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Keywords = ion chromatography

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26 pages, 5614 KB  
Article
Potentially Toxic Elements in Phosphate Processing: A Comparative Assessment of Solid Wastes and Effluents from Beneficiation and Fertilizer Production in Southwest Tunisia
by Elhem Bouchiba, Ariadna Verdaguer, Cristian Gómez Canela, Eduardo Alberto López-Maldonado and Mohamed Ali Borgi
Toxics 2026, 14(5), 438; https://doi.org/10.3390/toxics14050438 - 15 May 2026
Viewed by 237
Abstract
This study investigates the environmental and health impacts of potentially toxic elements (PTEs) in solid and liquid wastes from phosphate beneficiation and fertilizer production in the Mdhilla area, Gafsa Basin, Tunisia. Solid wastes, including phosphate tailings (PTs) and phosphogypsum (PG), and associated industrial [...] Read more.
This study investigates the environmental and health impacts of potentially toxic elements (PTEs) in solid and liquid wastes from phosphate beneficiation and fertilizer production in the Mdhilla area, Gafsa Basin, Tunisia. Solid wastes, including phosphate tailings (PTs) and phosphogypsum (PG), and associated industrial effluents from phosphate beneficiation (PBE) and fertilizer production (PFE), were characterized using physicochemical analysis, ICP-MS, SEM–EDX, and ion chromatography. Single and integrated pollution indices, along with conservative human health risk assessments, were applied to evaluate cumulative contamination and potential risks. PT exhibited near-neutral pH (7.64) and high PTE enrichment (Zn 350 mg kg−1, Cr 329 mg kg−1, Cd 38.8 mg kg−1), whereas PG was strongly acidic (pH 3.13) and comparatively depleted in metals, reflecting process-dependent partitioning. Despite neutral pH, PBEs contained markedly higher metal concentrations than PFEs, with Fe (163 mg L−1), Cr (3.09 mg L−1), Cd (0.49 mg L−1), and Pb (0.71 mg L−1) exceeding discharge limits. Pollution indices indicated severe to extreme contamination, with PBE showing an exceptionally high contamination degree (Cdeg = 63,659) compared to PFE (Cdeg = 12,815), and elevated Toxic Element Pollution Index (PTEPI) values confirmed stronger cumulative pollution in PBE. Potential ecological risk indices (PERI > 600) revealed very high ecological risk for both effluents, primarily driven by Cd, Co, and Tl. Although dermal contact may represent the most frequent exposure route, risk assessment results indicated that accidental oral ingestion is the dominant pathway contributing to both non-carcinogenic and carcinogenic risks, with children being particularly vulnerable. Non-carcinogenic risk thresholds (HQ > 1) were exceeded for PBE, while total carcinogenic risks approached or exceeded regulatory limits (10−6–10−4), mainly due to Cd and Cr. Overall, phosphate beneficiation was the primary source of cumulative metal loading and associated ecological and health risks, while fertilizer production partially reduced contamination. These findings underscore the urgent need for improved management and mitigation of phosphate-processing wastes in industrial regions. Full article
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27 pages, 8078 KB  
Article
Multi-Omics Integration to Investigate the Effects of Variety and Origin on Volatile and Non-Volatile Metabolites in Melons
by Junzhe Hua, Kemin Mao, Wenlong Yu, Zongyang Li, Runhan Wen, Lingyu Li, Liyan Song, Yaxin Sang and Xianghong Wang
Foods 2026, 15(10), 1746; https://doi.org/10.3390/foods15101746 - 15 May 2026
Viewed by 197
Abstract
This study investigated the effects of different cultivation environments on melon quality development and the underlying metabolic regulatory mechanisms. Using ‘Yangjiaocui’ and ‘Boyang 9’ melons, we systematically compared their physicochemical properties, nutritional components, volatile compounds, and metabolites under saline–alkali versus normal conditions, employing [...] Read more.
