification of the support beads (SA, SA-CS, and SA-ZE) and those complexed with PCrL (PCrL-SA, PCrL-SA-CS, and PCrL-SA-ZE) in the FE-SEM images.</p>
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<p>The effect of temperature on PCrL activity and stability. (<b>a</b>) The temperature–activity profile. This graph shows the activity of the free and immobilized PCrL at different temperatures. The activity of the immobilized PCrL at its optimal temperature (45 °C) is set at 100%. (<b>b</b>) Temperature stability. This graph illustrates the stability of the free and immobilized PCrL after incubation at different temperatures for 60 min. The residual activity was measured at pH value 9 using TC8 as a substrate. Each data point on the graph represents the average of three independent experiments.</p>
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<p>The effect of pH on PCrL activity and stability. (<b>a</b>) The pH activity profile of the free and immobilized PCrL at different pH values. The maximum activity at pH value 9 is set at 100%. (<b>b</b>) pH value stability of the free and immobilized PCrL after incubation at different pH values for 1 h at 4 °C. The residual activity was measured at pH value 9 and 37 °C using TC8 as the substrate. Each data point represents the average of three independent experiments.</p>
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<p>The effect of organic solvents on PCrL-CaCO<sub>3</sub> activity and stability. The enzyme was incubated with 25% (<span class="html-italic">v</span>/<span class="html-italic">v</span>) of each solvent for 24 h. The residual activity was measured under standard conditions, using TC8 as the substrate at 37 °C and pH 9, as described in Material and Methods, and then expressed as a percentage of the activity without any solvents. Each data point represents the average of three independent experiments, with the error bars indicating standard deviation.</p>
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<p>Performance evaluation of PCrL-CaCO<sub>3</sub>. (<b>a</b>) The kinetics of oleic acid esterification catalyzed by the free PCrL and immobilized PCrL-CaCO<sub>3</sub>. The reaction was performed at 40 °C, with stirring for 24 h, using 500 U of enzyme in hexane with a 3:1 molar ratio of methanol to oleic acid. (<b>b</b>) The reusability of immobilized PCrL-CaCO<sub>3</sub> in multiple reaction cycles. The enzyme was reused for 12 cycles, with each cycle lasting 12 h. The conversion yield of oleic acid to esters was monitored for each cycle.</p>
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<p>The thermodynamic parameters of the target PCrL. An Arrhenius diagram of Ln (<span class="html-italic">k</span><sub>d</sub>) vs. 1/temperature to calculate the activation energy (E<sub>a</sub>).</p>
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20 pages, 5619 KiB  
Article
Alginate Hydrogel Beads with a Leakproof Gold Shell for Ultrasound-Triggered Release
by Marcus Flowers, Alex Paulsen, Claire R. W. Kaiser, Adam B. Tuma, Hubert H. Lim, Brenda M. Ogle and Chun Wang
Pharmaceutics 2025, 17(1), 133; https://doi.org/10.3390/pharmaceutics17010133 - 19 Jan 2025
Viewed by 591
Abstract
Background/Objectives: Focused ultrasound has advantages as an external stimulus for drug delivery as it is non-invasive, has high precision and can penetrate deep into tissues. Here, we report a gold-plated alginate (ALG) hydrogel system that retains highly water-soluble small-molecule fluorescein for sharp off/on [...] Read more.
Background/Objectives: Focused ultrasound has advantages as an external stimulus for drug delivery as it is non-invasive, has high precision and can penetrate deep into tissues. Here, we report a gold-plated alginate (ALG) hydrogel system that retains highly water-soluble small-molecule fluorescein for sharp off/on release after ultrasound exposure. Methods: The ALG is crosslinked into beads with calcium chloride and layered with a polycation to adjust the surface charge for the adsorption of catalytic platinum nanoparticles (Pt NPs). The coated bead is subject to electroless plating, forming a gold shell. Ultrasound is applied to the gold-plated ALG beads and the release of fluorescein with or without ultrasound stimulation is quantified. Results: Polyethylenimine (PEI), not poly-L-lysine (PLL), is able to facilitate Pt NP adsorption. Gold shell thickness is proportional to the duration of electroless plating and can be controlled. Gold-plated ALG beads are impermeable to the fluorescein cargo and have nearly zero leakage. Exposure to focused ultrasound initiated the release of fluorescein with full release achieved after 72 h. Conclusions: The gold-plated ALG hydrogel is a new material platform that can retain highly water-soluble molecules with a sharp off/on release initiated by focused ultrasound. Full article
(This article belongs to the Section Drug Delivery and Controlled Release)
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<p>Schematic illustration of the general approach to ultrasound-triggered release of drugs from alginate hydrogel beads with leakproof gold shell.</p>
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<p>A schematic illustration of the pathways of the synthesis of gold-plated ALG hydrogel beads. Representative photos of the beads at key stages of the synthesis are shown. Catalytic Pt NPs were adsorbed to the surface of ALG beads without or with a precoated polycation (PLL or PEI) followed by electroless plating. Only the ALG beads precoated with PEI succeeded in forming a contiguous gold shell. (<b>A</b>–<b>D</b>) Photos of ALG beads at various stages of the synthesis.</p>
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<p>Visible light photographs and SEM images of ALG hydrogel beads with or without the gold shell. The gold shell was formed after either 2 min or 10 min plating.</p>
