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The natural compounds of boron have many applications, primarily as a dietary supplement. The research is based on the discovery that the diester chlorogenoborate complex can be detected and quantified from green coffee beans. The study reports that such a diester molecule can also be synthesized in a stable form via the direct reaction of boric acid and chlorogenic acid in a mixture of acetonitrile–water (1:1, v/v) and left to evaporate over a period of 48 h at room temperature, resulting in a spirocyclic form (diester complex). The diester complex, with its molecular structure and digestibility attributes, has potential application as a prebiotic in gut health and oral health, and as a micronutrient essential for microbiota in humans and animals. [ABSTRACT FROM AUTHOR]

Drugs obtained from medicinal plants have always played a pivotal role in the field of medicine and to identify novel compounds. Safety profiling of plant extracts is of utmost importance during the discovery of new biologically active compounds and the determination of their efficacy. It is imperative to conduct toxicity studies before exploring the pharmacological properties and perspectives of any plant. The present work aims to provide a detailed insight into the phytochemical and toxicological profiling of methanolic extract of Zephyranthes citrina (MEZ). Guidelines to perform subacute toxicity study (407) and acute toxicity study (425) provided by the organization of economic cooperation and development (OECD) were followed. A single orally administered dose of 2000 mg/kg to albino mice was used for acute oral toxicity testing. In the subacute toxicity study, MEZ in doses of 100, 200, and 400 mg/kg was administered orally, consecutive for 28 days. Results of each parameter were compared to the control group. In both studies, the weight of animals and their selected organs showed consistency with that of the control group. No major toxicity or organ damage was recorded except for some minor alterations in a few parameters such as in the acute study, leukocyte count was increased and decreased platelet count, while in the subacute study platelet count increased in all doses. In the acute toxicity profile liver enzymes Alanine aminotransferase (ALT), as well as, aspartate aminotransferase (AST) were found to be slightly raised while alkaline phosphatase (ALP) was decreased. In subacute toxicity profiling, AST and ALT were not affected by any dose while ALP was decreased only at doses of 200 and 400 mg/kg. Uric acid was raised at a dose of 100 mg/kg. In acute toxicity, at 2000 mg/kg, creatinine and uric acid increased while urea levels decreased. Therefore, it is concluded that the LD50 of MEZ is more than 2000 mg/kg and the toxicity profile of MEZ was generally found to be safe. [ABSTRACT FROM AUTHOR]

Drugs obtained from medicinal plants have always played a pivotal role in the field of medicine and to identify novel compounds. Safety profiling of plant extracts is of utmost importance during the discovery of new biologically active compounds and the determination of their efficacy. It is imperative to conduct toxicity studies before exploring the pharmacological properties and perspectives of any plant. The present work aims to provide a detailed insight into the phytochemical and toxicological profiling of methanolic extract of Zephyranthes citrina (MEZ). Guidelines to perform subacute toxicity study (407) and acute toxicity study (425) provided by the organization of economic cooperation and development (OECD) were followed. A single orally administered dose of 2000 mg/kg to albino mice was used for acute oral toxicity testing. In the subacute toxicity study, MEZ in doses of 100, 200, and 400 mg/kg was administered orally, consecutive for 28 days. Results of each parameter were compared to the control group. In both studies, the weight of animals and their selected organs showed consistency with that of the control group. No major toxicity or organ damage was recorded except for some minor alterations in a few parameters such as in the acute study, leukocyte count was increased and decreased platelet count, while in the subacute study platelet count increased in all doses. In the acute toxicity profile liver enzymes Alanine aminotransferase (ALT), as well as, aspartate aminotransferase (AST) were found to be slightly raised while alkaline phosphatase (ALP) was decreased. In subacute toxicity profiling, AST and ALT were not affected by any dose while ALP was decreased only at doses of 200 and 400 mg/kg. Uric acid was raised at a dose of 100 mg/kg. In acute toxicity, at 2000 mg/kg, creatinine and uric acid increased while urea levels decreased. Therefore, it is concluded that the LD50 of MEZ is more than 2000 mg/kg and the toxicity profile of MEZ was generally found to be safe.

