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Introduction. A specialized service for antifungal blood level determination is not available in Colombia. This service is essential for the proper follow-up of antifungal therapies. Objective. To standardize and validate a simple, sensitive, and specific protocol based on high-performance liquid chromatography with a diode array detector for voriconazole blood level quantification. Materials and methods. We used an Agilent HPLC™ series-1200 equipment with a UVdiode array detector with an analytical column Eclipse XDB-C18 and pre-column Eclipse- XDB-C18 (Agilent). We used voriconazole as the primary control and posaconazole as an internal control. We performed the validation following the Food and Drug Administration (FDA) recommendations. Results. The best chromatographic conditions were: Column temperature of 25°C, UV variable wavelength detection at 256 nm for voriconazole and 261 nm for posaconazole (internal standard); 50 μl of injection volume, 0,8 ml/min volume flow, 10 minutes of run time, and mobile phase of acetonitrile:water (60:40). Finally, retention times were 3.13 for voriconazole and 5.16 minutes for posaconazole. Quantification range varied from 0.125 μg/ml to 16 μg/ml. Conclusion. The selectivity and chromatographic purity of the obtained signal, the detection limits, and the standardized quantification make this method an excellent tool for the therapeutic monitoring of patients treated with voriconazole.

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Centuries have passed without tobacco medical evaluation, and similar catastrophes have happened from the Roman Empire to now. We are not aware when, how and how much our body is exposed to chemical carcinogens every day. As a result of such exposure, millions of people fall ill with malignant diseases every year. The objectives of this work are: 1) Determination of the main urinary markers of exposure to the most dangerous chemical carcinogens; 2) Globally raising awareness about necessity of scientific testing chemicals before widespread human use; 3) Introducing the public about ubiquity of: As, Ni, Cr(VI), Cd, Be, and necessity of maximal reducing people′s exposure to them. There are well known causal relations between the most dangerous chemical carcinogens and different types of human malignant diseases. Population based studies may determine persons with high concentrations of the urinary markers/metabolites of the most dangerous chemical carcinogens. Then, such selected persons should be removed from such circumstances and/or regularly checked. Better solution is to find out the source(s) of incriminated chemical cancerogens and eliminate or mitigate their emission. These are a kind of (pre)screening (primordial prevention) for persons with high risk of developing malignant diseases causally related to the most dangerous chemical carcinogens.

Mineral oil hydrocarbons (MOH), including saturated (MOSH) and aromatic (MOAH) hydrocarbons, are contaminants of petrogenic origin. On-line high-performance liquid chromatography (HPLC) - gas chromatography (GC) - flame ionization detector (FID) was used for determining MOH in olive oils (OOs) and olive pomace oils (OPOs) at different stages of the refining process and in samples from the Italian market. Deodorization reduced contamination by about 30 %, resulting in a significant reduction of endogenous n-alkanes generally up to n-C 31 . Comprehensive GC coupled to quadrupole time-of-flight (QTOF) mass spectrometry (MS) allowed investigating the effect of bleaching on a sample of OPO naturally contaminated with alkylated PAHs, demonstrating the removal capacity of this refining step on potentially carcinogenic genotoxic compounds derived from MOH contamination. OOs from the market contained on average 33.1 mg/kg of MOSH n-C 10 - 50 and 3.3 mg/kg of MOAH, while OPOs contained on average 160.7 and 36.1 mg/kg of MOSH and MOAH, respectively., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Soybean crude oils (SCO) were detected by ultra-performance liquid chromatography-high-definition mass spectrometry (UPLC-HDMS) for discovering novel compounds. Numerous chromatographic peaks in ESI + and ESI - modes showed that SCO was rich in numerous compounds. A total of 215 potential compounds with accurate mass-to-charge ratio, MSMS spectrum and CCS value were detected in SCOs. Among them, 105 compounds (47 known and 58 novel compounds) were identified and other 110 compounds weren't identified. Compared to peanut, sesame and olive oils, 65 compounds (genistein, foeniculoside X, 5,7-Dimethoxyflavone) were only detected in SCO; the types of fatty acids (32) and flavonoids (8) were higher in SCO. SCO was rich in fatty acids, fatty acid amides, flavonoids, stigmasterol, tocopherol, and soybean phospholipids. Overall, numerous novel and unique compounds with biological functions were first found in SCOs by UPLC/HDMS. Our results suggested the higher potential nutritional value of soybean oil., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Mushrooms have long been appreciated as a delicacy as well as used as vital dietary supplements and food. However, poisoning from mushroom consumption remains a worldwide health problem, resulting in morbidity and mortality. In this paper, for the first time an untargeted lipidomics analysis on Omphalotus olearius (O. olearius) and Cantharellus albovenosus (C. albovenosus) was performed by ultra-high-performance liquid chromatography high-resolution accurate mass-mass spectrometry (UHPLC-HR-AM/MS/MS). A total of 350 lipid molecular species from 21 classes were detected in the two mushrooms. Based on multivariate and univariate analyses, 37 differential lipids were selected as metabolic markers for distinguishing the two mushrooms. And only 5 % (w/w) adulteration level was sufficient to identify C. albovenosus mixed with O. olearius. This study indicated that lipidomics approaches can provide high-resolution markers for food safety evaluation, which can be used as an accurate evaluation for distinguishing poisonous mushrooms from edible ones., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Although the health benefits of chrysanthemums have been widely studied, there is a paucity of knowledge regarding Taihang chrysanthemum (Opisthopappus taihangensis). This study compared indoor shade drying, heat drying and freeze drying on the chemical profile and health-related activities of O. taihangensis. UPLC-Q-TOF-MS and other assays were used to evaluate changes in composition and antioxidant, antibacterial and enzyme inhibitory activities. Different drying methods significantly affected compositions and bioactivities of O. taihangensis. Lipids, phenylpropanoids and polyketides were the most abundant. Freeze-drying maintained bioactive compounbds like phenylpropanoids and superior antioxidant activities. Freeze-dried O. taihangensis also displayed robust antibacterial activity against Streptococcus hemolyticus-β and effective inhiition of pancreatic lipase. These results suggest O. taihangensis is a useful source of functional compounds., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

This study demonstrates the development and application of an ultra-high-performance liquid chromatography coupled with high-resolution mass spectrometry (UHPLC-HRMS) method for the rapid and sensitive identification of intact bovine milk proteins following simulated gastrointestinal infant digestion. The new method enables the differentiation between partially hydrolysed/modified and fully intact proteins. In the raw milk, intact α-lactalbumin was visible on SDS - PAGE until the end of the gastrointestinal digestion, while it was not detected with UHPLC-HRMS. Analysis of both raw and heated milk samples revealed that the method is applicable to various milk types. Interestingly, heated milk showed additional signals in the mass spectrum, indicating non-enzymatic post-translational modifications. The relative abundance of these proteoforms could be followed along digestion. These findings highlight the versatility and sensitivity of UHPLC-HRMS in elucidating protein structures and modifications, providing valuable insights into how simulated digestion affects milk protein composition., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 The Authors. Published by Elsevier Ltd.. All rights reserved.)

