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Search Results (2,037)

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16 pages, 3332 KiB  
Review
Complex Diagnostic Challenges in Glioblastoma: The Role of 18F-FDOPA PET Imaging
by David Sipos, Zsanett Debreczeni-Máté, Zsombor Ritter, Omar Freihat, Mihály Simon and Árpád Kovács
Pharmaceuticals 2024, 17(9), 1215; https://doi.org/10.3390/ph17091215 (registering DOI) - 15 Sep 2024
Viewed by 70
Abstract
Glioblastoma multiforme (GBM) remains one of the most aggressive and lethal forms of brain cancer, characterized by rapid proliferation and diffuse infiltration into the surrounding brain tissues. Despite advancements in therapeutic approaches, the prognosis for GBM patients is poor, with median survival times [...] Read more.
Glioblastoma multiforme (GBM) remains one of the most aggressive and lethal forms of brain cancer, characterized by rapid proliferation and diffuse infiltration into the surrounding brain tissues. Despite advancements in therapeutic approaches, the prognosis for GBM patients is poor, with median survival times rarely exceeding 15 months post-diagnosis. An accurate diagnosis, treatment planning, and monitoring are crucial for improving patient outcomes. Core imaging modalities such as Computed Tomography (CT) and Magnetic Resonance Imaging (MRI) are indispensable in the initial diagnosis and ongoing management of GBM. Histopathology remains the gold standard for definitive diagnoses, guiding treatment by providing molecular and genetic insights into the tumor. Advanced imaging modalities, particularly positron emission tomography (PET), play a pivotal role in the management of GBM. Among these, 3,4-dihydroxy-6-[18F]-fluoro-L-phenylalanine (18F-FDOPA) PET has emerged as a powerful tool due to its superior specificity and sensitivity in detecting GBM and monitoring treatment responses. This introduction provides a comprehensive overview of the multifaceted role of 18F-FDOPA PET in GBM, covering its diagnostic accuracy, potential as a biomarker, integration into clinical workflows, impact on patient outcomes, technological and methodological advancements, comparative effectiveness with other PET tracers, and its cost-effectiveness in clinical practice. Through these perspectives, we aim to underscore the significant contributions of 18F-FDOPA PET to the evolving landscape of GBM management and its potential to enhance both clinical and economic outcomes for patients afflicted with this formidable disease. Full article
(This article belongs to the Section Radiopharmaceutical Sciences)
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<p>The chemical structure of <sup>18</sup>F-FDOPA.</p>
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<p>Left frontal post craniotomy status. Inhomogeneous, mainly centrally, moderate enhancement of contrast material is observed on T1-weighted post-contrast MRI images. The lesion in the left hemisphere is surrounded by edema (<b>C</b>,<b>D</b>). Irregularly shaped intense, focal <sup>18</sup>F-FDOPA accumulation can be detected on the left side of the brain frontally, above the level of lateral ventricles (<b>A</b>,<b>B</b>). Pink line—GTV, green line—BTV 1.7 (<b>A</b>,<b>C</b>), green line—BTV 2.0 (<b>B</b>,<b>D</b>), red line—PTV, and yellow line—recurrence [<a href="#B42-pharmaceuticals-17-01215" class="html-bibr">42</a>].</p>
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13 pages, 2594 KiB  
Article
Evaluation of an Enzyme-Linked Magnetic Electrochemical Assay for Hepatitis a Virus Detection in Drinking and Vegetable Processing Water
by Cristine D’Agostino, Rocco Cancelliere, Antonio Ceccarelli, Danila Moscone, Loredana Cozzi, Giuseppina La Rosa, Elisabetta Suffredini and Laura Micheli
Chemosensors 2024, 12(9), 188; https://doi.org/10.3390/chemosensors12090188 (registering DOI) - 14 Sep 2024
Viewed by 266
Abstract
Globally, waterborne viral infections significantly threaten public health. While current European Union regulations stipulate that drinking water must be devoid of harmful pathogens, they do not specifically address the presence of enteric viruses in water used for irrigation or food production. Traditional virus [...] Read more.
Globally, waterborne viral infections significantly threaten public health. While current European Union regulations stipulate that drinking water must be devoid of harmful pathogens, they do not specifically address the presence of enteric viruses in water used for irrigation or food production. Traditional virus detection methods rely on molecular biology assays, requiring specialized personnel and laboratory facilities. Here, we describe an electrochemical sandwich enzyme-linked immunomagnetic assay (ELIME) for the detection of the hepatitis A virus (HAV) in water matrices. This method employed screen-printed electrodes as the sensing platform and utilized commercially available pre-activated magnetic beads to provide a robust foundation for the immunological reaction. The ELIME assay demonstrated exceptional analytical performance in only 185 min achieving a detection limit of 0.5 genomic copies per milliliter (g.c./mL) and exhibiting good reproducibility with a relative standard deviation (RSD) of 7% in HAV-spiked drinking and processing water samples. Compared with the real-time RT-qPCR method described in ISO 15216-1, the ELIME assay demonstrated higher sensitivity, although the overall linearity of the method was moderate. These analytical attributes highlight the potential of the ELIME assay as a rapid and viable alternative for HAV detection in water used for agriculture and food processing. Full article
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<p>Protocol used in the ELIME detection.</p>
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<p>Extraction method for HAV from drinking water and water for vegetable processing.</p>
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<p>General schematic of ELIME functioning. (<b>a</b>) Immobilization of Goat Anti-Mouse IgG magnetic nanoparticles (MN-MAb1) on SPE, (<b>b</b>) antigen–antibody interaction, (<b>c</b>) immunocomplex detection using Mab-AP, and (<b>d</b>) electrochemical detection using DPV.</p>
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<p>Mab1 optimization. (<b>a</b>) The effect of the MAbI concentration on the signal. Protocol: 3% dry milk (DM); [MAbI] 0, 5, 10, and 15 μg/mL; [HAV] 10<sup>−8</sup> UI/mL; [MAb-AP] 1:10,000 (<span class="html-italic">v</span>/<span class="html-italic">v</span>) in PBS; and 5 mg/mL 1-NPP; in red circle the selected concentration is underlined. (<b>b</b>) The DPV measurement potential range 0–600 mV, the pulse width of 50 ms, pulse amplitude of 70 mV, and a scan rate of 100 mV/s.</p>
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<p>Study of the blocking reagent at different concentrations of MAb-AP. Three percent BSA, 3% DM, and 1% PVA; [MAb-AP] 1:5000, 1:10,000, and 1:25,000 (<span class="html-italic">v</span>/<span class="html-italic">v</span>) in PBS; 5 mg/mL 1-NPP; DPV measurement potential range 0–600 mV; pulse width of 50 ms; pulse amplitude of 70 mV; and scan rate of 100 mV/s.</p>
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<p>Electrochemical LbL-EC of ELIME assembly. (<b>a</b>) cv voltammograms and (<b>b</b>) EIS spectra. At least three experiments for each curve were conducted.</p>
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<p>Calibration curve for HAV. [MAb<sub>I</sub>] 10 μg/mL, 3% BSA, [HAV] 0–10 g.c./mL, [MAb-AP] 1:25,000 (<span class="html-italic">v</span>/<span class="html-italic">v</span>), and 5 mg/mL 1-NPP. DPV measurement potential range 0–600 mV, pulse width of 50 ms, pulse amplitude of 70 mV, and a scan rate of 100 mV/s. (<b>a</b>) 4-parameter logistic calibration curv. Parameters: <span class="html-italic">a</span> = 96.53, <span class="html-italic">b</span> = −3.03, <span class="html-italic">x</span><sub>0</sub> = 0.89, <span class="html-italic">y</span><sub>0</sub> = −0.18. LOD = 0.5 g.c./mL, RSD% 7%. (<b>b</b>) DPV measures used for the calibration curve.</p>
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14 pages, 1182 KiB  
Article
Synthesis and Evaluation of 99mTc(CO)3 Complexes with Ciprofloxacin Dithiocarbamate for Infection Imaging
by Afroditi Papasavva, Nektarios N. Pirmettis, Antonio Shegani, Eleni Papadopoulou, Christos Kiritsis, Maria Georgoutsou-Spyridonos, Dimitrios C. Mastellos, Aristeidis Chiotellis, Patricia Kyprianidou, Maria Pelecanou, Minas Papadopoulos and Ioannis Pirmettis
Pharmaceutics 2024, 16(9), 1210; https://doi.org/10.3390/pharmaceutics16091210 (registering DOI) - 14 Sep 2024
Viewed by 155
Abstract
Background: The accurate diagnosis of bacterial infections remains a critical challenge in clinical practice. Traditional imaging modalities like computed tomography (CT) and magnetic resonance imaging (MRI) often fail to distinguish bacterial infections from sterile inflammation. Nuclear medicine, such as technetium-99m (99mTc) [...] Read more.
