Search Results (697)

Background: This study aimed to identify distinct metabolic signatures associated with disease progression by integrating high-resolution computed tomography (HRCT) visual scoring with comprehensive metabolomic profiling. Materials and Methods: This single-center, cross-sectional study enrolled 60 idiopathic pulmonary fibrosis/interstitial lung disease (IPF/ILD) patients with usual interstitial pneumonia pattern. Participants underwent standardized pulmonary function testing, HRCT imaging, and peripheral blood collection for metabolomic analysis using one-dimensional hydrogen nuclear magnetic resonance spectroscopy and ultra-high-performance liquid chromatography coupled to tandem mass spectrometry. Linear regression analysis integrated radiographic scores with metabolomic profiles, adjusted for multiple covariates. Results: Stable IPF/ILD exhibited moderate negative correlations between the six most significant metabolites and HRCT scores (r = −0.27 to −0.51), along with a high abundance of specific phospholipids (triacylglycerol, monoacylglycerol, phosphatidylglycerol, phosphatidylethanolamine, diacylglycerol), sphingomyelin, ceramide, and acylcarnitine. In contrast, progressive disease showed weak positive correlations between the six most significant metabolites and HRCT scores (r = 0.19–0.26), and moderate negative correlation between specific triacylglycerol species and HRCT scores (r = −0.37–0.4). Furthermore, metabolomic analysis in individuals with progressive disease revealed both high and low abundances of specific phospholipid species (including high and low triacylglycerol species, as well as low levels of phosphatidylglycerol, phosphatidylethanolamine, phosphatidylcholine, phosphatidylserine, and phosphatidylinositol), along with high levels of certain sphingomyelin, ceramide, taurine, and purine bases, and low levels of xanthine and lactic acid observed. Conclusions: Integration of systematic HRCT semi-quantitative scoring with metabolomic profiling successfully differentiated stable from progressive IPF/ILD through distinct molecular-radiographic signatures. Full article

Using reclaimed water for irrigation is an effective strategy in semi-arid regions facing water scarcity. However, this water may contain pharmaceutical residues, posing potential environmental and health risks. To ensure sustainable reuse, it is essential to study how these substances accumulate in soil and transfer to crops. The aim of this research was to develop and optimise a rapid Ultrasound-Assisted Extraction method combined with Ultra-High-Performance Liquid Chromatography–tandem Mass Spectrometry for quantifying 23 pharmaceuticals in non-cultivated soil. Following optimisation, 18 compounds were successfully extracted using a MeOH:H₂O ratio of 75:25. The detection and quantification limits were found to range from 0.52 to 0.5 ng·g⁻¹ and 1.75 to 35 ng·g⁻¹, respectively. The matrix effects and recoveries varied by compounds’ type and concentration, but most results were acceptable. The evidence suggested that some drugs underwent microbial degradation. Soil irrigated with reclaimed water via subsurface drip since 2012 occasionally contained four pharmaceuticals (caffeine, carbamazepine, tamoxifen, and venlafaxine) at low concentrations, while others were absent. This indicates the capacity of soil to act as a barrier, and highlights the importance of proper water management. The study concludes that reclaimed water reuse is safe if supported by efficient treatment and management, offering a promising approach for long-term sustainability in water-scarce regions. Full article

Aflatoxin M1 (AFM1), a hydroxylated metabolite of aflatoxin B1, is a persistent food safety hazard in the dairy production chain. This study investigated AFM1 occurrence in fermented dairy products collected from the Croatian market in spring 2025 and assessed associated dietary exposure risks. A total of 81 samples were analyzed using ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) following immunoaffinity column clean-up. AFM1 was detected in 48.1% of samples, with a mean concentration of 0.015 µg/kg. Products with thermophilic and probiotic bacterial cultures showed the lowest incidence rates, at 33.3% and 40.0%, respectively. Significantly higher AFM1 occurrence was found in Croatian samples than in imported ones (p < 0.05). Exposure assessment, based on estimated daily intake (EDI), hazard index (HI), and margin of exposure (MOE), identified toddlers and children as the most at-risk groups, with EDI ranging from 0.21 to 0.93 ng/kg bw/day, depending on AFM1 concentration. HI exceeded 1 even at mean AFM1 levels, while MOE fell below the safety threshold of 10,000 in worst-case scenarios, indicating potential health concerns. These findings underscore the need for continuous monitoring and targeted risk mitigation strategies for vulnerable populations, and support expanding regulatory limits to include processed dairy products. Full article

