Search Results (143)

Background and Objectives: Temporomandibular disorders (TMDs) encompass a broad spectrum of functional and structural abnormalities of the temporomandibular joint (TMJ). Conventional diagnostic tools, although essential, often fail to capture the underlying biochemical mechanisms driving disease progression. Synovial fluid (SF), by virtue of its direct proximity to intra-articular tissues, represents an accessible biological matrix for identifying molecular signatures of inflammation, cartilage degradation, lubrication failure, oxidative stress, and angiogenic activation. The objective of this review is to synthesize current evidence on SF proteomics in TMD and evaluate its potential translational value in precision medicine. Materials and Methods: A narrative review of the literature was conducted on PubMed to identify human studies focused on SF proteomic and biochemical biomarkers in TMD. Eligible studies included original research articles assessing SF composition in relation to specific TMJ pathologies, diagnostic categories, or clinical phenotypes. Extracted data included study design, sample characteristics, analytic methodology, biomarkers investigated, and key findings. Google Gemini (Google LLC, Mountain View, CA, USA) was used as an AI-assisted tool to support language editing and manuscript writing during the preparation of this article. The use of this tool was limited to linguistic refinement; all scientific content, data interpretation, and conclusions were formulated and verified by the authors. Results: Across the analyzed studies, TMD phenotypes—particularly disc displacement with or without reduction (DDwR, DDwoR) and osteoarthritis (OA)—were characterized by consistent alterations in cytokines (IL-1β, IL-6, IL-8, TNF-α), extracellular matrix (ECM) components (aggrecan, glycosaminoglycans (GAGs), decorin, MMP-2, MMP-9), lubrication molecules (lubricin/PRG4), oxidative stress mediators (myeloperoxidase (MPO), nitric oxide (NO), glutathione peroxidase (GPX)), adipokines (chemerin, resistin, adiponectin), and angiogenic factors (vascular endothelial growth factor (VEGF), fibroblast growth factor-2 (FGF-2)). Recent liquid chromatography–tandem mass spectrometry (LC–MS/MS) analyses further revealed phenotype-specific protein clusters and pathways related to inflammation, ferroptosis, hypoxia signaling, and proteoglycan metabolism. Conclusions: Current evidence suggests that SF proteomics and multi-analyte biomarker profiling offer a promising, hypothesis-generating approach for understanding the biological mechanisms underlying TMD. The integration of proteomic, metabolic, and inflammatory markers holds future potential for diagnostic panel development; however, prospective clinical validation is still required before SF-based molecular profiling can be implemented as a precision medicine tool in TMJ disorders. Full article

A multi-analytical investigation was carried out to elucidate the deterioration processes affecting the stone materials of the Arca di Cansignorio della Scala in Verona (Italy) and to characterize the surviving traces of its original polychrome and gilded decoration. The study combined macroscopic mapping, stratigraphic sampling, optical microscopy (OM), environmental scanning electron microscopy coupled with energy-dispersive X ray spectroscopy (ESEM-EDS), X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and ion chromatography (IC). The monument, predominantly carved from Candoglia marble, exhibits three principal weathering patterns: (i) rain washed areas affected by marble decohesion, (ii) grey deposits corresponding to dirt accumulation areas; and (iii) sulphation-induced black crusts developed in dirt wetting areas. In addition, severe mechanical deterioration was found to be associated with early twentieth-century structural consolidation interventions involving embedded iron bars, whose corrosion-driven volumetric expansion generated vertical cracking. Stratigraphic and microanalytical investigations revealed the presence of original azurite-based polychromy, proteinaceous and lipidic binding media, lead white preparatory layers, and multiple applications of gold leaf. The analytical results highlight the complex interplay between environmental exposure, atmospheric pollution, the incompatibility of materials introduced during past restorations campaigns. Furthermore, they contribute to a better understanding of the composition, execution techniques and preservation state of the surviving decorative layers, providing a scientific basis for future conservation strategies. Full article

