Search Results (193)

The complexity of the milk matrix, driven by its lipid-rich composition, complicates pesticide residue analysis. This study developed a simplified and robust analytical procedure for the quantification of 250 pesticides in cow’s milk. Sample preparation involved acidified ethyl acetate extraction followed by centrifugation at 0 °C. A subsequent clean-up step was performed using micro solid-phase extraction (μSPE) in a 96-well format with the enhanced matrix removal-lipid (EMR-lipid) sorbent. Final extracts were analyzed by gas chromatography coupled to high-resolution mass spectrometry (GC-Q-Orbitrap-MS). Method validation demonstrated satisfactory linearity within the 5–100 µg/L range, recoveries between 70.6% and 119.8%, and precision, expressed as relative standard deviation (RSD), was acceptable for both intraday (1.8–19.2%) and interday (1.6–18.5%) conditions. The limit of quantification (LOQ) was set at 10 µg/kg for all compounds. The method was applied to 23 commercial cow’s milk samples, and no pesticide residues were detected above the current European Union (EU) maximum residue limits (MRLs). Full article

Objective: To overcome the extremely low oral bioavailability of ginsenosides in traditional ginseng preparations, this study aimed to evaluate the efficacy of a novel ginseng-derived carbon quantum dots (G-CQDs) delivery system and to elucidate its core bioactive constituents and integrated mechanisms of action. Methods: G-CQDs were prepared from ginseng roots via ultrahigh-speed nitrogen jet pulverization combined with far-infrared pulse-assisted hydrothermal carbonization. Their physicochemical properties were characterized by transmission electron microscopy, Fourier-transform infrared spectroscopy, and fluorescence spectroscopy. The in vivo effects of G-CQDs versus traditional ginseng aqueous extract (G-AE) were compared in C57BL/6 mice (n = 12/group) using the PRO-MRRM-8 Comprehensive Laboratory Animal Monitoring System for real-time, non-invasive phenotyping of energy metabolism parameters (respiratory quotient, heat production, and oxygen consumption). Systemic exposure to ginseng bioactives was profiled using UHPLC-Q/Orbitrap/LTQ high-resolution mass spectrometry, followed by bivariate correlation analysis to identify key bioactive components linked to efficacy. Results: Compared with G-AE, G-CQDs significantly enhanced whole-body energy metabolism—respiratory quotient +2.8%, heat production +6.7%, and locomotor activity +22.9% (p < 0.05). A total of 110 in vitro constituents, 35 blood prototypes, and 29 metabolites were identified. Correlation analysis revealed eight core bioactive clusters linked to the metabolic benefits; all showed higher systemic exposure with G-CQDs (range +9.2% to +265.8%), notably ginsenoside Re +69.6%, cinnamic acid + O + SO₃ +157.4%, and linolenic acid–GSH conjugate +265.8%. Conclusions: Carbon quantum dot technology significantly enhances the systemic exposure of ginseng bioactivities by improving solubility and enhancing gastrointestinal absorption, providing a molecular basis for its superior efficacy in regulating energy metabolism compared to conventional extracts. This study establishes a novel framework for developing high-value, bioavailability-enhanced nano-preparations from traditional medicines. Full article

Cancer metabolomics has become a powerful way of understanding tumor biology, identifying biomarkers and metabolites, and helping precision oncology. Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS), among many other analytical platforms, has gained popularity over the past two and a half decades due to its unique ability of directly analyzing metabolites in tissue with spatial resolution. This review will study 2000–2025 MALDI-based strategies for cancer metabolite detection, spanning from early proof-of-concept protein profiling to the development of high-resolution MALDI-MS imaging (MALDI-MSI), which is capable of mapping thousands of metabolites at near single-cell resolution. Its applications include the differentiation of tumor versus normal tissue, discovery of stage and subtype specific biomarkers, mapping of metabolic heterogeneity, and the visualization of drug metabolism in situ. Breakthrough technological milestones, such as the advanced matrices, on-tissue derivatization, MALDI-2 post-ionization, and the integration with Orbitrap or Fourier-transform ion cyclotron resonance (FT-ICR) platforms, have significantly improved the overall sensitivity, metabolite coverage, and spatial fidelity. Clinically, MALDI-MS has shown its purpose in breast, prostate, colorectal, lung, and liver cancers by providing metabolic fingerprints that are linked to tumor microenvironments, hypoxia, and therapeutic response. However, challenges such as the inclusion of matrix interface with low-mass metabolites, limited quantitation, ion suppression, and the lack of standardized procedures do not yet allow for the transition from translation to routine diagnostics. Even with these hurdles, the future of MALDI-MS in oncology remains in a good position with major advancements in multimodal imaging, machine learning-based data integration, portable sampling devices, and clinical validation studies that are pushing the field towards precision treatment. Full article

