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Diatoms are single-celled photosynthetic eukaryotes responsible for CO2 fixation and primary production in aquatic ecosystems. The cosmopolitan marine diatom Coscinodiscus granii can form seasonal blooms in coastal areas and interact with various microorganisms, including the parasitic oomycete Lagenisma coscinodisci. This unicellular eukaryote is mainly present in the northern hemisphere as an obligate parasite of the genus Coscinodiscus. Understanding the interplay of abiotic factors such as temperature and biotic factors like parasitism on algal physiology is crucial as it dictates plankton community composition and is especially relevant during environmental changes and warming events. This study investigates the impact of two temperatures, 13 °C and 25 °C, on Coscinodiscus granii under laboratory conditions. A decreased infection rate of the parasite was observed at the elevated temperature. Comparative metabolomic analysis using UHPLC-HRMS revealed that temperature and parasitism significantly affect the algal cell metabolome. Abundances of metabolites related to sulfur metabolism, including cysteinoleic acid and dimethylsulfoniopropionate, as well as molecules linked to fatty acid metabolism, e.g., carnitine, acetylcarnitine, and eicosapentanoic acid, significantly increase in cells grown at a higher temperature, suggesting the enhanced rate of metabolism of host cells as the temperature rises. Our study reveals how temperature-induced metabolic changes can influence host–parasite dynamics in a changing environment. [ABSTRACT FROM AUTHOR]

Hospital pharmacy compoundings are crucial for maintaining patient care. They are time- and cost-effective in hospital pharmacy settings because they prevent waste, preparation errors, dosage errors, microbial contamination and breakage due to handling. Unfortunately, the drawbacks of hospital pharmacy compounding include the selection of inappropriate medical devices (MDs) for long-term storage, which could directly impact patients. In this study, three important hospital pharmaceutical compoundings, vancomycin in prefilled syringes (PFSs) made of polypropylene (PP) material, paediatric parenteral nutrition (PN) in ethylene vinyl acetate (EVA) bags and diluted insulin in cyclic olefin copolymer (COC) vials, were selected for leachate study and risk assessment. These compounds were studied via a semiquantitative screening approach by means of an ultrahigh-performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-HRMS) with postcolumn infusion and an in-house built database. 17 leachable compounds for the PFS, 25 for the PN, and 10 for the vial were identified, and their concentrations were estimated for toxicological assessments. In conclusion, all MDs used in hospital pharmacy compoundings were observed suitable thanks to risk assessments. However, suitable MDs recommended for long-term storage would remain with polymers like COC, for higher safety when exposed to frail and vulnerable patients like neonates and infants. [ABSTRACT FROM AUTHOR]

Summary: The blue crab is one of the most invasive alien species in the Mediterranean Sea. Its remarkable surge in availability suggests an imminent increase in consumption. However, blue crabs are vulnerable to contamination by per‐ and polyfluoroalkyl substances (PFAS), known to accumulate in the food chain and pose health risks to humans. Data on PFAS contamination levels in blue crabs are a few. This study investigates 26 PFAS in 113 blue crabs by UHPLC‐HRMS. Results revealed higher concentrations in cephalothorax than in claws. PFHpA, PFHxS, PFOA, PFNA, PFOS, PFUnDA, PFDoDA, PFTrDA, PFHpS, and PFBA were among the most detected PFAS. Total PFAS mean concentration ranged from 0.65 to 2.61 ng g−1 ww. Three crabs exceeded maximum residue limits for PFOA, PFNA, and PFHxS. Statistical analyses suggested a correlation between contaminants presence and crab size. PCA highlighted the weight as a potential predictor of PFOS concentration. PFAS intake evaluation showed no risk for consumers. [ABSTRACT FROM AUTHOR]

Polyphenols are responsible for wine colour and astringency, and, as antioxidants, they also have beneficial health properties. In this work, we developed a robust full-scan high-resolution mass spectrometry method for the quantification of 90 phenolic compounds in wine samples (either red, rosé, or white wine), using a UHPLC-OrbitrapTM system. With this method, we could conduct a detailed analysis of phenolic compounds in red, rosé, and white wines with great selectivity due to sub-ppm mass accuracy. Moreover, accessing the full-scan spectrum enabled us to monitor all the other compounds detected in the sample, facilitating the adaptability of this method to new phenolic compounds if needed. [ABSTRACT FROM AUTHOR]

Abstract In recent years, the exploration of the therapeutic potential of Salvia has gained considerable attention, leading to a growing number of scientific studies emphasizing its pharmacological properties. Despite this, therapeutic applications of Salvia remain underexploited, requiring further investigation. Iran is a major center for sage diversity in Asia, boasting 60 Salvia species, 17 of which are unique to the area. This study aimed to comprehensively explore and compare the extracts of 102 Salvia samples belonging to 20 distinct Salvia species from Iran, providing a deeper understanding of their specific polyphenol content and, consequently, their antioxidant capabilities and potential therapeutic uses. All samples were analyzed to determine the contents of total phenolics, total flavonoids, total tannin, photosynthetic pigments, and ascorbic acid, along with their antioxidant activity. These data were then combined with the forty distinct chemical fingerprints identified by ultrafast high-pressure liquid chromatography coupled with high-resolution mass spectrometry. Multivariate data analysis was employed to find correlations and differences among the huge number of data obtained and to identify Salvia species with similar phytochemical and/or antioxidant properties. The results show that each Salvia species is characterized by a distinct class of polyphenols recognized for their antidiabetic, anti-inflammatory, cardioprotective and neuroprotective properties. Overall, our findings reveal the potential of some Salvia species for targeted therapeutic applications and provide a rational basis for the development of Salvia-derived nutraceuticals, ultimately improving the prospects for the use of Salvia in medicine.

Marine-derived fungi are assuming an increasingly central role in the search for natural leading compounds with unique chemical structures and diverse pharmacological properties. However, some gene clusters are not expressed under laboratory conditions. In this study, we have found that a marine-derived fungus Aspergillus sp. SYPUF29 would survive well by adding an exogenous nitric oxide donor (sodium nitroprusside, SNP) and nitric oxide synthetase inhibitor (L-NG-nitroarginine methyl ester, L-NAME) in culture conditions. Moreover, using the LC-MS/MS, we initially assessed and characterized the difference in metabolites of Aspergillus sp. SYPUF29 with or without an additional source of nitrogen. We have found that the metabolic pathway of Arginine and proline metabolism pathways was highly enriched, which was conducive to the accumulation of alkaloids and nitrogen-containing compounds after adding an additional source of nitrogen in the cultivated condition. Additionally, the in vitro anti-neuroinflammatory study showed that the extracts after SNP and L-NAME were administrated can potently inhibit LPS-induced NO-releasing of BV2 cells with lower IC50 value than without nitric oxide. Further Western blotting assays have demonstrated that the mechanism of these extracts was associated with the TLR4 signaling pathway. Additionally, the chemical investigation was conducted and led to nine compounds (SF1–SF9) from AS1; and six of them belonged to alkaloids and nitrogen-containing compounds (SF1–SF6), of which SF1, SF2, and SF8 exhibited stronger activities than the positive control, and showed potential to develop the inhibitors of neuroinflammation. [ABSTRACT FROM AUTHOR]

In recent years, the exploration of the therapeutic potential of Salvia has gained considerable attention, leading to a growing number of scientific studies emphasizing its pharmacological properties. Despite this, therapeutic applications of Salvia remain underexploited, requiring further investigation. Iran is a major center for sage diversity in Asia, boasting 60 Salvia species, 17 of which are unique to the area. This study aimed to comprehensively explore and compare the extracts of 102 Salvia samples belonging to 20 distinct Salvia species from Iran, providing a deeper understanding of their specific polyphenol content and, consequently, their antioxidant capabilities and potential therapeutic uses. All samples were analyzed to determine the contents of total phenolics, total flavonoids, total tannin, photosynthetic pigments, and ascorbic acid, along with their antioxidant activity. These data were then combined with the forty distinct chemical fingerprints identified by ultrafast high-pressure liquid chromatography coupled with high-resolution mass spectrometry. Multivariate data analysis was employed to find correlations and differences among the huge number of data obtained and to identify Salvia species with similar phytochemical and/or antioxidant properties. The results show that each Salvia species is characterized by a distinct class of polyphenols recognized for their antidiabetic, anti-inflammatory, cardioprotective and neuroprotective properties. Overall, our findings reveal the potential of some Salvia species for targeted therapeutic applications and provide a rational basis for the development of Salvia-derived nutraceuticals, ultimately improving the prospects for the use of Salvia in medicine. [ABSTRACT FROM AUTHOR]

