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Search Results (2,029)

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Keywords = response surface methodology (RSM)

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19 pages, 5018 KiB  
Article
Biotechnological Applications of the Ubiquitous Fungus Penicillium sp. 8L2: Biosorption of Zn(II) and Synthesis of ZnO Nanoparticles as Biocidal Agents
by Antonio Jesús Muñoz Cobo, Francisco Espínola Lozano, Manuel Moya Vilar, Celia Martín Valenzuela and Encarnación Ruiz Ramos
Sustainability 2025, 17(6), 2379; https://doi.org/10.3390/su17062379 (registering DOI) - 8 Mar 2025
Abstract
In this study, the capacity of the ubiquitous filamentous fungus Penicillium sp. 8L2 to remove Zn(II) ions present in synthetic solutions was studied and the optimal operating conditions were obtained based on a response surface methodology (RSM). The contact time was optimized through [...] Read more.
In this study, the capacity of the ubiquitous filamentous fungus Penicillium sp. 8L2 to remove Zn(II) ions present in synthetic solutions was studied and the optimal operating conditions were obtained based on a response surface methodology (RSM). The contact time was optimized through kinetic tests. Equilibrium tests were then carried out, which allowed biosorption isotherms to be obtained for several mathematical models. At the same time, the capacity of the fungal cell extract to transform metal ions into ZnO nanoparticles with a biocidal capacity was evaluated. Its inhibitory capacity for five microbial strains was then determined. The biosorption mechanisms and nanoparticle synthesis were characterized by different crystallographic, spectrophotometric and microscopic analytical techniques. It was confirmed that the metal was bound superficially but also in the periplasmic space with a strong bond to phosphate groups, both in the biosorption stage and during the synthesis and consolidation of the nanoparticles. In addition, the presence of hydroxyl, amino, carbonyl and methylene groups was identified, which could promote the synthesis of nanoparticles, since some of them have a reducing nature. The kinetics showed that the biosorption of Zn(II) occurred in two stages, the first very fast and the second slower. Equilibrium tests identified a maximum biosorption capacity of 52.14 mg/g for the Langmuir model under optimized conditions: a contact time of 5 days, pH 5.6 and a 0.2 g/L biomass dose. The success of the biological synthesis route was confirmed and ZnO nanoparticles with an average size of 18 nm were obtained. The data showed that the nanoparticles showed a good inhibition ability against the tested microorganisms, with values ranging from 62.5 to 1000 µg/mL. Penicillium sp. 8L2 is a promising ubiquitous microorganism in the field of heavy metal biosorption and applied biotechnology. Full article
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<p>(<b>a</b>): Response surface obtained after fitting the data obtained in the experimental design for the biosorption of Zn(II) by <span class="html-italic">Penicillium</span> sp. 8L2. The graph identifies factor <span class="html-italic">A</span> (pH) and factor B (biomass dose) for an initial metal concentration of 50 mg/L. (<b>b</b>): Perturbation diagram in coded units obtained for the following conditions: <span class="html-italic">A</span> = 5.2 and <span class="html-italic">B</span> = 0.5. The diagram shows the influence of changes in the value of the variables on the response (q, mg/g).</p>
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<p>(<b>a</b>) Biosorption kinetics obtained for the Lagergren model. (<b>b</b>): Biosorption isotherm obtained for the Langmuir model.</p>
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<p>FT-IR spectra obtained before (blue color) and after (red color) the Zn(II) biosorption stage by <span class="html-italic">Penicillium</span> sp. 8L2.</p>
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<p>Images (<b>a</b>–<b>c</b>): FESEM image sequence of <span class="html-italic">Penicillium</span> sp. 8L2 hyphae after the Zn(II) biosorption step. The images show that by changing the kilovoltage and the detector of the instrument, information about the location of the retained metal can be obtained. Image (<b>d</b>): EDX spectrum obtained in the area indicated by the arrow.</p>
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<p>(<b>a</b>) SEM image of <span class="html-italic">Penicillium</span> sp. 8L2 biomass obtained after the Zn(II) biosorption process, where the arrows indicate the location where the EDX spectra were recorded (images (<b>g</b>,<b>h</b>)). (<b>b</b>–<b>f</b>) Elemental maps of image a for the elements C, O, P, S and Zn, respectively.</p>
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<p>UV-vis spectrum of a suspension of ZnO-NPs nanoparticles synthesized with cell extract of <span class="html-italic">Penicillium</span> sp. 8L2. A characteristic peak at 374 nm is identified.</p>
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<p>XRD spectra of ZnO-NPs. The blue spectrum corresponds to the NPs obtained from the unfiltered cell extract (protocol 1). The red spectrum was obtained from the NPs obtained from the filtered cell extract (protocol 2).</p>
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<p>(<b>a</b>): SEM image of ZnO-NPs obtained from the cell extract of <span class="html-italic">Penicillium</span> sp. 8L2 using protocol 1 (before calcination step). (<b>b</b>–<b>d</b>): Elemental maps obtained from image (<b>a</b>). (<b>e</b>): SEM image of ZnO-NPs obtained from the cell extract of <span class="html-italic">Penicillium</span> sp. 8L2 using protocol 2 (after calcination step). (<b>f</b>): Histogram and frequency polygon obtained from image (<b>d</b>).</p>
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<p>(<b>a</b>) FESEM image of the biomass of <span class="html-italic">Penicillium</span> sp. 8L2 obtained before exposure to Zn(II) ions. (<b>b</b>–<b>d</b>) Relative to image a, elemental maps of O, C and P, respectively. (<b>e</b>) EDX spectrum obtained at the location indicated by the arrow (<b>a</b>).</p>
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10 pages, 2079 KiB  
Proceeding Paper
Optimisation of Biodiesel Production from Waste Margarine Oil Using Response Surface Methodology
by Pascal Mwenge, Salvation Muthubi and Hilary Rutto
Eng. Proc. 2025, 87(1), 12; https://doi.org/10.3390/engproc2025087012 - 6 Mar 2025
Viewed by 58
Abstract
This work presents biodiesel production using waste margarine oil and response surface methodology (RSM) for optimisation. The transesterification of waste margarine oil was carried out using sodium hydroxide (NaOH) as a catalyst under atmospheric pressure in a lab-scale batch reactor. Central composite design [...] Read more.
