Search Results (399)

Xinhui Citri Reticulatae Pericarpium (CRP, “Chenpi”) is highly valued but is frequently challenged by origin-related adulteration and mislabeling. In this study, a rapid fingerprinting strategy based on direct analysis in real-time quadrupole time-of-flight mass spectrometry (DART-QTOF-MS) coupled with chemometric analysis was developed for the geographical characterization of CRP. DART-QTOF-MS enabled fast acquisition of mass spectral fingerprints with minimal sample preparation, and characteristic compounds were tentatively assigned on the basis of accurate mass and library matching. Comparative analysis showed that the high-mass region was dominated by polymethoxylated flavones and exhibited relatively limited between-region variation. In contrast, the low-mass region contained more evident origin-related differences and provided more informative variables for classification. Among the low-molecular-weight compounds, methyl N-methylanthranilate was markedly enriched in Xinhui samples, and 2-indolinone was identified as a promising candidate marker and further confirmed in CRP extracts by UPLC–MS/MS. OPLS-DA based on selected low-molecular-weight markers supported the discrimination of core Xinhui CRP and non-core Xinhui CRP. Overall, these results demonstrate the potential of DART-QTOF-MS as a screening tool for CRP origin authentication and highlight the value of low-molecular-weight markers for future quality-control applications. Full article

Peptaibols, predominantly secreted by Trichoderma species, are a class of linear peptides composed of five to twenty amino acid residues, synthesized non-ribosomally and enriched with α-amino isobutyric acid. These unique peptides appear to be highly effective in mediating the interactions between Trichoderma and plant pathogenic fungi. In this study, Ultra-Performance Liquid Chromatography–Quadrupole Time-Of-Flight Mass Spectrometry/Mass Spectrometry (UPLC-QTOF-MS/MS) technology was used to detect peptaibols profiles of Trichoderma strains during their interactions with the pathogen Fusarium graminearum. MS investigations of crude extracts derived from in vitro confrontations of Trichoderma atroviride T23 and its genetically modified counterparts, dual-culture assays of Mlae1, Mvel1, OElae1, and OEvel1 with F. graminearum were performed to shed light on the regulatory role of the velvet complex composed of LAE1&VEL1 in the synthesis of peptaibols during the microbial interaction. These results revealed intriguing variations in the total peptaibols produced during the interactions, as well as some differences in the specific peptaibol profiles between the confrontation and control tests. The overexpression strains, OElae1 and OEvel1, distinguished themselves by their proficiency in inducing long-residue peptaibols synthesis, attaining an impressive biocontrol index of up to 76%. The crude extracts containing peptaibols of OElae1 and OEvel1 demonstrated a capability to enhance cell membrane permeability and decrease DON toxin production in F. graminearum, and the crude extracts of OElae1 strains exhibited more effectiveness in reducing DON toxin production. In conclusion, the interaction with F. graminearum significantly impacted the peptaibol production in the examined Trichoderma strain, emphasizing the intricate interplay and reciprocal influence of genetic factors and environmental stimuli. Full article

The flowers of Sophora japonica L. (SJF) and Robinia pseudoacacia L. (RPF) are edible and similar in appearance. The chemical constituents of SJF and RPF were compared by UPLC-Q-TOF-MS/MS and HPLC analysis in this study. A total of 29 and 19 constituents were identified in SJF and RPF, respectively. Flavonoid glycosides were the main constituents found in both flowers. The main aglycon moieties found in SJF were quercetin, kaempferol and isorhamnetin, whereas acacetin and kaempferol were the main ones found in RPF. Additionally, the content of flavonoids in SJF was significantly higher than that in RPF, as determined by HPLC. Rutin was the most dominant flavonoid in SJF with a content range of 72.31~88.15 mg/g, followed by quercetin (13.05~20.30 mg/g). Kaempferol-di(rhamnoside)-hexoside was the most dominant flavonoid in RPF with a content range of 25.94~30.00 mg/g. The distinct flavonoid profiles indicated the chemical non-equivalence of SJF and RPF. Therefore, RPF should not be considered a direct substitute for SJF in herbal medicine without further pharmacological and clinical validation. Full article