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<p>Thickness of the gold shell as a function of electroless plating time. (<b>A</b>) Representative light microscopy images of the cross-section of gold-plated ALG hydrogel bead at various plating times. Red arrows in A indicate multiple locations of the shell where the thickness is measured. (<b>B</b>) A quantitative correlation between gold shell thickness and plating time. The dashed line is a linear fit of the data, which are the means ± SD of at least 5–20 measurements.</p>
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<p>Verification of the gold-plated ALG hydrogel beads with a leakproof shell. (<b>A</b>) Illustration of the leak test and its outcome. (<b>B</b>) Quantification of fluorescein leakage. Data representing mean ± SD. ***: <span class="html-italic">p</span> &lt; 0.001, Student’s <span class="html-italic">t</span> test (unpaired) and one-way ANOVA with Tukey–Kramer post hoc analysis, <span class="html-italic">n</span> &gt; 3 samples, with each sample measured in triplicate.</p>
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<p>Focused ultrasound experimental setup and ultrasound-generated spatial pressure profiles. (<b>A</b>) Graphic depiction of the experimental setup. (<b>B</b>) Ultrasound peak negative pressure profile produced by a range of waveform generator peak to peak output voltages. (<b>C</b>,<b>D</b>) Spatial mapping of the ultrasound beam pressure distribution measured beginning at the tip of the transducer fitted with a focusing cone using a waveform generator input of 45 mVpp. Panel (<b>D</b>) is a cross-section recorded at the depth of maximum peak negative pressure.</p>
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<p>Focused ultrasound-triggered release of fluorescein from gold-plated ALG beads. (<b>A</b>) Cumulative release of fluorescein with or without ultrasound trigger over 3 days. The duration of ultrasound actuation is 2 min. Data are the average of 3 different beads from each of the two separate batches. Unpaired <span class="html-italic">t</span> test, two-tailed <span class="html-italic">p</span> values calculated for two-group comparisons. (<b>B</b>) Representative brightfield and fluorescence microscopy images of the beads and the release medium taken on day 0 and day 3 before and after ultrasound-triggering.</p>
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6 pages, 1220 KiB  
Proceeding Paper
Formulation of Alginate- and Pectin-Based Beads Encapsulating Trichoderma for Sustainable and Efficient Agriculture
by Atália Inocêncio Ngulela, Zohra Bengharez, Imene Slamani and Selma Mahboubi
Chem. Proc. 2024, 16(1), 64; https://doi.org/10.3390/ecsoc-28-20186 - 14 Jan 2025
Viewed by 495
Abstract
The formulation of polysaccharide-based beads encapsulating Trichoderma spp. represents an eco-friendly strategy for promoting sustainable and efficient agriculture. Trichoderma, a beneficial fungus, is well known for its ability to enhance plant growth, combat phytopathogens, and improve soil health. Encapsulating Trichoderma spores in a [...] Read more.
The formulation of polysaccharide-based beads encapsulating Trichoderma spp. represents an eco-friendly strategy for promoting sustainable and efficient agriculture. Trichoderma, a beneficial fungus, is well known for its ability to enhance plant growth, combat phytopathogens, and improve soil health. Encapsulating Trichoderma spores in a polysaccharide matrix provides a protective environment that ensures their viability and facilitates their controlled release into the soil. Alginate is a natural polymer found in various species of brown algae and certain bacteria. Pectin is a heteropolysaccharide present naturally in the cell walls of all higher plants. Due to their distinctive characteristics, alginate and pectin are regarded as promising carrier materials for the encapsulation of bioactive agents. In this work, alginate (Alg) beads, pectin (Pec) beads extracted from orange peel, and Alg/Pec composite beads in a 50/50 (w/w) ratio encapsulating Trichoderma S1 (1.83 × 104 conidia/mL) and S2 (1.56 × 108 conidia/mL) were prepared using the ionic gelation method. The moisture content of the prepared beads was evaluated. The size and shape of the beads were determined by analyzing images obtained by an XE3910 optical microscope. The average size of the microcapsules (wet)varied from 1886 ± 6.557 μm to 1942 ± 28.688 μm. All samples were characterized by Fourier transform infrared spectroscopy (FTIR). The overall results demonstrated the successful encapsulation of Trichoderma spp. and highlighted the effects of the different formulations on the physicochemical properties of the beads. Full article
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<p>Wet samples of the formulated beads: (<b>a</b>) Alg/Tri S1, (<b>b</b>) Alg/Tri S2, (<b>c</b>) Alg/Pec/Tri S1, and (<b>d</b>) Alg/Pec/Tri S2.</p>
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<p>Microscopic images of (<b>a</b>) Alg, (<b>b</b>) Alg/Tri S1, and (<b>c</b>) Alg/Tri S2 beads.</p>
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<p>FTIR spectra of alginate and pectin beads and Trichoderma-loaded alginate beads.</p>
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17 pages, 3903 KiB  
Article
Lilium candidum Extract Loaded in Alginate Hydrogel Beads for Chronic Wound Healing
by Ioana Bâldea, Maria-Loredana Soran, Adina Stegarescu, Ocsana Opriș, Irina Kacso, Septimiu Tripon, Alexandra Adascalitei, Iulian George Fericel, Roxana Decea and Ildiko Lung
Gels 2025, 11(1), 22; https://doi.org/10.3390/gels11010022 - 1 Jan 2025
Viewed by 637
Abstract
Chronic wounds are a major health problem, affecting millions of people worldwide. Resistance to treatment is frequently observed, requiring an extension of the wound healing time, and improper care can lead to more problems in patients. Smart wound dressings that provide a controlled [...] Read more.