Gynostemma pentaphyllum, a popular tea ingredient, can be categorized into bitter, sweet, and tasteless varieties based on flavor. However, the metabolic causes of these disparities remain unclear. In this paper, sensory evaluation, untargeted metabolomic analysis using UPLC-QTOF-MS/MS, molecular docking and e-tongue testing were conducted to reveal and verify the structural characteristics and mechanisms underlying these different flavor substances. Component analysis indicated sweet saponins were characterized by glucose chains and protopanaxadiol-type aglycones featuring diagnostic ions m/z 459/475/491 in MS 2- spectra; whereas bitter saponins typically featured at least one terminal rhamnose and the higher unsaturated sapogenins with diagnostic ions m/z 473/489/521. Virtual screening on T2R14 and e-tongue testing consistently validated gypenosides with more terminal rhamnoses or higher unsaturated aglycone tended to be more bitter. Docking analysis revealed PHE 172, TYR 159 and ALA 77 were the key amino residue sites in bitterness conduction via hydrophobic and hydrogen bonding interactions., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

A pyridine-based ionic porous organic polymer bearing hydroxyl groups (OH-iPOP) was developed for the first time by quaternization and crosslinking of 4-pyridinemethanol with 4,4'-bis(chloromethyl)biphenyl. OH-iPOP exhibited strong adsorption capacity for endocrine disruptors (EDs) including bisphenol A, bisphenol F, p-tert-butylphenol and bisphenol B (82.59-183.9 mg g -1 ), much higher than that of commercial adsorbents. The adsorption mechanism of OH-iPOP to EDs involved π-π ⁎ interaction, hydrogen bond and electrostatic interaction. Using OH-iPOP as solid phase extraction adsorbent combined with high-performance liquid chromatography, a reliable method for the sensitive detection of trace EDs in natural water and tilapia fish was established. The detection limits (S/N = 3) were 0.01-0.04 ng mL -1 and 1.00-3.80 ng g -1 for natural water and tilapia fish, respectively. The method recoveries ranged from 81.5 % to 116 %. This work not only develops an efficient adsorbent for the enrichment of EDs, but also provides a new strategy for the synthesis of novel cationic POPs., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Hop leaves, a by-product from hop cone harvesting, contain phenolic compounds of potential value for food or beverage applications. However, the abundant phenolics in hop leaves remain largely unquantified. This study quantified phenolics in hop leaves over two crop years, for three commercially significant varieties, at different developmental stages post-flowering. Ethanolic hop extracts were characterised using LC-ESI-qTOF-MS/MS and HPLC-DAD for the annotation and quantification of phenolics and bitter resins. Hop leaf phenolic profile exhibited considerable structural diversity, differing significantly from that of respective cones. Kaempferol/quercetin 3-O-glycosides and chlorogenic acids were the most abundant sub-groups with phenolic acids, procyanidins, prenylflavonoids and bitter resins also present. Phenolic profile was mainly variety-dependent with some crop year and developmental effects. Flavonol 3-O-glycosides were the main compounds driving varietal differences. Findings demonstrate the structural diversity and high concentrations of phenolic compounds in hop leaf extracts and their potential as a source of bioactives for valorisation., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024. Published by Elsevier Ltd.)

Traceability and mislabelling of black tea for their geographical origin is known as a major fraud concern of the sector. Discrimination among various geographical indications (GIs) can be challenging due to the complexity of chemical fingerprints in multi-class metabolomics analysis. In this study, 302 black tea samples from 9 main cultivation GI regions were collected. A comprehensive non-targeted fingerprinting workflow was built on liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QToF), and a comparison between conventional chemometrics modelling and machine learning was performed. 229 and 145 metabolites were selected as biomarkers and the model robustness/performance were further validated through internal 7-fold cross-validation and external validation, showing 100 % accuracy for discriminating GI origin on both. This research provided a novel solution to enhance transparency and traceability in the black tea supply chain for lab scenarios. Furthermore, the proposed biomarker selection workflow revealed more insights for future machine learning-derived non-targeted metabolomics research., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 The Authors. Published by Elsevier Ltd.. All rights reserved.)

Hemerocallis citrina Baroni (HC) is usually soaked with sodium metabisulfite solution after harvest to keep its freshness. However, this will introduce bound sulfites with potential safety risks. In this study, formation pathways of bound sulfite in HC were explored using ultra-high performance liquid chromatography-Q-Exactive HF mass spectrometry (UHPLC-QE-MS) and statistical analysis. The results indicated that the chemical composition of HC changed the most at soaking times of 6-8 h and concentrations of 1.00-2.50 mg/mL. Primary metabolites and phenols in secondary metabolites were greatly affected during soaking. 71 compounds were identified in HC and 8 characteristic markers including 3 bound sulfites were screened which can be used to distinguish between non-soaked HC (NSHC) and sodium metabisulfite-soaked HC (SSHC). Among the 19 commercial HC samples analyzed, 79 % had been treated with sulfites. Mass spectrometry data further revealed two pathways of formation of bound sulfite in HC: one is the sulfonation of amino acids at the amino, the content initially increased with sulfite soaking time and concentration and then decreased until it disappeared; the other is that the addition of aldehyde at the carbonyl, the content increased continuously with sulfite soaking concentration. This study provides insight into bound sulfite formation in HC post‑sodium metabisulfite treatment., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

This study investigates the integration of Broadband Cavity Enhanced Absorption Spectroscopy (BBCEAS) with High-Performance Liquid Chromatography (HPLC) to detect synthetic antioxidants; BHA, BHT, and TBHQ in the deep-UV region below 300 nm. The research addresses the need for more sensitive and cost-effective detection methods in HPLC systems, particularly for low analyte concentrations, by exploring BBCEAS as a superior alternative to conventional detectors that often fall short in sensitivity. The sensitivity of the HPLC-BBCEAS system is assessed by calculating the minimum detectable change in the absorption coefficient (αmin) and comparing with those obtained using conventional HPLC and single-wavelength HPLC-CRDS methods. The findings demonstrate that the HPLC-BBCEAS system achieves αmin values of 1.8 × 10 -5  cm -1 for BHA, 2.8 × 10 -5  cm -1 for BHT, and 1.9 × 10 -5  cm -1 for TBHQ at 280 nm, with Limits of Detection (LOD) and Quantification (LOQ) up to 30 times lower than conventional HPLC systems., Competing Interests: Declaration of competing interest The authors state that they have no competing financial interests or personal relationships that could have influenced the research presented in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

In this research, β-cyclodextrin magnetic-graphene-oxide pyrenyl gel composite (β-mGOP) was employed to remove trace mycotoxins from food products. The β-mGOP gels exhibited a three-dimensional macroporous structure that facilitated the rapid diffusion of target molecules into the nanoporous structure of the covalent organic frameworks embedded within the gel. The adsorption process of mycotoxins onto the β-mGOP gels conformed to the pseudo-second-order kinetics and the Freundlich adsorption model. These findings demonstrated exceptional rapid adsorption kinetics without pore collapse, making the material suitable as fillers for solid-phase extraction adsorbents. Additionally, a novel screening technique utilizing β-mGOP gels in conjunction with cyclic ion mobility mass spectrometry was developed to illustrate the efficacy of β-mGOP gels in capturing various trace substances in food and enhancing detection resolution. The versatile, uncomplicated, and scalable characteristics of β-mGOP gels indicate their promising potential for future applications in high-throughput analysis of trace contaminants in food., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

