Search Results (1,832)

The dynamic metabolic landscape underlying goose meat quality deterioration during refrigerated storage remains incompletely elucidated. Here, ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS)-based widely targeted metabolomics was employed to characterize metabolic profiling in refrigerated goose meat. Orthogonal partial least squares discriminant analysis (OPLS-DA) revealed 211 differential metabolites, while random forest regression (RFR) identified 30 candidate biomarkers. Seven metabolites, including xanthine, oxidized glutathione, and inosine 5′-monophosphate, exhibited significant correlations with total volatile basic nitrogen (TVB-N). By integrating potential biomarkers, metabolic pathways involving purines, amino acids, and sugars were identified as underlying mechanisms of goose meat spoilage. Notably, through comprehensive analysis of time-dependent correlations between physicochemical properties and metabolic profiles, a temporal threshold for quality deterioration in refrigerated goose meat was identified as day 5. These findings deepen our understanding of metabolite variations in refrigerated goose meat and provide a basis for optimizing storage protocols. The identified biomarkers may enable rapid detection kits and smart packaging systems for poultry industry applications. Full article

Heliotropium procumbens, a Boraginaceae species native to Panama, has remained largely unexplored regarding its nitrogen-containing metabolites, including pyrrolizidine alkaloids (PAs). In the current study, a comprehensive phytochemical investigation of its aerial parts is presented using HPLC-DAD-IT-MS, UHPLC–HRMS, and GC-MS primarily to profile its PA composition. A total of twelve PAs and N-oxides (PANOs) were identified, along with two phenolamides—including N¹, N¹⁰-diferuloylspermidine, which is biosynthetically related to PAs—and the distinctive metabolite heliotropamide. The detected PAs included unsaturated necines, primarily monoesters of retronecine and heliotridine, as well as saturated PAs such as a platynecine-type PA and the less commonly encountered triol necines and their N-oxides. Among these, helifoline-N-oxide was isolated and structurally elucidated by NMR spectroscopy for the first time as a natural product. Comparison with the chemodiversity of PAs within the Heliotropium genus revealed a high degree of diversity in H. procumbens, which can be attributed both to the species’ inherent biosynthetic capacity for chemical variation and to the more comprehensive and extensive studies conducted on it, which naturally enrich the apparent diversity observed. This work expands the phytochemical knowledge of H. procumbens and contributes to a broader understanding of PA diversity in the genus, offering new insights into their potential ecological and toxicological significance. Full article

Gastrodiae Rhizoma (tianma, TM), a traditional medicine that has food and medicine homology, faces controversy over retaining its epidermis (tianma pi, TP) during processing due to unclear phytochemical value. This study presents the first integrated approach combining GC–IMS, UHPLC–MS, and Caenorhabditis elegans (C. elegans) aging models to compare TP with the tuber core (tianma xin, TX). The results include the following: (1) A total of forty-seven volatile compounds were identified by GC–IMS, including 12 key aroma substances via relative odor activity value (ROAV ≥ 1), of which seven ((Z)-4-heptenal, β-citronellol, hexanal, 1-pentanol, 1-octen-3-one, 2-methylpropanol, and 2-butanone) were enriched in TP. (2) Non-targeted metabolomics revealed 1025 metabolites via UHPLC–MS, highlighting phenylpropanoid biosynthesis as the primary differential pathway (p < 0.05). Phenylpropanoids and polyketides exhibited predominant enrichment in TP (|log2FC| > 2, VIP > 1, p < 0.01). (3) In C. elegans models, TP outperformed TX in pharyngeal pumping (4.16%, p < 0.05), while both extended stress-resistant lifespan (p < 0.01). In conclusion, TP plays an essential role in establishing the characteristic odor profile of TM and retaining bioactive components, particularly phenylpropanoids. Preserving TP during processing optimally maintains the distinctive aroma profile and pharmacological value of TM, which provides valuable guidance for industrial utilization. Full article

