Search Results (274)

Actinidia arguta is a valuable plant resource known for its diverse bioactive constituents. However, organ-dependent metabolic variation remains insufficiently explored. In this study, an integrated approach combining LC–QTOF–MS-based metabolomic profiling, multivariate analysis, and phytochemical isolation was employed to investigate metabolic differences among fruits, leaves, and roots of A. arguta. Comparative LC–QTOF–MS profiling and principal component analysis (PCA) revealed clear organ-specific metabolic differentiation. The root extract formed a distinct cluster, primarily characterized by flavan-3-ol oligomers, including procyanidin dimers and a trimer. Targeted isolation and spectroscopic analysis identified these compounds as major constituents of the root. Quantitative analysis showed that the root exhibited the highest antioxidant activity (60.8 ± 6.2%) and total phenolic content (10.8 ± 0.7 mg GAE/g dried weight), followed by leaves and fruits, indicating significant organ-dependent variation. The enhanced antioxidant activity observed in the root extract was consistent with the enrichment of oligomeric procyanidins, which are known for their strong radical-scavenging capacity. These findings demonstrate pronounced organ-specific metabolic specialization in A. arguta, with the root characterized by a condensed tannin–dominant chemical profile. This study highlights the potential of root-derived procyanidins as bioactive natural products and provides a basis for their utilization in functional and phytochemical applications, as well as insights into plant defense-related metabolism. Full article

Background: Citrus components potentially suppress adipogenic differentiation and lipid accumulation, and exhibit anti-inflammatory and antioxidant effects. We hypothesized that the bioactive compounds in Citrus junos Sieb ex Tanaka (yuzu) fruit peel can alter the systemic metabolism and productivity of beef cattle. Methods: Japanese Brown (JBR) steers were fed with a diet supplemented with 2.5% yuzu peel during the last month of the finishing period. To investigate the effect of dietary yuzu supplementation (DYS) on beef and liver metabolism, we explored the metabolomic profiles of longissimus thoracis (LT, loin) muscle at 14 d postmortem using capillary electrophoresis (CE-TOF/MS) and high-performance liquid chromatography time-of-flight mass spectrometry (LC-TOF/MS). Results: The DYS treatment enhanced the beef fat score compared to that recorded in beef in the no-DYS (None) group (p = 0.050); however, the other carcass quality traits were not significantly different between the DYS and None groups. CE-TOF/MS and LC-TOF/MS revealed 242 and 107 annotated peaks, respectively, for the LT muscle. DYS significantly increased 9(S)-hydroxyoctadecadienoic acid (9-HODE, a beef flavor precursor), cyclo(-Leu-Pro), spermidine, asymmetric dimethylarginine, and 7α-hydroxycholesterol levels and reduced 2-ethylhydracrylic acid (2-EHAA), γ-tocopherol, coenzyme Q10 (CoQ10), sphingomyelin(d18:1/16:0), Cys-Gly, Tyr-Arg, and palmitoylcarnitine levels in postmortem LT muscle (p < 0.050). Concomitantly, in the fresh liver, DYS increased acetyl-CoA, 6-phosphogluconic acid, S-methylglutathione, ATP, ribulose 5-phosphate, and ADP levels and suppressed the content of thiamine, Ala-Ala, riboflavin, and ascorbate 2-sulfate (p < 0.050). Conclusion: Collectively, yuzu ingredients activated ATP production in the liver through the elevation of hepatic energy metabolism primarily in the citrate cycle and β-oxidation, and potentially altered muscle metabolism, including linoleic acid oxidation, FAD-mediated electron transport chain, and isoleucine catabolism, as demonstrated in the reduced accumulation of 2-EHAA and CoQ10 in DYS beef. Moreover, DYS likely affects the gut microbiome by enhancing the production of cyclo(-Leu-Pro), an antimicrobial dipeptide. Full article

