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Keywords = High performance liquid chromatography

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15 pages, 1507 KiB  
Article
Determination of Fumonisins B1 and B2 in Food Matrices: Optimisation of a Liquid Chromatographic Method with Fluorescence Detection
by Óscar Cebadero-Domínguez, Santiago Ruiz-Moyano, Alberto Martín and Elisabet Martín-Tornero
Toxins 2025, 17(8), 391; https://doi.org/10.3390/toxins17080391 - 5 Aug 2025
Abstract
Fumonisins, primarily produced by Fusarium spp. and Aspergillus section nigri, are common contaminants in maize, cereal grains, and other processed and derived products, representing a significant risk to food safety and public health. This study presents the development and optimisation of a [...] Read more.
Fumonisins, primarily produced by Fusarium spp. and Aspergillus section nigri, are common contaminants in maize, cereal grains, and other processed and derived products, representing a significant risk to food safety and public health. This study presents the development and optimisation of a high-performance liquid chromatography method with fluorescence detection (HPLC-FLD) for the quantification of fumonisin B1 (FB1) and B2 (FB2) in various food matrices. In contrast with conventional protocols employing potassium phosphate buffers as the mobile phase, the proposed method utilises formic acid, offering enhanced compatibility with liquid chromatography systems. An automated online precolumn derivatisation with o-phthaldialdehyde (OPA) was optimised through experimental design and response surface methodology, enabling baseline separation of FB1 and FB2 derivatives in less than 20 min. The method demonstrated high sensitivity, with limits of detection of 0.006 µg mL−1 for FB1 and 0.012 µg mL−1 for FB2, and excellent repeatability (intraday RSD values of 0.85% and 0.83%, respectively). Several solid-phase extraction (SPE) strategies were evaluated to enhance sample clean-up using a variety of food samples, including dried figs, raisins, dates, corn, cornmeal, wheat flour, and rice. FumoniStar Inmunoaffinity columns were the only clean-up method that provided optimal recoveries (70–120%) across all tested food matrices. However, the MultiSep™ 211 column yielded good recoveries for both fumonisins in dried figs and raisins. Additionally, the C18 cartridge achieved acceptable recoveries for both fumonisins in dried figs and wheat flour. Full article
(This article belongs to the Section Mycotoxins)
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24 pages, 4384 KiB  
Article
Untargeted Metabolomic Identifies Potential Seasonal Biomarkers of Semen Quality in Duroc Boars
by Notsile H. Dlamini, Serge L. Kameni and Jean M. Feugang
Biology 2025, 14(8), 995; https://doi.org/10.3390/biology14080995 (registering DOI) - 4 Aug 2025
Abstract
High semen quality is vital for reproductive success in the swine industry; however, seasonal fluctuations often compromise this quality. The molecular mechanism underlying these seasonal effects on semen quality remains largely unclear. This study employed untargeted metabolomic profiling of boar seminal plasma (SP) [...] Read more.
High semen quality is vital for reproductive success in the swine industry; however, seasonal fluctuations often compromise this quality. The molecular mechanism underlying these seasonal effects on semen quality remains largely unclear. This study employed untargeted metabolomic profiling of boar seminal plasma (SP) to identify metabolites and metabolic pathways associated with semen quality during the summer and winter months. Semen samples were collected from mature Duroc boars at a commercial boar stud and classified as Passed or Failed based on motility and morphology. SP from five samples per group was analyzed using ultra-high-performance liquid chromatography–mass spectrometry (UHPLC-MS). In total, 373 metabolites were detected in positive ion mode and 478 in negative ion mode. Several differentially expressed metabolites (DEMs) were identified, including ergothioneine, indole-3-methyl acetate, and avocadyne in the summer, as well as LysoPC, dopamine, and betaine in the winter. These metabolites are associated with key sperm functions, including energy metabolism, antioxidant defense, and capacitation. KEGG pathway analysis indicated enrichment in starch and sucrose metabolism, pyrimidine metabolism, and amino acid metabolism across the seasons. Overall, the results reveal that SP metabolomic profiles vary with the season, thereby influencing semen quality. The identified metabolites may serve as potential biomarkers for assessing semen quality and enhancing reproductive efficiency in swine production. Full article
(This article belongs to the Special Issue Reproductive Physiology and Pathology in Livestock)
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15 pages, 449 KiB  
Article
Association Between Rest–Activity Rhythm and 27-Hydroxycholesterol (27-OH) in Patients with Amnestic Mild Cognitive Impairment (aMCI)
by Seong Jae Kim, Jung Hie Lee, Jae-Won Jang, Minseo Choi and In Bum Suh
J. Clin. Med. 2025, 14(15), 5481; https://doi.org/10.3390/jcm14155481 - 4 Aug 2025
Abstract
Background/Objectives: Rest–activity rhythm (RAR) disturbances can contribute to aging and dementia via metabolic dysregulation. Hydroxycholesterol (OH) is thought to mediate the link between hypercholesterolemia and neurodegeneration. This study compared sleep and RAR parameters between amnestic mild cognitive impairment (aMCI) patients and normal [...] Read more.