Focusing on the characteristic tea resource Zijuan tea, this study addresses the difficulty of grading on production lines and the complexity of quality evaluation. On the basis of the fusion of near-infrared (NIR) spectroscopy and visual features, a novel method is proposed for classifying different tenderness levels and quantitatively assessing key anthocyanin components in Zijuan tea fresh leaves. First, NIR spectra and visual feature data were collected, and anthocyanin components were quantitatively analyzed using UHPLC-Q-Exactive/MS. Then, four preprocessing techniques and three wavelength selection methods were applied to both individual and fused datasets. Tenderness classification models were developed using Particle Swarm Optimization–Support Vector Machine (PSO-SVM), Random Forest (RF), and Convolutional Neural Networks (CNNs). Additionally, prediction models for key anthocyanin content were established using linear Partial Least Squares Regression (PLSR), nonlinear Support Vector Regression (SVR) and RF. The results revealed significant differences in NIR spectral characteristics across different tenderness levels. Model combinations such as TEX + Medfilt + RF and NIR + Medfilt + CNN achieved 100% accuracy in both training and testing sets, demonstrating robust classification performance. The optimal models for predicting key anthocyanin contents also exhibited excellent predictive accuracy, enabling the rapid and nondestructive detection of six major anthocyanin components. This study provides a reliable and efficient method for intelligent tenderness classification and the rapid, nondestructive detection of key anthocyanin compounds in Zijuan tea, holding promising potential for quality control and raw material grading in the specialty tea industry. Full article

Daphne odora is an evergreen shrub belonging to the Thymelaeaceae family that is widely cultivated as an ornamental garden plant. Its roots, leaves, and flowers have traditionally been used in Chinese medicine to treat pain, skin diseases, and rheumatism. While previous phytochemical studies have reported the presence of phenols, coumarins, biflavonoids, lignans, and daphnane diterpenoids in D. odora, its flowers remain largely unexplored. In the present study, the first comprehensive investigation of daphnane diterpenoids contained in the flower buds and blooming flowers of D. odora was conducted using ultra-high-performance liquid chromatography coupled with Q-Exactive-Orbitrap high-resolution mass spectrometry (UHPLC-Q-Exactive-Orbitrap MS). A total of 30 daphnane diterpenoids were identified, including 12 previously unreported compounds, through detailed analysis of their retention times and MS/MS fragmentation patterns. Comparative profiling revealed that flower buds contained a higher abundance and greater diversity of daphnane diterpenoids than flowers. Furthermore, LC–MS-guided isolation enabled the purification of a novel compound, daphneodorin I (16), and its structure was elucidated through extensive physicochemical and spectroscopic analyses. Compound 16 represents the first daphnane diterpenoid with a Z-configured phenolic acyl moiety isolated from plants of the Thymelaeaceae family. Full article

Amphidinols (AM) are a diverse group of bioactive polyketides produced by dinoflagellates of the genus Amphidinium, known for their hemolytic, antifungal, and cytotoxic activities. This work presents the assessment of AM profiles in a comprehensive number of strains, whose species boundaries were previously established through detailed taxonomic analysis. Using UHPLC-MS/MS, we characterized the spectrum of AM analogs in 54 Amphidinium strains isolated from diverse geographical locations. In addition, toxicity was assessed using brine shrimp assays, which revealed significant inter- and intraspecific variability. Despite the broad diversity in AM content, no clear correlation was observed between total AM levels and toxicity across all strains. Multivariate analysis grouped the strains into clusters distinguished by distinct AM profiles and toxicity levels, suggesting that AM production alone does not predict toxicity. Our findings highlight the complexity of Amphidinium bioactivity, emphasizing the influence of strain-specific factors and other bioactive compounds. This work highlights the importance of integrating chemical, genetic, and biological assessments to understand better the factors that govern toxicity in this genus, with implications for ecological studies and the monitoring of harmful dinoflagellates. Full article

Sweet potato stems and leaves (SPSL) are rich in bioactive polyphenols, yet their utilization remains underexplored. This study established an efficient method for SPSL polyphenol enrichment using macroporous resins, with UHPLC-QE-MS/MS characterization of the purified polyphenols (PP) and subsequent evaluation of anti-inflammatory activity. The results showed that NKA-II resin demonstrated the best purification effect on SPSL polyphenols among the six tested resins. The optimal enrichment procedure of NKA-II resin was as follows: loading sample pH 3.0, 4.48 mg CAE/mL concentration, and 80% ethanol (v/v) eluent. A total of 19 major compounds were characterized in PP, including 12 phenolic acids and seven flavonoids, with a polyphenol purity of 75.70%. PP pretreatment (100 and 500 μg/mL) significantly inhibited LPS-induced release of NO (by 40.62% and 68.61%), IL-1β (by 40.07% and 68.34%), IL-6 (by 40.63% and 52.41%), and TNF-α (by 52.29% and 73.76%) compared to the LPS group (p < 0.05), demonstrating potent anti-inflammatory effects. Western blot analysis revealed that PP exerted anti-inflammatory effects by inhibiting the NF-κB (via suppression of IκBα phosphorylation/degradation and blockade of p65 nuclear translocation) and MAPK (via inhibition of p38, ERK, and JNK phosphorylation) signaling pathways. These findings support the utilization of this agricultural by-product in functional food development, particularly as a source of natural anti-inflammatory compounds for dietary supplements or fortified beverages. Full article