Background: The accurate diagnosis of bacterial infections remains a critical challenge in clinical practice. Traditional imaging modalities like computed tomography (CT) and magnetic resonance imaging (MRI) often fail to distinguish bacterial infections from sterile inflammation. Nuclear medicine, such as technetium-99m (99mTc) radiopharmaceuticals, offers a promising alternative due to its ideal characteristics. Methods: This study explores the development of [2 + 1] mixed-ligand 99mTc-labeled ciprofloxacin dithiocarbamate (Cip-DTC) complexes combined with various phosphine ligands, including triphenylphosphine (PPh3), tris(4-methoxyphenyl)phosphine (TMPP), methyl(diphenyl)phosphine (MePPh2), dimethylphenylphosphine (DMPP), and 1,3,5-triaza-7-phosphaadamantane (ADAP). The characterization of 99mTc-complexes was conducted using rhenium analogs as structural models to ensure similar coordination. Results: Stability studies demonstrated the high integrity (97–98%) of the complexes under various conditions, including cysteine and histidine challenges. Lipophilicity studies indicated that complexes with higher logD7.4 values (1.6–2.7) exhibited enhanced tissue penetration and prolonged circulation. Biodistribution studies in Swiss Albino mice with induced infections and aseptic inflammation revealed distinct patterns. Specifically, the complex fac-[99mTc(CO)3(Cip-DTC)(PPh3)] (2′) showed high infected/normal muscle ratios (4.62 at 120 min), while the complex fac-[99mTc(CO)3(Cip-DTC)(TMPP)] (3′) demonstrated delayed but effective targeting (infected/normal muscle ratio of 3.32 at 120 min). Conclusions: These findings highlight the potential of 99mTc-labeled complexes as effective radiopharmaceuticals for the differential diagnosis of bacterial infections, advancing nuclear medicine diagnostics. Future studies will focus on optimizing molecular weight, lipophilicity, and stability to further enhance the diagnostic specificity and clinical utility of these radiopharmaceuticals. Full article
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<p>Synthesis of rhenium complexes <b>1</b>–<b>6</b>: (<b>i</b>) method A: H<sub>2</sub>O, 50 °C, 4 h; (<b>ii</b>) methanol, 50 °C, 4 h; (<b>iii</b>) method B: methanol, reflux, 2 h; (<b>iv</b>) method C: P (TMPP, MePPh2, DMPP, or ADAP), 50 °C, 4 h.</p>
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<p>Radiosynthesis of technetium-99m complexes <b>1′</b>–<b>6′</b>.</p>
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<p>Representative comparative reverse-phase HPLC chromatograms: UV detection at 254 nm of complex <b>4</b> (solid). radiometric detection of complex <b>4′</b> (dash).</p>
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16 pages, 2676 KiB  
Article
Characterization of Inductive Moderate Hyperthermia Effects on Intratumor Sarcoma-45 Heterogeneity Using Magnetic Resonance, Ultrasound and Histology Image Analysis
by Valerii B. Orel, Olga Yo. Dasyukevich, Valerii E. Orel, Oleksandr Yu. Rykhalskyi, Larysa M. Kovalevska, Olexander Yu. Galkin, Karyna S. Matveichuk, Anatolii G. Diedkov, Vasyl V. Ostafiichuk and Oleksandr S. Shablii
Appl. Sci. 2024, 14(18), 8251; https://doi.org/10.3390/app14188251 - 13 Sep 2024
Viewed by 211
Abstract
Evaluating intratumor heterogeneity with image texture analysis offers a more sophisticated understanding of sarcoma response to treatment. We examined the effects of inductive moderate hyperthermia (IMH) on sarcoma-45 growth and intratumor heterogeneity across tissue, cellular and molecular levels using magnetic resonance imaging (MRI), [...] Read more.
Evaluating intratumor heterogeneity with image texture analysis offers a more sophisticated understanding of sarcoma response to treatment. We examined the effects of inductive moderate hyperthermia (IMH) on sarcoma-45 growth and intratumor heterogeneity across tissue, cellular and molecular levels using magnetic resonance imaging (MRI), ultrasound and histology image analysis. IMH (42 MHz, 20 W) inhibited sarcoma-45 growth kinetics by 34% compared to the untreated control group. T2-weighted MRI brightness was increased by 42%, reflecting more extensive tumor necrosis, while Young’s modulus increased by 37% due to more pronounced connective tissue replacement in response to IMH. Whereas calculations of Moran’s spatial autocorrelation index revealed distinctions in heterogeneity between tumor core, periphery and capsule regions of interest (ROIs) on MRI, ultrasound and histological examination in the untreated tumor-bearing animals, there was no significant difference between core and periphery after IMH. Exposure to IMH increased overall tumor ROI heterogeneity by 22% on MRI but reduced heterogeneity in the core and periphery on ultrasound and histology images. Ki-67 protein distribution was 25% less heterogeneous on the tumor periphery after IMH. Therefore, this study provides a quantitative characterization of IMH effects on different manifestations of intratumor sarcoma-45 heterogeneity using experimental imaging data. Full article
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<p>Computer modeling of specific absorption rate (<b>a</b>) and temperature distribution (<b>b</b>) in sarcoma-45 in response to IMH: 1—loop applicator; 2—magnetic dipoles; 3—tumor core; 4—tumor periphery; 5—tumor capsule.</p>
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<p>Tumor growth kinetics of sarcoma-45: 1—control group (no treatment); 2—IMH group. Insets: (<b>a</b>)—tumor; (<b>b</b>)—tumor capsule.</p>
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<p>T<sub>2</sub>-weighted coronal MRI scans of sarcoma-bearing animals on day 24 after tumor implantation ((<b>a</b>)—control group; (<b>b</b>)—treatment group): 1—tumor core ROI; 2—tumor periphery ROI; 3—tumor capsule ROI.</p>
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<p>Ultrasound B-mode (<b>a</b>,<b>c</b>) and elastography (<b>b</b>,<b>d</b>) scans of sarcoma-45 on day 24 after tumor implantation ((<b>a</b>,<b>b</b>)—control group; (<b>c</b>,<b>d</b>)—IMH group): 1—tumor core ROI; 2—tumor periphery ROI; 3—tumor capsule ROI.</p>
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<p>Wavelet transform scalogram of sarcoma-45 blood flow signals in control (<b>a</b>) and IMH (<b>b</b>) groups. Color bars represent the magnitude of continuous wavelet transform coefficients.</p>
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<p>Histological findings observed in sarcoma-45. H&amp;E, ×400. Control group ((<b>a</b>)—tumor core; (<b>c</b>)—tumor periphery; (<b>e</b>)—Ki-67 expression in tumor periphery; (<b>g</b>)—tumor capsule) and IMH group ((<b>b</b>)—tumor core; (<b>d</b>)—tumor periphery; (<b>f</b>)—Ki-67 expression in tumor periphery; (<b>h</b>)—tumor capsule): short arrows—nucleated cells; long arrows—nonnucleated cells and karyorrhexis; arrowhead—mitotic figure; dotted arrows—apoptotic bodies; asterisks—necrotic foci; triangles—connective tissue replacement.</p>
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13 pages, 1290 KiB  
Article
Determination of Ethanol Content in Alcoholic Products by LF-NMR
by Gianluca Farine, Maria Scilinguo, Chiara Calvagna, Silvia Romano, Marco Polito and Salvatore Sgrò
Analytica 2024, 5(3), 458-470; https://doi.org/10.3390/analytica5030031 - 12 Sep 2024
Viewed by 345
Abstract
Nuclear magnetic resonance (NMR) is a technique used for many years by chemists for elucidation of molecular structure. Technological progress over the years has enabled this technique, making it easier to use. Thus, the LF-NMR (low-field NMR) was introduced as a side technique, [...] Read more.