Background/Objectives: Rest–activity rhythm (RAR) disturbances can contribute to aging and dementia via metabolic dysregulation. Hydroxycholesterol (OH) is thought to mediate the link between hypercholesterolemia and neurodegeneration. This study compared sleep and RAR parameters between amnestic mild cognitive impairment (aMCI) patients and normal controls (NCs), and examined their associations with plasma 27-OH levels, reflecting peripheral cholesterol metabolism. Methods In total, 18 aMCI patients (76.6 ± 6.1 years) and 21 NCs (70.4 ± 6.7 years) underwent five-day actigraphy and dim light melatonin onset assessment. Plasma 27-OH levels were measured via high-performance liquid chromatography-mass spectrometry. Generalized linear models (GLMs) were used to analyze the relationships between sleep, RAR, and 27-OH levels. Results: The aMCI group had significantly lower 27-OH levels and 27-OH/total cholesterol ratios (p < 0.05). GLM revealed that longer sleep onset latency (SOL) was associated with higher 27-OH levels in aMCI, distinguishing them from NCs. Additionally, in aMCI, longer SOL, lower sleep efficiency (SE), and higher fragmentation index (FI) were associated with an increased 27-OH/total cholesterol ratio (p < 0.05). Higher relative amplitude of RAR was linked to lower 27-OH levels across groups (p < 0.01), but RAR parameters showed no significant association with the 27-OH/total cholesterol ratio. Sleep disturbances, including prolonged SOL, reduced SE, and increased FI, were associated with altered peripheral cholesterol oxygenation in aMCI. Conclusions: Greater RAR amplitude correlated with lower 27-OH levels, regardless of cognitive status. These findings suggest that peripheral cholesterol oxygenation in aMCI is related to both sleep disturbances and circadian rhythm dysregulation, highlighting their role in cholesterol metabolism and neurodegeneration. Full article
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19 pages, 3213 KiB  
Article
Comparison and Study on Flavor and Quality Characteristics of Different Grades of Tianshanhong (TSH)
by Shu-Ting Xiao, Xian-Zhou Huang, Jian-Feng Huang, Qing-Yang Wu, Yang Wu, Ting-Ting Deng, Xian-Xian Xu, Hao-Xiang Liu, Xiao-Hui Chen, Shi-Zhong Zheng and Zi-Wei Zhou
Beverages 2025, 11(4), 111; https://doi.org/10.3390/beverages11040111 - 4 Aug 2025
Abstract
Tianshanhong (TSH), black tea products originating from the Ningde Tianshan Mountain, has gained significant recognition in the market. However, the chemical characteristics contributing to the flavor of TSH have not yet been reported. To systematically investigate the non-volatile and volatile compounds in TSH, [...] Read more.
