Search Results (28)

The genus Oncosiphon (Asteraceae), consisting of aromatic herbs, is indigenous to southern Africa. Oncosiphon species have been documented in Khoi-San ethnobotany as herbal remedies for typhoid fever, pneumonia, and as diuretics. Research on the biological properties and comprehensive phytochemical profiling of these important Oncosiphon species is currently limited. This study was therefore undertaken to address the knowledge void in chemical profiling, through the application of various analytical techniques to analyse the volatile and non-volatile constituents of three South African Oncosiphon species. The aerial parts of Oncosiphon suffruticosus (n = 28), O. grandiflorus (n = 16), and O. africanus (n = 4) were collected from various locations in the Western Cape Province of South Africa. The stems and leaves (SL) were separated from the flowers (F) and analysed as distinct samples. The methanol: chloroform (1:1, v/v) extracts were prepared and analysed using ultra–high–performance liquid chromatography quadrupole time-of-flight time–of–flight mass spectrometry (UHPLC–QToF–MS) and a semi–automated high–performance thin–layer chromatography (HPTLC) system. Multivariate data analysis was performed on the UHPLC–QToF–MS data to determine interspecies chemical variation. Two-dimensional (2D) gas chromatography (GCxGC–ToF–MS) was used to determine the headspace volatile profiles of the intact aerial parts. The results show that the non-volatile profiles of the Oncosiphon species are characterised by amino acids, phenolic acids, flavonoids, sesquiterpene lactones, and fatty acid derivatives. The HPTLC profiles of O. grandiflorus and O. africanus are chemically more closely related, and O. suffruticosus has a distinct profile, which is supported by the chemometrics results of the flowers. The major headspace volatile compounds in Oncosiphon flowers are α-pinene, α-ocimene, eucalyptol, o-cymene, and artemisia alcohol, whereas the stems and leaves mainly consist of α-ocimene, eucalyptol, and yomogi alcohol. Full article

To date, the phytochemical composition of the aerial parts of Nanophyton iliense U.P. Pratov has not been comprehensively investigated. In the present study, qualitative metabolite profiling of the methanolic extract of the aerial parts was performed using liquid chromatography coupled with diode-array detection and quadrupole time-of-flight mass spectrometry (LC-DAD-QToF-MS) operating in both positive and negative electrospray ionization modes. A total of 81 metabolites were tentatively identified based on accurate mass measurements, MS/MS fragmentation patterns obtained in all-ion MS/MS mode, and comparison with previously reported literature data. The detected compounds included hydroxycinnamic acid amides, phenolic acids, flavonoids (including glycosides), amino acids, organic acids, sulfated derivatives, and nucleosides. Among them, the flavonoid narcissin (isorhamnetin-3-O-rutinoside) was isolated from the extract, and its structure was confirmed by ¹H and ¹³C NMR spectroscopy supported by COSY, HSQC, and HMBC experiments. Additionally, a compound with the molecular formula C₁₇H₁₄O₅ was detected; however, its structure could not be conclusively established based on the available spectroscopic data and is therefore reported as an unidentified metabolite. The present study provides the first systematic qualitative characterization of the metabolite profile of N. iliense and establishes a foundation for future quantitative and bioactivity-oriented investigations of this species. Full article

Legumes, a dietary staple for centuries, have seen an influx of conventional and unconventional varieties to cater to human care conscious consumers. These legumes often undergo pretreatments like baking, soaking, or boiling to mitigate the presence of non-proteinogenic amino acids (NPAAs) and reduce associated health risks. The recent tara flour health scare, linked to the NPAA baikiain, emphasizes the need for robust analytical methods to ensure the safety and quality of both traditional and novel plant-based protein alternatives. While traditional techniques provide insights into protein and non-proteinogenic amino acid profiles, modern liquid chromatography-mass spectrometry (LC-MS) offers superior sensitivity and specificity for NPAA detection. This study employed an LC-QToF method with MS/MS analysis to comprehensively map the distribution of free NPAAs and proteinogenic amino acids (PAAs) in various legume samples. A total of 47 NPAAs and 20 PAAs were identified across the legume samples, with at least 7–14 NPAAs detected in each sample. Sulfur-containing NPAAs, such as S-methyl-L-cysteine, γ-glutamyl-S-methyl cysteine, and S-methyl homoglutathione, were predominantly found in Phaseolus and Vigna species. Cysteine and methionine were the sulfur-containing PAAs identified. Gel electrophoresis and soluble protein quantification were also conducted to understand legume protein composition holistically. This orthogonal approach provides a valuable tool for ensuring the overall quality of plant-based proteins and may aid in investigating food poisoning or outbreaks related to such products. Full article

