Search Results (414)

To analyze the phytogenic components of honey of Amorpha fruticosa L. (AFH) and establish a targeted quantitative method, the liquid chromatography-mass spectrometry (LC-MS) based metabolomic technology was used in this study. Firstly, high performance liquid chromatography—quadrupole time-of-flight mass spectrometry (HPLC-QTOF-MS) untargeted metabolomics technology was used to screen candidate markers by comparing AFH metabolites with plant chemicals of Amorpha fruticosa L. Afterward, high performance liquid chromatography—triple quadrupole tandem mass spectrometry (HPLC-QQQ-MS/MS) was used to verify and identify the candidate markers, confirming ononin as the characteristic phytogenic marker of AFH, and determining its content range in AFH as 76.84–93.27 μg/kg (absent in acacia, rape, jujube, and Galla chinensis honey). Then, network pharmacology and molecular docking techniques were adopted to explore the gastric protective mechanism of ononin, and the results showed that ononin strongly binds AKT1 (binding free energy −8.0677 kcal/mol). Using the established method, the LC-MS analytical method for ononin in honey established in this study may be used for the authenticity identification of the characteristic phytogenic markers of AFH. Full article

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/Objectives: Lamiaceae species are valuable sources of bioactive natural products, often associated with anti-infective properties. This study investigated chemical composition and bioactivities of dry hydroethanolic extracts and essential oils from Micromeria nervosa (Desf.) Benth. aerial parts from two localities. Methods: Extracts and essential oils were analyzed using LC-DAD-QTOF-MS/MS and GC-FID/MS, respectively. Antimicrobial activity was assessed against 14 strains (microdilution method), and antiviral activity against three viruses by determining cytopathic effects, viral titers (end-point dilution assay) and viral loads (qPCR/RT-qPCR). Cytotoxicity was evaluated on three cancer cell lines (MTT assay) and antioxidant potential using three colorimetric tests. Composition–activity correlation was statistically analyzed; in silico molecular docking/dynamics simulations were performed. Results: Thirty-five compounds were annotated in extracts, including 30 reported for the first time in this species, with rosmarinic acid as the main component. Essential oils contained 31 constituents, dominated by carvacrol. Newly detected phenolics included lithospermic acid and several salvianolic and clinopodic acids. Extracts and oils exhibited notable antibacterial activity, especially against five Gram-positive strains (MIC = 0.313–2.5 mg/mL), and oils showed marked anticandidal effects (MIC = 0.313–0.625 mg/mL) and enhanced cytotoxicity against colon, gastric and hypopharyngeal cancer cells (selectivity indices ≥ 1.66). Extracts displayed potent antiviral activity against human herpesvirus 1 (HHV-1) and adenovirus Ad5, reducing cytopathic effects and viral titers, with qPCR revealing decreased HHV-1 load. In silico analysis suggested HHV-1 glycoprotein D binding. Extracts also showed strong antioxidant potential. Conclusions: These findings demonstrate that M. nervosa is a rich source of compounds with antimicrobial/antiviral, cytotoxic and antioxidant activities, warranting further research. Full article

Camellia hakodae Ninh flowers are an endemic Vietnamese species with limited phytochemical and biological characterization. This study aimed to characterize the phytochemical profile and evaluate antioxidant and anti-inflammatory activities of the total flower extract. Ultrasonic-assisted extraction (UAE) and maceration with methanol and ethanol at different concentrations were carried out to evaluate the efficiency of extracting total phenolic content (TPC) and total flavonoid content (TFC), quantified by colorimetric assays, along with the antioxidant and anti-inflammatory activities of the resulting extracts. The highest TPC (94.9 ± 4.5 mg GAE/g) and TFC (3.1 ± 0.2 mg QE/g) were obtained using UAE with 70% methanol, while maceration with 70% ethanol showed comparable TPC values. The optimized extract exhibited strong antioxidant activity with an IC₅₀ of 29.06 µg/mL, close to that of ascorbic acid (28.16 µg/mL) and significant anti-inflammatory activity in the proteinase inhibition assay (IC₅₀ = 2.72 mg/mL) compared to acetylsalicylic acid (IC₅₀ = 3.16 mg/mL). GC-MS and LC-QTOF-MS/MS analyses revealed diverse metabolites, including phenolic acids, flavonoids, fatty acids, terpenoids, and nitrogen-containing compounds, with representative constituents, such as quinic acid, catechins, flavonol glycosides, and loliolide, providing strong chemical evidence for the observed bioactivities. This integrated study demonstrates that C. hakodae flower is a rich source of multifunctional bioactive compounds and highlights its strong potential for applications in nutraceuticals, functional foods, and cosmeceuticals. Full article