(-)-Epicatechin (EC) is a commonly dietary phytochemical that presents multi-physiological activities on human health. Thermal processing is a common method to extract EC, albeit likely to degrade EC considering its thermal instability. In this study, an 85-min non-durable bathing incubation assay was designed to simulate the state of EC in boiling water while cooking. Monitoring of degradation products was performed using ultra-performance liquid chromatography combined with electrospray ionization quadrupole tandem mass spectrometric detection (UPLC-ESI-TSQ-MS/MS). The results revealed that ca. 65.2 % loss of EC was detected in the first 10 min, and over 99.5 % of EC was degraded within 30 min. A total of 22 degradation products were identified based on retention time, full and tandem MS data were the first to be comprehensively reported. Isomerization, oxidation, hydroxylation, dimerization, and ring cleavage were the main chemical reactions that occurred for EC in boiling aqueous solution., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 The Authors. Published by Elsevier Ltd.. All rights reserved.)

Conventional consecutive separation methods based on overlapping injection modes produce interactions between samples as the separation time increases. This will lead to a reduction in the purity of the target due to the gradual saturation of the stationary phase distribution. To enhance the purity of the sample preparation and separation efficiency, we devised a consecutive separation method under high-performance counter-current chromatography (HPCCC) utilizing co-current elution and overlapping injection. The method was used for the separation and preparation of olive leaves for their main bioactive polyphenolic constituents. Six HPCCC separations were conducted in reversed-phase mode using a two-phase solvent system consisting of petroleum ether/ethyl acetate/water (1:40:40, v/v). Finally, 302.7 mg of luteolin-4'-O-β-D-glucoside and oleuropein were isolated from 720 mg of crude sample with purities of 93.3% and 96.2%, respectively. The optimization strategy outlined in this study can be used to enhance the extraction of bioactive components from olive leaves., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Provence rosé wines have gained global popularity, making them vulnerable to fraud. This study aimed to identify specific chemical markers to detect counterfeit Provence rosé wines. An untargeted LC-MS-based metabolomics analysis was performed on a set of 30 wines classified as "Provence," "Non-Provence," and "Provence imitations." Using the Molnotator workflow, 1300 potential metabolites were generated, and five key chemomarkers were selected through a machine learning pipeline. Further targeted analysis and bioinformatics using in silico MS/MS fragmentation systems confidently annotated three specific chemomarkers for "Provence" rosé: acuminoside, tetrahydroxydimethoxyflavone, and 5'-methoxycastavinol. A composite score using a PLS model combining the 3 chemomarkers effectively distinguished authentic wines, with high accuracy (sensitivity 83.3 %, specificity 100 %, accuracy 93.3 %)., Competing Interests: Declaration of competing interest The authors declare the following financial interests/personal relationships which may be considered as potential competing interests: Jean-Charles Martin reports financial support was provided by the CDR and the CIVP. Gilles Masson reports a relationship with the CDR that includes: board membership and employment. Nathalie Pouzalgues reports a relationship with the CDR that includes: employment. Aurelie Chevallier reports a relationship with the CDR that includes: employment. If there are other authors, they declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 The Authors. Published by Elsevier Ltd.. All rights reserved.)

Supercritical carbon dioxide (SCCD) has been studied for its effectiveness in preserving vegetables, but most research has focused on overall changes in the total phenolic, carotenoid and sugar contents. However, the detailed changes in individual nutrients during storage, as well as their relationship, remain largely unexplored. Herein, in this work, high-performance liquid chromatography (HPLC) was used to analyze the variations in individual carotenoids and sugars in SCCD-treated carrots and pumpkins during 21 days of storage. The results demonstrated that SCCD effectively inhibited microbial growth, and maintained the low levels of polyphenol oxidase (PPO) and peroxidase (POD) activity during storage. SCCD also deferred the degradation of carotenoid profile and phenolic compounds. Additionally, SCCD accelerated the hydrolysis of sucrose content while postponing the reduction of glucose and fructose. In summary, the SCCD technique could delay the quality deterioration of fresh-cut vegetables, preserving them with minimal quality changes., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Bioactive compounds in food offer health benefits by influencing cellular and physiological functions. Tryptophan, an essential amino acid and precursor to neurotransmitters like melatonin and serotonin, regulates mood and circadian rhythms. However, its quantification in mushrooms is scarce studied. An eco-friendly ultrasound-assisted extraction (UAE) method has been optimized to quantify tryptophan using ultra high-performance liquid chromatography with a diode array and fluorescence detector (UHPLC-DAD-Fl). Tryptophan levels were determined in 26 wild mushroom samples of the genus Lactarius and Boletus. The concentrations ranged from 0.042 mg/g to 0.742 mg/g. The extracts' health benefits were assessed for antioxidant capacity using DPPH (17.7 % - 71.6 %) and ABTS (7.2 % - 24.9 %) methods, while acetylcholinesterase (AChE) inhibitory activity ranged from 13.1 % to 49.8 %. Promising results were obtained. Hierarchical cluster analysis demonstrated a correlation between tryptophan concentration, mushroom species, location, and extract properties, highlighting tryptophan's crucial role in these mushrooms' health benefits., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024. Published by Elsevier Ltd.)

Garcinia subfalcata, an edible species endemic to China, has limited research on its chemical composition and biological effects. This study aimed to analyze metabolites in different plant parts and identify potential anticancer constituents. Using UPLC-IMS-QTOF-MS-based metabolomics, a total of 124 compounds were identified, with xanthones, flavonoids and phloroglucinols being the predominant compounds. PCA and PLS-DA analyses revealed significant metabolite differences among plant parts, identifying 28 differential metabolites, including bronianone and (±)-fukugiside. Antiproliferative assays showed varying bioactivities, with bark exhibiting the highest cytotoxicity against A549, HeLa and HGC-27 cells (IC 50 : 2.72-5.71 μg/mL). Mechanism studies indicated that the bark inhibited cell proliferation by inducing apoptosis and disrupting mitochondrial membrane potential. S-plot models revealed 23 potential anticancer constituents, including (-)-epicatechin and 1,7-dihydroxyxanthone. These findings highlight G. subfalcata's potential as a source of functional food supplements and medicinal agents and indicate the efficacy of UPLC-IMS-QTOF-MS-based metabolomics in exploring bioactive components within Garcinia., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