Melicoccus bijugatus (Guinep) is traditionally consumed in the Caribbean and Latin America for its health benefits, yet its cardiovascular effects remain underexplored. This study investigated the therapeutic potential of Guinep by combining experimental and computational approaches. The biological evaluation of the Guinep extract was conducted by assessing the effects of modulating Angiotensin-Converting Enzyme (ACE), Angiotensin II Type 1 Receptor (AT1R), and Voltage-Gated Calcium Channels (VGCC) on vascular reactivity. Metabolites previously identified by high-resolution UHPLC-Q-Orbitrap mass spectrometry were further examined using in silico tools, including ADMET (Absorption, Distribution, Metabolism, Excretion, and Toxicity) prediction (pkCSM), biological activity prediction (PASS server), and molecular docking (AutoDock Vina) against cardiovascular targets (ACE: PDB 1O86, AT1R: PDB 4ZUD, VGCC: PDB 8WE8). Docking results revealed that phytochemicals such as isorhamnetin-3-O-glucoside and 3-O-caffeoylquinic acid displayed strong binding affinities with ACE (−9.3 and −8.5 kcal/mol), AT1R (−8.2 and −7.6 kcal/mol), and VGCC (−8.6 and −7.6 kcal/mol), in several cases matching or surpassing standard antihypertensive drugs. Key hydrogen bond interactions closely resembled those of reference ligands, suggesting pharmacophoric similarity. ADMET modeling confirmed favorable pharmacokinetic profiles and low predicted toxicity, supporting their drug-like potential. These findings are consistent with in vivo evidence of Guinep’s hypotensive, antioxidant, and vasodilatory properties. Vascular relaxation of Guinep extract was predominantly mediated by blockade of VGCC (53%) and AT1R (48%), while ACE inhibition accounted for 24%. Collectively, the results demonstrate that Guinep contains bioactive phytochemicals with multitarget cardiovascular activity, particularly as ACE, AT1R, and VGCC modulators. This study validates the traditional use of Guinep. Full article

Diterpenoid diester alkaloids (DDAs) are the primary toxic constituents in aconite herbs, while also being the key pharmacologically active components. Consequently, establishing rapid enrichment and highly sensitive analytical methods for DDAs is of critical importance. Herein, we developed and constructed a gas–liquid microextraction (GLME) device, which enables the rapid and selective enrichment of DDAs from complex matrices. The enriched extract can be directly analyzed by high-resolution Orbitrap mass spectrometry without requiring any further pretreatment. A comparative analysis of six commonly used Aconitum herbs medicines and their processed derivatives was conducted. Notably, GLME enhanced the mass spectrometric signals of DDAs by 3–4 orders of magnitude, facilitating the identification of 27 alkaloids, including 3 potential new compounds (15-Ethyl-13-deoxyanhydroaconitine, 13-Hydroxy-15-ethylanhydroaconitine and 8-eicosapentaenoic-benzoylmesaconine). It was found that among the tested samples, the DDAs response intensity of raw Caowu was the highest, and the DDA signals decreased significantly after processing. This result chemically validates the detoxification efficacy of traditional methods. The proposed GLME-MS strategy has the advantages of being green, economical, easy to operate, and highly selective (>1000-fold), which provides a technical reference for the rapid detection, safety assessment, and quality control of Aconitum herbs. Full article

