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Search Results (1,416)

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Keywords = high-performance liquid chromatography-tandem mass spectrometry

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31 pages, 2734 KB  
Article
Organ-Specific Phenolic Profiles, Antioxidant Capacity, and Enzyme-Inhibitory Activities of the Turkish Endemic Origanum bilgeri
by Zeyneb Karakus and Cengiz Sarikurkcu
Pharmaceuticals 2026, 19(9), 1429; https://doi.org/10.3390/ph19091429 - 10 Sep 2026
Abstract
Background/Objectives: Origanum bilgeri P.H. Davis is a Turkish endemic Lamiaceae species whose non-volatile phenolic composition and organ-specific bioactivities remain unexplored. This study investigated the phenolic composition of flower, leaf, stem, and root extracts and evaluated their antioxidant and enzyme-inhibitory activities. Methods: Ultrasound-assisted [...] Read more.
Background/Objectives: Origanum bilgeri P.H. Davis is a Turkish endemic Lamiaceae species whose non-volatile phenolic composition and organ-specific bioactivities remain unexplored. This study investigated the phenolic composition of flower, leaf, stem, and root extracts and evaluated their antioxidant and enzyme-inhibitory activities. Methods: Ultrasound-assisted ethanolic extracts of the four organs were characterized by liquid chromatography–tandem mass spectrometry (LC–MS/MS) targeting 28 phenolic compounds. Total phenolic and flavonoid contents, outcomes of six antioxidant assays, and inhibitory activities against acetylcholinesterase, butyrylcholinesterase, tyrosinase, α-amylase, and α-glucosidase were determined. Measurements were performed in triplicate as technical replicates, and organ-level differences were interpreted descriptively. The relative antioxidant capacity index (RACI) was calculated from the standardized outcomes of the six direct antioxidant assays, with total phenolic content (TPC) and total flavonoid content (TFC) excluded from the index. Pearson correlation analysis and principal component analysis (PCA) were used for exploratory evaluation of phytochemical and bioactivity patterns. Results: Twenty phenolic compounds were detected in at least one organ. Rosmarinic acid predominated in all organs and was most abundant in the leaf (3236 µg/g extract) and stem (3093 µg/g extract), whereas the root was markedly enriched in verbascoside (2775 µg/g extract) and chlorogenic acid (1461 µg/g extract) and exhibited the highest total phenolic content, reaching 160.87 mg gallic acid equivalents (GAE)/g extract. The assay-based RACI ranked the root highest (0.54), followed by the stem (0.02), leaf (−0.27), and flower (−0.30). The root also showed the strongest 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging activity (half-maximal inhibitory concentration, IC50 = 0.28 mg/mL) and cupric reducing antioxidant capacity (CUPRAC) (half-maximal effective concentration, EC50 = 0.22 mg/mL) among the investigated organ extracts. Under the present assay conditions, all organ extracts yielded lower α-glucosidase IC50 values (0.97–1.10 mg/mL) than acarbose (1.16 mg/mL). Exploratory Pearson correlation analysis indicated strong organ-level covariation among several antioxidant parameters, phenolic constituents, and α-glucosidase inhibitory activity. PCA based on the Pearson correlation matrix showed that principal components 1 and 2 (PC1 and PC2) accounted for 50.73% and 38.49% of the total variance, respectively (cumulative variance: 89.22%), providing an exploratory visualization of the multivariate organization of phytochemical and bioactivity variables. Conclusions: O. bilgeri exhibited distinct organ-specific phytochemical and bioactivity patterns under the conditions investigated. The root was particularly characterized by high verbascoside and chlorogenic acid contents, elevated total phenolic content, strong antioxidant performance across several assays, and α-glucosidase inhibitory activity. These findings support further investigation of O. bilgeri, particularly its root, using independent biological replicates and complementary phytochemical and biological approaches. Full article
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25 pages, 4547 KB  
Article
Physicochemical and Functional Comparison Between the Cetuximab Biosimilars Cetuxa® and Lupitux® and Cetuximab Originator Erbitux®
by Angela Capolupo, Fabio D’Amici, Luisa Buscajoni, Mattia Forchetta, Sofia Petrocchi, Erika Birolo, Daniela Bonetti, Lucia Colarusso, Simona Saporiti, Fabio Centola, Caterina Fusilli and Luigi Giunta
J. Pharm. BioTech Ind. 2026, 3(3), 21; https://doi.org/10.3390/jpbi3030021 - 10 Sep 2026
Abstract
ENZ-124, the first approved cetuximab biosimilar by Indian health authorities, was developed using the Chinese hamster ovary cell line, whereas the SP2/0 cell line was used for developing cetuximab originator (Erbitux®). Hence, this assessment aimed to evaluate the physiochemical, structural, and [...] Read more.
