Search Results (132)

Peach (Prunus persica) leaves, usually discarded in traditional Chinese medicine, were explored as a source of laxative agents. Using zebrafish larvae for bioactivity-guided fractionation, we isolated a single active flavanone that was identified by NMR and HR-MS as Sakuranetin. In vivo assays demonstrated that Sakuranetin (10–25 µM) accelerated intestinal transit in a dose-dependent fashion; at 25 µM, 64.8% of the fluorescent intestinal content was expelled. Untargeted LC-MS metabolomic analysis revealed significant perturbations in serine biosynthesis and N-glycan precursor biosynthesis, suggesting energetic rewiring of enterocytes. RNA-Seq analysis highlighted gnat1 as the most responsive gene, and molecular docking predicted a stable Sakuranetin–Gnat1 complex with a binding free energy of −8.7 kcal/mol. Concurrent down-regulation of rho transcripts indicated suppression of inflammatory signaling that often accompanies constipation. Our findings identified Sakuranetin as a potent promoter of gut motility and position the otherwise wasted peach leaves as an untapped botanical resource for developing anti-constipation therapeutics. Full article

In this study, water residue obtained from Salvia desoleana Atzei et Picci steam distillation was evaluated for its antioxidant activity in vitro using different experimental models. In particular, the study evaluated the antiradical and antioxidant activity of Salvia desoleana extracts using CUPRAC, FRAP, DPPH^•, and ABTS^•+ assays; and tested ROS scavenging activity in Caco-2 cell cultures. Phenolic compounds were identified by (HR) LC-ESI-QTOF MS/MS and quantified with HPLC-PDA. Furthermore, Keap1-Nrf2, iNOS, and NOX enzymes involved in oxidative stress and antioxidant defences were the targets of molecular docking on key polyphenols. Hydroxycinnamic acids and flavonoids are the most important classes of compounds detected in the extracts. Among these compounds, the most significant was rosmarinic acid, followed by caffeic acid, luteolin glucuronide, and methyl rosmarinate. Although all extracts have shown encouraging results, the ethanolic extract solubilised with water (SEtOHA) was the one with the highest hydroxycinnamic acid content and total phenol content (518.64 ± 5.82 mg/g dw and 106.02 ± 6.02 mg GAE/g dw), as well as the highest antioxidant and antiradical activity. The extracts have shown anti-inflammatory activity by inhibiting NO release in LPS-stimulated Caco-2 cells. Finally, the in silico evaluation against the three selected enzymes showed interesting results for both numerical affinity ranking and predicted ligand binding models. The outcome of this study suggests this by-product as a possible ally in counteracting oxidative stress, as established by its favourable antioxidant compound profile, thus suggesting an interesting future application as a nutraceutical. Full article

Marine organism-associated microbes are an important source of structurally diverse and biologically active secondary metabolites exhibiting antimicrobial, anticancer, and anti-inflammatory activities. In this study, we investigated Penicillium brevicompactum MSW10-1, isolated from Hydractinia echinata, a marine invertebrate adapted to extreme intertidal and subtidal environments with variable temperature, salinity, and oxygen conditions. Through a combination of LC/MS-guided chemical analysis and chromatographic purification, eight secondary metabolites were isolated, including brevicolactones A (1) and B (2). The absolute chemical structures of 1 and 2 were determined based on NMR spectroscopic experiments, HR-ESIMS data, and quantum chemical ECD calculations. The isolated compounds (1–8) were evaluated for their ability to inhibit hepatic lipogenesis, a key process in lipid metabolism that is dysregulated in metabolic-dysfunction-associated steatotic liver disease. Furthermore, the inhibitory effects of the isolated compounds on lipid accumulation were further evaluated in primary mouse hepatocytes, using Oil Red O staining. These findings suggested that the isolated compounds may serve as promising candidates for the treatment of metabolic liver diseases associated with lipid dysregulation. Full article

