Assessment of metabolome diversity in black and white pepper in response to autoclaving using MS- and NMR-based metabolomics and in relation to its remote and direct antimicrobial effects against food-borne pathogens.

Piper nigrum L. (black and white peppercorn) is one of the most common culinary spices used worldwide. The current study aims to dissect pepper metabolome using 1H-NMR targeting of its major primary and secondary metabolites. Eighteen metabolites were identified with piperine detected in black and white pepper at 20.2 and 23.9 µg mg-1, respectively. Aroma profiling using HS-SPME coupled to GC-MS analysis and in the context of autoclave treatment led to the detection of a total of 52 volatiles with an abundance of ß-caryophyllene at 82% and 59% in black and white pepper, respectively. Autoclaving of black and white pepper revealed improvement of pepper aroma as manifested by an increase in oxygenated compounds' level. In vitro remote antimicrobial activity against food-borne Gram-positive and Gram-negative bacteria revealed the highest activity against P. aeruginosa (VP-MIC 16.4 and 12.9 mg mL-1) and a direct effect against Enterobacter cloacae at ca. 11.6 mg mL-1 for both white and black pepper.

Comparison of autoclaving and γ-radiation impact on four spices aroma profiles and microbial load using HS-SPME GC-MS and chemometric tools.

Herbal spices are widely consumed as food additives owing to their distinct aroma and taste as well as a myriad of economic and health value. The aroma profile of four major spices including bay leaf, black pepper, capsicum, and fennel was tested using HS-SPME/GC-MS and in response to the most widely used spices´ processing methods including autoclaving and γ-radiation at low and high doses. Additionally, the impact of processing on microbial contamination of spices was tested using total aerobic count. GC-MS analysis led to the identification of 22 volatiles in bay leaf, 34 in black pepper, 23 in capsicum, and 24 in fennel. All the identified volatiles belonged to oxides/phenols/ethers, esters, ketones, alcohols, sesquiterpene and monoterpene hydrocarbons. Oxides/phenol/ethers were detected at high levels in all tested spices at ca. 44, 28.2, 48.8, 61.1%, in bay leaves, black pepper, capsicum, and fennel, respectively of the total blend and signifying their typical use as spices. Total oxides/phenol/ethers showed an increase in bay leaf upon exposure to γ-radiation from 44 to 47.5%, while monoterpene hydrocarbons were enriched in black pepper upon autoclaving from 11.4 in control to reach 65.9 and 82.6% for high dose and low dose of autoclaving, respectively. Cineole was detected in bay leaf at 17.9% and upon exposure to autoclaving at high dose and γ-radiation (both doses) its level increased by 29-31%. Both autoclaving and γ-radiation distinctly affected aroma profiles in examined spices. Further, volatile variations in response to processing were assessed using multivariate data analysis (MVA) revealing distinct separation between autoclaved and γ-radiated samples compared to control. Both autoclaving at 115 °C for 15 min and radiation at 10 kGy eliminated detected bioburden in all tested spices i.e., reduced the microbial counts below the detection limit (< 10 cfu/g).

Comparison of Balanites aegyptiaca parts: metabolome providing insights into plant health benefits and valorization purposes as analyzed using multiplex GC-MS, LC-MS, NMR-based metabolomics, and molecular networking.

Balanites aegyptiaca (L.) Delile (Zygophyllaceae), also known as the desert date, is an edible fruit-producing tree popular for its nutritional and several health benefits. In this study, multi-targeted comparative metabolic profiling and fingerprinting approaches were conducted for the assessment of the nutrient primary and secondary metabolite heterogeneity in different parts, such as leaves, stems, seeds, unripe, and ripe fruits of B. aegyptiaca using nuclear magnetic resonance (NMR), ultra-performance liquid chromatography (UPLC-MS), and gas chromatography mass-spectrometry (GC-MS) based metabolomics coupled to multivariate analyses and in relation to its cytotoxic activities. NMR-based metabolomic study identified and quantified 15 major primary and secondary metabolites belonging to alkaloids, saponins, flavonoids, sugars, and amino and fatty acids. Principal component analysis (PCA) of the NMR dataset revealed α-glucose, sucrose, and isorhamnetin as markers for fruit and stem and unsaturated fatty acids for predominated seeds. Orthogonal projections to latent structure discriminant analysis (OPLS-DA) revealed trigonelline as a major distinctive metabolite in the immature fruit and isorhamnetin as a major distinct marker in the mature fruit. UPLC-MS/MS analysis using feature-based molecular networks revealed diverse chemical classes viz. steroidal saponins, N-containing metabolites, phenolics, fatty acids, and lipids as the constitutive metabolome in Balanites. Gas chromatography-mass spectroscopy (GC-MS) profiling of primary metabolites led to the detection of 135 peaks belonging to sugars, fatty acids/esters, amino acids, nitrogenous, and organic acids. Monosaccharides were detected at much higher levels in ripe fruit and disaccharides in predominate unripe fruits, whereas B. aegyptiaca vegetative parts (leaves and stem) were rich in amino acids and fatty acids. The antidiabetic compounds, viz, nicotinic acid, and trigonelline, were detected in all parts especially unripe fruit in addition to the sugar alcohol d-pinitol for the first time providing novel evidence for B. aegyptiaca use in diabetes. In vitro cytotoxic activity revealed the potential efficacy of immature fruit and seeds as cytotoxic agents against human prostate cancer (PC3) and human colorectal cancer (HCT-116) cell lines. Collectively, such detailed profiling of parts provides novel evidence for B. aegyptiaca medicinal uses.