ENZ-124, the first approved cetuximab biosimilar by Indian health authorities, was developed using the Chinese hamster ovary cell line, whereas the SP2/0 cell line was used for developing cetuximab originator (Erbitux®). Hence, this assessment aimed to evaluate the physiochemical, structural, and biological characterization of four batches each of Cetuxa®, Lupitux® and cetuximab originator. Analytical methods like peptide mapping (liquid chromatography–tandem mass spectrometry [LC-MS/MS]), glycan mapping (liquid chromatography–fluorescence detection), isoform analysis (hydrophobic interaction chromatography [HIC]-high-performance liquid chromatography), charge variant analysis (capillary electrophoresis coupled with mass spectrometry), FcγRIIIa binding assays, cell-based antibody-dependent cell-mediated cytotoxicity (ADCC) measurement, and host cell protein analysis (LC-MS/MS) were utilized for analysis. Variations in physicochemical and biological attributes were observed between cetuximab originator and its biosimilars. HIC analysis revealed C-terminal heterogeneity and increased hydrophobicity in biosimilars, that with the different N-glycan profile affected charge distribution. Charge variant analysis indicated a more acidic profile for the biosimilars. The biosimilars showed higher oxidation levels and misincorporation. The biosimilars also showed an enhanced FcγRIIIa binding affinity and in vitro ADCC activation compared with cetuximab originator. The study outcomes highlight the ability to differentiate cetuximab originator from its biosimilars Cetuxa® and Lupitux® based on the observed physicochemical and biological differences. Full article
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17 pages, 1799 KB  
Article
Circulating Amino Acid Profiles in Adults with Abnormal Body Mass Index: Associations with Triglycerides, HDL Cholesterol, LDL Cholesterol, and Total Cholesterol in an Exploratory Cross-Sectional Metabolomic Pilot Study
by Marta Jaskulak, Iwona Rybakowska, Magdalena Gregorczyk, Klaudia Antoniak-Pietrynczak, Patrycja Jabłońska and Katarzyna Zorena
Biomolecules 2026, 16(9), 1305; https://doi.org/10.3390/biom16091305 - 9 Sep 2026
Abstract
Background/Objectives: Circulating amino acids are not only markers of nutritional status; in experimental and interventional models they have been linked to hepatic lipogenesis, lipoprotein assembly, mitochondrial fatty acid oxidation, and bile acid conjugation, which makes them plausible candidate correlates of obesity-related lipid dysregulation. [...] Read more.
Background/Objectives: Circulating amino acids are not only markers of nutritional status; in experimental and interventional models they have been linked to hepatic lipogenesis, lipoprotein assembly, mitochondrial fatty acid oxidation, and bile acid conjugation, which makes them plausible candidate correlates of obesity-related lipid dysregulation. Despite this, most metabolomic studies of excess adiposity have focused either on a single lipid parameter—typically triglycerides—or only on branched-chain amino acids (BCAAs). This pilot study was designed to generate hypotheses about these associations across the full standard lipid panel using a targeted 19-amino acid liquid chromatography–tandem mass spectrometry (LC-MS/MS) panel in adults spanning the body mass index (BMI) spectrum, with an analytical framework oriented around lipid phenotype variance rather than body weight classification. The design is cross-sectional and the analysis exploratory; no causal or predictive claim is made. Methods: Targeted LC-MS/MS quantification of 19 plasma amino acids was performed in 50 adults grouped as normal weight (n = 20; BMI 22 ± 1.5 kg/m2), overweight (n = 20; BMI 28 ± 1.5 kg/m2), or obese (n = 10; BMI 34 ± 2.0 kg/m2). The analytical framework included: (i) one-way analysis of variance (ANOVA) with Bonferroni correction; (ii) Pearson correlation analysis; (iii) principal component analysis (PCA) performed on the lipid profile itself with amino acid projection vectors; (iv) K-means clustering based on lipid phenotype (K = 3); (v) Ward-linkage hierarchical clustering of the amino acid–lipid correlation matrix; (vi) Random Forest permutation importance for all four lipid outcomes; and (vii) composite lipid risk indices including atherogenic index (TG/HDL-C) and non-HDL cholesterol. Results: A distinct amino acid correlation pattern was observed for each of the four lipid fractions. Triglycerides (TG) correlated most strongly with glutamic acid (r = 0.58) and inversely with glutamine (r = −0.58). High-density lipoprotein cholesterol (HDL-C) correlated most strongly with glutamic acid (r = −0.61) and serine (r = 0.49). The strongest correlates of low-density lipoprotein cholesterol (LDL-C) were phenylalanine (r = 0.56) and leucine (r = 0.56), and those of total cholesterol (TC) were leucine (r = 0.63) and, inversely, glycine (r = −0.54). The atherogenic index (TG/HDL-C) increased 2.9-fold from normal to obese and was most strongly correlated with glutamic acid, isoleucine, and glycine. In the multivariable models the amino acid panel accounted for a modest share of the variance in TG (adjusted