Search Results (171)

The present study focuses on recovering phenolic compounds and terpenes from olive leaves, which are generated as by-products during olive oil processing. To this end, conventional extraction/maceration (CE) and advanced extraction techniques such as subcritical water extraction (SWE), pressurized fluid extraction (PLE) and ultrasound-assisted extraction (UAE) were employed to compare and determine the most effective procedure. The phenolic and terpenoid composition of the extracts revealed a total of 33 compounds in HPLC-QTOF-MS analysis. According to these findings, the optimal extraction techniques for the maximum recovery of secoiridoids from olive leaves were PLE and UAE, with no significant difference between them (21.9891 ± 2.5521 mg/g DW and 21.0888 ± 1.3494 mg/g DW, respectively). Regarding to flavonoids, UAE was the most effective extraction technique, yielding 4.9837 ± 0.6739 mg/g DW. However, SWE recovered the highest amount of phenolic alcohols (7.4201 ± 0.9848 mg/g DW), which could be due to degradation of the secoiridoids during extraction. Conversely, UAE was more successful than the other techniques for the extraction of the terpene family (0.7373 ± 0.0601 mg/g DW). The present study therefore focuses on comparing different extraction techniques for revalorizing olive leaves as a source of bioactive compounds, specifically polyphenols and terpenes, due to their beneficial health properties. Full article

Background: Crataegus almaatensis, an endemic hawthorn species from Kazakhstan, is known for its rich content of phenolic compounds and flavonoids with significant pharmacological potential. This study aimed to optimize and compare conventional solid–liquid extraction (SLE) and ultrasound-assisted extraction (UAE) processes for maximizing the extractability of bioactive compounds from hawthorn leaves powder. Methods: The effects of temperature, extraction time, ethanol concentration, and solid-to-liquid ratio (or ultrasound power in the case of UAE) on total phenolic content (TPC), total flavonoid content (TFC), and antioxidant activity (FRAP, DPPH, and ABTS assays) were systematically evaluated. Results: The UAE method yielded higher concentrations of TPC and TFC, with up to 16% improvement in TPC and reduced ethanol usage (40% (v/v)) compared to SLE (75% (v/v)), demonstrating its efficiency and sustainability. Optimal extraction conditions were identified as 70 °C, 75% ethanol, 34 min, and an S/L ratio of 0.05 g/mL for SLE, 70 °C, 40% ethanol, 44 min, and 100 W US power for UAE. High-resolution HPLC-DAD and LC-Q/TOF-MS analyses confirmed the presence of key phenolic acids and flavonoid glycosides, including chlorogenic acid and apigenin-8-C-glucoside-2′-rhamnoside as the most abundant compounds identified. Conclusions: These findings validate UAE as an innovative, eco-friendly method for extracting bioactive compounds from hawthorn leaves and highlight its potential for developing natural antioxidants for pharmaceutical and nutraceutical applications. 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

This study evaluated the in vitro anti-inflammatory activity of serotonin derivatives from safflower seed powder and elucidated their mechanism against ulcerative colitis using network pharmacology. Compounds were extracted and purified via silica gel column chromatography, Sephadex LH-20 and semi-preparative HPLC. Structural characterization employed NMR and UPLC-Q-TOF-MS/MS with literature comparisons. Anti-inflammatory efficacy was assessed in lipopolysaccharide (LPS)-induced RAW 264.7 macrophages. Network pharmacology predicted targets, molecular docking analyzed binding interactions and molecular dynamics simulations assessed complex stability. Eleven serotonin derivatives were isolated; N-trans-Feruloyl-3,5-dihydroxyindolin-2-one (1) and Bufoserotonin A (2) were identified in safflower seed meal for the first time. Compounds 1, 3–7 and 10 significantly reduced inflammatory factors, with N-feruloyl serotonin (4, FS) showing the strongest activity. Mechanistic studies revealed FS targets key molecules (STAT3, EGFR, ESR1, PTGS2, NF-κB1, and JUN), modulating PI3K-Akt, MAPK and cancer-related pathways. Molecular dynamics simulations confirmed FS-EGFR complex stability. Thus, two novel derivatives were isolated and FS demonstrated significant anti-inflammatory and potential anti-ulcerative colitis effects through multi-target, multi-pathway synergy, providing a foundation for developing safflower seed meal therapeutics. Full article