The aim of the study was to analyze the potential health-promoting and nutritional components of leaves and figs from several Spanish varieties of Ficus carica L. The study focused to identify (by LC-PDA-QTof/MS) and quantify (by UPLC-PDA-FL) various components including carotenoids, chlorophylls, tocols, amino acids, phenolic acids, flavonols, anthocyanins. Besides, the sugar profile, the antioxidant capacity (ORAC, FRAP and ABTS) and the in vitro hypoglycaemic potential via inhibition of α-amylase and α-glucosidase were evaluated. The leaves were found to have significant antioxidant properties. This is attributed to their high content of carotenoids (3170.77-6763.77 mg/ 100 g dm), chlorophylls (405.58-744.23 mg/ 100 g dm), tocols (59.35-115.61 mg/ 100 g dm), and polyphenols (1150.34 mg/100 g dm). Additionally, figs presented greater sources of amino acids (725.07 mg/100 g dm) and exhibited higher anti-diabetic activity than leaves. Figs of "Cuello Dama Negra" variety presented the highest content of anthocyanins (108.22 mg/100 g dm). The study suggests that incorporating these vegetal materials into another food matrix could have potential health benefits, especially in terms of antioxidant and anti-diabetic effects., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Ethnopharmacological Relevance: Yougui Pill (YGP), originating from Jingyue Quanshu, comprises 10 traditional Chinese medicines (TCMs). This classic prescription is renowned for its ability to tonify the kidney, warm the kidney, promote yang, warm the interior, and dispel cold. YGP has proven effective in treating degenerative knee arthritis, osteoporosis, delayed fracture healing, and other orthopedic conditions, making it a widely used clinical prescription for knee osteoarthritis (KOA)., Aim of the Study: Although YGP is commonly used in clinical practice, its pharmacodynamic material basis and anti-arthritis mechanisms remain unclear. This study aims to comprehensively analyze the chemical constituents of YGP and elucidate its anti-arthritis mechanisms., Materials and Methods: Ultra-high performance liquid chromatography coupled with electrospray ionization-triple quadrupole-linear ion trap mass spectrometry(ESI-Q TRAP-MS/MS) was used to identify the chemical constituents of YGP. The Hulth method was utilized to establish KOA rat model, and pathological examinations were performed to assess the anti-arthritis effects of YGP. Integrated metabolomics and transcriptomics analyses were conducted to explore the anti-arthritis mechanisms of YGP. Key targets were confirmed via immunohistochemistry., Results: A total of 1981 chemical components were identified in YGP, predominantly phenolic acids and flavonoids. Compared with the model group, 422 differentially expressed metabolites and 214 differentially expressed genes were identified, primarily involving the MAPK signaling pathway, FoxO signaling pathway, and PI3K-Akt pathway. YGP exerted an anti-osteoarthritis effect by inhibiting the excessive activation of the EGFR/ERT/FOS signaling pathway., Conclusions: TCM offers significant advantages in the treatment of KOA, addressing the shortcomings of current clinical medications. YGP displayed exceptional pharmacodynamic effects. This study elucidated its pharmacodynamic material basis and anti-osteoarthritis mechanisms, providing substantial support for its clinical application and the development of related drugs., Competing Interests: Declaration of competing interest We wish to confirm that there are no known conflicts of interest associated with this publication and there has been no significant financial support for this work that could have influenced its outcome., (Copyright © 2024 Elsevier B.V. All rights reserved.)

Ethnopharmacological Relevance: Inflammation is a biological process in response to injury, resulting in altered blood flow, increased vascular permeability, tissue destruction, and the production of reactive oxygen species (ROS) and inflammatory mediators. Zygophyllum simplex L., a medicinal plant traditionally used in the Arabian Peninsula for inflammatory disorders, has demonstrated promising in vitro anti-inflammatory activity due to its phenolic content. Additionally, the ethyl acetate fraction has exhibited notable in vivo anti-inflammatory effects., Study Objective: This research aimed to evaluate the in vivo anti-inflammatory effects of a Z. simplex plant extract and its principal ethyl acetate isolate, isorhamnetin-3-O-β-D-glucoside (Isor-3-Glu). The study seeks to develop a straightforward and robust HPLC method for quantifying Isor-3-Glu within the total methanolic extract of Z. simplex., Materials and Methods: The total methanol extract of Z. simplex was successively partitioned with a variety of organic solvents and the ethyl acetate fraction was used to isolate Isor-3-Glu on a Sephadex LH-20 column. The in vivo anti-inflammatory activity was investigated using carrageenan-triggered inflammation in rats. Histological features and immunohistochemical expression of cyclooxygenase-2 (COX-2) and tumor necrosis factor-alpha (TNF-α) were analyzed, and the levels of interleukins (IL-1β and IL-6) as well as prostaglandin E2 (PGE2) of the paw tissues were examined by qRT-PCR and ELISA, respectively. Quantification of Isor-3-Glu was achieved using an HPLC-PDA method., Results: Isor-3-Glu considerably (p < 0.05) lowered the weight of the paw edema. The histological abnormalities were improved, and the percentage of the COX-2 and TNF-α immunoreactive cells substantially decreased in the Isor-3-Glu-treated group in comparison with the positive control and Z. simplex extract group. Isor-3-Glu significantly ameliorated PGE2, IL-1β, and IL-6 levels. A straightforward and dependable HPLC technique was established for quantifying Isor-3-Glu in the total extract. The proposed methodology effectively determined Isor-3-Glu in less than 5 min. The calibration curve exhibited a linear relationship over the concentration range of 1.0-40.0 μg/mL, with a correlation coefficient (r) ≥ 0.9995. The developed method demonstrated a high level of sensitivity, with a detection limit as low as 0.139 μg/mL. The concentration of Isor-3-Glu in the total extract of Z. simplex was determined to be 0.05% w/w of dry extract., Conclusion: Isor-3-Glu could be considered a promising anti-inflammatory compound that necessitates future clinical research. Isor-3-Glu was accurately quantified using a meticulously developed and optimized HPLC-PDA technique., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

Background: The demand for sustainable energy solutions has increased interest in natural microalgal dyes as photosensitizers in dye-sensitized solar cells (DSSCs). This study addresses the critical issue of maximizing dye integrity and yield during extraction, particularly the degradation that occurs at temperatures above 60 °C. Our investigation of dye extraction from Asterarcys quadricellulare and Scenedesmus sp. using hot solvent methods revealed significant findings. High-Performance Liquid Chromatography (HPLC) analysis identified essential pigments, including Chlorophyllide a and β-carotene., Results: Our research found that temperatures above 60 °C reduce chlorophyll (Chl) stability and extraction efficiency. Using multiple wavelengths in a photodiode array (PDA) detector improves Chl identification by targeting distinct absorption peaks, resolving overlap with other compounds, and confirming purity. This approach also helps validate extraction methods and ensures accurate quantification. Since high temperatures are detrimental to Chl stability, this method is crucial for reliable analysis and longer dye storage. Ethanol outperformed methanol in extraction efficiency, while the stability of the dyes was tied to specific derivatives. Notably, Scenedesmus sp. showed better preservation of chlorophyll compounds, influenced by extraction temperature and solvent characteristics., Significance: This research underscores the potential for optimising natural dye extraction methods, offering a pathway to enhance the sustainability and cost-effectiveness of DSSC production, thus contributing to greener energy technologies., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

A random forest algorithm combined with correlation analysis, was employed to identify key taste compounds in Huangjin green tea by using an electronic tongue. A total of 45 commercial Huangjin green teas were analysed for their amino acids, catechins, gallic acid, and caffeine using an amino acid analyser and HPLC. In this study, taste compounds of 30 were quantified, and 16 of these compounds exhibited taste activity values greater than 1 in the tea samples, including 6 amino acids, 8 catechins, as well as gallic acid and caffeine. Among these compounds, 5 compounds showed relatively high importance and strong correlations (P < 0.05) with the response of electronic tongue; specific for theanine, glutamic acid, lysine, gallocatechin, and catechin. A taste reconstruction experiment further confirmed that these 5 compounds significantly contributed to the overall taste profile, particularly enhancing the umami flavour., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

