[go: up one dir, main page]
More Web Proxy on the site http://driver.im/
You seem to have javascript disabled. Please note that many of the page functionalities won't work as expected without javascript enabled.
 
 
Sign in to use this feature.

Years

Between: -

Subjects

remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline

Journals

remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline

Article Types

Countries / Regions

remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline

Search Results (1,810)

Search Parameters:
Keywords = ATR FT-IR

Order results
Result details
Results per page
Select all
Export citation of selected articles as:
19 pages, 2563 KiB  
Article
Insulin-Sensitizing Properties of Decoctions from Leaves, Stems, and Roots of Cucumis prophetarum L.
by Zewdie Mekonnen, Giuseppe Petito, Getasew Shitaye, Gianluca D’Abrosca, Belete Adefris Legesse, Sisay Addisu, Maurizio Ragni, Antonia Lanni, Roberto Fattorusso, Carla Isernia, Lara Comune, Simona Piccolella, Severina Pacifico, Rosalba Senese, Gaetano Malgieri and Solomon Tebeje Gizaw
Molecules 2025, 30(1), 98; https://doi.org/10.3390/molecules30010098 (registering DOI) - 30 Dec 2024
Viewed by 109
Abstract
Type 2 diabetes mellitus (T2DM) is a chronic disease characterized by insulin resistance and impaired beta-cell secretory function. Since existing treatments often present side effects based on different mechanisms, alternative therapeutic options are needed. In this scenario, the present study first evaluates the [...] Read more.
Type 2 diabetes mellitus (T2DM) is a chronic disease characterized by insulin resistance and impaired beta-cell secretory function. Since existing treatments often present side effects based on different mechanisms, alternative therapeutic options are needed. In this scenario, the present study first evaluates the cytotoxicity of decoctions from the leaves, stems, and roots of Cucumis prophetarum L. on HepG2 and L6C5 cells. The extracts were chemically investigated by UV–Vis and ATR-FTIR spectroscopic techniques and by ultra high-performance chromatographic techniques, coupled with high-resolution mass spectrometry. Briefly, decoctions from the leaves and stems were mainly composed of apigenin C-glycosides, while the root decoction was rich in raffinose and cucumegastigmane II. To evaluate the insulin-sensitizing properties of the extracts in insulin-resistant L6 myoblasts, an evaluation by Western blot analysis of the proteins in the insulin signaling pathway was then performed. Particularly, key proteins of insulin signaling were investigated, i.e., insulin receptor substrate (IRS-1), protein kinase B (PKB/AKT), and glycogen synthase kinase-3 (GSK-3β), which have gained considerable attention from scientists for the treatment of diabetes. Under all conditions tested, the three decoctions showed low cytotoxicity. The stem and root decoction (300 μg/mL) resulted in a significant increase in the levels of p-IRS-1 (Tyr612), GSK3β (Ser9), and p-AMPK (Thr172) compared to those of the palmitic acid-treated group, and the leaf decoction resulted an increase in the level of p-IRS-1 (Tyr612) and p-AMPK (Thr172) and a decrease in p-GSK3β (Ser9) compared to the levels for the palmitic acid-treated group. The root decoction also reduced the level of p-mToR (Ser2448). Overall, the acquired data demonstrate the effect of reducing insulin resistance induced by the investigated decoctions, opening new scenarios for the evaluation of these effects aimed at counteracting diabetes and related diseases in animal models. Full article
Show Figures

Figure 1

Figure 1
<p>Extraction scheme applied to leaf (CpdL), stem (CpdS), and root (CpdR) organs of <span class="html-italic">Cucumis prophetarum</span> L. The plant parts were photographed during sample collection (around Lake Tana, Abay River Basin, northwestern Ethiopia, 2022/3).</p>
Full article ">Figure 2
<p>(<b>A</b>) UV–Vis spectra and (<b>B</b>) ATR-FTIR spectra of leaf decoction (CpdL), stem decoction (CpdS), and root decoction (CpdR); (<b>C</b>) enlarged region (500–2000 cm<sup>−1</sup>) of the ATR-FTIR spectrum of CpdR decoction.</p>
Full article ">Figure 3
<p>Total ion current (TIC) chromatograms of leaf, stem, and root extracts obtained by decoction. TOF-MS data are tabulated below, along with ring double bonds (RDB) data. Ox PUFA = oxidized polyunsaturated fatty acids.</p>
Full article ">Figure 4
<p>Cell viability evaluation. The viability of (<b>A</b>) HepG2 and (<b>B</b>) L6 cells was analyzed after 24 h for leaf, stem, and root decoction exposition compared to the results for the control (100%). Data are represented as mean ± SEM of the percentage of viable cells compared to that of the CTR group. * <span class="html-italic">p</span> &lt; 0.05; *** <span class="html-italic">p</span> = 0.0001; **** <span class="html-italic">p</span> &lt; 0.0001. ns = not significant.</p>
Full article ">Figure 5
<p>(<b>A</b>,<b>B</b>) Oil Red O staining and Oil Red O quantification (OD value) of L6 skeletal muscle cells treated with PA (0.75 mM), PA and a decoction extract of leaves, stems, and roots (300 μg/mL) of <span class="html-italic">C. prophetarum.</span> Cells were observed under 10X magnification, with a scale bar of 2 μm. Values are represented as means ± SEM; (n = 3/group). One-way ANOVA was used for statistical analysis. <span class="html-italic">p</span> &lt; 0.05 was considered significant. * <span class="html-italic">p</span> &lt; 0.05 vs. CTR; # <span class="html-italic">p</span> &lt; 0.05 vs. PA. CTR: control; PA: palmitic acid; PA + CpdL: palmitic acid plus leaf decoction extract; PA + CpdS: palmitic acid plus stem decoction extract; PA + CpdR: palmitic acid plus root decoction extract.</p>
Full article ">Figure 6
<p>Effect of leaf, stem, and root decoction extract from <span class="html-italic">C. prophetarum</span> on insulin signaling molecules. L6 cells were pretreated with PA (0.75 mM) for 18 h, followed by treatment with leaf, stem, and root decoction extract of <span class="html-italic">C. prophetarum</span> for 6 h. (<b>A</b>–<b>C</b>) Representative immunoblots of P-IRS1 (Tyr612), P-IRS1 (Ser307), P-AKT (Ser473), P-GSK3β (Ser9), P-AMPKα (Thr172), and P-mTOR (Ser2448). Histograms show the results of the densitometric analysis of immunoblots. B-ACTIN was used as a loading control. Data are represented as mean ± SEM; n = 3. * <span class="html-italic">p</span> &lt; 0.05 vs. CTR; # <span class="html-italic">p</span> &lt; 0.05 vs. PA (one-way ANOVA). <b>CTR:</b> control; <b>PA:</b> palmitic acid; <b>PA + CpdL:</b> palmitic acid plus leaf decoction extract; <b>PA + CpdS:</b> palmitic acid plus stem decoction extract; <b>PA + CpdR:</b> palmitic acid plus root decoction extract.</p>
Full article ">
17 pages, 6383 KiB  
Article
Optimization of the Heterogeneous Synthesis Conditions for Cellulose Tosylation and Synthesis of a Propargylamine Cellulosic Derivative
by Marcos V. Ferreira, Poliana Ricci, Henrique A. Sobreira, Anizio M. Faria, Rodrigo B. Panatieri, Brent S. Sumerlin and Rosana M. N. Assunção
Polymers 2025, 17(1), 58; https://doi.org/10.3390/polym17010058 (registering DOI) - 29 Dec 2024
Viewed by 399
Abstract
Cellulose tosylate (MCC-Tos) is a key derivative for surface modification and a crucial precursor for cellulose compatibilization in click reactions, enabling its functionalization for advanced applications. Replacing tosyl groups with alkyne groups broadens cellulose’s potential in biocompatible reactions, such as thiol-yne click chemistry [...] Read more.
Cellulose tosylate (MCC-Tos) is a key derivative for surface modification and a crucial precursor for cellulose compatibilization in click reactions, enabling its functionalization for advanced applications. Replacing tosyl groups with alkyne groups broadens cellulose’s potential in biocompatible reactions, such as thiol-yne click chemistry and protein/enzyme immobilization. To achieve this, we optimized the heterogeneous synthesis of MCC-Tos using a Doehlert matrix statistical design, evaluating the influence and interaction of the reaction conditions. The optimized conditions—144 h reaction time, 10:1 molar ratio, and 30 °C—yielded a degree of substitution for tosyl groups (DStos) of 1.80, determined via elemental analysis and FTIR-ATR spectroscopy. The reaction kinetics followed a first-order model. A subsequent reaction with propargylamine produced aminopropargyl cellulose (MCC-PNH), reducing DStos by 65%, which was confirmed via FTIR, and improving thermal stability by a margin of 30 °C (TGA/DTG). 13C CP/MAS NMR confirmed the alkyne group attachment, further validated via coupling an azide-functionalized coumarin through copper(I)-catalyzed alkyne-azide cycloaddition (CuAAC). Fluorescence microscopy and UV spectroscopy were used to estimate a substitution degree of 0.21. This study establishes a feasible route for synthesizing alkyne-functionalized cellulose, paving the way for eco-friendly materials, including protein/enzyme bioconjugates, composites, and advanced materials via thiol-yne and CuAAC reactions. Full article
(This article belongs to the Section Polymer Chemistry)
Show Figures