Tianshanhong (TSH), black tea products originating from the Ningde Tianshan Mountain, has gained significant recognition in the market. However, the chemical characteristics contributing to the flavor of TSH have not yet been reported. To systematically investigate the non-volatile and volatile compounds in TSH, four grades of TSH were evaluated using national standard sensory methods, revealing that overall quality improved with higher grades. Based on the detection of ultra-performance liquid chromatography–mass spectrometry (UPLC-MS), the content of ester-type catechins was relatively high and decreased with lower grades. A total of 19 amino acids (AAs) were clustered, among them, three amino acids, L-Theanine (L-Thea), Arg, and GABA, showed highly significant correlations with the refreshing taste of TSH. Notably, the content of Arg had the highest correlation with TSH grade, with a coefficient of 0.976 (p < 0.01). According to gas chromatography mass spectrometry (GC-MS) analysis, a total of 861 kinds of volatile compounds were detected, with 282 identified and aroma-active compounds across grades selected using the PLS model. Methyl salicylate and geraniol were particularly notable, showing strong correlations with TSH grades at 0.975 and 0.987 (p < 0.01), respectively. Our findings show that non-volatile and volatile compounds can rationally grade TSH and help understand its flavor quality. Full article
(This article belongs to the Section Tea, Coffee, Water, and Other Non-Alcoholic Beverages)
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13 pages, 1608 KiB  
Article
Enhanced Antioxidant and Anti-Inflammatory Activities of Diospyros lotus Leaf Extract via Enzymatic Conversion of Rutin to Isoquercitrin
by Yeong-Su Kim, Chae Sun Na and Kyung-Chul Shin
Antioxidants 2025, 14(8), 950; https://doi.org/10.3390/antiox14080950 (registering DOI) - 2 Aug 2025
Viewed by 103
Abstract
Isoquercitrin, a monoglucoside form of quercetin, exhibits superior antioxidant, anti-inflammatory, and cardiovascular protective effects in comparison to its precursor, rutin. However, its natural abundance is limited. This study aimed to increase the functional value of Diospyros lotus leaf extract through enzymatic conversion of [...] Read more.
Isoquercitrin, a monoglucoside form of quercetin, exhibits superior antioxidant, anti-inflammatory, and cardiovascular protective effects in comparison to its precursor, rutin. However, its natural abundance is limited. This study aimed to increase the functional value of Diospyros lotus leaf extract through enzymatic conversion of rutin to isoquercitrin using α-l-rhamnosidase and to evaluate the changes in biological activities after conversion. A sugar-free D. lotus leaf extract was prepared and subjected to enzymatic hydrolysis with α-l-rhamnosidase under optimized conditions (pH 5.5, 55 °C, and 0.6 U/mL). Isoquercitrin production was monitored via high-performance liquid chromatography. Antioxidant and anti-inflammatory activities were assessed using the 2,2-diphenyl-1-picrylhydrazyl radical scavenging and lipoxygenase (LOX) inhibition assays, respectively. The enzymatic reaction resulted in complete conversion of 30 mM rutin into isoquercitrin within 180 min, increasing isoquercitrin content from 9.8 to 39.8 mM. The enzyme-converted extract exhibited significantly enhanced antioxidant activity, with a 48% improvement in IC50 value compared with the untreated extract. Similarly, LOX inhibition increased from 39.2% to 48.3% after enzymatic conversion. Both extracts showed higher inhibition than isoquercitrin alone, indicating synergistic effects of other phytochemicals present in the extract. This study is the first to demonstrate that α-l-rhamnosidase-mediated conversion of rutin to isoquercitrin in D. lotus leaf extract significantly improves its antioxidant and anti-inflammatory activities. The enzymatically enhanced extract shows potential as a functional food or therapeutic ingredient. Full article
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24 pages, 1244 KiB  
Article
HPLC-ESI-HRMS/MS-Based Metabolite Profiling and Bioactivity Assessment of Catharanthus roseus
by Soniya Joshi, Chen Huo, Rabin Budhathoki, Anita Gurung, Salyan Bhattarai, Khaga Raj Sharma, Ki Hyun Kim and Niranjan Parajuli
Plants 2025, 14(15), 2395; https://doi.org/10.3390/plants14152395 - 2 Aug 2025
Viewed by 605
Abstract
A comprehensive metabolic profiling of Catharanthus roseus (L.) G. Don was performed using tandem mass spectrometry, along with an evaluation of the biological activities of its various solvent extracts. Among these, the methanolic leaf extract exhibited mild radical scavenging activity, low to moderate [...] Read more.