The present study aim to investigate the effects of three drying processes on the flavor-related compounds and sensory quality of summer black tea. A total of 234 flavonoids and 1200 volatile compounds were identified in tea samples by using UPLC-MS/MS and HS-SPME-GC-MS, respectively. It was found that the combining hot-air and roasting drying process increased the level of epigallocatechin, epicatechin, gallic acid, theaflavins, and umami and sweet amino acids in tea samples. Conversely, the contents of epigallocatechin gallate, caffeine, kaempferol and acylated kaempferol glycosides, and quercetin and acylated quercetin glycosides were found to decrease. Analysis of the volatile compounds revealed that combined drying process enhanced the contents of volatile substances with sweet, nutty, and floral properties while reducing those with green attributes. Sensory evaluation results showed that the combined drying process improved the mellow taste and pure aroma, decreased the bitterness and astringency, and weakened the unpleasant flavor of summer black tea. Overall result indicated that the combined drying process could improve the flavor quality of summer black tea. This study may provide data support and feasible strategies for improving summer congou black tea quality., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Illegal additives such as oxyphenisatine and its esters are prevalent in the slimming food industry, necessitating a robust analytical method for their detection. This study presents a novel UPLC-MS/MS method for the rapid and accurate quantification of total oxyphenisatine levels in fermented green plum, following hydrolysis of its esters. An efficient ultrasonic extraction with a methanol and 0.1 mol/L NaOH mixture (5:5, v/v ) was optimised to hydrolyse esters to oxyphenisatine within 18 min. Chromatographic separation was conducted on a C18 column (Waters Acquity UPLC BEH, 2.1 × 100 mm, 1.7 μm) with a mobile phase of 5 mmol/L ammonium acetate and acetonitrile under gradient elution at a flow rate of 0.3 mL/min. The method demonstrated linearity ( r 2 > 0.999) over 0.1-500 µg/L, with a LOD of 10 µg/kg and LOQ of 30 µg/kg. Quantitative analysis employed positive ion multi-response monitoring and external standardisation, achieving recoveries of 92.4-97.0% and RSDs of 2.9-4.1%. Application to ten real samples gave a 90% detection rate, with measured values closely aligning with theoretical predictions (-11.3 to 13.2% relative difference) and oxyphenisatine content ranging from 159 µg/kg to 452 mg/kg. This UPLC-MS/MS method provides a reliable and efficient tool for monitoring the presence of oxyphenisatine and its derivatives in the context of food safety.

Background: Early intervention in hepatic fibrosis (HF) is critical to reducing the risk of cirrhosis-related mortality and hepatocellular cancer. However, treating fibrosis has proven to be more challenging, with no approved anti-fibrotic therapies currently available for HF. Traditional Chinese medicines (TCMs) hold significant potential for the management of HF., Purpose: This study aims to propose a systematic approach for investigating the pharmacological basis of Baoganning (BGN) Decoction, providing empirical evidence to support future research on its targets and mechanisms of BGN., Study Design: Ultrahigh-performance liquid chromatography coupled with high- resolution mass spectrometry (UPLC-HRMS) was employed to analyze the chemical composition of BGN. Key compounds were investigated using disease databases to predict relevant targets, followed by molecular docking and molecular dynamics simulations to explore molecular-level interactions. The efficacy and critical targets of BGN were validated through in vivo and in vitro experiments., Methods: UPLC-HRMS was used to identify the chemical composition of the BGN, and serum pharmacology determined the active chemical constituents in rat plasma. Zebrafish, HSC-T6 cells, JS-1 cell line and mice served as experimental models to evaluate the antifibrotic effects of BGN., Results: BGN demonstrated significant antifibrotic effect in vivo and in vitro models. A total of 757 compounds were identified in BGN, with 18 prototypical components and metabolites detected. Three compounds-quillaic acid, methyl cholate, and 3β-hydroxy-5-cholenoic exhibited dose-dependent inhibitory effects on HF. Molecular docking studies revealed stable interactions between these compounds and predicted targets. Additionally, the screened components effectively reduced the expression of ‌α-SMA and COL-I in both a cellular model and a zebrafish fibrosis model in a dose-dependent manner., Conclusion: The comprehensive analysis of BGN's chemical composition and its metabolic processes provides valuable insights into its pharmacological effects. These findings support the potential clinical and international application of BGN in treating hepatic fibrosis and improving patient outcomes., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2025 Elsevier GmbH. All rights reserved.)

The present study explored the influence of submerged fermentation with different lactic acid bacteria (LAB) as a pre-treatment of moringa leaves before the extraction of phenolic compounds via sonotrode. The sonotrode extraction was optimized using a Box-Behnken design and the optimal conditions found were: 25 % ethanol, 5 min and 100 % amplitude. Folin-reacting substances and antioxidant activity were measured on hydroalcoholic extracts obtained from fermented moringa leaves and, individual phenolic compounds were determined by HPLC-ESI-TOF-MS for the first time. The findings revealed that P. acidilactici CECT 98 and La. plantarum CECT 9567 significantly increased phenolic acids levels (30.30 % and 27.55 %, respectively) and total flavonoids increased in the presence of P. acidilactici CECT 98, Leu. mesenteroides CECT 219 T, and La. plantarum CECT 9567 (50.12, 10.68 and 10.22 %, respectively). This approach increases the yield of health-promoting phytochemicals and demonstrates the potential for optimising the extraction processes in functional food development., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Xylooligosaccharides (XOS), short-chain polymers with prebiotic properties, have gained significant commercial attention over the past few decades due to their potential as nutraceutical components. Derived from lignocellulosic biomass (LCB), XOS serve as health promoting compounds with applications across multiple sectors, including food pharmaceutical and cosmetic. This comprehensive review provides an overview of XOS production, purification, characterization, and quantification, highlighting their derivation from various sources such as agricultural waste, agro-economical forest residues, and nutrient-dense energy crops. The production of XOS involves enzymatic hydrolysis, acid hydrolysis, and steam explosion, each offering distinct advantages and limitations in terms of cost-effectiveness and scalability for industrial applications. Methods for purification including chromatographic techniques, membrane filtration, capillary electrophoresis (CE) and enzyme-linked immunosorbent assay (ELISA) are evaluated based on their efficiency and feasibility. Characterization techniques such as nuclear magnetic resonance (NMR) spectroscopy, high-performance liquid chromatography (HPLC), and mass spectrometry (MS) provide detailed insight into XOS structure and composition. Conclusively, XOS are promising biological macromolecules with significant industrial and scientific interest due to their diverse applications and potential for cos-effective large-scale production., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 The Author(s). Published by Elsevier Ltd.. All rights reserved.)