Cyanobacterial blooms are becoming increasingly frequent and intense worldwide, often dominated by Microcystis aeruginosa, a species capable of producing a wide array of bioactive metabolites beyond microcystins. This study evaluates the ecotoxicological potential of a non-microcystin-producing strain, M. aeruginosa CCIBt3106, using acute immobilization assays with three microcrustacean species: Daphnia similis, Artemia salina, and Parhyale hawaiensis. Biomass was extracted using solvents of varying polarity, and selected extracts (aqueous and 50% methanol) were further fractionated and analyzed via high-resolution liquid chromatography–tandem mass spectrometry (HR-LC-MS/MS). Significant toxicity was observed in D. similis and P. hawaiensis, with EC₅₀ values ranging from 660 to 940 µg mL⁻¹. Metabolomic profiling revealed the presence of chemically diverse metabolite classes, including peptides, polyketides, and fatty acyls, with putative annotations linked to known bioactivities. These findings demonstrate that cyanobacterial strains lacking microcystins can still produce complex metabolite mixtures capable of inducing species-specific toxic effects under environmentally relevant exposure levels. Overall, the results highlight the need to expand ecotoxicological assessments and monitoring frameworks to include non-microcystin cyanobacterial metabolites and strains in water quality management. Full article

The degradation of pharmaceuticals in wastewater treatment plants (WWTPs), particularly the antidepressant Paroxetine (PXT), is a growing concern because their insufficient removal leads to their release in the aquatic environment, causing toxic effects on aquatic organisms. This study investigates g-C₃N₄ materials synthesized from urea, melamine, and thiourea, including thermally exfoliated variants, as potential photocatalysts for removing PXT from water and secondary-treated hospital wastewater (HWW). Comparative photocatalytic experiments under simulated solar radiation indicated that g-C₃N₄ prepared by urea (CN-U) and its thermally exfoliated form [CN-U(exf.)] were highly effective (100% removal in 45 min) depending on the degradation rate constants (0.036 and 0.085 min⁻¹ in U.P. water, respectively), with the latter achieving the fastest PXT degradation at 200 mg/L (k = 0.112 min⁻¹). The study also analyzed mineralization and transformation products (TPs) using liquid chromatography–high-resolution mass spectrometry (LC–HR-MS-Orbitrap) and assessed their ecotoxicity with ECOSAR (Version 2.2) software. Additionally, toxicity decreased following the photocatalytic processes, as revealed by the Microtox bioassay. Overall, CN-U and especially CN-U(exf.) show promise as eco-friendly photocatalysts for pharmaceutical removal from wastewater (WW). Full article

The ultra-high-performance liquid chromatography high-resolution mass spectrometry (LC-ESI-HR-MS/MS) technique was used to characterize the polyphenolic fraction of the hot water infusion (WI) of inflorescences of Cannabis sativa L. Kompolti variety, commercially used for food preparations or cosmetic purposes. On water infusion extract, we applied a multidisciplinary approach, where NMR, MS, in vitro cell-free and cell-based assays coupled with in silico studies, were used to rationalize at the molecular level the effects of the major component Cannabidiol (CBD), in a model of Parkinson’s disease (PD). The phytochemical analysis by LC-MS/MS led to the tentative identification of many components belonging to different classes of polyphenols, such as phenolic acids, flavonoids, and their glycosides. CBD and cannabidiolic acid (CBDA) were also detected in good amounts in the infusion, together with several minor cannabinoids. In addition, the water infusion WI was evaluated for mineral content, total phenolic content, flavonoid content, and antioxidant capacity by DPPH and FRAP methods. Notably, our results in a cellular model of PD highlight that CBD protects against rotenone-induced cell death without recovering neuronal morphology. These biological outcomes were rationalized by an in silico approach, where we hypothesize that CBD could influence the cellular response to oxidative stress via its interaction with the Keap1/Nrf2 pathway. In summary, these results enriched the nutraceutical profile of the water infusion of the inflorescences of the Kompolti cultivar, which demonstrated a high CBD content. This study could lead to the development of dietary supplements that could help in the management of clinical symptoms related to the antioxidant activity of CBD in the pathophysiology of PD, which remains poorly characterized. Full article