Chronic wounds are a major health problem, affecting millions of people worldwide. Resistance to treatment is frequently observed, requiring an extension of the wound healing time, and improper care can lead to more problems in patients. Smart wound dressings that provide a controlled drug release can significantly improve the healing process. In this paper, alginate beads with white lily leaf extract were prepared and tested for chronic wound healing. The obtained beads were characterized by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). Also, the efficiency of extract encapsulation in alginate was determined as being of. The obtained hydrogel was tested on two normal human cell lines, respectively, dermal fibroblasts (BJ-CRL-2522-ATCC) and endothelial cells (human umbilical vein endothelial cells—HUVEC 2). The longer release of bioactive compounds from plant extract loaded in the alginate hydrogel resulted in more effective wound closure, compared to the extract alone, and scar formation, compared to the alginate hydrogel. Therefore, the effect of the white lily extract in combination with that of sodium alginate hydrogel improves the biological activity of the alginate hydrogel and increases the wound healing properties of the alginate. Full article
(This article belongs to the Special Issue Recent Advances in Biopolymer Gels)
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<p>SEM image of the (<b>a</b>) microencapsulated Ext sample and (<b>b</b>) alginate beads.</p>
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<p>The FTIR spectra of sodium alginate (Alg), white lily extract (Ext), and microencapsulated extract (Alg-Ext).</p>
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<p>Viability assay. Dermal fibroblasts (BJ-upper panels) and endothelial cells (HUVECs-lower panels) were treated for 24 h with medium extract of alginate hydrogel formulations w/o the plant extract in different dilutions (left panels) and, respectively, different polyphenol concentrations of the plant extract (right panels). The resulting data is presented as a percentage of untreated control, average (n = 3) ± SD (standard deviation).</p>
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<p>Comparative microscopy aspect of the wounds at different time points (initial, at 8, 24, 48, 72 h) in experimental groups: 1. Control, 2. LPS (bacterial lipopolysaccharide), 3. LPS + A (lipopolysaccharide + alginate hydrogel), 4. LPS + AE (lipopolysaccharide + alginate hydrogel with plant extract), 5. LPS + E (lipopolysaccharide + plant extract), original magnification, objective 4×, bar = 10 µm.</p>
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<p>Wound area was measured at different time points (8, 24, 48, and 72 h) for each experimental group: 1. Control, 2. LPS (bacterial lipopolysaccharide), 3. LPS + A (lipopolysaccharide + alginate hydrogel), 4. LPS + AE (lipopolysaccharide + alginate hydrogel with plant extract), 5. LPS + E (lipopolysaccharide + plant extract), using the Image J software 1.8.0 and MiToBo plugging, data are presented as % of remaining wound area from the initial wound area, mean (n = 5) ± SD. * <span class="html-italic">p</span> &lt; 0.05, ** <span class="html-italic">p</span> &lt; 0.01.</p>
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<p>Viable cell count was estimated from the level of ATP measured in the cell cultures at 72 h in the wound scratch assay wells for each experimental group: 1. Control, 2. LPS (bacterial lipopolysaccharide), 3. LPS + A (lipopolysaccharide + alginate hydrogel), 4. LPS + AE (lipopolysaccharide + alginate hydrogel with plant extract), 5. LPS + E (lipopolysaccharide + plant extract), results are presented as % of controls, mean (n = 3) ± SD. * <span class="html-italic">p</span> &lt; 0.05.</p>
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<p>Western blot analysis of the protein levels of MMP9, MMP2, TIMP1, collagen 1, and caspase 3 for each experimental group: 1. Control, 2. LPS (bacterial lipopolysaccharide), 3. LPS + A (lipopolysaccharide + alginate hydrogel), 4. LPS + AE (lipopolysaccharide + alginate hydrogel with plant extract), 5. LPS + E (lipopolysaccharide + plant extract); WB bands quantification was conducted by densitometry, and for normalization, β actin was used. Data are presented as mean (n = 3) ± SD, * <span class="html-italic">p</span> &lt; 0.05, ** <span class="html-italic">p</span> &lt; 0.01, *** <span class="html-italic">p</span> &lt; 0.001, one-way ANOVA.</p>
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<p>Oxidative stress parameters measurement. Malondialdehyde (MDA). Superoxide dismutase (SOD). Catalase (CAT). Experimental groups: 1. Control, 2. LPS (bacterial lipopolysaccharide), 3. LPS + A (lipopolysaccharide + alginate hydrogel), 4. LPS + AE (lipopolysaccharide + alginate hydrogel with plant extract), 5. LPS + E (lipopolysaccharide + plant extract). Data are presented as mean (n = 3 ± SD), * <span class="html-italic">p</span> &lt; 0.05, ** <span class="html-italic">p</span> &lt; 0.01, *** <span class="html-italic">p</span> &lt; 0.001, one-way ANOVA.</p>