The quest to establish permanent outposts in space, the Moon, and Mars requires growing plants for nutrition, water purification, and carbon/nutrient recycling, as well as the psychological well-being of crews and personnel on extra-terrestrial platforms/outposts. To achieve these essential goals, the safety, quality, and sustainability of plant material grown in space should be comparable to Earth-grown crops. In this study, radish plants were grown at 2500 ppm CO₂ in two successive grow-outs on the International Space Station and at similar CO₂ partial pressure at the Kennedy Space Center. An additional control experiment was performed at the University of Louisiana Lafayette laboratory, at ambient CO₂. Subsequent analyses of glucosinolate and sugar species and content showed that regardless of growth condition, glucoraphasatin, glucoraphenin, glucoerucin, glucobrassicin, 4-hydroxyglucobrassicin, 4-methoxyglucobrassicin, and three aliphatic GSLs tentatively assigned to 3-methylpentyl GSL, 4-methylpentyl GSL, and n-hexyl GSL were present in all examined plants. The most common sugars were fructose, glucose, and sucrose, but some plants also contained galactose, maltose, rhamnose, and trehalose. The variability of individual secondary metabolite abundances was not related to gravity conditions but appeared more sensitive to CO₂ concentration. No indication was found that radish cultivation in space resulted in stress(es) that increased glucosinolate secondary metabolism. Flavor and nutrient components in space-grown plants were comparable to cultivation on Earth. Full article

This research investigates the metabolite composition and biofunctional activiteies of 41 Korean soybeans, categorized by application: bean sprout, bean paste, vegetable, and cooked-with-rice. Isoflavones were identified via UPLC-Q-TOF-MS/MS and quantified using HPLC, revealing malonylgenistin as the predominant composition (average 743.4 μg/g, 42.3% of total isoflavones). Bean sprout showed the highest average isoflavone (2780.6 μg/g), followed by bean paste (1837.8 μg/g), cooked-with-rice (1448.2 μg/g), and vegetable (883.2 μg/g), with significant differences in individual cultivars. Protein ranged from 36.8 to 46.6% and oil from 17.0 to 22.3%, with vegetable soybeans exhibiting the highest average protein (44.9%) and lowest average oil (18.6%). Moreover, PLS-DA and hierarchical clustering revealed distinct metabolic patterns in usage groups. Antioxidant activities (radical scavenging; DNA protection) and enzyme inhibition (tyrosinase; α-glucosidase) also varied significantly, correlating with isoflavone distributions. Particularly, Sorog exhibited the highest isoflavone (3722.7 μg/g) and strong antioxidant activity (DPPH: 72.2%; ABTS: 93.8%, 500 μg/mL), DNA protection (92.8%, 200 μg/mL), and inhibition of tyrosinase and α-glucosidase by 78.4% and 84.2% (500 μg/mL). These findings suggest that isoflavone-rich bean sprout soybeans, especially Sorog, are promising candidates for health-promoting foods and functional cultivar development. This is the first systematic study comparing the metabolites and health-related properties of soybeans based on Korean usage categories. Full article