Nuclear magnetic resonance (NMR) is a technique used for many years by chemists for elucidation of molecular structure. Technological progress over the years has enabled this technique, making it easier to use. Thus, the LF-NMR (low-field NMR) was introduced as a side technique, characterized by low management costs and shorter analysis time than its main counterpart. The application of 1H LF-NMR for the quantification of ethyl alcohol in different alcoholic matrices is herein described, comparing the results obtained with this technique with those determined by a reference gas chromatographic method. Full article
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<p>The 1D PROTON pulse sequence.</p>
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<p><sup>1</sup>H-NMR spectrum of a mixture consisting of the alcohol sample and salicylaldehyde in 1:3 volume ratio. The coloured arrows represent the different peaks examined for analysis: the orange arrow indicates the singlet (at 9.4 ppm) of the proton of salicylic aldehyde, used as the internal standard; the yellow arrow indicates the signal (at 3.9 ppm) of the proton of the hydroxyl group of ethyl alcohol, the black arrow indicates the quadruplet (at 3.2 ppm) related to the two methylene group’s protons of ethyl alcohol (-CH<sub>2</sub>); the grey arrow indicates the triplet (at 0.8 ppm) related to the three methyl group’s protons of ethyl alcohol (-CH<sub>3</sub>).</p>
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<p>Correlation between results obtained by NMR, based on-CH<sub>3</sub> (<b>a</b>) and -CH<sub>2</sub> (<b>b</b>) group signals, respectively, and GC-FID methods.</p>
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<p>The spectra 1 and 2, respectively, to the reference absolute ethyl alcohol and ethanol standard solution containing 14 denaturants. The coloured arrows represent the different peaks examined for analysis: the orange arrow indicates the singlet (at 9.4 ppm) of the proton of salicylic aldehyde, used as the internal standard; the yellow arrow indicates the signal (at 3.9 ppm) of the proton of the hydroxyl group of ethyl alcohol, the black arrow indicates the quadruplet (at 3.2 ppm) related to the two methylene group’s protons of ethyl alcohol (-CH<sub>2</sub>); the grey arrow indicates the triplet (at 0.8 ppm) related to the three methyl group’s protons of ethyl alcohol (-CH<sub>3</sub>).</p>
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<p>Linearity using -CH<sub>3</sub> (<b>a</b>) and -CH<sub>2</sub> (<b>b</b>) group signals of ethanol.</p>
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12 pages, 10424 KiB  
Article
Structural and Magnetic Properties of Dimeric Capsule Assemblies Formed by Cyclic Trinuclear Complexes
by Masahiro Muto, Kousuke Morinaga, Momoko Nishihashi, Yasunori Yamada and Masayuki Koikawa
Molecules 2024, 29(18), 4307; https://doi.org/10.3390/molecules29184307 - 11 Sep 2024
Viewed by 251
Abstract
Cyclic trinuclear homo-metal complexes, [{Fe(L3+2Br)py}3] (1) and [{Mn(L3+2Br)}3(py)2 MeOH] (2), along with a hetero-metal complex, [FeMn2(L3+2H)3(DMF)3] (3), were synthesized using [...] Read more.
Cyclic trinuclear homo-metal complexes, [{Fe(L3+2Br)py}3] (1) and [{Mn(L3+2Br)}3(py)2 MeOH] (2), along with a hetero-metal complex, [FeMn2(L3+2H)3(DMF)3] (3), were synthesized using asymmetric ditopic ligands (H3L3+2H: 2-(2-hydroxyphenyl)-6-ol-5-(salicylideneamino)benzoxazole, H3L3+2Br: 2-(2-hydrox-5-bromoyphenyl)-6-ol-5-(5-bromosalicylideneamino)benzoxazole). The molecular structure of 1 is characterized by a tripod structure with three-fold symmetry, where an enantiomer pair forms a dimeric capsule with dimensions of approximately 3 × 1.6 × 1.6 nm3. Complexes 2 and 3, which lack three-fold symmetry, exhibit similar molecular structures to previously reported complexes with these ligands, but do not form a capsule structure. Magnetic measurements of 13 reveal the presence of significantly weak antiferromagnetic interactions between the metal ions. Full article
(This article belongs to the Special Issue Advances in Coordination Chemistry 2.0)
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<p>(<b>a</b>) Molecular structure of <b>1</b> with thermal ellipsoids drawn at a 50% probability level. Symmetry code: (<sup>1</sup>) −<span class="html-italic">x</span> + <span class="html-italic">y</span>, −<span class="html-italic">x</span>, +<span class="html-italic">z</span>; (<sup>2</sup>) −<span class="html-italic">y</span>, <span class="html-italic">x</span> − <span class="html-italic">y</span>, +<span class="html-italic">z</span>. Hydrogen atoms have been omitted for clarity. (<b>b</b>) Coordination polyhedron of Fe with the ligand framework shown as a line drawing.</p>
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<p>(<b>a</b>) Ball-and-stick model for the enantiomeric pair of <b>1</b> viewed along the <span class="html-italic">c</span> axis. Each enantiomer is color coded. Symmetry code: (<sup>1</sup>) −<span class="html-italic">x</span> + <span class="html-italic">y</span>, −<span class="html-italic">x</span>, +<span class="html-italic">z</span>; (<sup>2</sup>) −<span class="html-italic">y</span>, <span class="html-italic">x</span> − <span class="html-italic">y</span>, +<span class="html-italic">z</span>. (<b>b</b>) Crystal packing view along the <span class="html-italic">c</span> axis.</p>
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<p>(<b>a</b>) Space-filling model of the enantiomeric pair viewed from the <span class="html-italic">a</span> axis. Hydrogen atoms and coordinating pyridine molecules have been omitted for clarity. (<b>b</b>) Hirshfeld surface of the enantiomeric pair. (<b>c</b>) Solvent mask mapping view (green surface) of the unit cell. (<b>d</b>) Solvent mask mapping view from the <span class="html-italic">c</span> axis.</p>
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<p>(<b>a</b>) Molecular structure of <b>2</b> showing thermal ellipsoids drawn at a 50% probability level. Only the disordered pyridine unit with larger occupancy is shown. Hydrogen atoms are omitted for clarity. (<b>b</b>) Space-filling model for the enantiomeric pair of <b>2</b>. Each monomer unit is color-coded.</p>
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<p>(<b>a</b>) Molecular structure of <b>3</b> showing thermal ellipsoids drawn at a 30% probability level. Hydrogen atoms have been omitted for clarity. (<b>b</b>) Ball-and-stick model of the nearest trinuclear units. Symmetry code: (*) 1 − <span class="html-italic">x</span>, −<span class="html-italic">y</span>, 1 − <span class="html-italic">z</span>.</p>
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<p>Temperature dependence of <span class="html-italic">χ</span><sub>M</sub><span class="html-italic">T</span> vs. <span class="html-italic">T</span> plots of <b>1</b> (red circles), <b>2</b> (blue triangles), and <b>3</b> (green squares). Solid lines are drawn with the best-fitted parameter values described in the text. The inset figure is the magnetic coupling scheme for <b>3</b>.</p>
Full article ">Scheme 1
<p>Reaction scheme and chemical diagrams of H<sub>4</sub>L<sup>3+3</sup>R, H<sub>3</sub>L<sup>3+2</sup>R, and [{M(H<sub>3</sub>L<sup>3+2</sup>R)X}<sub>3</sub>] (R = H or Br; M = Fe or Mn; X = pyridine, dimethylformamide, or methanol). The structure of the trinuclear complex is color-coded by mononuclear unit.</p>
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15 pages, 566 KiB  
Article
Improving the Extraction of Polyphenols from Cocoa Bean Shells by Ultrasound and Microwaves: A Comparative Study
by Vincenzo Disca, Fabiano Travaglia, Chiara Carini, Jean Daniel Coïsson, Giancarlo Cravotto, Marco Arlorio and Monica Locatelli
Antioxidants 2024, 13(9), 1097; https://doi.org/10.3390/antiox13091097 - 10 Sep 2024
Viewed by 338
Abstract
The extraction of bioactive compounds from food by-products is one of the most important research areas for the nutraceutical, pharmaceutical, and food industries. This research aimed to evaluate the efficiency of Ultrasound-Assisted Extraction (UAE) and Microwave-Assisted Extraction (MAE), either alone or in combination, [...] Read more.