Tea is a widely consumed beverage worldwide due to its rich secondary metabolites. Gallotanin: 1-O-galloyl-6-O-luteoyl-α-D-glucose (GLAG) has strong antioxidant activity and good resistance to a wide range of bacteria and malaria. Despite its potential, there have been few reports on GLAG in plants. In this study, we identified and validated the presence of GLAG in tea plants using UPLC-qTOF MS/MS and ESI-MS. We also identified a GLAG-rich tea variety, 'ZM2807', for the first time and observed significant variations in GLAG content across seasons and leaf positions. In addition, our analysis explored the variations and correlations of GLAG, catechin, and caffeine contents in a hybrid population (LJ43 × BHZ) consisting of 327 F 1 individuals over three consecutive years. These results provided new insights into the potential applications of GLAG in food and medicine and offered a valuable reference for studying the dynamics of GLAG, catechin, and caffeine contents in adult tea plants., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Perchlorate was reported to be taken up by tea (Camellia sinensis L.) plants and mainly stored in leaves. However, the change of contents in perchlorate in fresh tea leaf-made tea and tea infusion remains unclear. Here, we revealed the transfer of perchlorate during green/black tea processing and brewing using UPLC-MS/MS and established a corresponding dietary risk assessment method. The processing factors based on the dry-weight contents of perchlorate during green and black tea processing were in the range of 0.96-1.17. The content of perchlorate was stable throughout tea processing. Perchlorate in made tea was prone to leaching into infusions with an average leaching rate of 74.1 ± 12.6 %. Moreover, risk assessment was developed based on the above processing factor, leaching rate and risk quotient (RQ) method, which contributes to estimating the impact of perchlorate in fresh tea leaves on human dietary exposure via tea drinking., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024. Published by Elsevier Ltd.)

Two novel phosphodiesterase 5 (PDE-5) inhibitors were detected in pressed candy using high-performance liquid chromatography (HPLC)-diode array detection. Following extraction with acetonitrile and sonication, the compounds were isolated and purified via semi-preparative liquid chromatography. Structural characterisation was achieved through high-resolution mass spectrometry (HRMS) and nuclear magnetic resonance (NMR) spectroscopy. The results indicate that both compounds possess identical UV absorption spectra. The molecular formulas of compounds 1 and 2 are C 23 H 32 N 4 O 4 and C 22 H 30 N 4 O 4 , respectively, each featuring a pyrimidinone benzene structure with a single methylene group (-CH 2 ) variation. As studies on these illicit compounds in functional foods have not been conducted, regulatory agencies must take note and incorporate them for the assessment of illicit additives in functional and healthcare foods.

Mycotoxins are secondary metabolites of fungi and represent a serious problem for human health. Due to growing interest, various aspects have been widely studied by scientific groups. One of these aspects relates to the food industry and associated beer production. Mycotoxins can be present in the basic raw materials for beer production as well as in brewed beer. Problematic mycotoxins that pose a serious risk of toxicity are aflatoxins especially aflatoxin B 1 (AFB 1 ), fumonisins (FBs), and zearalenone (ZEN) and its metabolites, deoxynivalenol (DON) including its acetylated forms and also the modified form deoxynivalenol-3-glucoside (DON-3G), T-2 toxin, HT-2 toxin, and ochratoxin A. The Research Institute of Brewing and Malting has been dealing with the issue of mycotoxins since 2008. This study describes the analysis of the above mycotoxins during 2020-2024 in barley (n = 775), malt (n = 751), and commercially available beers (n = 522) using QuEChERS, immunoaffinity columns, and UPLC-MS/MS. The results showed positive samples of mycotoxins in brewing and malting matrices at the level of micrograms per kilogram (barley, malt) and nanograms per liter for beer. Therefore, it is a residual concentration and the accurate quantitative determination of mycotoxins, correct interpretation of the results in connection with toxicological values, and the maximum permissible levels of mycotoxins play a key role in global food safety and consumer protection., Competing Interests: Declarations. Competing interests: The authors declare no competing interests., (© 2024. The Author(s) under exclusive licence to Society for Mycotoxin (Research Gesellschaft für Mykotoxinforschung e.V.) and Springer-Verlag GmbH Germany, part of Springer Nature.)

Characterizing co-formulated monoclonal antibodies (mAbs) poses significant challenges in the pharmaceutical industry. Due to the high structural similarity of the mAbs, traditional analytical methods, compounded by the lengthy method development process, hinder product development and manufacturing efficiency. There is increasing critical need in the pharmaceutical industry to streamline analytical approaches, minimizing time and resources, ensuring a rapid clinical entry and cost-effective manufacturing. This study investigates the application of process analytical technologies (PAT) to address such challenges. Our investigation introduces two complementary technologies, on-line ultra-performance liquid chromatography (online UPLC) and multimode fluorescence spectroscopy (MMFS), as potential PAT tools tailored for characterizing critical quality attributes (CQA) in co-formulated mAb products. Specifically, the CQAs under evaluation include the total protein concentration of the mAbs within the co-formulation and the ratio of mAb A to mAb B. Online UPLC enables direct and automated measurement of the CQAs through physical separation, while MMFS determines them in a non-destructive and more swift manner based on chemometric modeling. We demonstrate these technologies' comparable performance to conventional methods, alongside substantial benefits such as reduced analytical turnaround time and decreased laboratory efforts. Ultimately, integrating them as innovative PAT tools expedites the delivery of therapeutic solutions to patients and enhances manufacturing efficiency, aligning with the imperative for swift translation of scientific discoveries into clinical benefits., (© 2024 Wiley Periodicals LLC.)

Herein, a new, environmentally friendly, and economical magnetic solid-phase extraction method for fluoroquinolones (FQs) from milk samples was developed using novel recyclable zeolitic imidazolate framework functionalized magnetic multiwalled carbon nanotubes (Fe 3 O 4 @MWCNTs@SiO 2 @ZIF-8) as adsorbents. Various characterization techniques, including scanning electron microscopy, N 2 adsorption-desorption analysis, and vibrating sample magnetometry, demonstrated that the adsorbent possessed a remarkable specific surface area, pore volume, and superparamagnetic properties, rendering it an excellent adsorbent. Combined with high-performance liquid chromatography, this method exhibited excellent linearity (R 2  ≥ 0.9991) over the concentration range of 0.5-500 μg L -1 , low limits of detection (0.10-0.34 μg kg -1 ), and low limits of quantification (0.30-1.00 μg kg -1 ). Finally, the developed method was successfully applied to analyze FQs in milk samples with recoveries ranging from 83.3% to 107.7% and relative standard deviations below 4.2%. The high efficiency and sensitivity of this method highlight the potential application of Fe 3 O 4 @MWCNTs@SiO 2 @ZIF-8 for analyzing FQs in complex matrices., Competing Interests: Declaration of competing interest The authors declare that there are no conflicts of interest., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