R2 = 0.43; F(19,30) = 2.97, p = 0.004) and HDL-C (adjusted R2 = 0.35; F(19,30) = 2.40, p = 0.016). For LDL-C and TC the adjusted R2 values were close to zero (0.06 for both) and the overall models were not statistically significant (both p > 0.33); no interpretable amino acid signal was therefore present for these two fractions, and no predictors are reported for them. Lipid-based K-means clustering identified three lipid-phenotype clusters (Favorable, Intermediate, Adverse lipid profiles) with differences in amino acid z-scores. Conclusions: In this exploratory pilot cohort, lipid dysregulation in abnormal BMI was associated with two partially separable amino acid axes: a glutamic acid–glutamine axis (TG and partially HDL-C), and a glycine–serine putatively protective pattern opposing all atherogenic lipid parameters. These findings extend the established BCAA–insulin-resistance paradigm and suggest that targeted amino acid profiling—particularly for glutamic acid, leucine, glycine, and serine—may serve as a way of discovering candidate biomarkers for further study for dyslipidemia in individuals with abnormal BMI. Full article
(This article belongs to the Special Issue Advances in Metabolomics in Health and Disease)
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25 pages, 458 KB  
Article
Antioxidant Properties and Bioactive Compounds of Oregano, Sage, Basil, Rosemary, and Herbal Mixtures
by Julia Płatkiewicz, Joanna Wróbel, Magdalena Jeszka-Skowron, Robert Frankowski, Zuzanna Grześkowiak, Beata Czarczyńska-Goślińska, Anna Maria Jeszka and Agnieszka Zgoła-Grześkowiak
Antioxidants 2026, 15(9), 1113; https://doi.org/10.3390/antiox15091113 - 4 Sep 2026
Viewed by 280
Abstract
Herbs and spices are traditionally added to food in cuisines around the world. Antioxidant activity and content of bioactive compounds were compared in oregano, sage, basil, rosemary, and herbal mixtures. After optimization of ultrasound-assisted extraction of the ethanol–water extracts, the content of reducing [...] Read more.
Herbs and spices are traditionally added to food in cuisines around the world. Antioxidant activity and content of bioactive compounds were compared in oregano, sage, basil, rosemary, and herbal mixtures. After optimization of ultrasound-assisted extraction of the ethanol–water extracts, the content of reducing compounds of the herb extracts was tested using the Folin–Ciocalteu method, and antioxidant capacity was evaluated with ABTS (2,2’-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid)diammonium salt) and DPPH (2,2-diphenyl-1-picrylhydrazyl radical) assays. Oregano showed the highest antioxidant activity in all tests used (2.6 mg of gallic acid equivalent (GAE) per mL in the Folin–Ciocalteu test, 4.6 mg Trolox/mL in the ABTS assay, and 3.3 mg Trolox/mL in the DPPH assay) while rosemary had the lowest antioxidant activity (1.2 mg GAE/mL (Folin–Ciocalteu), 1.5 mg Trolox/mL (ABTS), and 1.3 mg Trolox/mL (DPPH)). Apart from antioxidant properties, the content of bioactive compounds was determined with the use of high-performance liquid chromatography–tandem mass spectrometry (LC-MS/MS). It was found that in all tested Lamiaceae herbs and the herbal mixes, rosmarinic acid widely predominates as a major non-volatile phenolic constituent, and its content varies from 1121 µg/g in rosemary to 10,255 µg/g in herbes de Provence. High concentrations were also observed for quinic acid in both oregano and rosemary. Interestingly, the concentrations of rosmarinic acid in the group of herbs studied are positively correlated with the results obtained in the Folin–Ciocalteu, ABTS, and DPPH tests (Spearman’s correlation coefficient 0.7030, 0.6657, and 0.7188, respectively), whereas no such correlation is observed for quinic acid. Overall, the findings indicate that these herbs share a common hydroxycinnamate-based phytochemical framework but display clear species-specific differences reflecting their intrinsic metabolism. Furthermore, the concentration of 3-caffeoylquinic acid in the Sicilian herbs (1021 µg/g) was approximately 10 times higher compared to the samples of Dalmatian herbs, herbes de Provence, and pure herbs, which demonstrates the unique chemical composition of that mixture, including the presence of dried tomatoes and tarragon, which were not included in other tested herbal mixtures. Full article
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25 pages, 12200 KB  
Article
Integrated Metabolomic and Transcriptomic Analysis Reveals Tissue-Specific Secondary Metabolic Differentiation and Indole Alkaloid Accumulation in Evodia rutaecarpa
by Weiwei Zhao, Jihua Guo, Taihang Wang, Li Zhou, Guoyi Zhang and Yuanjiang Xu
Biology 2026, 15(17), 1500; https://doi.org/10.3390/biology15171500 - 2 Sep 2026
Viewed by 268
Abstract
Evodia rutaecarpa is a valuable medicinal plant, yet its non-medicinal tissues remain largely underexplored. Here, we integrated ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)-based widely targeted metabolomics and RNA sequencing (RNA-seq) transcriptomics to systematically profile the metabolic and transcriptional landscapes of roots, stems, leaves, [...] Read more.