The extraction of bioactive compounds from food by-products is one of the most important research areas for the nutraceutical, pharmaceutical, and food industries. This research aimed to evaluate the efficiency of Ultrasound-Assisted Extraction (UAE) and Microwave-Assisted Extraction (MAE), either alone or in combination, of phenolic compounds from cocoa bean shells (CBSs). These extraction techniques were compared with conventional methods, such as under simple magnetic stirring and the Soxhlet apparatus. After the preliminary characterization of the gross composition of CBSs, the total polyphenol content and radical scavenging of extracts obtained from both raw and defatted cocoa bean shells were investigated. Quantification of the main polyphenolic compounds was then performed by RP-HPLC-DAD, identifying flavonoids and phenolic acids, as well as clovamide. The application of MAE and UAE resulted in a similar or superior extraction of polyphenols when compared with traditional methods; the concentration of individual polyphenols was variously influenced by the extraction methods employed. Combining MAE and UAE at 90 °C yielded the highest antiradical activity of the extract. Spectrophotometric analysis confirmed the presence of high-molecular-weight melanoidins, which were present in higher concentrations in the extracts obtained using MAE and UAE, especially starting from raw material. In conclusion, these results emphasize the efficiency of MAE and UAE techniques in obtaining polyphenol-rich extracts from CBS and confirm this cocoa by-product as a valuable biomass for the recovery of antioxidant compounds, with a view to possible industrial scale-up. Full article
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<p>Extinction coefficient K<sub>mix</sub> at 280 nm (<b>a</b>), 320 nm (<b>b</b>), and 420 nm (<b>c</b>) in the different extracts of CBSs. MS: magnetic stirring; SOX: Soxhlet; US: ultrasound; MW: microwaves; US/MW 50: ultrasound and microwaves at 50 °C; US/MW 90: ultrasound and microwaves at 90 °C.</p>
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29 pages, 3830 KiB  
Review
Utilizing Molecular Dynamics Simulations, Machine Learning, Cryo-EM, and NMR Spectroscopy to Predict and Validate Protein Dynamics
by Ahrum Son, Woojin Kim, Jongham Park, Wonseok Lee, Yerim Lee, Seongyun Choi and Hyunsoo Kim
Int. J. Mol. Sci. 2024, 25(17), 9725; https://doi.org/10.3390/ijms25179725 - 8 Sep 2024
Viewed by 400
Abstract
Protein dynamics play a crucial role in biological function, encompassing motions ranging from atomic vibrations to large-scale conformational changes. Recent advancements in experimental techniques, computational methods, and artificial intelligence have revolutionized our understanding of protein dynamics. Nuclear magnetic resonance spectroscopy provides atomic-resolution insights, [...] Read more.
Protein dynamics play a crucial role in biological function, encompassing motions ranging from atomic vibrations to large-scale conformational changes. Recent advancements in experimental techniques, computational methods, and artificial intelligence have revolutionized our understanding of protein dynamics. Nuclear magnetic resonance spectroscopy provides atomic-resolution insights, while molecular dynamics simulations offer detailed trajectories of protein motions. Computational methods applied to X-ray crystallography and cryo-electron microscopy (cryo-EM) have enabled the exploration of protein dynamics, capturing conformational ensembles that were previously unattainable. The integration of machine learning, exemplified by AlphaFold2, has accelerated structure prediction and dynamics analysis. These approaches have revealed the importance of protein dynamics in allosteric regulation, enzyme catalysis, and intrinsically disordered proteins. The shift towards ensemble representations of protein structures and the application of single-molecule techniques have further enhanced our ability to capture the dynamic nature of proteins. Understanding protein dynamics is essential for elucidating biological mechanisms, designing drugs, and developing novel biocatalysts, marking a significant paradigm shift in structural biology and drug discovery. Full article
(This article belongs to the Special Issue Advanced Research on Protein Structure and Protein Dynamics)
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<p>Advanced Experimental Techniques and Applications for Studying Protein Dynamics. (<b>A</b>) Schematic diagram of advanced Cryo-Electron Microscopy (Cryo-EM) techniques, including Time-resolved cryo-EM, Cryo-electron tomography, and Micro-crystal electron diffraction (MicroED). (<b>B</b>) Application fields of protein dynamics research using Nuclear Magnetic Resonance (NMR) Spectroscopy techniques, including Relaxation dispersion experiments, Paramagnetic relaxation enhancement (PRE), and Residual dipolar couplings (RDCs). These methods are powerful tools for examining structural changes and complex molecular in-teractions of proteins. (<b>C</b>) Application fields of protein dynamics research using Fluorescence-Based Techniques, including Single-molecule FRET, Fluorescence correlation spectroscopy (FCS), and Fluorescence lifetime imaging microscopy (FLIM). These methods are utilized as powerful tools to investigate biomolecular dynamics, intracellular protein interactions, and structural changes of molecules, providing high sensitivity and the ability to identify proteins in living cells.</p>
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<p>Molecular Dynamics Simulations in Structural Proteomics. (<b>A</b>) Molecular dynamics (MD) simulations simulate atomic trajectories over time using Newton’s equations. Capturing atomic behavior throughout time increases temporal efficiency and allows detailed exploration of a large space. MD uses Verlet and Leapfrog algorithms. With the rapid development of computational resources and model development, it outperforms the Verlet and Leapfrog algorithms used in MD. (<b>B</b>) Polarizable force fields and quantum mechanics/molecular mechanics (QM/MM) method enable coarse-grained (CG) models to study biological processes on milli-second to second time scales and large-scale protein structural changes. As computing technology has advanced, machine learning (ML) and deep learning (DL) algorithms have showed promise in accuracy and analysis time by learning quantum mechanics data. (<b>C</b>) Although various analysis techniques have been developed, force field precision, sampling rare occurrences, and bridging femtosecond to second timeframes remain hurdles. These issues must be resolved to understand biomolecular dynamics and processes. Comprehensive sampling methods like Metadynamics and REMD have emerged to solve these challenges. These improved sampling methods are essential for understanding complicated biological systems and studying structural changes, and they are advancing MD simulation. The merging of ML and DL techniques has made computational resources and MD simulation models essential for understanding new protein dynamics.</p>
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<p>Utilization of Advanced Experimental and Computational Methods in Protein Dynamics Research. (<b>A</b>) A schematic diagram illustrating the application of experimental and computational methods to the dynamics of protein folding and misfolding. These methods expedite the identification of targeted protein relationships with drug targets. (<b>B</b>) Protein dynamics approaches are employed to apply enzyme-substrate complexes in a schematic diagram. These mechanisms regulate protein activity by utilizing the substrate to undergo conformational and electrochemical changes. (<b>C</b>) The application of protein dynamics approaches to membrane proteins. It is capable of predicting the structure of a protein that is bound to a membrane and improving our comprehension of signal transduction.</p>
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<p>Illustrates the future directions and challenges in protein dynamics research that can be addressed through computational and experimental methods. (<b>A</b>) A method for integrating atomic simulations, coarse-grained models, and experimental data to link temporal and spatial dimensions. This multi-scale technique helps understand complex protein behaviours at different resolutions. (<b>B</b>) Using advanced imaging and spectroscopic techniques like Cryo-ET, NMR, and single-molecule Fluorescence Resonance Energy Transfer (FRET) to visualize dynamic processes in live cells. (<b>C</b>) Forecasting functional protein dynamics and developing tailored proteins using deep learning and machine learning. These AI-driven methods can integrate huge information and rationally design proteins for specific biological purposes and model protein activity more accurately. (<b>D</b>) Expanding dynamics studies to massive macromolecular complexes and cellular machinery. By combining MD simulations with Cryo-EM, NMR, and FRET, researchers can gain deep insights into bigger protein assemblies’ dynamic characteristics. (<b>E</b>) Linking protein motions to biological functions using cutting-edge technology to simplify targeted therapy. Experimental methods, machine learning, and MD simulations will affect the development of customized medicines to address disease-related protein dysfunctions.</p>
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22 pages, 7074 KiB  
Article
Characterization and Cytotoxic Assessment of Bis(2-hydroxy-3-carboxyphenyl)methane and Its Nickel(II) Complex
by Ayman H. Ahmed, Ibrahim O. Althobaiti, Ebtsam K. Alenezy, Yazeed M. Asiri, Sobhy Ghalab and Omar A. Hussein
Molecules 2024, 29(17), 4239; https://doi.org/10.3390/molecules29174239 - 6 Sep 2024
Viewed by 343
Abstract
A condensation reaction of salicylic acid with formaldehyde in the presence of sulfuric acid led to the synthesization of the bis(2-hydroxy-3-carboxyphenyl)methane (BHCM) ligand, which was subsequently allowed to bind with nickel (II) ions. In light of the information obtained from the elemental analyses [...] Read more.