This systematic research was conducted as the first comprehensive scientific analysis of ancient lime plaster samples from Anuradhapura, a World Heritage Site in Sri Lanka. Five ancient heritage sites from 1st to 10th Century AD, covering two stupa domes: Abhayagiri (AP01) and Jethavana (AP02), Monk residence building near Ruwanweliseya Stupa (AP03), Deeghapashan Rock Shelter Building of Abhayagiri Monastery Complex (AP04), and Vessagiriya Rock Shelter wall lime Plaster (AP05) were examined by employing Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), X-ray fluorescence (XRF), thermogravimetric analysis (TGA), optical microscopy (OM), scanning electron microscopy (SEM) and gas chromatography-mass spectrometry (GC-MS). The current work investigated the composition, mineralogical and microstructural properties, binding media, and organic additives. Our findings indicate that calcareous lime from seashells and river sand are the main raw materials, with ratios of 1:2.7, 1:2.0, 1:2.4, 1:4.4, and 1:3.7 for the AP01, AP02, AP03, AP04, and AP05 samples, respectively. Data also suggest that plant-based materials, mainly wood apple wax, along with nanoscale fibrous materials, were used as the main additives to enhance the properties of lime plasters. This study provides insights into the raw materials, their mixing ratios, and the techniques employed in the lime plastering of ancient Anuradhapura City, and serves as a scientific reference for the conservation and restoration of ancient buildings resilient to climate change. Full article

Inborn errors of metabolism (IEMs) are a group of inherited genetic conditions that, in general, result from a specific enzyme defect. Clinical consequences caused by abnormal enzyme levels often disrupt affected metabolic pathways and their intermediary metabolites. Because diagnostic outcomes depend on early intervention, a timely and accurate diagnosis is essential. Quantitative targeted metabolomics (QTM) is an analytical approach that quantifies predefined metabolites and generates interpretable biochemical phenotypes. Instead of focusing solely on screening, expanded QTM methods enable higher coverage with multi-analyte profiling that can provide more comprehensive characterization of disease-associated metabolic perturbations, particularly in IEMs with overlapping biochemical profiles. This review summarizes diagnostic techniques for IEMs, outlines the principles and advantages of QTM, and evaluates its established role and emerging opportunities and limitations in advancing method development and deep metabolic phenotyping to support precision medicine. Full article

Silk fabrics and caftans preserved in the Topkapı Palace Museum collection constitute a distinguished group of cultural heritage objects reflecting the advanced weaving technologies, refined metal-thread use, and sophisticated natural dyeing practices of Ottoman court textile production. In this study, selected ceremonial caftans attributed to five Ottoman sultans were examined through a multidisciplinary and multi-analytical approach to characterize their structural, chromatic, and chemical properties. Color characteristics were evaluated in the CIE L*a*b* color space, while yarn properties, weave structures, and production techniques were investigated by optical microscopy. The morphology and elemental composition of the metal threads were analyzed using scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy (SEM–EDX), and dyestuffs were identified by high-performance liquid chromatography with diode-array detection (HPLC–DAD). The results show that compound silk weaving structures were widely used in Ottoman court textiles, metal threads were predominantly silver-based and often gold-gilded, and dyestuffs with high fastness properties were preferentially selected. The revised manuscript situates these findings within a broader international literature on historical textile analysis and natural dye characterization, while using only a limited number of directly relevant studies from the authors’ previous work. The present study therefore provides new, object-specific and comparable data for the scientific documentation, material characterization, and conservation-oriented understanding of Ottoman textile heritage. Full article

This study presents a multi-analytical investigation of two Baroque gilded terracotta sculptures—Hercules and the Nemean Lion (Hercules A) and Hercules and the Lernaean Hydra (Hercules B)—attributed to Lorenzo Vaccaro (1655–1706) and preserved at the Museo Civico Gaetano Filangieri in Naples. This research aimed to reconstruct the original manufacturing technique, characterize materials introduced by successive restoration interventions, and identify active degradation mechanisms. A systematic diagnostic approach integrating UV fluorescence imaging, digital optical microscopy, portable energy-dispersive X-ray fluorescence spectroscopy (EDXRF), Raman spectroscopy, Fourier-transform infrared spectroscopy in attenuated total reflectance mode (FTIR-ATR), scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDS), and spectrocolorimetry was applied. The original gilding system—comprising a ferruginous silico-aluminous terracotta substrate, a calcium sulfate ground, a lead-white imprimitura, an iron-rich bole, and a thin gold leaf—is consistent with documented Baroque mission gilding practices in Southern Italy. Analytical evidence further documented extensive non-original interventions, including copper-based artificial patination, bronze powder (porporina) integration, poly (vinyl acetate) adhesives, and acrylic protective coatings. Raman spectroscopy identified the in situ conversion of intentionally applied tenorite (CuO) to malachite (Cu₂CO₃(OH)₂) as an active degradation pathway. Spectrocolorimetric measurements quantified chromatic alterations of up to ΔE = 52 attributable to accumulated surface deposits. The proposed integrated methodology constitutes a replicable diagnostic framework for investigating gilded terracotta artefacts in museum collections. Full article