Evodia rutaecarpa is a valuable medicinal plant, yet its non-medicinal tissues remain largely underexplored. Here, we integrated ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)-based widely targeted metabolomics and RNA sequencing (RNA-seq) transcriptomics to systematically profile the metabolic and transcriptional landscapes of roots, stems, leaves, and flowers of Evodia rutaecarpa (Juss.) Benth. Our aim was to characterize tissue-specific metabolic differentiation and its underlying transcriptional regulatory mechanisms. Metabolomic analysis, employing principal component analysis (PCA) and orthogonal partial least squares-discriminant analysis (OPLS-DA) with robust model parameters (R2Y > 0.9, Q2 > 0.5), identified 3090 differential metabolite features (variable importance in projection, VIP > 1.0; p < 0.05) across the four tissues, which exhibited distinct tissue-specific clustering patterns. Integrated Kyoto Encyclopedia of Genes and Genomes (KEGG) enrichment analysis and weighted gene co-expression network analysis (WGCNA) revealed that roots specifically accumulated quinolone alkaloids and flavonoid glycosides, accompanied by the coordinated upregulation of genes involved in flavonoid and phenylpropanoid biosynthetic pathways. In contrast, stems, leaves, and flowers were enriched in indole alkaloids (evodiamine and rutaecarpine) and volatile oil precursors, with concurrent upregulation of genes involved in tryptophan metabolism and indole alkaloid biosynthesis (e.g., tryptophan decarboxylase, TDC; s N-methyltransferase, NMT). Notably, leaves and flowers displayed particularly high accumulation levels of these bioactive alkaloids, suggesting their potential as alternative sources for industrial and pharmaceutical applications. WGCNA further identified multiple transcription factors and structural gene modules tightly correlated with evodiamine accumulation, offering promising candidate regulators for future biosynthetic pathway engineering. Collectively, this multi-omics integration study systematically elucidates the tissue-partitioned secondary metabolism of Evodia rutaecarpa (Juss.) Benth. and provides a solid scientific foundation for full-plant resource utilization, targeted development of non-medicinal tissues, and future metabolic engineering of indole alkaloid production. Full article
(This article belongs to the Section Biochemistry and Molecular Biology)
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15 pages, 1706 KB  
Article
Residue Dissipation, Transformation Products, and Dietary Risk Assessment of Flonicamid in a Rice Paddy Ecosystem
by Yan Fu, Quansheng Wang, Liang Zhang and Yinliang Wu
Foods 2026, 15(17), 3104; https://doi.org/10.3390/foods15173104 - 1 Sep 2026
Viewed by 233
Abstract
Flonicamid is a systemic pyridinecarboxamide insecticide used to control sap-sucking pests in agricultural crops. An ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) method was developed for the simultaneous determination of flonicamid and its metabolites, N-(4-trifluoromethylnicotinoyl)glycine (TFNG), 4-(trifluoromethyl)nicotinamide (TFNA-AM), and 4-(trifluoromethyl)nicotinic acid (TFNA) in rice [...] Read more.
Flonicamid is a systemic pyridinecarboxamide insecticide used to control sap-sucking pests in agricultural crops. An ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) method was developed for the simultaneous determination of flonicamid and its metabolites, N-(4-trifluoromethylnicotinoyl)glycine (TFNG), 4-(trifluoromethyl)nicotinamide (TFNA-AM), and 4-(trifluoromethyl)nicotinic acid (TFNA) in rice plants, brown rice, rice husks, paddy soil, and paddy water. Method validation showed average recoveries of 73–115% with relative standard deviations of 1.1–9.9% across different matrices at three fortification levels. Field and laboratory experiments were conducted to characterize the dissipation, degradation, and transformation of flonicamid in the paddy ecosystem, and the dietary risk was assessed. Field dissipation followed first-order kinetics, with half-lives of 5.8, 2.9, and 7.1 days in rice plants, paddy soil, and paddy water, respectively. Under laboratory conditions, degradation proceeded markedly faster under aerobic than anaerobic conditions, with half-lives of 0.8–7.1 and 4.7–17.8 days in five typical Chinese soils, respectively. Six transformation products were identified by UHPLC–Q-TOF/MS coupled with UNIFI software (v1.9.4.0), including a novel product (M210) reported for the first time. At pre-harvest intervals of 7–21 days, terminal residues of flonicamid in brown rice were all below the Chinese maximum residue limit (MRL) of 0.1 mg/kg. Dietary risk assessment revealed that the acceptable daily intake percentages (%ADI) for 12 population subgroups ranged from 0.128% to 1.031% based on the parent compound, and from 0.404% to 3.808% under the EU residue definition. All values were far below 100%. These results indicate that flonicamid, when applied according to Good Agricultural Practice (GAP), poses a negligible dietary risk to consumers. Full article
(This article belongs to the Special Issue Assessment and Control of Food Safety Risks)
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17 pages, 2823 KB  
Article
Development of a Sensitive Analytical Method for the Determination of Sulforaphane in Vegetables by Automated Online In-Tube SPME/LC–MS/MS
by Keita Saito, Tomoaki Okamura and Hiroyuki Kataoka
Analytica 2026, 7(3), 61; https://doi.org/10.3390/analytica7030061 - 1 Sep 2026
Viewed by 272
Abstract
Sulforaphane (SFN), an isothiocyanate abundant in cruciferous vegetables, possesses well-documented anticancer, antioxidant, and anti-inflammatory properties, and has attracted interest as a dietary chemopreventive agent. However, sensitive and fully automated methods for its quantification in foods remain limited. In this study, we developed an [...] Read more.