A condensation reaction of salicylic acid with formaldehyde in the presence of sulfuric acid led to the synthesization of the bis(2-hydroxy-3-carboxyphenyl)methane (BHCM) ligand, which was subsequently allowed to bind with nickel (II) ions. In light of the information obtained from the elemental analyses (C, H, and M), spectral (IR, MS, 1H-NMR, and UV–Vis) and thermal and magnetic measurements, the most likely structures of the ligand and complex have been identified. It has been suggested that the BHCM coordinates in a tetradentate manner with two Ni(II) ions to produce an octahedral binuclear complex. The SEM and TEM morphology of the compounds showed spherical shapes. An X-ray diffraction analysis indicated a considerable difference in the diffraction patterns between BHCM (crystalline) and Ni–BHCM (amorphous), and the Scherrer equation was used to calculate the crystallite size. Some optical characteristics were estimated from UV–Vis spectra. The ligand and its nickel(II) complex underlie the range of semiconductors. It was verified that for human lung (A-549) cancer, the BHCM compound displayed a significant barrier to the proliferation test in noncancerous cells (human lung fibroblasts, WI-38), which was also undertaken. To demonstrate the binding affinities of the chosen compounds (BHCM and Ni–BHCM) in the receptor protein’s active site [PDB ID: 5CAO], a molecular docking (MD) study was carried out. Full article
(This article belongs to the Special Issue Advances in Coordination Chemistry 2.0)
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<p>BHCM and Ni–BHCM morphological pictures.</p>
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<p>XRD graph of Ni–BHCM.</p>
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<p>Changes in the nickel complex’s optical parameters include (<b>a</b>) transmittance—T, (<b>b</b>) band gap energy—E<sub>g</sub>, (<b>c</b>) refractive index—n, (<b>d</b>) optical conductivity—σ<sub>opt</sub> and (<b>e</b>) penetration depth—W.</p>
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<p>Changes in the nickel complex’s optical parameters include (<b>a</b>) transmittance—T, (<b>b</b>) band gap energy—E<sub>g</sub>, (<b>c</b>) refractive index—n, (<b>d</b>) optical conductivity—σ<sub>opt</sub> and (<b>e</b>) penetration depth—W.</p>
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<p>Changes in the nickel complex’s optical parameters include (<b>a</b>) transmittance—T, (<b>b</b>) band gap energy—E<sub>g</sub>, (<b>c</b>) refractive index—n, (<b>d</b>) optical conductivity—σ<sub>opt</sub> and (<b>e</b>) penetration depth—W.</p>
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<p>HOMO and LUMO transition, energy and optimized lowest energy structure of the ligand and nickel(II) complex. BHCM: [MM2 Minimization: Stretch: 2.1471, Bend: 8.8211, Stretch-Bend: −0.1542, Torsion: −16.3849, Non-1,4 VDW: −9.7095, 1,4 VDW: 12.6725, Dipole/Dipole: 0.3568, Total Energy: −2.2511 kcal/mol] and [MMFF94 Minimization: Final Energy: 36.2527 kcal/mol]. Ni–BHCM: [MM2 Minimization: Stretch: 118.3621, Bend: 331.6871, Stretch-Bend: −0.2150, Torsion: −9.8166, Non-1,4 VDW: −58.7081, 1,4 VDW: 4.6860, Dipole/Dipole: −62.5274, Total Energy: 323.4682 kcal/mol] and [MMFF94 Minimization: Final Energy: 683.54 kcal/mol].</p>
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<p>IC<sub>50</sub> and assessment of BHCM’s cytotoxicity on the human lung carcinoma (A-549) and fibroblast normal cells (WI-38).</p>
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<p>Interaction of BHCM with 5CAO as a receptor.</p>
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<p>Interaction of the Ni–BHCM complex with 5CAO as a receptor.</p>
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<p>FT-IR spectrum of Ni–BHCM complex.</p>
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<p>Electronic spectrum of Ni–BHCM.</p>
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<p>TGA of Ni–BHCM.</p>
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<p>Diagram illustrating the Ni–BHCM creation.</p>
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15 pages, 1867 KiB  
Article
Enzymatic Deracemization of Fluorinated Arylcarboxylic Acids: Chiral Enzymatic Analysis and Absolute Stereochemistry Using Chiral HPLC
by Oleg I. Kolodiazhnyi, Anastasiia O. Kolodiazhna, Oleh Faiziiev and Yuliia Gurova
Symmetry 2024, 16(9), 1150; https://doi.org/10.3390/sym16091150 - 4 Sep 2024
Viewed by 295
Abstract
The hydrolase-catalyzed kinetic resolution of fluorinated racemates of 3-arylcarboxylic acids is described. Hydrolysis of ethyl esters of fluorinated acids by esterases and hydrolases in all cases resulted in the formation of hydrolyzed (S)-carboxylic acids and unreacted (R)-esters in high [...] Read more.