This study aims to achieve the efficient preparation of sunflower calathide flavonoids (SCF) through optimized processes and to elucidate their composition and bioactivity. Total flavonoids were prepared by optimizing the ultra-high-pressure extraction (UHPE) process using a combination of single-factor experiments and response surface methodology, followed by purification and enrichment via macroporous resin. The components were identified with UPLC-QTOF-MS/MS technology, and their antioxidant activity and inhibitory capacity against xanthine oxidase (XOD) were systematically evaluated. The optimal extraction conditions were determined as follows: an extraction pressure of 290 MPa, a holding time of 8 min, an ethanol concentration of 67%, and a solid-to-liquid ratio of 1:14 g/mL. Under these conditions, the total flavonoid extraction yield reached 13.52 mg/g, which was further enriched to 16.74 mg/g after purification by macroporous resin. A total of 32 flavonoid compounds were identified, and the purified extract exhibited stronger free radical scavenging ability, total reducing power, ferric ion reducing activity, and XOD inhibitory effect compared to the unpurified extract. The combination of UHPE with macroporous resin separation technology effectively enriches SCF, and the resulting extract possesses both antioxidant and xanthine oxidase inhibitory activities, providing a theoretical basis and technical support for its industrial production and application. Full article

Background/Objectives: Ulcerative colitis (UC) involves inflammatory response, oxidative stress, changes in metabolites, and the gut microbiota. Jingangteng capsule (JGTC) has been utilized clinically for the treatment of inflammatory diseases for many years. However, the efficacy of JGTC in ameliorating UC remains unclear, and the underlying mechanisms have not yet been elucidated. This study aims to investigate the effect and mechanism of JGTC on UC. Methods: The chemical compositions of JGTC were examined using ultra-high-performance liquid chromatography with quadrupole time-of-fight mass spectrometry. The anti-UC effect of JGTC was evaluated by assessing the disease activity index (DAI), colon length, intestinal barrier recovery, and inflammatory factors in a dextran sulfate sodium (DSS)-induced colitis model. Mechanisms were investigated through fecal 16S rDNA sequencing, metabolomics analysis, enzyme-linked immunosorbent assay (ELISA), Western blotting, and network pharmacology analysis. Results: JGTC significantly reduced the DAI scores in UC mice, increased their body weight and colon length (p < 0.001), repairing damaged intestinal tissue. It decreased the levels of inflammatory cytokines TNF-α, IL-6, IL-1β, and LPS (p < 0.01, p < 0.001), alleviating intestinal inflammation. It also raised the expression of tight junction proteins ZO-1, Claudin-1, and Occludin (p < 0.05, p < 0.001), thereby enhancing intestinal barrier function. Fecal metabolomic analysis revealed that the favorable alterations in amino acid and lipid metabolites were more pronounced. Heat maps showed strong correlations between pharmacological indicators and gut microbiota, as well as between the main differential metabolites and gut microbial communities. UPLC-QTOF-MS detection yielded 33 components of JGTC, and network pharmacology analysis based on these components predicted pathways of action of JGTC in UC. Functional pathways closely associated with significantly differential metabolites and metabolic pathways were also investigated. The PI3K-AKT-mTOR pathway was one of them, which is consistent with the conclusions drawn from network pharmacology. JGTC significantly modulated key factors in this pathway, inhibiting the expression of PI3K, Akt, PDK1, and mTOR, while augmenting the expression of PTEN (p < 0.05, p < 0.01, p < 0.001). It also mitigated the levels of related oxidative stress factors MDA, MPO, and D-LA, and raised SOD levels (p < 0.01, p < 0.001). Conclusions: JGTC improved the excessive inflammatory response in UC by regulating intestinal flora and metabolic disorders, affecting the PI3K-AKT-mTOR signaling pathway, restoring intestinal tissue damage and intestinal barrier, and inhibiting inflammatory and oxidative stress factors. Full article