Platycladus orientalis, an evergreen tree belonging to the Cupressaceae family, has been traditionally used to treat various ailments, including fever, cough, diarrhea, diuresis, cold symptoms, and gastrointestinal disorders in folk medicine. As part of our ongoing investigation aimed at discovering bioactive natural products and elucidating their mechanisms of action from various natural sources, we investigated a methanol (MeOH) extract of P. orientalis leaves. This investigation led to the isolation and identification of a labdane-type diterpene, lambertianic acid (LA), via column chromatography and HPLC purification. The structure of LA was elucidated using LC/MS and NMR spectroscopic analyses, including HR-ESIMS, while its absolute configuration was confirmed through electronic circular dichroism (ECD) calculations. Recent studies have reported that labdane-type diterpenes exhibit diverse pharmacological activities, such as anticancer, anti-inflammatory, anti-obesity, and hypolipidemic effects. Notably, LA has been shown to modulate adipocyte metabolism via AMPK signaling; however, its role in skeletal muscle atrophy remains unexplored. Therefore, in this study, we investigated the effects of LA on dexamethasone (Dex)-induced muscle atrophy in C2C12 myotubes. Treatment with LA at concentrations of 25 µM and 50 µM significantly rescued myotube diameter and reduced the expression of atrophy-related proteins, including MuRF-1 and atrogin-1/MAFbx, without compromising cell viability at these moderate concentrations. These findings suggest that LA derived from P. orientalis exerts protective effects against skeletal muscle atrophy, highlighting its potential as a promising natural therapeutic candidate for muscle-wasting disorders. Full article

Microorganisms play a significant role in biofouling and biocorrosion within the maritime industry. Addressing these challenges requires an innovative and integrated approach utilizing marine natural products with beneficial properties. A comprehensive screening of 173 non-toxic EtOAc and H₂O extracts derived from diverse marine organisms collected in Indonesian waters was conducted using a robust panel of assays. These included antimicrobial tests and classical biosurfactant assays (drop collapse and oil displacement), as well as anti-quorum-sensing (QS) and anti-biofilm assays. These screening efforts identified five active extracts with promising activities. Among these, EtOAc extracts of the marine tunicate Sigilina cf. signifera (0159-22e) and the marine sponge Lamellodysidea herbacea (0194-24c) demonstrated significant anti-biofouling activity against Perna indica and anti-biocorrosion performance (mpy 10.70 ± 0.70 for S. cf. signifera; 7.87 ± 0.86 for L. herbacea; 13.60 ± 1.70 for positive control Tetracorr CI-2915). Further chemical analyses of the active extracts, including LC-HR-MS/MS, MS-based molecular networking, and chemoinformatics, revealed the presence of both known and new bioactive compounds. These included tambjamines and polybrominated diphenyl ethers (PBDEs), which are likely contributors to the observed bioactivities. Subsequent investigations uncovered new anti-QS and anti-biofilm properties in synthetic and natural PBDEs 1–12 previously derived from L. herbacea. Among these, 8 exhibited the most potent anti-QS activity, with an IC₅₀ value of 15 µM, while 4 significantly reduced biofilm formation at a concentration of 1 µM. This study highlights the potential of marine-derived compounds in addressing biofouling and biocorrosion challenges in a sustainable and effective manner. Full article