The hydrolase-catalyzed kinetic resolution of fluorinated racemates of 3-arylcarboxylic acids is described. Hydrolysis of ethyl esters of fluorinated acids by esterases and hydrolases in all cases resulted in the formation of hydrolyzed (S)-carboxylic acids and unreacted (R)-esters in high yields and high enantiomeric purity. The influence of separation conditions on the efficiency and enantioselectivity of biocatalytic conversion was also studied. The reactions were carried out under normal conditions (stirring with a magnetic stirrer at room temperature) and microwave irradiation in the presence of hydrolases. Amano PS showed excellent selectivity and good yields in the hydrolysis of fluorinated aromatic compounds. The absolute configuration of the resulting compounds was based on biokinetic studies and the use of chiral HPLC. A molecular modeling of the kinetic resolution of carboxylic acid esters was carried out. Full article
(This article belongs to the Collection Feature Papers in Chemistry)
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<p>Synthesis of racemic ethyl 3-aryl-2-methylpropanoates <b>2a</b>–<b>e</b> and ethyl 3-arylbutanoates <b>4a</b>–<b>f</b>.</p>
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<p>Enzymatic resolution of enantiomeric racemic arylcarboxylic acids esters <b>3a</b>–<b>e</b>.</p>
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<p>Additional deracemization of 2-methylarylcarboxylic acid <b>5a</b>.</p>
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<p>Enzymatic resolution by Amano PS of ethyl (<span class="html-italic">R</span>)-4,4,4-trifluoro-3-phenylbutanoate <b>5f</b> under microwave irradiation.</p>
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<p>An example of the analysis of 3-(4-fluorophenyl)-2-methylpropanoic acid by chiral HPLC: (<b>a</b>)—racemate; (<b>b</b>)—(<span class="html-italic">R</span>)-<b>2a</b> (chiral column Chiralcel OJ-H (250 × 4.6 mm, with Tris(4-methylbenzoate) cellulose selector deposited on 5 μm silica gel).</p>
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<p>The catalytic center and the covalently bound transition state complexes. The (<span class="html-italic">S</span>)-enantiomer is presented on the <b>left</b>, while the (<span class="html-italic">R</span>)-enantiomer is showcased on the <b>right</b>. To simplify visual noise, all protons were removed.</p>
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<p>The difference between the first and the last step of the ligand conformation in the MD simulation of the transition complex. The start of the simulation is shown in cyan; the end of the simulation is shown in magenta colors. To simplify visual noise, all protons were removed, even both polar hydrogens from histidine.</p>
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29 pages, 906 KiB  
Review
Getting Up to Speed: Rapid Pathogen and Antimicrobial Resistance Diagnostics in Sepsis
by Mariana P. Liborio, Patrick N. A. Harris, Chitra Ravi and Adam D. Irwin
Microorganisms 2024, 12(9), 1824; https://doi.org/10.3390/microorganisms12091824 - 3 Sep 2024
Viewed by 817
Abstract
Sepsis is a life-threatening organ dysfunction caused by a dysregulated host response to infection. Time to receive effective therapy is a primary determinant of mortality in patients with sepsis. Blood culture is the reference standard for the microbiological diagnosis of bloodstream infections, despite [...] Read more.
Sepsis is a life-threatening organ dysfunction caused by a dysregulated host response to infection. Time to receive effective therapy is a primary determinant of mortality in patients with sepsis. Blood culture is the reference standard for the microbiological diagnosis of bloodstream infections, despite its low sensitivity and prolonged time to receive a pathogen detection. In recent years, rapid tests for pathogen identification, antimicrobial susceptibility, and sepsis identification have emerged, both culture-based and culture-independent methods. This rapid narrative review presents currently commercially available approved diagnostic molecular technologies in bloodstream infections, including their clinical performance and impact on patient outcome, when available. Peer-reviewed publications relevant to the topic were searched through PubMed, and manufacturer websites of commercially available assays identified were also consulted as further sources of information. We have reviewed data about the following technologies for pathogen identification: fluorescence in situ hybridization with peptide nucleic acid probes (Accelerate PhenoTM), microarray-based assay (Verigene®), multiplex polymerase chain reaction (cobas® eplex, BioFire® FilmArray®, Molecular Mouse, Unyvero BCU SystemTM), matrix-assisted laser desorption-ionization time-of-flight mass spectrometry (Rapid MBT Sepsityper®), T2 magnetic resonance (T2Bacteria Panel), and metagenomics-based assays (Karius©, DISQVER®, Day Zero Diagnostics). Technologies for antimicrobial susceptibility testing included the following: Alfed 60 ASTTM, VITEK® REVEALTM, dRASTTM, ASTar®, Fastinov®, QuickMIC®, ResistellTM, and LifeScale. Characteristics, microbiological performance, and issues of each method are described, as well as their clinical performance, when available. Full article
(This article belongs to the Section Antimicrobial Agents and Resistance)
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<p>Time to receive results of selected rapid diagnostic tests in sepsis. Abbreviations: ID—identification; MALDI-TOF MS—matrix-assisted laser desorption-ionization time-of-flight mass spectrometry; PNA-FISH—fluorescence in situ hybridization with peptide nucleic acid probes; PCR—polymerase chain reaction; AST—antimicrobial susceptibility testing; BC+—blood culture positivity. Day zero diagnostics does not specify how many hours are needed for results.</p>
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16 pages, 1802 KiB  
Review
Applying the Atomic Force Microscopy Technique in Medical Sciences—A Narrative Review
by Karolina Krawczyk-Wołoszyn, Damian Roczkowski, Adam Reich and Magdalena Żychowska
Biomedicines 2024, 12(9), 2012; https://doi.org/10.3390/biomedicines12092012 - 3 Sep 2024
Viewed by 283
Abstract
Penetrating deep into the cells of the human body in real time has become increasingly possible with the implementation of modern technologies in medicine. Atomic force microscopy (AFM) enables the effective live imaging of cellular and molecular structures of biological samples (such as [...] Read more.
Penetrating deep into the cells of the human body in real time has become increasingly possible with the implementation of modern technologies in medicine. Atomic force microscopy (AFM) enables the effective live imaging of cellular and molecular structures of biological samples (such as cells surfaces, components of biological membranes, cell nuclei, actin networks, proteins, and DNA) and provides three-dimensional surface visualization (in X-, Y-, and Z-planes). Furthermore, the AFM technique enables the study of the mechanical, electrical, and magnetic properties of cells and cell organelles and the measurements of interaction forces between biomolecules. The technique has found wide application in cancer research. With the use of AFM, it is not only possible to differentiate between healthy and cancerous cells, but also to distinguish between the stages of cancerous conditions. For many years, AFM has been an important tool for the study of neurodegenerative diseases associated with the deposition of peptide amyloid plaques. In recent years, a significant amount of research has been conducted on the application of AFM in the evaluation of connective tissue cell mechanics. This review aims to provide the spectrum of the most important applications of the AFM technique in medicine to date. Full article
(This article belongs to the Section Biomedical Engineering and Materials)
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<p>(<b>A</b>) Photograph of the atomic force microscope; (<b>B</b>) schematic of the AFM construction. TIP: tip of the cantilever. (<b>C</b>) cantilever (white asterisk) with AFM tip (black asterisk) scanning hair—optical microscope view; (<b>D</b>) AFM graphic of the hair surface—3D projection: x—the dimension transverse to the longitudinal axis of the hair fiber; y—the dimension parallel to the longitudinal axis of the hair fiber; z—height of hair surface; (<b>E</b>) AFM image of the hair surface—deflection image: x—the dimension transverse to the longitudinal axis of the hair fiber; y—the dimension parallel to the longitudinal axis of the hair fiber; (<b>F</b>) AFM image of the hair surface—<span class="html-italic">Z</span>-axis image: x—the dimension transverse to the longitudinal axis of the hair fiber; y—the dimension parallel to the longitudinal axis of the hair fiber.</p>
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18 pages, 2411 KiB  
Article
Heterogeneous Photo-Fenton Degradation of Azo Dyes over a Magnetite-Based Catalyst: Kinetic and Thermodynamic Studies
by Jackson Anderson S. Ribeiro, Júlia F. Alves, Bruno César B. Salgado, Alcineia C. Oliveira, Rinaldo S. Araújo and Enrique Rodríguez-Castellón
Catalysts 2024, 14(9), 591; https://doi.org/10.3390/catal14090591 - 3 Sep 2024
Viewed by 404
Abstract
Textile wastewater containing dyes poses significant environmental hazards. Advanced oxidative processes, especially the heterogeneous photo-Fenton process, are effective in degrading a wide range of contaminants due to high conversion rates and ease of catalyst recovery. This study evaluates the heterogeneous photodegradation of the [...] Read more.