The herb and flowers of yarrow (Achillea millefolium) are sources of multiple bioactive secondary metabolites used in medicine and cosmetology. This study aimed to establish the location of phenolic compounds in tissues of flowers and stems of A. millefolium via light and fluorescence microscopy and histochemical assays. The spectrophotometric and HPLC methods were deployed to quantify total phenolic compounds (PC), phenolic acids, and flavonoids in extracts from flowers and herb, whereas the LC-QTOF-MS method was used for their qualitative analysis. The results demonstrated that PC occurred in external and internal tissues of yarrow stems, petals, and other parts of the flower, as well as in involucral bracts. Qualitative phytochemical analyses demonstrated ca. 16% more PC and flavonoids in flowers than in the herb. This analysis allowed identifying 48 PC. A higher number of PC was identified in flowers than in herbs, with rosmarinic acid followed by chlorogenic acid being the major polyphenols found in both sample types. One of the flavonoids, namely luteolin, was detected in significantly higher quantities in the flowers than in the herb. This study results provide new data on the location of PC in flowers and stems of A. millefolium as well as extend knowledge on their contents in the raw material of yarrow. Full article

Chronic alcohol consumption is a major contributor to gastric injury, yet current therapeutic strategies predominantly rely on chemical agents with limited efficacy and potential side effects. Natural products, with their multi-target biocompatibility and safety advantages, offer promising alternatives for gastric protection. We examined the phenolic compounds of Elaeagnus angustifolia honey (EAH) and investigated its prophylactic potential against ethanol-induced chronic gastric injury in mice. HPLC-DAD-Q-TOF-MS analysis showed that 21 phenolic compounds were tentatively and qualitatively identified in EAH, as well as 14 phenolic compounds. Moreover, gastric ulcer indices, histopathological morphology, oxidative stress markers (MDA, GSH, SOD), inflammatory mediators (NO, PGE2), and cytokine gene expression (TNF-α, IL-6, IL-1β, iNOS) were evaluated via enzyme-linked immunosorbent assay (ELISA) and quantitative real-time PCR. Western blot was employed to assess COX-2 protein expression, while 16^S rRNA sequencing analyzed gut microbiota composition. The results demonstrated that EAH could play a role in gastric injury caused by long-term alcoholism by protecting gastric tissue structure, interfering with oxidative stress and inflammatory response, and remodeling the intestinal microbial community. Full article

A dual-column tandem mode was used to establish the fingerprints of Sarcandrae herb from different origins, and their chemical compositions were characterized by UPLC-Q-TOF-MS/MS, which provided an experimental basis for the establishment of a rapid and efficient method for the overall quality control of Sarcandrae herba. For the first time, nine common components were identified from the Sarcandrae herba herbs of 24 origins, which were neochlorogenic acid, chlorogenic acid, 4-caffeoylquinic acid, eleutheroside B1, quercetin-3-O-β-D-glucuronide, neoastilbin, astilbin, isofraxidin, and rosmarinic acid, respectively. A total of 92 compounds were identified by liquid mass spectrometry. The quality of the Sarcandrae herb from 24 origins was analyzed by similarity evaluation, principal component analysis, and cluster analysis, and the chemical components of Sarcandrae herba were identified by UPLC-Q-TOF-MS/MS. The results showed that the overall analysis based on fingerprinting and mass spectrometry could differentiate the origins of the herbs. Full article

Chinese herbal medicines have played a significant role in the development of new and effective drugs, but how to identify the active ingredients from complex extracts of traditional Chinese herbal medicines was a research difficulty. In recent years, few studies have focused on high-efficiency identification of small-molecule inhibitors of Programmed Death Ligand 1 with lower antigenicity and flexible structure tunability. In order to identify small molecule inhibitors of PD-L1 from complex Chinese herbal extracts, this study established a protein–ligand trapping system based on high-performance liquid chromatography coupled with a photo-diode array detector, ion trap/quadrupole time-of-flight tandem mass spectrometry, and a Programmed Death Ligand 1 affinity chromatography unit (ACPD-L1-HPLC-PDA-IT-TOF (Q-TOF)-MS) to rapidly screen and identify small-molecule inhibitors of Programmed Death Ligand 1 from Toddalia asiatica (L.) Lam. Fourteen components were then identified as PD-L1 binders, and surface plasmon resonance (SPR) validation results showed that six of them—magnoflorine (6), nitidine (22), chelerythrine (24), jatrorrhizine (13), toddaculin (68), and toddanol (45)—displayed PD-L1 binding activity. Laser scanning confocal microscopy results demonstrated that these compounds effectively inhibited the binding of PD-1 to PD-L1 in a dose-dependent manner. Additionally, flow cytometry analysis indicated they could promote human lung cancer cell line (A549) apoptosis when co-cultured with Peripheral Blood Mononuclear Cells (PBMCs). The system’s innovation lies in its first integration of dynamic protein–ligand trapping with multi-dimensional validation, coupled with high-throughput screening capacity for structurally diverse natural products. This workflow overcomes traditional phytochemical screening bottlenecks by preserving native protein conformations during affinity capture while maintaining chromatographic resolution, offering a transformative template for accelerating natural product-derived immunotherapeutics through the PD-1/PD-L1 pathway. Full article

