Search Results (2,745)

Larrea ameghinoi Speg., an endemic species of Argentine Patagonia traditionally used in folk medicine to treat fever, stomach disorders, respiratory conditions, back pain, and as an emmenagogue, among others, still remains chemically and biologically underexplored compared to the other four members of the genus. This study aimed to perform a comprehensive metabolomic characterization of methanolic extracts from two populations (EMLaSAO and EMLaMAQ) using ultra-high-resolution liquid chromatography coupled with electrospray ionization quadrupole time-of-flight mass spectrometry (UHPLC–ESI–QTOF–MS) and to evaluate their antioxidant, antimicrobial, and enzyme-inhibitory activities of relevance to human health. Thirty-three compounds were tentatively identified by extensive UHPLC–MS analysis, including flavones, two major lignans, and oleanane-type triterpenes. Both extracts exhibited high phenolic content (215–239 mg of gallic acid equivalents (GAE)/g extract) and strong free radical scavenging activity, as evidenced by 2,2-diphenyl-1-picrylhydrazyl (DPPH, EC₅₀ ≈ 10 μg/mL), ferric-reducing antioxidant power (FRAP), and Trolox equivalent antioxidant activity (TEAC) assays. In addition, significant inhibition of butyrylcholinesterase (IC₅₀ ≈ 50 μg extract/mL) and α-glucosidase, together with selective antibacterial activity against methicillin-sensitive and resistant Staphylococcus aureus (MIC = 125 μg extract/mL), were recorded. These findings suggest that L. ameghinoi possesses a distinctive phytochemical composition conferring multitarget bioactivity, differing from other Larrea species dominated by lignans such as nordihydroguaiaretic acid (NDGA) and its derivatives. Overall, this work supports the potential of L. ameghinoi as a novel source of bioactive metabolites for managing oxidative stress-related disorders and opportunistic infections. This warrants future in vivo studies investigating biological activities associated with oxidative stress and their relevance to human health. Full article

The rising incidence of viral infections demands the creation of innovative, biocompatible antiviral drugs with broad-spectrum effectiveness. This study combines the green synthesis, optimization, and characterization of silver nanoparticles (AgNPs) utilizing Dacryodes edulis (D. edulis) extract, assessing their antiviral, and antimicrobial characteristics. AgNPs were synthesized through the bio-reduction of silver nitrate with D. edulis water extract as a reducing, capping and stabilizing agent. The synthesis was refined through a Design of Experiments methodology. The characterization techniques, UV-Vis, Fourier-transform infrared, transmission electron microscopy, and dynamic light scattering, validated the successful synthesis of AgNPs with an average size of 101.56 ± 28.22 nm (TEM) and 156 ± 0.81 nm (DLS), a polydispersity index of 0.34, and a zeta potential of −22 mV. High-resolution liquid chromatography–tandem mass spectrometry analysis identified some bioactive compounds which enhance the antimicrobial and antiviral properties of the samples. Enzyme kinetics experiments revealed substantial inhibitory efficacy against the SARS-CoV-2 papain-like protease (PL-pro), with AgNPs exhibiting a lower IC₅₀ (0.271 ± 0.051 mg/mL) than the D. edulis extract (0.337 ± 0.043 mg/mL). The AgNPs exhibited MIC of 0.063 mg/mL for E. coli, 0.125 mg/mL for S. aureus and 0.08 mg/mL for S. pyrogens. The corresponding MBC values were 0.125 mg/mL, 0.25 mg/mL and 0.31 mg/mL, respectively. The fungal strains C. glabrata and C. albicans displayed MIC of 0.63 mg/mL and 0.31 mg/mL, respectively, and MBC values of 0.63 mg/mL and 0.31 mg/mL, respectively. This study underscores the potential of D. edulis-derived AgNPs as a cost-efficient, environmentally sustainable, and highly bioactive antibacterial and antiviral nanomaterial, facilitating the advancement of nanotechnology-based therapies for viral infections. Full article