In this study, the magnetic biochar material derived from coconut clothing was firstly successfully synthesized by in-situ polymerization method and applied as QuEChERS adsorbents for extracting multi-pesticides. The obtained magnetic coconut-clothing biochar (MCCBC) presented alveolate structure with abundant large irregular pores. The Fe 3 O 4 particles was obviously attached on the surface of biochar. Under the optimized conditions, the modified QuEChERS process based on MCCBC coupled with HPLC-MS/MS for simultaneously extracting and determining 12 pesticides (organophosphorus insecticides and strobilurins) from different agricultural products (tomato, cucumber, cabbage, carrot, peach, pear, grape, apple) was established. After pretreated by MCCBC, most of pesticides had weak matrix effect. This proposed method showed good linearity (2-250 ng g -1 ) with R 2  ≥ 0.9915, and the limits of detection and the limits of quantification were in the range of 0.01-2.67 ng g -1 and 0.03-8.91 ng g -1 , respectively. The acceptable recovery was between 71.1 % and 114.0 % with relative standard deviations from 0.31 % to 13.94 %. These results fully demonstrated that the developed method was efficient for simultaneously extracting and determining organophosphorus insecticides and strobilurins in complex agricultural matrix, possessing obvious advantages of higher sensitivity, easier operation and good feasibility. More importantly, this study provided a useful strategy for magnetizing biochar, and the novel biochar from coconut clothing was also introduced as potential adsorbent for other trace organic pollutants., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

The effective differentiation and detection of multiple tea polyphenols are often challenging due to their subtle structural similarities. Although post-column derivatization HPLC strategies are commonly employed to distinguish multiple targets, the short physical distance between chromatographic column and detector limits reaction time, thereby reducing the derivatization efficiency. Dopamine (DA) reacts rapidly with resorcinol to form fluorescent azamonardine products, making fast fluorometric derivatization of tea polyphenols containing resorcinol motifs possible. In this study, a DA-driven rapid and post-column fluorescence derivatization method has been applied to sensitively detect eight tea polyphenols. This method is based on fluorescence derivatization and possesses low background interference, high sensitivity, and excellent reproducibility. Moreover, the practical application of this proposed fluorometric derivatization platform was further validated by simultaneous identification of multiple tea polyphenols in different tea samples. This work has great potential to become an alternative to the National Standard method for tea polyphenols determination., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

The physicochemical characterization of fresh, undiluted, cold-pressed oil from elderberry seeds (EO) is presented. The results showed EO's uniqueness for the 93 % presence of essential fatty acids, including linoleic n-6 (41 %), α-linolenic n-3 (38 %), and oleic n-9 (13 %) acids with favorable ratios for human nutrition, n-3/n-6 = 0.93. A γ-tocopherol is the dominant tocopherol (96 %), with a concentration of 20.62 mg/100 g, indicating low oil oxidative stability. DSC heating and cooling traces determined the thermal properties. These results also revealed the presence of metastable triacylglycerol (TAG) structures composed of polyunsaturated fatty acids. The presence of characteristic groups for fatty acids and TAGs in EO was confirmed by FTIR-ATR spectra. For the first time, Langmuir monolayer studies on EO revealed its low compressibility, indicating its low emulsifiability, and the presence of minor components of EO, including tocopherols, phenolic acids, polyphenols, flavonoids, and carotenoids, was determined using UV-Vis absorption and fluorescence excitation-emission matrix (EEM) along with the chemometric method., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interest or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

The quality evaluation of Dioscorea opposite Thunb. mainly focuses on determining water-soluble contents. Polysaccharides are now recognized as the significant constituents of yam with activities such as immune enhancement, and it is necessary to use polysaccharides as an indicator for quality control of yam in this study. Sixty batches of yam polysaccharides were obtained by conventional hot water extraction and analysis for their physicochemical properties and structure. The results showed the functional groups (four shared peaks including 3500-3300 cm -1 ) and molecular weights (2.06 × 10 3  Da-2.28 × 10 3  Da). The PMP-HPLC fingerprints calibrated 5 familiar peaks, and the relative retention times of each characteristic peak to the Glc peak (S peak) were 0.47 (Man), 0.86 (GalA), 1.00 (Glc), 1.13 (Gal), 1.24 (Ara), Glc and Gal, which were the main differentiated monosaccharide components in the HPLC fingerprinting of YPs. This study provided a preliminary data reference for quality control of YPs., Competing Interests: Declaration of competing interest I would like to declare on behalf of my co-authors that the work has not been published previously, and is not under consideration for publication elsewhere, in whole or in part. No conflict of interest exists in the submission of this manuscript and the manuscript is approved by all authors for publication., (Copyright © 2024. Published by Elsevier Ltd.)

Non-enzymatic browning (NEB) reduced the colour quality of hot-air dried peppers, but the specific mechanism remains unclear. This may be related to the degradation of chlorophyll, ascorbic acid, and polyphenols. The findings revealed that the surface of pepper gradually browned during hot-air drying, with the ΔE ⁎ value and browning degree (BD) significantly increasing by 119.4 % and 62.9 %, respectively. However, the total phenol content (TPC) and ascorbic acid content decreased by 74.2 % and 84.3 %, respectively. TPC was negatively correlated with BD (R = -0.86), and its value (31.7 %) was 300 times higher than that of other colour-related components (ascorbic acid, chlorophyll). UPLC-MS/MS analysis further identified 345 polyphenols, among which 1, 3-dicaffeoylquinic acid and 5,7-dihydroxy-3', 4', 5'-trimethoxyflavone were the two key monophenols influencing NEB (R = -0.87). The results suggested that NEB pathways involve chlorophyll and ascorbic acid degradation, the Maillard reaction, and polyphenol degradation, with the latter playing a major role., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Simplified and effective pretreatment methods combined with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) for the determination of four aminoglycoside antibiotic pesticides kasugamycin, validamycin, streptomycin sulfate and zhongshengmycin in high starchy content matrix (rice), high water and high acidic content matrix (citrus) and high water content matrix (melon) were established. Single-factor and central composite design (CCD) experiments were employed to optimize the pretreatment conditions, resulting in the optimal factor combinations and achieving scientifically accurate outcomes. Validation results proved satisfactory, with all four target compounds exhibiting correlation coefficients (r) exceeding 0.99 within the linear range in three matrices. The recoveries were 81.5-102.2 %, and both inter-day and intra-day relative standard deviations (RSDs) were below 10.7 %. The limits of detection (LODs) were 0.1-4.0 μg/kg, with limits of quantitation (LOQs) consistently at 50 μg/kg. Furthermore, the methods were applied to potato, grape, and cucumber matrices to further validate their applicability., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024. Published by Elsevier Ltd.)