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<p>Pro-inflammatory cytokine IL1 β and IL6 levels. Experimental groups: 1. Control, 2. LPS (bacterial lipopolysaccharide), 3. LPS + A (lipopolysaccharide + alginate hydrogel), 4. LPS + AE (lipopolysaccharide + alginate hydrogel with plant extract), 5. LPS + E (lipopolysaccharide + plant extract). Data are presented as mean (n = 3 ± SD), ** <span class="html-italic">p</span> &lt; 0.01, *** <span class="html-italic">p</span> &lt; 0.001, one-way ANOVA.</p>
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16 pages, 2038 KiB  
Article
Natrium Alginate and Graphene Nanoplatelets-Based Efficient Material for Resveratrol Delivery
by Cristina Mormile, Ocsana Opriș, Stefano Bellucci, Ildiko Lung, Irina Kacso, Alexandru Turza, Adina Stegarescu, Septimiu Tripon, Maria-Loredana Soran and Ioana Bâldea
Gels 2025, 11(1), 15; https://doi.org/10.3390/gels11010015 - 27 Dec 2024
Viewed by 435
Abstract
In this study, alginate-based composite beads were developed for the delivery of resveratrol, a compound with therapeutic potential. Two formulations were prepared: one with sodium alginate and resveratrol (AR) and another incorporating graphene nanoplatelets (AGR) to improve drug release control. The beads were [...] Read more.
In this study, alginate-based composite beads were developed for the delivery of resveratrol, a compound with therapeutic potential. Two formulations were prepared: one with sodium alginate and resveratrol (AR) and another incorporating graphene nanoplatelets (AGR) to improve drug release control. The beads were formed by exploiting alginate’s ability to gel via ionic cross-linking. For the AGR formulation, sodium alginate was dissolved in water, and graphene was dispersed in isopropyl alcohol to achieve smaller flakes. Resveratrol was dissolved in an ethanol/water mixture and added to the graphene dispersion; the resulting solution was mixed with the alginate one. For the AR formulation, the resveratrol solution was mixed directly with the alginate solution. Both formulations were introduced into a calcium chloride solution to form the beads. The release of resveratrol was studied in phosphate-buffered saline at different pH values. Results showed that the presence of graphene in the AGR sample increased drug release, particularly at pH 6.8, indicating a pH-driven release mechanism. Kinetic analysis revealed that the Higuchi model best describes the release mechanism. Finally, cytotoxicity tests showed the biocompatibility of the system in normal human cells. These findings suggest that graphene-enhanced alginate matrices have significant potential for controlled drug delivery applications. Full article
(This article belongs to the Special Issue Recent Advances in Biopolymer Gels)
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<p>AR (<b>a</b>) and AGR (<b>b</b>) samples.</p>
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<p>AR (<b>a</b>) and AGR (<b>b</b>) samples.</p>
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<p>SEM images of (<b>a</b>) Alginate beads; (<b>b</b>) Alginate and graphene beads; (<b>c</b>) Alginate and resveratrol beads; (<b>d</b>) Alginate, graphene, and resveratrol beads.</p>
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<p>SEM images of: (<b>a</b>) Alginate beads; (<b>b</b>) Alginate and graphene beads; (<b>c</b>) Alginate and resveratrol beads; (<b>d</b>) Alginate, graphene, and resveratrol beads.</p>
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<p>FTIR spectra of: (<b>a</b>) graphene Na alginate and AG spectral domain 1800–950 cm<sup>−1</sup>; (<b>b</b>) resveratrol, Na alginate, and AR, spectral domain 1700–500 cm<sup>−1</sup> s (<b>c</b>) resveratrol, AG, and AGR, spectral domain 3800–400 cm<sup>−1</sup>, break region 2750–1800 cm<sup>−1</sup>.</p>
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<p>Release pattern of the samples: (<b>a</b>) AGR and AR in PBS pH 6.8; (<b>b</b>) AGR and AR in PBS pH 7.4.</p>
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<p>Difference between AGR and AR of drug released at every sampling point. (<b>a</b>) Results at pH 6.8; (<b>b</b>) Results at pH 7.4.</p>
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<p>The effects of the gel extracts on the cell viability of dermal fibroblasts (BJ) (<b>a</b>), respectively endothelial cells (HUVEC) (<b>b</b>). Data is expressed as % of the untreated control, <span class="html-italic">n</span> = 3 (mean +/− SD). AR = alginate with resveratrol, AGR = alginate with resveratrol and graphene, AG = alginate with graphene. *** = <span class="html-italic">p</span> &lt; 0.0001, * = <span class="html-italic">p</span> &lt; 0.01 between the indicated groups.</p>
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<p>The effects of resveratrol (<b>a</b>) and graphene (<b>b</b>) on the cell viability of dermal fibroblasts (BJ), respectively, endothelial cells (HUVEC). Data are expressed as % of the untreated control, <span class="html-italic">n</span> = 3 (mean +/− SD). * = <span class="html-italic">p</span> &lt; 0.01, compared to the control group.</p>