Textile wastewater containing dyes poses significant environmental hazards. Advanced oxidative processes, especially the heterogeneous photo-Fenton process, are effective in degrading a wide range of contaminants due to high conversion rates and ease of catalyst recovery. This study evaluates the heterogeneous photodegradation of the azo dyes Acid Red 18 (AR18), Acid Red 66 (AR66), and Orange 2 (OR2) using magnetite as a catalyst. The magnetic catalyst was synthesized via a hydrothermal process at 150 °C. Experiments were conducted at room temperature, investigating the effect of catalyst dosage, pH, and initial concentrations of H2O2 and AR18 dye. Kinetic and thermodynamic studies were performed at 25, 40, and 60 °C for the three azo dyes (AR18, AR66, and OR2) and the effect of the dye structures on the degradation efficiency was investigated. At 25 °C for 0.33 mmolL−1 of dye at pH 3.0, using 1.4 gL−1 of the catalyst and 60 mgL−1 of H2O2 under UV radiation of 16.7 mWcm−2, the catalyst showed 62.3% degradation for AR18, 79.6% for AR66, and 83.8% for OR2 in 180 min of reaction. The oxidation of azo dyes under these conditions is spontaneous and endothermic. The pseudo-first-order kinetic constants indicated a strong temperature dependence with an order of reactivity of the type OR2 > AR66 > AR18, which is associated with the molecular size, steric hindrance, aromatic conjugation, electrostatic repulsion, and nature of the acid–base interactions on the catalytic surface. Full article
(This article belongs to the Special Issue Novel Nanocatalysts for Sustainable and Green Chemistry)
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<p>Effects of AR18 degradation at 25 °C with <span class="html-italic">I<sub>L</sub></span> = 16.7 mWcm<sup>−2</sup>. (<b>a</b>) Initial catalyst dosage using a <span class="html-italic">C</span><sub>0</sub>(AR18) of ca. 60 mgL<sup>−1</sup> and <span class="html-italic">C</span><sub>0</sub>(H<sub>2</sub>O<sub>2</sub>) of ca. 30 mgL<sup>−1</sup> at a pH of 3.0 during 120 min of reaction time. (<b>b</b>) Blank runs of the degradation of AR18 over magnetite in distinct reaction conditions. <span class="html-italic">C</span><sub>0</sub>(Fe<sub>3</sub>O<sub>4</sub>) = 1.4 gL<sup>−1</sup>, <span class="html-italic">C</span><sub>0</sub>(AR18) = 60 mgL<sup>−1</sup>, <span class="html-italic">C</span><sub>0</sub>(H<sub>2</sub>O<sub>2</sub>) = 60 mgL<sup>−1</sup>, <span class="html-italic">I<sub>L</sub></span> = 16.7 mWcm<sup>−2</sup>, and a pH of 3.0 at 120 min.</p>
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<p>(<b>a</b>) Influence of pH with an initial catalyst dosage <span class="html-italic">C</span><sub>0</sub>(Fe<sub>3</sub>O<sub>4</sub>) of 1.4 gL<sup>−1</sup> at a fixed condition of <span class="html-italic">C</span><sub>0</sub>(AR18) = 60 mgL<sup>−1</sup>, <span class="html-italic">C</span><sub>0</sub>(H<sub>2</sub>O<sub>2</sub>) = 30 mgL<sup>−1</sup> within 120 min. (<b>b</b>) Influence of the initial H<sub>2</sub>O<sub>2</sub> concentration using <span class="html-italic">C</span><sub>0</sub>(Fe<sub>3</sub>O<sub>4</sub>) of 1.4 gL<sup>−1</sup> and <span class="html-italic">C</span><sub>0</sub>(AR18) of about 60 mgL<sup>−1</sup> at a pH of 3.0 for 120 min. (<b>c</b>) Effect of <span class="html-italic">C</span><sub>0</sub>(AR18) with a <span class="html-italic">C</span><sub>0</sub>(Fe<sub>3</sub>O<sub>4</sub>) of 1.4 gL<sup>−1</sup>, <span class="html-italic">C</span><sub>0</sub>(H<sub>2</sub>O<sub>2</sub>) of 60 mgL<sup>−1</sup>, and a pH of 3.0 for 120 min. (<b>d</b>) Reuse of the Fe<sub>3</sub>O<sub>4</sub> at 25 °C after the heterogeneous photo-Fenton reaction using a 1.4 gL<sup>−1</sup>, <span class="html-italic">C</span><sub>0</sub>(AR18) of 60 mg L<sup>−1</sup>, <span class="html-italic">C</span><sub>0</sub>(H<sub>2</sub>O<sub>2</sub>) = 60 mgL<sup>−1</sup>, <span class="html-italic">I<sub>L</sub></span> = 16.7 mW cm<sup>−2</sup>, at a pH of 3.0 and <span class="html-italic">t</span> = 120 min.</p>
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<p>Degradation of AR18, AR66, and OR2 in a heterogeneous photo-Fenton-like process as a function of time. Reaction conditions: <span class="html-italic">C</span><sub>0</sub>(Fe<sub>3</sub>O<sub>4</sub>) = 1.4 gL<sup>−1</sup>, <span class="html-italic">C</span><sub>0</sub>(dye) = 0.33 mmolL<sup>−1</sup>, <span class="html-italic">C</span><sub>0</sub>(H<sub>2</sub>O<sub>2</sub>) = 60 mg L<sup>−1</sup>, <span class="html-italic">I<sub>L</sub></span> = 16.7 mWcm<sup>−2</sup>, and a pH of ca. 3.0.</p>
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<p>Arrhenius plots for heterogeneous photo-Fenton degradation of AR18, AR66, and OR2. <span class="html-italic">C</span><sub>0</sub>(Fe<sub>3</sub>O<sub>4</sub>) = 1.4 gL<sup>−1</sup>, <span class="html-italic">C</span><sub>0</sub>(dye) = 0.33 mmolL<sup>−1</sup>, <span class="html-italic">C</span><sub>0</sub>(H<sub>2</sub>O<sub>2</sub>) = 60 mgL<sup>−1</sup>, <span class="html-italic">I<sub>L</sub></span> = 16.7 mWcm<sup>−2</sup>, and a pH of ca. 3.0.</p>
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<p>The van’t Hoff plots for the heterogeneous photo-Fenton degradation of AR18, AR66, and OR2. <span class="html-italic">C</span><sub>0</sub>(Fe<sub>3</sub>O<sub>4</sub>) = 1.4 gL<sup>−1</sup>, <span class="html-italic">C</span><sub>0</sub>(dye) = 0.33 mmolL<sup>−1</sup>, <span class="html-italic">C</span><sub>0</sub>(H<sub>2</sub>O<sub>2</sub>) = 60 mgL<sup>−1</sup>, <span class="html-italic">I<sub>L</sub></span> = 16.7 mWcm<sup>−2</sup>, and a pH of ca. 3.0.</p>
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<p>Azo dye structures in a study adapted from <a href="http://worlddyevariety.com" target="_blank">worlddyevariety.com</a> (accessed on 28 August 2024). (<b>a</b>) OR2. (<b>b</b>) AR18. (<b>c</b>) AR66.</p>
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<p>Comparison of the degradation efficiency of the AR18 azo dye at 25 °C over distinct iron catalysts via the heterogeneous photo-Fenton process. Catalyst dosage = 1.4 gL<sup>−1</sup>, <span class="html-italic">C</span><sub>0</sub>(AR18) = 60 mgL<sup>−1</sup>, <span class="html-italic">C</span><sub>0</sub>(H<sub>2</sub>O<sub>2</sub>) = 60 mgL<sup>−1</sup>, <span class="html-italic">I<sub>L</sub></span> = 16.7 mWcm<sup>−2</sup>, and a pH of 3.0 at 180 min. <sup>a</sup> Synthesized according to [<a href="#B47-catalysts-14-00591" class="html-bibr">47</a>], <sup>b</sup> Synthesized according to [<a href="#B48-catalysts-14-00591" class="html-bibr">48</a>], <sup>c</sup> Commercial (Sigma-Aldrich, St. Louis, MO, USA), and <sup>d</sup> synthesized in this work.</p>
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<p>UV–Vis spectra of Orange 2 as a function of reaction time at 60 °C in the heterogeneous photo-Fenton-like reaction. Catalyst dosage = 1.4 gL<sup>−1</sup>, <span class="html-italic">C</span><sub>0</sub>(dye) = 0.33 mmolL<sup>−1</sup>, <span class="html-italic">C</span><sub>0</sub>(H<sub>2</sub>O<sub>2</sub>) = 60 mgL<sup>−1</sup>, and <span class="html-italic">I<sub>L</sub></span> = 16.7 mWcm<sup>−2</sup> at a pH of 3.0.</p>
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<p>XPS spectra of Fe 2<span class="html-italic">p</span> core levels for magnetite. (<b>a</b>) Fresh Fe<sub>3</sub>O<sub>4</sub>, and after the heterogeneous photo-Fenton-like process with (<b>b</b>) AR18 and (<b>c</b>) AR 66. Reaction conditions: Catalyst dosage = 1.4 gL<sup>−1</sup>, <span class="html-italic">C</span><sub>0</sub>(dye) = 0.33 mmolL<sup>−1</sup>, <span class="html-italic">C</span><sub>0</sub>(H<sub>2</sub>O<sub>2</sub>) = 60 mgL<sup>−1</sup>, and <span class="html-italic">I<sub>L</sub></span> = 16.7 mWcm<sup>−2</sup> at a pH of 3.0 at 60 °C.</p>