Evaluating the potential chronic health risks posed by pesticides to consumers is essential for ensuring food safety and protecting public health. An ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) method coupled with modified QuEChERS extraction was developed to simultaneously determine 26 pesticide residues in wheat grain and bran. Samples were extracted with acetonitrile with 2% (v/v) acetic acid and cleaned up using C₁₈ sorbent. Method validation demonstrated excellent linearity, accuracy, and precision. When applied to 48 wheat grain and 24 bran samples collected from major wheat-growing regions in China, 12 and 21 pesticides were detected at concentrations ranging from <0.005 to 1.785 mg kg⁻¹ and <0.01 to 2.188 mg kg⁻¹, respectively. Chronic hazard quotients (HQc) and acute hazard quotients (HQa) for all pesticides for grain and bran were far below the safety threshold of 100%. These results indicate that pesticide residues in wheat grain and bran present negligible chronic dietary risks to consumers across all age groups. Full article

In this study, the feasibility of tetracycline (TC) degradation in water using Fe–Mo co–supported biochar (FeMoBC) as catalyst combined with ozone and peroxymonosulfate (O₃/PMS) system is discussed. The experiment showed that the mineralization rate of TC by O₃/PMS/FeMoBC process reached 60.1% within 60 min, which was significantly higher than the treatment effect of O₃ or O₃/PMS system alone. Meanwhile, this process showed higher degradation efficiency under the background of raw water, and the loss of FeMoBC cycle attenuation performance was small. Twelve intermediates in the degradation of TC were identified by ultra-high performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS), and the possible degradation paths were inferred by quantum chemical calculation. In addition, the toxicity of intermediate products was evaluated by ecological structure–activity relationships (ECOSAR) and toxicity estimation software tool (T.E.S.T.) software, and the results showed that with the degradation of TC, its toxicity showed a downward trend as a whole. Therefore, this study confirmed that O₃/PMS/FeMoBC had high efficiency in degrading TC in actual water, which provided a new idea for the treatment of high concentration organic wastewater. Full article

The aim of this study is to investigate the occurrence of melamine and cyanuric acid in milk, baby food, and protein supplements collected in Croatia. A total of 56 samples were collected during 2022 and 2023 from retail stores in Zagreb, Croatia. Sample preparation involved acetonitrile extraction, followed by analysis using ultra-high-performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS). Cyanuric acid concentrations above the limit of quantification (LOQ) were found in five milk samples (33.3% detection frequency), with a range from 0.26 to 0.39 mg/kg and a mean concentration of 0.31 mg/kg. In protein supplements, melamine was detected above the LOQ in six samples (23% detection frequency), with a mean concentration of 0.30 mg/kg and concentrations ranging from 0.20 to 0.57 mg/kg. No concentrations above the LOQ were found in baby food samples. All detected values were below the EU maximum limits (2.5 mg/kg for general food and 1.0 mg/kg for baby food). The accuracy and reliability of the method were verified using certified reference material. This is the first study to confirm the presence of melamine and cyanuric acid in protein supplements and milk on the Croatian market. The detected levels do not indicate a potential health risk to consumers. Full article

Background/Objectives: Ergot alkaloids are mycotoxins produced mainly by fungi of the genus Claviceps, infecting a wide variety of plants, especially cereals. These toxins usually manifest as black, hardened sclerotia (ergots), though they may also be invisible when dispersed in grain. They pose a significant risk to animals and humans when present in contaminated cereals. They can cause ergotism, with vasoconstriction, ischemia, hallucinations, and in severe cases gangrene. This study was carried out in response to the European legislative actions which determine the permissible levels of ergot alkaloids in cereals. Historically, consumers manually removed visible sclerotia from grain, and farmers applied fertilizers or timed harvests to specific periods to mitigate contamination. However, these traditional methods have proven insufficient. We therefore explored advanced techniques for detecting and quantifying ergot-contaminated cereals, as well as methods for reducing ergot alkaloid concentrations. Methods: Searches were conducted in scientific databases including Google Scholar, PubMed, and Scopus to identify research articles, reviews, and experimental studies published mainly between 2012 and August 2025, including accepted or in-press manuscripts, with special attention to works from 2021 onward to capture the most recent advancements. Results/Conclusions: Ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) is the reference method for confirmatory, epimer-aware quantification of ergot alkaloids, and is already standardized. Recent QuEChERS-UHPLC-MS/MS workflows in cereal matrices, including oat-based products, routinely achieve limits of quantification of about 0.5–1.0 µg/kg with single-run analysis times of about 5–15 min. Rapid screening options complement, rather than replace, confirmatory mass spectrometry: magnetic bead-based immunoassays that use magnetic separation and a smartphone-linked potentiostat provide sub-hour turnaround and field portability for trained quality-assurance staff, although external validation and calibration traceable to LC-MS/MS remain prerequisites for routine use. In practice, operators are adopting tiered, orthogonal workflows (e.g., immunoassay or electronic-nose triage at intake followed by DNA-based checks on grain washings and LC–MS/MS confirmation, or hydrazinolysis “sum parameter” screening followed by targeted MS speciation). Such combinations reduce turnaround time while preserving analytical rigor. Biotechnology also offers potential solutions for reducing ergot alkaloid concentrations at the source. Finally, to enhance consumer safety, artificial intelligence and blockchain-based food traceability appear highly effective. These systems can connect all stakeholders from producers to consumers, allowing for real-time updates on food safety and rapid responses to contamination issues. This review primarily synthesizes advances in analytical detection of ergot alkaloids, while mitigation strategies and supply chain traceability are covered concisely as supporting context for decision making. Full article