This work presents the results of an archaeometric research study of the geomaterials used in the construction of the Late Antique wall of Emerita Augusta (currently Mérida, Spain). Dated to the 5th century C.E., this structure belongs to one of the best-preserved historical ensembles in Europe. In-depth knowledge of the geomaterials used in this ancient wall is essential for ensuring reliable restoration strategies and the successful long-term conservation of this monument. To this end, a rigorous sampling procedure was conducted in areas containing original archaeological remains. Samples were characterized using optical microscopy, X-ray diffraction (XRD), X-ray fluorescence (XRF), inductively coupled plasma–mass spectrometry (ICP-MS), thermogravimetry and differential thermal analyses (TGA-DTA), and scanning electron microscopy (SEM). This integrated multi-analytical approach is highly effective for the study of built heritage. The mineralogical, textural, and geochemical properties of the granites allowed for the identification of the granite types used in the wall, while the results obtained for the mortars indicated that lime, fully carbonated and transformed into calcite, was used as the binding agent. Furthermore, the binder/aggregate ratios were found to be consistent with traditional Roman mortar formulations. These findings provide a comprehensive understanding of the material provenance and construction techniques used in this landmark of late antiquity. Full article

Mesenchymal stromal/stem cells (MSCs) are increasingly explored for immune-mediated diseases, yet standardized analytical readouts that capture coordinated immunomodulatory output across complementary secretory pathways remain limited. Here, we report the feasibility of an HPLC-based multi-analyte secretome characterization panel that quantifies two small-molecule outputs—adenosine and kynurenine—alongside two immunomodulatory proteins—interleukin-10 (IL-10) and transforming growth factor-beta (TGF-β)—in conditioned media from canine adipose-derived MSCs (cAD-MSCs). Canine immune-mediated hemolytic anemia (IMHA) was used as a disease context to motivate the selection of these analytes, given the pro-inflammatory cytokine environment characteristic of this condition. Three independent cAD-MSC lines were evaluated under baseline conditions and following cytokine stimulation with recombinant interferon-gamma (IFN-γ; 100 ng/mL) and tumor necrosis factor-alpha (TNF-α; 50 ng/mL), referred to herein as inflammatory priming or licensing. Conditioned media were collected at 72 h for metabolite analysis and 48 h for protein analysis, and quantified by HPLC using external calibration and peak integration. Across all three lines, licensing produced directionally consistent increases: mean adenosine increased 2.3-fold, mean kynurenine increased 3.1-fold, mean IL-10 increased 1.6-fold, and mean TGF-β increased 1.7-fold compared with unlicensed controls. Metabolite measurements for adenosine and kynurenine are reported with full chromatographic selectivity data; IL-10 and TGF-β measurements by reversed-phase HPLC with UV detection are presented as exploratory/semi-quantitative outputs and will require orthogonal confirmation (e.g., immunoassay) in future work. These findings are preliminary, derived from three independent donor lines with no comparator group, and are intended to support feasibility of the analytical framework rather than establish definitive performance specifications. Collectively, the data support the potential of a multi-analyte HPLC-based characterization panel to capture licensing-responsive secretory shifts across mechanistically complementary pathways, providing a foundation for expanded development and validation. Full article