A comprehensive metabolic profiling of Catharanthus roseus (L.) G. Don was performed using tandem mass spectrometry, along with an evaluation of the biological activities of its various solvent extracts. Among these, the methanolic leaf extract exhibited mild radical scavenging activity, low to moderate antimicrobial activity, and limited cytotoxicity in both the brine shrimp lethality assay and MTT assay against HeLa and A549 cell lines. High-performance liquid chromatography–electrospray ionization–high-resolution tandem mass spectrometry (HPLC-ESI-HRMS/MS) analysis led to the annotation of 34 metabolites, primarily alkaloids. These included 23 indole alkaloids, two fatty acids, two pentacyclic triterpenoids, one amino acid, four porphyrin derivatives, one glyceride, and one chlorin derivative. Notably, two metabolites—2,3-dihydroxypropyl 9,12,15-octadecatrienoate and (10S)-hydroxypheophorbide A—were identified for the first time in C. roseus. Furthermore, Global Natural Products Social Molecular Networking (GNPS) analysis revealed 18 additional metabolites, including epoxypheophorbide A, 11,12-dehydroursolic acid lactone, and 20-isocatharanthine. These findings highlight the diverse secondary metabolite profile of C. roseus and support its potential as a source of bioactive compounds for therapeutic development. Full article
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17 pages, 1195 KiB  
Article
Phytochemical Profiling, Antioxidant Capacity, and α-Amylase/α-Glucosidase Inhibitory Effects of 29 Faba Bean (Vicia faba L.) Varieties from China
by Ying Li, Zhihua Wang, Chengkai Mei, Wenqi Sun, Xingxing Yuan, Jing Wang and Wuyang Huang
Biology 2025, 14(8), 982; https://doi.org/10.3390/biology14080982 (registering DOI) - 2 Aug 2025
Viewed by 179
Abstract
Faba bean (Vicia faba L.), a nutrient-rich legume beneficial to human health, is valued for its high L-3,4-dihydroxyphenylalanine (L-DOPA) and phenolic content. This study investigated phytochemical diversity and bioactivity across 29 Chinese faba bean varieties. Phenolics were profiled using ultrahigh-performance liquid chromatography [...] Read more.
Faba bean (Vicia faba L.), a nutrient-rich legume beneficial to human health, is valued for its high L-3,4-dihydroxyphenylalanine (L-DOPA) and phenolic content. This study investigated phytochemical diversity and bioactivity across 29 Chinese faba bean varieties. Phenolics were profiled using ultrahigh-performance liquid chromatography with quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS) and quantified via high-performance liquid chromatography (HPLC). Antioxidant capacity was evaluated, including DPPH (2,2-diphenyl-1-picrylhydrazyl), ABTS (2,2-azinobis (3-ethylbenzothiazoline-6-sulfonic acid)) radical scavenging activity, and ferric reducing antioxidant power (FRAP), along with α-amylase/α-glucosidase inhibitory effects. Twenty-five phenolics were identified, including L-DOPA (11.96–17.93 mg/g, >70% of total content), seven phenolic acids, and seventeen flavonoids. L-DOPA showed potent enzyme inhibition (IC50 values of 22.45 μM for α-amylase and 16.66 μM for α-glucosidase) but demonstrated limited antioxidant effects. Lincan 13 (Gansu) exhibited the strongest antioxidant activity (DPPH, 16.32 μmol trolox/g; ABTS, 5.85 μmol trolox/g; FRAP, 21.38 mmol Fe2+/g), which correlated with it having the highest flavonoid content (40.51 mg rutin/g), while Yican 4 (Yunnan) showed the strongest α-amylase inhibition (43.33%). Correlation analysis confirmed flavonoids as the primary antioxidants, and principal component analysis (PCA) revealed geographical trends (e.g., Jiangsu varieties were particularly phenolic-rich). These findings highlight faba beans’ potential as functional foods and guide genotype selection in targeted breeding programs aimed at enhancing health benefits. Full article
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17 pages, 1511 KiB  
Article
Impact of Selected Starter-Based Sourdough Types on Fermentation Performance and Bio-Preservation of Bread
by Khadija Atfaoui, Sara Lebrazi, Anas Raffak, Youssef Chafai, Karima El Kabous, Mouhcine Fadil and Mohammed Ouhssine
Fermentation 2025, 11(8), 449; https://doi.org/10.3390/fermentation11080449 - 1 Aug 2025
Viewed by 207
Abstract
The aim of this study is to evaluate the effects of different types of sourdough (I to IV), developed with a specific starter culture (including Lactiplantibacillus plantarum, Levilactobacillus brevis, and Candida famata), on bread fermentation performance and shelf-life. Real-time tracking of multiple [...] Read more.