Annatto, obtained from the seeds of achiote (Bixa orellana L.), is a widely used orange pigment rich in bixin and other apocarotenoids. This work reports the optimisation of a green extraction method of pigments and antioxidant compounds from achiote as well as its integration in a one-step green extraction-cosmetic formulation process. A biphasic solvent system of water and oil was used to recover simultaneously polar polyphenols, and less polar compounds, such as δ-tocotrienol and bixin. The optimisation of the ultrasound assisted extraction is presented, as well as a comparison of different vegetable oils used as extraction solvents. The composition, physicochemical properties and antioxidant activity of the oils were studied and their extraction performance was compared. Refined sunflower oil proved to be a better solvent than virgin olive, jojoba, coconut and grapeseed oils. Both aqueous and oil phases displayed an interesting antioxidant capacity. The oil phase contained 0.9% of bixin, as well as minor apocarotenoids and δ-tocotrienol. Twelve compounds, mainly phenolics, were identified by UHPLC-DAD-HRMS/MS in the aqueous phase. Twenty-one volatile compounds were identified in the volatile fraction by SPME-GC-MS. Lastly, a one-step green process is proposed to combine the extraction and the cosmetic formulation of the bioactive compounds. [ABSTRACT FROM AUTHOR]

Following recent successful results in the search for innovative semi-synthetic cosmeceutical Se-glycoconjugates, the work reported herein explores the development and evaluation of second-generation selenosugar-linked hydroxycinnamic acids as new potential cosmeceutical ingredients. Utilizing a Pummerer-like rearrangement for C1-acetylation, these novel compounds were synthesized and characterized using NMR spectroscopy and HRMS, confirming their structures and purity. The biological evaluation focused on their radical scavenging preliminary screening, and cytotoxic and antioxidant activities in human immortalized keratinocytes, revealing significant potential for use in skin care formulations aimed at counteracting oxidative stress and promoting skin health. Cellular uptake studies conducted on HaCaT keratinocytes using UHPLC-QqTOF-MS metabolomics demonstrated effective internalization of these compounds, which is crucial for their efficacy as topical agents. Furthermore, percutaneous absorption tests using the Franz diffusion cell method and subsequent HPLC-DAD analysis provided insights into the compound skin permeation capabilities, a critical factor for their practical application in cosmeceuticals.

Abstract Background Understanding the metabolic changes in colorectal cancer (CRC) and exploring potential diagnostic biomarkers is crucial for elucidating its pathogenesis and reducing mortality. Cancer cells are typically derived from cancer tissues and can be easily obtained and cultured. Systematic studies on CRC cells at different stages are still lacking. Additionally, there is a need to validate our previous findings from human serum. Methods Ultrahigh-performance liquid chromatography tandem high-resolution mass spectrometry (UHPLC-HRMS)-based metabolomics and lipidomics were employed to comprehensively measure metabolites and lipids in CRC cells at four different stages and serum samples from normal control (NR) and CRC subjects. Univariate and multivariate statistical analyses were applied to select the differential metabolites and lipids between groups. Biomarkers with good diagnostic efficacy for CRC that existed in both cells and serum were screened by the receiver operating characteristic curve (ROC) analysis. Furthermore, potential biomarkers were validated using metabolite standards. Results Metabolite and lipid profiles differed significantly among CRC cells at stages A, B, C, and D. Dysregulation of glycerophospholipid (GPL), fatty acid (FA), and amino acid (AA) metabolism played a crucial role in the CRC progression, particularly GPL metabolism dominated by phosphatidylcholine (PC). A total of 46 differential metabolites and 29 differential lipids common to the four stages of CRC cells were discovered. Eight metabolites showed the same trends in CRC cells and serum from CRC patients compared to the control groups. Among them, palmitoylcarnitine and sphingosine could serve as potential biomarkers with the values of area under the curve (AUC) more than 0.80 in the serum and cells. Their panel exhibited excellent performance in discriminating CRC cells at different stages from normal cells (AUC = 1.00). Conclusions To our knowledge, this is the first research to attempt to validate the results of metabolism studies of serum from CRC patients using cell models. The metabolic disorders of PC, FA, and AA were closely related to the tumorigenesis of CRC, with PC being the more critical factor. The panel composed of palmitoylcarnitine and sphingosine may act as a potential biomarker for the diagnosis of CRC, aiding in its prevention.

We investigated the pharmacokinetic pathway of berberine and its metabolites in vitro, in Caco-2 cells, and in human participants following the administration of dihydroberberine (DHB) and micellar berberine (LipoMicel®, LMB) formulations. A pilot trial involving nine healthy volunteers was conducted over a 24 h period; blood samples were collected and subjected to Ultra High-Performance Liquid Chromatography–High Resolution Mass Spectrometry (UHPLC-HRMS) analyses to quantify the concentrations of berberine and its metabolites. Pharmacokinetic correlations indicated that berberrubine and thalifendine follow distinct metabolic pathways. Additionally, jatrorrhizine sulfate appeared to undergo metabolism differently compared to the other sulfated metabolites. Moreover, berberrubine glucuronide likely has a unique metabolic pathway distinct from other glucuronides. The human trial revealed significantly higher blood concentrations of berberine metabolites in participants of the DHB treatment group compared to the LMB treatment group—except for berberrubine glucuronide, which was only detected in the LMB treatment group. Similarly, results from in vitro investigations showed significant differences in berberine metabolite profiles between DHB and LMB. Dihydroberberine, dihydroxy-berberrubine/thalifendine and jatrorrhizine sulfate were detected in LMB-treated cells, but not in DHB-treated cells; thalifendine and jatrorrhizine-glucuronide were detected in DHB-treated cells only. While DHB treatment provided higher blood concentrations of berberine and most berberine metabolites, both in vitro (Caco-2 cells) and in vivo human studies showed that treatment with LMB resulted in a higher proportion of unmetabolized berberine compared to DHB. These findings suggest potential clinical implications that merit further investigation in future large-scale trials. [ABSTRACT FROM AUTHOR]

Selenosugars are gaining growing interest due to their antioxidant efficacy, and their ability to inhibit glycosidases, repair skin tissue or reduce endothelial dysfunction. Among selenosugars, those in which selenium replaces heterocyclic oxygen in a 5-membered sugar were our focus, and their coupling with phenolic compounds appears to be a strategy aimed at producing new compounds with enhanced antioxidant efficacy. In this context, the Mitsunobu reaction has been advantageously explored to obtain trans-p-coumaroyl-1,4-deoxy-2,3-O-isopropylidene-4-seleno-d-ribose, trans-caffeoyl-1,4-deoxy-2,3-O-isopropylidene-4-seleno-d-ribose, and trans-feruloyl-1,4-deoxy-2,3-O-isopropylidene-4-seleno-d-ribose. These compounds underwent removal of the iso-propylidene group, to provide the corresponding hydroxycinnamoyl-1,4-deoxy-4-seleno-d-ribose. All compounds were characterized by Nuclear Magnetic Resonance (NMR) spectroscopy and High-Resolution Mass Spectrometry (HRMS). This latter technique was pivotal for ensuing cellular metabolomics analyses. In fact, after evaluating the anti-radical efficacy through 2,2-diphenyl-1-picrylhydrazyl (DPPH) and 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) methods, which underline the massive role of the phenolic moiety in establishing efficacy, the compounds, whose cytotoxicity was first screened in two highly oxidative-stress-sensitive cells, were tested for their wound healing properties towards human HaCaT keratinocytes cells. Caffeoyl- and feruloyl selenosugars exerted a dose-dependent repair activity, while, as highlighted by the metabolomic approach, they were poorly taken up within the cells. [ABSTRACT FROM AUTHOR]