Electric energy metering cabinets serve as critical nodes in power grid operations, providing essential protection for key components in distribution networks. Under environmental stressors, the non-metallic casings of electric energy metering cabinets are susceptible to aging-induced performance degradation, which may result in electrical safety hazards. However, rapid and precise methods for evaluating the performance of these non-metallic casings are still lacking. Laser-Induced Breakdown Spectroscopy (LIBS), capable of rapid multi-element detection with non-contact analytical advantages, was employed in this study. Thermal aging experiments were conducted to investigate the performance degradation mechanisms of sheet molding compound (SMC)—a representative non-metallic cabinet material. The research analyzed time-dependent trends in material performance and microstructural evolution during aging. By integrating LIBS with multi-analytical techniques, this study further explored the feasibility of quantitatively evaluating the bending strength of thermally aged SMC, which has rarely been reported in previous studies. Based on LIBS spectral data, bending strength characterization revealed its attenuation patterns with aging duration. The relationships between bending strength and plasma temperature, as well as the characteristic line intensity ratios of K, Al, and Ca, were systematically examined. A multivariate linear regression model incorporating these key variables was subsequently developed, yielding a high coefficient of determination (R² = 0.9657) between the predicted and measured bending strength values. This model represents a promising initial step, but further validation with a larger dataset is necessary to enhance its reliability and generalizability. Full article

Although polylactic acid (PLA) and acrylonitrile–butadiene–styrene (ABS) are among the most widely used polymers in material extrusion, their limited toughness and energy-absorption capacity often restrict the structural performance of 3D-printed functional components. To address the limited comparative understanding of how thermoplastic polyurethane (TPU) modifies the deformation behavior and phase characteristics of these two polymer systems, this study presents a multi-analytical evaluation of TPU-reinforced PLA and ABS blends. To this end, both polymers were blended with TPU at 10–50 wt% and processed into filaments via single-screw extrusion. The resulting filaments were used to fabricate ASTM D638 Type I tensile specimens via material extrusion under matrix-specific, but internally consistent, printing parameters. For each composition, five specimens were tested to obtain representative values of tensile strength, elongation at break, and toughness. In addition to conventional tensile testing, the evolution of strain during deformation was monitored using digital image correlation (DIC), enabling full-field characterization of local deformation behavior. To ensure experimental reliability, specimen masses were carefully controlled, and the datasets were analyzed using MATLAB. Thermal properties were investigated by differential scanning calorimetry (DSC) to determine the influence of TPU on glass transition, melting behavior, and phase mobility, and to relate these thermal characteristics to the mechanical response of the blends. The incorporation of TPU significantly increased ductility and energy absorption in both polymer matrices, although the magnitude of improvement differed. ABS/TPU blends exhibited the highest toughness enhancement, reaching 221.4% at 30 wt% TPU, while PLA/TPU systems showed nearly a twofold increase at 20 wt% TPU. DIC analysis further revealed a transition from localized brittle deformation in neat polymers to more distributed plastic deformation with increasing TPU content. DSC results indicated reduced crystallinity in PLA-rich blends and enhanced segmental mobility in ABS-based systems, consistent with the observed mechanical behavior. Overall, the combined mechanical, optical, and thermal analyses demonstrate that the optimal TPU content is matrix-dependent, providing practical guidelines for tailoring PLA- and ABS-based filaments to achieve a controlled balance between stiffness, ductility, and energy absorption in material extrusion applications. Full article

The efficient recovery of coalbed methane (CBM) is critically constrained by the inherent low permeability of coal reservoirs, a challenge predominantly attributed to mineral blockages within the pore-fracture structure. In this study, the deashing efficacy of several acid solutions (HCl, HNO₃, HF, and CH₃COOH) on bituminous coals from the Yushuwan (YSW) and Jiangna (JN) mines was initially assessed to determine the optimal acidizing system. Subsequently, the multi-scale evolution of pore-fracture structures and the fractal characteristics of coal samples treated with the optimized acids were systematically investigated. A multi-analytical approach, integrating scanning electron microscopy (SEM), X-ray diffraction (XRD) with microcrystalline peak-fitting, and low-temperature nitrogen gas adsorption (LT-N₂GA), was employed to quantitatively elucidate the underlying transformation mechanisms. The experimental results indicate that HCl and HNO₃ emerged as the most effective agents for the YSW and JN coals, respectively. Optimized acidification achieved significant reductions in ash content (specifically, an ash removal efficiency of 83.99% for HCl-treated YSW coal) through the selective dissolution of carbonate and clay minerals, thereby facilitating the exposure of the organic matrix and the induction of extensive dissolution pits and secondary fractures. Although the dissolution-induced collapse of mineral-supported fine pores led to a reduction in both total pore volume and BET specific surface area, the average pore diameter undergoes a substantial increase (e.g., nearly doubling from 9.0068 nm to 16.5126 nm for the JN coal). Furthermore, the reduction in Frenkel–Halsey–Hill (FHH) fractal dimensions (D₁ and D₂) indicates a decrease in pore-surface complexity and structural heterogeneity. These findings reveal that optimized acidification induces significant alterations in pore structure and mineral composition. The treatment facilitates the conversion of isolated pores into interconnected networks, accompanied by an increase in pore volume and a shift in pore size distribution toward larger dimensions. This research elucidates the mechanisms of mineral dissolution and pore expansion, providing a fundamental characterization of the microstructural evolution of coal in response to acid treatment. Full article