The aim of this study is to evaluate the effects of different types of sourdough (I to IV), developed with a specific starter culture (including Lactiplantibacillus plantarum, Levilactobacillus brevis, and Candida famata), on bread fermentation performance and shelf-life. Real-time tracking of multiple parameters (pH, dough rising, ethanol release, and total titratable acidity) was monitored by a smart fermentation oven. The impact of the different treatments on the lactic acid, acetic acid, and ethanol content of the breads were quantified by high performance liquid chromatography analysis. In addition, the bio-preservation capacity of the breads contaminated with fungi was analyzed. The results show that liquid sourdough (D3: Type 2) and backslopped sourdough (D4: Type 3) increased significantly (p < 0.05) in dough rise, dough acidification (lower pH, higher titratable acidity), production of organic acids (lactic and acetic), and presented the optimal fermentation quotient. These findings were substantiated by chemometric analysis, which successfully clustered the starters based on performance and revealed a strong positive correlation between acetic acid production and dough-rise, highlighting the superior heterofermentative profile of D3 and D4. These types of sourdough also stood out for their antifungal capacity, preventing the visible growth of Aspergillus niger and Penicillium commune for up to 10 days after inoculation. Full article
(This article belongs to the Section Fermentation for Food and Beverages)
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30 pages, 4423 KiB  
Review
Overview of Fatty Acids and Volatiles in Selected Nuts: Their Composition and Analysis
by Gbolahan Alagbe, Klara Urbanova and Olajumoke Alagbe
Processes 2025, 13(8), 2444; https://doi.org/10.3390/pr13082444 - 1 Aug 2025
Viewed by 296
Abstract
Nuts are nutrient-dense foods recognized for their complex chemical composition and associated health benefits. This review provides a comprehensive overview of the botanical classification, morphology, production, and consumption patterns of key nut species, including walnuts, almonds, pistachios, pecans, peanuts, cashews, bitter kola, and [...] Read more.
Nuts are nutrient-dense foods recognized for their complex chemical composition and associated health benefits. This review provides a comprehensive overview of the botanical classification, morphology, production, and consumption patterns of key nut species, including walnuts, almonds, pistachios, pecans, peanuts, cashews, bitter kola, and kola nuts. It emphasizes the fatty acid profiles, noting that palmitic acid (C16:0) is the predominant saturated fatty acid, while oleic acid (C18:1) and linoleic acid (C18:2) are the most abundant monounsaturated and polyunsaturated fatty acids, respectively. The review also details various analytical techniques employed for extracting and characterizing bioactive compounds, which are crucial for assessing nut quality and health benefits. Methods such as Soxhlet extraction, solid-phase microextraction (SPME), supercritical fluid extraction (SFE), gas chromatography (GC-FID and GC-MS), and high-performance liquid chromatography (HPLC) are highlighted. Furthermore, it discusses scientific evidence linking nut consumption to antioxidant and anti-inflammatory properties, improved cardiovascular health, and a reduced risk of type 2 diabetes, establishing nuts as important components in a healthy diet. This review underscores the role of nuts as functional foods and calls for standardized methodologies in future lipidomic and volatilomic studies. Full article
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16 pages, 1365 KiB  
Article
Generation of Formates Following 20 kHz Sonication of DSPE-mPEG2000 PEGylated Phospholipid Micelles
by Perouza Parsamian and Paul Pantano
Pharmaceutics 2025, 17(8), 1008; https://doi.org/10.3390/pharmaceutics17081008 - 1 Aug 2025
Viewed by 244
Abstract
Background: Previous research has demonstrated that 20 kHz probe or 37 kHz bath sonication of poloxamers comprising polypropylene glycol (PPG) and polyethylene glycol (PEG) blocks can generate degradation byproducts that are toxic to mammalian cells and organisms. Herein, an investigation of a [...] Read more.