This work presents biodiesel production using waste margarine oil and response surface methodology (RSM) for optimisation. The transesterification of waste margarine oil was carried out using sodium hydroxide (NaOH) as a catalyst under atmospheric pressure in a lab-scale batch reactor. Central composite design (CCD) was used to optimise four parameters: methanol-to-oil ratio (3–15 mol/mol), catalyst ratio (0.3–1.5 wt.%), reaction time (30–90 min), and reaction temperature (30–70 °C). Numeral optimisation was performed, and an optimum yield of 99.1% was obtained at an 11.906 methanol-to-oil mol ratio, 1.113 wt.% catalyst ratio, 59.646 min reaction time, 52.459 °C temperature, and a low percentage error yield of 0.942%. Analysis of variance (ANOVA) showed that the methanol-to-oil ratio had the highest influence on the biodiesel yield, followed by the catalyst ratio, and reaction time had the least impact after temperature. The kinetics study revealed that the reaction is controlled by a pseudo-first order, and the activation energy was found to be 62.41 kJ/mol. It was concluded that biodiesel could be produced using waste margarine oil as a cost-effective feedstock optimised by RSM. Full article
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<p>3D plots of effect of process parameters on biodiesel yield; (<b>a</b>) effect of interaction of methanol-to-oil ratio and catalyst ratio at constant temperature of 50 °C and 60 min; (<b>b</b>) effect of interaction of methanol-to-oil ratio and time at constant temperature of 50 °C and catalyst ratio of 0.9 wt. %; (<b>c</b>) effect of interaction of methanol-to-oil ratio and temperature at constant time of 60 min and catalyst ratio of 0.9 wt. %; (<b>d</b>) effect of interaction of catalyst ratio and time at constant methanol-to-oil ratio of 9 and temperature of 50 °C; (<b>e</b>) effect of interaction of catalyst ratio and temperature at constant methanol-to-oil ratio of 9 and time of 60 min; and (<b>f</b>) effect of interaction of temperature and time at constant methanol-to-oil ratio 9 of and catalyst ratio of 0.9 wt.%. From blue to red, low to high biodiesel yield.</p>
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<p>3D plots of effect of process parameters on biodiesel yield; (<b>a</b>) effect of interaction of methanol-to-oil ratio and catalyst ratio at constant temperature of 50 °C and 60 min; (<b>b</b>) effect of interaction of methanol-to-oil ratio and time at constant temperature of 50 °C and catalyst ratio of 0.9 wt. %; (<b>c</b>) effect of interaction of methanol-to-oil ratio and temperature at constant time of 60 min and catalyst ratio of 0.9 wt. %; (<b>d</b>) effect of interaction of catalyst ratio and time at constant methanol-to-oil ratio of 9 and temperature of 50 °C; (<b>e</b>) effect of interaction of catalyst ratio and temperature at constant methanol-to-oil ratio of 9 and time of 60 min; and (<b>f</b>) effect of interaction of temperature and time at constant methanol-to-oil ratio 9 of and catalyst ratio of 0.9 wt.%. From blue to red, low to high biodiesel yield.</p>
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<p>Kinetics plots: (<b>a</b>) plot of -lnk (1-X) vs. reaction time at different temperatures; (<b>b</b>) Arrhenius plot lnk vs. 1000/T for the transesterification reaction of waste margarine oil.</p>
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21 pages, 2040 KiB  
Article
A Multi-Type Ship Allocation and Routing Model for Multi-Product Oil Distribution in Indonesia with Inventory and Cost Minimization Considerations: A Mixed-Integer Linear Programming Approach
by Marudut Sirait, Peerayuth Charnsethikul and Naraphorn Paoprasert
Logistics 2025, 9(1), 35; https://doi.org/10.3390/logistics9010035 - 6 Mar 2025
Viewed by 158
Abstract
Background: Indonesia is an archipelagic country with 17,508 islands spread over the Pacific and Indian Oceans, with thousands of inter-island routes requiring a large and engaged fleet. The vast expanse of the country also leads to challenges related to optimal fleet coverage, [...] Read more.
Background: Indonesia is an archipelagic country with 17,508 islands spread over the Pacific and Indian Oceans, with thousands of inter-island routes requiring a large and engaged fleet. The vast expanse of the country also leads to challenges related to optimal fleet coverage, routing, and oil distribution while maintaining cost-effectiveness and reliable supply. Methods: This study combined a mixed-integer linear-programming (MILP) model with a response surface methodology (RSM) approach to optimize vessel assignment, vessel routes, and inventory control simultaneously and comprehensively across three regional clusters (i.e., Western, Central, and Eastern Indonesia). The model takes into account a fleet of 28 vessels (13 medium range [MR] and 15 general purpose [GP]) that can distribute three oil products: gasoline, diesel, and kerosene. Results: The optimized solution yields 100% service reliability at an operational cost of $ 2.83 million per month—far lower than currently operating services. The model is robust against variations in demand (±20%), port congestion (±50%), and changing fuel prices (±50%), which is confirmed by a sensibility analysis. The close correlation coefficient (0.987) between the MILP and RSM results confirms the framework’s accuracy. At the same time, the critical performance factors were found to be vessel speed (13.5 knots), fleet size, and port operation time. Conclusions: The study offers a cost-efficient and data-intensive model that could be implemented as a maritime logistics framework, as well as potential areas for future work and insight for relevant stakeholders. Future research will have to integrate real-time data fusion, mainly due to the need for environmental and stochastic modeling methods to foster operational resilience in dynamic maritime business ecosystems. Full article
(This article belongs to the Section Maritime and Transport Logistics)
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<p>Flow diagram of oil distribution.</p>
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<p>Location supply port and demand port.</p>
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<p>Comparison of route time and utilization.</p>
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<p>Interaction between factors.</p>
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<p>Vessel speed sensitivity.</p>
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<p>Port time sensitivity.</p>
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<p>Fleet size sensitivity.</p>
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<p>Graphic of impact travel time on performance.</p>
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20 pages, 4352 KiB  
Article
Synergistic Effects of Dielectric Barrier Discharge Plasma Treatment on Hemp Fiber Surface Modification and Mechanical Properties of Hemp-Fiber-Reinforced Epoxy Composites
by Choncharoen Sawangrat, Kittisak Jantanasakulwong, Jonghwan Suhr, Kannikar Kaewapai, Thidarat Kanthiya, Parichat Thipchai, Pornchai Rachtanapun and Pitiwat Wattanachai
Appl. Sci. 2025, 15(5), 2818; https://doi.org/10.3390/app15052818 - 5 Mar 2025
Viewed by 215
Abstract
This study focused on improving the mechanical properties of hemp-fiber-reinforced epoxy (HFRE) composites by modifying the surface of hemp fibers (HFs) using dielectric barrier discharge (DBD) plasma treatment. By exposing the fibers to different gas mixtures Ar, Ar+N2, and Ar+O2 [...] Read more.
This study focused on improving the mechanical properties of hemp-fiber-reinforced epoxy (HFRE) composites by modifying the surface of hemp fibers (HFs) using dielectric barrier discharge (DBD) plasma treatment. By exposing the fibers to different gas mixtures Ar, Ar+N2, and Ar+O2, the surface of the fibers was altered, adding functional groups, increasing surface roughness, and improving crystallinity. The researchers created HFRE composites using both untreated and plasma-treated HF, and then tested their mechanical properties. The results revealed that Ar+O2 plasma treatment boosted both the tensile strength (by 15.2%) and energy absorption of the composites. To fine-tune the process, the response surface methodology (RSM) was used to determine the most important factors for optimizing the treatment: input power and treatment time. The ideal conditions were found to be 162.63 W of power and 10 min of treatment. These findings highlight the potential of DBD plasma as a reliable method for modifying the surface of hemp fibers, even with changes in the setup or reactor design. Overall, this approach shows great promise for industrial applications, providing an effective way to improve the strength and durability of HFRE composites for a variety of uses. Full article
(This article belongs to the Special Issue Modernly Designed Materials and Their Processing)
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<p>Schematic of the DBD cell operated under atmospheric pressure.</p>
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<p>Test specimens for tensile testing according to technical standard.</p>
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<p>Representative optical emission spectra of the DBD plasma.</p>
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<p>XRD patterns of hemp fiber untreated and treated with Ar, Ar+N<sub>2</sub>, and Ar+O<sub>2</sub> plasma.</p>
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<p>FT-IR spectra of hemp fiber untreated and treated with Ar, Ar+N<sub>2</sub>, and Ar+O<sub>2</sub> plasma.</p>
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<p>Surface morphology of hemp fiber was untreated and treated with Ar, Ar+N<sub>2</sub>, and Ar+O<sub>2</sub> plasma, Note: Main figures before expansion (1000×) and insets show the same images after expansion (15,000×).</p>
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<p>SEM image of (<b>a</b>,<b>b</b>) cracking patterns of composite samples, (<b>c</b>) a model pattern of fracture area observed in side view, (<b>d</b>,<b>e</b>) a fracture surface overview of composite samples, (<b>f</b>,<b>g</b>) a fracture surface overview of composite samples after expansion (600×), and (<b>h</b>) a model pattern of fracture area observed in top view.</p>
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<p>(<b>a</b>) Tensile strength and elongation at break and (<b>b</b>) calculated energy absorption of the epoxy, the epoxy composite reinforced with untreated HF (HFRE), and the epoxy composite reinforced with plasma-treated HF (HF<sub>tr</sub>RE) in various gasses.</p>
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<p>Multiple response prediction plots for maximum-tensile-strength O<sub>2</sub>plasma-treatedHF-reinforced epoxy composite sample.</p>
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<p>Response curved surface (<b>a</b>) and its equal-height line plot (<b>b</b>).</p>
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22 pages, 2738 KiB  
Article
Optimization of Microwave-Assisted Extraction of Phenolic Compounds from Opuntia ficus-indica Cladodes
by Amira Oufighou, Fatiha Brahmi, Sabiha Achat, Sofiane Yekene, Sara Slimani, Younes Arroul, Lila Boulekbache-Makhlouf and Federica Blando
Processes 2025, 13(3), 724; https://doi.org/10.3390/pr13030724 - 3 Mar 2025
Viewed by 312
Abstract
Background: Opuntia ficus-indica (OFI) cladodes are valuable and underestimated by-products that provide significant amounts of biologically active compounds. In this paper, microwave-assisted extraction (MAE) was performed for the recovery of phenolic compounds from OFI cladodes using two approaches: response surface methodology (RSM) and [...] Read more.