Dissecting the role of microorganisms in tea production of different fermentation levels: a multifaceted review of their action mechanisms, quality attributes and future perspectives.

Tea is one of the most popular beverages worldwide, with several health benefits attributed for its rich chemical composition and further associated with fermentation process to improve its quality attributes. Most tea types originate from the leaves of Camellia sinensis with differences in fermentation levels yielding black tea, green tea, pouchong tea, oolong tea. Teas like pu-erh or kombucha to encompass both green and red types are further post-fermented. Tea fermentation is a traditional process involving physical, biochemical, and microbial changes which are associated with improved organoleptic characters, nutritive value, and health outcomes. The production of fermented tea relies on naturally occurring enzymes and microbial metabolic activities. This review focuses on presenting a holistic overview on the effect of different microorganisms including bacteria, yeast, and fungi on the biochemical changes and sensory attributes of fermented tea products reported in research articles along the last 15 years. Moreover, production conditions and major biochemical changes are dissected to present the best factors influencing fermented tea quality. This review presents an evidence-based reference for specialists in tea industry to optimize tea fermentation process for targeted attributes.

Bee Pollen and Bread as a Super-Food: A Comparative Review of Their Metabolome Composition and Quality Assessment in the Context of Best Recovery Conditions.

Recently, functional foods have been a subject of great interest in dietetics owing not only to their nutritional value but rather their myriad of health benefits. Moreover, an increase in consumers' demands for such valuable foods warrants the development in not only production but rather tools of quality and nutrient assessment. Bee products, viz., pollen (BP) and bread, are normally harvested from the flowering plants with the aid of bees. BP is further subjected to a fermentation process in bee hives to produce the more valuable and bioavailable BB. Owing to their nutritional and medicinal properties, bee products are considered as an important food supplements rich in macro-, micro-, and phytonutrients. Bee products are rich in carbohydrates, amino acids, vitamins, fatty acids, and minerals in addition to a myriad of phytonutrients such as phenolic compounds, anthocyanins, volatiles, and carotenoids. Moreover, unsaturated fatty acids (USFAs) of improved lipid profile such as linoleic, linolenic, and oleic were identified in BP and BB. This work aims to present a holistic overview of BP and BB in the context of their composition and analysis, and to highlight optimized extraction techniques to maximize their value and future applications in nutraceuticals.

Phytochemical investigation of Ludwigia adscendens subsp. diffusa aerial parts in context of its biological activity.

Ludwigia adscendens subsp. diffusa (Onagraceae), an important aquatic herb widely distributed in the Nile River and canals in Egypt. The goal of the current study is to investigate the phytochemical composition of L. adscendens aerial parts n-butanol and ethyl acetate fractions and screening of its biological activities. Phytochemical investigation of L. adscendens resulted in the isolation and purification of eleven compounds belonging to flavonoids, saponins, triterpenoids, and oligosaccharides, of which one compound was identified as new using different spectroscopic techniques. Compound 2 was identified as a new compound namely, 3-O-[ß-D-glucopyranoside (1 → 4) α-L-rhamnopyranoside]-23-O-feruloyl-hederagenin-28-O-[α-L-rhamnopyranoside (1 → 2) ß-D-glucopyranoside], along with other 10 well know compounds. Furthermore, antidiabetic, hepatoprotective and cytotoxic activities of n-butanol and ethyl acetate fractions were investigated in vitro, revealing that ethyl acetate fraction was the most active as antidiabetic (IC50 = 62.3 µg/mL), hepatoprotective (IC50 = 80.75 µg/mL), and cytotoxic against human prostate cancer cell line (IC50 = 52.2 µg/mL). Collectively, L. adscendens aerial part is rich with a myriad of phytochemicals with potential health benefits.