Graphical abstract

Graphical abstract
Full article ">Figure 1
<p>Three-dimensional response surfaces and contour plots for the Doehlert matrix at encoded values of (0,0,0): (<b>A</b>) molar ratio (x<sub>3</sub>) = 5 equiv (TosCl); (<b>B</b>) time (x<sub>2</sub>) = 38 h; (<b>C</b>) temperature (x<sub>1</sub>) = 60 °C.</p>
Full article ">Figure 2
<p>(<b>A</b>) MCC, MCC-Tos, and MCC-P<sub>NH</sub> 24 to 168 h FTIR spectra in the 1650 to 650 cm<sup>−1</sup> range. (<b>B</b>) Plot of DS<sub>tos</sub> as a function of propargyl reaction time.</p>
Full article ">Figure 3
<p>(<b>A</b>) TGA curves; and (<b>B</b>) DTG curves for MCC, MCC-Tos, and MCC-P<sub>NH</sub> 168 h.</p>
Full article ">Figure 4
<p>CP/MAS <sup>13</sup>C-NMR spectra of (<b>A</b>) cellulose (MCC); (<b>B</b>) tosyl-cellulose (MCC-Tos); and (<b>C</b>) amino propargyl-cellulose (MCC-P<sub>NH</sub>) after 168 h of amino propargylation reaction.</p>
Full article ">Figure 5
<p>Fluorescence microscopy images of MCC-P<sub>NH</sub> after azide-coumarin attachment: (<b>A</b>) wide-field image; and (<b>B</b>–<b>D</b>) images for different regions of the same sample, excited at 315 nm with emission at around 430 nm.</p>
Full article ">Scheme 1
<p>(<b>A</b>) Synthetic approach toward the obtention of tosyl-cellulose (MCC-Tos); (<b>B</b>) synthetic route for the obtention of aminopropargyl-cellulose (MCC-PNH) from MCC-Tos.</p>
Full article ">Scheme 2
<p>Synthetic route to obtention of the azide-coumarin attached to MCC-P<sub>NH</sub> via CuAAC reaction.</p>
Full article ">
24 pages, 2390 KiB  
Article
Goat’s Milk Powder Enriched with Red (Lycium barbarum L.) and Black (Lycium ruthenicum Murray) Goji Berry Extracts: Chemical Characterization, Antioxidant Properties, and Prebiotic Activity
by Danijel D. Milinčić, Aleksandar Ž. Kostić, Steva Lević, Uroš M. Gašić, Dragana D. Božić, Relja Suručić, Tijana D. Ilić, Viktor A. Nedović, Bojana B. Vidović and Mirjana B. Pešić
Foods 2025, 14(1), 62; https://doi.org/10.3390/foods14010062 (registering DOI) - 29 Dec 2024
Viewed by 312
Abstract
The current trend in food innovations includes developing products containing plant ingredients or extracts rich in bioactive compounds. This study aimed to prepare and characterize skimmed thermally treated goat’s milk powders enriched with lyophilized fruit extracts of Lycium ruthenicum Murray (GMLR) and Lycium [...] Read more.
The current trend in food innovations includes developing products containing plant ingredients or extracts rich in bioactive compounds. This study aimed to prepare and characterize skimmed thermally treated goat’s milk powders enriched with lyophilized fruit extracts of Lycium ruthenicum Murray (GMLR) and Lycium barbarum L. (GMLB). Proximate analysis, ultra-high performance liquid chromatography with quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS), Fourier transform infrared spectroscopy using attenuated total reflection (FTIR-ATR), and electrophoretic analysis were assessed. Total phenolic content (TPC), total protein content, and antioxidant properties of enriched goat milk powders were determined spectrophotometrically, and prebiotic potential was evaluated by the broth microdilution method. A total of 25 phenolic compounds and 18 phenylamides were detected in the enriched goat milk powders. Electrophoretic analysis showed the absence of proteolysis in the prepared powders. The GMLR showed the highest TPC and displayed a ferric ion-reducing power, probably contributed by anthocyanins and some phenylamides. GMLR and GMLB had higher ABTS radical scavenging activity but lower ferrous ion-chelating capacity than control goat′s milk powder. GMLB and GMLR in a dose-dependent manner (0.3–5 mg/mL) showed a growth-promoting effect on probiotic strains. In summary, prepared goji/goat milk powders, primarily GMLR, might be used as prebiotic supplements or functional food additives. Full article
(This article belongs to the Section Nutraceuticals, Functional Foods, and Novel Foods)
Show Figures

Figure 1

Figure 1
<p>Images of spray-dried powders: (<b>a</b>) goat’s milk powder without extract (control sample) (GM); (<b>b</b>) goat’s milk powder enriched with <span class="html-italic">L. ruthenicum</span> extract (GMLR); and (<b>c</b>) goat’s milk powder enriched with <span class="html-italic">L. barbarum</span> extract (GMLB).</p>
Full article ">Figure 2
<p>FTIR-ATR spectra of goat′s milk (GM) and goat′s milk/goji extracts (GMLR and GMLB) powders. Abbreviations: “GMLR”—goat’s milk powder enriched with <span class="html-italic">L. ruthenicum</span> extract; “GMLB”—goat’s milk powder enriched with <span class="html-italic">L. barbarum</span> extract; and “GM”—goat’s milk powder without extract (control sample).</p>
Full article ">Figure 3
<p>Characteristic MS/MS fragmentation patterns and predicted structures of non-glycosylated spermidine derivatives: (<b>a</b>) <span class="html-italic">N</span>-dihydrocaffeoyl-<span class="html-italic">N</span>′-coumaroyl spermidine (<span class="html-italic">m</span>/<span class="html-italic">z</span> 456); (<b>b</b>) <span class="html-italic">N</span>-caffeoyl-<span class="html-italic">N</span>′-dihydrocaffeoyl spermidine (<span class="html-italic">m</span>/<span class="html-italic">z</span> 472); and (<b>c</b>) <span class="html-italic">N</span>-feruloyl-<span class="html-italic">N</span>′-dihydrocaffeoyl spermidine (<span class="html-italic">m</span>/<span class="html-italic">z</span> 486).</p>
Full article ">Figure 4
<p>Electrophoretic patterns of goat′s milk (GM) and goat′s milk/goji extract (GMLR and GMLB) powders, analyzed by SDS-PAGE in reducing conditions. Lines: “GMLR”—goat’s milk powder enriched with <span class="html-italic">L. ruthenicum</span> extract; “GMLB”—goat’s milk powder enriched with <span class="html-italic">L. barbarum</span> extract; “GM”—goat’s milk powder without extract (control sample); molecular weight standard (LMW); and bovine milk protein standard (SP). Abbreviations: bovine serum albumin (BSA); immunoglobulin hard chain (Ighc); αs2-casein (αs2-CN); αs1-casein (αs1-CN); β-casein (β-CN); κ-casein (κ-CN); β-lactoglobulins (β-LG); and α-lactalbumin (α-LA).</p>
Full article ">Figure 5
<p>The prebiotic potential of the goat′s milk and goat′s milk/goji extract powders on various probiotic strains of microorganisms. The results are presented as minimum and maximum percent of growth stimulation of prepared powders in the range of 0.312–5 mg/mL. Abbreviations: “GMLR”—goat’s milk powder enriched with <span class="html-italic">L. ruthenicum</span> extract; “GMLB”—goat’s milk powder enriched with <span class="html-italic">L. barbarum</span> extract; and “GM”—goat’s milk powder without extract (control sample).</p>
Full article ">
27 pages, 1069 KiB  
Article
Anti-Inflammatory, Antithrombotic, and Antioxidant Properties of Amphiphilic Lipid Bioactives from Shrimp
by Alexandros Tsoupras, Paschalis Cholidis, Dimitrios Kranas, Evangelia Aikaterini Galouni, Anna Ofrydopoulou, Pavlos Efthymiopoulos, Katie Shiels, Sushanta Kumar Saha, George Z. Kyzas and Chryssa Anastasiadou
Pharmaceuticals 2025, 18(1), 25; https://doi.org/10.3390/ph18010025 (registering DOI) - 28 Dec 2024
Viewed by 287
Abstract
Background/Objectives: Marine organisms, including shrimps, have gained research interest due to containing an abundance of bioactive lipid molecules.This study evaluated the composition and the in vitro biological activities of amphiphilic bioactive compounds from four different wild shrimp species: Litopenaeus vannamei, Penaeus kerathurus [...] Read more.
Background/Objectives: Marine organisms, including shrimps, have gained research interest due to containing an abundance of bioactive lipid molecules.This study evaluated the composition and the in vitro biological activities of amphiphilic bioactive compounds from four different wild shrimp species: Litopenaeus vannamei, Penaeus kerathurus, Aristaeomorpha foliacea, and Parapenaeus longirostris. Methods: Total lipid (TL) extracts were obtained from shrimp and separated into total amphiphilic (TAC) and total lipophilic (TLC) compounds. Phenolic (TPC) and carotenoid (TCC) contents, antioxidant activities (DPPH, ABTS, FRAP assays), and biological effects on platelet-activating factor (PAF) and ADP-induced platelet activation were evaluated. Structural analyses were performed using ATR-FTIR spectroscopy, while LC-MS was used to elucidate the fatty acid composition and overall structure of polar lipids (PLs) present in shrimp TAC extracts. Results: TAC extracts, rich in phenolics, carotenoids, PL, and unsaturated fatty acids (UFAs), exhibited stronger anti-inflammatory and antithrombotic activities compared with TLC extracts, which showed potent antioxidant capacity. Significant amounts of UFAs, such as the monounsaturated fatty acid (MUFA) oleic acid (C18:1n9) and omega-3 (n3) polyunsaturated fatty acids (PUFAs) like eicosapentaenoic acid (EPA; C20:5n3) and docosahexaenoic acid (DHA; C22:6n3), were detected in the PLs of shrimp TAC extracts, with favorable anti-inflammatory values for their n6/n3 PUFA ratio. Shrimp amphiphilic bioactives present in the TAC extracts provide anti-inflammatory effects against the PAF pathway and antithrombotic effects against ADP and eicosanoid pathways. Conclusions: The overall findings support further study on the use of shrimp extracts rich in anti-inflammatory, anti-thrombotic, and antioxidant amphiphilic bioactives as ingredients to produce new bio-functional health-promoting products, in the context of sustainable development and circular economy. Full article
(This article belongs to the Section Natural Products)
Show Figures