Introduction: Luffa aegyptiaca Mill, sponge gourd or Egyptian cucumber, is grown worldwide for its edible fruit consumed as a vegetable like cucumber. Unlike young fruit (YF), the fully mature ripened fruit (MF) is strongly fibrous and is used as a cleanser to make scrubbing bath sponges. YF undergoes a complex series of physiological and biochemical changes during fruit ripening. However, the chemical compositional differences between YF and MF in Luffa aegyptiaca have not been distinguished to date. Objectives: Comprehensively compare the metabolites profile of YF and MF to give insight on how maturation stage affects chemical composition. Methods: Mass-based metabolomics comprising GC/MS and UHPLC/MS were adopted in this study targeting its volatile and non-volatile metabolites coupled with chemometrics to rationalize for the differences. Results: A total of 53 volatile metabolites were identified via headspace solid phase microextraction (SPME) comprising 66.2% aldehydes/furans, 51.6% alcohols, 38.2% ketones, 15.1% acids and 10.1% aromatics of which aldehydes/ furans were dominant at both fruit stages. Young fruit was in general more erniched in metabolites as revealed from UHPLC/MS and GC/MS analyses. The YF group encompassed higher levels of short chain alcohols (1-octen-3-ol) and aldehydes ((E)-2-hexenal and cucumber aldehyde) in addition to terpenoids (linalool). In contrast, fatty acids (octanoic acid) predominated MF specimens. UHPLC/MS analysis revealed for several oleanene triterpene glycosides as major secondary bioactive compounds, dihydroxy-oxo-oleanenoic acid glycoside found more abundant in YF versus MF as revealed from multivariate data analyses. Conclusions: Our results reveal for the distinct metabolite changes in L. aegyptiaca fruit in its different stages and to rationalize for its different usage.

The natural compounds of boron have many applications, primarily as a dietary supplement. The research is based on the discovery that the diester chlorogenoborate complex can be detected and quantified from green coffee beans. The study reports that such a diester molecule can also be synthesized in a stable form via the direct reaction of boric acid and chlorogenic acid in a mixture of acetonitrile–water (1:1, v/v) and left to evaporate over a period of 48 h at room temperature, resulting in a spirocyclic form (diester complex). The diester complex, with its molecular structure and digestibility attributes, has potential application as a prebiotic in gut health and oral health, and as a micronutrient essential for microbiota in humans and animals.

Coffee is a popular beverage owing to its unique flavor and diverse health benefits. The current study aimed at investigating the antioxidant activity, in relation to the phytochemical composition, of authenticated Brazilian green and roasted Coffea arabica and C. robusta, along with 15 commercial specimens collected from the Middle East. Ultra-high-performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-ESI–HRMS) and UV spectrometry were employed for profiling and fingerprinting, respectively. With the aid of global natural product social molecular networking (GNPS), a total of 88 peaks were annotated as belonging to different chemical classes, of which 11 metabolites are reported for the first time in coffee seeds. Moreover, chemometric tools showed comparable results between both platforms, with more advantages for UV in the annotation of roasting products, suggesting that UV can serve as a discriminative tool. Additionally, antioxidant assays coupled with the UHPLC-ESI–HRMS dataset using partial least-squares discriminant analysis (PLS-DA) demonstrated that caffeoylquinic acid and caffeine were potential antioxidant markers in unroasted coffee versus dicaffeoyl quinolactone and melanoidins in roasted coffee. The study presents a multiplex metabolomics approach to the quality control of coffee, one of the most consumed beverages. [ABSTRACT FROM AUTHOR]

Differences in the components of the crude drug Saposhnikoviae radix, both wild and cultivated, and the cultivation duration were examined by UHPLC/MS. As a result, there was no significant difference in composition depending on the region in China where the drug was produced. The most abundant components in all samples were prim-O-glucosylcimifugin, 4′-O-glucosyl-5-O-methylvisamminol, 3′-O-acetylhamaudol and cimifugin. The 1 year-old Saposhnikoviae radix cultivated in Japan had a low component content overall. A comparison of components according to root thickness revealed that glycosides, such as prim-O-glucosylcimifugin and 4'-O-glucosyl-5-O-methylvisamminol, were accumulated in thin roots. In a comparison of the components according to the drying temperature, a large difference was observed in the content of glycosides, and a difference was observed depending on the sugar-binding position. According to a metabolome analysis in domestic commercial products by LC/MS, a characteristic component in the cultivated product was found and its content was low in the 1 year-old sample and high in the 2 year-old sample. If the cultivation duration is prolonged up to about 6 years, the contents of the ingredients are close to those of wild products. [ABSTRACT FROM AUTHOR]