This study investigated the effects of different cultivation environments on melon quality development and the underlying metabolic regulatory mechanisms. Using ‘Yangjiaocui’ and ‘Boyang 9’ melons, we systematically compared their physicochemical properties, nutritional components, volatile compounds, and metabolites under saline–alkali versus normal conditions, employing an integrated multi-omics analytical model. The results showed that saline–alkali cultivation significantly increased several nutritional components (e.g., soluble solids, vitamin C, flavonoids, and polyphenols) compared to normal conditions. Gas chromatography–ion mobility spectrometry (GC-IMS) detected 36 volatiles, predominantly esters and ketones, with 13 key markers such as isovaleric acid isovaleryl ester and ethyl butyrate, effectively discriminating cultivars and growth origins. Liquid chromatography–mass spectrometry (LC-MS) detected 702 metabolites, chiefly organic acids and lipids. KEGG pathway enrichment analysis revealed that flavonoid biosynthesis was the most significantly enriched pathway (enrichment factor ~1, extreme significance), with coordinated regulation of tyrosine and phenylalanine metabolism redirecting metabolic flux toward defensive secondary metabolites. In conclusion, our results suggest that saline–alkali cultivation may contribute to improved nutritional profiles, and multi-omics analysis effectively differentiates melon varieties and origins. This study provides a theoretical basis for understanding the quality, flavor, and metabolite profiles of melon under saline–alkali stress, employing a multi-omics approach. Full article
(This article belongs to the Special Issue Sensory Detection and Analysis in Food Industry)
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24 pages, 1154 KB  
Article
Polysaccharides from the Coelomic Fluid of Urechis unicinctus: Extraction, Structural Diversity, and Potential Against Hypoxia
by Xiaodi Wang, Wenjie Wang, Rongfeng Li, Kun Gao, Ronge Xing, Xuexin Zhang, Gaoli Zhou, Lijing Yin, Junhao Chen, Hang Li and Guantian Li
Polymers 2026, 18(10), 1203; https://doi.org/10.3390/polym18101203 - 14 May 2026
Viewed by 509
Abstract
The marine benthic invertebrate Urechis unicinctus exhibits extraordinary tolerance to hypoxic environments, making its coelomic fluid a unique and promising biological source for discovering novel stress-adapting macromolecules. Polysaccharides derived from the coelomic fluid of U. unicinctus were systematically extracted, fractionated, and characterized to [...] Read more.
The marine benthic invertebrate Urechis unicinctus exhibits extraordinary tolerance to hypoxic environments, making its coelomic fluid a unique and promising biological source for discovering novel stress-adapting macromolecules. Polysaccharides derived from the coelomic fluid of U. unicinctus were systematically extracted, fractionated, and characterized to investigate their structural features and associated biological activities. Gradient ethanol precipitation (30–80%) combined with DEAE-52 ion exchange chromatography yielded twelve fractions with distinct physicochemical properties. Significant variations were observed in molecular weight (103–105 Da), sulfate content (3.77–24.26%), and monosaccharide composition. High-ethanol fractions, particularly U68P and U18P (extracted at 60 °C and 100 °C, respectively, and both precipitated with 80% ethanol), were enriched in low-molecular-weight, highly sulfated heteropolysaccharides composed of galactose, fucose, glucosamine, and ribose. These fractions exhibited superior antioxidant activities, including strong scavenging effects against DPPH, ABTS, and hydroxyl radicals. Moreover, they demonstrated pronounced neuroprotective effects in the oxygen–glucose deprivation/reoxygenation (OGD/R) model using SH-SY5Y cells, significantly improving cell viability. Structure–activity relationship analysis revealed that reduced molecular weight, increased sulfation degree, and more diverse monosaccharide composition (e.g., more diverse monosaccharide composition) synergistically contribute to improved bioactivity by facilitating cellular uptake and exposing functional groups. In contrast, high-molecular-weight homoglucan fractions showed relatively weak effects. Overall, this study identifies U. unicinctus coelomic fluid as a promising source of bioactive polysaccharides and provides a theoretical basis for the development of marine-derived anti-hypoxic and antioxidant agents. Full article
(This article belongs to the Special Issue Polysaccharides: Synthesis, Properties and Applications—2nd Edition)
15 pages, 1106 KB  
Article
Effect of Microwave-Assisted Heat–Moisture Treatment on Structure, Physicochemical Properties and In Vitro Digestibility of Wheat Starch
by Liuyan Chen, Jiawen Liu, Chao Yuan and Bo Cui
Foods 2026, 15(10), 1698; https://doi.org/10.3390/foods15101698 - 12 May 2026
Viewed by 181
Abstract
Wheat starch serves as a major dietary carbohydrate. Optimizing its structural and functional properties is essential for developing health foods. In the present study, microwave-assisted heat–moisture treatment (MHT) was applied to modify wheat starch and the effects of the physical treatments on its [...] Read more.