Sulforaphane (SFN), an isothiocyanate abundant in cruciferous vegetables, possesses well-documented anticancer, antioxidant, and anti-inflammatory properties, and has attracted interest as a dietary chemopreventive agent. However, sensitive and fully automated methods for its quantification in foods remain limited. In this study, we developed an automated analytical system coupling in-tube solid-phase microextraction (IT-SPME) with high-performance liquid chromatography–tandem mass spectrometry (LC–MS/MS) to determine SFN in vegetable samples. Vegetable samples were autohydrolyzed in aqueous solution at 37 °C to generate SFN, which was then extracted with methanol by sonication. The extract was concentrated onto a Carboxen 1006 capillary column by IT-SPME, separated within 5 min on an Inertsil C8 column, and detected in positive electrospray ionization mode using multiple reaction monitoring. The detection limit was 5.6 pg/mL, with good linearity (R2 = 0.9995) over 0.1–100 ng/mL, intra- and inter-day precisions below 2.9% and 3.9%, respectively, and accuracy of 98–102%. SFN was detected at concentrations of 600 μg/g or higher in broccoli sprouts, florets, and stems, but was found at less than one-tenth of these levels in other vegetables tested. This method provides a simple, sensitive, and solvent-efficient tool for SFN quantification in vegetables, with potential application in food functionality assessment and chemopreventive research. Full article
(This article belongs to the Section Sample Pretreatment and Extraction)
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27 pages, 6593 KB  
Article
All-Trans Retinoic Acid and Curcumin Exhibit Hormesis or Synergistic Anticancer Effects in U87 Glioblastoma Cells: Defining the Proteome Accompanying Synergism
by Ceyda Sönmez, Meric A. Altinoz, Aleyna Baltacıoğlu, Büşra Ergün and Aysel Özpınar
Int. J. Mol. Sci. 2026, 27(17), 7795; https://doi.org/10.3390/ijms27177795 - 31 Aug 2026
Viewed by 229
Abstract
Persistently poor glioblastoma (GBM) survival necessitates better elucidation of tumor drug responses. After observing that low curcumin and all-trans retinoic acid (ATRA) doses stimulated cell proliferation and counteracted each other’s high-dose antiproliferative effects in U87 GBM cells, drug influences on cell growth, migration, [...] Read more.
Persistently poor glioblastoma (GBM) survival necessitates better elucidation of tumor drug responses. After observing that low curcumin and all-trans retinoic acid (ATRA) doses stimulated cell proliferation and counteracted each other’s high-dose antiproliferative effects in U87 GBM cells, drug influences on cell growth, migration, and death and the antiproliferative interaction proteome were further studied. Cell proliferation and migration were assessed by xCELLigence Real-Time Cell Analysis (RTCA). Cell death was defined using flow cytometry. Drug interactions were determined with CompuSyn software (version 1.0). Liquid Chromatography–Tandem Mass Spectrometry (LC-MS/MS), High-Performance Liquid Chromatography (HPLC), and SequestHT software (version 1.4) were utilized for peptide generation and identification. ATRA at high doses inhibited cell growth and migration more efficiently. Curcumin was more proliferative and antagonistic against anti-growth effects at low doses. Migration inhibition and apoptosis occurred synergistically at the highest drug doses. ATRA influenced the proteome more remarkably, reducing Transforming Growth Factor Beta Induced (TGFBI), Phosphoglycerate Dehydrogenase (PHGDH), tenascin, and Sequestosome 1 (SQSTM1). These effects were alleviated by curcumin, except for SQSTM1. Uveal Autoantigen With Coiled-Coil Domains And Ankyrin Repeats (UACA) and Sad1 And UNC84 Domain Containing 2 (SUN2) were increased by ATRA and curcumin, and to a lesser extent by the combination. Hexokinase 2 (HXK2) was increased by curcumin and the combination. Heme Oxygenase 1 (HMOX1) was depleted by the combination, but not by the single agents. SQSTM1 and HMOX1 reductions may mediate anticancer synergism, while the remaining changes may indicate ongoing hormetic pathways not reflected in cell counts. Full article
(This article belongs to the Special Issue Brain Cancers: Molecular Diagnostic and Therapeutic Approaches)
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14 pages, 2175 KB  
Article
Targeted Quantitative Metabolomics and Lipidomics Reveal Dysregulated Metabolic Networks and a Serum Candidate Biomarker for Atrial Fibrillation
by Yuqing Zhang, Yunpeng Xie, Xinyu Liu, Zhen Ning, Guowang Xu, Yunlong Xia and Xinjie Zhao
Metabolites 2026, 16(9), 630; https://doi.org/10.3390/metabo16090630 - 29 Aug 2026
Viewed by 242
Abstract
Background: Atrial fibrillation (AF) is the most prevalent clinical arrhythmia with severe cardiovascular complications, yet its metabolic molecular mechanisms remain poorly defined. Omics-based metabolic profiling provides a powerful strategy to systematically decode AF-associated metabolic disorders. Methods: In this work, high-coverage targeted liquid chromatography–tandem [...] Read more.