Background: Yupingfeng San (YPFS) is a classic formula for treating allergic rhinitis (AR), which is composed of Astragalus mongholicus Bunge (AST), Atractylodes macrocephala Koidz (AMR), and Saposhni-kovia divaricata (Turcz.) Schischk (SR) at a ratio of 3:1:1. However, the potential bioactive components of YPFS relevant to AR treatment are currently unknown. Methods: This study combined in vivo chemical profiling, network pharmacology, and experimental validation to identify the substances in YPFS that are active against AR. Results: Firstly, 98 compounds in YPFS were identified using high-performance liquid chromatography–quadrupole time-of-flight mass spectrometry (HPLC-Q-TOF-MS/MS) with the assistance of Global Natural Products Social (GNPS) molecular networking. Then, 42 prototype components and 57 metabolites were detected in the plasma, urine, and feces of mice with AR. A network pharmacological analysis based on 42 in vivo prototypical components was also conducted to screen 15 key components and 10 core targets, and 6 key components were further selected through molecular docking. Finally, the four key active components (cimifugin, wogonin, formononetin, and atractylenolide I) were revealed to be the main ingredients of YPFS through validation (in vitro and in vivo). Conclusions: This is the first systematic study of the components of YPFS in AR mice, laying the foundation for elucidating the overall material basis of this formulation. This study provides rich basic data for further pharmacological and mechanistic studies on YPFS. Full article

Among aquatic organisms, marine dinoflagellates are essential sources of bioactive metabolites. The benthic dinoflagellate Coolia malayensis produces metabolites that have exhibited substantial and specific cytotoxicity on cancer cells; however, isolation and identification of the purified compounds remain a challenge. This study reports C. malayensis biomass multi-step extraction plus chemical analyses for identifying compounds with antineoplastic activity. Through bio-directed fractionation, the cytotoxicity of extracts and fractions was tested on H1299 (lung), PC-3 (prostate), HeLa (cervical), and MCF-7 (breast) cancer cell lines. Dichloromethane (DCM) phase, hydroalcoholic (HYD) secondary extract, and methanolic (MET) extract showed cytotoxic effects on all cell lines. Active extracts and fractions were analyzed by HPLC-QTOF-MS, ¹H, and ¹³C NMR. Cell lines H1299 and PC-3 treated with fractions F4, F7, and DCM2-AQ-Ch sub-extract showed morphological changes resembling those observed in the apoptosis control, and no signs of necrosis were observed. The selectivity of fraction F7 was above 100 μg mL⁻¹ for healthy cells, while cytotoxic activity was observed in cancer cells. This fraction was identified as mostly fatty acids (FA) by NMR. Seventeen compounds with reported biological activities, such as antioxidant, analgesic, antiviral, and anticancer, were identified from C. malayensis extracts and fractions. Among them, the phycotoxins gambieric acid A and B, okadaic acid, and dinophysistoxin-1 were detected. Further studies are needed to reveal more significant anti-cancer potential from C. malayensis. Full article

