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Search Results (4,082)

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Keywords = HPLC–MS/MS

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24 pages, 13107 KB  
Article
Assessing the Insecticidal Performance of Commiphora myrrha Essential Oil Against Prostephanus truncatus and Sitophilus zeamais Using a Metabolomic Approach
by Nickolas G. Kavallieratos, Maria C. Boukouvala, Constantin S. Filintas, Demeter Lorentha S. Gidari, Anna Skourti, Vasiliki Panagiota C. Kyrpislidi, Filippo Maggi, Riccardo Petrelli, Eleonora Spinozzi, Marta Ferrati, Cristina Teruzzi and Fabrizio Araniti
Plants 2025, 14(19), 3031; https://doi.org/10.3390/plants14193031 - 30 Sep 2025
Abstract
Botanical insecticides have gained interest due to a rising demand for environmentally friendly pest control methods for stored-product protection. The insecticidal effectiveness of the essential oil (EO) obtained from the oleo-gum-resin of myrrh (Commiphora myrrha (Nees) Engl.), against Prostephanus truncatus (Horn) and [...] Read more.
Botanical insecticides have gained interest due to a rising demand for environmentally friendly pest control methods for stored-product protection. The insecticidal effectiveness of the essential oil (EO) obtained from the oleo-gum-resin of myrrh (Commiphora myrrha (Nees) Engl.), against Prostephanus truncatus (Horn) and Sitophilus zeamais Motschulsky, and the metabolic shifts of the two species, were investigated in this work. A thorough gas chromatography-mass spectrometry (GC-MS) investigation showed that the composition of this EO was dominated by furanosesquiterpenes, specifically, furanoeudesma-1,3-diene and curzerene. Commiphora myrrha EO treatments, especially at 1000 ppm, resulted in high adult mortality for P. truncatus (up to 85.6%), while S. zeamais showed only moderate mortality (up to 25.6%). To investigate the different species-specific effectiveness of the EO, untargeted GC-MS metabolomic profiling was conducted to elucidate the impact of the EO on the metabolism of the insects, with subsequent data analysis employing multivariate, univariate, and network methods. Each species reacts differently to the treatments (myrrh EO versus the synthetic insecticide pirimiphos-methyl (PM)), according to the analysis results. In particular, myrrh EO caused distinct shifts in metabolic pathways that varied between P. truncatus and S. zeamais. Overall, C. myrrha EO exhibits potential as a botanical insecticide, especially against P. truncatus, and it causes metabolic disturbances specific to the species. The results demonstrate the significance of metabolomic technologies in assessing bioinsecticide mechanisms and lend credence to their possible incorporation in integrated pest management methodologies or their contribution to the creation of diagnostic indicators of insecticidal exposure. Full article
(This article belongs to the Special Issue Green Insect Control: The Potential Impact of Plant Essential Oils)
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23 pages, 1644 KB  
Article
Characteristics of Novel Fermented Cloudy Fruit Juices Produced Using Lactiplantibacillus plantarum and Lactic Acid-Producing Lachancea spp. Yeasts
by Paweł Satora, Magdalena Skotniczny and Martyna Maziarek
Molecules 2025, 30(19), 3928; https://doi.org/10.3390/molecules30193928 - 30 Sep 2025
Abstract
Fermented fruit juices are considered functional beverages because they contain bioactive compounds derived from plant materials and produced by the microorganisms involved in fermentation. The composition of these beverages can vary depending on the strain used. This study aimed to determine the effect [...] Read more.