Lichens are complex symbiotic systems known for synthesizing diverse secondary metabolites with documented antimicrobial, antioxidant, and antiproliferative activities. The present study focused on Pseudevernia furfuracea, a species widely distributed across Moroccan habitats. Two hydrodistillation-derived extracts (HE1 and HE2) were analyzed through ultra-high-Performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS) to characterize their metabolite composition, and their effects were evaluated on Jurkat cells, a representative human cell line of the immune system. As the results of the characterization, the main compounds identified were Caprolactam, N,N-Diethylaniline, Erucamide, and 4-Isopropylaniline. Cytotoxicity assessment revealed that both HE1 and HE2 decreased the viability of Jurkat cells in a concentration-dependent manner. The mean effective concentrations (EC₅₀) after 24 h of treatment were 53.79 ± 2.92 µg/mL for HE1 and 59.76 ± 2.01 µg/mL for HE2. Cell death mechanisms were further examined by flow cytometry, revealing that apoptosis predominated after 24 h of treatment, progressing mainly to late apoptotic stages after 48 h. In parallel, the expression levels of key cytokine genes, including IL-2, TNF-α, and IFN-γ, were quantified at the mRNA level to evaluate potential immunomodulatory effects. Up-regulation was observed in IL-2 after exposure to both extracts for 24 and 48 h, and in the case of IFN-γ after exposure to HE2 for 24 h; in contrast, HE1 and HE2 produced down-regulation in TNF-α at 24 h. These findings suggest that HE1 and HE2 have immunomodulatory activity in Jurkat cells. Further investigations are needed to elucidate the underlying mechanisms and to clarify how HE1 and HE2 influence immune responses in human systems. Full article

Background: Rifaximin is a non-aminoglycoside antibiotic utilized for the treatment of mastitis in cows, but its milk disposition kinetics, residue, and bacteriological status in lactating cow milk have hardly been reported. This study aimed to assess the milk disposition kinetics and residue of rifaximin in milk and to evaluate the bacteriological status in milk after intramammary treatment with rifaximin. Methods: An ultra-high-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) approach was developed to assess rifaximin concentrations in milk. Milk disposition kinetics parameters of rifaximin in cow milk were obtained by non-compartment model analysis. Rifaximin residues in milk were analyzed up to 108 h post-administration to estimate the withdrawal period. Clinically, the efficacy of Rifaximin Intramammary Infusion (Lactating Cow) was evaluated in mastitis cases caused by various pathogens and compared with lincomycin as the control drug, including clinical cure rate, bacteriological cure rate, and somatic cell count (SCC) at D21 post-treatment. Results: The C_max of rifaximin in milk was 54,273.3 ± 12,421.32 ng/mL, the area under the curve (AUC) was 340,731.8 ± 43,968.82 h⋅ng/mL, the T_1/2 was 5.57 ± 0.68 h, the mean resident time (MRT) was 7.3927 ± 1.34 h, and the area under the moment curve (AUMC) was 2,475,745 ± 230,305.1 h⋅h⋅ng/mL. Based on rifaximin residues in milk, the withdrawal period for cow milk was calculated to be 95.1 h. Clinically, Rifaximin Intramammary Infusion (Lactating Cow) demonstrated a clinical cure rate of 83.33% and a bacteriological cure rate of 76.67% in mastitis cases caused by various pathogens, with both rates being 10% higher than those of lincomycin. At D21 post-treatment, the rifaximin group had a significantly lower SCC than the lincomycin group (p < 0.05). Conclusions: Rifaximin exhibits favorable milk disposition kinetics, an acceptable withdrawal period of 95.1 h, and good clinical and bacteriological cure rates in bovine mastitis. These findings support rifaximin as a useful intramammary option and contribute to rational antimicrobial use and milk safety in dairy. Full article

