Search Results (36)

Bamboo leaves contain structurally diverse flavonoid glycosides; whereas, compound-level information for Bambusa textilis remains limited. In this study, a flavonoid-enriched 40% ethanol fraction prepared from B. textilis leaves by petroleum-ether partitioning and AB-8 resin adsorption was analyzed by ultra-high-performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry (UHPLC-ESI-Q-TOF-MS/MS) in negative-ion mode. Retention times and MS/MS spectra were compared with seven in-house reference standards, while the remaining constituents were annotated from accurate-mass measurements, diagnostic product ions, fragmentation behavior, and data from the literature. According to Metabolomics Standards Initiative criteria, seven compounds were assigned at Level 1 and twenty-four were reported as Level 3 annotations because their exact positional structures were not confirmed by additional standards or NMR. Thirty-one flavonoid-related constituents were annotated in the analyzed fraction, encompassing six glycoside classes; most annotations, by count, were apigenin- or luteolin-derived. These annotations add compound-level information for the analyzed B. textilis fraction and allow qualitative comparison with other bamboo flavonoid profiles. Because the sample was selectively enriched, the results do not describe the complete leaf metabolome or compound concentrations. Additional standards or NMR analysis are needed to confirm the glycosylation positions of tentatively annotated compounds. Full article

Calophyllum spp. infusions are used to treat varicose veins, hemorrhoids, and hypertension. However, the chemical composition and mechanisms of action are poorly understood. Accordingly, the aim of this study was to investigate the phytochemical composition and vascular effects of hydroalcoholic extracts of Calophyllum longifolium. Phytochemical profiling was performed using ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UHPLC-ESI-Q-TOF-MS). Extract effects on rat aortic rings and aortic vascular smooth muscle cells (VSMCs) were evaluated using wire myography and photometric measurement of intracellular Ca²⁺, respectively. UHPLC-ESI-Q-TOF-MS revealed the presence of coumarins, xanthones, flavonoids, triterpenes, and phenolic acids. Coumarin–resveratrol hybrids, such as gut-70 derivatives, were also abundant. In aortic rings from normotensive rats, C. longifolium induced a biphasic vascular response whereby low concentrations (1 μg/mL) produced significant vascular relaxation, whereas high concentrations (100 μg/mL) produced contraction. Blockade of ATP-sensitive (K_ATP) or voltage-gated (K_V) potassium channels attenuated these effects. Furthermore, effects were not observed in preparations preincubated with L-NG-Nitro-L-arginine methyl ester (L-NAME) or in endothelium-denuded rings. In aortic VSMCs, extracts (1 µg/mL) rapidly reduced sarcoplasmic reticulum (SR) Ca²⁺ content. This study provides the first UHPLC-ESI-Q-TOF-MS chemical profile of C. longifolium, revealing diverse bioactive metabolites. It is also the first to demonstrate that C. longifolium exerts an endothelium-dependent, nitric oxide- and Ca²⁺-mediated biphasic effect on vascular function. Taken together, these findings highlight C. longifolium as a potential novel source of vasculotropic phytopharmaceuticals. Full article

The all-d-enantiomeric-peptide RD2 was developed for the treatment of Alzheimer’s disease. This study aimed to develop a specific and highly sensitive liquid chromatography-mass-spectrometric (UHPLC-ESI-QTOF) method for quantifying RD2 in the mouse brain and to validate it according to the ICH M10 guideline to investigate the pharmacokinetic profile of RD2 in its target organ. Sample preparation, chromatographic separation and quantification were very challenging due to RD2’s highly hydrophilic properties, the complex matrix and the required lower limit of quantification (LLOQ). Chromatographic separation was performed on an Acquity UPLC BEH C18 column (2.1 × 100 mm, 1.7 μm particle size) within 5 min at 50 °C with a flow rate of 0.5 mL·min⁻¹. Mobile phases consisted of water and acetonitrile with 0.2% formic acid and 0.015% heptafluorobutyric acid. Ions were generated by electrospray ionization in the positive mode, and RD2 was quantified by QTOF-MS. The developed extraction method revealed complete recovery. The linearity of the calibration curve was in the range of 2 ng·mL⁻¹ to 500 ng·mL⁻¹ (R² > 0.99) with a LLOQ of 5 ng·mL⁻¹. The intraday and interday accuracy and precision ranged from 0.4% to 12.2% and from 1.0% to 12.0%. RD2 remained stable in the freshly homogenized brain even after several freeze–thaw cycles, but stability decreased over time during long-term storage at −80 °C. Using this validated method, RD2-spiked brain homogenate samples and samples of a pharmacokinetic study with RD2 in mice were analyzed. Full article