This study investigates the phenolic composition and antioxidant potential of root extracts from three Opuntia ficus-indica varieties (green, red, and orange) using ultra-high-performance liquid chromatography coupled with diode array detection and electrospray ionization–tandem mass spectrometry (UHPLC-DAD-ESI-MS/MS). Phenolic compounds were extracted with a hydromethanolic solvent and quantified by spectrophotometric assays, while antioxidant activity was assessed through DPPH, ABTS, iron III reduction, hydroxyl radical, and nitric oxide scavenging methods. A total of 26 compounds were identified, including piscidic acid, epicatechin-3-O-gallate, and isovitexin, with several phenolics newly reported for O. ficus-indica roots. The green and red varieties showed the highest phenolic contents (up to 147.82 mg/g extract) and strong antioxidant capacity, particularly in ABTS (IC₅₀ = 29.38 μg/mL) and hydroxyl radical inhibition (>90%). Relative Antioxidant Capacity Index (RACI) analysis confirmed a consistent correlation between phenolic/flavonoid content and antioxidant efficacy. These findings highlight the analytical relevance of UHPLC-DAD-ESI-MS/MS for profiling underutilized plant matrices and support the potential use of O. ficus-indica root extracts as natural sources of bioactive compounds for pharmaceutical and biomedical applications. Full article

Background and Objectives: The cultivation of Humulus lupulus has been encouraged in Brazil, despite the country’s climate generally being unfavorable for its development. This study aimed to evaluate the chemical composition, antioxidant activity, and photoprotective potential of four H. lupulus varieties, Cascade, Columbus, Comet, and Nugget, cultivated in the northwestern region of Paraná State, Brazil. Methods: The varieties were grown in experimental plots. Crude extracts (CEs) of cones and leaves were obtained through dynamic maceration with solvent renewal (96% ethanol), followed by concentration in a rotary evaporator. Assays for sun protection factor (SPF), total phenolic content (TPC), total flavonoid content (TFC), ferric reducing antioxidant power (FRAP), 2.2-diphenyl-1-picrylhydrazyl (DPPH^•) radical scavenging activity, and 2.2′-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS^•⁺) were performed to assess antioxidant activity. Chemical profiling was performed using UHPLC-MS/MS. Results: UHPLC-MS/MS analysis revealed the presence of phenolic and organic acids, flavonoids, phenolic aldehydes, alkaloids, and α-benzopyrone-type lactones, with high concentrations of rutin (>500 µg/g) in both cones and leaves. Total phenolic content ranged from 69.70 to 95.95 µg gallic acid equivalent/mg CE; flavonoids from 170.53 to 696.67 µg quercetin equivalent/mg CE; DPPH^• EC₅₀ values ranged from 1.34 to 3.13 mg/mL; FRAP from 1.19 to 2.52 µM ferrous sulfate/mg; ABTS^•⁺ from 5.11 to 22.60 mM Trolox/mg CE; and SPF ranged from 16.02 to 39.48 in the CE of H. lupulus cones and leaves. Conclusions: These findings demonstrate that the cultivated varieties possess antioxidant and photoprotective properties, encouraging further studies to explore their potential applications. Full article

In recent years, numerous studies have emerged on the biological activities of endemic berries from the Valdivian Forest and their potential for therapeutic use. However, some species appear to have been relatively neglected. The objective of this study was to conduct, for the first time, a phytochemical composition analysis of a hydroalcoholic extract of Luzuriaga radicans Ruiz & Pav. and to evaluate its potential as an antioxidant and as an enzyme inhibitor in relation to chronic non-communicable diseases. The berries were collected in the Saval Park in Valdivia and were subsequently extracted via sonication in ethanol/water. UHPLC-DAD, HPLC-APCI (+)-MS, and UHPLC-ESI (+)-TOF-MS analysis allowed for the identification of several carotenoid ester species. According to UHPLC-DAD, the sum of carotenoids yielded was 983.4 ± 26.3 mg/kg DW, while the concentration of the phenolic compounds was 9.33 ± 0.01 mg GAE/g dry fruit. The extract exhibited antioxidant properties by scavenging DPPH (2,2-diphenyl-1-picrylhydrazyl), ABTS (2,2-azinobis-(3-ethylbenzothioazolin-6-sulfonic acid)) radicals, and ferric reducing antioxidant power (FRAP). It also demonstrated cholinesterase enzyme inhibitor capacities (AChE and BuChE—IC₅₀: 6.904 ± 0.42 and 18.38 ± 0.48 µg/mL, respectively). Docking calculations were additionally performed for a selection of compounds in the berries. The data obtained suggest that the hydroalcoholic extract of L. radicans possesses significant potential as a natural antioxidant and for the inhibition of enzymes, making it a promising candidate for the development of phytotherapeutic and nutraceutical products, especially as a supplement against chronic diseases. Full article