Figure 1

Figure 1
<p>The anti-inflammatory potency of TAC and TLC extracts from all shrimp species, assessed against the PAF-induced thrombo-inflammatory pathway. Biological activity against human platelet aggregation induced via the inflammatory and thrombotic mediator PAF was assessed. Results are expressed as means of the IC<sub>50</sub> values (half-maximal inhibitory concentrations) in μg of TAC and TLC extract in the aggregometer cuvette that caused 50% inhibition of PAF-induced platelet aggregation in 250 μL of human PRP (the lower the IC<sub>50</sub> value for a lipid extract, the higher its inhibitory anti-inflammatory effect against PAF). * denotes a statistically significant difference, <span class="html-italic">p</span> &lt; 0.05, in the anti-PAF activity of TAC extract from a shrimp species compared to its TLC extract. TAC, total amphiphilic compound; TLC, total lipophilic compound; PAF, platelet activating factor.</p>
Full article ">Figure 2
<p>The antithrombotic (antiplatelet) potency of TAC and TLC extracts from all shrimp species assessed against platelet aggregation induced by the thrombotic ADP pathway. Biological activity against human platelet aggregation induced via the classic thrombotic platelet agonist, ADP, was assessed. Results are expressed as means of the IC<sub>50</sub> values (half-maximal inhibitory concentrations) in μg of TAC and TLC extract in the aggregometer cuvette that caused 50% inhibition of ADP-induced platelet aggregation in 250 μL of human PRP (the lower the IC<sub>50</sub> value for a lipid extract, the higher its inhibitory antithrombotic (antiplatelet) effect against ADP). * denotes a statistically significant difference, <span class="html-italic">p</span> &lt; 0.05, in anti-ADP activity of TAC extract from a shrimp species compared with its TLC extract. TAC, total amphiphilic compound; TLC, total lipophilic compound; ADP, adenosine 5′ diphosphate.</p>
Full article ">
18 pages, 4958 KiB  
Article
Scots Pine Bark Extracts as Co-Hardeners of Epoxy Resins
by Tomasz Szmechtyk
Molecules 2025, 30(1), 65; https://doi.org/10.3390/molecules30010065 (registering DOI) - 27 Dec 2024
Viewed by 168
Abstract
Extracts from natural waste like bark or leaves are great sources of phytochemicals, which contain functional groups (hydroxyl, carboxylic, vinyl, allyl) attractive in terms of polymer synthesis. In this study, the synthesis of epoxy with an extract of Scots pine bark as a [...] Read more.
Extracts from natural waste like bark or leaves are great sources of phytochemicals, which contain functional groups (hydroxyl, carboxylic, vinyl, allyl) attractive in terms of polymer synthesis. In this study, the synthesis of epoxy with an extract of Scots pine bark as a natural co-hardener was evaluated. Ultraviolet-visible (UV-Vis) spectroscopy was used for the identification of phytochemicals with conjugated dienes and quantification of TPC. Also, the total solid content (TSC) of representative extracts was calculated. The best extract in terms of total phenolic content (TPC) value was selected as a co-hardener and investigated using differential scanning calorimetry (DSC) for thermal effects and attenuated total reflectance Fourier transform infrared spectroscopy (ATR FTIR) for reactions between functional groups. Also, the mechanical properties (flexural modulus, flexural strength, impact strength, Shore D hardness) and density of composition were obtained for extract-based epoxy and compared to reference sample values. Results were discussed in terms of future research and improvement of compositions. Also, potential applications were proposed. Full article
Show Figures

Graphical abstract

Graphical abstract
Full article ">Figure 1
<p>UV-Vis spectra of selected eight representative extracts.</p>
Full article ">Figure 2
<p>DSC curves of REF and EXPINE samples—two cycles of curing from 35 °C to 300 °C.</p>
Full article ">Figure 3
<p>DSC curves of substrates—cycle from 35 °C to 300 °C.</p>
Full article ">Figure 4
<p>ATR FTIR spectra of BADGE epoxy cured with TFF and C120 extract—full range.</p>
Full article ">Figure 5
<p>ATR FTIR spectra of BADGE epoxy cured with TFF and C120 extract—range from 4000 to 2650 cm<sup>−1</sup>.</p>
Full article ">Figure 6
<p>ATR FTIR spectra of BADGE epoxy cured with TFF and C120 extract—range from 1640 to 1470 cm<sup>−1</sup>.</p>
Full article ">Figure 7
<p>ATR FTIR spectra of BADGE epoxy cured with TFF and C120 extract—range from 1370 to 620 cm<sup>−1</sup>.</p>
Full article ">Figure 8
<p>Charpy impact strength results.</p>
Full article ">Figure 9
<p>Shore D hardness results.</p>
Full article ">Figure 10
<p>Samples pieces—REF (at the bottom) and EXPINE (at the top).</p>
Full article ">
13 pages, 2914 KiB  
Article
Physiological Root Resorption of Deciduous Teeth: An ATR-FTIR Approach
by Giulia Orilisi, Alessia Cosi, Flavia Vitiello, Chiara Santoni, Valentina Notarstefano, Elisabetta Giorgini, Giovanna Orsini and Domenico Tripodi
J. Clin. Med. 2025, 14(1), 48; https://doi.org/10.3390/jcm14010048 - 26 Dec 2024
Viewed by 198
Abstract
Background: The study exploited, for the first time, Attenuated Total Reflectance-Fourier Transform-InfraRed (ATR-FTIR) spectroscopy on human dental pulps at different timings of root resorption (RR) to deepen the biological mechanisms occurring in deciduous teeth (De) during their replacement with permanent ones. Methods [...] Read more.
Background: The study exploited, for the first time, Attenuated Total Reflectance-Fourier Transform-InfraRed (ATR-FTIR) spectroscopy on human dental pulps at different timings of root resorption (RR) to deepen the biological mechanisms occurring in deciduous teeth (De) during their replacement with permanent ones. Methods: N:36 dental pulps from sound De were divided into the following: G0 (no RR); G1 (RR less than 1/3 of root length); G2 (RR not exceeding 2/3 of root length); and G3 (RR more than 2/3 of root length). Samples were analyzed by ATR-FTIR, and the spectral data were submitted to univariate (One-way ANOVA and Tukey’s multiple comparison tests; statistical significance set at p < 0.05) and multivariate (Principal Component Analysis, PCA) analyses. Results: PCA displayed good discrimination among groups, ascribable to: (i) the intensity of the peaks of nucleic acids (~1715 cm−1, ~1237 cm−1, ~964 cm−1, and ~815 cm−1) and carbohydrates (~1159 cm−1) which increased from G0 to G3 (p < 0.05); (ii) the relative amount of lipids which decreased from G0 to G3 (p < 0.05); and (iii) the intensity of the peaks at ~1014 cm−1, and ~875 cm−1 (phosphates and carbonates in hydroxyapatite), which decreased from G0 to G3 (p < 0.05). Conclusions: This study confirmed ATR-FTIR as a reliable and quick technique for the characterization of the dental pulp and highlighted a correlation between specific molecular changes in the dental pulp of deciduous teeth and different RR stages, shedding new light on this process and paving the way for future research, which could improve the clinical management of the primary dentition. Full article
(This article belongs to the Section Dentistry, Oral Surgery and Oral Medicine)
Show Figures