American ginseng (Panax quinquefolium L.) is used as tonic plant and high-grade nourishment. Ultra-high-performance liquid chromatography–high resolution mass spectrometry (UHPLC–HRMS) method was established for identifying the chemical constituent in three morphological regions of American ginseng, including main root (MR), rhizome (RH) and lateral root (LR). The 63 saponins was identifed in diferent morphological regions of 10 American ginseng samples. The chemical maker compounds in corresponding morphological region, while the major compounds of MR (malonyl-ginsenoside Rb1, ginsenoside Rd, Rs2 and pseudo-RC1), LR (stipuleanoside R2, ginsenoside Re and malonyl-ginsenoside Rc), and RH (malonyl-ginsenoside Rd, Rb3, and chikusetsu saponin II) were discovered. Correlation analysis showed that 11 compounds were positively correlated with the antioxidant activity of American ginseng. [ABSTRACT FROM AUTHOR]

Background: Understanding the metabolic changes in colorectal cancer (CRC) and exploring potential diagnostic biomarkers is crucial for elucidating its pathogenesis and reducing mortality. Cancer cells are typically derived from cancer tissues and can be easily obtained and cultured. Systematic studies on CRC cells at different stages are still lacking. Additionally, there is a need to validate our previous findings from human serum. Methods: Ultrahigh-performance liquid chromatography tandem high-resolution mass spectrometry (UHPLC-HRMS)-based metabolomics and lipidomics were employed to comprehensively measure metabolites and lipids in CRC cells at four different stages and serum samples from normal control (NR) and CRC subjects. Univariate and multivariate statistical analyses were applied to select the differential metabolites and lipids between groups. Biomarkers with good diagnostic efficacy for CRC that existed in both cells and serum were screened by the receiver operating characteristic curve (ROC) analysis. Furthermore, potential biomarkers were validated using metabolite standards. Results: Metabolite and lipid profiles differed significantly among CRC cells at stages A, B, C, and D. Dysregulation of glycerophospholipid (GPL), fatty acid (FA), and amino acid (AA) metabolism played a crucial role in the CRC progression, particularly GPL metabolism dominated by phosphatidylcholine (PC). A total of 46 differential metabolites and 29 differential lipids common to the four stages of CRC cells were discovered. Eight metabolites showed the same trends in CRC cells and serum from CRC patients compared to the control groups. Among them, palmitoylcarnitine and sphingosine could serve as potential biomarkers with the values of area under the curve (AUC) more than 0.80 in the serum and cells. Their panel exhibited excellent performance in discriminating CRC cells at different stages from normal cells (AUC = 1.00). Conclusions: To our knowledge, this is the first research to attempt to validate the results of metabolism studies of serum from CRC patients using cell models. The metabolic disorders of PC, FA, and AA were closely related to the tumorigenesis of CRC, with PC being the more critical factor. The panel composed of palmitoylcarnitine and sphingosine may act as a potential biomarker for the diagnosis of CRC, aiding in its prevention. [ABSTRACT FROM AUTHOR]

Disorders of lipid metabolism are a common cause of coronary heart disease (CHD) and its comorbidities. In this study, ultra‐performance liquid chromatography–high‐resolution mass spectrometry in data‐independent acquisition (DIA) mode was applied to collect abundant tandem mass spectrometry data, which provided valuable information for lipid annotation. For the lipid isomers that could not be completely separated by chromatography, parallel reaction monitoring (PRM) mode was used for quantification. A total of 223 plasma lipid metabolites were annotated, and 116 of them were identified for their fatty acyl chain composition and location. In addition, 152 plasma lipids in patients with CHD and its comorbidities were quantitatively analyzed. Multivariate statistical analysis and metabolic pathway analysis demonstrated that glycerophospholipid and sphingolipid metabolism deserved more attention for CHD. This study proposed a method combining DIA and PRM for high‐throughput characterization of plasma lipids. The results also improved our understanding of metabolic disorders of CHD and its comorbidities, which can provide valuable suggestions for medical intervention. [ABSTRACT FROM AUTHOR]

Diatoms are single-celled photosynthetic eukaryotes responsible for CO2 fixation and primary production in aquatic ecosystems. The cosmopolitan marine diatom Coscinodiscus granii can form seasonal blooms in coastal areas and interact with various microorganisms, including the parasitic oomycete Lagenisma coscinodisci. This unicellular eukaryote is mainly present in the northern hemisphere as an obligate parasite of the genus Coscinodiscus. Understanding the interplay of abiotic factors such as temperature and biotic factors like parasitism on algal physiology is crucial as it dictates plankton community composition and is especially relevant during environmental changes and warming events. This study investigates the impact of two temperatures, 13 °C and 25 °C, on Coscinodiscus granii under laboratory conditions. A decreased infection rate of the parasite was observed at the elevated temperature. Comparative metabolomic analysis using UHPLC-HRMS revealed that temperature and parasitism significantly affect the algal cell metabolome. Abundances of metabolites related to sulfur metabolism, including cysteinoleic acid and dimethylsulfoniopropionate, as well as molecules linked to fatty acid metabolism, e.g., carnitine, acetylcarnitine, and eicosapentanoic acid, significantly increase in cells grown at a higher temperature, suggesting the enhanced rate of metabolism of host cells as the temperature rises. Our study reveals how temperature-induced metabolic changes can influence host–parasite dynamics in a changing environment.

Polyphenols are responsible for wine colour and astringency, and, as antioxidants, they also have beneficial health properties. In this work, we developed a robust full-scan high-resolution mass spectrometry method for the quantification of 90 phenolic compounds in wine samples (either red, rosé, or white wine), using a UHPLC-OrbitrapTM system. With this method, we could conduct a detailed analysis of phenolic compounds in red, rosé, and white wines with great selectivity due to sub-ppm mass accuracy. Moreover, accessing the full-scan spectrum enabled us to monitor all the other compounds detected in the sample, facilitating the adaptability of this method to new phenolic compounds if needed.

Mealworm, migratory locust, and house cricket have recently been recognized by the European Commission as novel foods, thus being suitable in different food applications. In this work, we tested their powders as meat extenders at 5% (w/w) inclusion in beef burgers, considering their ability to vehicle phenolic compounds during simulated in vitro static gastrointestinal digestion (INFOGEST). Insect powders were abundant in different phenolic classes, recording the highest values in locust (LP; 314.69 mg/kg), followed by cricket (CP; 113.3 mg/kg) and mealworm (MWP; 51.9 mg/kg). Following a pan-cooking process, LP burgers were confirmed as the best source of phenolics, with a marked abundance of flavonoids and phenolic acids. Interestingly, the insect powders were found to affect the in vitro gastrointestinal bioaccessibility of phenolic compounds when compared with the CTR burger, likely promoted by the interactions between the phenolic compounds and proteins characterizing the tested insect powders. Among the most discriminant phenolic metabolites at the gastrointestinal level, we found several phenolic acids (mainly hydroxycinnamics), recording the highest content for the digested CP-containing burgers. Finally, stilbenes showed significant correlation values at the intestinal level with both antioxidant and enzymatic activities, while total flavonoids were the most correlated with the inhibition of acetylcholinesterase. Taken together, our preliminary findings demonstrated that insect powders added to beef burgers can promote the bioaccessibility and potential bioavailability of phenolics in the distal tracts of the intestine. [ABSTRACT FROM AUTHOR]