Background: Previous research has demonstrated that 20 kHz probe or 37 kHz bath sonication of poloxamers comprising polypropylene glycol (PPG) and polyethylene glycol (PEG) blocks can generate degradation byproducts that are toxic to mammalian cells and organisms. Herein, an investigation of a PEGylated phospholipid micelle was undertaken to identify low-molecular-weight sonolytic degradation byproducts that could be cytotoxic. The concern here lies with the fact that sonication is a frequently employed step in drug delivery manufacturing processes, during which PEGylated phospholipids can be subjected to shear forces and other extreme oxidative and thermal conditions. Methods: Control and 20 kHz-sonicated micelles of DSPE-mPEG2000 were analyzed using dynamic light scattering (DLS) and zeta potential analyses to study colloidal properties, matrix-assisted laser desorption/ionization–time of flight (MALDI-TOF) mass spectroscopy (MS) and proton nuclear magnetic resonance (1H-NMR) spectroscopy to study the structural integrity of DSPE-mPEG2000, and 1H-NMR spectroscopy and high-performance liquid chromatography (HPLC) with ultraviolet (UV) detection to quantitate the formation of low-molecular-weight degradation byproducts. Results: MALDI-TOF-MS analyses of 20 kHz-sonicated DSPE-mPEG2000 revealed the loss of ethylene glycol moieties in accordance with depolymerization of the PEG chain; 1H-NMR spectroscopy showed the presence of formate, a known oxidative/thermal degradation product of PEG; and HPLC-UV showed that the generation of formate was dependent on 20 kHz probe sonication time between 5 and 60 min. Conclusions: It was found that 20 kHz sonication can degrade the PEG chain of DSPE-mPEG2000, altering the micelle’s PEG corona and generating formate, a known ocular toxicant. Full article
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36 pages, 3621 KiB  
Review
Harnessing Molecular Phylogeny and Chemometrics for Taxonomic Validation of Korean Aromatic Plants: Integrating Genomics with Practical Applications
by Adnan Amin and Seonjoo Park
Plants 2025, 14(15), 2364; https://doi.org/10.3390/plants14152364 - 1 Aug 2025
Viewed by 311
Abstract
Plant genetics and chemotaxonomic analysis are considered key parameters in understanding evolution, plant diversity and adaptation. Korean Peninsula has a unique biogeographical landscape that supports various aromatic plant species, each with considerable ecological, ethnobotanical, and pharmacological significance. This review aims to provide a [...] Read more.
Plant genetics and chemotaxonomic analysis are considered key parameters in understanding evolution, plant diversity and adaptation. Korean Peninsula has a unique biogeographical landscape that supports various aromatic plant species, each with considerable ecological, ethnobotanical, and pharmacological significance. This review aims to provide a comprehensive overview of the chemotaxonomic traits, biological activities, phylogenetic relationships and potential applications of Korean aromatic plants, highlighting their significance in more accurate identification. Chemotaxonomic investigations employing techniques such as gas chromatography mass spectrometry, high-performance liquid chromatography, and nuclear magnetic resonance spectroscopy have enabled the identification of essential oils and specialized metabolites that serve as valuable taxonomic and diagnostic markers. These chemical traits play essential roles in species delimitation and in clarifying interspecific variation. The biological activities of selected taxa are reviewed, with emphasis on antimicrobial, antioxidant, anti-inflammatory, and cytotoxic effects, supported by bioassay-guided fractionation and compound isolation. In parallel, recent advances in phylogenetic reconstruction employing DNA barcoding, internal transcribed spacer regions, and chloroplast genes such as rbcL and matK are examined for their role in clarifying taxonomic uncertainties and inferring evolutionary lineages. Overall, the search period was from year 2001 to 2025 and total of 268 records were included in the study. By integrating phytochemical profiling, pharmacological evidence, and molecular systematics, this review highlights the multifaceted significance of Korean endemic aromatic plants. The conclusion highlights the importance of multidisciplinary approaches including metabolomics and phylogenomics in advancing our understanding of species diversity, evolutionary adaptation, and potential applications. Future research directions are proposed to support conservation efforts. Full article
(This article belongs to the Special Issue Applications of Bioinformatics in Plant Science)
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18 pages, 2077 KiB  
Article
Impact of Omega-3 and Vitamin D Supplementation on Bone Turnover Markers in Children with Leukemia: Follow-Up During and After Supplementation
by Lourdes Barbosa-Cortés, Sharon B. Morales-Montes, Michelle Maldonado-Alvarado, Jorge A. Martin-Trejo, Salvador Atilano-Miguel, Emmanuel Jiménez-Aguayo, Fabián I. Martínez-Becerril, Víctor M. Cortés-Beltrán, Atzin V. Hernández-Barbosa, Karina A. Solís-Labastida, Jorge Maldonado-Hernández, Benito A. Bautista-Martínez, Azalia Juárez-Moya, Zayra Hernández-Piñón, Juan M. Domínguez-Salgado, Judith Villa-Morales and Israel Domínguez-Calderón
Nutrients 2025, 17(15), 2526; https://doi.org/10.3390/nu17152526 - 31 Jul 2025
Viewed by 264
Abstract
Background/Objective: In patients with acute lymphoblastic leukemia (ALL), it has been demonstrated that the treatment has a negative effect on bone health. The n-3 polyunsaturated fatty acids (LCPUFAs-ω3) may attenuate bone resorption. We evaluated the effects of LCPUFAs-ω3, vitamin D, and [...] Read more.