[Display omitted] Luffa aegyptiaca Mill, sponge gourd or Egyptian cucumber, is grown worldwide for its edible fruit consumed as a vegetable like cucumber. Unlike young fruit (YF), the fully mature ripened fruit (MF) is strongly fibrous and is used as a cleanser to make scrubbing bath sponges. YF undergoes a complex series of physiological and biochemical changes during fruit ripening. However, the chemical compositional differences between YF and MF in Luffa aegyptiaca have not been distinguished to date. Comprehensively compare the metabolites profile of YF and MF to give insight on how maturation stage affects chemical composition. Mass-based metabolomics comprising GC/MS and UHPLC/MS were adopted in this study targeting its volatile and non-volatile metabolites coupled with chemometrics to rationalize for the differences. A total of 53 volatile metabolites were identified via headspace solid phase microextraction (SPME) comprising 66.2% aldehydes/furans, 51.6% alcohols, 38.2% ketones, 15.1% acids and 10.1% aromatics of which aldehydes/ furans were dominant at both fruit stages. Young fruit was in general more erniched in metabolites as revealed from UHPLC/MS and GC/MS analyses. The YF group encompassed higher levels of short chain alcohols (1-octen-3-ol) and aldehydes ((E)-2-hexenal and cucumber aldehyde) in addition to terpenoids (linalool). In contrast, fatty acids (octanoic acid) predominated MF specimens. UHPLC/MS analysis revealed for several oleanene triterpene glycosides as major secondary bioactive compounds, dihydroxy-oxo-oleanenoic acid glycoside found more abundant in YF versus MF as revealed from multivariate data analyses. Our results reveal for the distinct metabolite changes in L. aegyptiaca fruit in its different stages and to rationalize for its different usage. [ABSTRACT FROM AUTHOR]

Verbena litoralis is a plant popularly known as “gervãozinho-do-campo” in Portuguese. It is traditionally used for stomach, liver and gallbladder problems, and as an anti-inflammatory and anthelmintic. The goal of this study was to determine the chemical composition of the crude extract obtained from the aerial parts of V. litoralis by Ultra High Performance Liquid chromatography coupled with Mass Spectrometry in Tandem (UHPLC-MS/MS); assess the anti-inflammatory activity of ethyl acetate fraction and of crude extract; and verify liver, kidney and pancreas damage. In this study, the chemical composition of the extract was identified via UHPLC/MS/MS, assessing the anti-inflammatory activity of the crude extract and the acetate fraction in an induction model of the granulomatous tissue, as well as given liver, kidney and pancreas damage markers. Chlorogenic acid, luteolin, caffeic acid, apigenin, p-coumaric acid, vanillic acid, ferulic acid and quercetin were quantified in the extract. After the seven-day treatment, the granuloma of the animals treated with the plant extract and fraction presented values very close to the positive control (nimesulide). The V. litoralis crude extract and ethyl acetate fraction show anti-inflammatory activity similar to the nimesulide without evidence of liver, kidney and pancreas damage, which attributes the plant’s pharmacological action to the flavonoids found.

Coffee is a popular beverage owing to its unique flavor and diverse health benefits. The current study aimed at investigating the antioxidant activity, in relation to the phytochemical composition, of authenticated Brazilian green and roasted Coffea arabica and C. robusta, along with 15 commercial specimens collected from the Middle East. Ultra-high-performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-ESI–HRMS) and UV spectrometry were employed for profiling and fingerprinting, respectively. With the aid of global natural product social molecular networking (GNPS), a total of 88 peaks were annotated as belonging to different chemical classes, of which 11 metabolites are reported for the first time in coffee seeds. Moreover, chemometric tools showed comparable results between both platforms, with more advantages for UV in the annotation of roasting products, suggesting that UV can serve as a discriminative tool. Additionally, antioxidant assays coupled with the UHPLC-ESI–HRMS dataset using partial least-squares discriminant analysis (PLS-DA) demonstrated that caffeoylquinic acid and caffeine were potential antioxidant markers in unroasted coffee versus dicaffeoyl quinolactone and melanoidins in roasted coffee. The study presents a multiplex metabolomics approach to the quality control of coffee, one of the most consumed beverages.

The ultrahigh-performance liquid chromatography-mass spectrometry (UHPLC/MS) method was optimized and validated for the determination of oxylipins in human plasma using the targeted approach with selected reaction monitoring (SRM) in the negative-ion electrospray ionization (ESI) mode. Reversed phase UHPLC separation on an octadecylsilica column enabled the analysis of 63 oxylipins including numerous isomeric species within 12-min run time. The method was validated (calibration curve, linearity, limit of detection, limit of quantification, carry-over, precision, accuracy, recovery rate, and matrix effect) and applied to 40 human female plasma samples from breast cancer patients and age-matched healthy volunteers (control). Thirty-six oxylipins were detected in human plasma with concentrations above the limit of detection, and 21 of them were quantified with concentrations above the limit of quantitation. The concentrations determined in healthy controls are in a good agreement with previously reported data on human plasma. Quantitative data were statistically evaluated by multivariate data analysis (MDA) methods including principal component analysis (PCA) and orthogonal partial least square discriminant analysis (OPLS-DA). S-plot and box plots showed that 13-HODE, 9-HODE, 13-HOTrE, 9-HOTrE, and 12-HHTrE were the most upregulated oxylipin species in plasma of breast cancer patients. [ABSTRACT FROM AUTHOR]