Figure 1

Figure 1
<p>Principal Component Analysis was performed on G0 (red circles), G1 (green circles), G2 (pink circles), and G3 (violet circles) spectral populations. PCA score plots are displayed both on (<b>A</b>) absorbance (Abs) and (<b>B</b>) second derivative (DII) spectra. (<b>A</b>) As regards spectra in Absorbance mode, a complete separation is observed between G0 and G3 samples (PC1 axis, explained variance 96.1%), while G1 and G2 are almost overlapping but segregated with respect both to G0 and G3 (PC2 axis, explained variance 2.8%). (<b>B</b>) As regards spectra in the Second Derivative mode, a complete separation is displayed among all groups; G0, G1, and G2 are segregated with respect to G3 (PC1 axis, explained variance 77.1%), while G0 and G1 are separated with respect to G2 and G3 (PC2 axis, explained variance 15.1%).</p>
Full article ">Figure 2
<p>The IR spectrum of a representative dental pulp collected from a sound deciduous tooth. The spectrum is shown in absorbance mode in the 3050–750 cm<sup>−1</sup> spectral interval. The position of the main absorption bands is reported, together with the corresponding organic and inorganic components (light blue, LIPIDS; green, PROTEINS; violet, NUCLEIC ACIDS; red, CARBOHYDRATES, and black, hydroxyapatite HA).</p>
Full article ">Figure 3
<p>Average IR spectra of dental pulps collected from deciduous teeth at different timing of root resorption: (<b>A</b>) G0; (<b>B</b>) G1; (<b>C</b>) G2, and (<b>D</b>) G3 experimental groups (red and blue arrows indicate the bands that arise or decrease in G3 respect to G0). IR spectra are shown in absorbance (Abs) and second derivative (DII) modes in the 1800–750 cm<sup>−1</sup> spectral interval. The position of the main absorption bands is reported below DII spectra. Red and blue arrows over peaks indicate the bands which change RR: red ones display an increase in absorbance, while blue ones a decrease.</p>
Full article ">Figure 4
<p>Statistical analysis of the spectral parameters related to the relative amount of nucleic acids: A<sub>1715</sub>, A<sub>1237</sub>, A<sub>964</sub>, and A<sub>815</sub>. Data are presented as mean ± S.D.; different letters indicate statistically significant differences among groups (one-way ANOVA and Tukey’s multiple comparison tests; <span class="html-italic">p</span> &lt; 0.05).</p>
Full article ">Figure 5
<p>Statistical analysis of the spectral parameter A<sub>1159</sub> related to the relative amount of carbohydrates. Data are presented as mean ± S.D.; different letters indicate statistically significant differences among groups (one-way ANOVA and Tukey’s multiple comparison tests; <span class="html-italic">p</span> &lt; 0.05).</p>
Full article ">Figure 6
<p>Statistical analysis of the spectral parameters related to the relative amount of hydroxyapatite: A<sub>1014</sub> (inorganic phosphates), and A<sub>875</sub> (inorganic carbonates). Data are presented as mean ± S.D.; different letters indicate statistically significant differences among groups (one-way ANOVA and Tukey’s multiple comparison tests; <span class="html-italic">p</span> &lt; 0.05).</p>
Full article ">Figure 7
<p>Statistical analysis of the spectral parameters related to the relative amount of lipids (A<sub>CH2</sub>), and proteins (A<sub>AI+II</sub>). Data are presented as mean ± S.D.; different letters indicate statistically significant differences among groups (one-way ANOVA and Tukey’s multiple comparison tests; <span class="html-italic">p</span> &lt; 0.05).</p>
Full article ">
14 pages, 1395 KiB  
Article
Combination ATR-FTIR with Multiple Classification Algorithms for Authentication of the Four Medicinal Plants from Curcuma L. in Rhizomes and Tuberous Roots
by Qiuyi Wen, Wenlong Wei, Yun Li, Dan Chen, Jianqing Zhang, Zhenwei Li and De-an Guo
Sensors 2025, 25(1), 50; https://doi.org/10.3390/s25010050 - 25 Dec 2024
Viewed by 265
Abstract
Curcumae Longae Rhizoma (CLRh), Curcumae Radix (CRa), and Curcumae Rhizoma (CRh), derived from the different medicinal parts of the Curcuma species, are blood-activating analgesics commonly used for promoting blood circulation and relieving pain. Due to their certain similarities in chemical composition and pharmacological [...] Read more.
Curcumae Longae Rhizoma (CLRh), Curcumae Radix (CRa), and Curcumae Rhizoma (CRh), derived from the different medicinal parts of the Curcuma species, are blood-activating analgesics commonly used for promoting blood circulation and relieving pain. Due to their certain similarities in chemical composition and pharmacological effects, these three herbs exhibit a high risk associated with mixing and indiscriminate use. The diverse methods used for distinguishing the medicinal origins are complex, time-consuming, and limited to intraspecific differentiation, which are not suitable for rapid and systematic identification. We developed a rapid analysis method for identification of affinis and different medicinal materials using attenuated total reflection-Fourier-transform infrared spectroscopy (ATR-FTIR) combined with machine learning algorithms. The original spectroscopic data were pretreated using derivatives, standard normal variate (SNV), multiplicative scatter correction (MSC), and smoothing (S) methods. Among them, 1D + MSC + 13S emerged as the best pretreatment method. Then, t-distributed stochastic neighbor embedding (t-SNE) was applied to visualize the results, and seven kinds of classification models were constructed. The results showed that support vector machine (SVM) modeling was superior to other models and the accuracy of validation and prediction was preferable, with a modeling time of 127.76 s. The established method could be employed to rapidly and effectively distinguish the different origins and parts of Curcuma species and thus provides a technique for rapid quality evaluation of affinis species. Full article
(This article belongs to the Section Chemical Sensors)
Show Figures

Figure 1

Figure 1
<p>Main producing areas of eight kinds of medicinal materials.</p>
Full article ">Figure 2
<p>The average spectra of rhizomes and tubers of <span class="html-italic">Curcuma</span> species.</p>
Full article ">Figure 3
<p>t-SNE visual analysis results of rhizomes and tubers of four <span class="html-italic">Curcuma</span> species, (<b>a</b>) raw spectra, (<b>b</b>) pre-processed spectra.</p>
Full article ">Figure 4
<p>The performances of SVM models based on 1D + MSC + 13S spectral data, (<b>a</b>) minimum classification error, (<b>b</b>) confusion matrices of testing set, (<b>c</b>) confusion matrices of training set.</p>
Full article ">
17 pages, 3033 KiB  
Article
Advanced Copper Oxide Chemical and Green Synthesis: Characterization and Antibacterial Evaluation
by Ecaterina Magdalena Modan, Adriana-Gabriela Schiopu, Sorin Georgian Moga, Denis Aurelian Negrea, Daniela Istrate, Ion Ciuca and Mihai Oproescu
Crystals 2025, 15(1), 7; https://doi.org/10.3390/cryst15010007 - 25 Dec 2024
Viewed by 294
Abstract
Recent advancements in nanotechnology have improved the application of copper oxide (CuO) nanostructures, known for their diverse antibacterial, electrical, catalytic, optical, and pharmacological properties, which depend on nanoparticle morphology. This study investigated two synthesis methods for structured CuO: microwave-assisted hydrolysis and ultrasound using [...] Read more.
Recent advancements in nanotechnology have improved the application of copper oxide (CuO) nanostructures, known for their diverse antibacterial, electrical, catalytic, optical, and pharmacological properties, which depend on nanoparticle morphology. This study investigated two synthesis methods for structured CuO: microwave-assisted hydrolysis and ultrasound using copper acetate and KOH, and an eco-friendly method involving cholesterol-free egg white albumin and Solanum lycopersicum extract. Characterization techniques, including XRD, FTIR, and SEM-EDS, were utilized to analyze the produced CuO. XRD confirmed high-purity monoclinic CuO structures in the sample obtained via the chemical method, while characteristic peaks of tenorite and dolerophanite were observed in the albumin-synthesized sample. ATR-FTIR analysis revealed O-H stretching bands around 3400 cm−1, indicating adsorbed H-OH or -OH and strong Cu-O bond peaks at 434 cm−1. The CuO synthesized via microwave and ultrasound methods displayed superior crystallinity compared to commercial CuO. SEM illustrated various morphologies, such as flakes, microspheres, and irregular polyhedra, influenced by the presence of proteins and organic acids. Antibacterial tests demonstrated the effective inhibition of Escherichia coli and Enterococcus faecalis, confirming the potential of CuO as a promising antibacterial agent. Overall, the findings highlight the effectiveness of green chemistry in developing crystalline CuO for various applications. Full article
(This article belongs to the Section Inorganic Crystalline Materials)
Show Figures