Background: Gardnerella vaginalis is a natural inhabitant of the vagina, but when an imbalance occurs in the vaginal microbiota, this bacterium can cause vaginosis, a condition that must be treated when symptomatic and prior to a gynecological intervention. Cannabidiol (CBD) is an anti-inflammatory compound that also has antibacterial activities against several Gram-positive and certain Gram-negative bacteria. Objectives: Since G. vaginalis is an opportunistic pathogenic Gram-variable bacterium, we investigated its response to CBD. Methods: The antibacterial activity of CBD was studied by broth dilution assay, changes in intracellular ATP levels, and the ability of bacteria to recover on chocolate agar plates. The antibiofilm activity was investigated by MTT metabolic assay, crystal violet staining, and HR-SEM. Flow cytometric analyses were performed to measure changes in membrane potential, membrane perforation, and metabolic activity. Reactive oxygen species (ROS) production was analyzed using the nitro blue tetrazolium (NBT) reagent. Gene expression was determined by semi-quantitative real-time PCR, while protein composition was determined by LC-MS/MS analysis. Results: We observed that G. vaginalis clinical isolates exhibited high susceptibility to CBD with a minimum inhibitory concentration (MIC) of 2.5 µg/mL CBD. CBD induced rapid membrane hyperpolarization and caused cytoplasmic leakage of ATP without increasing propidium iodide uptake. This was accompanied by reduced metabolic activity and loss of survivability. Proteomic analysis revealed decreased expression of some ribosomal-associated proteins. CBD exhibited antioxidant activity by reducing intracellular ROS levels in a dose-dependent manner. The antibacterial effect was neutralized by the free radical scavenger α-tocopherol, suggesting the involvement of radicals in executing the antibacterial effect. Importantly, CBD not only prevented the biofilm formation of G. vaginalis but also reduced the metabolic activity and biofilm biomass of preformed, mature biofilms. Real-time PCR analysis of G. vaginalis treated with CBD for 6 h showed an increase in the expression of biofilm-associated genes, suggesting that the antibiofilm activity of CBD is mainly due to its antibacterial effect. CBD did not alter the ability of G. vaginalis to adhere to HeLa cervical carcinoma cells and CBD-treated bacteria were still phagocytosed by RAW264.7 macrophages. Conclusions: Our study shows that CBD exhibits antibacterial and antibiofilm activities against G. vaginalis clinical isolates and is thus a potential drug for the treatment of vaginosis caused by this bacterium. Full article

The leaves of Ginkgo biloba have been used in treating freckles and effectively reducing cough and sputum in folk medicines. Recently, investigations into the correlation between ginkgo leaves and the proliferative activity of osteogenic differentiation have been conducted. However, bioactive compounds that enhance osteogenesis or exhibit osteoporosis prevention from G. biloba have not been fully identified. Phytochemical investigation of the MeOH extract of G. biloba leaves led to the isolation and identification of a new biflavonoid glycoside, (aS)-glucosciadopitysin (1), along with five flavonoids (2–6), through LC/MS-guided isolation approach. The structure of the new compound 1 was elucidated by the spectroscopic methods, including 1D and 2D NMR analysis, as well as HR-ESIMS. The absolute configuration of sugar moiety was established through acid hydrolysis, followed by chemical derivatization reaction and the axial chirality arising from the biaryl system with substituents was determined by electronic circular dichroism (ECD) calculations. The isolated flavonoids (1–6) were tested for their effects on mesenchymal stem cell (MSC) differentiation at 20 μM using Oil Red O and alkaline phosphatase (ALP) staining. Ginkgetin (2) was further evaluated for osteogenic activity on C3H10T1/2 cells at concentrations of 1, 2.5, 5, and 10 μM for 10 days. ALP staining and RT-PCR assessed the gene expression of osteogenic markers ALP and osteopontin (OPN). Ginkgetin (2) demonstrated the strongest osteogenic activity, significantly increasing the expression of ALP (12.5-fold) and OPN (4.0-fold) at 10 μM, comparable to the positive control, oryzativol A. Ginkgetin (2) shows potential as a therapeutic agent for osteopenia by promoting osteogenesis in MSCs, suggesting its promising role in treating osteoporosis. Full article