Fermented fruit juices are considered functional beverages because they contain bioactive compounds derived from plant materials and produced by the microorganisms involved in fermentation. The composition of these beverages can vary depending on the strain used. This study aimed to determine the effect of different microorganisms conducting lactic acid fermentation on the chemical composition and bioactive component content of naturally cloudy fermented pear and plum juices. The process used Lactiplantibacillus plantarum K7 bacteria, which were isolated during sauerkraut fermentation, as well as Lachancea thermotolerans PYCC6375 and Lachancea fermentati PYCC5883 yeast cultures, which have poor ethanol fermentation capabilities. The pH, acidity, sugars (HPLC), free amino nitrogen, selected organic acids (HPLC), color (CIELAB), polyphenols (HPLC), volatiles (GC-MS), aroma-active volatiles (GC-MS-O), and sensory characteristics were analyzed. The fermented juices obtained were rich in organic acids (of plant and microbial origin), polyphenols, and had a reduced sugar content (with polyols replacing glucose and fructose), as well as a low alcohol content (<0.2%). At the same time, all three microorganisms significantly enhanced the fruity aroma of the juices. Lachancea yeasts proved to be a viable alternative to lactic acid bacteria for producing fermented juices and were significantly better suited to fermenting plum juices. The highest polyphenol content and highest consumer preference rating were obtained with plum juices fermented with L. fermentati yeast. Full article
(This article belongs to the Special Issue Bioactive Compounds in Foods and Their By-Products)
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13 pages, 1595 KB  
Article
Differential Plasma Carotenoid Profiles in Hypertensive Disorders of Pregnancy
by Colman I. Freel, Jonah Scheffler, Rebecca A. Drakowski, Elizabeth Lyden, Matthew VanOrmer, Melissa K. Thoene, Paras Kumar Mishra, Corrine K. Hanson and Ann L. Anderson-Berry
Nutrients 2025, 17(19), 3104; https://doi.org/10.3390/nu17193104 - 29 Sep 2025
Abstract
Background: Hypertensive disorders of pregnancy (HDP) affect one in six pregnancies globally. The etiology of HDP remains unclear but is known to involve oxidative stress. While the body produces endogenous antioxidants, antioxidative nutrients, like carotenoids, remain critical in modulating oxidative stress. The [...] Read more.
Background: Hypertensive disorders of pregnancy (HDP) affect one in six pregnancies globally. The etiology of HDP remains unclear but is known to involve oxidative stress. While the body produces endogenous antioxidants, antioxidative nutrients, like carotenoids, remain critical in modulating oxidative stress. The statuses of several carotenoids have been linked to hypertension in both pregnant and non-pregnant populations. However, their associations with the spectrum of HDP, including gestational hypertension (GH), chronic hypertension (CH), and preeclampsia (PE), remains unclear. Our objective was to quantify and compare carotenoid intake and plasma levels among HDP. Methods: We conducted a prospective cohort study of patients presenting for delivery at a Midwestern academic medical center between 2015 and 2023. Women ≥ 19 years old delivering at least one infant were eligible for inclusion. Mothers with diseases affecting nutrient metabolism or birthing newborn wards of the state were excluded. Subjects were recruited at delivery for Harvard Food Frequency Questionnaire and plasma sample collection. Plasma carotenoids were analyzed by HPLC-MS. Results: A total of 488 patients, including 270 normotensive (NT), 61 CH, 102 GH, and 55 PE, were recruited. Plasma carotenoid analyses were available for 225 subjects. Plasma total, cis-, and trans-β-carotene were significantly lower in PE (73 mcg/L) compared to NT (170 mcg/L), CH (194 mcg/L), and GH (190 mcg/L) groups. Lutein + zeaxanthin and β-cryptoxanthin were also reduced in PE (142 mcg/L and 81 mcg/L) compared to NT (209 mcg/L and 123 mcg/L) but only β-cryptoxanthin was lower in PE compared to GH (126 mcg/L). Levels of α-carotene were lower in PE (18 mcg/L) compared to both CH (43 mcg/L) and GH (48 mcg/L). Conclusions: These results demonstrate that plasma carotenoid levels differ among HDP and may suggest that oxidative stress in PE depletes circulating carotenoids, differentiating it from other HDP. Full article
(This article belongs to the Section Nutrition in Women)
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27 pages, 3871 KB  
Article
A Cascade Approach to Valorizing Camellia oleifera Abel Shell: Ultrasound-Assisted Extraction Coupled with Resin Purification for High-Efficiency Production of Multifunctional Polyphenols
by Jingyi Chen, Wei Li, Tao Liang, Yuting Yang, Rui Zhou, Rui Li, Daiyu Xie, Dayan Xiang, Shiling Feng, Tao Chen, Lijun Zhou and Chunbang Ding
Antioxidants 2025, 14(10), 1192; https://doi.org/10.3390/antiox14101192 - 29 Sep 2025
Abstract
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 [...] Read more.