Sulfur fumigation, as a highly effective method for preservation and appearance enhancement, has been widely applied in fruits, vegetables, and food products. However, excessive sulfur fumigation can pose safety risks. Currently, there is limited research on the bound sulfites produced by sulfur fumigation, and no consensus has been reached regarding their structure and toxicity. Using ultra-performance liquid chromatography–quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF-MS/MS), a total of 34 compounds were identified in 12 lily bulb samples subjected to different sulfur fumigation durations. These derivatives were all hypothesized to form via nucleophilic addition to carbon–carbon double bonds. Based on multivariate statistical analysis, 9 characteristic markers were established to rapidly differentiate between non-fumigated (NF) and sulfur-fumigated (SF) samples. The practicality of this strategy was validated using 18 commercial batches. Molecular docking simulations predicted that the modifications might enhance toxicity toward liver injury-related targets, both by altering the spatial conformation of the compounds and because the sulfonic acid group itself serves as an ideal hydrogen-bond acceptor. Overall, mild fumigation led to a gradual accumulation of free sulfur dioxide in lily bulbs, increased the total content of phenolic components and antioxidant capacity, and did not generate excessive bound sulfur dioxide. However, with further extension of fumigation time, the content of sulfur-containing derivatives rose rapidly, accompanied by a noticeable decline in antioxidant activity. This study elucidates the sulfur-driven chemical transformation mechanisms in lily bulbs and establishes a targeted methodology for the quality control and safety assessment of processed herbal products. Full article

Extra virgin olive oil (EVOO) is a key component of the Mediterranean diet, valued for its bioactive constituents and associated health benefits. This study evaluated the influence of four agronomic and processing factors—harvest month, destoning, fruit washing, and bottling delay—on the chemical composition of Kolovi EVOOs from the PGI Lesvos region. A total of 34 oils were produced under standardized conditions and analyzed for phenolic compounds, tocopherols, pigments, and squalene using UPLC-QTOF-MS and HPLC-DAD. The oils were characterized by consistently high nutritional quality, with most samples fulfilling EFSA health claim thresholds for hydroxytyrosol, tyrosol and its derivatives, and α-tocopherol. Harvest month was the most influential parameter: early harvested oils (October) contained significantly higher levels of phenolics, α-tocopherol, and lutein, whereas later harvests (November) were richer in squalene. Destoning produced modest changes, with slightly higher phenolics in non-destoned oils and reduced lipophilic antioxidants in destoned samples. Fruit washing selectively decreased hydrophilic phenolics, while lipophilic compounds were largely unaffected. Bottling delays of up to 48 h under protective conditions had negligible effects on composition, aside from minor increases in specific phenolic derivatives. These findings suggest that early harvesting and careful consideration of destoning are the most effective strategies for supporting the antioxidant profile of Kolovi EVOOs, while other practices can be adjusted with limited impact on quality. Full article