Emerging contaminants (ECs), encompassing pharmaceuticals, personal care products, pesticides, and industrial chemicals, represent a growing threat to ecosystems and human health due to their persistence, bioaccumulation potential, and often-unknown toxicological profiles. Addressing these challenges necessitates advanced analytical tools capable of detecting and quantifying trace levels of ECs in complex environmental matrices. This review highlights the pivotal role of mass spectrometry (MS) in monitoring ECs, emphasizing its high sensitivity, specificity, and versatility across various techniques such as Gas Chromatography-Mass Spectrometry (GC-MS), Liquid Chromatography-Mass Spectrometry (LC-MS), and High-Resolution Mass Spectrometry (HR-MS). The application of MS has facilitated the real-time detection of volatile organic compounds, the comprehensive non-targeted screening of unknown contaminants, and accurate quantification in diverse matrices including water, soil, and air. Despite its effectiveness, challenges such as matrix interferences, a lack of standardized methodologies, and limited spectral libraries persist. However, recent advancements, including hybrid MS systems and the integration of artificial intelligence (AI), are paving the way for more efficient environmental monitoring and predictive modeling of contaminant behavior. Continued innovation in MS technologies and collaborative efforts are essential to overcome existing challenges and ensure sustainable solutions for mitigating the risks associated with emerging contaminants. Full article

Salix koreensis Anderss (Salicaceae), commonly referred to as Korean willow, is native to East Asia, particularly Korea and China, and it has been used in traditional Korean folk medicine for its potent anti-inflammatory, analgesic, and antioxidant properties. In our ongoing research efforts to discover biologically new natural products, phytochemical analysis on an ethanolic extract of S. koreensis twigs yielded the isolation and identification of ten phenolic compounds (1–10), including a newly discovered phenolic glycoside (1) named isograndidentatin D, isolated via HPLC purification. The structure of compound 1 was determined through extensive 1D and 2D NMR spectral data analysis and high-resolution electrospray ionization mass spectrometry (HR-ESIMS). Its absolute configuration was established using DP4+ probability analysis combined with gauge-including atomic orbital NMR chemical shift calculations and chemical reaction methods. The other known compounds were identified as isograndidentatin B (2), trichocarposide (3), glanduloidin C (4), tremuloidin (5), 3-O-acetylsalicin (6), 2-O-acetylsalicin (7), salicin (8), salireposide (9), and coumaric acid (10), confirmed by comparing their NMR spectra with previously reported data and further verified through liquid chromatography/mass spectrometry (LC/MS) analysis. The isolated compounds 1–10 were tested for their anti-Helicobacter pylori activities. Among these, compounds 4 and 5 demonstrated moderate anti-H. pylori activity at a concentration of 100 μM. Specifically, compound 5 showed an inhibitory activity of 35.9 ± 5.4%, making it slightly more potent than compound 4, with 34.0 ± 1.0% inhibition. These results were comparable to that of quercetin, a known anti-H. pylori agent used as a positive control in this study, which showed 38.4 ± 2.3% inhibition. The remaining compounds exhibited very weak inhibitory effects. This study highlights the potential of S. koreensis twigs as a valuable natural source of bioactive compounds for therapeutic applications against H. pylori. Full article