Camellia oleifera Abel shell is an abundant lignocellulosic byproduct of the Chinese woody oil industry, which is currently underutilized. To achieve its high-value utilization, this study developed an innovative cascade process integrating ultrasound-assisted extraction and macroporous resin purification for the efficient preparation of purified polyphenols from the shell (P-CPCS). The major constituents were identified by quadrupole/Orbitrap high-resolution mass spectrometry (HPLC-Q-Exactive-MS: Biotech Pack Co., Ltd., Beijing, China) analysis. The optimized process significantly enhanced the polyphenol yield (40.05 ± 0.58 mg GAE/g dw) and purity (57.72%), surpassing conventional methods. P-CPCS exhibited exceptional multifunctional bioactivities, including potent antioxidant capacity (with low IC₅₀ values against DPPH, ABTS⁺·, and ·OH radicals), effective tyrosinase inhibition (whitening effect), and significant bacteriostatic effects against various pathogens. Furthermore, P-CPCS notably suppressed the LPS-induced inflammatory response in RAW264.7 macrophages by reducing NO overproduction. This work highlights a novel and efficient strategy for upcycling agricultural waste into a high-performance natural antioxidant, positioning P-CPCS as a promising ingredient for applications in functional foods, cosmetics, and biomaterial stabilization. Full article

Nonylphenols (NPs), widely used as emulsifiers in petroleum production and refining, are compounds of environmental concern, with endocrine-disrupting effects. They can be released during oil extraction and processing, carried into petroleum products, and subsequently emitted during downstream applications such as combustion. Despite these potential pathways, information on their occurrence in petroleum streams remains limited, partly due to the lack of reliable methods for measuring NPs in complex petroleum matrices. In this study, we developed an analytical method combining normal-phase chromatography (NPC), solid-phase extraction (SPE), and liquid chromatography–Orbitrap high-resolution mass spectrometry (LC–Orbitrap-HRMS) for NP determination in crude oils and petroleum products. NPC was performed using alumina (5% water deactivation) as the stationary phase. The column was eluted sequentially with n-hexane, n-hexane/dichloromethane (4:1 and 1:1, v/v), dichloromethane, and dichloromethane/methanol (2:1, v/v). The first three fractions were discarded, and the remaining two fractions were combined and further purified using a C₁₈ SPE cartridge to analysis. The method showed high recovery (82.8 ± 2.6%) and a low detection limit (1.0 ng/g) in crude oil. Application revealed widespread occurrence of NPs, with concentrations up to 784.4 ng/g in crude oils and up to 439.1 ng/g in refined fuels, indicating that these compounds can persist through refining and may be released during downstream use. These results demonstrate that the method is suitable for the routine monitoring of NPs in petroleum-related samples and provide a practical tool for supporting sustainable refining practices and improved environmental management in the upstream oil and gas sector. Full article

Wild mushroom poisoning is an emerging global food safety issue, especially in subtropical regions like southwestern China, where incidents are geographically clustered. Current detection methods are often time-consuming and overlook region-specific toxins. We developed a rapid, sensitive, and accurate method for the simultaneous detection of ten characteristic mushroom toxins prevalent in Guizhou, China. The method combines graphite multi-walled carbon nanotubes (G-MWCNTs) for sample preparation with Orbitrap high-resolution mass spectrometry (HRMS). Wild mushroom samples were extracted via ultrasonic-assisted methanol–water extraction, purified using G-MWCNTs, and separated on a Hypersil GOLD C18 column (100 mm × 2.1 mm, 1.9 μm). Gradient elution was performed with 0.1% formic acid + 0.01% ammonia and acetonitrile; quantification used the external standard method. The method achieved LODs of 0.005–0.2 mg/kg and LOQs of 0.015–0.6 mg/kg, with RSDs below 18.11% and excellent linearity (R² = 0.9936–0.9989). Among 45 wild mushroom samples, toxin levels ranged from 0.032 to 445.10 mg/kg, with a detection rate of 22.22%, suggesting notable poisoning risk. This method reduces pretreatment time while ensuring high analytical performance, offering a reliable tool for rapid toxin screening and supporting regional surveillance of wild mushroom poisoning. Full article