Abstract: α‐Glucosidases have been a major target in controlling and managing postprandial blood glucose and therefore diabetes treatment. This study aims to further identify and purify active compounds from the most active ethyl acetate fraction collected previously in Tinta Cão grape pomace extract (TCEE) using a newly developed and highly effective immobilization method, including obtaining compounds previously shown to inhibit the enzyme. Purification used crosslinked chitosan beads with α‐glucosidases bound to polymer, which acted as immobilized enzyme vehicle to collect inhibitors. Compounds absorbed into the beads were eluded using methanol, where collected fraction was subjected to UHPLC‐MS analysis to identify active compounds. Results presented 5 major compounds: viniferifuran (amurensin H), p‐coumaroyl‐6‐O‐D‐glucopyranoside, p‐coumaroyl‐6‐O‐hexoside, (epi)catechin‐hexoside, 10‐carboxyl‐pyranopeonidin 3‐O‐(6′′‐O‐p‐coumaroyl)‐glucoside. These findings indicated the particular molecules can be utilized as potent α‐glucosidases inhibitors, and may be further tested for postprandial glucose control. Practical Application: A potential approach enriched and identified α‐glucosidase inhibitors of grape pomace. Set‐up of UHPLC/MS detection and identification of active compounds provide qualify assessment in developing grape pomace extract into potent dietary supplement and new drug for diabetes. [ABSTRACT FROM AUTHOR]

Olive mill by-products are effluents generated during olive oil production process. The two-phase centrifugation system produces a semi-solid olive pomace called "alperujo." This by-product is a combination of liquid and solid wastes derived from the three-phase manufacturing process. A direct and fast analytical method by ultra-high-pressure liquid chromatography-DAD coupled with ESI/MS-MS has been developed for the profiling of phenolic compounds. Thirtyfive metabolites belonging to phenyl alcohols, secoiridoids, flavonoids, and iridoids were identified as the main constituents of alperujo in 12 min, including p-coumaroyl aldarate and a verbascoside derivative found for the first time in alperujo and a new ligstroside derivative. Six quantitatively significant components were determined at concentrations ranging from 17.7 mg/L for p-coumaric acid to 370.7 mg/L for hydroxytyrosol. Our data confirm that alperujo is an interesting source of phenolic compounds that could be extracted for use as nutraceuticals. [ABSTRACT FROM AUTHOR]

Neurotransmitters, small molecules widely distributed in the central nervous system are essential in transmitting electrical signals across neurons via chemical communication. Dysregulation of these chemical signaling molecules is linked to numerous neurological diseases including tauopathies. In this study, a precise and reliable liquid chromatography method was established with tandem mass spectrometry detection for the simultaneous determination of aspartic acid, asparagine, glutamic acid, glutamine, γ-aminobutyric acid, N-acetyl- l -aspartic acid, pyroglutamic acid, acetylcholine and choline in human brain tissue. The method was successfully applied to the analysis of human brain tissues from three different tauopathies; corticobasal degeneration, progressive supranuclear palsy and parkinsonism-dementia complex of Guam. Neurotransmitters were analyzed on ultra-high performance chromatography (UHPLC) using an ethylene bridged hybrid amide column coupled with tandem mass spectrometry (MS/MS). Identification and quantification of neurotransmitters was carried out by ESI+ mass spectrometry detection. We optimized sample preparation to achieve simple and fast extraction of all nine analytes. Our method exhibited an excellent linearity for all analytes (all coefficients of determination >0.99), with inter-day and intra-day precision yielding relative standard deviations 3.2%–11.2% and an accuracy was in range of 92.6%–104.3%. The present study, using the above method, is the first to demonstrate significant alterations of brain neurotransmitters caused by pathological processes in the brain tissues of patient with three different tauopathies. [ABSTRACT FROM AUTHOR]