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23 pages, 2600 KiB  
Article
Formulation of Hydrogel Beads to Improve the Bioaccessibility of Bioactive Compounds from Goldenberry and Purple Passion Fruit and Evaluation of Their Antiproliferative Effects on Human Colorectal Carcinoma Cells
by Ana María Naranjo-Durán, Diego Miedes, Juan Manuel Patiño-Osorio, Antonio Cilla, Amparo Alegría, Catalina Marín-Echeverri, Julián Quintero-Quiroz and Gelmy Luz Ciro-Gómez
Gels 2025, 11(1), 10; https://doi.org/10.3390/gels11010010 - 27 Dec 2024
Viewed by 856
Abstract
Goldenberry and purple passion fruit contain bioactive compounds (BCs) that can prevent gastrointestinal cancers; hydrogel beads can protect and control their release in the gastrointestinal tract. This study aimed to develop an encapsulating material for fruit hydrogel beads (FHBs) to increase their bioaccessibility [...] Read more.
Goldenberry and purple passion fruit contain bioactive compounds (BCs) that can prevent gastrointestinal cancers; hydrogel beads can protect and control their release in the gastrointestinal tract. This study aimed to develop an encapsulating material for fruit hydrogel beads (FHBs) to increase their bioaccessibility and to assess antiproliferative effects. A blend of goldenberry–purple passion fruit was encapsulated using ionic gelation and electrospraying. Through a mixture experimental design with sodium alginate (SA), hydroxypropylmethylcellulose (HPMC) and arabic gum (AG) as components, the following response variables were optimized: polyphenol bioaccessibility and encapsulation efficiency. Polyphenols and antioxidant activity were quantified before and after digestion. Antiproliferative effect was evaluated on Caco-2 colon cancer cells. Variations in formulation proportions had a significant effect (p < 0.05) on most responses. An SA-AG mixture in a 0.75:0.25 ratio maximized polyphenol bioaccessibility to 213.17 ± 19.57% and encapsulation efficiency to 89.46 ± 6.64%. Polyphenols and antioxidant activity were lower in FHBs than in the fruit blend (F). Both F and FHBs inhibited tumor cell proliferation by 17% and 25%, respectively. In conclusion, encapsulating BCs in hydrogel beads with SA-AG can enhance the effectiveness of polyphenols in food applications by improving their bioaccessibility and showing a more pronounced effect in inhibiting tumor cell proliferation. Full article
(This article belongs to the Special Issue Functional Gels Loaded with Natural Products)
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<p>Effect of the percentage of fruit solids in the hydrogel beads formulation on (<b>a</b>) the load of the beads, (<b>b</b>) the polyphenol bioaccessibility and (<b>c</b>) the polyphenol encapsulation efficiency (EE). Different letters indicate statistically significant differences (<span class="html-italic">p</span> &lt; 0.05).</p>
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<p>Trace graphics for (<b>a</b>) polyphenol bioaccessibility, (<b>b</b>) carotenoid bioaccessibility, (<b>c</b>) polyphenol encapsulation efficiency (EE), (<b>d</b>) Particle size, (<b>e</b>) Sphericity, (<b>f</b>) FRAP and (<b>g</b>) ABTS. Blue line represents the proportion of sodium alginate in the blend, red line the proportion of hydroxypropyl methylcellulose and pink line the proportion of Arabic gum.</p>
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<p>Trace graphics for (<b>a</b>) polyphenol bioaccessibility, (<b>b</b>) carotenoid bioaccessibility, (<b>c</b>) polyphenol encapsulation efficiency (EE), (<b>d</b>) Particle size, (<b>e</b>) Sphericity, (<b>f</b>) FRAP and (<b>g</b>) ABTS. Blue line represents the proportion of sodium alginate in the blend, red line the proportion of hydroxypropyl methylcellulose and pink line the proportion of Arabic gum.</p>
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<p>SEM micrographs (<b>a</b>–<b>c</b>) for hydrogel beads and (<b>d</b>–<b>f</b>) for fruit blend hydrogel beads.</p>
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<p>Action mechanism of polyphenols on inhibiting tumor cell proliferation.</p>
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<p>Effect of bioaccessible fractions of samples (diluted 1:15 <span class="html-italic">v</span>/<span class="html-italic">v</span> with DMEM) (fruit blend (F), fruit hydrogel beads (FHBs) and hydrogel bead in blank (HB)) on the cell viability of Caco-2 cell lines, (<b>a</b>) non-differentiated as a tumoral model and (<b>b</b>) differentiated as an intestinal epithelial-like non tumoral model. Different letters indicate statistically significant differences (<span class="html-italic">p</span> &lt; 0.05).</p>
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<p>Effect of bioaccessible fractions of samples (diluted 1:15 <span class="html-italic">v</span>/<span class="html-italic">v</span> with DMEM) (fruit blend (F), fruit hydrogel beads (FHBs) and hydrogel bead in blank (HB)) on cell death status distribution of Caco-2 tumoral model line. Different letters indicate statistically significant differences (<span class="html-italic">p</span> &lt; 0.05) among samples in the same cell state.</p>