Mass spectrometry (MS) is the only instrumental analytical technology that utilizes unique properties of matter, that is, its mass (m) and electrical charge (z). In the magnetic and/or electric fields of mass spectrometers, electrically charged native or chemically modified (millions) endogenous and (thousands) exogenous substances, the analytes, are separated according to their characteristic mass-to-charge ratio (m/z) values. Mass spectrometers coupled to gas chromatographs (GC) or liquid chromatographs (LC), the so-called hyphenated techniques, i.e., GC-MS and LC-MS, respectively, enable reliable determination of the concentration of analytes in complex biological samples such as plasma, serum, and urine. A particular technology is represented by inductively coupled plasma-mass spectrometry (ICP-MS), which is mainly used for the analysis of metal ions. The highest analytical accuracy is reached by using mass spectrometers with high mass resolution (HR) or by tandem mass spectrometers, as it can be realized with quadrupole-type instruments, such as GC-MS/MS and LC-MS/MS, in combination with stable-isotope labeled analytes that serve as internal standards, like a standard weight in scales. GC-MS belongs to the oldest and most advanced instrumental analytical technology. From the very beginning, GC-MS found broad application in basic and applied research sciences. GC-MS has played important roles in discovering biochemical pathways, exploring underlying mechanisms of disease, and establishing new evidence-based pharmacological therapy. In this article, we make an inventory of the use of instrumental mass spectrometry in the life sciences and attempt to provide a perspective study on the future of analytical mass spectrometry in clinical science, mainly focusing on GC-MS and LC-MS. We used information freely available in the scientific database PubMed (retrieved in August–November 2024). Specific search terms such as GC-MS (103,000 articles), LC-MS (113,000 articles), and ICP-MS (14,000 articles) were used in the Title/Abstract in the “PubMed Advanced Search Builder” including filters such as search period (1970–2024). In total, around 103,000 articles on GC-MS, 113,000 articles on LC-MS (113,000), and 14,000 articles on ICP-MS were found. In the period 1995–2023, the yearly publication rate accounted for 3042 for GC-MS articles and 3908 for LC-MS articles (LC-MS/GC-MS ratio, 1.3:1). Our study reveals that GC-MS/MS, LC-MS/MS, and their high-resolution variants are indispensable instrumentations in clinical science including clinical pharmacology, internal and forensic medicine, and doping control. Long-tradition manufacturers of analytical instruments continue to provide increasingly customer-friendly GC-MS and LC-MS apparatus, enabling fulfillment of current requirements and needs in the life sciences. Quantitative GC-MS and GC-MS/MS methods are expected to be used worldwide hand in hand with LC-MS/MS, with ICP-MS closing the gap left for metal ions. The significance of analytical chemistry in clinical science in academia and industry is essential. Full article

Plant triterpenoids represent a diverse group of secondary metabolites and are thought to be valuable for therapeutic applications. For drug development, lead optimization, better knowledge of biological pathways, and high-throughput detection of secondary metabolites in plant extracts are crucial. This paper describes a qualitative method for the rapid and accurate identification of various triterpenoids in plant extracts using the LC-HR-ESI-MS/MS tool in combination with the data-dependent acquisition (DD) approach. A total of 44 isolated, purified, and characterized triterpenoids were analyzed. HR-MS spectra and tandem mass spectra (MS/MS) of each compound were recorded in the positive ionization mode in two different sets of collisional energies, i.e., (25–62.5 eV), and fixed collisional energies (10, 20, 30, and 40 eV). As a result, three triterpenoids were identified in all plant extracts using the retention time, high-resolution mass spectra, and/or MS/MS spectra. The developed method will be helpful with other plant extracts/botanicals, as well as in the search for new triterpenoids in the kingdom Plantae. Full article

Developing new nanomaterials and performing functionalization to increase their photocatalytic capacity are essential in developing low-cost, eco-friendly, and multipurpose-capacity catalysts. In this research, SnO₂/Se-doped quantum dots (QDs) covered with glycerol (SnO₂/Se-GLY) were synthesized using microwave irradiation. Then, their cover was replaced with glutaraldehyde through a ligand exchange procedure (SnO₂/Se-GLUT). The XRD analyses confirmed a tetragonal rutile structure of SnO₂. The HR-TEM analysis confirmed the generation of QDs with a size around 8 nm, and the optical analysis evidenced low bandgap energies of 3.25 and 3.26 eV for the SnO₂/Se-GLY and SnO₂/Se-GLUT QDs, respectively. Zeta-sizer analysis showed that the hydrodynamic sizes for both nanoparticles were around 230 nm (50 mg/L), and the zeta potential confirmed that SnO₂/Se-GLUT QDs were more stable than SnO₂/Se-GLY QDs. The cover-modified QDs (SnO₂/Se-GLUT) showed a higher and faster adsorption capacity, followed by a slower photocatalytic process than the original QDs (SnO₂/Se-GLY). The QTOF-LC-MS analysis confirmed MB degradation through the identification of intermediates such as azure A, azure B, azure C, and phenothiazine. Adsorption isotherm analysis indicated Langmuir model compliance, supporting the high monolayer adsorption capacity and efficiency of these QDs as adsorbent/photocatalytic agents for organic pollutant removal. This dual capability for adsorption and photodegradation, along with the demonstrated reusability, highlights the potential of SnO₂/Se QDs in wastewater treatment and environmental remediation. Full article