Per- and polyfluoroalkyl substances (PFAS) are persistent contaminants that require very strict performance criteria from the methods that want to analyze them in food for research or regulatory purposes. This systematic literature review tried to evaluate Quick, Easy, Cheap, Effective, Rugged, Safe (QuEChERS) extraction methodologies coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) and high-resolution mass spectrometry (HRMS) for PFAS determination in food. Peer-reviewed articles (2010–2025) were eligible if they analyzed PFAS in food matrices using QuEChERS extraction protocols with LC-MS/MS or HRMS and reported performance and/or validation data. Scopus, WoS and Google Scholar were searched up to 18 December 2025. Due to heterogeneity in matrices, PFAS panels and reported validation metrics, no meta-analysis was performed, and the results were synthesized narratively. Twenty-four studies met the inclusion criteria. Most methods used acidified acetonitrile (ACN)-based QuEChERS workflows and achieved limits of quantification (LOQ) reported to be compatible with EU Regulation 2023/915 and Commission Implementing Regulation 2022/1428. Analytical scope expanded from 9 to 15 legacy PFAS to >40 analytes. Short-chain PFAS analyses in vegetable matrices and methods from developing countries are underrepresented. QuEChERS-based LC-MS/MS and HRMS methods support regulatory PFAS monitoring and PFAS research. The main limitation of this review is the heterogeneity of included studies and the absence of formal meta-analysis. Full article

Emerging contaminants (ECs) and microplastics (MPs) are increasingly detected in surface waters, wastewaters, and drinking water, often as complex mixtures, transformation products, and particle-associated burdens that challenge routine monitoring. This critical review examines current analytical strategies for the detection and characterization of both molecular and particulate emerging contaminants in aquatic systems, with particular emphasis on their relevance to environmental and human health risk assessment. For molecular ECs, targeted LC–MS/MS and GC–MS and GC–MS/MS approaches are evaluated alongside high-resolution mass spectrometry (HRMS)-based suspect and non-target screening, retrospective data mining, and transformation-product elucidation. For MPs, particle-resolved vibrational spectroscopy including µ-FTIR and µ-Raman is critically assessed in comparison with complementary thermal analysis methods, such as pyrolysis–GC–MS and thermal extraction–desorption GC–MS (TED–GC–MS). Particular attention is given to the influence of sampling design, matrix-adapted sample preparation, analytical confidence, and method-dependent size and polymer coverage on data quality and interstudy comparability. The review further highlights the risks of ECs in relation to exposure pathways, mixture effects, and the potential carrier role of MPs for ECs, additives, and microorganisms. Finally, key priorities are identified for next-generation monitoring frameworks, including harmonized workflows, transparent confidence reporting, and stronger integration of analytical evidence with fate, exposure, and risk assessment. Full article

Ring chromosome 14 (RC14) syndrome is an ultra-rare disorder characterized by drug-resistant epilepsy, intellectual disabilities, autism, and recurrent infections, suggesting a possible underlying immune dysregulation. We analyzed immunoglobulin G (IgG) N-glycosylation profiles in six RC14 patients and compared them with age-matched healthy controls using ultra-high-performance liquid chromatography (UHPLC) coupled with fluorescence detection (FLR) and high-resolution electrospray ionization mass spectrometry (ESI-MS). Patients showed decreased galactosylation and sialylation, resembling pro-inflammatory patterns observed in autoimmune diseases. These alterations were not observed in total serum glycoproteins, indicating a selective effect on IgG. One patient treated with intravenous immunoglobulin (IVIG) showed clinical improvement, which led us to investigate causality. Full article