Wheat starch serves as a major dietary carbohydrate. Optimizing its structural and functional properties is essential for developing health foods. In the present study, microwave-assisted heat–moisture treatment (MHT) was applied to modify wheat starch and the effects of the physical treatments on its structure and digestibility were investigated. X-ray diffraction analysis revealed that the crystallinity of wheat starch slightly decreased after MHT. Ion chromatography revealed changes in the chain length distribution of wheat starch after modification, with a continuous increase in short-chain components over treatment time. MHT enhanced the enzymatic resistance of wheat starch, which resulted in a resistant starch content of 36.89% after 1.5 h of MHT. Excess heat disrupted the ordered structure of starch when the treatment was extended to 2 h, leading to a slight reduction in enzymatic resistance. The study provided a theoretical basis for designing functional starch ingredients through low water content physical treatment. Full article
(This article belongs to the Special Issue Novel Technologies in Food Processing)
14 pages, 1131 KB  
Article
Simultaneous Determination of Aromatic Amines in Tattoo Ink by Gas Chromatography–Electron Ionization (GC-EI)–Mass Spectrometry (MS) and Tandem MS (MS/MS)
by Eunyoung Shin, Hyebeen Kim, Jihye Choi, Minjae Kang, Juhui Shin and Sangwon Cha
Molecules 2026, 31(10), 1623; https://doi.org/10.3390/molecules31101623 - 12 May 2026
Viewed by 243
Abstract
Aromatic amines (AAs) are potent carcinogens found in tattoo inks that pose significant health risks. Precise quantitative analysis is essential for safety. In this study, we developed and validated a robust method for the simultaneous quantification of 21 regulated AAs using both gas [...] Read more.
Aromatic amines (AAs) are potent carcinogens found in tattoo inks that pose significant health risks. Precise quantitative analysis is essential for safety. In this study, we developed and validated a robust method for the simultaneous quantification of 21 regulated AAs using both gas chromatography–electron ionization (GC-EI)–mass spectrometry (MS) and tandem MS (MS/MS). After optimizing separation conditions, MS-based selected ion monitoring (SIM) and MS/MS-based multiple reaction monitoring (MRM) were evaluated. While both methods were largely sufficient to ensure compliance with international safety thresholds, the MRM-based approach exhibited superior detection capability with comparable analytical accuracy and precision, providing a more effective tool for trace-level hazardous compound analysis. The developed MRM method was applied to eight commercial tattoo inks, identifying five AAs in five products. Notably, o-toluidine, o-anisidine, and 3,3′-dichlorobenzidine significantly exceeded the regulatory limit (5.0 mg/kg), particularly in green and yellow inks. The dual-capability GC-MS platform—combining high-performance MRM quantification with robust spectral confirmation—ensures the high throughput and analytical confidence necessary for regulatory compliance and public health protection. Full article
(This article belongs to the Special Issue Chromatography—The Ultimate Analytical Tool, 3rd Edition)
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29 pages, 7188 KB  
Article
Identification of Bioactive Medium Chain Fatty Acids (C10, C8, and C6) in Ozonated Sunflower Oil: Comparative Evaluation of Their Potent Antioxidant Activities and Anti-Inflammatory Effects in the Hyperinflammatory Zebrafish Model
by Kyung-Hyun Cho, Kyoung Ah Min, Krismala Djayanti, Yunki Lee, Sang Hyuk Lee, Yassmine Benmokadem and Ashutosh Bahuguna
Antioxidants 2026, 15(5), 606; https://doi.org/10.3390/antiox15050606 (registering DOI) - 10 May 2026
Viewed by 344
Abstract
Three medium-chain fatty acids (MCFAs), namely decanoic acid, octanoic acid, and hexanoic acid, were identified in ozonated sunflower oil (OSO) using high-performance liquid chromatography (HPLC) and liquid chromatography-mass spectrometry (LC/MS). All three MCFAs exhibited strong in vitro antioxidant activity to enhance high-density lipoprotein [...] Read more.