Background: Opuntia ficus-indica (OFI) cladodes are valuable and underestimated by-products that provide significant amounts of biologically active compounds. In this paper, microwave-assisted extraction (MAE) was performed for the recovery of phenolic compounds from OFI cladodes using two approaches: response surface methodology (RSM) and artificial neural network–genetic algorithm (ANN-GA), which were then compared following statistical indicators. Materials and Methods: Four independent factors were employed in the optimization process (solvent concentration, microwave power, irradiation time, and solid-to-liquid ratio) by selecting the total phenolic content (TPC), estimated by the Folin–Ciocalteu method, as a response. The optimized extract was tested for antioxidant capacity using the Folin–Ciocalteu reagent, Trolox Equivalent Antioxidant Capacity (TEAC), and oxygen radical absorbance capacity (ORAC) assays and for antimicrobial activity against 16 pathogenic strains using the agar well diffusion method. Results: The maximum TPC values predicted with maximizing desirability function for RSM were 2177.01 mg GAE/100 g DW and 1827.38 mg GAE/100 g DW for the ANN. Both models presented certain advantages and could be considered reliable tools for predictability and accuracy purposes. Using these conditions, the extract presented high antioxidant capacity for FCR assay (13.43 ± 0.62 mg GAE/g DW), TEAC (10.18 ± 0.47 µmol TE/g DW), and ORAC (205.47 ± 19.23 µmol TE/g DW). The antimicrobial activity of the optimized extract was pronounced only with respect to S. aureus alimentarius, Streptococcus, E. coli, P. aeruginosa, and A. flavus. Conclusions: This study underlines the high effectiveness of the optimization approaches in providing a maximum recovery of bioactive compounds from OFI cladodes to formulate food and pharmaceutical products with functional qualities. Full article
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<p>Single-factor results of <span class="html-italic">Opuntia ficus-indica</span> cladode extract. (<b>a</b>) The effect of sol vent concentration; (<b>b</b>) the effect of microwave power; (<b>c</b>) the effect of extraction time; (<b>d</b>) the effect of ratio. The significant differences are mentioned by the letters on the bars.</p>
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<p>Three-dimensional plot of the interactions between solvent concentration and extraction power (<b>a</b>), solvent concentration and solid-to-liquid ratio (<b>b</b>), solvent concentration and extraction time (<b>c</b>), extraction power and extraction time (<b>d</b>), extraction power and solid-to-liquid ratio (<b>e</b>), and extraction time and solid-to-liquid ratio (<b>f</b>) on the total phenolic content of <span class="html-italic">Opuntia ficus-indica</span> cladodes extract.</p>
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<p>Optimal three-layer ANN topology.</p>
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<p>The correlation coefficient for predicted and experimental values for training, validation, testing, and overall neural network dataset.</p>
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16 pages, 4478 KiB  
Article
Extraction Technology, Component Analysis, and Biological Activity of Essential Oils from Ligusticum jeholense Nakai et Kitag. Vegetables
by Miao Wang, Jiangkuo Li, Yamin Xu, Pengyu Liu, Qiang Zheng, Xia Bai and Donghua Li
Processes 2025, 13(3), 721; https://doi.org/10.3390/pr13030721 - 2 Mar 2025
Viewed by 312
Abstract
In this study, we aimed to optimize the process of extracting essential oils from Ligusticum jeholense Nakai et Kitag. vegetables (LJ-Vs) by means of hydrodistillation (HD), analyze the essential oils’ chemical composition, and evaluate their antioxidant and antibacterial activities so as to provide [...] Read more.
In this study, we aimed to optimize the process of extracting essential oils from Ligusticum jeholense Nakai et Kitag. vegetables (LJ-Vs) by means of hydrodistillation (HD), analyze the essential oils’ chemical composition, and evaluate their antioxidant and antibacterial activities so as to provide a certain research basis for their development and utilization. A single-factor test and the response surface methodology (RSM) were used to optimize the essential oil extraction process. The chemical constituents of the LJ-V essential oils were analyzed via GC-MS, and the antibacterial and antioxidant activities of the oils were studied. The optimal extraction process conditions were as follows: a solid–liquid ratio of 1:16.3 g/mL, a soaking time of 120 min, and crushing using a mesh size of 40. The validation result for the optimized process was 0.872%. A total of 32 chemical components were detected in LJ-V essential oils, among which the main components were neocnidilide, myristicin, elemicin, and germacrene. LJ-V essential oils with a 20% volume concentration had obvious inhibitory effects on four tested bacteria. The effect on Staphylococcus aureus was stronger than that on others. When the dilution concentration exceeded 100 times, the antibacterial effect was not ideal. The sensitivity of the tested bacteria to the essential oils followed the order Staphylococcus aureus > Salmonella > Pseudomonas fluorescens > Escherichia coli. Further, LJ-V essential oil had an ideal capacity to scavenge free radicals when compared to Vc control groups. Under the optimized conditions, the essential oil extraction rate was higher, and the process was stable and feasible. This study could provide theoretical and technical support for the cultivation, comprehensive development, and processing of Ligusticum jeholense Nakai et Kitag. resources. Full article
(This article belongs to the Section Separation Processes)
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<p>The effects of the solid–liquid ratio (<b>A</b>), soaking time (<b>B</b>), and particle size (<b>C</b>) on the yield of essential oil from <span class="html-italic">Ligusticum jeholense</span> vegetables. Different lowercase letters indicated a significant difference (<span class="html-italic">p</span> &lt; 0.05), while the same letter indicated no significant difference (<span class="html-italic">p</span> &gt; 0.05).</p>
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<p>The effects of the solid–liquid ratio (<b>A</b>), soaking time (<b>B</b>), and particle size (<b>C</b>) on the yield of essential oil from <span class="html-italic">Ligusticum jeholense</span> vegetables. Different lowercase letters indicated a significant difference (<span class="html-italic">p</span> &lt; 0.05), while the same letter indicated no significant difference (<span class="html-italic">p</span> &gt; 0.05).</p>
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<p>Response surface diagrams and contour maps showing the effects of interactions of various factors on the extraction yield of LJ-V essential oil.</p>
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<p>Component type and quantity analysis of three <span class="html-italic">Ligusticum jeholense</span> essential oils.</p>
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<p>Scavenging rates of LJ-V essential oil. Different lowercase letters indicated a significant difference (<span class="html-italic">p</span> &lt; 0.05), while the same letter indicated no significant difference (<span class="html-italic">p</span> &gt; 0.05).</p>
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<p>Scavenging rates of LJ-V essential oil. Different lowercase letters indicated a significant difference (<span class="html-italic">p</span> &lt; 0.05), while the same letter indicated no significant difference (<span class="html-italic">p</span> &gt; 0.05).</p>
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21 pages, 4529 KiB  
Article
Enhancing Physicochemical and Piezoelectric Properties of Eggshell Membrane Proteins by Ultrasonic-Assisted Enzymes for Food and Sensor Applications
by Xinhua Liang, Honglian Cong, Gaoming Jiang and Haijun He
Int. J. Mol. Sci. 2025, 26(5), 2190; https://doi.org/10.3390/ijms26052190 - 28 Feb 2025
Viewed by 144
Abstract
This research sought to explore the impact of ultrasonic pretreatment on the physicochemical characteristics of proteins derived from eggshell membranes through enzymatic extraction. Response surface methodology (RSM) and Box-Behnken design were employed to identify the ideal conditions for the extraction process. The optimal [...] Read more.