Blueberry (Vaccinium corymbosum) leaves are often discarded as agricultural by-products despite their potential abundance in bioactive compounds. However, comprehensive knowledge of their phytochemical profile remains limited, especially at the cultivar level. To address this gap, this study performed untargeted metabolomic profiling of blueberry leaves from ten cultivars using UHPLC-QTOF MS. Metabolites were annotated using high-resolution mass spectrometry and MS/MS fragmentation patterns. Multivariate statistical techniques were employed to investigate inter-cultivar variability and identify distinctive metabolites. A total of 76 metabolites were discovered, with 64 being confidently annotated and grouped into ten main phytochemical classes. The relative abundances of phenolic acids, flavonols, and flavan-3-ols varied significantly among cultivars. Several metabolites were annotated for the first time in V. corymbosum leaves, such as miscanthoside, glucoliquiritin, apiin, khelloside, and aromadendrin. These metabolites are known in other plants for their biological activities, demonstrating blueberry leaves’ bioactive potential. This study highlights the importance of untargeted metabolomic approaches in elucidating the biochemical diversity of plant matrices. The metabolomic data revealed significant cultivar-specific variations and novel bioactive metabolite annotation. These findings establish a complete phytochemical fingerprint for each cultivar, providing a basis for future research to validate key metabolites’ biological activities and support the valorisation of V. corymbosum leaves. Full article

Aralia chinensis L. has shown potential in breast cancer treatment, yet its pharmacodynamically active components and mechanisms remain undefined. To systematically identify the bioactive constituents absorbed into the bloodstream and elucidate their multi-target mechanisms against breast cancer, we employed ultra-high-performance liquid chromatography in conjunction with Q Exactive Orbitrap mass spectrometry (UHPLC-Q Exactive Orbitrap-MS) alongside serum pharmacochemistry to analyze the chemical constituents of total saponins derived from A. chinensis (TSAC) and to identify the blood-absorbed prototypes in a rat model. Network pharmacology predicted targets and pathways of serum prototypes, validated by molecular docking and in vitro experiments. We identified 38 triterpenoid saponins, 3 steroidal saponins, and 8 triterpenoids in TSAC, with 22 prototype compounds detected in serum. An integrative analysis encompassing 486 compound targets and 1747 genes associated with breast cancer elucidated critical pathways, notably the PI3K-Akt signaling pathway and resistance mechanisms to EGFR tyrosine kinase inhibitors. Molecular docking confirmed strong binding of araloside A and elatoside L to SRC, PIK3R1, PIK3CA, STAT3, and EGFR. In MCF-7 cells, TSAC suppressed proliferation and migration while downregulating Src, PI3K, and EGFR expression at the gene and protein levels. This study successfully identified TSAC’s serum-absorbed bioactive components and demonstrated their anti-breast cancer effects via multi-target mechanisms involving the Src/PI3K/EGFR axis, providing a crucial pharmacological foundation for developing A. chinensis-derived breast cancer therapies. Full article