Three medium-chain fatty acids (MCFAs), namely decanoic acid, octanoic acid, and hexanoic acid, were identified in ozonated sunflower oil (OSO) using high-performance liquid chromatography (HPLC) and liquid chromatography-mass spectrometry (LC/MS). All three MCFAs exhibited strong in vitro antioxidant activity to enhance high-density lipoprotein (HDL)-associated paraoxonase and protected low-density lipoproteins (LDL) from oxidative damage caused by Cu2+ ions. Consistently, MCFAs displayed substantial cellular antioxidant activity and minimized carboxymethyllysine (CML)-induced reactive oxygen species (ROS) generation and apoptotic cell death in zebrafish embryos. In adult zebrafish, MCFAs treatment mitigated CML-induced acute death and swimming abnormalities, and substantially augmented plasma sulfhydryl content, ferric ion reduction ability (FRA), and paraoxonase (PON)-like activity. Also, MCFA-treated zebrafish showed lower blood glucose, total cholesterol (TC) and triglycerides (TG) with raising HDL cholesterol levels. The MCFAs showed substantial inhibition of hepatic ROS generation, neutrophil efflux, interleukin (IL)-6 production, and steatosis, leading to hepatoprotection against CML-triggered adversity. Consistent with hepatic histology results, reduced plasma hepatic function biomarkers aspartate aminotransferase (AST) and alanine aminotransferase (ALT) levels were observed in MCFA-treated groups than in the CML-treated group. In the kidney, MCFA treatment effectively reduced oxidative stress and cellular senescence and protected against kidney damage induced by exposure to CML. The study concludes the presence of three MCFAs in the OSO, which serve as functional antioxidants and anti-inflammatory agents, accounting for its diverse pharmacological properties. Full article
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24 pages, 2184 KB  
Article
Preanalytical Quality Evaluation of Low-Volume Citrate Evacuated Blood Collection Tubes—Anticoagulant Solution Volume Accuracy, pH, and Anionic–Cationic Composition
by Nataša Gros and Zala Hriberšek
Molecules 2026, 31(9), 1516; https://doi.org/10.3390/molecules31091516 - 2 May 2026
Viewed by 453
Abstract
Blood collection tubes are widely used medical devices. Inaccurate citrate anticoagulant concentration can influence the results of coagulation tests. The producer’s expertise and responsibility are considered the quality safeguards. However, the tubes undergo changes during their lifecycle, partly due to storage conditions, and [...] Read more.
Blood collection tubes are widely used medical devices. Inaccurate citrate anticoagulant concentration can influence the results of coagulation tests. The producer’s expertise and responsibility are considered the quality safeguards. However, the tubes undergo changes during their lifecycle, partly due to storage conditions, and the end user or a third party has no comprehensive insight. A methodology is necessary to reveal the tube’s inherent characteristics. We provide insight into the anionic–cationic composition and pH of anticoagulant solutions in commercial tubes using high-performance ion exchange chromatography on a purified water model, making the anticoagulant volume accuracy assessment possible through a direct dye-dilution method. The results revealed differences between the tubes of two producers, Greiner BIO-ONE (A and A(nr)) and BD (C). Tube C has the most accurate anticoagulant amount. Both brands contain buffered citrate. The method of buffer preparation is not a source of interferant for the spectrometric method of the tubes’ quality evaluation. Acetate, formate, chloride, nitrite, sulfate, oxalate, bromide, and nitrate impurities were determined in anticoagulant solutions, all in tube A and some in the others. Tubes C exhibit the highest contamination with cations. Full article
(This article belongs to the Special Issue Exclusive Feature Papers in Analytical Chemistry)
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16 pages, 2359 KB  
Article
Rule-Based Ion Prediction with Orthogonal Constraints Reveals Bacterial Phospholipid Remodeling Signatures
by Wanying Hu, Wenhan Li, Meirong Song, Jianfei Zhu and Kui Zhu
Antibiotics 2026, 15(5), 459; https://doi.org/10.3390/antibiotics15050459 - 30 Apr 2026
Viewed by 265
Abstract
Background: Phospholipids are essential components of bacterial membranes and play central roles in membrane integrity and adaptation to antibiotic stress. However, confident annotation of phospholipid molecular species remains challenging due to the complexity of the lipidome and the limited structural constraints in conventional [...] Read more.