Background/Objectives: This study provides the first comprehensive evaluation of the antioxidant, antimicrobial, and enzyme inhibitory activities of Onosma alboroseum subsp. alboroseum var. alboroseum, including a novel nanoformulation-based comparative assessment of its most active extract. The study further aimed to investigate whether nanoparticles modulate the biological performance of the extract. Methods: Antioxidant activity was assessed using DPPH, FRAP, and CUPRAC assays, and total phenolic content was determined by the Folin–Ciocalteu method. Antimicrobial activity was evaluated using agar well diffusion and microdilution assays, while enzyme inhibitory activities were assessed through anticholinesterase and anti-urease assays. The most biologically active extract was subjected to LC–QTOF–MS-based tentative metabolite profiling and subsequently formulated into nanoparticles for comparative biological evaluation. Results: Among the extracts studied, the methanol extract had the highest total phenolic content and demonstrated superior antioxidant, antimicrobial, and enzyme inhibitor activities. LC–QTOF–MS profiling indicated a phenolic-rich composition, with rosmarinic acid as the predominant compound based on relative peak area. The methanol extract was encapsulated within alginate nanoparticles for subsequent comparative biological assessment. While the crude extract showed superior activity in antioxidant assays, nanoparticles enhanced cholinesterase and urease inhibition (28.03% and 12.11%, respectively) and improved antibacterial efficacy in microdilution assays (MIC range: 3.13–12.5 µg/mL), although no inhibition was observed in agar diffusion tests. Conclusions: These findings indicate the first time that the methanol extract of Onosma alboroseum subsp. alboroseum var. alboroseum represents a phenolic-rich source of bioactive constituents and a nanoparticle formulation that can modulate specific biological activities depending on the assay system, highlighting the relevance of formulation strategy in phytochemical-based pharmaceutical applications. Full article

Crete’s rich heritage of indigenous wine grapes remains underexplored in terms of chemical composition, with many cultivars yet to be fully characterized. This study presents a comprehensive analysis of the phenolic profile of 67 monovarietal Cretan wines produced by 10 wineries (42 white, 25 red) from 12 varieties—eight white (Assyrtiko, Dafni, Malvazia, Melissaki, Moschato Spinas, Plito, Vidiano, and Vilana) and four red (Kotsifali, Liatiko, Mandilaria, and Romeiko). A targeted LC–QTOF–MS workflow covering 45 phenolic compounds (flavonoids and non-flavonoids) was applied. Varietal differences were assessed using heteroscedasticity-robust univariate statistics (Welch’s ANOVA with Games–Howell post hoc comparisons and effect-size estimation) and explored by multivariate analyses (PCA and HCA); cross-validated PLS-DA was used for descriptive classification, and MFA integrated the targeted phenolic matrix with classical indices (e.g., total phenolics, tannins, and color metrics). Red wines exhibited stronger variety-linked phenolic structuring than white wines, whereas white-wine differentiation was driven by a limited subset of marker phenolics. Given the central role of phenolic composition in overall wine quality, this study provides the first detailed phenolic characterization of 12 key indigenous Cretan grape varieties. Full article

This study used the QuEChERS method in combination with liquid chromatography–quadrupole-time-of-flight mass spectrometry (LC-Q-TOF/MS) to develop a method for simultaneous detection of 187 pesticides and 10 mycotoxins in Astragalus. The samples were extracted using an acetonitrile–water solution containing 5% formic acid, and the amount of purification materials was optimized through response surface methodology. The results show that 197 compounds exhibit good linear relationships within their respective linear ranges (R² > 0.995). The screening detection limits (SDLs) and the limits of quantification (LOQs) ranged from 0.001 to 0.02 mg/kg and 0.002 to 0.02 mg/kg, respectively. At the spiked levels of 1, 2, and 10 times LOQ, compound recoveries ranged from 61.5% to 118.9%, 67.1% to 119.6%, and 72.0% to 119.3%, respectively, with relative standard deviations (RSDs) all less than 20.0%. The intra-day precision and inter-day precision are less than 10% and 20%, respectively. This method was applied to detect 20 batches of commercially available Astragalus samples. Six compounds (three pesticides and three mycotoxins) were detected; the residues of aflatoxin and ochratoxin A in two batches exceeded the maximum residue limits and required attention. The established method is simple, rapid, and highly sensitive. It is also reproducible and meets the requirements for the accurate quantitative analysis of multiple pesticide residues and mycotoxins in Astragalus. Full article