Figure 1

Figure 1
<p>Flow diagram for the hydrolytic synthesis of nanostructured copper oxide assisted by microwave and ultrasound.</p>
Full article ">Figure 2
<p>Flow diagram for the green synthesis of nanostructured copper.</p>
Full article ">Figure 3
<p>XRD pattern of nanostructured CuO prepared by microwave- and ultrasound-assisted hydrolytic synthesis, annealed at a temperature of 550 °C.</p>
Full article ">Figure 4
<p>XRD patterns of copper oxide elaborated by green synthesis from egg whites and extract of <span class="html-italic">Solanum lycopersicum</span>.</p>
Full article ">Figure 5
<p>ATR-FTIR spectra of CuO_ac_550_2h powder compared to commercial CuO.</p>
Full article ">Figure 6
<p>ATR-FTIR spectra ofcalcinated CuO_ofc_550/2h and CuO_b_550/2h compared to commercial CuO.</p>
Full article ">Figure 7
<p>(<b>a</b>) SEM micrographs of CuO calcined at 550 °C for 2 h and (<b>b</b>) EDS spectrum of CuO developed by microwave- and ultrasound-assisted hydrolytic synthesis.</p>
Full article ">Figure 8
<p>(<b>a</b>) SEM image of CuO prepared by green synthesis from cholesterol-free egg white; (<b>b</b>) EDS spectra of CuO prepared by green synthesis from cholesterol-free egg white; (<b>c</b>) SEM image of CuO prepared by green synthesis from <span class="html-italic">Solanum lycopersicum</span> extract; and (<b>d</b>) EDS spectra of CuO prepared by green synthesis from <span class="html-italic">Solanum lycopersicum</span> extract.</p>
Full article ">
24 pages, 5118 KiB  
Article
Development of a Novel Co-Amorphous Curcumin and L-Arginine (1:2): Structural Characterization, Biological Activity and Pharmacokinetics
by Jose Antonio Mancillas-Quiroz, Miriam del Carmen Carrasco-Portugal, Karina Mondragón-Vásquez, Juan Carlos Huerta-Cruz, Juan Rodríguez-Silverio, Leyanis Rodríguez-Vera, Juan Gerardo Reyes-García, Francisco Javier Flores-Murrieta, Jorge Guillermo Domínguez-Chávez and Héctor Isaac Rocha-González
Pharmaceutics 2025, 17(1), 11; https://doi.org/10.3390/pharmaceutics17010011 - 25 Dec 2024
Viewed by 350
Abstract
Background: Curcumin appears to be well tolerated and effective for managing chronic inflammatory pain, but its poor oral bioavailability has been a hurdle in its use as a therapeutic agent. The current study was performed to characterize a novel co-amorphous compound based on [...] Read more.
Background: Curcumin appears to be well tolerated and effective for managing chronic inflammatory pain, but its poor oral bioavailability has been a hurdle in its use as a therapeutic agent. The current study was performed to characterize a novel co-amorphous compound based on curcumin/L-arginine 1:2 (CAC12). Methods: Stability, solubility and structural characterization of the CAC12 were carried out by spectrometry techniques and in vitro assays, whereas the antinociceptive and anti-inflammatory effects were evaluated by CFA or carrageenan models. The mechanism of action was determined by cytokine quantification, and pharmacokinetic parameters were obtained through UPLC-MS/MS. The co-amorphous compound was prepared by fast solvent evaporation. Powder XRD, 13C-NMR, ATR-FTIR and TGA/DSC thermal analysis showed a 1:2 stoichiometry for the CAC12. Results: CAC12 was 1000 times more soluble than curcumin, and it was stable for 1 month at 40 °C and 75% relative humidity or for 60 min in physiological medium at pH 4.5–6.8. Co-amorphous curcumin/L-arginine, but not curcumin + L-arginine, decreased carrageenan- or CFA-induced inflammation and nociception by decreasing IL-1α, IL-1β, IL-6, TNF-α, MCP-1 and CXCL1 cytokines. The bioavailability of free plasmatic curcumin increased about 22.4 times when it was given as CAC12 relative to a phytosome formulation at the equivalent dose. Conclusions: Results suggest the possible use of CAC12 to treat inflammatory pain disorders in human beings. Full article
(This article belongs to the Section Physical Pharmacy and Formulation)
Show Figures