Insoluble dietary fibers: structure, metabolism, interactions with human microbiome, and role in gut homeostasis.

Consumption of food rich in dietary fibers (DFs) has been long recognized to exert an overall beneficial effect on human health. This review aims to provide a holistic overview on how IDFs impact human gut health either directly, or through modulation of the gut microbiome. Several databases were searched for collecting papers such as PubMed, Google Scholar, Web of Science, Scopus and Reaxys from 2000 till 2022. Firstly, an overview of the chemical structure of the various IDFs and the pathways employed by gut microbiota for their degradation is provided. The impact of IDFs on microbial community structure and pathogens colonization inside the human gut was discussed. Finally, the impact of IDFs on gut homeostasis and systemic effects at the cellular level, as well as the overall immunological benefits of IDFs consumption were analyzed. IDFs viz., cellulose, hemicellulose, resistant starch, and lignin found enriched in food are discussed for these effects. IDFs were found to induce gut immunity, improve intestinal integrity and mucosal proliferation, and favor adhesion of probiotics and hence improve human health. Also, IDFs were concluded to improve the bioavailability of plant polyphenols and improve their health-related functional roles. Ultimately, dietary fibers processing by modification shows potential to enhance fibers-based functional food production, in addition to increase the economic value and usage of food-rich fibers and their by-products.

Phytochemical and biological diversity of triterpenoid saponins from family Sapotaceae: A comprehensive review.

Sapotaceae is a flowering plants family reported for its richness in triterpenoid saponins. Sapotaceae comprises a large number of fruit-producing plants of nutritional and medicinal value. Different species of family Sapotaceae received a considerable interest owing to their rich triterpenoid saponins content of a myriad pharmacological effects and health benefits. Several databases were searched for collecting papers for this review in the scope of phytochemistry, bioactivity and record of triterpenoid saponins from family Sapotacese such as PubMed, Google Scholar, Web of Science, Scopus and Reaxys from 1990 till now. Triterpenoid saponins reported from Sapotaceae plants are mostly of protobassic acid, 16-α-hydroxyprotobassic acid, bayogenin, and oleanolic acid derivatives with both monodesmosidic and/or bidesmosidic attached sugar side chains. Besides, the most frequently attached sugar units are glucose, glucoronic acid, apiose, xylose, rhamnose, and arabinose. The reported health effects of Sapotaceae plants in folk medicine in relation to their bioactive saponins were also reviewed with special attention to anti-inflammatory, antiulcer activity, antimicrobial activity, cytotoxic, anti-hypercholesterolemic, antioxidant, and immunomodulatory activities. This review aims to present a holistic compile on the phytochemical and biological diversity of triterpenoid saponins reported from family Sapotaceae with future perspectives.

Comparative aroma and nutrients profiling in six edible versus nonedible cruciferous vegetables using MS based metabolomics.

Cruciferous vegetables, also known as brassicaceae vegetables, are widely consumed worldwide for their nutritive and substantial health benefits. Compositional heterogeneity was explored in six cruciferous vegetables viz, cauliflower, turnip, broccoli, watercress, radish and cabbage leaves targeting their aroma and nutrients profile. A headspace solid-phase micro extraction (HS-SPME) technique combined with gas chromatography-mass spectrometry (GC-MS) was employed for metabolite profiling. Results revealed extensive variation in volatiles and nonvolatile profiles among the six cruciferous vegetables. A total of 55 nutrient metabolites were identified, whereas a total of 190 volatiles were detected. Aldehydes and ketones appeared as the most discriminatory among leaves, accounting for its distinct aroma. Furthermore, chemometric analysis of both datasets showed clear classification of the six vegetables, with several key novel markers. This study provides the first comparative study between edible and inedible parts of cruciferous vegetables, suggesting novel uses as functional foods.

Ficus natalensis extract alleviates Cadmium chloride-induced testicular disruptions in albino rats.