This study aimed to characterize the chemical composition and evaluate the biological activities of the aerial parts of Alkanna corcyrensis Hayek (AC), an endemic Greek species not previously studied. Phytochemical analysis of the methanolic extract was performed using UHPLC-ESI-Q-TOF–MS/MS combined with molecular networking analysis. Additionally, the total phenolic content (TPC) and total flavonoid content (TFC) were determined. Chromatographic separations were carried out to isolate major compounds, and the antioxidant capacity, along with enzyme inhibitory activity, was assessed. The analysis led to the tentative identification of 86 compounds, including 67 phenolic compounds (mainly caffeic acid derivatives and flavonoid glycosides), 10 pyrrolizidine alkaloids of trachelanthamidine, platynecine, and retronecine types, and nine organic and fatty acid derivatives. Among these, one flavonol glycoside (kaempferol-O-malonyl methyl ester hexoside) and three pyrrolizidine alkaloids (9-sarracinoyl-trachelanthamidine/isoretronecanol, retronecine-pentoside, and trachelanthamidine/isoretronecanol-hexoside) were reported for the first time. The extract exhibited high TPC (74.45 mg GAE/g extract) and TFC (46.66 mg GAE/g extract). Chromatographic separations resulted in the isolation of five major metabolites, namely rosmarinic acid, danshensu, kaempferol-3-O-glucoside, kaempferol-3-O-galactoside, and quercetin-3-O-glycoside. Biological evaluation revealed considerable antioxidant activity and inhibitory effects against α-glucosidase (6.65 mmol ACAE/g extract). Overall, this study highlights the remarkable phytochemical diversity and richness of AC among alkanet species and demonstrates its promising antioxidant potential, laying the foundation for further investigations towards its future exploitation. Full article

American ginseng (Panax quinquefolius L.) is a rare and valuable plant utilized for medicinal and culinary purposes, with its geographic origin and cultivation significantly affecting its quality and efficacy. However, the metabolic differences between cultivated and wild American ginseng are not well understood. An accurate and reliable method for tracing the origin and evaluating the quality of American ginseng is therefore urgently required. This study introduces a UHPLC-Q/TOF-MS-based comparative metabolomics and machine learning strategy for the rapid identification of wild and cultivated American ginseng. Both principal component analysis and hierarchical cluster analysis revealed distinct metabolic phenotypes between wild and cultivated American ginseng. Furthermore, the integration of univariate and multivariate statistical analyses identified eight differential metabolites in the ESI⁺ mode and three in the ESI^- mode, including seven ginsenosides. A potential ginsenosides marker panel was used to construct five machine learning models to assist in diagnosing the metabolic phenotypes of American ginseng. The Random Forest model, based on the eight differential metabolites in the ESI⁺ mode, achieved a 100% classification rate in both test and validation sets for distinguishing between wild and cultivated American ginseng. This study highlights the feasibility and application of our artificial intelligence-driven comparative metabolomics strategy for cultivar identification and geographic tracing of American ginseng, offering new insights into the molecular basis of metabolic variation in cultivated American ginseng. Full article