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
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16 pages, 520 KB  
Article
Co-Occurrence of Major Mycotoxins and Emerging Alternaria Toxins in Couscous Marketed in Algeria
by Sarah Mohammedi-Ameur, Terenzio Bertuzzi, Roberta Battaglia, Federico Siboni, Paola Giorni and Dahmane Mohammedi
Toxins 2025, 17(10), 483; https://doi.org/10.3390/toxins17100483 - 26 Sep 2025
Abstract
Cereal contamination by mycotoxins represents a major food safety concern. This study aimed to assess the co-occurrence of 15 mycotoxins in 50 couscous samples marketed in Algeria using HPLC/FLD and LC-MS/MS techniques. The samples included various couscous types, differing in ingredients, production method [...] Read more.
Cereal contamination by mycotoxins represents a major food safety concern. This study aimed to assess the co-occurrence of 15 mycotoxins in 50 couscous samples marketed in Algeria using HPLC/FLD and LC-MS/MS techniques. The samples included various couscous types, differing in ingredients, production method (organic or conventional), processing operations, and granularity. The most frequently detected mycotoxins were tentoxin (76%), deoxynivalenol (74%), tenuazonic acid (72%), and ochratoxin A (54%). For the regulated mycotoxins, none of the concentrations exceeded the maximum levels set by the European Union. In contrast, tenuazonic acid and tentoxin, which are not yet regulated, were the most common compounds detected. Contamination with multiple mycotoxins was commonly observed: 90% of the samples contained at least two mycotoxins, with some containing up to seven. The most frequent combination involved tenuazonic acid-tentoxin-ochratoxin A. These findings highlight the need for frequent and systematic monitoring of couscous and other processed cereal-based products. Full article
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21 pages, 3713 KB  
Article
Unraveling the Chemical Composition and Biological Activity of Geum aleppicum Jacq.: Insights from Plants Collected in Kazakhstan
by Gulnur N. Kuntubek, Martyna Kasela, Kaldanay K. Kozhanova, Wirginia Kukula-Koch, Łukasz Świątek, Kinga Salwa, Piotr Okińczyc, Aleksandra Józefczyk, Jarosław Widelski, Gulnara M. Kadyrbayeva, Aigerim Z. Mukhamedsadykova, Zuriyadda B. Sakipova and Anna Malm
Molecules 2025, 30(19), 3888; https://doi.org/10.3390/molecules30193888 - 26 Sep 2025
Abstract
Geum aleppicum Jacq. (yellow avens), a species traditionally used in folk medicine, remains understudied in the ethnopharmacological aspects. In this study, we comprehensively evaluated the phytochemical composition and biological activity of a hydroethanolic (50:50, v/v) extract from the aerial parts [...] Read more.
Geum aleppicum Jacq. (yellow avens), a species traditionally used in folk medicine, remains understudied in the ethnopharmacological aspects. In this study, we comprehensively evaluated the phytochemical composition and biological activity of a hydroethanolic (50:50, v/v) extract from the aerial parts of G. aleppicum collected in Kazakhstan. Using the high-performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry (HPLC-ESI-QTOF-MS/MS), we identified 24 compounds, predominantly phenolic acids, flavonoids, tannins, and triterpenoids. The major compound was ellagic acid (2.28 mg/g dry extract) as revealed by the reverse phase high-performance liquid chromatography–diode array detector (RP-HPLC-DAD). The extract exhibited a high polyphenol content (131.45 mg GAE/g) and strong antioxidant activity in Ferric Reducing Antioxidant Power (FRAP) assay and 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging assay (3.82 ± 0.07 mmol Fe2+/g and 106.61 ± 0.89 mg GAE/g, respectively). Antimicrobial assay of the extract revealed notable antifungal activity against Candida spp., especially against C. glabrata and C. tropicalis with minimum inhibitory concentration (MIC) of as low as 0.125 mg/mL, showing fungistatic effect. Although the extract inhibited the cytopathic effect induced by Human Herpesvirus 1 (HHV-1) in VERO cells, it did not significantly reduce viral replication. Moreover, among human cancer cell lines studied, the extract exerted moderate and selective cytotoxicity against A549 lung cancer cells (CC50 = 75.51 µg/mL, SI = 9). These findings highlight G. aleppicum as a rich source of bioactive compounds, especially phenolics, supporting its potential for development of pharmaceutical and cosmetic applications. Full article
(This article belongs to the Special Issue Biological Evaluation of Plant Extracts)
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17 pages, 5455 KB  
Article
Untargeted Metabolomics Reveals the Effect of Carbon Dots on Improving the Shelf Life of Postharvest Goji Berries (Lycium barbarum L.)