Introduction: Fungal species are an attractive resource for physiologically functional food and drug precursor. Fomes officinalis Ames, a medicinal fungus, is traditionally used as a folk medicine in traditional Chinese medicine prescription for the therapy of cough and asthma. The water‐soluble substances in Chinese herbal medicines are likely to play an important physiological function. However, information on probing and identifying chemical components of the aqueous extract of Fomes officinalis Ames (AFO) remains unknown. Objective: This study was conducted to screen and characterise the chemical components of AFO. Material and Methods: An effective and sensitive ultrahigh‐performance liquid chromatography tandem quadrupole‐Orbitrap high‐resolution mass spectrometry (UHPLC‐Q‐Orbitrap‐HRMS) method with the Full MS/PIL/dd‐MS2 acquisition approach was applied for the profiling of chemical components in AFO. An HSS T3 column was used for component separation, and a strategy of simultaneous targeted and untargeted multicomponent characterisation was implemented. Multiple identification approaches were used, including accurate molecular mass and elemental composition matching, literature and database searching, and fragmentation rules elucidation. Results: A total of 115 components, including 20 amino acids and derivatives, six nucleobases, nine nucleosides, 75 dipeptides, two tripeptides, and three other components, were tentatively identified. Among them, the targeted exploring method screened six nucleobases and nine nucleosides including modified nucleosides. To our best knowledge, this is the first time a report has been done on the presence of the 115 compounds in AFO. Conclusion: Profiling and characterisation compounds of AFO enriched its material basis, which would lay the foundation for improving potential medicinal and nutritional values and effecting comprehensive quality control of Fomes officinalis Ames. The information on identifying the hydrophilic constituents of the aqueous extract of Fomes officinalis Ames was reported based on ultrahigh‐performance liquid chromatography tandem quadrupole‐Orbitrap high‐resolution mass spectrometry. Meanwhile, a comprehensive approach that consists of targeted and untargeted analytical strategy, database searching, and fragmentation rules elucidation was used to characterize the chemical composition. In total, 115 components, including 20 amino acids and derivatives, 6 nucleobases, 9 nucleosides, 75 dipeptides, 2 tripeptides, and 3 other components, were tentatively identified. [ABSTRACT FROM AUTHOR]

An oleaginous microalga Micractinum inermum isolated from Mariana Lake, AB, Canada was cultured in a 1000 L photobioreactor with an f/2 medium to study its lipid content and neutral lipid profile. Algal biomass was collected at the stationary phase contained a significant amount of lipids (44.2%), as determined by Folch's method. The lipid was fractionated into neutral lipid, glycolipid and phospholipid fractions. The neutral lipid constitutes almost 77.3% of the total lipid species and is mainly composed of triacylglycerols (TAGs) determined by a proton NMR study. UHPLC-HRMS analysis allows us for the first time to identify 81 TAGs in the neutral lipid fraction of M. inermum. The fatty acid acyl side chains were identified based on fragment ions observed in MSMS analysis. TAGs with fatty acid acyl chains 18:1/18:1/18:1, 18:1/18:1/16:0, 18:2/18:1/16:0, and 18:2/18:2/18:0 were the major ones among the identified TAGs. Fatty acid analysis further supports the fact that oleic acid was the major fatty acid present in the neutral lipid fraction of M. inermum constituting 41.7%, followed by linoleic acid at 21.5%, and palmitic acid at 21.2%. The saturated and monounsaturated fatty acids were 67.8% or higher in the lipid fraction. Long-chain fatty acids were only present in a minor quantity. The results clearly demonstrate that M. inermum is an excellent source for TAGs. [ABSTRACT FROM AUTHOR]

Sideritis scardica Griseb, also known as "mountain tea" and "Olympus tea" (Lamiaceae family) is an endemic plant from the mountainous regions of the Balkan Peninsula. In this study, we focused on an in-depth phytochemical analysis of S. scardica infusion using ultra-high-performance liquid chromatography hyphenated with high-resolution mass spectrometry (UHPLC–HRMS). Quantitative determination of the main secondary metabolites was carried out by UHPLC–HRMS analyses using the external standard method. The results revealed more than 100 metabolites, including five sugar acids and saccharides, 21 carboxylic, hydroxybenzoic, hydroxycinnamic acids, and derivatives, 15 acylquinic acids, 10 phenylpropanoid glycosides, four iridoid glycosides, 28 flavonoids, seven fatty acids, and four organosulfur compounds. Furthermore, a dereplication and fragmentation patterns of five caffeic acids oligomers and four acylhexaric acids was performed for the first time in S. scardica. Regarding the quantitative analysis, the phenylethanoid verbascoside (53) (151.54 ± 10.86 mg/g lyophilized infusion, li), the glycosides of isoscutellarein (78) (151.70 ± 14.78 mg/g li), methylisoscutelarein (82) (107.4 ± 9.07 mg/g li), and hypolaetin (79) (78.33 ± 3.29 mg/g li), as well as caffeic acid (20) (87.25 ± 6.54 mg/g li), were found to be the major compounds in S. scardica infusion. The performed state-of-the-art phytochemical analysis of S. scardica provides additional knowledge for the chemical constituents and usage of this valuable medicinal plant. [ABSTRACT FROM AUTHOR]

A validated UHPLC-HRMS method was developed to identify and quantify polar phenolic metabolites in the EtOH extract from H. aucheri Jaub. & Spach's aerial parts. The external standards, chlorogenic acid, mangiferin, and hyperoside were selected in this analysis. Forty-four compounds, encompassing hydroxybenzoic and hydroxycinnamic acids derivatives, benzophenones, catechins, xanthones, flavonols, biflavones, and chromones were detected and quantified in the aerial parts of the titled plant. Pentahydroxyxanthone-C-glycoside 15, maclurin-O-(benzoyl)-hexoside 37, norathyriol-O-(benzoyl)-hexosides 38 and 42 were suggested to be new natural compounds, while maclurin-O-hexoside 2 was reported for the first time for Hypericum genus. Additionally, more than 22 secondary metabolites, including benzophenones, hydroxycinnamic acid derivatives, catechins, and a chromone, were identified for the first time in H. aucheri. The amounts of the detected metabolites were calculated relative to external standards. The dominant polar phenolic constituents were chlorogenic acid (11.55 mg/g D.W.) and mangiferin (9.13 mg/g D.W.). [ABSTRACT FROM AUTHOR]

Rhizobium rhizogenes mediated genetic transformation is a promising biotechnological tool to obtain specialized metabolites having valuable biological activities. The present study reports a reliable transformation protocol for hairy root induction with sustainable growth and identification of specialized metabolites with antioxidant activities in hybrid poplar clone 717-1B4 (Populus tremula × Populus alba). Four different wild type agropine R. rhizogenes strains ATCC 15834, A4, MSU 440 and LBA 9402 were employed to check their efficiency on hairy root induction and accumulation of specialized metabolites. Results indicated that the transformation efficiency was highly dependent on strain used and could be increased by adding acetosyringone into the co-cultivation medium. PCR amplification of rolB and rolC genes confirmed the transgenic nature of the hairy roots. Adding polyvinylpyrrolidone into the culture media not only circumvented the problem of browning due to phenolics but also resulted in healthy and fast growth of hairy roots. Colorimetric assays revealed the presence of phenolic compounds, among which flavonoids in ethanolic extracts of different hairy root lines which could be associated with the significant antioxidant activities as depicted by FRAP and DPPH assays. The hairy root lines obtained with different R. rhizogenes strains showed similar phytochemical profiles. UHPLC-HRMS analysis allowed the separation of 136 peaks, out of which catechin, nigracin, salireposide, trichocarpin and tremulacin were identified. In conclusion, poplar hairy roots are a promising raw material for producing specialized metabolites with bioactive properties that could be further used for various pharmaceutical, food and cosmetics applications.Key message: A sustainable hairy root culture system was developed on poplar model tree. A first UHPLC-MS phytochemical analysis of the root compartment is provided, revealing the presence of antioxidant bioactive compounds. [ABSTRACT FROM AUTHOR]

ABSTRACT STW 5, a blend of nine medicinal plant extracts, exhibits promising efficacy in treating functional gastrointestinal disorders, notably irritable bowel syndrome (IBS). Nonetheless, its effects on the gastrointestinal microbiome and the role of microbiota on the conversion of its constituents are still largely unexplored. This study employed an experimental ex vivo model to investigate STW 5’s differential effects on fecal microbial communities and metabolite production in samples from individuals with and without IBS. Using 560 fecal microcosms (IBS patients, n = 6; healthy controls, n = 10), we evaluated the influence of pre-digested STW 5 and controls on microbial and metabolite composition at time points 0, 0.5, 4, and 24 h. Our findings demonstrate the potential of this ex vivo platform to analyze herbal medicine turnover within 4 h with minimal microbiome shifts due to abiotic factors. While only minor taxonomic disparities were noted between IBS- and non-IBS samples and upon treatment with STW 5, rapid metabolic turnover of STW 5 components into specific degradation products, such as 18β-glycyrrhetinic acid, davidigenin, herniarin, 3-(3-hydroxyphenyl)propanoic acid, and 3-(2-hydroxy-4-methoxyphenyl)propanoic acid occurred. For davidigenin, 3-(3-hydroxyphenyl)propanoic acid and 18β-glycyrrhetinic acid, anti-inflammatory, cytoprotective, or spasmolytic activities have been previously described. Notably, the microbiome-driven metabolic transformation did not induce a global microbiome shift, and the detected metabolites were minimally linked to specific taxa. Observed biotransformations were independent of IBS diagnosis, suggesting potential benefits for IBS patients from biotransformation products of STW 5.IMPORTANCESTW 5 is an herbal medicinal product with proven clinical efficacy in the treatment of functional gastrointestinal disorders, like functional dyspepsia and irritable bowel syndrome (IBS). The effects of STW 5 on fecal microbial communities and metabolite production effects have been studied in an experimental model with fecal samples from individuals with and without IBS. While only minor taxonomic disparities were noted between IBS- and non-IBS samples and upon treatment with STW 5, rapid metabolic turnover of STW 5 components into specific degradation products with reported anti-inflammatory, cytoprotective, or spasmolytic activities was observed, which may be relevant for the pharmacological activity of STW 5.