In the context of the ten-year fishing ban on the Yangtze River, illegal poaching for profit persists. To support the enforcement of this ban and protect the river’s ecosystem, an efficient and precise method for distinguishing between wild and farmed common carp is essential. This study utilized ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) combined with metabolomics technology to analyze and compare the metabolic differences between wild and farmed common carp. Principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA) revealed a clear separation between the two groups, which was further verified by metabolic fingerprint profiles. Moreover, 16 metabolites with high discriminatory potential were identified from 491 differentially metabolites, such as phytosphingosine, succinic acid and threonine. In addition, a cluster analysis of the differential metabolites classified them into four classes: peptides, fatty acyls, steroids and steroid derivatives, and glycerophospholipids. Furthermore, candidate biomarkers, including 3-hydroxybutyrylcarnitine, 3-hydroxyhexanoylcarnitine and jasminoside were identified to potential distinguish wild populations. To our knowledge, this is the first study to apply metabolomics technology to differentiate wild from farmed common carp, providing a new theoretical basis for ecological restoration efforts in the context of the Yangtze River fishing ban. Full article

A method combining magnetic solid-phase extraction (MSPE) with ultra-high performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) was developed for the determination of diazepam residues in aquatic products. A novel magnetic nanoparticle material, Fe₃O₄@SiO₂@DVB-NVP, was synthesized and applied as an adsorbent for sample cleanup. The sample preparation procedure involved extraction with 1% ammonia–acetonitrile, followed by purification using the MSPE technique to efficiently remove matrix interferents. Chromatographic separation was achieved on an ACQUITY UPLC BEH C₁₈ column with a gradient elution program using a mobile phase composed of 0.1% formic acid–2 mM ammonium acetate solution and methanol. Detection was performed under multiple-reaction monitoring (MRM) mode with positive electrospray ionization (ESI⁺). Quantification was carried out using the external standard method. The synthesized magnetic material was characterized using SEM, TEM, FTIR, XRD, BET, and VSM, confirming its mesoporous structure, strong adsorption capacity, and excellent magnetic responsiveness. The method demonstrated good linearity over the concentration range of 0.25–50 μg/L (r² = 0.997). The limits of detection and quantification were 0.20 μg/kg and 0.50 μg/kg, respectively. Average recoveries from spiked blank matrices at three levels (0.5, 2.5, and 5.0 μg/kg) ranged from 89.3% to 119.7%, with relative standard deviations (RSDs) between 0.8% and 10.2%. The proposed method is highly selective, exhibits minimal matrix interference, and provides reliable quantitative performance, making it suitable for the qualitative and quantitative analysis of diazepam residues in aquatic products. Full article

Background/Objectives: Phytochemicals from Chaenomeles japonica (CJ) (Thunb.) Lindl. ex Spach, a plant belonging to the Rosaceae family, are recognized for their potential to inhibit enzymes associated with diabetes, obesity, neurodegeneration, and inflammation. However, the influence of constituents from different plant parts on cytokine secretion has not yet been explored or comparatively analyzed. Methods: This study aimed to evaluate the anti-inflammatory potential of CJ by assessing its effects on chemokine and cytokine secretion, including interleukin (IL)-8, IL-1β, TNF-α, IL-6, and IL-10. Extracts from various plant parts (fruit, seed, flower, and leaf) were examined for their ability to modulate cytokine production in human neutrophils (PMNs). Among them, the aqueous fruit extract exhibited the strongest activity and was subsequently tested on peripheral blood mononuclear cells (PBMCs) and the human intestinal epithelial cell line Caco-2. The extract was also subjected to in vitro gastrointestinal digestion to assess the stability and bioactivity of its metabolites. The phytochemical composition of CJ preparations was characterized by ultra-high-performance liquid chromatography coupled with diode-array detection and tandem mass spectrometry (UHPLC-DAD-MS/MS). Results: The aqueous fruit extract significantly reduced the secretion of pro-inflammatory cytokines across all tested models. Fractions obtained after in vitro digestion also inhibited IL-8 release in Caco-2 cells. Conclusions: The most active fractions were rich in flavan-3-ols and proanthocyanidins. These findings indicate that CJ fruit possesses notable anti-cytokine properties and may serve as a promising natural source for developing functional food. Full article