Background: Atrial fibrillation (AF) is the most prevalent clinical arrhythmia with severe cardiovascular complications, yet its metabolic molecular mechanisms remain poorly defined. Omics-based metabolic profiling provides a powerful strategy to systematically decode AF-associated metabolic disorders. Methods: In this work, high-coverage targeted liquid chromatography–tandem mass spectrometry (LC-MS/MS) metabolomics and lipidomics were applied to absolutely quantify 746 serum metabolites from AF patients and healthy controls. Results: We systematically characterized global metabolic perturbations in AF serum, including impaired fatty acid metabolism, suppressed mitochondrial β-oxidation, myocardial lipotoxic lipid accumulation, and systemic depletion of glycerophospholipids. Global multiscale embedded correlation network analysis (MECNA) further identified 11 AF-specific dysregulated metabolic modules and core hub metabolites driving metabolic remodeling. Leveraging binary logistic regression, we constructed and independently validated a two-molecule diagnostic biomarker panel to distinguish AF patients from healthy subjects. The combined biomarkers Phe-Trp and FA 22:5 achieved outstanding diagnostic performance, with area under the curve (AUC) values of 0.964 in the discovery cohort and 0.993 in the validation cohort. Conclusions: Collectively, this study adopts high-depth targeted quantitative omics to comprehensively map AF metabolic signatures, dissect disease-relevant metabolic networks, and establish a robust serum biomarker panel with great translational potential for non-invasive AF clinical diagnosis. Full article
(This article belongs to the Special Issue Analytical Techniques Applied in Metabolomics)
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22 pages, 10356 KB  
Article
γ-Valerolactone Reprograms Tomato Metabolism to Enhance Seedling Growth
by Xin Tao, Shangbo Yan, Ranran Chen, Fangfang Ren, Hongjie Yang, Wenheng Long and Nan Gao
Metabolites 2026, 16(9), 621; https://doi.org/10.3390/metabo16090621 - 27 Aug 2026
Viewed by 215
Abstract
Background: γ-Valerolactone (GVL), a green volatile platform compound derived from lignocellulosic biomass, has recently been identified as one volatile organic compound produced by the plant growth-promoting rhizobacterium Stutzerimonas stutzeri NRCB010. Although our previous transcriptomic and phenotypic studies have verified that exogenous GVL can [...] Read more.
Background: γ-Valerolactone (GVL), a green volatile platform compound derived from lignocellulosic biomass, has recently been identified as one volatile organic compound produced by the plant growth-promoting rhizobacterium Stutzerimonas stutzeri NRCB010. Although our previous transcriptomic and phenotypic studies have verified that exogenous GVL can promote the growth of tomato seedlings, the global metabolic reprogramming behind this promoting effect remains unclear. Methods: Tomato seedlings were subjected to exogenous GVL treatments at three concentrations (0, 0.25, 0.5 g/L) for 24 h and 48 h separately. Combined with physiological growth measurements, ultra-high-performance liquid chromatography–tandem mass spectrometry-based widely targeted metabolomics was applied to systematically characterize GVL-mediated metabolic reprogramming. Results: GVL remarkably improved seedling height, biomass and root development, with 0.25 g/L GVL showing the strongest promoting effect. A total of 703 metabolites including lipids, flavonoids and alkaloids were identified. Principal component analysis and orthogonal partial least squares discriminant analysis revealed distinct metabolic separation between control and treated groups, verifying time and concentration dependent metabolic shifts. After 24 h, GVL activated primary pathways (the tricarboxylic acid cycle, amino acid and purine metabolism) to supply growth energy; after 48 h, central carbon and secondary biosynthetic pathways were enriched, and 0.5 g/L GVL specifically triggered defensive isoquinoline and indole alkaloid biosynthesis. Conclusions: GVL coordinately remodels primary and secondary metabolic networks to accelerate tomato seedling growth, which provides sufficient metabolomic evidence for developing GVL as a novel bio-based plant biostimulant. Full article
(This article belongs to the Special Issue Metabolites and Plant Stress Resistance)
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19 pages, 4156 KB  
Article
Determination of 25 Organophosphate Ester Flame Retardants in Soils by Accelerated Solvent Extraction–Ultra-High Performance Liquid Chromatography
by Ban Cao, Yinjun Shi, Zuguo Hu and Mingli Ye
Toxics 2026, 14(9), 763; https://doi.org/10.3390/toxics14090763 - 26 Aug 2026
Viewed by 525
Abstract
Organophosphate esters (OPEs) are commonly used flame retardants and plasticizers, which can easily be released into the soil environment and have potential hazards such as neurotoxicity and developmental toxicity. Establishing an efficient and sensitive detection method plays a crucial role in soil pollution [...] Read more.