Background: Liquid biopsy using bodily fluids enables noninvasive acquisition of diverse tumor-derived molecules for comprehensive characterization of tumor profiles. Metabolomic analysis, in particular, may accurately reflect disease pathogenesis and holds promise for clinical diagnostic applications. Objective: This study explored metabolic alterations associated with pancreatic ductal adenocarcinoma (PDAC) using non-targeted metabolomic analysis of pancreatic juice to construct a preliminary diagnostic model based on selected metabolites. Methods: Pancreatic juice samples were collected intraoperatively and postoperatively from patients undergoing pancreaticoduodenectomy for PDAC (n = 11) and from those who had non-PDAC diseases, including benign conditions such as chronic pancreatitis and non-pancreatic malignancies such as distal bile duct adenocarcinoma and ampullary adenocarcinoma (n = 14). Non-targeted metabolomic analysis was performed using LC-QTOF-MS. Data were processed using MS-DIAL and MetaboAnalyst, and components showing intergroup differences were selected via PLS-DA. A diagnostic model was constructed using logistic regression based on annotated metabolites. Results: PLS-DA identified 56 discriminative components, of which 19 were successfully annotated. One metabolite was notably increased and 22 were relatively decreased in pancreatic juice of patients with PDAC. Among known metabolites that tended to decrease were isocitric acid, citric acid, and several oxidized fatty acids. A tentative logistic regression-based diagnostic model using these selected metabolites showed moderate discriminative performance. Citric acid was included in the final three-variable model, suggesting its potential as a candidate marker for PDAC discrimination. Conclusions: Pancreatic juice reflects PDAC-associated metabolic changes and may contain candidate diagnostic biomarkers. Metabolites annotated in this study may have potential as novel markers, and further studies on unknown components could help advance PDAC diagnosis and treatment. Full article

Isoniazid (INH) is an antitubercular drug that exhibits high toxicity in dogs due to the absence of N-acetyltransferase activity in this species. Consequently, it has been implicated in both accidental and intentional poisonings in dogs. The aim of this study was to develop and validate an analytical method for the quantification of INH in canine liver samples and to apply it in the forensic investigation of seven suspected poisoning cases. The method, based on liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (LC-QTOF-MS), enabled both accurate INH measurement and analysis of the molecular pattern of its metabolite formation. In addition, histopathological examination of the stomach, pancreas, liver, and brain was performed. Liver INH concentrations ranged from 11.822 to 30.484 μg/g and were associated with extensive necrotic lesions across all examined tissues. A strong signal for isonicotinic acid was observed in all samples, whereas the acetylated metabolite was negligible. The developed method allows precise quantification of INH in canine liver and facilitates identification of the characteristic molecular profile of its metabolites. 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

Sweet potatoes (Ipomoea batatas (L.) Lam.) are known for their anti-inflammatory effects, which are attributed to their phytochemical content. Our previous study revealed that ethanol extracts of sweet potato storage roots (SP-EtOH-Ex) inhibit interleukin-6 (IL-6) production in RAW264.7 cells stimulated with lipopolysaccharide (LPS). However, the causative compounds responsible for the anti-inflammatory effect have not yet been identified. This study aims to identify the compounds responsible for the anti-inflammatory effect of SP-EtOH-Ex using liquid chromatography–quadrupole time-of-flight mass spectrometry (LC-Q-TOF-MS). The unknown compounds were measured using the auto MS/MS mode (data-dependent acquisition; DDA) of LC-Q-TOF-MS, and the resulting data were analyzed using MS-DIAL and MS-FINDER and also compared with those of the corresponding reference standards in terms of retention time and fragment ions. As a result, β-sitosterol (2.527–4.850 µg/mL), campesterol (75.74–93.63 ng/mL), and lauroyl diethanolamide (4.568–9.260 ng/mL) were identified and quantified in SP-EtOH-Ex. Moreover, the anti-inflammatory effect of these three compounds against RAW264.7 cells was investigated at varying concentrations of β-sitosterol (1 µg/mL, 5 µg/mL, 10 µg/mL), campesterol (10 ng/mL, 100 ng/mL, 1000 ng/mL), and lauroyl diethanolamide (1 ng/mL, 10 ng/mL, 100 ng/mL). The phytosterols β-sitosterol and campesterol suppressed LPS-induced IL-6 production at concentrations comparable to those present in SP-EtOH-Ex. In contrast, lauroyl diethanolamide did not similarly suppress LPS-induced IL-6 production. These results suggest that β-sitosterol and campesterol in sweet potato storage roots contribute to their anti-inflammatory effects. The lack of activity in lauroyl diethanolamide further supports that phytosterols are the primary anti-inflammatory constituents. The edible portion of sweet potatoes holds promise as a promising raw material with anti-inflammatory properties. Full article