• Flavonoids identified in Ochradenus baccatus were mainly O -glycosides of quercetin. • Two glucosinolates and three nitrile-containing glycosides were among identified compounds. • O. baccatus is enriched in hydroxylated fatty acids with C16 and C18 chains. • O. baccatus extract showed significant and selective antineoplastic activity against HeLa cells (CC 50 39.1 µg/mL). Ochradenus baccatus Delile (Resedaceae) is a desert plant with edible fruits native to the Middle East. Few investigators have reported antibacterial, antiparasitic and anti-cancer activities of the plant. Herein we evaluated the cytotoxic activity of O. baccatus using four cell lines and a zebrafish embryo model. Additionally, liquid chromatography coupled with mass spectroscopy was performed to characterize the extract's main constituents. The highest cytotoxicity was observed against human cervical adenocarcinoma (HeLa), with CC 50 of 39.1 µg/mL and a selectivity index (SI) of 7.23 (p < 0.01). Metabolic analysis of the extract resulted in the annotation of 57 metabolites, including fatty acids, flavonoids, glucosinolates, nitrile glycosides, in addition to organic acids. The extract showed an abundance of hydroxylated fatty acids (16 peaks). Further, 3 nitrile glycosides have been identified for the first time in Ochradenus sp., in addition to 2 glucosinolates. These identified phytochemicals may partially explain the cytotoxic activity of the extract. We propose O. baccatus as a possible safe food source for further utilization to partially contribute to the increasing food demand specially in Saharan countries. [ABSTRACT FROM AUTHOR]

The potential of ultrahigh-performance liquid chromatography–mass spectrometry (UHPLC/MS) and ultrahigh-performance supercritical fluid chromatography (UHPSFC) coupled to negative-ion electrospray ionization mass spectrometry (ESI–MS) for the analysis of 46 oxylipins and 2 fatty acid standards is compared in terms of their chromatographic resolution with the emphasis on distinguishing isobaric interferences and the method sensitivity. UHPLC provides the baseline separation of 24 isobaric oxylipins within 13 min, while UHPSFC enables the separation of only 20 isobaric oxylipins within 8 min. Moreover, the UHPLC/ESI–MS method provides an average improvement of sensitivity by 3.5-fold. A similar trend is observed in the analysis of human plasma samples, but lower ion suppression effects caused by lysophospholipids (LPL) are observed in case of UHPSFC/ESI–MS due to better separation of LPL. Both methods are fully applicable for the analysis of oxylipins, but UHPLC/ESI–MS method is preferred due to better separation and higher sensitivity, which results in the identification of 31 oxylipins in human plasma based on available standards and additional tentative 20 identifications based on accurate m / z values and the fragmentation behavior known from the literature. [ABSTRACT FROM AUTHOR]

Ethnopharmacological relevance Dolichandra unguis-cati L. is a native climbing plant of Brazil, popularly known as “unha de gato”. It has been traditionally used mainly as an antipyretic, anti-inflammatory and anti-tumor agent, yet little toxicological information is found in the literature. Aim of the study To identify the chemical composition of the hydroethanolic extract obtained from the leaves of Dolichandra uniguis-cati and to evaluate the acute and subacute toxicity in male and female rats, in order to assess the safety profile of this plant. Materials and methods In the acute study, a single dose (2000 mg/kg) of the extract was orally administered to male and female rats. In the subacute study, the extract was orally administered to male and female rats at doses 100, 200 and 400 mg/kg for 28 days. Behavioral changes, catalase and tbars evaluations, biochemical, hematological and histopathological analysis were determined. The extract’ chemical composition was accessed through UHPLC/MS. Results Chlorogenic acid, caffeic acid, ferulic acid, vanillinic acid, p-coumaric acid, rosmarinic acid, trans -cinnamic acid, luteolin, apigenin, quercitrin and quercetin were identified in the extract. In the acute treatment, the extract was classified as safe (category 5), according to the OECD guide. In relation to the subacute study, females showed a reduction in AST (100, 200 and 400 mg/kg), ALT (200 mg/kg) and BUN (100 and 200 mg/kg) levels, while male rats 400 mg/kg presented an increase in AST levels. The Chol dosage significantly decreased in female rats in a dose-dependent manner, whereas for male rats this parameter showed no statistically significant reductions. No behavioral and histopathological changes were recorded. Conclusions Our results indicate that the hydroethanolic extract of Dolichandra unguis-cati leaves did not present relevant toxic effects when administered orally to male and female rats. The extract also showed a potential hypocholesterolemic activity. [ABSTRACT FROM AUTHOR]