The utilization of brown rice from long-term stored paddy is severely limited by lipid deterioration, which is primarily characterized by a high free fatty acid value (FAV). Although microwave treatment shows promise in mitigating lipid deterioration, its underlying mechanism in degraded grains remains poorly understood. This study systematically investigated the efficacy and mechanism of microwave treatment using a multi-analytical approach. Brown rice from long-term stored paddy (Longjing-46, stored for 6 years) was treated using a laboratory microwave oven (420 W or 560 W, 1–5 min). The reduction in FAV was quantified, lipid structural changes were analyzed by FT-IR spectroscopy, and lipid metabolic alterations were profiled using untargeted lipidomics. Results showed that microwave treatment significantly reduced FAV in a time- and power-dependent manner, with a maximum reduction of 76.3%. Treatment at 420 W for 4 min was identified as the optimal condition. FT-IR analysis confirmed that the treatment inhibited lipid oxidation and hydrolysis at the molecular level. Importantly, lipidomics revealed that the mechanism extended beyond simple enzyme inactivation. Microwave treatment induced a reprogramming of the lipid metabolic network, characterized by the synergistic downregulation of key lipid species and the activation of the autophagy pathway. This study provides a comprehensive, lipid-centric explanation of microwave-mediated quality improvement in long-term stored brown rice, integrating enzyme inactivation with metabolic network reprogramming. The findings offer a novel scientific basis for applying this technology to valorize degraded grain stocks, contributing to the reduction in postharvest loss. Full article

Background/Objectives: Systemic lupus erythematosus (SLE) is a chronic autoimmune disease characterized by fluctuating disease activity and multi-organ involvement. The identification of reliable biomarkers that accurately reflect disease activity remains a significant clinical challenge, particularly in predicting disease flares. Chemokines are key mediators of immune cell recruitment and inflammation, making them promising candidates for disease activity monitoring. Therefore, we evaluated serum concentrations of CCL2, CCL4, CCL5, CXCL8, and CXCL10 and examined their associations with disease activity and clinical manifestations in patients with SLE. Patients and Methods: A total of 52 patients with SLE were enrolled in the study, of whom 15 (28.8%) had active disease (SLE Disease Activity Index [SLEDAI] ≥ 5) and 37 (71.2%) were in remission (SLEDAI < 5). An additional group of 12 age- and sex-matched healthy individuals without a family history of autoimmune diseases served as controls. All SLE patients fulfilled the 2019 EULAR/ACR classification criteria. Serum levels of the selected chemokines were measured in all participants using the Luminex Human Premixed Multi-Analyte Discovery Assay. Results: Serum concentrations of CCL2 and CCL4 did not differ between SLE patients and healthy controls, nor between active and inactive disease subgroups (p > 0.05, for all). In contrast, CCL5 levels were 34.30% higher in patients with SLE compared with controls (p = 0.013), with the strongest increase observed in the inactive disease subgroup as compared to controls (by 40.29%, p = 0.021). CXCL8 levels were markedly elevated in patients with active SLE relative to those in remission (by 123.30%, p = 0.011) and to healthy individuals (by 183.96%, p = 0.049). CXCL10 levels were higher in both active and inactive SLE groups compared with controls (increase of 180.80%, p < 0.001 and increase of 100.80%, p = 0.018, respectively). No differences in chemokine levels were detected between patients with renal flares and those with non-renal flares, nor among patients in remission with and without a history of lupus nephritis (p > 0.05, for all). CXCL8 and CXCL10 correlated positively with disease activity scores, inflammatory markers, and several immune parameters, indicating their relevance to ongoing inflammatory processes (p < 0.05, for all). CCL5 was associated with complement components C3 (r_S = 0.36, p = 0.008) and C4 (r_S = 0.38, p = 0.006), while CXCL10 showed negative correlations with white blood cell (r_S = −0.34, p = 0.013), lymphocyte counts (r_S = −0.36, p = 0.008) and neutrophils (r_S = −0.32, p = 0.019). In the longitudinal follow-up of patients in remission (median follow-up time of 5.5 years), baseline chemokine levels did not predict subsequent disease flares among SLE patients who were inactive as the study baseline (p > 0.05, for all). Conclusions: In our study, serum levels of CXCL8 and CXCL10 reflect disease activity and systemic inflammation in SLE, supporting their potential value as biomarkers for monitoring ongoing immune activation. Baseline concentrations of the examined chemokines did not predict future disease flares, indicating their limited utility in this context. Full article