Contrast-induced acute kidney injury (CIAKI) has emerged as the third most prevalent etiology of clinically acquired acute kidney injury, with a lack of specific preventive and therapeutic strategies. Rubia Cordifolia L. (madder root), a medicinal herb with a long-standing history and extensive clinical application, exhibits multiple pharmacological activities. This study aimed to clarify the renal protective effect of Rubia cordifolia L. dichloromethane extract (RCDE) on CIAKI modeling rats and investigate potential anti-apoptotic and autophagy-inducing effects molecular mechanisms. In this study, RCDE constituents were identified by UPLC-Q-TOF-MS. A CIAKI rat model was established to evaluate the nephroprotective effect of RCDE. The results showed that RCDE high-dose group significantly decreased serum SCr and BUN levels, attenuated renal histopathological damage, and modulated oxidative stress markers by decreasing MDA and CAT while increasing SOD, compared with the model group. It downregulated the expressions of Bcl-2, caspase-3 and p62, upregulated the expressions of Bax, Beclin1 and reduced the LC3B-II/LC3B-I ratio in renal tissues. Molecular docking indicates that anthraquinone compounds are probably the principal active constituents of RCDE. This study provides experimental evidence for the intervention efficacy of RCDE against CIAKI. Full article

Background: Distinguishing between osteoarthritis (OA), rheumatoid arthritis (RA), and psoriatic arthritis (PsA) remains challenging despite different underlying mechanisms. Synovial fluid reflects metabolic changes within affected joints, yet comprehensive metabolomic comparisons across these conditions are limited. We aimed to identify disease-specific metabolic signatures in synovial fluid that could improve differential diagnosis and reveal therapeutic targets. Methods: We collected synovial fluid from 39 patients (20 OA, 5 RA, and 14 PsA) during routine knee arthrocentesis between January 2023 and February 2024. Following metabolite extraction, we performed untargeted metabolomic profiling using quadrupole time-of-flight liquid chromatography–mass spectrometry (Q-TOF LC/MS). Data underwent multivariate statistical analysis, including principal component analysis (PCA) and partial least squares–discriminant analysis (PLS-DA), to identify discriminatory metabolites. Results: While unsupervised analysis showed overlap between groups, supervised PLS-DA achieved clear metabolic separation. RA samples showed elevated itaconic acid, indicating inflammatory macrophage activation, and increased O-acetylserine, suggesting altered one-carbon metabolism. Hypoxanthine was decreased, which reflected severe metabolic stress. PsA exhibited the unique elevation of 4,4-dimethylcholestane and 2-oxoarginine. These metabolites have previously been unreported in this disease. OA demonstrated increased hippuric acid and indoleacetic acid, which are both gut microbiota products, supporting the gut–joint axis hypothesis. Conclusions: Each arthritis type displayed distinct metabolic fingerprints in synovial fluid. Candidate discriminatory metabolites, including gut-derived metabolites in OA and specific lipid alterations in PsA, open new diagnostic and therapeutic avenues. Given the limited RA sample size (n = 5), RA-related results should be viewed as exploratory and requiring validation in larger independent cohorts. These metabolites may, after rigorous validation in larger and independent cohorts, contribute to multi-metabolite biomarker panels for earlier diagnosis and to the rational design of targeted therapeutics addressing disease-specific metabolic disruptions. Full article

Recently, some cases of intentional animal poisoning using Carbofuran (CF) occurred in the Czech Republic, although CF is no longer available in the EU market. The present study describes a novel non-targeted analysis (NTA) workflow developed to possibly characterize 13 CF formulations from various sources to be certainly identified in real samples. Furthermore, a detection and quantification method for CF was developed for analyzing three animal samples, obtained from dead animals. The analyses were conducted using the liquid electron ionization (LEI) interface coupled with a quadrupole time-of-flight (QTOF) mass spectrometer, allowing the simultaneous characterization of the formulation’s volatile and low-volatile fractions. Almost all compounds detected in the different formulations were identified by comparing the experimental spectra with the NIST library at high probability values (95–99.38%). Determination of molecular ions, followed by MS/MS analysis, was performed to confirm compound identities at a high level of confidence. The quantification method for CF was successfully validated, showing negligible matrix effects (107%). CF was detected in two out of the three real samples. Only 3-keto-carbofuran was detected in one of the real samples; without any other marker, it was not possible to identify the specific formulation used in the three poisoning cases. Full article