Kratom (Mitragyna speciosa Korth.) has gained increasing global attention due to its traditional use, psychoactive properties, and emerging therapeutic potential; however, concerns regarding adulteration, substitution, and inconsistent quality of commercial products necessitate robust authentication strategies. This study aimed to integrate DNA barcoding and comprehensive chemical profiling to authenticate kratom variants and discriminate them from closely allied Mitragyna species for quality control and forensic applications. Nine DNA barcoding regions were analyzed, alongside chemical characterization using UHPLC, GC–MS, and LC–MS/QTOF. Among the tested loci, the internal transcribed spacer (ITS) and ITS2 regions exhibited the highest interspecific variation and effectively distinguished kratom from allied species. UHPLC and GC–MS analyses confirmed that mitragynine was exclusively detected in kratom variants, with Kan Khiao exhibiting the highest content (94.33 ± 0.14 mg/g) when quantified against the mitragynine standard using UHPLC analysis. LC–MS/QTOF profiling revealed an alkaloid-rich chemotype in kratom dominated by mitragynine and 7-hydroxymitragynine, whereas M. diversifolia, M. hirsuta, and M. rotundifolia showed distinct profiles enriched in phenolic acids and flavonoid glycosides. Multivariate analyses further identified procyanidin B1, datiscetin-3-O-rutinoside, mitragynine, and 7-hydroxymitragynine as key discriminatory markers. Overall, the combined molecular and chemical workflow provides a robust framework for kratom authentication, supporting regulatory monitoring, quality assurance, and forensic identification of kratom materials. Full article

Species of the genus Stachys (Lamiaceae) are recognized for their ethnobotanical importance and chemical diversity. In this study, the essential oil (EOS) and solvent extracts of the endemic species Stachys sparsipilosa were investigated using integrated GC–MS and LC–ESI–QTOF/MS approaches. GC–MS analysis showed that identified constituents accounted for 94.62% of the total oil, with caryophyllene oxide, kauran-16-ol, and cubebol as major components. Targeted LC–MS analysis quantified prominent phenolic compounds, including chlorogenic acid, rutin, and hesperidin, while untargeted metabolomics tentatively annotated 168 metabolites belonging to phenolics, terpenoids, and other classes. Antioxidant capacity was evaluated using complementary in vitro assays, and enzyme inhibitory activities against α-amylase, α-glucosidase, tyrosinase, acetylcholinesterase, and butyrylcholinesterase were assessed in comparison with standard inhibitors. The extracts demonstrated measurable but generally moderate activities relative to the corresponding positive controls. The essential oil exhibited moderate, non-selective cytotoxic effects at relatively high concentrations, whereas solvent extracts showed limited activity within the tested range. Molecular docking analyses were performed as supportive tools to explore possible enzyme–ligand interactions. Overall, S. sparsipilosa displays a chemically diverse metabolite profile associated with composition-dependent bioactivities, providing a basis for further mechanistic and in vivo studies. 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

Background: In this study, we aimed to compare metabolomic profiles, biodistribution, and detoxification patterns of the novel SN-38 derivative NMe with irinotecan (IR), and to identify NMe-specific metabolites to evaluate its preclinical pharmacokinetic advantages. Methods: In vivo ADME studies were conducted for NMe, a 9-aminomethyl SN-38 derivative, and IR following a single intraperitoneal dose of 40 mg/kg in mice. Additionally, ADMET properties were predicted using ADMETlab and SwissADME tools for comparison. Levels of NMe and irinotecan absorbed into plasma, distributed to tissues, and metabolized were monitored in liver, lung, spleen, kidney, and stool samples at 15, 30, and 60 min post-administration. Tissue extracts were analysed using high-performance liquid chromatography (HPLC), liquid chromatography–electrospray ionization quadrupole time-of-flight-tandem mass spectrometry (LC-ESI-QTOF-MS), and nuclear magnetic resonance (NMR) techniques after lyophilization and reconstitution. We compared the metabolomic profiles of irinotecan and NMe. Results: We identified and confirmed NMe-specific metabolites, including 9-CH₂-S-cysteine conjugate, 9-CH₂OH, and NMe-formyl. Notably, novel irinotecan metabolites (IR-OH and IR-ΔE) were detected in small amounts in kidney samples. In some cases, two literature-known photodegradation products of irinotecan were present. NMe was found to quickly metabolize with different distribution to tissues, significantly greater to kidney and liver. Two SN-38 glucuronides, SN-38G(α) and SN-38G(β), were detected corresponding to α- and β-anomers. Where it was possible, NMe, IR and SN-38 were quantified using external calibration curves. In IR group, controlled and prolonged release of SN-38 was confirmed in all samples, yet SN-38G was observed in minority only in plasma, kidney, or lungs. In NMe groups, great relative amounts of SN-38 and SN-38G were detected. Greater content of SN-38G in NMe group than in irinotecan is expected to contribute to modulation and alleviation of some side effects in irinotecan-involved therapies, such as gastrointestinal toxicities (GIT). Conclusions: NMe shows a distinct metabolic profile characterized by rapid biotransformation, higher systemic glucuronidation of SN-38, and formation of unique metabolites, suggesting a potentially wider therapeutic window and reduced toxicity compared with IR. 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