Liquid chromatography coupled with mass spectrometry is an outstanding methodology for fast analysis of phenolic compounds in biological samples. Twenty two compounds were quickly and accurately identified in the methanolic extract of the Antarctic lichen Ramalina terebrata for the first time using ultra high pressure liquid chromatography coupled with photodiode array detector and high resolution mass spectrometry (UHPLC-PDA- Q/Orbitrap/MS/MS). In addition, the extract and the four compounds isolated from this species were tested for the inhibitory activity of tau protein aggregation, which is a protein involved in Alzheimer's disease (AD). All compounds showed null activity with the exception of parietin, which it was able to inhibit aggregation process of tau in a concentration range between 3 µg/mL (10 µM) to 28 µg/mL (100 µM). In addition, we show how parietin interact with tau 306VQIVYK311 hexapeptide inside of the microtubule binding domain (4R) with the help of molecular docking experiments. Finally, the constituents present in the methanolic extract could possibly contribute to the established anti- aggregation activity for this extract and this in-depth analysis of the chemical composition of R. terebrata could guide further research into its medicinal properties and potential uses. [ABSTRACT FROM AUTHOR]

Differences among lipidomic profiles of healthy volunteers, obese people and three groups of cardiovascular disease (CVD) patients are investigated with the goal to differentiate individual groups based on the multivariate data analysis (MDA) of lipidomic data from plasma, erythrocytes and lipoprotein fractions of more than 50 subjects. Hydrophilic interaction liquid chromatography on ultrahigh-performance liquid chromatography (HILIC-UHPLC) column coupled with electrospray ionization mass spectrometry (ESI-MS) is used for the quantitation of four classes of polar lipids (phosphatidylethanolamines, phosphatidylcholines, sphingomyelins and lysophosphatidylcholines), normal-phase UHPLC—atmospheric pressure chemical ionization MS (NP-UHPLC/APCI-MS) is applied for the quantitation of five classes of nonpolar lipids (cholesteryl esters, triacylglycerols, sterols, 1,3-diacylglycerols and 1,2-diacylglycerols) and the potential of matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) is tested for the fast screening of all lipids without a chromatographic separation. Obtained results are processed by unsupervised (principal component analysis) and supervised (orthogonal partial least squares) MDA approaches to highlight the largest differences among individual groups and to identify lipid molecules with the highest impact on the group differentiation. [ABSTRACT FROM AUTHOR]

• B-type procyanidin dimer and new catechin dimeric oxidation products were analyzed. • Depending on dimer type (B, C O C or C C), specific mass fragments were obtained. • 3 oxidation markers were identified in seeds with an increasing trend with ripening. • 3 oxidation markers were identified in wines with a decreasing trend with ageing. B-type procyanidin dimers and (+)-catechin dimeric oxidation products were analyzed in grape seed extracts and red wines (UHPLC-Q-Orbitrap MS). The different dimers had different fragmentation patterns according to their interflavan linkage position. Oxidation dimeric compounds had a specific fragment ion at m / z 393, missing for B-Type dimers fragmentations. A fragment ion at m / z 291 occurred and was specific for oxidation dimeric compounds with a C O C linkage. Higher level oxidation products had abundant specific fragments: m / z 425, 397 and 245. These fragmentations were useful to identify them in complex samples such as grape seed extracts and wines. Three grape varieties and three ripening stages were selected and the corresponding seed extracts were obtained. The analyses revealed an increasing trend for the oxidation markers during grape ripening. The analysis of Syrah wines (2018, 2014, 2010) showed a decreasing trend of these molecules during wine ageing which might be due to further oxidation. [ABSTRACT FROM AUTHOR]

Liquid chromatography coupled with mass spectrometry is an outstanding methodology for fast analysis of phenolic compounds in biological samples. Twenty two compounds were quickly and accurately identified in the methanolic extract of the Antarctic lichen Ramalina terebrata for the first time using ultra high pressure liquid chromatography coupled with photodiode array detector and high resolution mass spectrometry (UHPLC-PDA-Q/Orbitrap/MS/MS). In addition, the extract and the four compounds isolated from this species were tested for the inhibitory activity of tau protein aggregation, which is a protein involved in Alzheimer’s disease (AD). All compounds showed null activity with the exception of parietin, which it was able to inhibit aggregation process of tau in a concentration range between 3 µg/mL (10 µM) to 28 µg/mL (100 µM). In addition, we show how parietin interact with tau 306VQIVYK311 hexapeptide inside of the microtubule binding domain (4R) with the help of molecular docking experiments. Finally, the constituents present in the methanolic extract could possibly contribute to the established anti-aggregation activity for this extract and this in-depth analysis of the chemical composition of R. terebrata could guide further research into its medicinal properties and potential uses.