Mycotoxin contamination in wheat, a staple food critical to human nutrition, poses significant public health concerns. This study investigated the natural occurrence of 17 mycotoxins in Tunisian durum wheat, assessed the influence of soil tillage practices on mycotoxin contamination, and performed an associated exposure risk assessment. A total of 167 wheat samples were randomly collected over two years (2021 and 2022) from fields managed under conventional tillage (CT) and no-tillage (NT) systems during both pre- and post-harvest periods. Mycotoxins were extracted using the QuEChERS method and quantified via UHPLC-MS/MS. The results demonstrated contamination by ZEN, DON, OTA, ENA1, ENB, and ENB1. Among regulated mycotoxins, OTA was the most prevalent, detected in 68 out of 167 samples with a mean concentration of 1.85 µg/kg. ZEN was the most abundant, detected in 65 samples with a mean concentration of 26.85 µg/kg, while DON was less frequently detected in 62 samples with a mean concentration of 0.68 µg/kg. Regarding emerging mycotoxins, ENB was the most prevalent and abundant, found in 51 samples with a mean concentration of 10.13 µg/kg; ENB1 and ENA1 were detected in 20 and 10 samples, with mean concentrations of 3.38 µg/kg and 1.69 µg/kg, respectively. Furthermore, mycotoxin concentrations varied according to agricultural practices. DON, ZEN, ENA1, ENB, and ENB1 showed higher frequencies and concentrations (ranging from 0.08 to 210.11 µg/kg) in samples collected during the 2021 pre-harvest period from NT fields. In contrast, OTA exhibited greater prevalence and higher concentrations (ranging from 2.33 to 9.78 µ/kg) in samples collected during the 2022 post-harvest period from CT fields. The Estimated Daily Intake (EDI) of mycotoxins by Tunisian adults was calculated based on contamination levels in raw durum wheat from fields under NT and CT practices, resulting in the following values (ng/kg bw/day), with the first value corresponding to NT samples and the second to CT samples: OTA (17.3; 20.8), ZEN (466.3; 194.0), DON (8.0; 7.56), ENA1 (4.30; 18.85), ENB (105.17; 121.08), and ENB1 (49.91; 40.91). Both the Margin of Exposure (MOE) values for OTA and the Hazard Quotients (HQ) for ZEN and DON exceeded established safety thresholds, indicating potential health risks for Tunisian adults. These findings highlight the urgent need to implement stricter mycotoxin regulations in Tunisia and enhance surveillance systems. Further research is warranted to elucidate the mechanisms by which soil tillage practices influence mycotoxin contamination and to develop targeted mitigation strategies to ensure food safety. Full article

Isothiocyanates (ITCs), which are derivatives of glucosinolates (GSLs) from Brassica plants, have been investigated as anticancer agents. An extensively studied anticancer ITC is sulforaphane, which is found in low amounts in Chinese cabbage. We aim to investigate the types and content of GSLs (precursors of ITCs with anticancer activity) in Chinese cabbage seeds. GSLs from Chinese cabbage seeds were isolated and purified using acidic Al₂O₃ column chromatography and preparative HPLC. GSL and ITC profiles were further identified using UHPLC-Q-TOF-MS. The antitumor activities of ITC (produced by exogenous enzymatic hydrolysis of GSLs) were evaluated in vitro. Seventeen GSLs and seven ITCs were identified, and the dominant GSLs were gluconapin, glucobrassicanapin, and progoitrin in Chinese cabbage seeds. High-purity gluconapin (>99%) was purified. The ITCs showed synergistic-, dose-, and time-dependent effects on the inhibition of HepG2 cells, and the key ITCs were 3-butenyl ITC, sulforaphane, and 2-phenylethyl ITC. The corresponding parent GSLs were gluconapin, glucoraphanin, and gluconasturtiin, respectively. 3-Butenyl ITC could significantly induce HepG2 cell proliferation (IC50 = 89.44 μg/mL) and apoptosis (p < 0.05). Our results suggested that Chinese cabbage seed could be a valuable source of natural antitumor ingredients. Full article

Objectives: A thorough understanding of pharmacokinetics and metabolism is critical during early drug development. This study investigates the absorption, distribution, metabolism, and excretion (ADME) profile of R14, a novel compound, using a combination of in vitro and in vivo approaches. Methods: In vitro studies included Caco-2 permeability assays, metabolic stability evaluations in liver microsomes and hepatocytes, and identification of CYP isoforms responsible for R14 metabolism. In vivo pharmacokinetic and metabolic profiling was conducted in rats following oral administration. R14 was quantified using UHPLC-MS/MS. Metabolites were identified using high-resolution UHPLC- QTOF MS/MS, and relative exposure was estimated using peak area-derived AUCs. Results: R14 exhibited low oral bioavailability (13.4%) and high systemic clearance (2.63 L/h/kg), indicating high hepatic extraction. A total of 21 plasma and 38 urine metabolites were identified. Major metabolic pathways included initial hydroxylation and hydrogenation, followed by sequential methylation and Phase II conjugations (glucuronidation and sulfation). Key metabolites (M3, M4, M22, M38) accounted for the majority of systemic exposure. Less than 1% of the unchanged drug was excreted in urine, confirming extensive metabolism. Notably, discrepancies between in vitro and in vivo metabolite profiles suggested rapid further transformation of initial metabolites in vivo, which were not fully captured in vitro. Conclusions: This study demonstrates an efficient and integrated strategy for early-phase ADME characterization. The combined use of in vitro assays and in vivo studies, guided by advanced analytical techniques, provides a robust framework for understanding drug metabolism. These findings can inform drug optimization and help minimize risks in later stages of development. Full article