BACKGROUND: Cadmium is a potential environmental pollutant with worldwide health problems. Many Ficus species are reported to have an extensive diversity of traditional uses, among them the treatment of reproductive toxicity. OBJECTIVES: This study set out to evaluate the effect of Ficus natalensis extract on the testicular impairments induced by cadmium chloride (CdCl2) and investigated the potential mechanisms associated with its treatment. METHODS: Thus, 40 male albino rats were categorized into 4 groups (n = 10); group I (control), group II (cadmium-treated group) orally received 5 mg/kg/day CdCl2 for one month, group III (cadmium + Ficus natalensis extract) orally received 5 mg/kg/day CdCl2 for one month plus 200 mg/kg/day Ficus natalensis extract for another month, and group IV (cadmium + reference drug (mesterolone) orally received 5 mg/kg/day CdCl2 for one month plus 4.16 mg/kg/day mesterolone for another month. RESULTS: At the end of experiment, CdCl2 administration markedly induced histological and histo-morphometric changes with a substantial (p < 0.05) decrease in the sperm count, sperm motility, serum TAC, serum testosterone, downregulation in the mRNA expression levels of testicular 17ß-HSD and StAR, in addition to a significant increase in serum TNF-α and testicular MDA level compared to the control group. Conversely, the treatment with Ficus natalensis methanolic extract as well as the reference drug significantly ameliorated the above-mentioned adverse effects induced by CdCl2. CONCLUSIONS: Our results suggested that Ficus natalensis extract can attenuate the CdCl2-induced testicular impairments via inhibiting the oxidative cell damage and inflammation that contributed to CdCl2 toxicity.

How Does Allium Leafy Parts Metabolome Differ in Context to Edible or Inedible Taxa? Case Study in Seven Allium Species as Analyzed Using MS-Based Metabolomics.

Genus Allium (F. Amaryllidaceae) includes a wide variety of edible foods widely consumed for their nutritive as well as health benefits. Seven Allium species, viz., chives, Egyptian leek, French leek, red garlic, white garlic, red onion, and white onion aerial parts were assessed for metabolome heterogeneity targeting both aroma and nutrients phytochemicals. A headspace solid-phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) were employed. Results revealed extensive variation in volatiles and nutrients profile among the seven Allium species represented by a total of 77 nutrients and 148 volatiles. Among edible Allium species, French leek encompassed high levels of nutrients, viz., sugars, fatty acids/esters, organic acids, and amino acids, compared to Egyptian leek. Sulfur aroma compounds appeared as the most discriminatory among Allium, taxa accounting for its distinct flavor. Furthermore, chemometric analysis of both datasets showed clear discrimination of the seven Allium species according to several key novel markers. This study provides the first comparative approach between edible and inedible aerial leafy parts of Allium species providing novel insight into their use as functional foods based on such holistic profiling.

Comparative Volatile Profiling of Ludwigia stolonifera Aerial Parts and Roots Using VSE-GC-MS/MS and Screening of Antioxidant and Metal Chelation Activities.

Ludwigia stolonifera (Guill. & Perr.) P.H.Raven belonging to the family Onagraceae is an important aquatic herbal plant of economic importance in water bioremediation. We explored the compositional heterogeneity in the aroma profile of L. stolonifera aerial parts and roots. Volatile profiling was employed for the first time using volatile solvent extraction (VSE-GC-MS/MS) of both aerial parts and roots. A total of 85 volatiles were identified belonging to eight classes, viz., aliphatic, aromatic, and oxygenated hydrocarbons, monoterpenes, diterpenes, alcohols, acids/esters, and sterols. Aliphatic and aromatic hydrocarbons were found to be the most abundant metabolite groups in both aerial parts and roots. Furthermore, antioxidant and metal chelation activities of aerial parts and roots were investigated, revealing a potent activity as an antioxidant and high metal chelation capacity for heavy metals.

The potential and outgoing trends in traditional, phytochemical, economical, and ethnopharmacological importance of family Onagraceae: A comprehensive review.

ETHNOPHARMACOLOGICAL RELEVANCE: The Onagraceae is a widely distributed family of flowering plants comprises about 17 genera and more than 650 species of herbs, shrubs, and trees. Onagraceae also common as willowherb family or evening primrose family is divided into two subfamilies; Ludwigioideae (mainly genus; Ludwigia) and Onagroideae. Family Onagraceae is characterized by its numerous traditional uses as treatment of hormonal imbalances, urinary system ailments, prostate health maintenance, and antimicrobial effects. AIM OF THE STUDY: This review aims to introduce a holistic overview on the phytochemical composition, economical importance and ethnopharmacological value of different species of family Onagraceae. MATERIALS AND METHODS: Literature review was performed using different data bases such as PubMed, Web of Science, Google Scholar and Reaxys searching for articles focused on phytochemical composition, bioactivity and ethnopharmacological history of Onagraceae species. RESULTS: Different species of Onagraceae were reported to have a great variety of phytochemicals including flavonoids, tannins, phenolic acids, triterpenoids, saponins, and volatile/fixed oils. Onagraceae exhibited several health benefits and pharmacological activities including anti-inflammatory, antiarthritic and analgesic, antioxidant, cytotoxic, antidiabetic, and antimicrobial. CONCLUSIONS: Family Onagraceae is an extremely important family with diverse phytochemical composition which enriches their pharmacological importance and hence it's commercial and economical value.