Background: The use of illicit drugs and stimulants is a burgeoning socioeconomic problem, ultimately leading to an increase in street crimes and deteriorating human health. The persistent presence of CNS drugs in wastewater can also lead to downstream adverse effects on aquatic wildlife and humans. Objectives: In the present study, a method was developed for the solid-phase extraction and quantitative liquid chromatography coupled with tandem quadrupole/time-of-flight mass spectrometry (LC-QToF-MS) analysis of CNS stimulant drugs and their metabolites in municipal wastewater. The targeted species included amphetamine, methamphetamine, methylenedioxy-methamphetamine (MDMA), methylenedioxyethylamphetamine (MDEA), cocaine, and benzoylecgonine (BE). Methods: The method was validated and applied to analyzing wastewater samples collected at the University of Mississippi and the City of Oxford wastewater treatment plants (WWTPs) during weekends when the university hosted home college football games. Results: Our results indicate that while amphetamine, methamphetamine, MDMA, cocaine, and BE were all detected at quantifiable levels, amphetamine and BE were present in significantly higher concentrations in wastewater during football games. Conclusion: The insights from this study can be utilized to monitor long-term drug use trends, providing local law enforcement agencies with relevant data on consumption patterns over time. Full article

Green propolis, particularly from the unique flora of the Brazilian Caatinga biome, has gained significant interest due to its diverse chemical composition and biological activities. This study focuses on the chemical characterization and antimicrobial evaluation of Caatinga green propolis. Twelve compounds were isolated through different chromatographic techniques, including flavanones (naringenin, 7-O-methyleriodictyol, sakuranetin), flavones (hispidulin, cirsimaritin), flavonols (quercetin, quercetin-3-methyl ether, kaempferol, 6-methoxykaempferol, viscosine, penduletin), and one chalcone (kukulkanin B). Using liquid chromatography–quadrupole time-of-flight tandem mass spectrometry (LC-QToF-MS), a total of 55 compounds excluding reference standards were tentatively identified, which include flavonoids, phenolic acids derivatives, and alkaloids, with flavonols, flavanones, and flavones being predominant. Antimicrobial testing against pathogens revealed that the crude extract exhibited low inhibitory activity, against Gram-positive bacteria, including methicillin-resistant Staphylococcus aureus (MRSA) and vancomycin-resistant Enterococcus faecium (VRE) (IC₅₀: 148.4 and 120.98 µg/mL, respectively). Although the isolated compounds showed limited individual activity, a fraction containing sakuranetin and penduletin (Fraction 8) exhibited moderated activity against Cryptococcus neoformans (IC₅₀: 47.86 µg/mL), while a fraction containing quercetin and hispidulin showed moderated activity against VRE (IC₅₀: 16.99 µg/mL). These findings highlight the potential application of Caatinga green propolis as an antimicrobial agent, particularly against resistant bacterial strains, and underscore the importance of synergistic interactions between compounds in enhancing biological effects. Full article

Background/Objectives: Sixty-eight percent of service members are living with overweight or obesity, some who may not consult a healthcare provider when they decide to lose weight. Instead, they often turn to weight-loss dietary supplements for self-care solutions. The purpose of this case series study was to examine the label accuracy and quality of select weight-loss dietary supplements sold on or near US military bases across the country. Methods: Weight-loss dietary supplements (n = 44) were selected and purchased in GNCs, Exchanges, and Shoppettes across 12 military installations from March 2023 to January 2024. Liquid chromatography-mass spectrometry was used to verify the label accuracy according to the Supplement Facts listed ingredients and whether they contained any ingredients prohibited for use in the military. Product label claims were analyzed using the Operation Supplement Safety (OPSS) Risk Assessment Scorecard. Results: Thirty-six products (82%) had inaccurate labels. Twenty-seven (61%) had ingredients listed on the label not detected through analysis. Sixteen products (36%) contained hidden ingredients. The four products purchased within one mile from the base listed multiple prohibited ingredients on the labels, with all detected. Forty (91%) products scored a “no-go” according to the OPSS Scorecard and none contained a third-party certification seal on the label. Multiple stimulants were included in products such that the product safety was unknown. Conclusions: The majority of weight-loss dietary supplements analyzed in this case series study had inaccurate labels and were considered a “no-go” according to the Scorecard. Service members should only have access to safe, high-quality dietary supplement products. OPSS is collaborating with the Department of Defense stakeholders to determine the most effective ways for service members to have access to third-party certified products on all military establishments. Full article