by Yuan-Zhe Wang, Juan Du, Wen-Ping Ma, Run-Hui Ma, Kiran Thakur, Zhi-Jing Ni, Wei Wang and Zhao-Jun Wei
Foods 2025, 14(19), 3336; https://doi.org/10.3390/foods14193336 - 26 Sep 2025
Abstract
Lycium barbarum L. (goji berry) undergoes rapid quality deterioration after harvest owing to its high water activity and abundant reactive oxygen species (ROS). Carbon-dot-mediated photodynamic treatment (CD-PDT) has recently been shown to extend shelf life by modulating ROS-scavenging and defense enzymes, yet the [...] Read more.
Lycium barbarum L. (goji berry) undergoes rapid quality deterioration after harvest owing to its high water activity and abundant reactive oxygen species (ROS). Carbon-dot-mediated photodynamic treatment (CD-PDT) has recently been shown to extend shelf life by modulating ROS-scavenging and defense enzymes, yet the global metabolic reprogramming that supports this protection remains unresolved. Here, we applied ultra-high-performance liquid chromatography–tandem mass spectrometry (HPLC-MS/MS)-based untargeted metabolomics to decode the metabolic footprint of CD-PDT in freshly harvested goji berries. Our results revealed a total of 17,603 differentially expressed metabolites between the treatment and control groups under both positive- and negative-ion modes. Principal component analysis indicated that CD-mediated PDT significantly altered the metabolic profile of fresh goji berries. The treatment activated the phenylpropanoid biosynthesis pathway, promoting the accumulation of compounds such as kaempferol-3-sophoroside, kaempferol-3-O-β-D-glucoside, and galactoside, thereby enhancing the antioxidant capacity of the fruit. Furthermore, CD-mediated PDT induced the tricarboxylic acid cycle, providing sufficient energy to support the phenylpropanoid biosynthesis pathway. In conclusion, these findings provide the systems-level evidence that CD-PDT orchestrates a coordinated activation of primary and secondary metabolism in postharvest goji berries, establishing a mechanistic framework for preservation of horticultural products. Full article
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24 pages, 2415 KB  
Article
Antibacterial, Antifungal, and Wound-Healing Activities and Chemical Characterization of Propolis from Apis mellifera in Michoacan, Mexico
by Ana Bertha Hernandez-Hernandez, Mario Rodriguez-Canales, Pilar Dominguez-Verano, Uriel Nava-Solis, Marco Aurelio Rodriguez-Monroy and María Margarita Canales-Martinez
Molecules 2025, 30(19), 3880; https://doi.org/10.3390/molecules30193880 - 25 Sep 2025
Abstract
The aim of this study was to evaluate the antibacterial and antifungal activities, wound-healing efficacy, and chemical characteristics of hexanic, chloroformic, and methanolic extracts of propolis from Michoacan, Mexico. Antibacterial activity was determined using Gram-positive and Gram-negative bacteria, antifungal activity was determined using [...] Read more.