Severe browning often occurs in Multivitamin Iron Oral Solution during storage, which directly leads to the decline of product quality. To clarify the main mechanism of browning in this preparation, the contents of 5-hydroxymethylfurfural (5-HMF) and carbohydrates, as well as the relevant characteristic parameters such as color and fluorescence, were determined at different storage times in this study. Subsequently, four reaction models, namely sucrose-lysine, sucrose-citric acid, sucrose-niacin, and sucrose-folic acid, were constructed according to the formulation of the preparation to systematically investigate the effects of each system on browning. The results showed that the sucrose-lysine model was the main color-forming reaction system of the preparation. Citric acid could significantly promote the hydrolysis of sucrose to produce two reducing sugars, glucose and fructose, which not only provided sufficient substrates for the Maillard reaction (MR), but also led to the massive accumulation of 5-HMF. Further analysis revealed that heating temperature and heating time were significantly positively correlated with the contents of 5-HMF, browning index (BI), color density (CD), and reducing sugars in the solution, while significantly negatively correlated with sucrose content (p < 0.05). Two fractions, P1 and P2, were isolated by Sephadex LH-20 column chromatography. Among them, P1 with a molecular weight of 61,660 Da was identified as the key fluorescent color-forming component, whose ultraviolet and fluorescence characteristics were basically consistent with those of Multivitamin Iron Oral Solution. Ultra-performance liquid chromatography-quadrupole-time-of-flight tandem mass spectrometry (UPLC-Q-TOF-MS/MS) analysis confirmed that P1 contained characteristic fragments of conjugated unsaturated structure, which was the key chromophore responsible for its fluorescence properties. In summary, this study explored the main browning mechanism of Multivitamin Iron Oral Solution. It was found that after citric acid catalyzed the hydrolysis of sucrose, the generated reducing sugars underwent Maillard reaction with lysine to produce fluorescent color-forming substances, and heat treatment significantly aggravated the browning process. The results of this study not only provide a solid theoretical basis for optimizing the preparation process and improving the storage stability of Multivitamin Iron Oral Solution, but also offer an important reference for the research on the browning mechanism and stability of other sugar-containing liquid preparations. Full article

Raspberry (Rubus idaeus L.) fruits have been widely used due to their abundance of diverse polyphenolic compounds, whereas research on the chemical composition and bioactivity of their stems and leaves remains limited. In this study, the ethyl acetate extract of raspberry stems and leaves was evaluated for inhibitory activity against α-glucosidase and α-amylase. Guided by affinity ultrafiltration–mass spectrometry, 16 potential active components were further isolated and characterized. Among these, 13 compounds exhibited binding affinity for α-amylase, while 5 compounds showed binding affinity for α-glucosidase. Quercetin-3-O-β-D-glucoside-7-O-β-D-gentiobioside was isolated from raspberry stems and leaves for the first time. Procyanidin C₃ and quercetin exhibited significant inhibitory effects on the two enzymes. Molecular docking studies hinted at the interactions between these compounds and the key active sites of the two enzymes. These findings suggest that phenolic compounds in raspberry stems and leaves may possess potential as α-glucosidase and α-amylase inhibitors, providing a scientific basis for further research on their application as functional components for blood glucose control. Full article

Dandelion, a herb with medicinal and nutritional properties, was studied for the stability and neuroprotective effects of polyphenols from its flowers, roots, and leaves during in vitro simulated digestion. Using UPLC-QTOF-ESI-MS/MS, 84 phenolic metabolites were identified, with flavonoids being most abundant in flowers and phenolic acids in leaves and roots. In vitro neuroprotection assays revealed that leaf polyphenols exhibited the highest inhibition rates against acetylcholinesterase and lipoxygenase, while flower polyphenols showed the strongest scavenging activity against reactive nitrogen species. After simulated digestion, total phenol and flavonoid contents increased significantly. Notably, polyphenols from all dandelion parts demonstrated the strongest inhibition of acetylcholinesterase during the oral phase, while the small intestine phase showed the greatest inhibition of lipoxygenase and reactive nitrogen species. Moreover, leaf polyphenols maintained the highest inhibitory effect on acetylcholinesterase throughout all digestive stages, suggesting that dandelion leaves are a promising functional food for preventing neurodegenerative diseases. Full article