Marine-derived fungi are assuming an increasingly central role in the search for natural leading compounds with unique chemical structures and diverse pharmacological properties. However, some gene clusters are not expressed under laboratory conditions. In this study, we have found that a marine-derived fungus Aspergillus sp. SYPUF29 would survive well by adding an exogenous nitric oxide donor (sodium nitroprusside, SNP) and nitric oxide synthetase inhibitor (L-NG-nitroarginine methyl ester, L-NAME) in culture conditions. Moreover, using the LC-MS/MS, we initially assessed and characterized the difference in metabolites of Aspergillus sp. SYPUF29 with or without an additional source of nitrogen. We have found that the metabolic pathway of Arginine and proline metabolism pathways was highly enriched, which was conducive to the accumulation of alkaloids and nitrogen-containing compounds after adding an additional source of nitrogen in the cultivated condition. Additionally, the in vitro anti-neuroinflammatory study showed that the extracts after SNP and L-NAME were administrated can potently inhibit LPS-induced NO-releasing of BV2 cells with lower IC50 value than without nitric oxide. Further Western blotting assays have demonstrated that the mechanism of these extracts was associated with the TLR4 signaling pathway. Additionally, the chemical investigation was conducted and led to nine compounds (SF1–SF9) from AS1; and six of them belonged to alkaloids and nitrogen-containing compounds (SF1–SF6), of which SF1, SF2, and SF8 exhibited stronger activities than the positive control, and showed potential to develop the inhibitors of neuroinflammation.

Annatto, obtained from the seeds of achiote (Bixa orellana L.), is a widely used orange pigment rich in bixin and other apocarotenoids. This work reports the optimisation of a green extraction method of pigments and antioxidant compounds from achiote as well as its integration in a one-step green extraction-cosmetic formulation process. A biphasic solvent system of water and oil was used to recover simultaneously polar polyphenols, and less polar compounds, such as δ-tocotrienol and bixin. The optimisation of the ultrasound assisted extraction is presented, as well as a comparison of different vegetable oils used as extraction solvents. The composition, physicochemical properties and antioxidant activity of the oils were studied and their extraction performance was compared. Refined sunflower oil proved to be a better solvent than virgin olive, jojoba, coconut and grapeseed oils. Both aqueous and oil phases displayed an interesting antioxidant capacity. The oil phase contained 0.9% of bixin, as well as minor apocarotenoids and δ-tocotrienol. Twelve compounds, mainly phenolics, were identified by UHPLC-DAD-HRMS/MS in the aqueous phase. Twenty-one volatile compounds were identified in the volatile fraction by SPME-GC-MS. Lastly, a one-step green process is proposed to combine the extraction and the cosmetic formulation of the bioactive compounds.

Traditional strategies for the metabolic profiling of doping are limited by the unpredictable metabolic pathways and the numerous proportions of background and chemical noise that lead to inadequate metabolism knowledge, thereby affecting the selection of optimal detection targets. Thus, a stable isotope labeling-based nontargeted strategy combined with ultra-high-performance liquid chromatography–high-resolution mass spectrometry (UHPLC-HRMS) was first proposed for the effective and rapid metabolism analysis of small-molecule doping agents and demonstrated via its application to a novel doping BPC-157. Using 13C/15N-labeled BPC-157, a complete workflow including automatic 13C0,15N0-13C6,15N2 m/z pair picking based on the characteristic behaviors of isotope pairs was constructed, and one metabolite produced by a novel metabolic pathway plus eight metabolites produced by the conventional amide-bond breaking metabolic pathway were successfully discovered from two incubation models. Furthermore, a specific method for the detection of BPC-157 and the five main metabolites in human urine was developed and validated with satisfactory detection limits (0.01~0.11 ng/mL) and excellent quantitative ability (linearity: 0.02~50 ng/mL with R2 > 0.999; relative error (RE)% < 10% and relative standard deviation (RSD)% < 5%; recovery > 90%). The novel metabolic pathway and the in vitro metabolic profile could provide new insights into the biotransformation of BPC-157 and improved targets for doping control. [ABSTRACT FROM AUTHOR]

The excreta of Trogopterus xanthipes ("Wulingzhi" in Chinese, WLZ) is a well‐known traditional Chinese medicine. It has been used for centuries to treat amenorrhea, menstruation and postpartum abdominal pain. However, a systematic quality study on WLZ chemical markers has yet to be conducted. This study aimed to establish an ultra‐high‐performance liquid chromatography coupled with a hybrid quadruple extraction Orbitrap high‐resolution mass spectrometry (UHPLC–Q‐Orbitrap–HRMS) method for the simultaneous quantitative determination of 20 compounds in 53 batches of WLZ; the method rapidly and sensitively determined the 20 plant‐ or animal‐derived compounds. Firstly, the proposed approach was validated to satisfy the method's linearity, detection limits, precision, repeatability, stability and accuracy. Subsequently, multivariate analysis was used to identify correlations between the samples and feed, processing and regions. Finally, this method was used to further identify chemical markers for quality control in combination with chemometrics. This is the first report on pinusolide, betaine, hippuric acid, 4‐oxorentinoic acid, 15‐methoxypinusolidic acid and 4‐oxoisotrentinoin in WLZ; the quality of WLZ became homogeneous after processing with vinegar (V‐WLZ). Moreover, we screened for potential component markers, including uridine, allantoin, amentoflavone, hippuric acid, 3,4‐dihydroxybenzoic acid, pinusolide, quercetin and kaempferol. These results were practical and efficient for the chemical clarification of WLZ and V‐WLZ. [ABSTRACT FROM AUTHOR]

The seeds of Paeonia clusii Stern subsp. clusii and Paeonia mascula (L.) Mill. subsp. mascula growing wild in Greece, though not previously investigated, has been studied as a source of bioactive stilbenoids and other phenolics. Their methanol extracts were analyzed using ultra high-performance liquid chromatography—high-resolution mass spectrometry (UHPLC-HRMS), and among the identified metabolites (62), 19 paeoniflorin's derivatives, 17 flavonoids and 12 stilbenes were detected. Moreover, through classic phytochemical separation procedures, twelve among them were isolated and fully spectrally determined as trans-resveratrol, trans-resveratrol-4′-O-β-D-glucopyranoside, cis-resveratrol-4′-O-β-D-glucopyranoside, trans-gnetin-H, trans-ε-viniferin, luteolin, luteolin-3′-O-β-D-glucopyranoside, luteolin-3′,4′-di-O-β-D-glucopyranoside, apigenin, hispidulin, paeoniflorin and benzoyl-paeoniflorin. All seed extracts were measured for their total phenolic content (TPC), appearing as a rich source (116.04 and 103.63 mg GAE/g extract, respectively), followed by free radical (DPPH) scavenging capacity (75.24% and 91.54% inhibition at the concentration of 200 μg/mL). The evaluation of tyrosinase inhibition for both extracts (61% and 70%, respectively) confirmed the potential for their future application in skin health care, comparable with other paeonies of Chinese origin, which are well-known as skin whitening and anti-aging promoters. [ABSTRACT FROM AUTHOR]