Drugs obtained from medicinal plants have always played a pivotal role in the field of medicine and to identify novel compounds. Safety profiling of plant extracts is of utmost importance during the discovery of new biologically active compounds and the determination of their efficacy. It is imperative to conduct toxicity studies before exploring the pharmacological properties and perspectives of any plant. The present work aims to provide a detailed insight into the phytochemical and toxicological profiling of methanolic extract of Zephyranthes citrina (MEZ). Guidelines to perform subacute toxicity study (407) and acute toxicity study (425) provided by the organization of economic cooperation and development (OECD) were followed. A single orally administered dose of 2000 mg/kg to albino mice was used for acute oral toxicity testing. In the subacute toxicity study, MEZ in doses of 100, 200, and 400 mg/kg was administered orally, consecutive for 28 days. Results of each parameter were compared to the control group. In both studies, the weight of animals and their selected organs showed consistency with that of the control group. No major toxicity or organ damage was recorded except for some minor alterations in a few parameters such as in the acute study, leukocyte count was increased and decreased platelet count, while in the subacute study platelet count increased in all doses. In the acute toxicity profile liver enzymes Alanine aminotransferase (ALT), as well as, aspartate aminotransferase (AST) were found to be slightly raised while alkaline phosphatase (ALP) was decreased. In subacute toxicity profiling, AST and ALT were not affected by any dose while ALP was decreased only at doses of 200 and 400 mg/kg. Uric acid was raised at a dose of 100 mg/kg. In acute toxicity, at 2000 mg/kg, creatinine and uric acid increased while urea levels decreased. Therefore, it is concluded that the LD 50 of MEZ is more than 2000 mg/kg and the toxicity profile of MEZ was generally found to be safe., Competing Interests: The authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest., (Copyright © 2022 Rehman, Saleem, Ahmad and Rashid.)

Abstract: Metabolomics is a new approach based on the systematic study of the full complement of small molecular metabolites in a biological sample. It could map the perturbations of early biochemical changes on diseases and hence provides an opportunity to develop predictive biomarkers that can result in earlier intervention and possess valuable insights into the mechanisms of diseases. Given the poor diagnosis of myocardial ischemia syndrome (heart-qi deficiency, HQD), biomarkers of great significance are urgently needed. Fortunately, metabolomics may offer the possibility of identifying marker metabolites and pathways activated in HQD. This paper was designed to explore globally metabolomics characters of the HQD and the therapeutic effects of traditional Chinese medicine Wen-Xin-Formula (WXF). Serum biochemical analysis and histopathological examinations were simultaneously performed. Global metabolic profiling with UHPLC/MS (ultra high-performance liquid chromatography–mass spectrometry), multivariate analysis and database searching were performed to discover differentiating metabolites. Seventeen biomarkers were identified and pathway analysis tools suggest that the glycolysis or gluconeogenesis metabolism, biosynthesis of unsaturated fatty acids metabolism, fatty acid biosynthesis and purine metabolism networks were acutely perturbed by HQD. Of note, WXF has potential pharmacological effect through regulating multiple perturbed pathways to normal state, correlates well to the assessment of biochemistry and histopathological assay. Overall, this study successfully demonstrated that the power of metabolomics in unraveling protective effects of WXF and these findings may help better understand the mechanisms of disease, and the underlying pathophysiologic processes. [Copyright &y& Elsevier]

The methanolic extract of the stem bark of a wild species of jujube, Ziziphus lotus (L.) Lam., growing in Sicily, was chemically and biologically investigated. The chemical profile was defined by UHPLC-HR-ESI-Orbitrap/MS analysis whereas antioxidant and tyrosinase inhibitory activities were investigated by in vitro assays. The extract showed a high total phenolic and flavonoid content (TPC=271.65 GAE/g and TFC=188.11 RE/g extract). Metabolomic analysis revealed a rich phytocomplex characterized by phenols, cyclopeptide alkaloids, and triterpenoid saponins, some of which here detected for the first time. The mushroom tyrosinase inhibition assay displayed that the methanolic extract efficiently inhibits the monophenolase and diphenolase activity. Furthermore, the extract showed a strong ability to scavenge DPPH, a good Fe 3+ reducing antioxidant power, in addition to a Fe 2+ chelating activity. Taken together, these results suggest possible novel applications of wild jujube stem bark as a source of potential skin-care agents with several uses in pharmaceutical and cosmetic industries., (© 2022 The Authors. Chemistry & Biodiversity published by Wiley-VHCA AG, Zurich, Switzerland.)