Amazonian fruits are increasingly recognized for their functional properties due to their rich composition of bioactive metabolites. While species such as Euterpe oleracea Mart., Euterpe precatoria Mart., Mauritia flexuosa L., and Theobroma grandiflorum (Wild. ex Spreng.) have been extensively studied in countries like Brazil, research on these fruits in Colombia remains limited. This study aimed to characterize the secondary metabolites in freeze-dried pulp and seed samples of açaí, mirití, and cupuassu at different ripening stages, collected in Mitú (Vaupés, Colombia). Eleven samples of different fruits were collected and analyzed by untargeted metabolomics. Untargeted metabolomic profile was performed using LC-QTOF-MS and GC-QTOF-MS techniques. The pulp of M. flexuosa showed high concentrations of galacturonic acid. In T. grandiflorum, both pulp and seeds contained significant levels of galactose and citric acid. Notably, flavonoids such as fisetin and kaempferol-O-rutinoside were abundant in the pulp of E. oleracea and E. precatoria. Additionally, quinic acid and mannitol were detected in the unripe stages of Euterpe and Mauritia species. The diverse profile of secondary metabolites identified in these Colombian Amazonian fruits underscores their functional and nutritional potential. These findings support further exploration of native species for food, nutraceutical, and industrial applications, contributing to the valorization of Amazonian biodiversity. Full article

Background: Oxazolidinone derivatives are a novel class of synthetic antibacterial agents, characterized by a five-membered heterocyclic ring containing oxygen and nitrogen and a carbonyl functionality at position 2. This pharmacophore is responsible not only for antibacterial activity but also for a variety of other biological activities, including anticancer activity, anticoagulant activity, and several others. A series of novel oxazolidinone derivatives containing a hydroxamic acid moiety were synthesized in our laboratories and identified as potent inhibitors of the enzyme 5-lipoxygenase (5-LO), a key enzyme involved in the biosynthesis of leukotrienes (LTs). LTs are proinflammatory mediators implicated in allergic and inflammatory diseases. Currently, zileuton is the only FDA-approved 5-LO inhibitor, emphasizing the need to develop new agents for the treatment of such diseases. This project aims to develop validated stability-indicating analytical methods for the four most potent novel 5-(hydroxamic acid)methyl oxazolidinone derivatives (PH-211, PH-247, PH-249, and PH-251). Methods: The compounds were analyzed using Waters Acquity Ultra-High-Performance Liquid Chromatography (UHPLC-UV) with an ultraviolet detector to determine their stability in human plasma and under various forced degradation conditions, including acidic, basic, oxidative, and thermal conditions. Liquid chromatography–quadrupole time-of-flight mass spectrometry (LC-QToF-MS) was used to identify possible degradation products. Results: The compounds were found to be stable in human plasma and under thermal degradation conditions with high extraction recoveries (82–90%) but unstable in acidic, basic, and oxidative conditions. Conclusions: The findings show that the compounds are stable in biological conditions; they hold promise for the treatment of inflammatory and allergic diseases. Full article

Perilla frutescens Britton var. acuta Kudo leaves are widely consumed in East Asia due to their culinary and medicinal properties, which are largely attributed to their high levels of bioactive metabolites such as rosmarinic acid. In this study, we investigated the variation in rosmarinic acid content and overall metabolite profile of P. frutescens leaves collected from six different provinces in Republic of Korea. Quantitative analysis of the rosmarinic acid content was performed using HPLC, revealing significant regional differences, with the highest concentration observed in the leaves collected in Gyeongsangbuk-do and the lowest concentration in those from Jeollanam-do. HRESIMS and ¹H-NMR spectrometry were used to determine the chemical structure of the isolated rosmarinic acid. LC-Q-TOF/MS analysis identified ten major metabolites, including phenolic acids, flavonoids, and triterpenoids. Multivariate statistics (OPLS-DA) revealed distinct clustering of populations, indicating a strong relationship between metabolites and environmental parameters. The distribution of the metabolite fingerprints and rosmarinic acid contents in P. frutescens leaves were also found to differ according to the cultivation region, suggesting that secondary metabolite expression is influenced by environmental and geographic factors. This work shows that metabolome profiles can be used in quality control and the development of high-quality products derived from P. frutescens. Full article