This research sought to explore the impact of ultrasonic pretreatment on the physicochemical characteristics of proteins derived from eggshell membranes through enzymatic extraction. Response surface methodology (RSM) and Box-Behnken design were employed to identify the ideal conditions for the extraction process. The optimal parameters determined were enzyme usage at 4.2%, pH level at 2.4, a solid-to-solvent ratio of 1:20 g/mL, and an extraction time of 21.5 h. The eggshell membrane was pretreated by ultrasound before pepsin hydrolysis under optimized conditions. The findings indicated that the hydrolyzed products subjected to ultrasonic pretreatment exhibited enhanced solubility, surface hydrophobicity, water and oil retention, foaming characteristics, and emulsifying ability compared to the untreated hydrolyzed products. Furthermore, the piezoelectric properties of the protein with ultrasonic pretreatment were also significantly improved. Additionally, the protein-based piezoelectric device displayed excellent sensing performance and was successfully applied for human motion detection and precise identification of different pressure positions. These findings indicate that ultrasound has great potential to improve the physicochemical quality of eggshell membrane proteins, providing a theoretical basis and research approach for food protein modification and the preparation of green electronic devices. Full article
(This article belongs to the Section Physical Chemistry and Chemical Physics)
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Graphical abstract

Graphical abstract
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<p>The three-dimensional (3D) response surface graphs and two-dimensional (2D) contour plots exhibiting the interactive effects of enzyme usage (<b>a</b>); pH (<b>b</b>); solid-to-solvent ratio (<b>c</b>); and time (<b>d</b>) on EY. Interaction between (<b>a</b>,<b>a′</b>) enzyme usage and pH; (<b>b</b>,<b>b′</b>) enzyme usage and solid-to-solvent ratio; (<b>c</b>,<b>c′</b>) enzyme usage and time; (<b>d</b>,<b>d′</b>) pH and solid-to-solvent ratio; (<b>e</b>,<b>e′</b>) pH and time; (<b>f</b>,<b>f′</b>) solid-to-solvent ratio and time.</p>
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<p>The functional properties of different samples. (<b>a</b>) solubility and H<sub>0</sub>; (<b>b</b>) WHC and OHC; (<b>c</b>) FC and FS; (<b>d</b>) EAI and ESI. Mean value ± standard deviations of three independent experiments were shown (<span class="html-italic">n</span> = 3). Different letters labeled mean significant difference (<span class="html-italic">p</span> &lt; 0.05).</p>
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<p>(<b>a</b>) FTIR spectra of ESMP, PSC, and UPSC; (<b>b</b>) FTIR of the range of 650 to 2200 cm<sup>−1</sup> for the samples; (<b>c</b>–<b>e</b>) FTIR amide I regions of ESMP, PSC, UPSC, and deconvolution of amide I bands into individual peaks; (<b>f</b>) The secondary structure contents of ESMP, PSC, and UPSC.</p>
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<p>SEM image of different samples. (<b>a</b>,<b>b</b>) ESM; (<b>c</b>) ESM with enzyme treatment; (<b>d</b>) ESM with ultrasonic-assisted enzyme treatment; (<b>e</b>) PSC, and (<b>f</b>) UPSC.</p>
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<p>Mechanical properties of different samples. (<b>a</b>) Stress-strain curves; (<b>b</b>) The maximum tensile stress; (<b>c</b>) Breaking strain; (<b>d</b>) Young’s modulus of different samples. Mean ± SD of three independent experiments are shown (<span class="html-italic">n</span> = 3).</p>
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<p>Piezoelectric performance of all samples. (<b>a</b>) The voltages and (<b>b</b>) currents of different samples; (<b>c</b>) Piezoelectric voltages and (<b>d</b>) currents at 1.5 Hz under different applied forces (5–40 N); (<b>e</b>) Piezoelectric voltages and (<b>f</b>) currents under 10 N at different frequencies (0.3–1.5 Hz); (<b>g</b>,<b>h</b>) Stability test of the device under 3000 working cycles.</p>
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<p>Applications of the device in detecting various human motions. (<b>a</b>) Diagram of the test on the human body; (<b>b</b>–<b>e</b>) The signals corresponding to finger bending, wrist bending, elbow bending, and knee bending; (<b>f</b>) Schematic diagram of a 4 × 4 pixel sensing array; (<b>g</b>) The voltages corresponding to spatial pressure distributions.</p>
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25 pages, 15725 KiB  
Article
Columnar-to-Equiaxed Transition on Laser Powder Bed Fusion Ultra-Precision Additive Manufacturing Accuracy and Surface Roughness for Solidified 316L Micro-Lattice Structure
by Chenxu Li, Zhanqiang Liu, Xiaoliang Liang, Jinfu Zhao, Yukui Cai and Bing Wang
Metals 2025, 15(3), 267; https://doi.org/10.3390/met15030267 - 28 Feb 2025
Viewed by 126
Abstract
The improvement of PBF manufacturing accuracy has been an urgent problem to solve. The columnar-to-equiaxed transition of rapid solidification during laser powder bed fusion (L-PBF) has been reported, while its influence on the accuracy and surface roughness of fabricated 316L micro-lattice structures remains [...] Read more.