“Heijin” (the literal translation from Chinese being “Black Gold”) seal stone represents a unique variety of sulfur-rich, dickite-dominant jade, yet its mineralogical genesis and structural properties remain insufficiently characterized. This study utilizes a multi-analytical approach comprising polarized light microscopy, X-Ray diffraction (XRD), Raman spectroscopy, Fourier-transform infrared spectroscopy (FTIR), Scanning Electron Microscopy coupled with Energy-Dispersive X-Ray Spectroscopy (SEM-EDS), Electron Probe Microanalysis (EPMA), and Thermogravimetry and Differential Scanning Calorimetry (TG-DSC) to investigate the phase composition, crystalline order, and thermal evolution of this material. The results demonstrate that “Heijin” stone is primarily composed of highly ordered 2M₁ dickite with a Hinckley index (HI) ranging from 0.92 to 1.50. Its distinctive black appearance originates from the disseminated distribution of micrometer-scale pyrite, which is accompanied by trace amounts of svanbergite. This aluminum phosphate–sulfate (APS) mineral serves as a critical indicator of high sulfur fugacity and acidic hydrothermal alteration environments. Furthermore, a significant correlation exists between the crystalline order of dickite, its micro-morphology, and its thermal stability. Samples characterized by high crystallinity (HI ≈ 1.50) exhibit well-developed, euhedral book-like aggregates and elevated dehydroxylation temperatures (T_m ≈ 665 °C), whereas samples with lower crystalline order correspond to fragmented microstructures and reduced thermal stability. This research defines the mineralogical identity of “Heijin” stone and provides a scientific basis for employing thermal analysis to evaluate the crystalline quality of dickite-based jade materials. Full article

Rosin, a renewable natural resin derived from pine trees, is a promising biomass material for sustainable product development, though its distinct intrinsic odor limits broader use. This study implemented a comprehensive analytical strategy to mitigate the odor by incorporating essential oils (EOs)—eucalyptus (EUC) and peppermint (MINT)—and to conduct a multi-analytical characterization of the modified rosin jewelry. By integrating complementary analytical techniques, including LC-Q/TOF-MS for non-volatile components and GC-Q/TOF-MS for volatile organic compounds (VOCs), we achieved a systematic chemical profiling of the materials. The core composition of rosin, dominated by abietic acid (>48%), remained stable across all samples. The incorporation of EOs significantly altered the VOC profiles: The total VOC signal (summed peak area) in MINT-modified rosin was 2.57-fold that of the EUC-modified sample, with monoterpenoids comprising 87.62% of its VOC signature. Eucalyptol and limonene were tentatively identified as the major components in the EUC sample, whereas menthone, menthol, and limonene predominated in the MINT sample. Multivariate statistical analysis highlighted that variations in specific VOCs—particularly menthone, menthol, eucalyptol, and allo-ocimene—were closely associated with differences in the scent profiles of each modification. This work illustrates how a multi-technique analytical strategy can both guide and assess the functional modification of sustainable biomass materials. The findings offer a practical approach to improving rosin’s functional properties while providing a methodological framework for the integrated characterization of complex biomaterials, supporting the development of eco-friendly products aligned with green chemistry and sustainable design principles. Full article