Human follicular development depends on coordinated communication between granulosa cells (GCs) and oocytes through endocrine cues, direct contacts, and extracellular vesicles (EVs). Exosomes are key EV mediators of intrafollicular signaling, but their cargo and functions in gonadotropin-stimulated GCs remain poorly defined. The human granulosa-like tumor cell line KGN was used to investigate exosome secretion and protein composition following human chorionic gonadotropin (hCG) stimulation. Exosomes were isolated by ultracentrifugation, characterized via nanoparticle tracking analysis (NTA), Scanning Electron Microscopy (SEM) and Western blotting, and analyzed using high-resolution mass spectrometry. Comparative proteomics integrating exosomal profiles with the whole secretome were performed, followed by bioinformatic analyses of protein networks, gene ontology, and pathway enrichment. hCG reshaped exosomal cargo, identifying 59 proteins enriched in exosomes, including Integrin α3 (ITGα3), Galectin-3-binding protein (LGALS3BP), tetraspanins (CD63, CD151), and proteasome subunits. Functional enrichment indicated roles in extracellular matrix remodeling, integrin signaling, proteostasis, and steroidogenesis. Comparison with the secretome revealed distinct protein distributions, supporting selective exosomal packaging. Western blot confirmed increased ITGα3 and LGALS3BP levels in exosomes upon hCG treatment. In conclusion, hCG modulates exosome cargo composition in granulosa cells, uncovering a novel mechanism of extracellular regulation. Full article

Medium-throughput forensic toxicology laboratories are increasingly expected to detect highly polar metabolites while working under tight resource and time constraints. To meet these requirements, a workflow is proposed that includes two stages: The first is computational metabolite prediction, followed by capillary zone electrophoresis (CZE), and the second stage is mass spectrometry (MS). The predictive step generates plausible metabolites and relevant physicochemical properties, which help guide early separation strategies. CZE then provides a rapid, low-cost way to test these predictions, identify informative samples, and exclude those unlikely to yield meaningful findings. Only samples that warrant further investigation proceed to targeted LC–MS/MS or high-resolution MS for confirmation. This approach shifts analytical effort toward the least resource-intensive stages, reducing unnecessary MS runs and improving turnaround time without compromising evidentiary standards. In practice, the workflow also improves day-to-day laboratory efficiency by overcoming equipment limitations and helping analysts focus on samples with genuine interpretive value. This stepwise combination of techniques is therefore suitable for routine forensic casework, where analytical decisions must be transparent, reproducible, and defensible. Full article

Rhodamine 110 (R110) peptide conjugates are widely used fluorogenic substrates in proteolytic assays; however, their inherent symmetry results in two identical hydrolysis sites, complicating their application as well-defined substrates. Here, we report a preparative enzymatic strategy for the desymmetrization of the symmetric derivative (Acetyl-Leu-Pro-Lys)₂-R110 using the bovine trypsin variant D189S. Due to pronounced differences in the rates of the two sequential hydrolysis steps, a mono-substituted intermediate accumulates under controlled reaction conditions. On a preparative scale, Acetyl-Leu-Pro-Lys-R110 was generated by partial hydrolysis and isolated by preparative HPLC in 28.8% yield and 95.8% purity. The structure of the asymmetric product was fully characterized by NMR and high-resolution mass spectrometry. This work demonstrates that selective enzymatic hydrolysis provides a simple and effective preparative route to asymmetric Rhodamine 110 derivatives, offering a practical alternative to conventional multistep synthetic approaches and enabling improved substrate design for kinetic studies. Full article

This study provides a comprehensive overview of emerging contaminants in water resources. It includes a global perspective with specific insights from Portugal. Following PRISMA 2020 guidelines, peer-reviewed studies published between 2020 and 2025 were critically assessed to identify patterns of contamination, monitoring gaps and technological readiness levels. Results indicate frequently detected emerging contaminants including pesticides, antibiotics and antidepressants in surface water, groundwater and wastewater systems. Advanced analytical methods, particularly liquid chromatography coupled with high-resolution mass spectrometry, stands out as the main detection technique, allowing the identification of trace levels of contaminants. These techniques also support the identification of pollution patterns associated with agriculture, urban and industrial effluents. However, significant asymmetries persist between international and Portuguese research. Particularly evident in systematic monitoring networks and integrated risk assessment approaches. Conventional water/wastewater treatment plants show limited removal efficiency, while advanced oxidation processes, adsorption technologies and microalgae-based systems demonstrate promising but variable performance depending on scale and operational maturity. The findings highlight gaps between scientific advances and regulatory implementation, emphasizing the need for strengthened monitoring frameworks and technology scale-up strategies. They also call for improved integration between science, governance, and sustainability policies to ensure resilient water resource management in line with the Sustainable Development Goals. Full article