The levels of 37 pesticides in dandelion were analyzed using gas chromatography-tandem mass spectrometry (GC-MS/MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The dandelion samples were treated with different irradiation doses, pH levels, moisture contents, and initial concentrations. Additionally, the respective contents of chicoric, chlorogenic, and caffeic acids in the dandelion samples were determined using high-performance liquid chromatography (HPLC) with DAD detector. The results showed that the pesticide degradation rate was positively correlated with the irradiation dose and negatively correlated with pesticide concentration. The degradation of most pesticides followed first-order kinetics. The pesticide degradation rate initially decreased and subsequently increased with an increase in the pH. Irradiation below 8 kGy had an insignificant effect on the three active ingredients of dandelion. The chicoric acid content decreased with an increase in water content and pH, whereas the caffeic acid content increased., Competing Interests: Declaration of competing interest The authors declare that they have no competing financial interests or personal relationships that may have influenced the work reported in this study., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

In this study, novel triple-template magnetic nanospheres by surface imprinting, called triple-template magnetic molecularly imprinted polymers (tri-MMIPs), were prepared for the detection of steroid hormones in human serum. The polymers were constructed by Fe 3 O 4 as support, estrone (E1), progesterone (PROG), and estradiol (E2) as triple templates, acrylic acid (AA) as functional monomer and ethylene glycol dimethacrylate (EGDMA) as cross-linker. The resulting tri-MMIPs were further characterized and applied as sorbents in human serum pretreatment. Coupled with ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry (UHPLC-MS/MS) profiling after derivatization, 15 steroids (E1, 6-ketoE1, 4-OHE1, 16α-OHE1, DHEA, 4-MeOE1, PROG, PREG, 17-OHPROG, 7-DHE2, E2, 2-OHE2, 16-epiE3, E3, 2-MeOE2) were successfully quantified. The developed method exhibited a good recovery (78.9-114%) and low limit of quantitation (LLOQ, 5-10 pg/mL), which indicates a great potential for application in the analysis of multiple steroid hormones in complex biological samples., Competing Interests: Declarations. Conflict of interest: The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (© 2024. The Author(s), under exclusive licence to The Japan Society for Analytical Chemistry.)

4-Hydroxy-2-nonenal (HNE), a reactive compound produced during the peroxidation of polyunsaturated fatty acids, is implicated in numerous diseases and the degradation of food quality. Although the detection of HNE in meat has a long history, methods for detecting HNE in freshwater fish are inadequate due to the significant influence of matrix differences (i.e., the matrix effect). We developed a method to measure HNE in six freshwater fish species: Grass carp, Silver carp, Bighead carp, Common carp, Crucian carp, and Wuchang bream. This method showed excellent linearity (R 2 values from 0.9943 to 0.9958) and high recovery rates (95.45-104.41 %), with limits of detection (LOD) between 0.029 and 0.176 μmol/kg, covering a range of 0.006 to 25.600 μmol/kg. Matrix effect assessment revealed matrix factors (Mf) between 0.13 and 0.47. This study enhances our understanding of lipid oxidation in fish and guides improvements in food processing techniques., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Elucidating the combined exposure of agrochemicals is essential for safeguarding human health and agroecosystem safety. A rapid and high-sensitivity UHPLC-MS/MS method was developed for simultaneous quantification of nine compounds in sorghum by an assembly-line optimization process with a limit of quantitation of 0.001 mg/kg. The concentration variation of atrazine, quinclorac, fluroxypyr-meptyl and metabolites was reflected by terminal magnitudes of ≤0.0665 mg/kg. Additionally, atrazine was dealkylated to deethyl atrazine and desethyl desisopropyl atrazine at concentrations of 0.0014-0.0058 mg/kg during the sorghum harvest. Acceptable health hazardous of atrazine and quinclorac for all life cycle populations were comparatively assessed via deterministic and probabilistic models, in which atrazine gained an 83.55 % share of cumulative dietary risks. Rural residents had significantly higher risks than urban residents, and children were the most sensitive group. Despite the low health risks, combined exposure to herbicides and their metabolites should be continuously stressed, given their cumulative amplification effects., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024. Published by Elsevier Ltd.)

The silymarin complex extracted from milk thistle provides significant health benefits, particularly due to its antioxidant and hepatoprotective properties. However, plant substances can be contaminated by a number of fungi types and their secondary metabolites-mycotoxins. This work deals with the determination of aflatoxins and zearalenone and its metabolites in 39 different samples grown in 2020 and 2021. Analysis of mycotoxins was performed by UHPLC-MS/MS after immunoaffinity column AFLAPREP ® and EASI-EXTRACT ® ZEARALENONE clean-up. The presence of aflatoxins was not confirmed in the monitored samples, but 1/3 of the samples were contaminated with zearalenone in the range of 2.8-378.9 µg/kg. Metabolites of zearalenone such as α-zearalenol, α-zearalanol, and β-zearalanol were not detected in any of the samples. β-Zearalenol was found in two samples (2.6 µg/kg and 29.8 µg/kg)., Competing Interests: Declarations. Competing Interests: The authors declare no competing interests., (© 2024. The Author(s) under exclusive licence to Society for Mycotoxin (Research Gesellschaft für Mykotoxinforschung e.V.) and Springer-Verlag GmbH Germany, part of Springer Nature.)

An efficient, sensitive, and precise method for investigating the metabolism of four sulfonamides in grass carp has been established using high-performance liquid chromatography-mass spectrometry. By optimizing the experimental conditions, the method achieved a coefficient of determination above 0.999, with detection and quantification limits set at 0.5 μg/kg and 1.0 μg/kg, respectively. Recovery rates were between 92.90 % and 102.84 %, and relative standard deviations ranged from 1.70 % to 9.83 %, enabling the precise detection of these sulfonamides in grass carp tissue. The factors affecting the metabolic rate during the medicated bath process were investigated, and obtained the optimal parameter conditions for screening the candidate materials. The candidate materials screened through this method exhibit good stability when used to prepare matrix standard substances, this work not only provides a scientific basis for screening sulfonamide candidate materials but also offers insights for developing other matrix reference materials., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Environmental phenols are a group of typical endocrine disruptors, and widely detectable in human breast milk and infant formulas. However, exposures data are scarce in early infancy, a particularly sensitive period to environmental pollutants exposures. We aimed to prospectively assess urinary concentrations of eighteen environmental phenols in infants from birth to 6 months of age and their associations with feeding patterns (breastfeeding, formula and mixed-feeding). This study included 197 mother-infant pairs. Urinary concentrations of six parabens (PBs), seven bisphenols, four benzophenones (BPs) and triclosan were measured in infants at the ages of 3 days, 42 days, 3 and 6 months by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Multivariable linear regression models were applied to evaluate the associations between infant feeding types and urinary phenol concentrations in log 10 -transformed scale. The detection rates of bisphenol A and S, methyl 4-hydroxybenzoate (MeP), ethyl 4-hydroxybenzoate (EtP), and propyl 4-hydroxybenzoate (PrP) were persistently high (ranged 48.7%-100.0%) across all ages (3 days, 42 days, 3 and 6 months). The detection rates of bisphenol P, B and AP were high (ranged 76.9%-95.9%) at age 3 days, and lower (14.4%-88.0%) at later ages. Compared to exclusive breastfeeding, mixed feeding was associated with 0.32 (95% CI: 0.01, 0.62, p < 0.05) higher log (BPA) (μg/g creatinine) at 42 days, 0.69 (0.03, 1.35) higher log (TCS) (μg/g creatinine) at 3 months, 0.54 (0.08, 1.00) higher log (EtP) (μg/g creatinine) at 6 months; formula feeding was associated with 1.30 (0.59, 2.00) and 0.91 (0.22, 1.60) higher log (BPB) (μg/g creatinine) at the age of 42 days and 3 months respectively, 1.19 (0.003-2.37) higher log (BPP) and 0.95 (0.27-1.64) higher log (BPS) (μg/g creatinine) at 3 months. In conclusion, exposures to BPA and its analogs, and parabens (MeP, EtP, and PrP) were extensive in early postnatal life of infants. Breastfeeding might be a safer form of feeding for infants against exposure to some phenols., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)