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15 pages, 2208 KiB  
Article
Sex-Related Differences in the Associations between Adiponectin and Serum Lipoproteins in Healthy Subjects and Patients with Metabolic Syndrome
by Iva Klobučar, Hansjörg Habisch, Lucija Klobučar, Matias Trbušić, Gudrun Pregartner, Andrea Berghold, Gerhard M. Kostner, Hubert Scharnagl, Tobias Madl, Saša Frank and Vesna Degoricija
Biomedicines 2024, 12(9), 1972; https://doi.org/10.3390/biomedicines12091972 - 1 Sep 2024
Viewed by 279
Abstract
The strong associations between the serum levels of adiponectin and the lipoprotein subclasses observed in healthy subjects are much weaker in patients with metabolic syndrome (MS). However, the impact of sex on these associations remained unexplored. Therefore, in the present study, we examined [...] Read more.
The strong associations between the serum levels of adiponectin and the lipoprotein subclasses observed in healthy subjects are much weaker in patients with metabolic syndrome (MS). However, the impact of sex on these associations remained unexplored. Therefore, in the present study, we examined associations between adiponectin and the lipoprotein subclasses, analyzed by nuclear magnetic resonance spectroscopy, separately in healthy females and males, as well as in females and males with MS. We observed negative correlations between adiponectin and VLDL, IDL, and small-dense LDL in healthy males, but neither in healthy females nor in females or males with MS. Additionally, adiponectin was positively correlated with some HDL subclasses in healthy males and females with MS, but not in healthy females or males with MS. Adjusting for age and either body mass index, waist circumference, C-reactive protein, or interleukin-6 weakened the associations between adiponectin and VLDL and IDL but not small-dense LDL. The adjustment weakened the associations between adiponectin and HDL in healthy males but not in females with MS. Based on our results, we conclude that sex and the presence of MS are strong determinants of the associations between adiponectin and serum lipoproteins and that the complex regulatory network comprising adiponectin and other molecular players involved in the regulation of lipoprotein metabolism is primarily operative in healthy males and females with MS. Full article
(This article belongs to the Special Issue Recent Advances in Adipokines—2nd Edition)
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Graphical abstract

Graphical abstract
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<p>Heatmap of correlation analyses between the serum levels of adiponectin and the VLDL subclasses, performed separately for healthy females and males, as well as females and males with MS. Spearman correlation coefficients with |r| ≥ 0.5 are depicted in bold. ApoB, apolipoprotein B; C, cholesterol; FC, free cholesterol; PL, phospholipid; TG, triglyceride; VLDL, very low-density lipoprotein.</p>
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<p>Heatmap of correlation analyses between the serum levels of adiponectin and IDL, performed separately for the healthy females and males, as well as females and males with MS. Spearman correlation coefficients with |r| ≥ 0.5 are depicted in bold. ApoB, apolipoprotein B; C, cholesterol; FC, free cholesterol; IDL, intermediate-density lipoprotein; PL, phospholipid; TG, triglyceride.</p>
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<p>Heatmap of correlation analyses between the serum levels of adiponectin and the LDL subclasses, performed separately for healthy females and males, as well as females and males with MS. Spearman correlation coefficients with |r| ≥ 0.5 are depicted in bold. ApoB, apolipoprotein B; C, cholesterol; FC, free cholesterol; LDL, low-density lipoprotein; PL, phospholipid; TG, triglyceride.</p>
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<p>Heatmap of correlation analyses between the serum levels of adiponectin and the HDL subclasses, performed separately for the healthy females and males, as well as females and males with MS. Spearman correlation coefficients with |r| ≥ 0.5 are depicted in bold. ApoB, apolipoprotein B; C, cholesterol; FC, free cholesterol; HDL, high-density lipoprotein; PL, phospholipid; TG, triglyceride.</p>
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18 pages, 911 KiB  
Review
Bioactive Polysaccharides from Gracilaria lemaneiformis: Preparation, Structures, and Therapeutic Insights
by Min Wang, Zhen Zhu, Xiaocheng Wu, Kitleong Cheong, Xiaohua Li, Wanli Yu, Yinlin Yao, Jiang Wu and Zhanhui Cao
Foods 2024, 13(17), 2782; https://doi.org/10.3390/foods13172782 - 31 Aug 2024
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Abstract
Gracilaria lamaneiformis, a red seaweed, is an abundant source of bioactive polysaccharides with significant health-promoting properties. Nevertheless, the broad application of G. lamaneiformis in the nutraceutical and pharmaceutical sectors remains constrained due to the absence of comprehensive data. This review provides a [...] Read more.
Gracilaria lamaneiformis, a red seaweed, is an abundant source of bioactive polysaccharides with significant health-promoting properties. Nevertheless, the broad application of G. lamaneiformis in the nutraceutical and pharmaceutical sectors remains constrained due to the absence of comprehensive data. This review provides a detailed examination of the preparation methods, structural characteristics, and biological activities of G. lamaneiformis polysaccharides (GLPs). We explore both conventional and advanced extraction techniques, highlighting the efficiency and yield improvements achieved through methods such as microwave-, ultrasonic-, and enzyme-assisted extraction. The structural elucidation of GLPs using modern analytical techniques, including high-performance liquid chromatography, gas chromatography, and nuclear magnetic resonance spectroscopy, is discussed, providing comprehensive insights into their molecular composition and configuration. Furthermore, we critically evaluate the diverse biological activities of GLPs, including their antioxidant, anti-inflammatory, antitumor, and gut microbiota modulation properties. This review underscores the therapeutic potential of GLPs and suggests future research directions to fully harness their health benefits. Full article
(This article belongs to the Special Issue Advanced Research and Development of Carbohydrate from Foods)
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<p>The pros and cons of the conventional extraction method and advanced extraction techniques, including microwave-assisted, ultrasonic-assisted, and enzymatic-assisted extraction. Red indicates the extraction methods, green highlights the advantages of each extraction method, and grey points out the disadvantages of each extraction method.</p>
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<p>Summary of the advantages and disadvantages of different purification techniques for GLPs, including ethanol precipitation, column chromatography, and membrane technology.</p>
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