Background/Objective: In patients with acute lymphoblastic leukemia (ALL), it has been demonstrated that the treatment has a negative effect on bone health. The n-3 polyunsaturated fatty acids (LCPUFAs-ω3) may attenuate bone resorption. We evaluated the effects of LCPUFAs-ω3, vitamin D, and calcium supplementation on bone turnover markers and changes in vitamin D concentrations during 6 weeks of supplementation and during 6 weeks of post-intervention follow-up in pediatric patients with ALL. Methods: Thirty-six pediatric patients with ALL were randomly assigned to the ω-3VDCa group (100 mg/kg/d LCPUFAs-ω3 + 4000 IU vitamin D + 1000 mg calcium) or the VDCa group (4000 IU vitamin D + 1000 mg calcium) for 6 weeks. Blood samples were collected to determine 25(OH)D, PTH, ICTP, and TRAP-5b (biomarkers of bone resorption) and osteocalcin (OC, a biomarker of bone production) levels at baseline, 6 weeks, and 12 weeks after supplementation. The 25(OH)D analysis was performed using ultra-high-performance liquid chromatography coupled to a mass spectrometer, and PTH and bone turnover markers were measured by ELISA. Results: The 25(OH)D concentration increased in both groups (ω3VDCa group: 19.4 ng/mL vs. 44.0 ng/mL, p < 0.0001; VDCa group: 15.3 ng/mL vs. 42.8 ng/mL, p = 0.018) and remained significantly higher at 12 weeks. At 12 weeks, ICTP showed lower concentrations in the ω-3VDCa group than in the VDCa group (0.74 ng/mL vs. 1.05 ng/mL, p = 0.024). Conclusions: Combined omega-3 and 4000 IU vitamin D supplementation for 6 weeks had a positive effect on bone health, as indicated by serum ICTP, with no effect on serum 25(OH)D levels over vitamin D supplementation alone. Full article
(This article belongs to the Special Issue Dietary Supplements and Chronic Diseases)
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24 pages, 1766 KiB  
Article
From Waste to Resource: Chemical Characterization of Olive Oil Industry By-Products for Sustainable Applications
by Maria de Lurdes Roque, Claudia Botelho and Ana Novo Barros
Molecules 2025, 30(15), 3212; https://doi.org/10.3390/molecules30153212 - 31 Jul 2025
Viewed by 242
Abstract
The olive oil industry, a key component of Southern Europe’s agricultural sector, generates large amounts of by-products during processing, including olive leaves, branches, stones, and seeds. In the context of growing environmental concerns and limited natural resources—particularly in the Mediterranean regions—there is increasing [...] Read more.
The olive oil industry, a key component of Southern Europe’s agricultural sector, generates large amounts of by-products during processing, including olive leaves, branches, stones, and seeds. In the context of growing environmental concerns and limited natural resources—particularly in the Mediterranean regions—there is increasing interest in circular economy approaches that promote the valorization of agricultural residues. These by-products are rich in bioactive compounds, particularly phenolics such as oleuropein and hydroxytyrosol, which are well known for their antioxidant and anti-inflammatory activities. This study aimed to evaluate the phenolic content and antioxidant capacity of by-products from three olive cultivars using high-performance liquid chromatography with photodiode array detection (HPLC–PDA) and mass spectrometry (MS). The leaves and seeds, particularly from the “Cobrança” and a non-identified variety, presented the highest antioxidant activity, as well as the highest concentration of phenolic compounds, demonstrating once again the direct relationship between these two parameters. The identification of the compounds present demonstrated that the leaves and branches have a high diversity of phenolic compounds, particularly secoiridoids, flavonoids, phenylpropanoids, phenylethanoids, and lignans. An inverse relationship was observed between the chlorophyll and carotenoid content and the antioxidant activity, suggesting that phenolic compounds, rather than pigments, are the major contributors to antioxidant properties. Therefore, the by-products of the olive oil industry are a valuable source of sustainable bioactive compounds for distinct industrial sectors, such as the food, nutraceutical, and pharmaceutical industries, aligning with the European strategies for resource efficiency and waste reduction in the agri-food industries. Full article
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16 pages, 1659 KiB  
Article
Ricinus communis L. Leaf Extracts as a Sustainable Alternative for Weed Management
by Aline Mazoy Lopes, Lucas Kila Ribeiro, Maurício Ricardo de Melo Cogo, Lucas Mironuk Frescura, Marcelo Barcellos da Rosa, Alex Schulz, Flávio Dias Mayer, Ederson Rossi Abaide, Marcus Vinícius Tres and Giovani Leone Zabot
Sustainability 2025, 17(15), 6942; https://doi.org/10.3390/su17156942 - 30 Jul 2025
Viewed by 181
Abstract
Weeds pose a significant challenge to agricultural productivity, requiring control strategies that are both effective and environmentally sustainable. Therefore, this study evaluated the inhibitory potential of aqueous extracts from Ricinus communis L. leaves to manage the weeds Oryza sativa L. (weedy rice) and [...] Read more.