Organophosphate esters (OPEs) are commonly used flame retardants and plasticizers, which can easily be released into the soil environment and have potential hazards such as neurotoxicity and developmental toxicity. Establishing an efficient and sensitive detection method plays a crucial role in soil pollution assessment. Currently, there have been numerous studies on the detection of OPEs in soil using ultrasonic extraction and solid-phase extraction, while relatively few studies have focused on the analysis of multiple OPEs in soil by accelerated solvent extraction combined with d-SPE clean-up and ultra-high performance liquid chromatography–tandem mass spectrometry. The d-SPE purification method eliminates the need for column passage, shortens sample preparation time, and avoids the risk of background contamination from OPEs that may be introduced by SPE. This study developed a liquid chromatography–tandem quadrupole mass spectrometry (LC-MS/MS) method for the determination of 25 OPEs in soil, and systematically optimized the pretreatment and instrumental analysis conditions. Accelerated solvent extraction was used for pretreatment, and dichloromethane–methanol (1:1, V/V) was determined as the optimal extraction solvent. A mixed adsorbent of N-propyl ethylenediamine (PSA) and C18 was selected for dispersive purification, effectively removing matrix interference and improving recovery rates. The mass spectrometry parameters such as collision energy and declustering voltage were optimized, significantly enhancing ion response intensity and detection sensitivity. The method showed good linearity within the concentration range of 1–100 ng/mL, with correlation coefficients all greater than 0.994. The spiked recovery rates ranged from 70.6% to 111% with a relative standard deviation (RSD) of 1.2–11.8%. The precision and accuracy met the requirements for environmental sample analysis. The method was applied to the detection of actual soil samples, and the results were stable and reliable. This method is simple to operate, highly sensitive, and widely applicable, providing reliable technical support for the pollution monitoring, source tracing, and ecological risk assessment of OPEs in soil. Full article
(This article belongs to the Section Toxicity Reduction and Environmental Remediation)
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21 pages, 11810 KB  
Article
Per- and Polyfluoroalkyl Substances (PFAS) in Michigan: A Novel High-Throughput Method with Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS) Analysis of 39 PFAS Compounds in Human and Bovine Dried Blood Spots (DBS)
by Jessica M. Morrison, Sarah Y. Lockwood-O’Brien, Chelsea A. Bielicki, Douglas J. Carmack, Julia R. Feeley, Timothy A. Karrer and Matthew J. Geiger
Toxics 2026, 14(9), 753; https://doi.org/10.3390/toxics14090753 - 26 Aug 2026
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Abstract
This study presents a novel method for analyzing per- and polyfluoroalkyl substances (PFAS) in dried blood spots (DBS), employing a hybrid solvent-based and matrix-matched calibration curve, minimal sample volume, and high-throughput preparation. This process produces a concentrated, purified sample, which is analyzed using [...] Read more.
This study presents a novel method for analyzing per- and polyfluoroalkyl substances (PFAS) in dried blood spots (DBS), employing a hybrid solvent-based and matrix-matched calibration curve, minimal sample volume, and high-throughput preparation. This process produces a concentrated, purified sample, which is analyzed using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). As part of method validation, key performance metrics such as accuracy, precision, sensitivity, carryover, specificity, interferences, and maximum dilution capability were assessed. The method quantifies 39 PFAS compounds across various classes, achieving limits of detection in the low ng L−1 range, with most analytes having a limit of quantitation below the first calibrator (50 ng L−1). The total method accuracy exceeded 81%, surpassing the performance goal of ≥70%, while method imprecision was below 28%, outperforming the goal of ≤30%. Specificity, as measured by a normalized percent matrix bias, was below 11%, with limited and minimal matrix effects observed. Interference from bile acids was determined to be insignificant at biologically relevant concentrations. Over the past three years, this method has been successfully utilized in biomonitoring studies of Michigan residents, demonstrating its robustness and efficiency. Full article
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14 pages, 1383 KB  
Article
Acidified Acetonitrile Extraction and Ultra-High Performance Liquid Chromatography–Tandem Mass Spectrometry for Multiresidue Determination of 136 Pesticides in Tahiti Lime (Citrus latifolia)
by Karolaine da Silva Albarnaz, Juliana Diniz de Barros Kuntz, Luana Floriano, Franciele Fátima Machado, Martha Bohrer Adaime, Renato Zanella and Osmar Damian Prestes
Foods 2026, 15(17), 2967; https://doi.org/10.3390/foods15172967 - 24 Aug 2026
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Abstract
The determination of pesticide residues in citrus fruits remains analytically challenging due to their high acidity and complex chemical compositions, which can compromise extraction efficiency and promote significant matrix effects, particularly for acidic compounds. In this study, an acidified acetonitrile-based QuEChERS method was [...] Read more.