Geographical provenience is nowadays a relevant aspect of the authenticity and the quality of many food commodities. Dehydrated apple cubes/slices represent an ingredient commonly used by food companies for bakery products. However, this apple‐based matrix is not so known and studied from an analytical point of view. In the present work, seven compounds were identified as key molecules to distinguish between Italian and non‐Italian samples, through an untargeted ultrahigh‐pressure liquid chromatography‐high‐resolution mass spectrometry (UHPLC‐HRMS) approach. This methodology was merged with multivariate statistical analysis, and the principal features were studied and identified considering several identification steps. Samples from 2020 and 2021 harvesting campaigns, with partial and total dehydration rates, with or without peel, and from different apple varieties were considered for the study, for a total of 91 samples. Afterward, the same analysis protocol was applied to an external set (n = 12 samples), included in the statistical models, searching for the key compounds identified in the training set. Interesting and significant results underlined the potentiality of the UHPLC‐HRMS technology as a confirmatory strategy for the geographical origin assessment of dehydrated apple commodities. [ABSTRACT FROM AUTHOR]

Selenosugars are gaining growing interest due to their antioxidant efficacy, and their ability to inhibit glycosidases, repair skin tissue or reduce endothelial dysfunction. Among selenosugars, those in which selenium replaces heterocyclic oxygen in a 5-membered sugar were our focus, and their coupling with phenolic compounds appears to be a strategy aimed at producing new compounds with enhanced antioxidant efficacy. In this context, the Mitsunobu reaction has been advantageously explored to obtain trans-p-coumaroyl-1,4-deoxy-2,3-O-isopropylidene-4-seleno-d-ribose, trans-caffeoyl-1,4-deoxy-2,3-O-isopropylidene-4-seleno-d-ribose, and trans-feruloyl-1,4-deoxy-2,3-O-isopropylidene-4-seleno-d-ribose. These compounds underwent removal of the iso-propylidene group, to provide the corresponding hydroxycinnamoyl-1,4-deoxy-4-seleno-d-ribose. All compounds were characterized by Nuclear Magnetic Resonance (NMR) spectroscopy and High-Resolution Mass Spectrometry (HRMS). This latter technique was pivotal for ensuing cellular metabolomics analyses. In fact, after evaluating the anti-radical efficacy through 2,2-diphenyl-1-picrylhydrazyl (DPPH) and 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) methods, which underline the massive role of the phenolic moiety in establishing efficacy, the compounds, whose cytotoxicity was first screened in two highly oxidative-stress-sensitive cells, were tested for their wound healing properties towards human HaCaT keratinocytes cells. Caffeoyl- and feruloyl selenosugars exerted a dose-dependent repair activity, while, as highlighted by the metabolomic approach, they were poorly taken up within the cells.

Genipin, an aglycone of geniposide, is a rich iridoid component in the fruit of Gardenia jasminoides Ellis and has numerous biological activities. However, its metabolic profiles in vivo and vitro remain unclear. In this study, an effective analytical strategy based on ultra-high-performance liquid chromatography-high resolution mass spectrometry (UHPLC-HRMS) in positive and negative ion modes was developed to analyze and identify genipin metabolites in rat urine, blood, feces, and fecal fermentation in combination with many methods including post-collection data mining methods, high-resolution extracted ion chromatography (HREIC), and multiple mass defect filtering (MMDF). Simultaneously, the metabolites of genipin in vivo were verified by fecal fermentation of SD rats at different times. Finally, based on information such as reference substances, chromatographic retention behavior, and accurate mass determination, a total of 50 metabolites (including prototypes) were identified in vivo. Among them, 7, 31 and 28 metabolites in vivo were identified in blood, urine, and feces, respectively. Our results showed that genipin could generate different metabolites that underwent multiple metabolic reactions in vivo including methylation, hydroxylation, dehydroxylation, hydrogenation, sulfonation, glucuronidation, demethylation, and their superimposed reactions. Forty-six metabolites were verified in vitro. Meanwhile, 2 and 19 metabolites identified in blood and urine were also verified in fecal fermentation at different times. These results demonstrated that metabolites were produced in feces and reabsorbed into the body. In conclusion, the newly discovered metabolites of genipin can provide a new perspective for understanding its pharmacological effects and build the foundation for thee toxicity and safety evaluations of genipin. [ABSTRACT FROM AUTHOR]

Lipidomics refers to the full characterization of lipids present within a cell, tissue, organism, or biological system. One of the bottlenecks affecting reliable lipidomic analysis is the extraction of lipids from biological samples. An ideal extraction method should have a maximum lipid recovery and the ability to extract a broad range of lipid classes with acceptable reproducibility. The most common lipid extraction relies on either protein precipitation (monophasic methods) or liquid–liquid partitioning (bi- or triphasic methods). In this study, three monophasic extraction systems, isopropanol (IPA), MeOH/MTBE/CHCl3 (MMC), and EtOAc/EtOH (EE), alongside three biphasic extraction methods, Folch, butanol/MeOH/heptane/EtOAc (BUME), and MeOH/MTBE (MTBE), were evaluated for their performance in characterization of the mouse lipidome of six different tissue types, including pancreas, spleen, liver, brain, small intestine, and plasma. Sixteen lipid classes were investigated in this study using reversed-phase liquid chromatography/mass spectrometry. Results showed that all extraction methods had comparable recoveries for all tested lipid classes except lysophosphatidylcholines, lysophosphatidylethanolamines, acyl carnitines, sphingomyelines, and sphingosines. The recoveries of these classes were significantly lower with the MTBE method, which could be compensated by the addition of stable isotope-labeled internal standards prior to lipid extraction. Moreover, IPA and EE methods showed poor reproducibility in extracting lipids from most tested tissues. In general, Folch is the optimum method in terms of efficacy and reproducibility for extracting mouse pancreas, spleen, brain, and plasma. However, MMC and BUME methods are more favored when extracting mouse liver or intestine. [ABSTRACT FROM AUTHOR]

Color is a major quality trait of rosé wines due to their packaging in clear glass bottles. This color is due to the presence of phenolic pigments extracted from grapes to wines and products of reactions taking place during the wine-making process. This study focuses on changes occurring during the alcoholic fermentation of Syrah, Grenache and Cinsault musts, which were conducted at laboratory (250 mL) and pilot (100 L) scales. The color and phenolic composition of the musts and wines were analyzed using UV-visible spectrophotometry, and metabolomics fingerprints were acquired by ultra-high performance liquid chromatography−high-resolution mass spectrometry. Untargeted metabolomics data highlighted markers of fermentation stage (must or wine) and markers related to the grape variety (e.g., anthocyanins in Syrah, hydroxycinnamates and tryptophan derivatives in Grenache, norisoprenoids released during fermentation in Cinsault). Cinsault wines contained higher molecular weight compounds possibly resulting from the oxidation of phenolics, which may contribute to their high absorbance values. [ABSTRACT FROM AUTHOR]

In the context of climate change, faba beans are an interesting alternative to animal proteins but are characterised by off-notes and bitterness that decrease consumer acceptability. However, research on pulse bitterness is often limited to soybeans and peas. This study aimed to highlight potential bitter non-volatile compounds in faba beans. First, the bitterness of flours and air-classified fractions (starch and protein) of three faba bean cultivars was evaluated by a trained panel. The fractions from the high-alkaloid cultivars and the protein fractions exhibited higher bitter intensity. Second, an untargeted metabolomic approach using ultra-high-performance liquid chromatography–diode array detector–tandem–high resolution mass spectrometry (UHPLC–DAD–HRMS) was correlated with the bitter perception of the fractions. Third, 42 tentatively identified non-volatile compounds were associated with faba bean bitterness by correlated sensory and metabolomic data. These compounds mainly belonged to different chemical classes such as alkaloids, amino acids, phenolic compounds, organic acids, and terpenoids. This research provided a better understanding of the molecules responsible for bitterness in faba beans and the impact of cultivar and air-classification on the bitter content. The bitter character of these highlighted compounds needs to be confirmed by sensory and/or cellular analyses to identify removal or masking strategies. [ABSTRACT FROM AUTHOR]