Anemone baicalensis, a plant abundant in Northeast China, has garnered attention for its potential medicinal properties. While its aerial parts (ABAP) have demonstrated significant antioxidant activity, the rhizome (ABR) remains less explored, particularly in comparison to the well-documented Anemones raddeanae Rhizoma, a valuable traditional Chinese medicine. This study investigates the chemical composition and bioactivity of ABR, comparing it with ABAP and evaluating its potential as a substitute for Anemones raddeanae Rhizoma. Phytochemical analyses, including qualitative and quantitative assessments, were conducted on ABR extracts using various solvents. Antioxidant activity was evaluated through multiple assays, and stability studies were performed on methanol and 80% ethanol extracts. UHPLC-ESI-Q-TOF-MS was employed to identify chemical constituents. Acute toxicity and hepatoprotective effects were assessed in vivo using a rat model. The results revealed that ABR and ABAP share nearly half of their chemical components, with ABR containing a higher diversity of triterpenoid saponins. The 80% ethanol extract of ABR exhibited the highest extraction yield, rich in phenolics and triterpenoids, and demonstrated superior antioxidant activity and stability. In vivo studies showed that ABR significantly reduced liver injury markers (ALT, AST, $\gamma$-GT, and MDA), enhanced antioxidant enzyme activity (CAT), and increased albumin concentration, comparable to the effects of Anemones raddeanae Rhizoma. Acute toxicity tests indicated low toxicity, supporting its safety for medicinal use. ABR shows significant potential as a substitute for Anemones raddeanae Rhizoma, particularly due to its rich triterpenoid content and hepatoprotective effects. While ABAP outperforms ABR in terms of antioxidant activity, ABR’s unique chemical profile and liver-protective capabilities highlight its value in drug development. This study provides a scientific foundation for the further exploration of ABR as a sustainable alternative in traditional medicine. Full article

Diplopterys pubipetala (Malpighiaceae) is a liana native to the Brazilian Cerrado biome, traditionally used in Ayahuasca preparations. Despite its cultural importance, research on its chemical composition and biological activities, which may have therapeutic potential, is limited. This study investigated the volatile and non-volatile secondary metabolites of D. pubipetala leaves, their antioxidant capacity, and their antibacterial and antifungal activities. Volatile compounds were identified using gas chromatography-mass spectrometry (GC-MS) coupled to solid-phase microextraction (SPME), while non-volatile compounds were annotated using UHPLC-MS/MS-ESI-Q-TOF. Antioxidant capacity was evaluated by DPPH assay, and antimicrobial activity was assessed in vitro against Staphylococcus aureus, Escherichia coli, Pseudomonas aeruginosa, and Candida species (C. albicans, C. tropicalis, C. glabrata). GC-MS analysis revealed 25 predominant volatile compounds, including ethyl dodecanoate, ethyl tetradecanoate, nonanoic acid, and 5-methylhexan-2-one, with documented antifungal, antioxidant, and antimicrobial activities. The crude extract and ethyl acetate fraction showed strong antioxidant capacity (EC₅₀ 9.83 µg/mL and 6.42 µg/mL, respectively), and antifungal effects were observed against Candida species. This study provides the first comprehensive investigation of the antioxidant capacity and antibacterial and antifungal activities of D. pubipetala, together with a detailed chemical profile of its volatile compounds. Full article

Prosthechea karwinskii is an endemic orchid of Mexico with significant value for its traditional uses: ornamental, ceremonial, and medicinal. The pharmacological activity of this plant has been studied using specimens recovered from religious use during Holy Week in Oaxaca, Mexico, sourced from various localities within this state. Geographical variability can influence the chemical composition of plants, as environmental factors affect the production of their secondary metabolites, which impact their biological properties. This research evaluated the variability in the chemical composition of leaves and pseudobulbs of P. karwinskii obtained from different localities in Oaxaca, comprising 95–790 g and 376–3900 g of fresh material for leaves and pseudobulbs, respectively, per locality. Compounds were identified using UHPLC-ESI-qTOF-MS/MS following ultrasound-assisted hydroethanolic extraction. Twenty-one compounds were identified in leaves and twenty in pseudobulb. The findings revealed differences in chemical composition across localities and between leaves and pseudobulbs of the species. The Roaguia locality exhibited the highest extraction yield and pharmacological potential in leaves. For pseudobulbs, Cieneguilla specimens showed the highest yield, and El Lazo had the lowest yield but the highest pharmacological potential. This study represents the first comprehensive analysis of the variation in the chemical composition of a native Mexican orchid. In all localities, leaves and pseudobulbs contained compounds with known biological activity, validating the use of the species in traditional medicine and highlighting its potential for medical and biological applications. Full article