Gastrodiae Rhizoma (GR) is known to have a medicinal and food-based homology. It is used to treat infantile convulsion, epilepsy, spasm, tetanus, and vertigo. In this study, an ultra-high performance liquid chromatography/tandem mass spectrometry (UHPLC-MS/MS) method was developed and validated to quantify fourteen components (p-hydroxybenzyl alcohol, gastrodin, parishin E, p-hydroxybenzoic acid, parishin C, parishin A, parishin B, nicotinamide, p-hydroxybenzaldehyde, adenosine, 3,4-dihydroxybenzaldehyde, syringaldehyde, dauricine, and nobiletin) of GR in rat plasma. Methanol precipitation was used to prepare the samples with astragalin, serving as the internal standard. In multiple reaction monitoring (MRM) mode, the fourteen components were separated by gradient elution on a Waters ACQUITY UPLC^® HSS T3 column. Under these conditions, all fourteen analytes’ calibration curves demonstrated strong linearity within wide concentration ranges (r > 0.9941). Accuracy for the intra-day and inter-day assessments ranged from −13.74% to 12.76%, and the precision for all analytes remained below 8.88%. The analytes’ extraction recoveries ranged from 66.78% to 114.2%, accompanied by matrix effects ranging from 63.65% to 117.61%. Under the evaluated conditions, stability tests confirmed that the compounds remained stable, with relative standard deviations below 13.83%. Consequently, the UHPLC-MS/MS method was effectively used to determine the pharmacokinetics of fourteen components in rat plasma after oral administration of GR extract. This study provides supportive data for rational application of GR. Full article

Background: To investigate the endogenous metabolites in Polygonatum odoratum (Mill.) Druce from different geographical origins within Guizhou Province, the metabolic profiles of samples from 12 regions were analyzed using ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). Methods: Multivariate statistical methods including principal component analysis (PCA), hierarchical clustering analysis (HCA), and Kyoto Encyclopedia of Genes and Genomes (KEGG) pathway enrichment analysis were employed to explore the influence of geographical origin on the metabolic composition of P. odoratum. Results: PCA revealed significant differences among samples from different regions which showed clear clustering patterns in our study, indicating that the growing environment considerably affects the metabolite profiles of P. odoratum. A total of 6055 potential metabolites were detected in both positive and negative ion modes. Significantly differential metabolites were then screened based on a fold change (FC) ≥ 2 or ≤0.5 and p < 0.05. Comparative analysis was conducted on representative samples from three clustered regions: As, ZYMT, and XY−1. The results indicated that alcohols, nucleotides and their derivatives were the major differential metabolites between AS and ZYMT, and alcohols were the key differential metabolites between AS and XY−1, while ketones and sphingolipids were the most significant differential metabolites between ZYMT and XY−1. KEGG enrichment analysis revealed that the pathways of nucleotide metabolism, amino acid biosynthesis, and aminoacyl-tRNA biosynthesis were notably disturbed, suggesting their crucial roles in the synthesis of differential metabolites in P. odoratum. Conclusions: These findings demonstrated the notable differences in the metabolite composition of P. odoratum from different regions of Guizhou province. Full article

Bovine adipose-derived neural crest stem cells (baNCSCs) are an ideal model for studying the mechanism of adipogenesis. Lipidomics provides a powerful technical means to comprehensively analyze the dynamic changes in lipid metabolism during cell differentiation. However, the lipidomic remodeling throughout the adipogenic differentiation of baNCSCs is still lacking in-depth research. This study used ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) to perform non-targeted lipidomic analysis on baNCSCs on day 0 (CON0) and day 9 (DIF9) of adipogenic induction and differentiation. Differential lipid metabolites were screened through multivariate statistical analysis and univariate analysis. A total of 1639 lipid molecules were identified. Compared with the CON0 group, 568 lipids were significantly altered in the DIF9 group, involving 6 major categories and 20 subclasses. The relative content and types of triacylglycerols (TAG) and diacylglycerols (DAG) increased significantly, becoming the most important markers of successful differentiation. Glycerophospholipids (GP) underwent complex remodeling, with subclasses such as phosphatidylethanolamine (PE), phosphatidylserine (PS), and cardiolipin (CL) significantly increased, indicating extensive restructuring of the cell and organelle membranes to adapt to lipid storage and energy metabolism. Sphingolipids (SP) such as ceramides (Cer) and sphingomyelins (SM) were generally downregulated. The content of acylcarnitines (ACar) and hydroxy fatty acids (FAHFA) increased, suggesting enhanced fatty acid β-oxidation and metabolic health. This study systematically reveals the comprehensive lipidome reprogramming during the adipogenic differentiation of baNCSCs, which involves not only the accumulation of storage lipids but also the precise coordination of membrane lipid remodeling, signaling lipid regulation, and metabolic adaptation. These findings provide a valuable lipidomic perspective for understanding the molecular mechanism of bovine adipogenesis. Full article