The determination of pesticide residues in citrus fruits remains analytically challenging due to their high acidity and complex chemical compositions, which can compromise extraction efficiency and promote significant matrix effects, particularly for acidic compounds. In this study, an acidified acetonitrile-based QuEChERS method was developed and validated for the multiresidue determination of 136 pesticides in Tahiti lime (Citrus latifolia) using ultra-high-performance liquid chromatography coupled with tandem mass spectrometry (UHPLC–MS/MS). The proposed approach employs 1% formic acid in acetonitrile and omits the conventional clean-up step, aiming to improve analyte recovery and analytical throughput. Method validation was performed according to SANTE guidelines, demonstrating satisfactory linearity (R2 ≥ 0.99 for all analytes), limits of quantification of 0.01 mg kg−1, and recoveries within 70–120%, with relative standard deviations ≤ 20% for the vast majority of compounds. Notably, the method achieved consistent and reliable performance for 12 acidic pesticides, which are typically problematic in conventional QuEChERS approaches. Application to 22 real samples revealed the presence of 14 pesticide residues, with some compounds exceeding European Union (EU) maximum residue limits. The proposed method provides a simple, efficient, and robust alternative for comprehensive pesticide monitoring in citrus fruits, with particular advantages for the determination of acidic compounds in highly complex matrices. Full article
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20 pages, 3384 KB  
Article
Extracellular Yellow Pigments Produced by Chaetomium globosum H-1 Isolated from Spalted Wood: Fermentation Regulation, Multidimensional Characterization, and Sustainable Wool Dyeing
by Boxi Chen, Mengqi Wu and Jianping Sun
Microorganisms 2026, 14(8), 1818; https://doi.org/10.3390/microorganisms14081818 - 18 Aug 2026
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Abstract
Microbial extracellular pigments are renewable colorants for sustainable textile dyeing. A yellow-pigment-producing fungal strain, H-1, isolated from spalted wood, was identified as Chaetomium globosum and evaluated for pigment production, characterization, stability, bioactivity, and wool dyeing. Stepwise single-factor screening indicated suitable culture conditions of [...] Read more.
Microbial extracellular pigments are renewable colorants for sustainable textile dyeing. A yellow-pigment-producing fungal strain, H-1, isolated from spalted wood, was identified as Chaetomium globosum and evaluated for pigment production, characterization, stability, bioactivity, and wool dyeing. Stepwise single-factor screening indicated suitable culture conditions of initial pH 7, 25 °C, 10 d, 25 g/L glucose, 7 g/L fish peptone, and 0.25 g/L K2HPO4. Fourier-transform infrared spectroscopy (FTIR) revealed hydroxyl, aromatic, and C-O-C groups, and ultra-high-performance liquid chromatography-high-resolution tandem mass spectrometry (UHPLC-HRMS/MS) putatively annotated representative components including Chaetomugilin D and Armochaetoglobin G. The crude pigment produced preliminary inhibition zones of 14.30 ± 0.04 and 10.01 ± 0.17 mm against Staphylococcus aureus and Escherichia coli, respectively, while crude fermentation filtrates showed measurable hydroxyl and 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical-scavenging capacities under fixed assay conditions. The pigment was more stable under neutral to alkaline pH and short-term heating at 40–100 °C. Wool showed higher dye affinity than cotton, linen, and silk. Response surface methodology (RSM) optimized wool dyeing at pH 2.35, 91 °C, 80 min, and 2.04 g/L potassium aluminum sulfate, yielding a color strength (K/S) value of 11.65. After three dye-bath reuse cycles, K/S decreased by 16.28%, and washing/rubbing fastness remained above grade 3 under GB/T tests. These results support further development of Chaetomium globosum H-1 extracellular pigments for natural wool coloration and dye-bath reuse. Full article
(This article belongs to the Section Microbial Biotechnology)
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14 pages, 11202 KB  
Article
Metabolomics Analysis of Different Varieties of Pouteria caimito Fruit Based on UHPLC-MS/MS
by Haijie Huang, Li Zhao, Zhikai Wang, Yang Qiao, Huidong Deng, Yingjun Ye, Kaili Ding, Xuejie Feng and Yijun Liu
Foods 2026, 15(16), 2855; https://doi.org/10.3390/foods15162855 - 15 Aug 2026
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Abstract
To investigate the differences in pulp metabolites among four varieties of Pouteria caimito fruit (JZL1, JZL3, JZL5, and JZL6), ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was employed for the separation and identification of metabolites. A total of 1285 metabolites were identified, including [...] Read more.
To investigate the differences in pulp metabolites among four varieties of Pouteria caimito fruit (JZL1, JZL3, JZL5, and JZL6), ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was employed for the separation and identification of metabolites. A total of 1285 metabolites were identified, including 648 in positive ion mode and 637 in negative ion mode. At the class level, carboxylic acids and derivatives (14.32%) and organooxygen compounds (11.83%) accounted for the highest proportions; at the subclass level, amino acids, peptides, and analogues (12.53%) as well as carbohydrates and carbohydrate conjugates (9.49%) were the main categories. PLS-DA analysis revealed significant differences in metabolite profiles among the four varieties, with numerous up-regulated and down-regulated metabolites in each comparison group, and some metabolites showed fold changes > 10 or <0.1. KEGG pathway enrichment analysis further indicated that differential metabolites were primarily enriched in pathways such as ABC transporters, citrate cycle (TCA cycle), starch and sucrose metabolism, and linoleic acid metabolism. This study provides an important metabolomic basis for variety identification, nutritional quality evaluation, and functional component development of Pouteria caimito fruit. Full article
(This article belongs to the Section Plant Foods)
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