Copaifera langsdorffii Desf. is recognised as one of most famous medicinal and economic species of Copaiba, occurring in several distinct biomes. An untargeted metabolomic approach was used to evaluate the chemical variability of C. langsdorffii from contrasting climates biomes (Atlantic Rainflorest and the semiarid Cerrado). Metabolomic analysis enabled the identification of 11 compounds, including glycosylated flavonoids and galloylquinic acid derivatives. Multivariate analysis highlighted that Cerrado population had a significantly higher concentrations of galloylquinic acid derivatives in comparison to the rainforest biome. Meanwhile, Atlantic Rainforest populations presented higher content of flavonols. Semiarid biome, reduced the concentration of flavonoids, mainly concerning quercetin and kaempferol derivatives, however, in this biome flavonoids were more diverse. Both chemical classes presented relevance to be used as geographical origin chemical markers by qualitative and quantitative features. [ABSTRACT FROM AUTHOR]

The global population growth has led to a higher demand for food production, necessitating improvements in agricultural productivity. However, abiotic and biotic stresses pose significant challenges, reducing crop yields and impacting economic and social welfare. Drought, in particular, severely constrains agriculture, resulting in unproductive soil, reduced farmland, and jeopardized food security. Recently, the role of cyanobacteria from soil biocrusts in rehabilitating degraded land has gained attention due to their ability to enhance soil fertility and prevent erosion. The present study focused on Nostoc calcicola BOT1, an aquatic, diazotrophic cyanobacterial strain collected from an agricultural field at Banaras Hindu University, Varanasi, India. The aim was to investigate the effects of different dehydration treatments, specifically air drying (AD) and desiccator drying (DD) at various time intervals, on the physicochemical properties of N. calcicola BOT1. The impact of dehydration was assessed by analyzing the photosynthetic efficiency, pigments, biomolecules (carbohydrates, lipids, proteins, osmoprotectants), stress biomarkers, and non-enzymatic antioxidants. Furthermore, an analysis of the metabolic profiles of 96-hour DD and control mats was conducted using UHPLC-HRMS. Notably, there was a significant decrease in amino acid levels, while phenolic content, fatty acids, and lipids increased. These changes in metabolic activity during dehydration highlighted the presence of metabolite pools that contribute to the physiological and biochemical adjustments of N. calcicola BOT1, mitigating the impact of dehydration to some extent. Overall, present study demonstrated the accumulation of biochemical and nonenzymatic antioxidants in dehydrated mats, which could be utilized to stabilize unfavorable environmental conditions. Additionally, the strain N. calcicola BOT1 holds promise as a biofertilizer for semi-arid regions. [ABSTRACT FROM AUTHOR]

In the last decades, Primula veris subsp. veris (roots and flowers) has been over harvested through legal and illegal ways in Greece, due to its extremely high commercial demand, as it is used in industry because of its well-known therapeutic properties. As ex situ cultures of the plant have been already developed, in the current comparative study, the herbal teas (infusions) from both flowers of cowslip growing wild in the Prespa Lake Park (NW Greece), and from ex situ propagated and cultivated plant material, have been investigated, with the ultimate goal of assessing them qualitatively. Furthermore, through classic phytochemical studies, the ten most abundant metabolites, belonging to the chemical categories of flavonol-glycosides and methoxy flavones, have been identified and structurally determined. The chemical profile of both infusions has been further analyzed through UHPLC-HRMS, showing that they show only light differences. The total phenolic content (TPC) of both studied samples (wild and ex situ cultivation), was determined by the Folin–Ciocalteau method, followed by an antioxidant activity assay though DPPH where, in both cases, wild plants exerted higher phenolic load and stronger antioxidative properties. According to the reported results, it could be proposed that the ex situ cultivated plant material could facilitate the mass production of plants and the sustainable cultivation of cowslip in the Greek mountains. [ABSTRACT FROM AUTHOR]

Echinops ritro L. (Asteraceae) is traditionally used in the treatment of bacterial/fungal infections and respiratory and heart ailments. The aim of this study was to evaluate the potential of extracts from E. ritro leaves (ERLE) and flowering heads (ERFE) as antioxidant and hepatoprotective agents on diclofenac-induced lipid peroxidation and oxidative stress under in vitro and in vivo conditions. In isolated rat microsomes and hepatocytes, the extracts significantly alleviated oxidative stress by increasing cell viability and GSH levels and reducing LDH efflux and MDA production. During in vivo experiments, the administration of the ERFE alone or in combination with diclofenac resulted in a significant increase in cellular antioxidant protection and a decrease in lipid peroxidation witnessed by key markers and enzymes. A beneficial influence on the activity of the drug-metabolizing enzymes ethylmorphine-N-demetylase and aniline hydroxylase in liver tissue was found. In the acute toxicity test evaluation, the ERFE showed no toxicity. In the ultrahigh-performance liquid chromatography–high-resolution mass spectrometry analysis, 95 secondary metabolites were reported for the first time, including acylquinic acids, flavonoids, and coumarins. Protocatechuic acid O-hexoside, quinic, chlorogenic and 3, 5-dicaffeoylquinic acid, apigenin; apigenin 7-O-glucoside, hyperoside, jaceosidene, and cirsiliol dominated the profiles. The results suggest that both extracts should be designed for functional applications with antioxidant and hepatoprotective capacity. [ABSTRACT FROM AUTHOR]

A hydroxyl-functionalized covalent organic framework aerogel COFTHB-TAPB-aerogel was designed and prepared as an adsorbent for the removal of multiple lipids from human plasma. The applications of 1,3,5-tris(4′-hydroxy-5′-formylphenyl)benzene (THB) and 1,3,5-tris(4-aminophenyl)benzene (TAPB) as monomers, DMSO/mesitylene (v/v, 4/1) as reaction solvent, and n-propylamine as reaction regulator endow COFTHB-TAPB-aerogel with good adsorption performance for multiple lipids. The morphology, phase purity, specific surface area, pore size, surface charge, and stability of COFTHB-TAPB-aerogel were characterized. Adsorption thermodynamics and adsorption kinetics studies showed that COFTHB-TAPB-aerogel had high equilibrium adsorption capacities (> 15913 mg g−1) and fast adsorption equilibrium (≤ 10 s) for the four model lipids tested. COFTHB-TAPB-aerogel had good reusability with the removal of the model lipids being still more than 91% after 10 use cycles. The sample pretreatment conditions and adsorbent amounts used in lipids removal experiments were optimized. Under the optimized conditions, the method of ultra-high performance liquid chromatography–high-resolution mass spectrometry (UHPLC–HRMS) using COFTHB-TAPB-aerogel as solid-phase extraction sorbent was validated with negligible matrix effects (0.4–3.0%) and good accuracy (86.7–110%) and was applied to determine 20 amino acids in human plasma samples from healthy individuals and gastric adenocarcinoma (GA) patients. The established method has been proved to have good application potential for the removal of multiple lipids in human plasma to reduce the matrix effects and improve the accuracy of clinical LC–MS analysis. [ABSTRACT FROM AUTHOR]

More than 7000 synthetic compounds known as per- and poly-fluoroalkyl substances (PFAS) are applied to food packaging and other materials to provide fat, fire, and/or water resistance properties. These compounds have exceptional environmental stability and persistence due to the strong C-F chemical bond, earning them the moniker "forever chemicals". Emission of PFAS from industrial waste leads to water, air, and soil contamination. Due to this ubiquitous nature, combined with the fact that PFAS in humans are known to have carcinogenic and reprotoxic effects and to cause vaccine resistance and depression of the immunity system, PFAS may constitute a major threat to human health. For this reason, the attention of the scientific community and of control bodies is increasing and as a consequence legislation and the scientific literature on PFAS are constantly evolving. This review aims to provide a comprehensive overview of the state of the art about current legislation addressing PFAS; targeted and screening method for identification, detection and quantification of PFAS; toxicity of PFAS; and contamination of environmental and food matrices and from food contact matrices. A comprehensive review of the latest scientific research and recent developments in the legislation of PFAS will provide insights into the current understanding of PFAS and its health implications. Moreover, it will serve as a valuable reference for further studies related to PFAS and could help in informing future policy decisions. [ABSTRACT FROM AUTHOR]