This study investigated the chemical composition of the essential oil (EO) and the phenolic profiles of methanol extracts from Satureja boissieri Hausskn. ex Boiss. EO analysis by Gas Chromatography–Mass Spectrometry (GC-MS) identified carvacrol (45.2%), cymene (26.0%) and γ-terpinene (17.5%) as the primary constituents. Phenolic profiles were quantified via Liquid Chromatography–High-Resolution Mass Spectrometry (LC-HRMS), revealing syringic acid (56,647.96 mg/kg extract), rosmarinic acid (47,777.98 mg/kg extract) and hesperidin (6353.49 mg/kg extract) as major components in the extract. The antioxidant potential was evaluated through three distinct radical scavenging assays (DPPH, ABTS and DMPD) and the determination of ferric (Fe³⁺) and cupric (Cu²⁺) reducing capacities. Notably, S. boissieri exhibited potent antioxidant activity, with IC₅₀ values of 11.74 µg/mL for DPPH and 9.90 µg/mL for ABTS radical scavenging, demonstrating performance comparable to standard antioxidants such as α-tocopherol (11.31 and 8.37 µg/mL, respectively). Furthermore, the in vitro inhibitory activities against acetylcholinesterase (AChE) and butyrylcholinesterase (BChE) enzymes were evaluated. While both extracts exhibited similar and significant AChE inhibition (35.3% and 32.4%, respectively), the essential oil was notably more potent against BChE than the methanol extract. These findings suggest that S. boissieri is a significant source of bioactive compounds with promising antioxidant and neuroprotective potential for pharmaceutical applications. Full article

The multidirectional bioactivity of betulin (BN), its widespread occurrence in plants, relatively low toxicity, and acceptable safety profile make it an attractive scaffold for scientific research and potential therapeutic applications. Due to the presence of reactive functional groups (C-3-OH and C-28-OH), BN is an interesting source of new semisynthetic bioactive compounds obtained via structural modifications of the parent backbone. In our study, we designed new BN–amino acid (BNAA) molecular hybrids, aiming to exploit synergistically the properties of both components. We prepared and evaluated a total of 18 new compounds for antitumor activity against the two human cancer cell lines (HCT 116 and MCF-7) and one non-cancerous cell line (NHDF) using a standard Cell Counting Kit-8 (CCK-8) assay. The potential signaling pathways of the obtained BN derivatives were identified based on the measurement of p21 and Bax mRNA expression levels using the RT-qPCR method. We successfully synthesized a series of new BN hybrids by conjugation of the C-3 and C-28 hydroxyl groups via a succinyl (-CO-CH₂-CH₂-CO-, Suc) linker with selected amino acid methyl esters. The structures of all obtained BNAA molecular hybrids were confirmed by spectroscopic analysis (¹H and ¹³C NMR) and high-resolution mass spectrometry (HR-MS). Analysis of the biological activity of the obtained BN derivatives indicated that both the attached amino acids and the substituents at C3 carbon alter BN activity. The obtained BN–amino acid hybrids represent a useful platform for further optimization, especially derivatives (3a, 3e, 3f, and 7d), which showed the most relevant biological profiles in this study. Full article