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<p>Effect of bioaccessible fractions of samples (diluted 1:15 <span class="html-italic">v</span>/<span class="html-italic">v</span> with DMEM) (fruit blend (F), fruit hydrogel beads (FHBs) and hydrogel bead in blank (HB)) on the different phases of the cell cycle of Caco-2 cell tumoral model line. Different letters indicate statistically significant differences (<span class="html-italic">p</span> &lt; 0.05) in the same cell cycle phase.</p>
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<p>Effect of bioaccessible fractions of samples (diluted 1:15 <span class="html-italic">v</span>/<span class="html-italic">v</span> with DMEM) (fruit blend (F), fruit hydrogel beads (FHBs) and hydrogel bead in blank (HB) on (<b>a</b>) the intracellular levels of ROS and (<b>b</b>) the intracellular levels of GSH of Caco-2 cell tumoral model line. Different letters indicate statistically significant differences (<span class="html-italic">p</span> &lt; 0.05).</p>
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16 pages, 3094 KiB  
Article
Optimization of Glucose Dehydrogenase Immobilization Strategies in a 3D-Printed Millireactor
by Vilim Marijan Boroša, Kristian Koštan, Renata Vičević, Ivan Karlo Cingesar, Domagoj Vrsaljko, Bruno Zelić, Ana Jurinjak Tušek and Anita Šalić
Micromachines 2024, 15(12), 1514; https://doi.org/10.3390/mi15121514 - 20 Dec 2024
Viewed by 985
Abstract
Enzymatic reactions play an important role in numerous industrial processes, e.g., in food production, pharmaceuticals and the production of biofuels. However, a major challenge when using enzymes in industrial applications is maintaining their stability and activity, especially under harsh operating conditions. To solve [...] Read more.
Enzymatic reactions play an important role in numerous industrial processes, e.g., in food production, pharmaceuticals and the production of biofuels. However, a major challenge when using enzymes in industrial applications is maintaining their stability and activity, especially under harsh operating conditions. To solve this problem, enzyme immobilization techniques have been developed. Immobilization involves fixing the enzymes on solid supports, which increases their stability, enables their reusability and facilitates the easy separation of reaction mixtures. In addition, immobilized enzymes are ideal for continuous flow systems such as millireactors, where they allow better control of reaction conditions, improving efficiency and product consistency. Glucose dehydrogenase is an important enzyme in biotechnology, particularly in biosensors and the production of biofuels, as it catalyzes the oxidation of glucose to gluconolactone, reducing NAD+ to NADH. However, like many other enzymes, it tends to lose activity over time. The immobilization of glucose dehydrogenase in a millireactor provides a controlled environment that increases the stability and activity of the enzyme. The aim of this study was to investigate the effects of different immobilization strategies on the performance of glucose dehydrogenase in a 3D printed millireactor. The enzyme was immobilized in alginate gel in three immobilization strategies: as beads, on the bottom surface, and on both the top and bottom surfaces of the millireactor. The results showed that the application of the enzyme on both surfaces improved the glucose conversion two-fold compared to immobilization in beads and four-fold compared to immobilization only on the bottom surface. The dual-surface enzyme immobilization strategy showed the highest efficiency, achieving the highest conversion of 95.76 ± 1.01% (τ = 131 min) and NADH productivity of 0.166 ± 0.01 mmol/(L·min) (τ = 7.11 min) combined with operational stability over five days. Effective diffusion rates comparable to those of aqueous solutions confirmed the suitability of alginate gels for biocatalysis. These advancements highlight the potential of this modular and scalable platform for various biotechnological applications. Full article
(This article belongs to the Special Issue Feature Papers of Micromachines in Biology and Biomedicine 2024)
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<p>Schematic representation of (<b>a</b>) design specifications (in mm) with height = 5 mm and average hydraulic diameter = 6.69 ± 0.98 mm and (<b>b</b>) key millireactor elements.</p>
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<p>Different GDH immobilization strategies (<b>a</b>) as beads, (<b>b</b>) on the bottom surface of the millireactor, and (<b>c</b>) on both the bottom and the top surface of the millireactor.</p>
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<p>Experimental setup used for glucose oxidation.</p>
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<p>Experimental setup for measuring the diffusion of glucose and NADH through alginate pores.</p>
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<p>Fluid flow characteristics in (<b>a</b>) a rectangular millireactor and (<b>b</b>) a millireactor proposed in this research for a flow rate of 400 µL/min.</p>