Background: Phospholipids are essential components of bacterial membranes and play central roles in membrane integrity and adaptation to antibiotic stress. However, confident annotation of phospholipid molecular species remains challenging due to the complexity of the lipidome and the limited structural constraints in conventional lipidomics workflows. Methods: Here, we present a bacterial phospholipidomic framework that integrates orthogonal structural evidence to achieve high-confidence and traceable annotation. Thin-layer chromatography (TLC) provides phospholipid headgroup assignment, gas chromatography–mass spectrometry (GC–MS) defines the acyl-chain pool, and Paternò–Büchi derivatization enables C=C localization, collectively restricting the structural search space prior to liquid chromatography–tandem mass spectrometry (LC–MS/MS) analysis. A rule-based ion prediction library further standardizes diagnostic ion assignment and reduces annotation ambiguity. Results: Applying this platform, we found Escherichia coli in the stationary phase remodeled the membrane phospholipids, with cardiolipin (CL) increasing from ~5% to ~10% and cyclopropane-containing phospholipid species rising to ~75%. Similar remodeling patterns are observed under diverse antibiotic exposures at sub-inhibitory concentrations, consistent with convergence toward a tolerance-associated membrane state. Extension of the framework to Enterococcus faecium supports proof-of-concept application in an additional Gram-positive model, with vancomycin-resistant strains exhibiting pronounced phosphatidylglycerol (PG) enrichment and reduced CL. Conclusions: Our work provides a scalable and reproducible strategy for bacterial phospholipid annotation, enabling molecular-species-resolved investigation of membrane adaptation and offering a framework for future exploration of lipid homeostasis pathways as potential antimicrobial targets. Full article
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15 pages, 1805 KB  
Article
Comparative Antioxidant Evaluation and GC-MS Identification of Bioactive Constituents in Litsea cubeba (Lour.) Pers. Fractions
by Mengyue Wei, Zihan Yu, Wenyi Fang, Yunbin Zhang and Xiaofei Zhou
Molecules 2026, 31(9), 1506; https://doi.org/10.3390/molecules31091506 - 30 Apr 2026
Viewed by 307
Abstract
In this study, five solvent fractions from Litsea cubeba (Lour.) Pers. fruit were extracted and investigated for their antioxidant profiles. Results showed that the petroleum ether fraction (PEF) and n-butanol fraction (NBF) exhibited prominent free radical scavenging capacities in DPPH, ABTS, and hydroxyl [...] Read more.
In this study, five solvent fractions from Litsea cubeba (Lour.) Pers. fruit were extracted and investigated for their antioxidant profiles. Results showed that the petroleum ether fraction (PEF) and n-butanol fraction (NBF) exhibited prominent free radical scavenging capacities in DPPH, ABTS, and hydroxyl radical assays. Gas chromatography–mass spectrometry (GC-MS) identified citral as the dominant bioactive component in both active fractions. Further mechanism analysis demonstrated that citral exerted potent antioxidant effects via dual pathways: direct free radical scavenging and transition metal ion chelation. These findings not only elucidate the material basis and molecular mechanism underlying the antioxidant activity of L. cubeba but also provide a scientific rationale for the high-value utilization of citral-rich fractions in functional foods, cosmetics, and healthcare products. Full article
(This article belongs to the Section Food Chemistry)
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18 pages, 12993 KB  
Article
Influence of 60Co Irradiation on the Volatile Organic Compounds of Cnidii Fructus
by Junmei Huang, Yuhuan Liu, Yuqing Liu, Jianye Yan, Shunxiang Li and Dan Huang
Metabolites 2026, 16(5), 309; https://doi.org/10.3390/metabo16050309 - 30 Apr 2026
Viewed by 263
Abstract
Background/Objectives: As a traditional Chinese medicinal herb, Cnidii Fructus is widely used in clinical practice. Its volatile organic compounds (VOCs) are closely related to its antipruritic effect and insecticidal properties. Due to the susceptibility of this medicinal herb to mold contamination, adopting appropriate [...] Read more.