• This study provides the first metabolome map for Egyptian olive fruits. • 201 Metabolites were identified including both primary and secondary metabolites. • 10 Secoiridoids are first time to be reported in fresh and pickled olive fruits. • Specific markers mainly secoiridoids and/or sugars were revealed for olive varieties. • Changes in phenolics, secoiridoids, sugars were markers of pickled olives. The role of variety and effects of pickling on Egyptian olive fruit metabolome was determined using mass spectrometry-based metabolomics targeting nutrients and bioactive metabolities. The analyzed fresh olive fruit varieties included Manzanilo, Picual, Koroneiki, and Coratina, while the pickled samples included the Manzanilo and Picual varieties. Profiling of primary and secondary metabolites resulted in the detection of 201 metabolites. Variation between varieties was mostly observed among sugars, sugar alcohols, secoiridoids, and flavonoids. An abundance of carbohydrates and O -glycosides in Picual and Manzanilo versus enrichment of secoiridoids in Picual and Coratina olives viz. dehyro-oleuropein could account for the difference in palatability and health benefits among varieties. Herein, 13 new compounds are reported in the tested varieties, of which 10 appeared exclusively in pickled samples. Generally, pickled samples were characterized by the relative abundance of secoiridoids regarded as important markers for the pickling process. Metabolites profiling provided greater insight into the pickling process as a preservation method and accounted for the improved organoleptic characters in pickled fruits. [ABSTRACT FROM AUTHOR]

Introduction: Luffa aegyptiaca Mill, sponge gourd or Egyptian cucumber, is grown worldwide for its edible fruit consumed as a vegetable like cucumber. Unlike young fruit (YF), the fully mature ripened fruit (MF) is strongly fibrous and is used as a cleanser to make scrubbing bath sponges. YF undergoes a complex series of physiological and biochemical changes during fruit ripening. However, the chemical compositional differences between YF and MF in Luffa aegyptiaca have not been distinguished to date., Objectives: Comprehensively compare the metabolites profile of YF and MF to give insight on how maturation stage affects chemical composition., Methods: Mass-based metabolomics comprising GC/MS and UHPLC/MS were adopted in this study targeting its volatile and non-volatile metabolites coupled with chemometrics to rationalize for the differences., Results: A total of 53 volatile metabolites were identified via headspace solid phase microextraction (SPME) comprising 66.2% aldehydes/furans, 51.6% alcohols, 38.2% ketones, 15.1% acids and 10.1% aromatics of which aldehydes/ furans were dominant at both fruit stages. Young fruit was in general more erniched in metabolites as revealed from UHPLC/MS and GC/MS analyses. The YF group encompassed higher levels of short chain alcohols (1-octen-3-ol) and aldehydes ((E)-2-hexenal and cucumber aldehyde) in addition to terpenoids (linalool). In contrast, fatty acids (octanoic acid) predominated MF specimens. UHPLC/MS analysis revealed for several oleanene triterpene glycosides as major secondary bioactive compounds, dihydroxy-oxo-oleanenoic acid glycoside found more abundant in YF versus MF as revealed from multivariate data analyses., Conclusions: Our results reveal for the distinct metabolite changes in L. aegyptiaca fruit in its different stages and to rationalize for its different usage., Competing Interests: 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., (© 2020 The Authors. Published by Elsevier B.V. on behalf of Cairo University.)

The potential of ultrahigh-performance liquid chromatography-mass spectrometry (UHPLC/MS) and ultrahigh-performance supercritical fluid chromatography (UHPSFC) coupled to negative-ion electrospray ionization mass spectrometry (ESI-MS) for the analysis of 46 oxylipins and 2 fatty acid standards is compared in terms of their chromatographic resolution with the emphasis on distinguishing isobaric interferences and the method sensitivity. UHPLC provides the baseline separation of 24 isobaric oxylipins within 13min, while UHPSFC enables the separation of only 20 isobaric oxylipins within 8min. Moreover, the UHPLC/ESI-MS method provides an average improvement of sensitivity by 3.5-fold. A similar trend is observed in the analysis of human plasma samples, but lower ion suppression effects caused by lysophospholipids (LPL) are observed in case of UHPSFC/ESI-MS due to better separation of LPL. Both methods are fully applicable for the analysis of oxylipins, but UHPLC/ESI-MS method is preferred due to better separation and higher sensitivity, which results in the identification of 31 oxylipins in human plasma based on available standards and additional tentative 20 identifications based on accurate m/z values and the fragmentation behavior known from the literature., (Copyright © 2017 Elsevier B.V. All rights reserved.)