The improvement of PBF manufacturing accuracy has been an urgent problem to solve. The columnar-to-equiaxed transition of rapid solidification during laser powder bed fusion (L-PBF) has been reported, while its influence on the accuracy and surface roughness of fabricated 316L micro-lattice structures remains to be studied. This study presents a novel fully coupled finite volume method for cellular automata (CA), integrated with response surface methodology (RSM), which is applied to investigate the columnar-to-equiaxed transition influence on the accuracy and surface roughness of ultra-precision additive manufactured 316L lattice structure by L-PBF. It is proven that the higher overlap is identified as the optimal strategy for improving both surface quality and dimensional accuracy. Both the CA model prediction and the experimental results reveal that the effect of latent heat releases from the grain refinement on the adhesion of the surrounding powder is an increment of the surface roughness, while the decrement of the surface quality and accuracy. The overlap strategy is promoted to be the most suitable measure to achieve both high surface quality and manufacturing accuracy. The surface roughness Ra (SP) can rapidly decrease by 68.6%, and the mean diameters decrease by 18.7% under the overlap strategy. Full article
(This article belongs to the Special Issue Advances in Laser Processing of Metals and Alloys)
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<p>(<b>a</b>) The outlook of additive manufacturing equipment WXL-120E; (<b>b</b>) The forming chamber of WXL-120E; (<b>c</b>) Micro-morphology of 316L stainless steel powder; (<b>d</b>) The CAD design of the lattice structure.</p>
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<p>L-PBF fabricated lattice specimens (#9 missing).</p>
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<p>(<b>a</b>) Schematics of three directions; (<b>b</b>) SEM image taken at 100× magnification showing the top-view surface morphology of the 45° inclined struts of specimen #1–#15 (#9 missing); The surface roughness and 3D height topography in the (<b>c</b>) vertical direction, (<b>d</b>) incline direction, and (<b>e</b>) top direction of specimens.</p>
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<p>(<b>a</b>) Schematics of three directions; (<b>b</b>) SEM image taken at 100× magnification showing the top-view surface morphology of the 45° inclined struts of specimen #1–#15 (#9 missing); The surface roughness and 3D height topography in the (<b>c</b>) vertical direction, (<b>d</b>) incline direction, and (<b>e</b>) top direction of specimens.</p>
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<p>(<b>a</b>) Schematics of three directions; (<b>b</b>) SEM image taken at 100× magnification showing the top-view surface morphology of the 45° inclined struts of specimen #1–#15 (#9 missing); The surface roughness and 3D height topography in the (<b>c</b>) vertical direction, (<b>d</b>) incline direction, and (<b>e</b>) top direction of specimens.</p>
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<p>Microstructural evolution of the cellular automata simulations of the single-layer laser melted part, which demonstrate the dendrite growth at (<b>a</b>) 0.01 s, (<b>b</b>) 0.1 s, (<b>c</b>) 0.2 s, and (<b>d</b>) 0.6 s; (<b>e</b>) Illustration of microstructural evolution and solidification during the manufacturing process.</p>
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<p>(<b>a</b>) Inverse pole figure (IPF) maps showing the cross-sectional microstructural features of #8 manufacturing specimens; (<b>b</b>) pole figure (PF) maps corresponding to (<b>a</b>).</p>
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<p>Normal probability plot of (<b>a</b>) vertical mean diameter, (<b>b</b>) incline top roughness, and (<b>c</b>) incline mean diameter.</p>
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<p>The predicted value against the actual experimental data for (<b>a</b>) vertical mean diameter, (<b>b</b>) incline top roughness, and (<b>c</b>) incline mean diameter.</p>
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<p>Contour graph showing vertical mean diameter (μm). (<b>a</b>) Under the combined effect of variable A and B, (<b>b</b>) Under the combined effect of variable A and C.</p>
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<p>The surface plot for vertical mean diameter (μm). (<b>a</b>) Under the combined effect of variable A and B, (<b>b</b>) Under the combined effect of variable A and C.</p>
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<p>Contour graph showing incline top roughness (μm). (<b>a</b>) Under the combined effect of variable A and B, (<b>b</b>) Under the combined effect of variable A and C.</p>
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<p>The surface plot for incline top roughness (μm). (<b>a</b>) Under the combined effect of variable A and B, (<b>b</b>) Under the combined effect of variable A and C.</p>
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<p>Contour graph showing incline mean diameter (μm). (<b>a</b>) Under the combined effect of variable A and B, (<b>b</b>) Under the combined effect of variable A and C.</p>
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<p>The surface plot for incline mean diameter (μm). (<b>a</b>) Under the combined effect of variable A and B, (<b>b</b>) Under the combined effect of variable A and C.</p>
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<p>Desirability contour graphs for each factor with terms: (<b>a</b>) laser power and scan speed; (<b>b</b>) laser power and overlap. The combined desirability value is 0.743.</p>
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<p>Desirability contour graphs for each factor with terms: (<b>a</b>) laser power and scan speed; (<b>b</b>) laser power and overlap. The combined desirability value is 0.743.</p>
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<p>Optimization solution and validation for input factor and response variables with a desirability of 0.743. Under the optimal parameter set of laser power 377.157 W, scan speed 200 mm/s, and overlap 0.08 mm, it is predicted that the best actual manufacturing size and roughness will be achieved.</p>
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<p>(<b>a</b>–<b>c</b>) Inverse pole figure (IPF) maps showing the cross-sectional microstructural features of #13, #15, and #14 manufacturing specimens, respectively; (<b>d</b>–<b>f</b>) pole figure (PF) maps corresponding to (<b>a</b>–<b>c</b>), respectively.</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 216
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>
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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>
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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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31 pages, 11309 KiB  
Article
Water–Fertilizer Synergistic Effects and Resource Optimization for Alfalfa Production: A Central Composite Design and Response Surface Methodology Approach
by Gaiya Mu, Yuanbo Jiang, Haiyan Li, Sinan Wei, Guangping Qi, Yanxia Kang, Minhua Yin, Yanlin Ma, Yayu Wang, Yanbiao Wang and Jinwen Wang
Plants 2025, 14(5), 731; https://doi.org/10.3390/plants14050731 - 27 Feb 2025
Viewed by 172
Abstract
This study posits that strategically optimizing irrigation and fertilization regimes can enhance the productivity and water use efficiency (WUE) of alfalfa (Medicago sativa L.), thereby mitigating the constraints imposed by soil impoverishment and water scarcity in forage production systems of arid and [...] Read more.
This study posits that strategically optimizing irrigation and fertilization regimes can enhance the productivity and water use efficiency (WUE) of alfalfa (Medicago sativa L.), thereby mitigating the constraints imposed by soil impoverishment and water scarcity in forage production systems of arid and semi-arid regions. Conducted over two years, the outdoor pot experiment investigated the effects of water regulation during the branching and bud stages (each at 60–100% θ0.85, where θ0.85 = 0.85θfc) and different levels of nitrogen and phosphorus fertilization (0–280 kg/ha each) on alfalfa yield and WUE. Using Response Surface Methodology (RSM) with a Central Composite Design (CCD), we modeled the relationships between input variables and key response parameters: total yield, evapotranspiration (ET), and WUE. The response surface models exhibited high reliability, with coefficients of determination R2, adjusted R2, predicted R2, and adequate precision exceeding 0.94, 0.90, 0.86, and 13.6, respectively. Sensitivity analysis indicated that water regulation during critical growth stages, particularly the branching stage, had the most significant impact on yield and ET, while nitrogen and phosphorus fertilization positively influenced WUE. Within the appropriate range of water management, judicious fertilization significantly enhanced alfalfa production performance, although excessive inputs resulted in diminishing returns. This study identified the optimal conditions for sustainable production: branching stage water regulation (82.26–83.12% θ0.85) and bud stage water regulation (78.11–88.47% θ0.85), along with nitrogen application (110.59–128.88 kg/ha) and phosphorus application (203.86–210 kg/ha). These findings provide practical guidelines for improving the sustainability and efficiency of alfalfa production in resource-limited environments. Full article
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<p>The violin plots of experimental run response variables (yield, water consumption (ET), and water use efficiency (WUE)) versus the independent factors of branching stage water (<b>A</b>), budding stage water (<b>B</b>), nitrogenous fertilizer (<b>C</b>), and phosphate fertilizer (<b>D</b>), respectively. In the plot, n denotes the number of replicates corresponding to each specific level of a given factor.</p>