Background/Objectives: As a traditional Chinese medicinal herb, Cnidii Fructus is widely used in clinical practice. Its volatile organic compounds (VOCs) are closely related to its antipruritic effect and insecticidal properties. Due to the susceptibility of this medicinal herb to mold contamination, adopting appropriate sterilization measures is of great significance for its storage. 60Co irradiation is widely used for this purpose due to its various advantages. Methods: This study employed Gas Chromatography–Ion Mobility Spectrometry (GC-IMS) combined with multivariate statistical analysis to systematically investigate the influence of different 60Co irradiation doses (0, 3, 6, 9 kGy) on the VOCs of Cnidii Fructus and associated metabolic regulatory mechanisms. Results: A total of 115 VOCs were tentatively identified. Statistical analysis revealed dose-dependent effects: 3 kGy irradiation caused the least compositional perturbation, best preserving original chemical characteristics; 6 kGy induced more pronounced compositional changes; and 9 kGy triggered substantial chemical composition reconstruction. Differential metabolite enrichment analysis indicated that medium and high doses of irradiation primarily perturbed central carbon metabolic pathways, including pyruvate metabolism, glycolysis/gluconeogenesis, and glyoxylate and dicarboxylate metabolism. Key differential components were tentatively identified (e.g., α-Thujone, α-Pinene, β-Pinene) that possess pharmacological activities closely associated with the traditional efficacy of Cnidii Fructus. Conclusions: When the irradiation dose is 3 kGy, the VOCs profile of Cnidii Fructus is most similar to that of the non-irradiated control group, suggesting that its compositional profile may be closer to that of traditional high-quality medicinal materials. Meanwhile, the differential metabolites and core metabolic pathways identified in this study can provide a chemical reference for the quality control of irradiated Cnidii Fructus. The findings provide a theoretical basis and technical support for the rational application of 60Co irradiation sterilization in the processing of Chinese medicinal materials and their powders. Full article
(This article belongs to the Special Issue New Technology and Workflows for Advancing Metabolomics)
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15 pages, 2090 KB  
Article
Development of a 12-Valent HPV L1 Virus-like Particle Vaccine Using an Enhanced Baculovirus Expression System
by Jae-Deog Kim, Eun-Ha Kim, Ji-Hoon Lee, Seong-Yeong Kim, Jong-Min Oh, Yerae Cho, Hyunil Kim, WonSeok Gwak, Soo-Dong Woo, Beom-Ku Han and Jae-Bang Choi
Vaccines 2026, 14(5), 398; https://doi.org/10.3390/vaccines14050398 - 29 Apr 2026
Viewed by 397
Abstract
Background/Objectives: Cervical cancer, predominantly driven by persistent infection with high-risk human papillomaviruses (HPVs), is one of the most common malignancies and an important cause of cancer-related mortality among women worldwide. Although existing licensed prophylactic HPV vaccines confer excellent protection, their global use [...] Read more.
Background/Objectives: Cervical cancer, predominantly driven by persistent infection with high-risk human papillomaviruses (HPVs), is one of the most common malignancies and an important cause of cancer-related mortality among women worldwide. Although existing licensed prophylactic HPV vaccines confer excellent protection, their global use remains suboptimal due to concentrated manufacturing capacity and high production costs. This study aimed to establish a cost-effective multivalent HPV virus-like particle (VLP) vaccine platform. Specifically, we used an enhanced baculovirus expression vector system to produce a 12-valent HPV VLP vaccine to improve antigen yield, thereby reducing manufacturing costs and ultimately improving affordability and availability in low- and middle-income countries. Methods: Optimized expression cassettes and an insect cell culture process were designed to enhance productivity across 12 HPV L1 genotypes. A scalable purification scheme integrating ion-exchange and adsorption chromatography was developed to produce high-purity VLPs with consistent structural integrity. Immunogenicity was assessed in a murine model. Elicited HPV type-specific IgG antibody responses were compared with those induced by the licensed 9-valent HPV vaccine. Results: The assembled 12-valent VLPs were comprehensively characterized using biophysical and immunochemical analyses, confirming structural stability and correct antigenicity. In vivo immunogenicity studies in mice showed strong and serotype-specific IgG responses, comparable or superior to those induced by the licensed 9-valent commercial vaccine. Conclusions: The enhanced baculovirus expression vector system is a versatile and economically sustainable platform for next-generation HPV vaccine production. This technology offers a promising approach to lowering vaccine manufacturing costs and improving global access, particularly in low- and middle-income regions heavily burdened by HPV-associated diseases. Full article
(This article belongs to the Section Human Papillomavirus Vaccines)
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13 pages, 3254 KB  
Article
Potentiometric Solid-Contact K+ Ion-Selective Electrodes Based on the KMnFe(CN)6 Transducer
by Huali Deng, Zhanhao Liu, Li Niu and Shiyu Gan
Membranes 2026, 16(5), 156; https://doi.org/10.3390/membranes16050156 - 29 Apr 2026
Viewed by 390
Abstract
Solid-contact ion-selective electrodes (SC-ISEs) are typically constructed using ion-selective membrane (ISM)-based configurations. However, such structures often suffer from water-layer formation and the weak mechanical stability of the ISM. Herein, we report an ISM-free K+-SC-ISE based on a Prussian blue analogue transducer, [...] Read more.