Prosthechea karwinskii is an endemic orchid of Mexico with cultural significance for its ornamental, food, religious, and medicinal uses. In traditional medicine, diabetic patients use the leaves of this plant to lower glucose levels. The present study evaluated the effect of P. karwinskii leaves extract on the antioxidant enzymes superoxide dismutase (SOD) and catalase (CAT) in a model of obese rats with insulin resistance for its nutraceutical potential to reduce insulin resistance and oxidative stress. Obesity and insulin resistance were induced with 40% sucrose in water for 20 weeks. Four groups (control rats, obese rats, obese rats administered the extract, and obese rats administered metformin) were evaluated. Extract compounds were identified by UHPLC-ESI-qTOF-MS/MS. Glucose, insulin, triglyceride, and insulin resistance indices (HOMA-IR and TyG), as well as the activity of the antioxidant enzymes, increased in rats in the obese group. Administration of P. karwinskii extract and metformin reduced glucose, insulin, triglyceride, and insulin resistance indices and antioxidant enzyme activity to values similar to those of the control group. Therefore, this study shows the nutraceutical potential of P. karwinskii extract as an ingredient in the formulation of dietary supplements or functional foods to help treat diseases whose pathophysiology is related to oxidative stress and insulin resistance. Full article

Verbascum sinaiticum (Qetetina or yeahya Joro) is a medicinal plant with secondary metabolites such as phenolics, flavonoids, glycosides, saponins, and alkaloids. This study was designed to optimize the ultrasonic-assisted extraction (UAE) parameters to enhance the phenolic content and characterize the phenolic compounds using ultra-high-performance liquid chromatography, coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry (UHPLC-ESI-QTOF-MS/MS), and antioxidant activities in Verbascum sinaiticum extract. Extraction time, sample-to-solvent ratio, and extraction temperature were considered for UAE optimization. It was found that UAE generated the highest extraction yield (21.6%), total phenolic content (179.8 GAE mg/g), total flavonoid content (64.49 CE mg/g), DPPH (61.85 µg/mL), and ABTS (38.89 µg/mL) when compared to maceration extraction. Metabolite analysis in this study showed the detection of 17 phenolic compounds, confirming antioxidant capacities. The optimization parameters have significant effects on phenolic compounds. Scanning electron microscopy showed the presence of structural changes when UAE was used over the maceration method. The optimized UAE parameters for extraction temperature (41.43 °C), sample-to-solvent ratio (36.32 g/mL), and extraction time (33.22 min) for TPC were obtained. This study shows the potential application for UAE of Verbascum sinaiticum leaves in the development of pharmaceutical and nutraceutical products. Full article

Phytophthora parasitica is an oomycete pathogen that infects a broad range of crops of worldwide economic interest; among them are citrus species. In general, some Citrus and the rootstocks of related genera offer considerable resistance against P. parasitica; therefore, understanding the mechanisms involved in the virulence of this pathogen is crucial. In this work, P. parasitica secondary metabolite production was studied using matrix-assisted laser desorption/ionization mass spectrometry imaging (MALDI-MSI) and ultrahigh-performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry (UHPLC/ESI-Q-TOF-MS) combined with chemometric tools, and its metabolic profile was evaluated under the influence of Citrus sunki (a highly susceptible host) and Poncirus trifoliata (a resistant genotype) extracts. The root extracts of Citrus sunki had an influence on the growth and hyphae morphology, and the root extracts of P. trifoliata had an influence on the zoospore behavior. In parallel, the spatial distribution of several metabolites was revealed in P. parasitica colonies using MALDI-MSI, and the metabolite ion of m/z 246 was identified as the protonated molecule of Arg-Ala. The MALDI-MSI showed variations in the surface metabolite profile of P. parasitica under the influence of the P. trifoliata extract. The P. parasitica metabolome analysis using UHPLC-ESI-Q-TOF-MS resulted in the detection of Arg-Gln (m/z 303.1775), as well as L-arginine (m/z 175.1191) and other unidentified metabolites. Significant variations in this metabolome were detected under the influence of the plant extracts when evaluated using UHPLC-ESI-Q-TOF-MS. Both techniques proved to be complementary, offering valuable insights at the molecular level when used to assess the impact of the plant extracts on microbial physiology in vitro. The metabolites identified in this study may play significant roles in the interaction or virulence of P. parasitica, but their functional characterization remains to be analyzed. Overall, these data confirm our initial hypotheses, demonstrating that P. parasitica has the capabilities of (i) recognizing host signals and altering its reproductive programing and (ii) distinguishing between hosts with varying responses in terms of reproduction and the production of secondary metabolites. Full article