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<p>The predicted versus actual values plots of the experimental results: yield in 2022 (<b>a</b>) and 2023 (<b>d</b>), water consumption (ET) in 2022 (<b>b</b>) and 2023 (<b>e</b>), and water use efficiency (WUE) in 2022 (<b>c</b>) and 2023 (<b>f</b>).</p>
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<p>The normal probability plots of the experimental results: yield in 2022 (<b>a</b>) and 2023 (<b>d</b>), water consumption (ET) in 2022 (<b>b</b>) and 2023 (<b>e</b>), and water use efficiency (WUE) in 2022 (<b>c</b>) and 2023 (<b>f</b>).</p>
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<p>Pareto chart of standardized effects for yield in 2022 (<b>a</b>) and 2023 (<b>b</b>), water consumption in 2022 (<b>c</b>) and 2023 (<b>d</b>), and water use efficiency (WUE) in 2022 (<b>e</b>) and 2023 (<b>f</b>). Here, factor A represents water during the branching stage, factor B represents water during the budding stage, factor C denotes nitrogen fertilization, and factor D signifies phosphorus fertilization. The x-axis represents the coefficient of each parameter in the regression model divided by its standard error. All parameters extending beyond the vertical dotted line at <span class="html-italic">p</span> = 0.05 (<span class="html-italic">p</span> = 0.01) have significant (highly significant) effects on the response variable.</p>
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<p>The 3D response surface plots of the interaction of AB (<b>a</b>), AC (<b>b</b>), AD (<b>c</b>), BC (<b>d</b>), BD (<b>e</b>), and CD (<b>f</b>) on yield in 2022. Here, factor A represents water during the branching stage, factor B represents water during the budding stage, factor C denotes nitrogen fertilization, and factor D signifies phosphorus fertilization.</p>
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<p>The 3D response surface plots of the interaction of AB (<b>a</b>), AC (<b>b</b>), AD (<b>c</b>), BC (<b>d</b>), BD (<b>e</b>), and CD (<b>f</b>) on yield in 2023. Here, factor A represents water during the branching stage, factor B represents water during the budding stage, factor C denotes nitrogen fertilization, and factor D signifies phosphorus fertilization.</p>
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<p>The 3D response surface plots of the interaction of AB (<b>a</b>), AC (<b>b</b>), AD (<b>c</b>), BC (<b>d</b>), BD (<b>e</b>), and CD (<b>f</b>) on water consumption (ET) in 2022. Here, factor A represents water during the branching stage, factor B represents water during the budding stage, factor C denotes nitrogen fertilization, and factor D signifies phosphorus fertilization.</p>
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<p>The 3D response surface plots of the interaction of AB (<b>a</b>), AC (<b>b</b>), AD (<b>c</b>), BC (<b>d</b>), BD (<b>e</b>), and CD (<b>f</b>) on water consumption (ET) in 2022. Here, factor A represents water during the branching stage, factor B represents water during the budding stage, factor C denotes nitrogen fertilization, and factor D signifies phosphorus fertilization.</p>
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<p>The 3D response surface plots of the interaction of AB (<b>a</b>), AC (<b>b</b>), AD (<b>c</b>), BC (<b>d</b>), BD (<b>e</b>), and CD (<b>f</b>) on water consumption (ET) in 2023. Here, factor A represents water during the branching stage, factor B represents water during the budding stage, factor C denotes nitrogen fertilization, and factor D signifies phosphorus fertilization.</p>
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<p>The 3D response surface plots of the interaction of AB (<b>a</b>), AC (<b>b</b>), AD (<b>c</b>), BC (<b>d</b>), BD (<b>e</b>), and CD (<b>f</b>) on water consumption (ET) in 2023. Here, factor A represents water during the branching stage, factor B represents water during the budding stage, factor C denotes nitrogen fertilization, and factor D signifies phosphorus fertilization.</p>
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<p>The 3D response surface plots of the interaction of AB (<b>a</b>), AC (<b>b</b>), AD (<b>c</b>), BC (<b>d</b>), BD (<b>e</b>), and CD (<b>f</b>) on water use efficiency (WUE) in 2022. Here, factor A represents water during the branching stage, factor B represents water during the budding stage, factor C denotes nitrogen fertilization, and factor D signifies phosphorus fertilization.</p>
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<p>The 3D response surface plots of the interaction of AB (<b>a</b>), AC (<b>b</b>), AD (<b>c</b>), BC (<b>d</b>), BD (<b>e</b>), and CD (<b>f</b>) on water use efficiency (WUE) in 2022. Here, factor A represents water during the branching stage, factor B represents water during the budding stage, factor C denotes nitrogen fertilization, and factor D signifies phosphorus fertilization.</p>
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<p>The 3D response surface plots of the interaction of AB (<b>a</b>), AC (<b>b</b>), AD (<b>c</b>), BC (<b>d</b>), BD (<b>e</b>), and CD (<b>f</b>) on water use efficiency (WUE) in 2023. Here, factor A represents water during the branching stage, factor B represents water during the budding stage, factor C denotes nitrogen fertilization, and factor D signifies phosphorus fertilization.</p>
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<p>Desirability ramp for numerical optimization of goals in 2022 (<b>a</b>) and 2023 (<b>b</b>). Optimal factor settings are shown with red points and optimal response prediction values are displayed in blue. Here, ET denotes water consumption and WUE refers to water use efficiency.</p>
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<p>Environmental factors and timeline of the alfalfa growth periods in 2022 (<b>a</b>) and 2023 (<b>b</b>). Tmax, maximum temperature; Tmin, minimum temperature; Rmax, maximum radiation; and Rmin, minimum radiation.</p>
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<p>CCD-RSM optimization diagram based on experimental design.</p>
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18 pages, 1031 KiB  
Article
Optimization of Surfactant-Mediated Green Extraction of Phenolic Compounds from Grape Pomace Using Response Surface Methodology
by Milica Atanacković Krstonošić, Darija Sazdanić, Mira Mikulić, Dejan Ćirin, Jovana Milutinov and Veljko Krstonošić
Int. J. Mol. Sci. 2025, 26(5), 2072; https://doi.org/10.3390/ijms26052072 - 27 Feb 2025
Viewed by 134
Abstract
Grape pomace is a by-product abundant in phenolic compounds that can be used in the food, cosmetic, and pharmaceutical industries. For the efficient extraction of such compounds, an aqueous solution of non-ionic surfactant Brij S20 was applied as a green extraction medium, and [...] Read more.
Grape pomace is a by-product abundant in phenolic compounds that can be used in the food, cosmetic, and pharmaceutical industries. For the efficient extraction of such compounds, an aqueous solution of non-ionic surfactant Brij S20 was applied as a green extraction medium, and the optimization was performed using surface response methodology. The effects of four independent factors (surfactant concentration, time, pH, and solvent-to-material ratio) were evaluated, and total phenolic content (TPC), DPPH radical inhibition, and selected polyphenol compound concentrations were analyzed as responses. Using response surface methodology (RSM), five regression equations were derived and good adequacy of the models was confirmed. The solvent-to-material (SM) ratio was the most influential factor. Surfactant concentration of 3% (m/V), extraction time of 120 min, pH value of 4.06, and SM ratio of 50 mL/g were determined as optimum conditions to maximize all responses. Under the optimal conditions, the mean validated values obtained for TPC, DPPH, gallic acid, catechin, and quercetin concentrations were 968.50 ± 37.06 mg GAE/L, 61.41 ± 7.13%, 5.10 ± 0.05 mg/L, 10.62 ± 0.79 mg/L, and 6.04 ± 0.10 mg/L, respectively. Furthermore, the established conditions were applied for the extraction of phenolic compounds from grape pomace of four grape varieties. The proposed extraction method proved effective, providing extracts rich in polyphenols suitable for further applications. Full article
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<p>Response surface plots showing the interaction effect of process variables (C (Brij S20), time, pH, and SM ratio) on TPC (<b>A</b>), DPPH inhibition (<b>B</b>), gallic acid concentration (<b>C</b>), catechin concentration (<b>D</b>), and quercetin concentration (<b>E</b>). Only the interactive effect between C (Brij S20) and SM ratio was statistically significant (<span class="html-italic">p</span> = 0.0263) (<a href="#ijms-26-02072-t002" class="html-table">Table 2</a>). A study on optimization of the extraction of phenolic compounds from grape juice and wine pomaces using ethanol and acetone showed that four factors were significant for DPPH inhibition, including temperature, time, solvent type, and pomace type [<a href="#B33-ijms-26-02072" class="html-bibr">33</a>].</p>
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23 pages, 10251 KiB  
Article
Comparative Analysis and Optimization of LID Practices for Urban Rainwater Management: Insights from SWMM Modeling and RSM Analysis
by Yepeng Mai, Xueliang Ma, Fei Cheng, Yelin Mai and Guoru Huang
Sustainability 2025, 17(5), 2015; https://doi.org/10.3390/su17052015 - 26 Feb 2025
Viewed by 127
Abstract
Urbanization necessitates Low Impact Development (LID) practices for sustainable development, but existing studies lack analysis about the comprehensive effect and optimal allocation of LID combination practices. To address this gap, this study conducted an in-depth analysis of the runoff control effects of individual [...] Read more.