Spirulina (Arthrospira spp.) and klamath (Aphanizomenon flos-aquae) are widely consumed cyanobacteria-based food supplements valued for their nutritional and health-promoting properties. However, these products are susceptible to contamination by cyanotoxins, which are potent toxins produced by co-occurring cyanobacteria that may pose health risks to consumers. In this study, we applied an integrated targeted and suspect screening approach to comprehensively assess the presence of cyanotoxins in commercial spirulina- and klamath-based food supplements. Targeted analysis was performed using UHPLC-QqQ under dynamic multiple reaction-monitoring conditions optimized for the determination of twelve cyclic peptide cyanotoxins. Suspect screening was conducted using high-resolution mass spectrometry (HRMS) with a Q-Orbitrap analyser, applying a specific workflow to detect additional related compounds lacking analytical standards. The method enabled the detection and identification of multiple cyanotoxins, including microcystins, nodularin, and anabaenopeptins. The combination of targeted and suspect workflows allowed for a broader coverage of potential related cyanotoxins. Several cyanotoxins were detected in a klamath-based supplement, with high concentrations of microcystin-RR, while additional variants were identified through suspect screening. These findings highlight the need for routine monitoring and stricter regulatory oversight of cyanobacteria-based supplements to ensure consumer safety. 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

Polycyclic aromatic hydrocarbon (PAH) derivatives, specifically azaarenes and nitrated and oxygenated PAHs, are emerging contaminants of concern due to their increased toxicity and persistence compared to the parent PAHs. Despite their toxicity, their simultaneous analysis in complex matrices, such as in fumes emitted from bituminous mixtures, remains challenging due to limitations of conventional analytical techniques. To address this, an advanced methodology was developed using Ultra-High-Performance Liquid Chromatography coupled with High-Resolution Mass Spectrometry (UHPLC-HRMS Orbitrap Eclipse) equipped with an APCI source for the simultaneous identification and quantification of 14 PAH derivatives. Chromatographic and ionization parameters were optimized to ensure maximum sensitivity and selectivity. Following ICH Q2(R2) guidelines, the method was validated, demonstrating excellent linearity (R² > 0.99), high mass accuracy (≤5 ppm), strong precision (<15%), and excellent sensitivity. Limits of detection (LODs) ranged from 0.1 µg L⁻¹ to 0.6 µg L⁻¹ and limits of quantification (LOQs) ranged from 0.26 µg L⁻¹ to 1.87 µg L⁻¹. The validated method was successfully applied to emissions from asphalt pavement materials collected on quartz filters under controlled conditions, enabling the identification and quantification of all 14 targeted compounds. These results confirm the method’s robustness and suitability for trace-level analysis of PAH derivatives in complex environmental matrices. Full article

This study investigates the compositional characteristics and quantitative differences of ginsenosides across various ginseng tissues, with a particular focus on the specific accumulation patterns of malonyl ginsenosides. Five tissue samples—ginseng fruit (F), leaf (L), taproot (TR), lateral root (LR), and fibrous root (FR)—were analyzed using Orbitrap Fusion high-resolution liquid chromatography–mass spectrometry. A total of 413 ginsenosides, including 33 standards, were identified, encompassing 172 protopanaxadiol (PPD)-type, 188 protopanaxatriol (PPT)-type, 14 oleanolic acid (OA)-type, and 12 ocotillol (OT)-type ginsenosides, of which 160 were malonyl ginsenosides. Statistical analysis revealed significant variations in the relative content per unit mass of malonyl ginsenosides across tissues, with the highest levels in fibrous roots, followed by fruits, lateral roots, leaves, and taproots. Distinct tissue-specific differences in malonyl ginsenoside types and quantities were observed: fruits exhibited 51 malonyl ginsenosides with significantly higher levels, compared to 8, 14, and 17 in lateral roots, fibrous roots, and leaves, whereas TR showed no significant enrichment. This study elucidates the diversity and unique distribution of malonyl ginsenosides in ginseng roots, leaves, and fruits, providing a valuable basis for the targeted selection of tissues with high malonyl ginsenoside content and the development of functional food and medicinal products. 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