Surface browning plays a major role in the quality loss of fresh-cut potatoes. Untargeted metabolomics were used to understand the metabolic changes of fresh-cut potato during the browning process. Their metabolites were profiled by ultra-high performance liquid chromatography coupled with high resolution mass spectrometry (UHPLC-HRMS). Data processing and metabolite annotation were completed by Compound Discoverer 3.3 software. Statistical analysis was applied to screen the key metabolites correlating with browning process. Fifteen key metabolites responsible for the browning process were putatively identified. Moreover, after analysis of the metabolic causes of glutamic acid, linolenic acid, glutathione, adenine, 12-OPDA and AMP, we found that the browning process of fresh-cut potatoes was related to the structural dissociation of the membrane, oxidation and reduction reaction and energy shortage. This work provides a reference for further investigation into the mechanism of browning in fresh-cut products. [ABSTRACT FROM AUTHOR]

The global population growth has led to a higher demand for food production, necessitating improvements in agricultural productivity. However, abiotic and biotic stresses pose significant challenges, reducing crop yields and impacting economic and social welfare. Drought, in particular, severely constrains agriculture, resulting in unproductive soil, reduced farmland, and jeopardized food security. Recently, the role of cyanobacteria from soil biocrusts in rehabilitating degraded land has gained attention due to their ability to enhance soil fertility and prevent erosion. The present study focused on Nostoc calcicola BOT1, an aquatic, diazotrophic cyanobacterial strain collected from an agricultural field at Banaras Hindu University, Varanasi, India. The aim was to investigate the effects of different dehydration treatments, specifically air drying (AD) and desiccator drying (DD) at various time intervals, on the physicochemical properties of N. calcicola BOT1. The impact of dehydration was assessed by analyzing the photosynthetic efficiency, pigments, biomolecules (carbohydrates, lipids, proteins, osmoprotectants), stress biomarkers, and non-enzymatic antioxidants. Furthermore, an analysis of the metabolic profiles of 96-hour DD and control mats was conducted using UHPLC-HRMS. Notably, there was a significant decrease in amino acid levels, while phenolic content, fatty acids, and lipids increased. These changes in metabolic activity during dehydration highlighted the presence of metabolite pools that contribute to the physiological and biochemical adjustments of N. calcicola BOT1, mitigating the impact of dehydration to some extent. Overall, present study demonstrated the accumulation of biochemical and non-enzymatic antioxidants in dehydrated mats, which could be utilized to stabilize unfavorable environmental conditions. Additionally, the strain N. calcicola BOT1 holds promise as a biofertilizer for semi-arid regions.

The time involved and the high economic cost of using oak barrels to age wines have led to a significant price difference compared to non-oak barrel aged wines and may lead to some fraudulent sales in the market. In this study, an untargeted metabolomic strategy was developed to detect the metabolite composition of oak barrel aged and non-oak barrel aged wines in both positive and negative ion modes by using UHPLC–HRMS combined with the recently developed chemometric method AntDAS. The results of partial least squares discrimination analysis (PLS-DA) showed that the samples were characterized into two categories. Finally, 51 compounds were identified in positive ion mode, while 26 compounds were identified in negative ion mode. The results indicate that combining UHPLC–HRMS with AntDAS can reveal the material basis of wines and has excellent potential to differentiate between oak barrel aged and non-oak barrel aged wines. [ABSTRACT FROM AUTHOR]

Cicerbita alpina (L.) Wallr. is a perennial herbaceous plant in the tribe Cichorieae (Lactuceae), Asteraceae family, distributed in the mountainous regions in Europe. In this study, we focused on the metabolite profiling and the bioactivity of C. alpina leaves and flowering heads methanol-aqueous extracts. The antioxidant activity of extracts, as well as inhibitory potential towards selected enzymes, involving in several human diseases, including metabolic syndrome (α-glucosidase, α-amylase, and lipase), Alzheimer's disease, (cholinesterases: AChE, BchE), hyperpigmentation (tyrosinase), and cytotoxicity were assessed. The workflow comprised ultra-high-performance liquid chromatography—high-resolution mass spectrometry (UHPLC-HRMS). UHPLC-HRMS analysis revealed more than 100 secondary metabolites, including acylquinic, acyltartaric acids, flavonoids, bitter sesquiterpene lactones (STLs), such as lactucin, dihydrolactucin, their derivatives, and coumarins. Leaves showed a stronger antioxidant activity compared to flowering heads, as well as lipase (4.75 ± 0.21 mg OE/g), AchE (1.98 ± 0.02 mg GALAE/g), BchE (0.74 ± 0.06 mg GALAE/g), and tyrosinase (49.87 ± 3.19 mg KAE/g) inhibitory potential. Flowering heads showed the highest activity against α-glucosidase (1.05 ± 0.17 mmol ACAE/g) and α-amylase (0.47 ± 0.03). The obtained results highlighted C. alpina as a rich source of acylquinic, acyltartaric acids, flavonoids, and STLs with significant bioactivity, and therefore the taxon could be considered as a potential candidate for the development of health-promoting applications. [ABSTRACT FROM AUTHOR]

Horse milk (HM) is one of the high-quality milks which is highly potential to be adulterated with lower price milk such as cow milk (CM) to get economic profit. This study aimed to develop an analytical method based on an untargeted metabolomics approach using ultrahigh-performance liquid chromatography-high-resolution mass spectrometry (UHPLC-HRMS) for HM authentication. The untargeted metabolomics results showed that HM and CM consist of different metabolite composition. Combined with chemometrics of principal component analysis (PCA), the developed method could distinguish pure HM, pure CM, and adulterated HM. Classification analysis using orthogonal projections to latent structure-discriminant analysis (OPLS-DA) successfully discriminated pure HM and adulterated HM in two separate classes without misclassification with a good of fitness (R2X = 0.771; R2Y = 0.999) and good predictivity (Q2 = 0.990). Metabolite's analysis found that ceramide (d18:1/24:1(15Z)), N-hexacosanoylglycine, and DG(16:1(9Z)/18:3(9Z, 12Z, 15Z)/0:0) could be used as a potential marker of HM. In contrast, metabolites of 1-O-(1Z-tetradecenyl)-2-(9Z-octadecenoyl)-sn-glycerol and 1,3-dihydroxy-2-propanyl (11Z,14Z)-11,14-icosadienoate were found to be potential markers of CM. Analysis using partial least square (PLS) and orthogonal PLS (OPLS) successfully predict the adulterant concentration (CM) in HM with high accuracy (R2 > 0.990). Good precision was obtained as demonstrated by the low value of root mean square error of estimation (RMSEE) and root mean square error of cross-validation (RMSECV) in both models. It can be concluded that untargeted metabolomics using UHPLC-HRMS in combination with chemometrics could be used as a powerful analytical method for horse milk authentication. [ABSTRACT FROM AUTHOR]

BACKGROUND: Atypical ageing (ATA) is an aroma defect that occurs in white wines and entails a loss of varietal aromas as well as scents of wet mop, shoe polish and dish rag. 2‐Aminoacetophenone (2AAP) – a degradation product of indole‐3‐acetic acid (IAA) – has been described as the main odour‐active compound and chemical marker responsible for this off‐flavour. A stress reaction in the vineyard triggered by climatic, pedological and viticultural factors can ultimately cause ATA development in wines and remarkably affect wine quality. The aim of this research was to investigate the influence of three grapevine management systems on the occurrence of ATA. The experiments were carried out on Pinot Blanc grape samples from vines cultivated using one conventional and two organic approaches. The management systems mainly differed for the fertilisation regime and the weed control. RESULTS: The amino acid profiles as well as 2AAP and its precursors were quantified in musts and wines using ultra‐high‐performance liquid chromatography coupled to a high‐resolution mass spectrometer. The results showed the existence of a strong vintage effect, while no influence of the use of different agronomic systems was observed. CONCLUSION: The study revealed that an efficient implementation of different grapevine production systems did not affect ATA development in Pinot Blanc wines. This finding is of great relevance for winegrowers and winemakers as it demonstrates that a well‐planned organic management system correctly adjusted to the climatic conditions does not pose a threat towards the development of ATA‐related compounds in wine. © 2022 The Authors. Journal of The Science of Food and Agriculture published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry. [ABSTRACT FROM AUTHOR]