The aim of this study was to evaluate the antibacterial and antifungal activities, wound-healing efficacy, and chemical characteristics of hexanic, chloroformic, and methanolic extracts of propolis from Michoacan, Mexico. Antibacterial activity was determined using Gram-positive and Gram-negative bacteria, antifungal activity was determined using yeast and filamentous fungi and wound-healing efficacy was determined using the tensiometric and histological methods in mouse skin. Antioxidant capacity, phenols, and total flavonoids were quantified. Propolis was subjected to high-performance liquid chromatography (HPLC-DAD), high-performance liquid chromatography–mass spectrometry (HPLC-TOF-MS), and gas chromatography–mass spectrometry (GC-MS). The methanolic extract showed the best antibacterial activity, and the most sensitive bacteria was Staphylococcus aureus. For antifungal activity, yeasts and filamentous fungi showed sensitivity to the methanolic extract, with Candida albicans and Trichophyton mentagrophytes being the strains with the highest sensitivity to the extract. Regarding wound-healing efficacy, when using the tensiometric method, the methanolic extract presented the highest efficacy, surpassing the positive control (Recoveron). In the histological evaluation, the methanolic extract provided more resistance to the wound and demonstrated an antioxidant capacity of 12.23 µg/mL, a total phenolic content of 580 mg GAE/g, and a total flavonoid content of 12.35 mg QE/g. In the chemical analysis, flavanols, flavones, and flavanones were identified. Full article
(This article belongs to the Special Issue Bee Products: Recent Progress in Health Benefits Studies, 2nd Edition)
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32 pages, 5159 KB  
Article
Phytochemical Analysis and Phytometabolomic Profiling of Ficus lindsayana Leaf Extract with Evaluation of Antioxidant, Anti-Inflammatory, Cyto- and Genotoxic Activities
by Arisa Imsumran, Woorawee Inthachat, Piya Temviriyanukul, Jirarat Karinchai, Tanongsak Laowanitwattana, Pensiri Buacheen, Ararat Jaiaree, Uthaiwan Suttisansanee, Ariyaphong Wongnoppavich and Pornsiri Pitchakarn
Int. J. Mol. Sci. 2025, 26(19), 9374; https://doi.org/10.3390/ijms26199374 - 25 Sep 2025
Abstract
Ficus lindsayana is recognized for its medicinal properties, with previous studies highlighting the antioxidant and anti-inflammatory effects of its latex (FLtA) and root (FRE) extracts. Harvesting these plant parts, however, raises ecological concerns. This study evaluates the phytochemical profiles, safety, and biological activities [...] Read more.
Ficus lindsayana is recognized for its medicinal properties, with previous studies highlighting the antioxidant and anti-inflammatory effects of its latex (FLtA) and root (FRE) extracts. Harvesting these plant parts, however, raises ecological concerns. This study evaluates the phytochemical profiles, safety, and biological activities of F. lindsayana leaf (FL) extracts as more sustainable alternatives. Leaves were extracted using hot water (FLA) and 80% ethanol (FLE), yielding 32.9% and 11.4%, respectively. Metabolomic and targeted HPLC-MS/MS analyses revealed distinct phytochemical compositions. FLE was enriched in flavonoid aglycones and lipophilic compounds, while FLA contained higher levels of polar phenolics. FLA showed greater total phenolic and flavonoid contents and stronger antioxidant activity, with an SC50 of 159 μg/mL for the DPPH assay. In contrast, FLE demonstrated more pronounced anti-inflammatory activity. In LPS-stimulated RAW 264.7 macrophages, FLE significantly reduced nitric oxide production and iNOS expression at both the protein and mRNA levels. FLE also reduced IL-6 secretion in a dose-dependent manner without affecting TNF-α, suggesting selective cytokine modulation. Both extracts exhibited low cytotoxicity (IC20 > 800 µg/mL in most cell types), non-hemolytic properties, and no mutagenic activity in the Drosophila wing spot assay. Compared to root and latex extracts, FLE ranked second in anti-inflammatory potency (FRE > FLE > FLA = FLtA). FLE, therefore represents a promising candidate, combining potent bioactivity with environmental responsibility and supporting the further development of F. lindsayana leaf-derived products for use in functional foods or botanical therapeutics. Full article
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18 pages, 8396 KB  
Article
Extraction, Enrichment, Characterization, and Antioxidant Activities of Sargassum fusiforme Polyphenols
by Hui Wang, Min Zhang, Weiqin Yang, Linwu Zhuang and Lei Guo
Foods 2025, 14(19), 3317; https://doi.org/10.3390/foods14193317 - 24 Sep 2025
Viewed by 11
Abstract
This study investigated the extraction, enrichment, characterization, and antioxidant activities of Sargassum fusiforme polyphenols (SFPs). The optimal extraction process conditions of SFPs are as follows: an ethanol volume fraction of 28%, a liquid–solid ratio of 29 mL/g, an extraction temperature of 80 °C, [...] Read more.