Buds of poplar trees (Populus species) are often covered with sticky, usually polyphenol-rich, exudates. Moreover, accessible data showed that some Populus bud extracts may be excellent antibacterial agents, especially against Gram-positive bacteria. Due to the fragmentary nature of the data found, we conducted a systematic screening study. The antimicrobial activity of two extract types (semi-polar—ethanolic and polar—ethanolic-water (50/50; V/V)) from 27 bud samples of different poplar taxons were compared. Antimicrobial assays were performed against Gram-positive (five strains) and Gram-negative (six strains) bacteria as well as fungi (three strains) and covered the determination of minimal inhibitory, bactericidal, and fungicidal concentrations. The composition of extracts was later investigated by ultra-high-performance liquid chromatography coupled with ultraviolet detection (UHPLC-DAD) and with electrospray-quadrupole-time-of-flight tandem mass spectrometry (UHPLC-ESI-qTOF-MS). As a result, most of the extracts exhibited good (MIC ≤ 62.5 µg/mL) or moderate (62.5 < MIC ≤ 500 µg/mL) activity against Gram-positives and Helicobacter pylori, as well as fungi. The most active were ethanolic extracts from P. trichocarpa, P. trichocarpa clone ‘Robusta’, and P. tacamahaca × P. trichocarpa. The strongest activity was observed for P. tacamahaca × P. trichocarpa. Antibacterial activity was supposedly connected with the abundant presence of flavonoids (pinobanksin, pinobanksin 3-acetate, chrysin, pinocembrin, galangin, isosakuranetin dihydrochalcone, pinocembrin dihydrochalcone, and 2′,6′-dihydroxy-4′-methoxydihydrochalcone), hydroxycinnamic acids monoesters (p-methoxycinnamic acid cinnamyl ester, caffeic acid phenethylate and different isomers of prenyl esters), and some minor components (balsacones). Full article

This research was designed to investigate the metabolite profiling, phenolics, and flavonoids content as well as the potential nematicidal properties of decoction (ZpDe), orange-yellow resin (ZpRe) and essential oil (ZpEO) from Argentinean medicinal plant Zuccagnia punctata Cav. Additionally, the antioxidant and antibacterial properties of ZpDe and ZpEO were determined. Metabolite profiling was obtained by an ultrahigh-resolution liquid chromatography MS analysis (UHPLC-ESI-QTOF/OT-MS-MS) and GCMS. The nematicidal activity was assayed by a standardized method against Meloidogyne incognita. The antioxidant properties were screened by four methods: (2,2-diphenyl-1-picrylhydrazyl assay (DPPH), Trolox equivalent antioxidant activity assay (TEAC), ferric-reducing antioxidant power assay (FRAP), and lipid peroxidation in erythrocytes (ILP). The antibacterial activity was evaluated according to the Clinical and Laboratory Standards Institute (CLSI) rules. The ZpDe, ZpRe and ZpEO displayed a strong nematicidal activity with an LC₅₀ of 0.208, 0.017 and 0.142 mg/mL, respectively. On the other hand, the ZpDe showed a strong DPPH scavenging activity (IC₅₀ = 28.54 µg/mL); ILP of 87.75% at 250 µg ZpDe/mL and moderated antimicrobial activity. The ZpEO showed promising activity against a panel of yeasts Candida albicans and non-albicans (ATCC and clinically isolated) with MIC values from 750 to 1500 µg/mL. The ZpDe showed a content of phenolics and flavonoid compounds of 241 mg GAE/g and 10 mg EQ/g, respectively. Fifty phenolic compounds were identified in ZpDe by ultrahigh-resolution liquid chromatography (UHPLC–PDA– Q-TOF-MS) analysis, while forty-six phenolic compounds were identified in ZpRe by UHPLC-ESI-Q-OT-MS-MS and twenty-nine in ZpEO using a GC-MS analysis, updating the knowledge on the chemical profile of this species. The results support and standardize this medicinal plant mainly as a potential environmentally friendly and sustainable bionematicide for the control of Argentinean horticultural crops including tomatoes and peppers and as a source of antimicrobial and antioxidant compounds which could be further explored and exploited for potential applications. Full article