Solid-contact ion-selective electrodes (SC-ISEs) are typically constructed using ion-selective membrane (ISM)-based configurations. However, such structures often suffer from water-layer formation and the weak mechanical stability of the ISM. Herein, we report an ISM-free K+-SC-ISE based on a Prussian blue analogue transducer, KMnFe(CN)6, eliminating the need for a conventional ionophore-based ISM layer. KMnFe(CN)6 was synthesized via a one-step citrate-assisted co-precipitation method. The material functions as a bifunctional transducer, in which the open framework structure with ion-transport channels enables selective K+ recognition, while the redox-active Mn centers facilitate ion-to-electron transduction. The fabricated KMnFe(CN)6-based K+ sensor exhibits a near-Nernstian response with a sensitivity of 52.3 ± 1.0 mV dec−1 and a rapid response time of 25 s. The linear range and limit of detection were determined to 10−4 to 10−1 M and 5.8 × 10−5 M, respectively. The sensor also demonstrates selectivity to representative interfering ions, with log Kij of −2.39 ± 0.12 (Na+), −2.86 ± 0.09 (Li+), −3.06 ± 0.09 (Ca2+), −2.74 ± 0.12 (Mg2+) and −0.95 ± 0.08 (NH4+). By eliminating the ISM layer, the water-layer effect is effectively avoided, resulting in excellent long-term stability with a potential drift of 57.2 ± 6.1 μV h−1 over 7 days. The sensor was further applied to the analysis of K+ in real lake water samples, where the measured concentration showed good agreement with ion chromatography results. This work provides an ISM-free SC-ISE strategy for ion analysis in water environments. Full article
(This article belongs to the Section Membrane Applications for Other Areas)
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17 pages, 5302 KB  
Article
Development of an Automated Cell-Based Assay for the Detection of the Functional Activity of Saxitoxin
by Rachel Whiting, Isobel Picken, Grace Howells, A. Christopher Green, Chris Elliott and Graeme C. Clark
Toxins 2026, 18(5), 206; https://doi.org/10.3390/toxins18050206 - 29 Apr 2026
Viewed by 442
Abstract
Saxitoxin (STX) is one of the most potent natural neurotoxins known and is the only marine toxin to be declared a chemical weapon. In both marine and freshwater systems filter feeding organisms can accumulate saxitoxin and human consumption of toxin-contaminated food can result [...] Read more.
Saxitoxin (STX) is one of the most potent natural neurotoxins known and is the only marine toxin to be declared a chemical weapon. In both marine and freshwater systems filter feeding organisms can accumulate saxitoxin and human consumption of toxin-contaminated food can result in paralytic shellfish poisoning. Here we highlight for the first time a human cell-based assay for the detection and neutralisation of STX activity on an automated patch clamp (APC) system. We demonstrate that a human embryonic kidney (HEK) cell line expressing human Nav1.6 can rapidly and sensitively detect the presence of a range of sodium ion channel blockers including STX. The use of neutralising monoclonal antibody GT13-A and/or saxiphilin was found to confer specificity to the assay by being able to dissociate between STX (along with closely related analogues) and tetrodotoxin. Finally, the application of the functional assay for the detection of STX in complex samples was evaluated during an international exercise led by the Organisation for the Prohibition of Chemical Weapons (OPCW). The neutralisation of STX activity in blinded samples enabled the indirect detection of the toxin in the relevant samples and provided an alternative orthogonal technique to corroborate the findings of liquid chromatography–mass spectrometry (LC-MS). Collectively this work demonstrates the significant potential for functional assays in the analysis of samples suspected of being contaminated with STX and related sodium ion channel targeting toxins; complementing traditional direct identification methods such as high-performance liquid chromatography with fluorescence detection (HPLC-FLD), LC-MS or enzyme-linked immunosorbent assay (ELISA). Full article
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17 pages, 686 KB  
Article
Liquid Chromatography coupled with Mass Spectrometry as an Analytical Strategy to Assess the Occurrence of Potentially Toxic Cyanogenic Glycosides in Edible Microgreens
by Mariachiara Bianco, Ilario Losito, Beniamino Leoni, Onofrio Davide Palmitessa, Massimiliano Renna, Pietro Santamaria, Cosima Damiana Calvano and Tommaso R. I. Cataldi
Plants 2026, 15(9), 1358; https://doi.org/10.3390/plants15091358 - 29 Apr 2026
Viewed by 344
Abstract
Microgreens are increasingly promoted as sustainable, nutrient-dense foods, yet their content of potentially harmful specialized metabolites remains poorly explored. Here, we developed and applied a reversed-phase liquid chromatography–electrospray ionization high-resolution mass spectrometry (RPLC-ESI-HRMS) method for the detection of cyanogenic glycosides (CNGs) in edible [...] Read more.