Asparagopsis has gained global attention for its chemical properties and environmental applications. However, its two main species, Asparagopsis armata and Asparagopsis taxiformis, remain understudied, with limited information available regarding their bioactive potential, especially across their development. In this study, we examined the phenolic profiles and antioxidant potentials of gametophyte and tetrasporophyte life stages and compared differences between conventional solvent extraction (CSE) and ultrasound-assisted extraction (UAE), including total phenol content, total flavonoid content, determination of condensed tannins, and seven types of antioxidant activity detections such as DPPH and ABTS. In general, the phenolic compounds and antioxidant potential of the Asparagopsis species vary significantly at different life stages and under different extraction techniques. Among them, the phenolic profile and antioxidant capacity of A. armata were recorded as significantly higher than those of A. taxiformis, as reflected by its greater relative antioxidant capacity index scores. In our study, while UAE did not universally outperform CSE, species- and life stage-specific improvements were recorded. Moreover, LC-ESI-QTOF-MS/MS tentatively identified 24 phenolic compounds (17 in A. armata and 14 in A. taxiformis), pointing to a diverse bioactive profile. Overall, Asparagopsis species demonstrated marked variability in phenolic and antioxidant potentials across life stages and extraction techniques. Full article

Breast cancer is a highly heterogeneous malignancy, characterized by diverse genetic, epigenetic, and phenotypic variations, as well as by metabolic reprogramming and oxidative stress. Lipid peroxidation bioactive product 4-hydroxynonenal (4-HNE) plays a significant role in the development and progression of cancer. In this study, we quantified circulating 4-HNE-modified proteins and performed comprehensive untargeted metabolomic profiling of the patients’ plasma using LC-ESI-QTOF-MS and GC-EI-QMS, aiming to investigate systemic metabolic pathways associated with oxidative damage in breast cancer. Significantly elevated levels of 4-HNE-modified proteins were detected in breast cancer patients compared to healthy controls, accompanied by distinct metabolomic signatures enriched in lipid metabolism. Several metabolites, including specific long-chain fatty acids, exhibited significant correlations with circulating 4-HNE-modified proteins, suggesting an interaction between lipid peroxidation-driven protein modification and breast cancer-associated metabolic reprogramming. Overall, this study provides evidence of associations between systemic 4-HNE-mediated protein modification and altered metabolic profiles in breast cancer, highlighting oxidative stress–related metabolites as potential biomarkers and pointing to redox-metabolic crosstalk in breast cancer patients. 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

Schisandra is a plant whose fruit possesses high biological potential and beneficial health effects. The pharmacological properties of Schisandra are attributed to its bioactive components, primarily polyphenols and polysaccharides. This study aimed to obtain Schisandra fruit extracts (SCE) from different locations in China and Poland, as well as Schisandra polysaccharides (SPO), and to compare their chemical composition and selected biological activities. The prebiotic and antibacterial effects of SCE and SPO on lactic acid bacteria (LAB), human and foodborne pathogens, and gut microbiota were investigated. The chemical composition of the three Chinese SCE was similar, whereas SCE from Poland (SCE-PL) differed. The main bioactive compounds differentiating the Chinese SCE were quercetin, isorhamnetin, and nicotiflorin, while gamma-tocopherol and mevalonic acid distinguished SCE-PL, as indicated through LC-QTOF-MS/MS metabolomic profiling. All SCE and SPO promoted the growth of LAB strains, confirming their prebiotic potential and ability to serve as effective carbon sources for LAB. Additionally, all SCE inhibited the growth of certain pathogens, with S. chinensis extract from China showing the strongest activity, whereas SPO did not exhibit such activity. Variations in chemical composition among SCE and SPO contribute to differences in their prebiotic and antimicrobial activity, highlighting the importance of species and geographical origin in determining their functional properties. Full article