Objectives: We have previously shown that inhibition of the mTORC1 nutrient-sensing complex by rapamycin and mTORC1/mTORC2 inhibition by either Torin-2 or RapaLink-1 have differential effects on the global untargeted metabolomics in in vivo and in vitro cell culture models. Methods: In this study, we leveraged the mummichog Python algorithm to analyze the high-dimension untargeted metabolomics data to model the biochemical pathways and metabolic networks and predict their functional activity. We used pancreatic beta-cell culture (Beta TC6) and incubated the cells with either Rapalink-1, Rapamycin or the vehicle control for 24 h. Cells were harvested and flush-frozen in liquid nitrogen. Cells were extracted in ethanol, and the supernatant was collected. The untargeted metabolomics was performed using the high-resolution mass spectrometry LC-MS/MS HILIC peak detection of ESI-positive and -negative polarity modes. The data were collected using Bruker’s maXis-II ESI-Q-q-TOF coupled to Dionex Ultimate-3000 U(H)PLC system using Sequant ZIC-HILIC 150 × 2.1 mm column (Bruker, Hamburg, Germany). We compared the high-resolution untargeted precision metabolomics (LC-MS/MS) between groups using positive and negative polarity modes to capture both hydrophilic and hydrophobic metabolites. We employed the XCMS plus bioinformatics platform to link mTOR-regulated metabolites to the predicted biological pathways. Statistical significance (p < 0.001) was assessed by ANOVA and Ranked order data by Whitney-Cox followed by ad hoc unpaired t-test. Results: The cluster heatmap deconvolution and cloud plot analysis show the differential pattern of metabolites between Rapamycin and Rapalink-treated pancreatic beta cell lines. Mapping the downstream metabolites data onto predictive metabolic pathways and activity networks revealed that the top pathways affected included the pentose phosphate pathway, dopamine and ubiquinol degradation pathways in the ESI-positive polarity mode, and creatine synthesis/glycine degradation and nicotine degradation pathways in the ESI negative polarity mode. Conclusions: The high-resolution untargeted metabolomics can be leveraged as a proxy of the internal exposome yielding high-dimensional data that provide mechanistic insights into metabolic and signaling pathways, and the underlying biology. This approach will have beneficial applications of the internal exposome in determining the optimal precision nutrition pathways for personalized medicine. Full article

Laportea bulbifera (Sieb. et Zucc.) Wedd., a plant with a long history of medicinal use, possesses uncertainly defined medicament portions while its antioxidant capacity remains largely unexplored. To gain a better understanding of its medicinal value, this study focused on investigating the Laportea bulbifera aboveground part (LBAP) and the Laportea bulbifera root (LBR). Through an assessment of the bioactive compound content, a significant finding emerged: the LBR exhibited notably higher levels of these bioactive phytochemicals compared to the LBAP. This observation was further reinforced by the antioxidant assays, which demonstrated the superiority of the LBR’s antioxidant capacity. The experimental results unequivocally indicate that the root is the optimal medicament portion for Laportea bulbifera. Furthermore, it was discovered that the presence of alcohol in the extraction solvent significantly enhanced the extraction of active ingredients, with the methanol extract of LBR performing the best among the extracts tested. Consequently, this extract was selected for further research. Leveraging cutting-edge UHPLC-ESI-Q-TOF-MS technology, the methanol extract of LBR was meticulously analyzed, revealing the presence of 41 compounds, primarily belonging to the phenolics and fatty acids. Remarkably, stability experiments demonstrated that the phenolics in the methanol extract maintained their stability across various pH values and during in vitro simulations of the human digestive system, albeit showing gradual degradation under high temperatures. Furthermore, the oxidative stability tests conducted on oils revealed the potential of the methanol extract as a stabilizer for olive oil and sunflower oil. Moreover, oral acute toxicity studies confirmed the low toxicity of the methanol extract, further supporting its safe use for medicinal purposes. Of particular note, histopathological examination and biochemical analysis affirmed the remarkable protective effects of the methanol extract against d-galactosamine-induced liver damage. These findings underscore the therapeutic potential of the methanol extract from the LBR in the treatment of diseases associated with oxidative imbalance. Full article