Methyl jasmonate (MeJA) is a defence-related phytohormone that triggers metabolic reprogramming in grapevines and modulates pathways associated with stress responses and secondary metabolism. However, the temporal organisation of leaf metabolic responses following MeJA elicitation remains insufficiently characterised. In this study, an untargeted metabolomic approach based on UPLC-QTOF-MS was applied to investigate the time-resolved metabolic response of Vitis vinifera L. cv. Tempranillo leaves following foliar application of 10 mM MeJA under controlled greenhouse conditions. Leaf samples were collected at 0, 3, 6, 18, 24, and 48 h post-treatment. After quality filtering, 2552 metabolite features were detected, of which 40 discriminant features met stringent statistical criteria (maximum fold change ≥ 2 and p ≤ 0.05). Putative annotation according to Metabolomics Standards Initiative guidelines (MSI levels 2–3) revealed modulation of several metabolite classes, including carbohydrate-derived conjugates, terpenoid-related metabolites, hydroxycinnamic acid derivatives, and flavonoid-associated compounds. Temporal profiling revealed structured and non-monotonic metabolic responses characterised by rapid early changes between 3 and 6 h, followed by delayed accumulation patterns peaking around 24 h. Early phases were mainly associated with carbohydrate-related metabolites, suggesting rapid redistribution of carbon resources after elicitor perception. These results indicate that MeJA-induced metabolic adjustment in Tempranillo leaves occurs through temporally differentiated response phases rather than a uniform metabolic shift, providing a time-resolved metabolomic framework for interpreting elicitor-driven defence responses in grapevine. Full article

Maclekarpine E is a minor alkaloid from Macleaya species with reported in vitro anti-inflammatory activity, but its in vivo metabolism remains unexplored. This study investigated the metabolic fate of maclekarpine E in rats and evaluated the potential pharmacological relevance of its metabolites. Maclekarpine E was orally administered to male Sprague-Dawley rats (250 mg/kg). Plasma, urine and feces were collected and analyzed by UPLC-Q-TOF-MS/MS. CYP phenotyping was performed using recombinant human enzymes. Molecular docking against ABCG2 and ABCC2 was conducted to assess potential interactions of all fecal compounds with these efflux transporters. Network pharmacology was employed to predict potential anti-ulcerative colitis-related targets of the metabolites, generating hypotheses for future experimental validation. Nineteen phase I metabolites were identified. Biotransformations included ring-opening, demethylation and oxidation. All 19 metabolites were detected in feces, nine in plasma and two in urine. No phase II conjugates were observed. CYP2C19 was the only significantly active isoform under the tested conditions, mediating approximately 16.5% substrate depletion (p < 0.05). All 20 fecal compounds bound ABCG2 (ΔG < −5.0 kcal/mol); 19 bound ABCC2. Network pharmacology yielded 57 overlapping targets with ulcerative colitis, enriched in PI3K-Akt and MAPK pathways. This study provides the first comprehensive metabolic profile of maclekarpine E in rats. The compound undergoes CYP2C19-mediated oxidation and is predominantly excreted into feces. Its fecal metabolites are potential ABCG2/ABCC2 substrates and may target UC-associated pathways based on network pharmacology predictions, warranting further experimental validation. Full article

Background/Objectives: Alzheimer’s disease (AD) involves amyloid and tau pathology with neuroimmune dysregulation, and Yixin Yangshen Granules (YXYS) shows neuroprotective promise, though mechanisms remain unclear. This study aimed to elucidate the multi-target mechanisms of YXYS in AD. Methods: The study began by analyzing a public human AD hippocampal snRNA-seq dataset to identify cell-type-specific pathological pathways and profiled YXYS constituents by UPLC-QTOF-MS. In vitro, YXYS cytoprotection against mitochondrial dysfunction and oxidative stress was tested in Aβ_25–35-challenged HT22 cells; in vivo efficacy was assessed in Aβ_1–42-induced mice via behavioral and histopathological analyses. Integrated transcriptomic and proteomic profiling of brain tissue, with ELISA, qRT-PCR, and Western blot validation, confirmed pathway targets. Using the intersection of transcriptomic and proteomic targets as biological input, the DTIAM deep learning framework was employed to prioritize active YXYS constituents. Finally, molecular docking and 100-ns dynamics simulations demonstrated direct binding of Ganosporelactone A to HIF−1α. Results: AD snRNA-seq analysis highlighted HIF−1 and AGE-RAGE signaling as prominent pathways in the AD hippocampus, particularly enriched in brain microvascular endothelial cells, implicating neurovascular hypoxic and inflammatory stress. In Aβ-induced mice, YXYS improved cognition, reduced Aβ pathology, suppressed neuroinflammation, and promoted neuronal survival, consistent with in vitro evidence of restored mitochondrial function. Multi-omics confirmed convergence on HIF−1 and AGE-RAGE pathways, with YXYS rebalancing the neuroimmune microenvironment by reducing pro-inflammatory M0 macrophages. Screening against these consensus signaling hubs, deep learning analysis prioritized Ganosporelactone A as the top-ranked modulator, and molecular further demonstrated the stable binding of Ganosporelactone A to HIF−1α, linking YXYS to mitigation of hypoxic stress. Conclusions: Guided by multi-omics and deep learning, our findings suggest that YXYS may alleviate AD-related phenotypes through multi-target modulation of the HIF−1 and AGE-RAGE pathways, with associated improvements in neuro-immune homeostasis and reductions in oxidative stress, neuroinflammation, and hypoxia. Full article