Background: Chronic atrophic gastritis precancerous lesions (PL-CAG) are characterized by the atrophy of gastric mucosal glands, often accompanied by intestinal metaplasia or dysplasia. Timely intervention and treatment can effectively reverse its malignant progression and prevent the onset of gastric cancer. Bombyx Batryticatus (BB) exhibits a range of pharmacological effects, including anticoagulation, antiepileptic properties, anticancer activity, and antibacterial effects. However, the pharmacological basis and mechanisms underlying BB’s efficacy in treating PL-CAG remain unclear. Methods: A three-factor modeling approach was implemented to develop a rat PL-CAG model, while the MNNG-induced PLGC (precancerous lesions of gastric cancer) cell model was served as a cell PL-CAG model. UPLC-QE-Orbitrap-MS/MS (Ultra performance liquid chromatography-quadrupole-electrostatic field orbital trap high-resolution mass spectrometry) was utilized to perform an in-depth analysis of the components in the plasma extract of BB. Leveraging network pharmacology, molecular docking analyses, and experimental validation, we initially elucidated the potential mechanisms through which BB mediates its therapeutic effects on PL-CAG at both in vivo and in vitro levels. Results: Prototype compounds of 42 blood-entering components were identified by UPLC-QE-Orbitrap-MS/MS analysis. Network pharmacology analysis and molecular docking studies indicate that the core targets are primarily enriched in the PI3K-Akt signaling pathway, and the key components, including Nepitrin, Quercetin 3-O-neohesperidoside, Rutin, and others, exhibited stable docking conformations with the first eleven pivotal targets. Both in vivo and in vitro experiments validated that BB may effectively treat PL-CAG via modulation of the PI3K-Akt signaling pathway. Conclusions: The therapeutic efficacy of BB in the management of PL-CAG may be achieved through the synergistic interaction of multiple components and targets, which may be more closely related to the inhibition of the PI3K/AKT signaling pathway. This approach will establish a solid experimental foundation and provide essential data for the clinical application of BB in treating PL-CAG, while also facilitating further research initiatives. Full article

Yinhua Pinggan Granules (YPG) is a patented traditional Chinese medicine (TCM) compound prescription, with wide clinical application against cold, cough, and relevant diseases. However, the chemical profiles of YPG in vivo are still unknown, hindering further pharmacological and quality control (QC) researches. This study presents an ultra-high-performance liquid chromatography coupled with high-resolution orbitrap mass spectrometry (UHPLC-MS)-based method. Using the Compound Discoverer platform and a self-built ‘in-house’ compound database, the metabolic profiles and pharmacokinetics characters of YPG were investigated. Consequently, a total of 230 compounds (including 39 prototype components and 191 metabolites) were tentatively identified, in which the parent compounds were mainly flavonoids, alkaloids, and terpenoids, and the main metabolic pathways of metabolites include hydration, dehydration, and oxidation. The serum concentration of seven major representative compounds, including quinic acid, chlorogenic acid, amygdalin, 3′-methoxypuerarin, puerarin, glycyrrhizic acid, and polydatin, were also measured, to elucidate their pharmacokinetics behaviors in vivo. The pharmacokinetic study showed that the seven representative compounds were quantified in rat plasma within 5 min post-administration, with T_max of less than 2 h, followed by a gradual decline in concentration over a 10 h period. The method demonstrated excellent linearity (R² > 0.998), precision, and recovery (RSD < 15%). As the first systematic characterization of YPG’ s in vivo components and metabolites using UHPLC-MS, this study may contribute to comprehensively elucidate the metabolic profiles of the major components in YPG, and provide a critical foundation for further investigation on the QC and bioactivity research of YPG. Full article