Recent evidence highlights the therapeutic potential of Astragali radix-Huaier fermentation products for hyperuricemia treatment, although the dynamics of the fermentation process remain poorly understood. This study employed high-resolution mass spectrometry and untargeted metabolomics for real-time monitoring of chemical components and hypouricemic activity throughout fermentation. The results revealed significant alterations in the chemical composition, with distinct sample separations observed on days 7, 14, 21, and 28. A total of 33 differential components were identified, including 20 flavonoids and 13 saponins, eight of which showed notable changes. Polysaccharides and saponins were found to correlate positively with the uric acid-lowering effect. On day 21, the levels of total polysaccharides and cycloastragenol-6-glucoside, a saponin derivative, peaked, coinciding with the highest hypouricemic activity of the Astragalus fungal fermentation products. This study provides the first evidence of dynamic changes in the chemical profile and pharmacological activity of Astragali radix-Huaier during fermentation, paving the way for optimizing fermentation processes and developing medicinal and dietary products based on Astragali radix. Full article

The Saudi Arabia National Newborn Screening (NBS) program is a pillar of public health, offering timely detection of treatable, life-threatening, or disabling conditions in neonates. This comprehensive review critically examines the current laboratory diagnostic practices employed for metabolite analysis within this program. It focuses primarily on biochemical NBS conducted via dried blood spot testing and evaluates the methodologies, technical challenges, and stringent quality assurance measures that underpin successful screening. This review examines the critical role of tandem mass spectrometry, sample integrity protocols, and the establishment of robust cutoff values. Furthermore, this review explores persistent challenges such as false-positive and false-negative results, ethical and logistical hurdles in global implementation, and the transformative potential of recent advancements, including the integration of genomics and high-resolution metabolomics. In addition, this review explores the future of the program, highlighting the transformative potential of high-resolution metabolomics and the integration of genomic sequencing to ensure early diagnosis and intervention. Full article

This study focuses on the search and determination of organic pollutants in aerosol particles (PM_2.5) collected in Arkhangelsk, the largest urban agglomeration in the Arctic, during winter and summer periods. Thermal desorption gas chromatography coupled with high-resolution mass spectrometry was applied for non-targeted screening of atmospheric aerosols, enabling the detection of compounds at low concentrations ranging from 10 pg/m³ to several ng/m³. Representatives of various chemical classes were detected in samples from both seasons, including CHO compounds (with phthalates as the predominant subgroup), nitrogen-containing compounds (e.g., pyridines, quinolines, nicotine), phenols and monoaromatics, as well as polycyclic aromatic hydrocarbons and their oxygenated derivatives. In winter, PAHs and oxy-PAHs significantly predominated, likely due to increased combustion of fossil fuels and biomass for heating purposes. A total of approximately 300 compounds were identified via non-targeted screening, of which 32 were confirmed and quantified using authentic reference standards across six chemical classes. Seasonal variations in both the composition and concentration levels highlight the impact of local emission sources and atmospheric conditions on the organic aerosol profile in this arctic urban environment. Full article

The growing interest in epitranscriptomes has emphasized the need for accurate quantification of RNA modifications. However, the stability of RNA modifications under different experimental conditions remains poorly characterized. In this study, we use N1-methyladenosine (m¹A) as a model for assessing stability. After exposing m¹A ribonucleoside to various conditions that are commonly used in RNA protocols, the sample was analyzed using untargeted high-resolution mass spectrometry. Under alkaline or neutral pH, different extents of m¹A were converted to N6-methyladenosine (m⁶A). Complete m¹A-to-m⁶A conversion occurred at elevated temperatures. The m¹A-to-m⁶A conversion was also dependent on the initial m¹A concentration; the higher the concentration, the higher the rate of conversion. This poses a challenge to comparative studies if the initial amount of m¹A in the control and sample of interest are not equal. No demethylation or depurination was detected. However, trace amount of N1-methylinosine was detected as a result of non-enzymatic deamination of m¹A. Furthermore, the m¹A-to-m⁶A conversion was consistently observed in a biological sample. To eliminate the bias that resulted from m¹A-to-m⁶A conversion, the standard addition method was adopted. This report highlighted the challenges of having different extents of m¹A-to-m⁶A conversion under specific experimental conditions and demonstrated a viable solution for resolving the issue. Full article