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<p>Comparison of the available surface area depending on the immobilization strategy.</p>
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<p>Influence of residence time on the concentration of glucose (•) and NADH (◦) when the enzyme was immobilized in (<b>a</b>) alginate beads and alginate hydrogen, (<b>b</b>) bottom surface, and (<b>c</b>) bottom and top surface on the millireactor.</p>
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<p>Change in (<b>a</b>) conversion and (<b>b</b>) productivity upon immobilization of the enzyme in alginate beads (<span style="color:#538135">•</span>) and alginate hydrogen, bottom surface (<span style="color:red">•</span>), and bottom and top surface of the millireactor (<span style="color:#0070C0">•</span>).</p>
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<p>Enzyme deactivation.</p>
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<p>Changes in (<b>a</b>) glucose and (<b>b</b>) NADH concentrations in chamber 1 (•) and chamber 2 (◦) during the time.</p>
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<p>Estimation of the effective diffusivity coefficient for (<b>a</b>) glucose and (<b>b</b>) NADH.</p>
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17 pages, 5566 KiB  
Article
Hybrid Systems of Oleogels and Probiotic-Loaded Alginate Carriers for Potential Application in Cosmetics
by Anna Łętocha, Małgorzata Miastkowska, Elżbieta Sikora, Alicja Michalczyk, Marta Liszka-Skoczylas and Mariusz Witczak
Molecules 2024, 29(24), 5984; https://doi.org/10.3390/molecules29245984 - 19 Dec 2024
Viewed by 905
Abstract
Oleogels (organogels) are systems resembling a solid substance based on the gelation of organic solvents (oil or non-polar liquid) through components of low molecular weight or oil-soluble polymers. Such compounds are organogelators that produce a thermoreversible three-dimensional gel network that captures liquid organic [...] Read more.
Oleogels (organogels) are systems resembling a solid substance based on the gelation of organic solvents (oil or non-polar liquid) through components of low molecular weight or oil-soluble polymers. Such compounds are organogelators that produce a thermoreversible three-dimensional gel network that captures liquid organic solvents. Oleogels based on natural oils are attracting more attention due to their numerous advantages, such as their unsaturated fatty acid contents, ease of preparation, and safety of use. As a result of the research, two oleogels were developed, into which freeze-dried alginate carriers with a probiotic, L. casei, were incorporated. Two techniques were used to produce probiotic-loaded capsules—extrusion and emulsification. Alginate beads obtained by the extrusion process have a size of approximately 1.2 mm, while much smaller microspheres were obtained using the emulsification technique, ranging in size from 8 to 17 µm. The trehalose was added as a cryoprotectant to improve the survival rate of probiotics in freeze-dried alginate carriers. The encapsulation efficiency for both of the methods applied, the emulsification and the extrusion technique, was high, with levels of 90% and 87%, respectively. The obtained results showed that the production method of probiotic-loaded microspheres influence the bacterial viability. The better strain survival in the developed systems was achieved in the case of microspheres produced by the emulsification (reduction in bacterial cell viability in the range of 1.98–3.97 log in silica oleogel and 2.15–3.81 log in sucragel oleogel after 7 and 30 days of storage) than by the extrusion technique (after a week and a month of oleogel storage, the decrease in cell viability was 2.52–4.52 log in silica oleogel and 2.48–4.44 log in sucragel oleogel). Full article
(This article belongs to the Special Issue Multifunctional Natural Ingredients in Skin Protection and Care)
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<p>Scheme of oleogel-based systems [by author].</p>
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<p>Schematic description of the incorporation of encapsulated probiotics into the oleogel system [by author].</p>
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<p>Survival rate of free cells and encapsulated probiotics in the emulsification and extrusion techniques. The bars represent standard deviations of the means according to three independent repeated experiments. *—<span class="html-italic">p</span> = 0.05–0.011; ****—<span class="html-italic">p</span> ≤ 0.0001.</p>
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<p>SEM micrographs of freeze-dried microspheres obtained by emulsification: (<b>a</b>) alginate–Tween 80 microspheres, (<b>b</b>) alginate–Span 80 microspheres, and (<b>c</b>) alginate–Tween 80–trehalose microspheres.</p>
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<p>SEM micrographs and cross sections of freeze-dried beads obtained by extrusion: (<b>a</b>) alginate beads and (<b>b</b>) alginate–trehalose beads.</p>