Figure 1

Figure 1
<p>Powder X-ray diffractograms obtained for CAC12, L-arginine and curcumin.</p>
Full article ">Figure 2
<p>Solid-state carbon-13 nuclear magnetic resonance (<sup>13</sup>C-NMR) spectra of curcumin, L-arginine and CAC12. (<b>A</b>) Proposed chemical structure of CAC12. (<b>B</b>) The main displacements and (<b>C</b>) typical <sup>13</sup>C-NMR spectra of CAC12, L-arginine and curcumin. Abbreviations: ws = wide signal, ss = small shoulder. As expected, the signals in the spectrum corresponding to the co-amorphous compound were observed to be broader and much less defined than those of the raw materials. In the CAC12 spectrum, we observed that the typical L-arginine signal at 54.8 ppm decreases to 49.0 ppm (Δδ = 5.8 ppm); likewise, the signal observed in the curcumin spectrum at 150.2 ppm, which is assigned to the hydroxyl-bonded aromatic carbons (C8 and C8′) shifts to 147.1 ppm (Δδ = 3.1 ppm) in the CAC12 spectrum.</p>
Full article ">Figure 3
<p>Attenuated total reflectance–Fourier transform infrared (ATR-FTIR) spectra for CAC12, L-arginine and curcumin.</p>
Full article ">Figure 4
<p>Differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA) of CAC12.</p>
Full article ">Figure 5
<p>X-ray powder diffractograms acquired from CAC12 stability studies. (<b>A</b>) Powder X-ray diffractograms of CAC12 obtained after 1 month of storage under several temperature and relative humidity (RH) conditions. (<b>B</b>) Powder X-ray diffractograms of CAC12 obtained after 12 h in distilled water, phosphate buffer (pH = 6.8), acetate buffer (pH = 4.5) or HCl solution (pH = 1.2).</p>
Full article ">Figure 6
<p>Lack of anti-inflammatory effect of oral curcumin and L-arginine in Freund’s complete adjuvant or carrageenan models. Time courses show the effects of increasing doses (100–320 mg/kg) of curcumin and L-arginine on inflammation induced by Freund’s complete adjuvant (<b>A</b>,<b>C</b>) or carrageenan (<b>E</b>,<b>G</b>). The bar graphs show a lack of anti-inflammatory effect of increasing doses of curcumin and L-arginine in Freund’s complete adjuvant (<b>B</b>,<b>D</b>) or carrageenan (<b>F</b>,<b>H</b>) models. Curcumin and L-arginine were orally administered at −1 h with respect to intra-articular injection of Freund’s complete adjuvant (100 µL, 0.1%) or subcutaneous administration of carrageenan (50 µL, 1%). Data are expressed as the mean ± S.E.M. of 6 animals per experimental group. There was no statistical difference based on one-way ANOVA. The area under the curve (AUC) was calculated from the time courses using the trapezoidal rule.</p>
Full article ">Figure 7
<p>Anti-inflammatory effects of oral CAC12 (1:2) in Freund’s complete adjuvant or carrageenan models. Time courses show the effects of increasing doses (10–100 mg/kg) of CAC12 on inflammation induced by Freund’s complete adjuvant (<b>A</b>) or carrageenan (<b>C</b>). The bar graphs show the anti-inflammatory effect produced by increasing doses of CAC12 in Freund’s complete adjuvant (<b>B</b>) or carrageenan (<b>D</b>) models. Curcumin and L-arginine were orally administered at −1 h with respect to intra-articular injection of Freund’s complete adjuvant (100 µL, 0.1%) or subcutaneous administration of carrageenan (50 µL, 1%). Data are expressed as the mean ± S.E.M. of 6 animals per experimental group. * Statistically different from the vehicle based on one-way ANOVA followed by Dunnett’s test with <span class="html-italic">p</span> &lt; 0.05. Statistical differences in time courses were omitted for the sake of clarity. The area under the curve (AUC) was calculated from the time courses using the trapezoidal rule.</p>
Full article ">Figure 8
<p>Effect of oral administration of 100 mg/kg of the crystalline mixture of curcumin (Cur, 51.4 mg) + L-arginine (Arg, 48.6 mg), diclofenac (Dic) and CAC12 (Co-amorph, 1:2) on inflammation induced by Freund’s complete adjuvant or carrageenan. The time courses show the anti-inflammatory effect produced by 100 mg/kg of diclofenac and CAC12 on the inflammation induced by Freund’s complete adjuvant (<b>A</b>) and carrageenan (<b>C</b>). The bar graphs indicate that 100 mg/kg of diclofenac and CAC12, but not the curcumin + L-arginine combination, have anti-inflammatory effects in Freund’s complete adjuvant (<b>B</b>) and carrageenan (<b>D</b>) models. Data are expressed as the mean ± S.E.M. of 6 animals per experimental group. * Statistically different from the vehicle group (Veh) based on one-way ANOVA followed by Tukey’s test with <span class="html-italic">p</span> &lt; 0.05. Statistical differences in time courses were omitted for the sake of clarity. The area under the curve (AUC) was calculated from the time courses using the trapezoidal rule.</p>
Full article ">Figure 9
<p>Effects of oral administration of 100 mg/kg of curcumin (Cur), L-arginine (Arg) and CAC12 (Co-amorph, 1:2) on nociception induced by Freund’s complete adjuvant or carrageenan. The time courses show the antinociceptive effect produced by 100 mg/kg of the CAC12 on the nociception induced by complete Freund’s adjuvant (<b>A</b>) and carrageenan (<b>C</b>). The bar graphs strongly suggest that 100 mg/kg of CAC12 exhibits an antinociceptive effect in Freund’s complete adjuvant (<b>B</b>) and carrageenan (<b>D</b>) models. Data are expressed as the mean ± S.E.M. of 6 animals per experimental group. * Statistically different with respect to the vehicle (Veh) group or ** CAC12 group based on one-way ANOVA followed by Tukey’s test with <span class="html-italic">p</span> &lt; 0.05. Statistical differences in time courses were omitted for the sake of clarity. The area under the curve (AUC) was calculated from the time courses using the trapezoidal rule.</p>
Full article ">Figure 10
<p>Effect of oral administration of CAC12 (1:2) on the levels of interleukin 1 alpha (IL-1α), interleukin 1 beta (IL-1β), interleukin 6 (IL-6), tumor necrosis factor-alpha (TNF-α), monocyte chemoattractant protein 1 (MCP-1) and CXC motif chemokine ligand 1 (CXCL1), induced by Freund’s complete adjuvant (<b>A</b>) or carrageenan (<b>B</b>). The bar graphs indicate that 100 mg/kg of CAC12 is able to prevent the increase in tissue concentrations of IL-1α, IL-1β, IL-6, TNF-α, MCP-1 and CXCL1 in Freund’s complete adjuvant (<b>A</b>) and carrageenan (<b>B</b>) models of inflammation for 8 h. Data are expressed as the mean ± S.E.M. of 3–4 animals per experimental group. * Statistically different from the vehicle group and ** statistically different from the carrageenan or CFA groups based on Newman–Keuls’ test with <span class="html-italic">p</span> &lt; 0.05. The area under the curve (AUC) was calculated from time courses (from 0 to 8 h) using the trapezoidal rule.</p>
Full article ">Figure 11
<p>Pharmacokinetic profile of oral administration of the reference compound (curcumin phytosome, Mericart<sup>®</sup>) and the test compound (CAC12, CurQsen<sup>®</sup>). The data are expressed as the mean of the plasmatic-free curcumin of 18 healthy subjects.</p>
Full article ">
14 pages, 3113 KiB  
Article
Assessment of the Presence of Microplastics in Stabilized Sewage Sludge: Analysis Methods and Environmental Impact
by Jagoda Worek, Kamil Kawoń, Joanna Chwiej, Katarzyna Berent, Rosa Rego and Katarzyna Styszko
Appl. Sci. 2025, 15(1), 1; https://doi.org/10.3390/app15010001 - 24 Dec 2024
Viewed by 369
Abstract
Wastewater treatment processes can fragment microplastics (MPs), which may subsequently enter fertilizers applied in agricultural settings. This study aimed to quantify the occurrence of MPs in stabilized sewage sludge intended for fertilizer production. Matrix elimination was performed using an oxidative method to isolate [...] Read more.
Wastewater treatment processes can fragment microplastics (MPs), which may subsequently enter fertilizers applied in agricultural settings. This study aimed to quantify the occurrence of MPs in stabilized sewage sludge intended for fertilizer production. Matrix elimination was performed using an oxidative method to isolate MPs, followed by MPs separation with a saturated salt solution of appropriate density to enhance the accuracy of identification. The resulting samples were analyzed using spectroscopic and microscopic techniques to provide the detailed characterization of MPs content. The highest concentrations of MPs were recorded during the months of June, July, and May, with average values of 2942, 2341, and 1746 fragments per 100 g of dry weight, respectively. The analysis revealed that fragments were the dominant morphological form, and low-density polyethylene was the most common polymer type detected. These findings underscore a significant risk of MPs re-emission into the environment through the agricultural application of fertilizers derived from sewage sludge. Such practices may lead to the introduction of between 6110 and 13,889 MPs per square meter of soil, depending on the application rates, thereby posing potential risks to soil health and the broader ecosystem. This study highlights the importance of monitoring MPs content in fertilizers derived from wastewater treatment by-products. Full article
(This article belongs to the Section Environmental Sciences)
Show Figures

Figure 1

Figure 1
<p>Primary and secondary sources of MPs.</p>
Full article ">Figure 2
<p>FTIR microscope imaging of MPs extracted from stabilized sewage sludge (<b>A</b>–<b>D</b>).</p>
Full article ">Figure 3
<p>Confocal microscopy imaging of MPs separated from stabilized sewage sludge (<b>A</b>–<b>C</b>).</p>
Full article ">Figure 4
<p>Number of MPs separated from stabilized sewage samples according to month.</p>
Full article ">Figure 5
<p>The amount of MPs divided into black and colored fragments and fibers, depending on the month.</p>
Full article ">Figure 6
<p>The size in µm of the separated MPs, depending on the month.</p>
Full article ">Figure 7
<p>FTIR spectra of LDPE separated from stabilized sewage sludge.</p>
Full article ">Figure 8
<p>SEM imaging of different structure of microplastics ((<b>A</b>)—flat surface; (<b>B</b>)—porous surface).</p>
Full article ">
13 pages, 3352 KiB  
Article
The Addition of MoO3 or SiO2 Nano-/Microfillers Thermally Stabilized and Mechanically Reinforce the PVDF-HFP/PVP Polymer Composite Thin Films
by Urška Gradišar Centa, Anja Pogačnik Krajnc, Lidija Slemenik Perše, Matic Šobak and Mohor Mihelčič
Coatings 2024, 14(12), 1603; https://doi.org/10.3390/coatings14121603 - 21 Dec 2024
Viewed by 356
Abstract
The properties of thin polymer films are influenced by the size of the fillers, their morphology, the surface properties and their distribution/interaction in the polymer matrix. In this work, thin polymer composite films with MoO3 or SiO2 nano and micro fillers [...] Read more.
The properties of thin polymer films are influenced by the size of the fillers, their morphology, the surface properties and their distribution/interaction in the polymer matrix. In this work, thin polymer composite films with MoO3 or SiO2 nano and micro fillers in PVDF-HFP/PVP polymer matrix were successfully fabricated using the solvent casting method. The effects of different types, sizes and morphologies of the inorganic fillers on the crystallization of the PVDF-HFP polymer were investigated, as well as the effects on the thermal and mechanical properties of the composites. Scanning electron microscopy, ATR-FTIR spectroscopy, differential scanning calorimetry, nanoindentation and uniaxial mechanical tests were used for characterization. The results showed that MoO3 nanowires thermally stabilized the polymer matrix, induced crystallization of the PVDF-HFP polymer in all three polymorphs (α-, β-, γ-phase) and formed a geometrical network in the polymer matrix, resulting in the highest elastic moduli, hardness and Young’s modulus. Full article
Show Figures