Human exposure to mycotoxins is a global concern since several mycotoxins, such as enniatins and aflatoxins, have shown carcinogenic and neurotoxic effects, and the toxicologic mechanisms of most of them still need to be clarified. This study aims to investigate the metabolic pathways affected by mycotoxin exposure by evaluating metabolite alterations in urine. The participants were 540 women from the Spanish Childhood and Environment Project (INMA). For metabolite identification, a dilute and shoot extraction, followed by HPLC-Q-TOF-MS identification analysis, was performed. Data were processed using Agilent Mass Hunter Workstation with the METLIN database, Agilent Mass Profiler Professional 10.0, and Metaboanalyst 6.0. Over 2000 metabolites were obtained in each sample after feature extraction, and the most significant metabolites (p-value ≤ 0.05, fold change ≥ 2.0) were considered for pathway analysis. Enrichment analysis and topology showed that the most significantly affected pathway was the biosynthesis of unsaturated fatty acids (adjusted p-value = 0.007), with four metabolomic hits associated: linoleic acid, octadecanoic acid/stearic acid, an arachidonic acid metabolite, and (9Z)-octadecenoic acid/oleic acid. Other related pathways (unadjusted p-value ≤ 0.1) included fatty acid biosynthesis, glycerophospholipid metabolism, and ether lipid metabolism. The present study highlights the importance of metabolomics in increasing knowledge of the toxicity mechanisms and health effects of mycotoxins, especially emerging ones. Full article

The division of labor among honeybee workers contributes to efficient pollination activities. Lipids play a crucial role in behavioral regulation, with pollen serving as a primary source of these lipids. However, the regulatory effect of pollen lipids on the division of labor of honeybee workers remains to be studied. In this study, an in-depth lipidomic analysis based on HPLC-QTOF-MS and UPLC-IM-QTOF-MS was applied. We conducted the first comprehensive lipidomic profiling of the abdomen, brain, and intestine of emerging, nursing, and foraging bees, as well as pollen, thereby establishing a lipid library comprising 646 lipid species. The lipid composition of pollen was found to exhibit characteristics similar to those of honeybee workers, with alpha linolenic acid (ALA) validated as a key labor characteristic lipid. Moderate dietary ALA supplementation reshaped lipid levels and facilitated metabolism related to the labor of division. These findings advance the field of lipidomic analysis in honeybee workers, revealing a novel behavioral regulator and extending the understanding of the nutritional regulation of ALA in the division of labor among honeybee workers. Full article

Avocado (Persea americana Mill.) is a widely cultivated fruit known for its nutritional benefits, with the seed representing a significant portion of the fruit that is often discarded as waste. In the Dominican Republic, the cultivar Semil 34 represents 58% of the national production. This study aimed to explore the potential of Semil 34 avocado seed (AS) as a source of bioactive compounds with applications in the food industry. We conducted the chemical characterization of the seed extract, focusing on its total phenolic content, total flavonoids, and antioxidant capacity. High-performance liquid chromatography–quadrupole time-of-flight mass spectrometry (HPLC-QTOF-MS) was employed to identify key phytochemicals, including phenolic acids and flavonoids, that were responsible for the antioxidant properties of the extract. The hydroalcoholic extract of the Semil 34 seeds exhibited an antioxidant capacity of 1743.3 ± 52.3 µM Trolox/g extract, total phenolic content of 25.86 ± 2.17 mg gallic acid equivalents/g extract, and total flavonoid content of 2.09 ± 0.10 mg quercetin equivalents/g extract. However, the extract’s antioxidant capacity was found to be sensitive to pH changes, suggesting the need for stabilization when used in acidic or basic food matrices. The present work identified 53 compounds in the Semil 34 seed extracts; among these, 23 are being reported for the first time in avocado seeds. This study demonstrates the potential of the avocado seed as a source of bioactive compounds and hence a functional ingredient, supporting its value in sustainable production and its possible contribution to environmental goals by reducing waste in the avocado industry. Full article