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<p>Examples of stress sweeps for the studied oleogels. G′: storage modulus (filled symbols); G″: loss modulus (empty symbols)—temperature 20 °C.</p>
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<p>Example stress sweeps for the studied oleogels. G′: storage modulus (filled symbols); G″: loss modulus (empty symbols)—temperature 37 °C.</p>
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<p>Frequency sweeps for the different oleogels studied. G′: storage modulus (filled symbols); G″: loss modulus (empty symbols)—temperature 20 °C.</p>
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<p>Frequency sweeps for the different oleogels studied. G′: storage modulus (filled symbols); G″: loss modulus (empty symbols)—temperature 37 °C.</p>
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<p>Schematic description of the process of obtaining probiotic microspheres by emulsification [by author].</p>
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<p>Schematic description of the process of obtaining probiotic microspheres by extrusion [by author].</p>
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17 pages, 10974 KiB  
Article
Mercury Adsorption by Ca-Based Shell-Type Polymers Synthesized by Self-Assembly Mineralization
by Yang Peng, Chuxuan Zhang, Xiaomin Li, Tianyi Feng and Xun Gong
Polymers 2024, 16(24), 3454; https://doi.org/10.3390/polym16243454 - 10 Dec 2024
Viewed by 728
Abstract
Adsorption is one of the most promising strategies for heavy metal removal. For Hg(II) removal, mineralized Ca-based shell-type self-assembly beads (MCABs) using alginate as organic polymer template were synthesized in this work. The adsorbent preparation consists of gelation of a Ca-based spherical polymer [...] Read more.
Adsorption is one of the most promising strategies for heavy metal removal. For Hg(II) removal, mineralized Ca-based shell-type self-assembly beads (MCABs) using alginate as organic polymer template were synthesized in this work. The adsorbent preparation consists of gelation of a Ca-based spherical polymer template (CAB) and rate-controlled self-assembly mineralization in bicarbonate solution with various concentrations. The comparative study demonstrates that 1% (MCAB-1) is the optimal concentration of bicarbonate. Based on this condition, the maximum adsorption capacity (48 ± 4 mg/g) of MCAB-1 was observed at pH = 5 in a batch test, which was 2.67 times more than that of the unmodified one, CAB, at 18 ± 1 mg/g. Long-duration (10 h) adsorption tests showed that MCAB-1 exhibited remarkable performance stability and anti-wear ability (43.2% removal efficiency and 74.3% mass retention, compared to 2.7% and 38.6% for CAB at pH = 3, respectively). The morphology determination showed that a shell-type porous amorphous carbonate layer was formed at the surface of the organic polymer template by rate-controlled self-assembly mineralization. This transition not only promotes the pore structure and activated cation binding functional sites, but also improves the anti-wear ability of materials effectively. Full article
(This article belongs to the Special Issue Application and Characterization of Polymer Composites)
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<p>Sectional views of CAB and the three MCAB samples.</p>
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<p>XRD spectra of CAB and MCAB-1.</p>
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<p>Statistical analysis of the average mass of a single adsorbent particle.</p>
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<p>Effect of the dosage on the Hg(II) adsorption efficiency (initial Hg(II) concentration = 1 mg/L, oscillation time = 180 min, pH = 5, temperature = 30 °C).</p>
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<p>Effect of pH on the Hg(II) adsorption efficiency (initial Hg(II) concentration = 1 mg/L, oscillation time = 180 min, dosage = 1 g/L, temperature = 30 °C).</p>
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<p>Adsorption kinetics models (pH = 5, initial Hg(II) concentration = 1 mg/L, adsorbent dosage = 1 g/L, temperature = 30 °C).</p>
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<p>Adsorption isotherm fitting curves (pH = 5; oscillation time = 180 min; adsorbent dosage = 1 g/L; test temperature = 30 °C).</p>
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<p>Mass weight and adsorption efficiency during adsorption process (pH = 3, initial Hg(II) concentration = 1 mg/L, dosage = 1 g/L, temperature = 30 °C).</p>
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<p>FTIR spectra of CAB and MCAB-1 before and after Hg(II) adsorption (pH = 5, oscillation time = 180 min, adsorbent dosage = 1 g/L, test temperature = 30 °C).</p>
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<p>Effect of pH on the morphology changes of CAB and the three MCAB samples (initial Hg(II) concentration = 1 mg/L, dosage = 1 g/L, temperature = 30 °C, oscillation time = 10 h).</p>
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<p>Potential adsorption mechanism.</p>
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