Urbanization necessitates Low Impact Development (LID) practices for sustainable development, but existing studies lack analysis about the comprehensive effect and optimal allocation of LID combination practices. To address this gap, this study conducted an in-depth analysis of the runoff control effects of individual and combined LID practices and pollutants under varying retrofit proportions, utilizing the Storm Water Management Model (SWMM). Four evaluation metrics were employed for parameter calibration and validation assessment to ensure the accuracy of the SWMM. The Response Surface Methodology (RSM) was then employed to optimize the retrofit proportions of LID practices due to its high efficiency and statistical rigor. The results showed that, under the same retrofit ratio, bio-retention (BC) has a better runoff reduction rate and pollutant removal rate. For example, when the retrofit proportion is 100%, the runoff pollutant removal rates of BC in Parcel 1 and Parcel 2 are 29.6% and 32.9%, respectively. To achieve a 70% runoff control rate, the optimal retrofit proportions for Parcel 1 were 67.5% for green roofs (GR), 92.2% for permeable pavements (PP), 88.9% for bio-retention cells (BC), and 50% for low-elevation greenbelts (LEG); these correspond to the proportions for Parcel 2 that were 65.1%, 68.1%, 82.0%, and 50%, respectively. In conclusion, this study provides scientific and technical support for urban planners and policymakers in urban rainwater management, especially in similar regions. Full article
(This article belongs to the Section Sustainable Water Management)
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<p>Frame flowchart of this research.</p>
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<p>Study area information: (<b>a</b>) study area parcel delineation; (<b>b</b>) type of subsurface in the study.</p>
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<p>Rain gauge and flow meter installation locations and sampling locations for each underlayment.</p>
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<p>Comparison of the simulated flow value and the measure flow value in Parcel 1. (<b>a</b>) 20180527, (<b>b</b>) 20180724, (<b>c</b>) 20190722, (<b>d</b>) 20190902.</p>
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<p>Comparison of the simulated flow value and the measure flow value in Parcel 2. (<b>a</b>) 20180527, (<b>b</b>) 20180724, (<b>c</b>) 20190722, (<b>d</b>) 20190902.</p>
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<p>Site status and suitable areas for LID practices. (<b>a</b>) Underlying surface types of suitable renovation areas; (<b>b</b>) LID practices in renovation areas.</p>
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<p>Runoff volume reduction under different retrofit proportions: (<b>a</b>) Parcel 1; (<b>b</b>) Parcel 2.</p>
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<p>Runoff pollutant reduction under different retrofit proportions: (<b>a</b>) Parcel 1; (<b>b</b>) Parcel 2.</p>
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24 pages, 8116 KiB  
Article
Nanostructured Strategies for Melanoma Treatment—Part I: Design and Optimization of Curcumin-Loaded Micelles for Enhanced Anticancer Activity
by Valentina Paganini, Andrea Cesari, Silvia Tampucci, Patrizia Chetoni, Susi Burgalassi, Michele Lai, Giulia Sciandrone, Silvia Pizzimenti, Fabio Bellina and Daniela Monti
Pharmaceuticals 2025, 18(3), 327; https://doi.org/10.3390/ph18030327 - 26 Feb 2025
Viewed by 177
Abstract
Background/Objectives: Melanoma is a pathology that affects a large part of the population, and the currently available therapies have many limitations, including the selective targeting of the site of action. This study explores the development of curcumin (CUR)-loaded nanostructured delivery systems for [...] Read more.
Background/Objectives: Melanoma is a pathology that affects a large part of the population, and the currently available therapies have many limitations, including the selective targeting of the site of action. This study explores the development of curcumin (CUR)-loaded nanostructured delivery systems for topical melanoma treatment, addressing CUR’s limitations in bioavailability, solubility, and stability. Methods: Binary surfactant mixtures of Vitamin E-TPGS (TPGS) and Kolliphor ELP (ELP) were selected to form stable micelles for curcumin encapsulation. A Design of Experiments (DoE) approach was applied to optimize the surfactant ratios for enhanced drug solubilization and improved cytotoxic effects on melanoma cells. The final formulation was characterized using Fourier Transform Infrared Spectroscopy (FTIR), Differential Scanning Calorimetry (DSC), and Nuclear Magnetic Resonance (NMR) spectroscopy to confirm its properties. Results: The final formulation, TPGS30ELP15, contained 30 mM TPGS and 15 mM ELP and led to formation of nanostructures of the expected size (hydrodinamic diameter, Dh: 13.11 ± 0.01 nm; polydispersivity index, PDI = 0.371 ± 0.05), able to solubilize 5.51 ± 1.09 mM CUR. The formulation was stable for a 120-day period stored at 4 °C and room temperature in the dark. Cytotoxicity testing in A375 melanoma cells demonstrated that curcumin-loaded micelles significantly reduced cell viability compared to free curcumin. Long-term exposure (24 h) revealed that free curcumin caused an 85% reduction in cell viability, while TPGS30ELP15 resulted in a 70% reduction. Additionally, free curcumin induced a 30% increase in cytoplasmic area, indicating necrosis, whereas TPGS30ELP15 decreased the cytoplasmic area by 20%, suggesting apoptosis. Conclusions: This study demonstrates that TPGS30ELP15 nanomicelles enhance curcumin’s anticancer effects while promoting apoptosis and minimizing necrosis, which is associated with lower inflammation and tissue damage. These findings suggest that TPGS30ELP15 offers a more favorable therapeutic profile for melanoma treatment, paving the way for safer and more effective topical therapies. Full article
(This article belongs to the Special Issue Self-Assembling Nanostructures for Cancer Therapy)
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Graphical abstract

Graphical abstract
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<p>Response surfaces for the two dependent variables: CUR solubilized (<b>a</b>) and Cell viability (<b>b</b>). Blue dots represent experimental values.</p>
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<p>ATR- FTIR spectra of raw materials (curcumin, TPGS, ELP) and freeze-dried micelles with and without curcumin (TPGS30ELP15-F and empty TPGS30ELP15-F, respectively).</p>
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<p>DSC thermograms of raw materials (curcumin, TPGS, ELP) and freeze-dried micelles with and without curcumin (TPGS30ELP15-F and empty TPGS30ELP15-F, respectively).</p>
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<p>H NMR WATERGATE (500 MHz, D<sub>2</sub>O, 25 °C) spectra of CUR, ELP, TPGS and TPGS30ELP15.</p>
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<p>Microscopic observation of TPGS30ELP15 under TEM; scale bar 40 nm.</p>
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<p>Time-dependent changes in size (•, D<sub>h</sub>) and recovered CUR percentage (■, CUR recovered) for the TPGS30ELP15 formulation stored at 4 °C and room temperature, both in the dark (<b>A</b>) and under light exposure (<b>B</b>) (n = 3).</p>
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<p>Time-dependent effect of the curcumin-loaded nanomicellar formulation, TPGS30ELP15, on A375 cells. Results are presented as means ± SEM from three independent replicates. * statistical significance <span class="html-italic">p</span> &lt; 0.05; **** statistical significance <span class="html-italic">p</span> &lt; 0.0001.</p>
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<p>CUR and TPGS30ELP15 induce cell death by different pathways. (<b>a</b>) Illustration of the experimental workflow. (<b>b</b>) Representative images of A375 cells treated or not with CUR or TPG30ELP15 and analyzed 24 h after. Nuclei were stained with Hoechst 33,342 (Blue) and cytoplasm was reconstructed using Digital Phase Contrast (Gray). Number of nuclei (%) (<b>c</b>) and cytoplasmatic area (<b>d</b>) were measured by high-content confocal microscopy assays and expressed compared to the untreated counterparts. Data are expressed as mean ± SEM and were analysed using one-way ANOVA (n = 3; **** <span class="html-italic">p</span> &lt; 0.0001).</p>
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<p>Percentage cell viability of Balb/3T3 clone A31 cells after treatments with TPGS30ELP15 at CUR concentration ranging from 0.1 to 15 μg/mL for 24 h.</p>
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16 pages, 4337 KiB  
Article
Innovative Methods for Intensifying the Processing of Zinc Clinker: Synergy of Microwave Treatment and Ultrasonic Leaching
by Bagdaulet Kenzhaliyev, Tatiana Surkova, Ainur Berkinbayeva, Zhazira Baltabekova, Kenzhegali Smailov, Yerkezhan Abikak, Shynar Saulebekkyzy, Nazerke Tolegenova, Tursynkul Omirbek and Zamzagul Dosymbaeva
Metals 2025, 15(3), 246; https://doi.org/10.3390/met15030246 - 25 Feb 2025
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Abstract
This study presents an innovative approach to processing refractory zinc-bearing clinker through the synergistic application of microwave thermal treatment and ultrasonic-assisted leaching. Microwave irradiation induces phase transformations in the clinker, improving its reactivity and facilitating subsequent zinc dissolution, while ultrasonic cavitation enhances mass [...] Read more.