Figure 1

Figure 1
<p>Samples of (<b>A</b>) polymer matrix and polymer composites: with (<b>B</b>) MoO<sub>3</sub> nanowires, (<b>C</b>) MoO<sub>3</sub> microparticles, (<b>D</b>) SiO<sub>2</sub> nanoparticles, (<b>E</b>) SiO<sub>2</sub> microparticles for characterization.</p>
Full article ">Figure 2
<p>SEM images of nano- and micro-particles used: (<b>a</b>) MoO<sub>3</sub> nanowires, (<b>b</b>) MoO<sub>3</sub> microparticles, (<b>c</b>) SiO<sub>2</sub> nanoparticles, (<b>d</b>) SiO<sub>2</sub> microparticles.</p>
Full article ">Figure 3
<p>SEM images of the surface of (<b>a</b>) PVDF-HFP/PVP polymer matrix and polymer composite thin films and with the addition of: (<b>b</b>) MoO<sub>3</sub> nanowires, (<b>c</b>) MoO<sub>3</sub> microparticles, (<b>d</b>) SiO<sub>2</sub> nanoparticles, (<b>e</b>) SiO<sub>2</sub> microparticles. The enlargement of the polymer domains is shown in the insert.</p>
Full article ">Figure 4
<p>ATR-FTIR curves for PVDF-HFP/PVP polymer matrix and polymer composites with MoO<sub>3</sub> nanowires, MoO<sub>3</sub> microparticles, SiO<sub>2</sub> nanoparticles, SiO<sub>2</sub> microparticles.</p>
Full article ">Figure 5
<p>DSC curves for polymer composites: (<b>a</b>) second heating step, (<b>b</b>) cooling step.</p>
Full article ">Figure 6
<p>Nanoindentation: (<b>a</b>) elastic modulus and (<b>b</b>) hardness of PVDF-HFP/PVP polymer blend and polymer composites with MoO<sub>3</sub> and SiO<sub>2</sub> nano- and micro-particles.</p>
Full article ">Figure 7
<p>Mechanical properties of the polymer nanocomposites samples obtained with uniaxial mechanical tests. (<b>a</b>) Stress-strain curves, (<b>b</b>) values of Young’s modulus for PVDF-HFP/PVP polymer blend and polymer composites with MoO<sub>3</sub> and SiO<sub>2</sub> nano- and micro-particles.</p>
Full article ">
18 pages, 2661 KiB  
Article
High-Energy-Density Hydrochar and Bio-Oil from Hydrothermal Processing of Spent Coffee Grounds—Experimental Investigation
by Mariusz Wądrzyk, Jakub Katerla, Rafał Janus, Marek Lewandowski, Marek Plata and Łukasz Korzeniowski
Energies 2024, 17(24), 6446; https://doi.org/10.3390/en17246446 - 21 Dec 2024
Viewed by 338
Abstract
Spent coffee grounds (SCGs), a by-product of coffee brewing, have high application potential. However, their high moisture content complicates conventional conversion without energy-intensive drying. This study explores a new route to convert SCGs to high-carbon bioproducts, such as hydrochar and bio-oil, through hydrothermal [...] Read more.
Spent coffee grounds (SCGs), a by-product of coffee brewing, have high application potential. However, their high moisture content complicates conventional conversion without energy-intensive drying. This study explores a new route to convert SCGs to high-carbon bioproducts, such as hydrochar and bio-oil, through hydrothermal processing. The effect of the processing variables, i.e., temperature, residence time, and the application of the binary solvent as a reaction medium, on the distribution of the resultant bioproducts was investigated. The quality of the fabricated bioproducts was analyzed by means of instrumental techniques such as EA, ATR-FTIR, GC-MS, and GC-TCD-FID. Two dominant fractions were liquid bio-oil and solid hydrochar. The highest char yield (39 wt.%) was observed under milder conditions (low T and short residence times), while more severe conditions led to an increase in bio-oil formation, which reached a maximum of 46 wt.%. The resulting bio-oils were of similar quality, presenting high carbon content (71–74 wt.%) and energetic values (approximately 35 MJ/kg). Also, hydrochars showed a noticeable energy densification compared to raw materials, where the C content and HHV reached up to 73.8 wt.% and 30 MJ/kg, respectively. The addition of co-solvent to water improves the bio-oil yield as a result of the enhanced stabilization of reactive intermediates. Full article
Show Figures

Figure 1

Figure 1
<p>Effect of processing temperature ranging between 260 and 320 °C on the distribution of HTL bioproducts yields (residence time of 30 min and water as solvent).</p>
Full article ">Figure 2
<p>Effect of residence time ranging between 30 and 60 min on the distribution of HTL bioproducts yields (processing temperatures at 280 and 300 °C, and water as solvent).</p>
Full article ">Figure 3
<p>Yields of liquefaction products for water and water–isopropanol as reaction media (processing temperature: 320 °C; residence time: 30 min).</p>
Full article ">Figure 4
<p>Comprehensive van Krevelen diagram for the studied bio-oils and hydrochars obtained at different processing conditions, i.e., processing temperature between 260 and 320 °C and single (water) and binary solvent system (water–isopropanol) (<b>A</b>) together with energy recovery in the form of bio-oil as a target group of products (<b>B</b>).</p>
Full article ">Figure 5
<p>FT-IR spectra of coffee spent grounds and bio-oils obtained by its liquefaction using single—(water) and binary solvent system (water–isopropanol) (processing temperature: 320 °C, residence time: 30 min).</p>
Full article ">Figure 6
<p>Group composition of the bio-oils obtained through thermochemical liquefaction using single—(water) and binary solvent system (water–isopropanol) (processing temperature: 320 °C, residence time: 30 min) (based on GC-MS analysis).</p>
Full article ">
27 pages, 2279 KiB  
Article
Titanium(IV), Zirconium(IV), and Cerium(IV) Phosphates Synthesized Under Mild Conditions—Composition Characteristics and Evaluation of Sorption Properties Towards Copper Ions in Comparison to Commercially Available Ion-Exchange Resins
by Marta Marszałek, Marcin Piotrowski, Barbara Dziełak, Mariola Blicharz, Wiktoria Malarska and Zbigniew Wzorek
Materials 2024, 17(24), 6226; https://doi.org/10.3390/ma17246226 - 20 Dec 2024
Viewed by 519
Abstract
The removal of copper from wastewater of mine origin requires the use of an appropriate method. Sorption methods are considered to be one of the best solutions for removing copper from industrial wastewater at low levels. Metal(IV) phosphates have been reported as excellent [...] Read more.
The removal of copper from wastewater of mine origin requires the use of an appropriate method. Sorption methods are considered to be one of the best solutions for removing copper from industrial wastewater at low levels. Metal(IV) phosphates have been reported as excellent sorption materials that can be highly selective for copper. Therefore, the aim of this research was to synthesize titanium(IV), zirconium(IV), and cerium(IV) phosphates with a wide range of P:Metal(IV) molar ratios (0.5–10) in the reaction mixture and under mild conditions, using a simple scalable approach which requires minimal financial outlays. The obtained materials were characterized using XRD, ATR-FTIR, SEM-EDS techniques, and pH titration. To evaluate the performance of the resulting materials, their sorption properties towards copper ions were examined in comparison with selected commercially available ion-exchange resins. In each group of metal(IV) phosphates, the best material has a high ion-exchange capacity: 16.9 meq/g for titanium sorbent, 8.8 meq/g for zirconium sorbent, and 7.0 meq/g for cerium sorbent. Zirconium phosphate synthesized at a P:Zr molar ratio in the reaction mixture of 10:1 exhibits the best sorption properties towards copper ions in a solution similar to mining wastewater (acidic, saline, and containing heavy metals), better than some commercial ion-exchange resins. Full article
Show Figures