Microgreens are increasingly promoted as sustainable, nutrient-dense foods, yet their content of potentially harmful specialized metabolites remains poorly explored. Here, we developed and applied a reversed-phase liquid chromatography–electrospray ionization high-resolution mass spectrometry (RPLC-ESI-HRMS) method for the detection of cyanogenic glycosides (CNGs) in edible microgreens. Method optimization, performed using dhurrin and lotaustralin as model standards, showed that positive ion detection of sodium adducts provided the most informative and selective HRMS/MS response, with diagnostic fragmentation patterns suitable for CNG recognition in complex matrices. Quantitative validation for lotaustralin showed excellent linearity (R2 = 0.998), low detection/quantification limits (LOD 0.16 mg/L; LOQ 0.53 mg/L), good extraction recovery, and a negligible matrix effect. Application of the method revealed a clear species-dependent profile. No detectable CNGs were found in broccoli raab and kale microgreens, supporting their safety as ready-to-eat products in this respect. In contrast, flax microgreens contained four CNGs: linamarin, lotaustralin, linustatin, and neolinustatin. Monoglycosylated species predominated, with lotaustralin quantified at 5.5 ± 0.6 mg/g dry weight and linamarin estimated at even higher levels. Diglycosylated CNGs were present at much lower concentrations and displayed multiple chromatographic peaks, consistent with the occurrence of structurally related isomeric forms. These quantitative results are specific to the flax microgreen samples analyzed here, obtained by pooling the lyophilized material obtained from several plants; thus, they do not account for biological variability among individual plants. Based on the measured CNG levels, flax microgreens showed a non-negligible cyanogenic potential. Assuming 1, 10 and 25% conversion to hydrogen cyanide, the estimated release would be, respectively, about 3, 33 and 81 mg HCN/kg of fresh flax microgreens, values lower than the current EU limit (150 mg HCN/kg of edible product) for flaxseed intended for direct consumption but comparable to values reported for other foods. These findings highlight the need to complement the nutritional evaluation of novel microgreens with targeted toxicological screening. Full article
(This article belongs to the Special Issue Microgreens—a New Trend in Plant Production)
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Article
Rapid Monitoring of Storage Deterioration in Processed Coix Seeds Using Near-Infrared Spectroscopy Guided by GC–IMS
by Jiangshan Zhang, Tongtong Wu, Xiangyang Yu, Ming Yang, Penghui Zeng, Xiaolin Xiao and Yushan Li
Foods 2026, 15(9), 1542; https://doi.org/10.3390/foods15091542 - 29 Apr 2026
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Abstract
Processed coix seeds are widely consumed as both food and traditional medicinal materials, but their quality gradually deteriorates during storage due to lipid oxidation and rancid odor formation. In this study, volatile changes during storage were characterized using gas chromatography–ion mobility spectrometry (GC–IMS), [...] Read more.
Processed coix seeds are widely consumed as both food and traditional medicinal materials, but their quality gradually deteriorates during storage due to lipid oxidation and rancid odor formation. In this study, volatile changes during storage were characterized using gas chromatography–ion mobility spectrometry (GC–IMS), and a rapid monitoring method based on near-infrared spectroscopy (NIRS) was developed. GC–IMS identified 74 volatile compounds, with aldehydes and ketones increasing significantly during storage, indicating progressive lipid oxidation. Key markers, including 2-furaldehyde, 1-pentanoic acid, and γ-caprolactone, were identified as indicators of quality deterioration. Based on these markers, composite flavor and storage deterioration indices were constructed and used as reference parameters for NIRS calibration. Partial least squares regression models developed in the 1300–2500 nm region showed strong predictive performance for these composite indices, with R2p > 0.93 and RPD > 4.0. The long-wave NIR region exhibited superior sensitivity to oxidation-related spectral changes. These results demonstrate that NIRS combined with GC–IMS analysis provides an effective, chemically interpretable approach for rapid, non-destructive monitoring of storage quality in processed coix seeds. Full article
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