This study investigated the extraction, enrichment, characterization, and antioxidant activities of Sargassum fusiforme polyphenols (SFPs). The optimal extraction process conditions of SFPs are as follows: an ethanol volume fraction of 28%, a liquid–solid ratio of 29 mL/g, an extraction temperature of 80 °C, and an extraction time of 3.2 h. After enrichment by D101 macroporous resin, the purity of SFPs increased from 1.20 ± 0.08% to 10.78 ± 0.25%, increasing by approximately 8 times. SFPs were mainly composed of polyphenols, flavonoids, and polysaccharides. Furthermore, after identification by HPLC-QQK-ESI-MS/MS, they were found to contain 11 phlorotannins (mainly of the fuhalol type), 2 flavonoids, etc. In three antioxidant evaluation systems (DPPH free radical scavenging ability, reducing power, and total antioxidant capacity), the enriched SFPs all exhibited superior activities compared to tea polyphenols. The research results provide a theoretical basis and experimental evidence for the development of a new type of food preservative based on SFPs. Full article
(This article belongs to the Section Food Nutrition)
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19 pages, 3532 KB  
Article
The Regulation of the Albomycin and Desferrioxamine E Biosynthesis in Streptomyces globisporus bja209
by Julia A. Buyuklyan, Mikhail V. Biryukov, Yulia V. Zakalyukina and Artemy A. Sacharov
Molecules 2025, 30(19), 3871; https://doi.org/10.3390/molecules30193871 - 24 Sep 2025
Viewed by 52
Abstract
We identified Streptomyces globisporus bja209 through a targeted screen of actinomycetes from natural habitats using an E. coli JW5503 ΔtolC DualRep2(c) reporter strain. This strain produced antibacterial compounds whose action depended on the growth medium. HPLC-MS and genomic analysis revealed two metabolites: albomycin [...] Read more.
We identified Streptomyces globisporus bja209 through a targeted screen of actinomycetes from natural habitats using an E. coli JW5503 ΔtolC DualRep2(c) reporter strain. This strain produced antibacterial compounds whose action depended on the growth medium. HPLC-MS and genomic analysis revealed two metabolites: albomycin δ2 (a translation inhibitor) and desferrioxamine E. The latter induced the SOS response. Desferrioxamine E exhibited a narrow spectrum of antagonistic activity against carbapenem-resistant A. baumannii and C. michiganensis, and its production was critically regulated by iron concentration. Notably, the structurally similar desferrioxamine B was inactive. Contrary to previous reports, pangenome analysis of published GenBank genomes revealed that albomycin BGC is restricted to specific S. globisporus strains and not present in other Streptomycetes phylogenetic clades. The C-1027 BGC was found in a large linear plasmid (165.5 kb) of the S. globisporus bja209 strain and also found exclusively on linear plasmids in some of the published S. globisporus genomes. Full article
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37 pages, 2381 KB  
Article
Sequencing Analysis and Radiocarbon Dating of Yarn Fragments from Six Paracas Mantles from Bundle WK12-382
by Jaime Williams, Avi Dragun, Malak Shehab, Imani Peterkin, Ann H. Peters, Kathryn Jakes, John Southon, Collin Sauter, James Moran and Ruth Ann Armitage
Heritage 2025, 8(10), 398; https://doi.org/10.3390/heritage8100398 - 23 Sep 2025
Viewed by 153
Abstract
The Necrópolis de Wari Kayan, at the Paracas site in the coastal desert of south–central Peru, is a large archeologically excavated mortuary complex with fine textile preservation, dated approximately to 2000 BP. This study investigates loose yarns associated with textiles from Wari Kayan [...] Read more.