Metabolome-based profiling of African baobab fruit (Adansonia digitata L.) using a multiplex approach of MS and NMR techniques in relation to its biological activity.

Adansonia digitata L. also known as African baobab is one of the most important fruit-producing trees, widely distributed in the African continent. Baobab fruits are known to possess potential health benefits and nutritional value. This study aimed to holistically dissect the metabolome of A. digitata fruits using a novel comparative protocol using three different analytical platforms. Ultra high performance liquid chromatography coupled to high-resolution tandem mass spectrometry (UHPLC-HRMS/MS), and headspace solid-phase microextraction/gas chromatography coupled to mass spectrometry (HS-SPME/GC-MS) were respectively employed for phytonutrients and aroma profiling, whereas GC-MS post silylation provided an overview of nutrients i.e., sugars. UHPLC-HRMS/MS analysis allowed for the assignment of 77 metabolites, among which 50% are reported for the first time in the fruit. While GC-MS of silylated and aroma compounds led to the identification of 74 and 16 compounds, respectively. Finally, NMR-based metabolite fingerprinting permitted the quantification of the major metabolites for future standardization. In parallel, in vivo antidiabetic potential of the baobab fruit using a streptozotocin (STZ) induced diabetic rat model was assessed. Histopathological and immune-histochemical investigations revealed hepatoprotective and renoprotective effects of A. digitata fruit along with mitigation against diabetes complications. Moreover, the administration of A. digitata fruits (150 mg kg-1) twice a week lowered fasting blood glucose levels.

Metabolome-Based Analysis of Herbal Cough Preparations Via Headspace Solid-Phase Microextraction GC/MS and Multivariate Data Analyses: A Prospect for Its Essential Oil Equivalency.

Liquid cough preparations containing essential oils pose a challenge for isolating and quantifying their volatile components from such a complex matrix enriched with nonvolatile constituents and excipients. This study aims to develop a strategy integrating QC analysis of seven natural cough preparations in the Egyptian market and to assess volatile variation among the preparations using multivariate data analyses. Cough preparations were subjected to headspace solid-phase microextraction (HS-SPME) for determination of their essential oil composition mediating for their actions and to assess volatile differences among them. HS-SPME is a suitable technique for sample preparation that allows for extraction and enrichment of volatiles from complex nonvolatile matrices and their direct desorption into the gas chromatography analytical system. A total of 88 volatile components were identified belonging to seven classes, viz. aromatics, aliphatic hydrocarbons, mono/sesquiterpene hydrocarbons, and oxygenated mono/sesquiterpenes. Oxygenated monoterpenes, viz., menthol, cineole, thymol, and (E)-anethole, were the major volatiles identified in five cough preparations (79.5-98.6%), whereas aromatics, chiefly cinnamate derivatives, constituted the second class amounting for 50.5 and 27.4% in the other two cough preparations. Meaningful results regarding the products' efficacy and safety were extrapolated from this analytical procedure, where artificial preservatives (parabens) were detected in five cough preparations. This study established an efficient strategy for exploring volatile profiling and defining different markers among the different cough preparations. Additionally, authenticity of listed herbal ingredients in the cough preparations was also confirmed in certain preparations, while other formulations failed to show representative volatile components. Volatile variation among preparations was assessed using multivariate data analyses in an attempt to prioritize cough preparations for usage, suggesting the preference of Bronchicum and Babetone among examined cough products.

UHPLC-MS metabolome based classification of umbelliferous fruit taxa: a prospect for phyto-equivalency of its different accessions and in response to roasting.

Herbs of the Umbelliferae family are popular spices valued worldwide for their many nutritional and health benefits. Herein, five chief umbelliferous fruits viz., cumin, fennel, anise, coriander and caraway were assessed for its secondary metabolites diversity along with compositional changes incurring upon roasting as analyzed via ultra-high performance liquid chromatography coupled to photodiode array and electrospray ionization mass detectors UHPLC-qToF/MS. A total of 186 metabolites were annotated, according to metabolomics society guidelines, belonging mainly to flavonoids, fatty acids and phenolic acids. Multivariate models viz., PCA, HCA and OPLS-DA were further employed to assess fruits' heterogeneity in an untargeted manner and determine mechanistic changes in bioactive makeup post roasting viz., glycosidic cleavage, lipid degradation and Maillard reaction. Finally, the fruits' antioxidant activity showed decline upon roasting and in correlation with its total phenolic content. This study presents the first complete map of umbelliferous fruit metabolome, compositional differences and its roasting effect.