This study presents an innovative approach to processing refractory zinc-bearing clinker through the synergistic application of microwave thermal treatment and ultrasonic-assisted leaching. Microwave irradiation induces phase transformations in the clinker, improving its reactivity and facilitating subsequent zinc dissolution, while ultrasonic cavitation enhances mass transfer by disrupting passivation layers. Key process parameters, including acid concentration, temperature, pulp density, and leaching time, were systematically investigated using response surface methodology (RSM) and central composite design (CCD). The results demonstrate that the optimized process conditions led to a significant increase in zinc recovery from refractory materials. Full article
(This article belongs to the Special Issue Advances in Mineral Processing and Hydrometallurgy—3rd Edition)
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<p>A flow diagram of the experiment.</p>
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<p>Schematic diagram of the leaching experimental setup. The lower part of the figure illustrates the ultrasonic probe and the cavitation effect, where microbubbles collapse, generating localized high pressure and temperature, which enhances the leaching efficiency.</p>
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<p>Sphalerite.</p>
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<p>Diffractogram of the clinker (reprinted from Ref. [<a href="#B49-metals-15-00246" class="html-bibr">49</a>]).</p>
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<p>(<b>a</b>) Microstructure of the initial sample and energy-dispersive analysis of sphalerite prior to microwave irradiation at 25 °C; (<b>b</b>,<b>c</b>) microstructure and energy-dispersive analysis of sphalerite after microwave irradiation at 600 °C for 3–4 min; (<b>d</b>) microstructure and energy-dispersive analysis of sphalerite after microwave irradiation at 600 °C for 5–7 min.</p>
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<p>(<b>a</b>) A plot of normal probability vs. the internally studentized residuals, (<b>b</b>) internally studentized residuals vs. the predicted responses, (<b>c</b>) internally studentized residuals vs. run number, and (<b>d</b>) predicted responses vs. the actual values.</p>
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<p>Three-dimensional response surfaces (with other parameters maintained at their central levels), illustrating the combined effects of B and A (<b>a</b>); D and A (<b>b</b>); D and B (<b>c</b>) (A—leaching duration, B—sulfuric acid concentration, D—temperature).</p>
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<p>Ultrasonic cavitation.</p>
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<p>The effect of ultrasound on clinker leaching.</p>
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18 pages, 4976 KiB  
Article
Optimising Supercritical Carbon Dioxide Extraction of Rosmarinic Acid from Rosmarinus officinalis L. and Enhancing Yield Through Soxhlet Coupling
by Meryem Boufetacha, Elkhadir Gharibi and Mohammed Benali
Processes 2025, 13(3), 655; https://doi.org/10.3390/pr13030655 - 25 Feb 2025
Viewed by 357
Abstract
Rosmarinic acid (RA) is a bioactive phenolic compound prevalent in various medicinal plants, renowned for its significant pharmacological properties. This study aims to optimise the extraction conditions of this compound from Rosmarinus officinalis L. using the response surface methodology (RSM) with a three-variable, [...] Read more.
Rosmarinic acid (RA) is a bioactive phenolic compound prevalent in various medicinal plants, renowned for its significant pharmacological properties. This study aims to optimise the extraction conditions of this compound from Rosmarinus officinalis L. using the response surface methodology (RSM) with a three-variable, three-level Box–Behnken design. Optimising the parameters for supercritical CO2 (scCO2) extraction focused on pressure (150 to 350 bar), temperature (40 to 80 °C), and co-solvent weight percentage (5 to 15% ethanol), evaluating their impact on overall yield and RA content. The optimal conditions determined were a pressure of 150 bar, a temperature of 80 °C, and 15% ethanol, yielding a total extract of 21.86 ± 1.55%, with an RA content of 3.43 ± 0.13 mg/g dry matter (DM). Scanning electron microscopy revealed that the scCO2 treatment induced microcracks on the surface of the rosemary powder, enhancing the fluid’s ability to penetrate the plant matrix. By employing the combined scCO2-Soxhlet method, the RA content increased to 5.78 mg/g DM. Furthermore, the final extract obtained using the Soxhlet post-scCO2 treatment contained only trace amounts of carnosic acid (0.38 ± 0.10 mg/g DM) and carnosol (0.38 ± 0.20 mg/g DM), compared to the crude extract obtained solely with Soxhlet, which exhibited significantly higher concentrations of 8.45 ± 2.98 mg/g DM of carnosol and 16.67 ± 0.94 mg/g DM of carnosic acid. This work highlighted an innovative extraction strategy based on the coupling of scCO2 and Soxhlet, which significantly increased RA content while reducing concentrations of other compounds such as CA and CAR. This approach makes it possible to produce RA-enriched extracts, offering considerable potential for future large-scale applications and commercialisation. Full article
(This article belongs to the Section Chemical Processes and Systems)
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Graphical abstract
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<p>Chemical structure of RA (C₁₈H₁₆O₈).</p>
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<p>Response surfaces showing the combined effects of temperature (<b>A</b>), pressure (<b>B</b>), and percentage of co-solvent (<b>C</b>) on total extraction yield.</p>
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<p>Graph of the coefficients for the response of the RA content.</p>
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<p>Response surfaces showing the combined effects of temperature (<b>A</b>), pressure (<b>B</b>), and percentage of co-solvent (<b>C</b>) on RA content.</p>
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<p>SEM images of rosemary powder before and after ScCO<sub>2</sub> extraction: (<b>A</b>) rosemary powder before extraction; (<b>B</b>) rosemary powder after extraction.</p>
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<p>RA, CA, and CAR content obtained with Soxhlet alone and Soxhlet after scCO<sub>2.</sub></p>
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<p>HPLC chromatogram of rosemary leaf extracts and rosmarinic acid, carnosol, and carnosic acid structures (showing absorption peaks at 284 nm).</p>
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