The Necrópolis de Wari Kayan, at the Paracas site in the coastal desert of south–central Peru, is a large archeologically excavated mortuary complex with fine textile preservation, dated approximately to 2000 BP. This study investigates loose yarns associated with textiles from Wari Kayan tomb 12 (bundle 382), collected by the late Dr. Anne Paul in 1985 at what is now the Museo Nacional de Arqueología Antropología e Historia del Perú (MNAAHP). Sequencing multiple state-of-the-art analyses, including direct analysis in real time mass spectrometry (DART-MS), high performance liquid chromatography (HPLC) with diode array detection, and accelerator mass spectrometry, on the same small sample, seeks to “squeeze out every drop” of information. Six mantles from the outer layer include different sets of color hues and values, representing either different time periods or different producer groups. Plasma oxidation at low temperature (<100 °C) prepared carbon dioxide for AMS radiocarbon analysis. Fibers remaining after oxidation were combusted for light-stable isotope analysis. The sequential analysis results in fiber and dye composition, radiocarbon age, and stable isotope fractionation values may suggest fiber origin, continuing and updating a project started over 40 years ago. Full article
(This article belongs to the Special Issue Dyes in History and Archaeology 43)
36 pages, 6718 KB  
Article
Transylvanian Grape Pomaces as Sustainable Sources of Antioxidant Phenolics and Fatty Acids—A Study of White and Red Cultivars
by Veronica Sanda Chedea, Liliana Lucia Tomoiagă, Mariana Ropota, Gabriel Marc, Floricuta Ranga, Maria Doinița Muntean, Alexandra Doina Sîrbu, Ioana Sorina Giurca, Maria Comșa, Ioana Corina Bocsan, Anca Dana Buzoianu, Hesham Kisher and Raluca Maria Pop
Antioxidants 2025, 14(10), 1152; https://doi.org/10.3390/antiox14101152 - 23 Sep 2025
Viewed by 244
Abstract
Grape pomace (GP), a significant by-product of winemaking, is gaining increasing recognition for its potential as a source of bioactive compounds with antioxidant and cardioprotective properties. This study aimed to characterize the polyphenolic profile, fatty acid composition, and antioxidant activity of 17 GP [...] Read more.
Grape pomace (GP), a significant by-product of winemaking, is gaining increasing recognition for its potential as a source of bioactive compounds with antioxidant and cardioprotective properties. This study aimed to characterize the polyphenolic profile, fatty acid composition, and antioxidant activity of 17 GP samples from Transylvanian cultivars. Polyphenolic content was determined using the Folin–Ciocalteu method and high-performance liquid chromatography coupled with diode array detection and electrospray ionization mass spectrometry (HPLC–DAD–ESI MS) analysis. Fatty acid composition was analyzed using gas chromatography with flame ionization detection (GC–FID). Antioxidant capacity was assessed using five methods, which included the 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging, 2,2′-azino-bis (3-ethylbenzothialzoline-6-sulfonic acid) (ABTS) radical scavenging, ferric-reducing antioxidant power (FRAP), cupric ion reducing antioxidant capacity (CUPRAC), and reducing power (RP) assays. Additionally, all extracts were analyzed by Fourier transform infrared (FTIR) spectroscopy to identify the presence of functional groups and chemical bonds associated with bioactive compounds. The results showed that Neuburger (NE), Radames (RA), and Regent (RE) cultivars had the highest phenolic concentrations, particularly of catechin, epicatechin, and procyanidin dimers. NE and Feteascǎ Regalǎ (FR) exhibited the greatest radical scavenging and electron transfer activities across multiple antioxidant assays. Rose Blaj (RB) and Astra (AS) displayed the most favorable fatty acid profiles, with high unsaturated-to-saturated fatty acid (UFA/SFA) and hypocholesterolemic-to-hypercholesterolemic fatty acid (H/H) ratios, as well as low atherogenicity (AI) and thrombogenicity (TI) indices, suggesting cardioprotective potential. Additionally, RB and NE cultivars also demonstrated a strong chelation of Cu2+ and Fe2+ ions, enhancing their antioxidant efficacy by mitigating metal-catalyzed oxidative stress. These findings underscore the potential of GP, particularly from NE, RB, RA, and AS cultivars, the last three of which were homologated in Transylvania at SCDVV Blaj, as valuable sources of health-promoting compounds for use in food, nutraceuticals, and other health-related applications. Full article
(This article belongs to the Section Natural and Synthetic Antioxidants)
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14 pages, 1654 KB  
Article
Plasma-Free Metanephrine and Normetanephrine Quantification for Clinical Applications Validated by Combining Solid-Phase Extraction and HPLC-MS/MS
by Hyebin Choi, Jisook Yim, Jiwon Yun, Jong Kwon Lee, Keun Ju Kim, Minjeong Nam, Myung Hyun Nam, Yunjung Cho and Seung Gyu Yun
Molecules 2025, 30(19), 3847; https://doi.org/10.3390/molecules30193847 - 23 Sep 2025
Viewed by 135
Abstract
Plasma-free metanephrines are the most sensitive and specific biochemical markers for diagnosing catecholamine-secreting tumors, such as pheochromocytoma and paraganglioma. In this study, we developed and validated a liquid chromatography–tandem mass spectrometry method for quantifying metanephrine and normetanephrine in human plasma, using solid-phase extraction [...] Read more.