Weeds pose a significant challenge to agricultural productivity, requiring control strategies that are both effective and environmentally sustainable. Therefore, this study evaluated the inhibitory potential of aqueous extracts from Ricinus communis L. leaves to manage the weeds Oryza sativa L. (weedy rice) and Cyperus ferax. Extracts were obtained through pressurized liquid extraction using water as the solvent. Bioassays were conducted during pre- and post-emergence stages by foliar spraying 15 and 30 days after sowing (DAS). The effect of extraction time (1–30 min) on inhibitory efficacy was also assessed. Chemical profiles of the extracts were characterized using high-performance liquid chromatography. The extracts significantly inhibited seed germination, with suppression rates reaching 92.7%. Plant growth was also diminished, particularly with earlier treatments (at 15 DAS), resulting in reductions of up to 32% and 53% in shoot length, and 69% and 73% in total dry mass for O. sativa L. and C. ferax, respectively. Mortality rates of O. sativa L. and C. ferax reached 64% and 58%, respectively. Phenolic compounds were identified in the extracts, and higher concentrations were observed at shorter extraction times. These findings underscore the potential of R. communis L. leaf extracts as an ecologically sustainable alternative for weed management, providing an effective and natural approach that may reduce reliance on synthetic herbicides and mitigate their environmental impact. Full article
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10 pages, 1225 KiB  
Article
Development of an LC-MS Method for the Analysis of Birch (Betula sp.) Bark Bioactives Extracted with Biosolvents
by Inmaculada Luque-Jurado, Jesús E. Quintanilla-López, Rosa Lebrón-Aguilar, Ana Cristina Soria and María Luz Sanz
Molecules 2025, 30(15), 3181; https://doi.org/10.3390/molecules30153181 - 29 Jul 2025
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Abstract
Birch (Betula sp.) bark is a well-known natural source of betulin (Bet) and betulinic acid (BAc), both of which have several bioactive properties. The evaluation of the extraction performance, relative to these lupane-type triterpenoids, provided by different biosolvents requires the development of [...] Read more.
Birch (Betula sp.) bark is a well-known natural source of betulin (Bet) and betulinic acid (BAc), both of which have several bioactive properties. The evaluation of the extraction performance, relative to these lupane-type triterpenoids, provided by different biosolvents requires the development of a high-resolution and high-sensitivity liquid chromatography-mass spectrometry (LC-MS) approach that is also compatible with challenging extractants such as natural deep eutectic solvents (NADESs). In this work, an LC-MS method was developed and analytically characterized prior to its application for the quantitation of Bet and BAc in birch bark extracts obtained using conventional solvents (methanol and acetone) and biosolvents (limonene and NADESs). High precision (RSD < 3.3%), sensitivity (LOD: 23 ng mL−1 and 29 ng mL−1 for Bet and BAc, respectively), and accuracy (95–102% recovery) were found for this optimized method, using an acidulated water–methanol mixture as the mobile phase and sodium acetate as an additive. Extraction experiments conducted at 55 °C revealed that the NADESs, particularly thymol:1-octanol (1:1 molar ratio), outperformed the other solvents and were highly effective for the recovery of both triterpenoids (17.50 mg g−1 and 0.92 mg g−1 of Bet and BAc, respectively). This method can also be applied to similar extracts obtained from other biomasses. Full article
(This article belongs to the Special Issue New Advances in Deep Eutectic Solvents, 2nd Edition)
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