Figure 1

Figure 1
<p>XRD patterns of: (<b>a</b>) titanium(IV) phosphate sorbents; (<b>b</b>) zirconium(IV) phosphate sorbents; and (<b>c</b>) cerium(IV) phosphate sorbents.</p>
Full article ">Figure 2
<p>Titration curves of: (<b>a</b>) titanium(IV) phosphate sorbents; (<b>b</b>) zirconium(IV) phosphate sorbents; and (<b>c</b>) cerium(IV) phosphate sorbents.</p>
Full article ">Figure 3
<p>ATR-FTIR spectra of: (<b>a</b>) titanium(IV) phosphate sorbents; (<b>b</b>) zirconium(IV) phosphate sorbents; and (<b>c</b>) cerium(IV) phosphate sorbents.</p>
Full article ">Figure 4
<p>The sorption isotherms for: (<b>a</b>) titanium(IV) phosphate sorbents; (<b>b</b>) zirconium(IV) phosphate sorbents; and (<b>c</b>) cerium(IV) phosphate sorbents. The best-fitted Langmuir model is marked with a solid line, while the Freundlich model is marked with a dotted line.</p>
Full article ">Figure 5
<p>Correlation between: (<b>a</b>) <span class="html-italic">q<sub>m</sub></span> and P:Metal(IV) molar ratio in the reaction mixture; (<b>b</b>) <span class="html-italic">K<sub>L</sub></span> and P:Metal(IV) molar ratio in the reaction mixture.</p>
Full article ">
19 pages, 4522 KiB  
Article
Study of Water Resistance of Polyurethane Coatings Based on Microanalytical Methods
by Chao Xie, Yufeng Shi, Zhuozhuo Si, Ping Wu, Binqiang Sun and Wenzhe Ma
Polymers 2024, 16(24), 3529; https://doi.org/10.3390/polym16243529 - 18 Dec 2024
Viewed by 345
Abstract
This study investigates the effect of microstructural changes in polyurethane coatings on their water resistance properties. Polyurethane coatings with varying diluent contents were prepared and tested for water penetration resistance and mechanical property retention. The time-dependent behavior of water within the coatings at [...] Read more.
This study investigates the effect of microstructural changes in polyurethane coatings on their water resistance properties. Polyurethane coatings with varying diluent contents were prepared and tested for water penetration resistance and mechanical property retention. The time-dependent behavior of water within the coatings at different immersion durations was analyzed using low-field nuclear magnetic resonance (NMR). Furthermore, the free volume and characteristic molecular groups of each coating were analyzed using microscopic techniques, including positron annihilation lifetime spectroscopy (PALS) and attenuated total reflectance Fourier-transform infrared spectroscopy (ATR−FTIR). Results indicate that diluent content significantly alters the microstructure of the coatings. With increasing diluent content, both the average pore volume and free volume fraction initially decrease and then increase, while characteristic molecular groups, including hydrophilic groups, gradually decline. The water resistance performance of the coatings was significantly influenced by the combined effects of free volume and characteristic molecular groups. Among the five tested coating formulations, coatings with diluent contents of 20% and 25% showed a superior water penetration resistance, higher retention of mechanical properties after immersion, and relatively low total content of bound and free water at all immersion ages. The entropy weight method and the equal weight method were used to assess the overall water resistance, with the following ranking of scores: f20 > f25 > f30 > f15 > f10. This study offers theoretical support to guide the design and practical application of polyurethane coatings in real-world engineering projects. Full article
Show Figures

Graphical abstract

Graphical abstract
Full article ">Figure 1
<p>Electric flux test results.</p>
Full article ">Figure 2
<p>Saturated water absorption of the coating.</p>
Full article ">Figure 3
<p>Tensile strength retention of the coating.</p>
Full article ">Figure 4
<p>Retention ration of tensile properties of the coating.</p>
Full article ">Figure 5
<p><span class="html-italic">T</span><sub>2</sub> test results of each coating group at different soaking ages.</p>
Full article ">Figure 6
<p>Moisture content of each coated sample at different <span class="html-italic">T</span><sub>2</sub> time intervals for different immersion ages.</p>
Full article ">Figure 7
<p>The <span class="html-italic">o</span>-Ps annihilation lifetime of each sample.</p>
Full article ">Figure 8
<p>The average free volume radius and content of each sample.</p>
Full article ">Figure 9
<p>ATR−FTIR test results for each group of specimens.</p>
Full article ">Figure 10
<p>Characteristic peak areas of characteristic molecular groups for each group of samples.</p>
Full article ">Figure 11
<p>Curing reaction process of polyurethane coating: (<b>a</b>) -NCO reacts with H<sub>2</sub>O to form a binary or polyamine, (<b>b</b>) the amine reacts with unreacted –NCO in a chain expansion reaction.</p>
Full article ">Figure 12
<p>The apparent morphology of each group of coatings before and after water resistance deterioration.</p>
Full article ">Figure 13
<p>Comprehensive scores for each sample of the entropy weight method and equal weight method.</p>
Full article ">
16 pages, 4329 KiB  
Article
Porphyrin-Based Aluminum Metal-Organic Framework with Copper: Pre-Adsorption of Water Vapor, Dynamic and Static Sorption of Diethyl Sulfide Vapor, and Sorbent Regeneration
by Mohammad Shahwaz Ahmad and Alexander Samokhvalov
Materials 2024, 17(24), 6160; https://doi.org/10.3390/ma17246160 - 17 Dec 2024
Viewed by 321
Abstract
Metal–organic frameworks (MOFs) are hybrid inorganic–organic 3D coordination polymers with metal sites and organic linkers, which are a “hot” topic in the research of sorption, separations, catalysis, sensing, and environmental remediation. In this study, we explore the molecular mechanism and kinetics of interaction [...] Read more.
Metal–organic frameworks (MOFs) are hybrid inorganic–organic 3D coordination polymers with metal sites and organic linkers, which are a “hot” topic in the research of sorption, separations, catalysis, sensing, and environmental remediation. In this study, we explore the molecular mechanism and kinetics of interaction of the new copper porphyrin aluminum metal–organic framework (actAl-MOF-TCPPCu) compound 4 with a vapor of the volatile organic sulfur compound (VOSC) diethyl sulfide (DES). First, compound 4 was synthesized by post-synthetic modification (PSM) of Al-MOF-TCPPH2 compound 2 by inserting Cu2+ ions into the porphyrin ring and characterized by complementary qualitative and quantitative chemical, structural, and spectroscopic analysis. Second, the interaction of compound 4 with DES vapor was analyzed dynamically by the novel method of in situ time-dependent attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy at controlled humidity levels. The sorbent–adsorbate interactions, as analyzed by the shifts in IR peaks, indicate that the bonding includes the hydroxy O-H, carboxylate COO, and phenyl groups. The kinetics of sorption obeys the Langmuir pseudo-first-order rate law. The pre-adsorption of water vapor by compound 4 at the controlled relative humidity under static (equilibrium) conditions yields the binary stoichiometric adsorption complex (Al-MOF-TCPPCu)1.0(H2O)8.0. The pre-adsorption of water vapor makes the subsequent sorption of DES slower, while the kinetics obey the same rate law. Then, static pre-adsorption of water vapor was followed by static sorption of DES vapor, and the ternary adsorption complex (Al-MOF-TCPPCu)1.0(H2O)8.0(DES)3.8 was obtained. Despite the pre-adsorption of significant amounts of water, the binary complex adsorbs a large amount of DES: ca. 36.6 wt. % (per compound 4). Finally, the ternary complex is facilely regenerated by gentle heating under vacuum. Compound 4 and related MOFs are promising for adsorptive removal of vapor of DES and related VOSCs from dry and humid air. Full article
(This article belongs to the Special Issue Adsorbents and Their Applications (Second Volume))
Show Figures

Graphical abstract

Graphical abstract
Full article ">Figure 1
<p>Diethyl sulfide and its presence in nature, technology, and the environment.</p>
Full article ">Figure 2
<p>The 2D molecular structure of the structural unit of copper-containing porphyrin aluminum MOF, compound <b>4</b> actAl-MOF-TCPPCu.</p>
Full article ">Figure 3
<p>Powder XRD patterns of activated compounds: (<b>a</b>) compound <b>2</b> actAl-MOF-TCPPH<sub>2</sub>; (<b>b</b>) the target compound <b>4</b> actAl-MOF-TCPPCu.</p>
Full article ">Figure 4
<p>The starting in situ time-dependent ATR-FTIR spectra of compound 4 in the flow of DES vapor. (<b>a</b>) High wavenumbers; (<b>b</b>) mid-IR; (<b>c</b>) low wavenumbers.</p>
Full article ">Figure 5
<p>The proposed model of bonding DES molecules to compound <b>4</b>.</p>
Full article ">Figure 6
<p>Kinetics of in situ sorption of DES vapor by the activated compound <b>4</b>. (<b>a</b>) Integration of IR peak due to the asymmetric CH<sub>2</sub> stretching at 2965 cm<sup>−1</sup>; (<b>b</b>) kinetic analysis of the integrated peak.</p>
Full article ">Figure 7
<p>The in situ time-dependent ATR-FTIR spectra of the binary adsorption complex hydAl-MOF-TCPPCu in the flow of DES vapor. (<b>a</b>) High wavenumber range; (<b>b</b>) mid-IR range; (<b>c</b>) low wavenumber range.</p>
Full article ">Figure 8
<p>Kinetics of in situ sorption of DES vapor by compound <b>4hyd</b>. (<b>a</b>) Integrated IR peak of asymmetric CH<sub>2</sub> stretching; (<b>b</b>) formal kinetic analysis of peak area in time.</p>
Full article ">Figure 9
<p>Powder XRD patterns of sorbent compound 4 and its adsorption complexes. (<b>a</b>) actAl-MOF-TCPPCu and hydAl-MOF-TCPPCu (binary adsorption complex). (<b>b</b>) hydAl-MOF-TCPPCu and DES-hydAl-MOF-TCPPCu (ternary adsorption complex). (<b>c</b>) actAl-MOF-TCPPCu and regAl-MOF-TCPPCu (regenerated ternary adsorption complex).</p>
Full article ">
Back to TopTop