Plasma-free metanephrines are the most sensitive and specific biochemical markers for diagnosing catecholamine-secreting tumors, such as pheochromocytoma and paraganglioma. In this study, we developed and validated a liquid chromatography–tandem mass spectrometry method for quantifying metanephrine and normetanephrine in human plasma, using solid-phase extraction with a weak cation-exchange mechanism. Validation was performed according to the FDA Bioanalytical Method Validation Guidance and CLSI guideline C62-A. The method showed excellent linearity over concentration ranges of 0.11–13.92 nmol/L for metanephrine and 0.14–26.43 nmol/L for normetanephrine, with correlation coefficients exceeding 0.999. The accuracy, precision, and lower limit of quantification met the acceptance criteria of the study. Matrix effect evaluation revealed a process efficiency of 121% for metanephrine at the lowest concentration, slightly exceeding the acceptable range of 100 ± 15%. This was likely because of matrix-induced ion enhancement or variability in extraction efficiency. However, all other tested concentrations were within the acceptable limits. Overall, this method demonstrated high sensitivity, specificity, and reproducibility, making it suitable for routine clinical applications. Minor deviations at low concentrations do not compromise reliability; however, future optimizations, such as matrix-matched calibration, may further improve performance. Full article
(This article belongs to the Special Issue Recent Developments in Chromatographic Applications in Medicine)
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Article
Development of an Efficient HPLC-MS/MS Method for the Detection of a Broad Spectrum of Hydrophilic and Lipophilic Contaminants in Marine Waters: An Experimental Design Approach
by Daniel Bona, Marina Di Carro, Emanuele Magi and Barbara Benedetti
Separations 2025, 12(10), 257; https://doi.org/10.3390/separations12100257 - 23 Sep 2025
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Abstract
The present study develops and optimizes a targeted chromatographic method coupled with mass spectrometry, employing design of experiments, for the determination of several emerging contaminants in environmental waters. Their widespread presence poses environmental and health risks due to their pseudo-persistence and unknown long-term [...] Read more.
The present study develops and optimizes a targeted chromatographic method coupled with mass spectrometry, employing design of experiments, for the determination of several emerging contaminants in environmental waters. Their widespread presence poses environmental and health risks due to their pseudo-persistence and unknown long-term effects. Therefore, sensitive and selective analytical methods are essential for their reliable environmental monitoring. This work focuses on 40 organic micro-contaminants with a wide range of polarities, including drugs, pesticides and UV-filters. Chromatographic separation was performed on a pentafluorophenyl column, and a Face-Centered Design was applied for multivariate optimization. Mobile phase flow and temperature were chosen as the study factors, and retention time and peak width as the responses, as indicators of analytical performance. Two optimized runs (for positive and negative electrospray ionization modes) were obtained, enabling the analysis of all 40 analytes in a total of 29 min. The final method was successfully applied to seawater samples from different sites of the Genoa harbor area. Several analytes were detected and quantified, down to the ng L−1 level, with tracers and pharmaceuticals showing the highest concentrations. The method demonstrated satisfactory accuracy, precision and specificity and is suitable for routine monitoring of a broad range of emerging contaminants in seawater. Full article
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