Indigofera stachyodes Lindl. (I. stachyodes), a fundamental herb in Miao ethnomedicine, possesses a broad pharmacological profile including antitumor potential. However, its antitumor bioactive compounds and their underlying mechanisms remain poorly characterized. Here, we developed a spectrum-effect relationship analysis integrated with UPLC-Q-TOF-MS/MS, which enabled the identification of 7 compounds with potential antitumor activity from I. stachyodes. A secondary screening of candidate compounds was performed using network pharmacology, which led to the identification of fisetin, luteolin, wogonin, and liquiritigenin as potential antitumor compounds. Enrichment analysis and molecular docking studies predicted the key involvement of the PI3K-AKT signaling pathway in mediating the antitumor activities of these compounds. Subsequently, in vitro cell experiments confirmed that the fisetin, wogonin, luteolin and liquiritigenin inhibited the proliferation of HepG2 cells, with IC₅₀ values of 82.13 ± 6.74, 123.38 ± 5.71, 141.76 ± 6.37, and 151.04 ± 3.08 µM, respectively, while exhibiting moderate antitumor activity compared to chemotherapeutic agents. This antiproliferative effect was further corroborated by confocal laser scanning microscopy (CLSM). These results not only validate the potential of I. stachyodes as a source for antitumor agents but also provide a foundation for its further development. Full article

Biopolymers are increasingly explored as safer and more sustainable food packaging materials. This study evaluated the migration behavior of intentionally and non-intentionally added substances (IAS and NIAS), as well as the safety of gelatin and xanthan gum blends reinforced with microcrystalline cellulose, with and without oxygen plasma treatment, incorporating glycerol and limonene as plasticizers. Migration tests were conducted according to European Union (EU) Regulation No. 10/2011 using simulants of different polarities, and IAS/NIAS were analyzed by gas chromatography–mass spectrometry and ultra-high-pressure liquid chromatography–quadrupole time-of-flight mass spectrometry (GC–MS and UPLC-QTOF-MS). Films containing limonene were also evaluated for antioxidant activity. Results showed that plasticizer migration is strongly influenced by simulant polarity, glycerol predominantly migrated into hydrophilic media, whereas limonene and its derivatives exhibited higher migration in fatty simulants. Ethanol 95% acted as a conservative worst-case simulant, promoting extensive migration, while substantially lower migration levels were observed in isooctane and tenax plasma treatment resulted in modest changes in volatile compound migration, while significantly enhancing the antioxidant activity of limonene-containing films. Although overall migration levels were low under most of the tested conditions, NIAS formation, particularly from limonene degradation, highlights the need to account for chemical stability and simulant type when assessing bio-based films. Overall, the study demonstrates that film composition, surface modification, and simulant characteristics jointly influence migration behavior and functional performance under the evaluated conditions reinforcing the need to adapt current regulatory frameworks to the specific behavior of biopolymeric packaging materials. Full article