Atraphaxis pyrifolia, a native medicinal plant of Central Asia, has a long history of traditional medicinal use; however, scientific research on its phytochemical and biological properties remains scarce. This paper aims to elucidate its chemical profile and assess its pharmacological potential through a comprehensive investigation of the phytochemical composition of stems and leaves using Liquid Chromatography-Mass Spectrometry (LC-MS), in conjunction with the assessment of its antioxidant (DPPH and ABTS) and cytotoxicity test on Artemia salina. Predominantly, glycosylated flavonoids were detected in stems and leaves extracts, notably including 8-Acetoxy-3′,4′,5,5′-tetrahydroxy-7-methoxy-3-α-L-rhamno-pyranosyloxyflavone, pyrifolin, and dehydroxypyrifolin. While the latter compound is exclusive to A. pyrifolia, the former compounds serve as shared chemical markers with other Atraphaxis species. The methanolic extracts of A. pyrifolia leaves exhibited significant antioxidant capacity without toxicity against Artemia salina. This study contributes to current research through providing valuable insights into the chemical diversity and potential medicinal properties of this plant species. Full article

The Brassicaceae family, commonly referred to as cruciferous plants, is globally cultivated and consumed, with the Brassica genus being particularly renowned for its functional components. These vegetables are rich sources of nutrients and health-promoting phytochemicals, garnering increased attention in recent years. This study presents a comprehensive microscopic, chromatographic, and spectroscopic characterization of Brassica napus L. seeds from Kazakhstan aimed at elucidating their morphological features and chemical composition. Microscopic analysis revealed distinct localization of flavonoids, total lipids, and alkaloids. High-performance thin-layer chromatography (HPTLC) analysis of seed extracts demonstrated a complex chemical profile with significant quantities of non-polar compounds in the hexane extracts. Additionally, methanolic extracts revealed the presence of diverse chemical compounds, including alkaloids, flavonoids, and glucosinolates. The chemical composition exhibited varietal differences across different Brassica species, with B. napus L. seeds showing higher concentrations of bioactive compounds. Furthermore, liquid chromatography–quadrupole time-of-flight mass spectrometry (LC-QToF-MS) analysis provided insights into the chemical composition, with sinapine isomers, feruloyl, and sinapoyl choline derivatives as major compounds in the seeds. This study contributes to a better understanding of the chemical diversity and quality control methods’ approximations of B. napus L. seeds, highlighting their importance in functional food and nutraceutical applications. Full article

Limonium (L.) gmelinii is a valuable pharmacopoeial Kazakhstani plant. Several studies have reported on the various biological activities of the plant. The purpose of our research was to study and compare the extraction yields, immunomodulatory activities, and chemical compositions of extracts from the above-ground parts of L. gmelinii obtained via conventional extraction (CE; Extract 1) and ultrasound-assisted extraction (UAE; Extract 2). The extracts were characterized by a considerable number of polyphenols and flavonoids: 378.1 ± 4.5 and 382.2 ± 3.3 GAE mg/g, and 90.22 ± 2.8 and 94.61 ± 1.9 QE mg/g in Extract 1 and Extract 2, respectively. Extract 2 had a slightly higher extraction yield (33.5 ± 2.4%) than Extract 1 (30.2 ± 1.6%). Liquid Chromatography–Diode-Array Detection–Electrospray Ionization–Quadrupole Time-of-Flight Mass Spectrometry (LC-QToF-MS) revealed the presence of 54 biologically active compounds in both extracts. It was shown that the studied extracts stimulate the secretion of TNF-α and IL-6 by intact mouse peritoneal macrophages and splenic lymphocytes, whilst they have an inhibitory effect on the secretion of these cytokines by activated immune cells. Both extracts demonstrated similar patterns of stimulation and inhibition in a splenocyte proliferation assay. Altogether, the L. gmelinii extracts obtained via CE and UAE might be suggested as effective immunomodulatory agents. The application of UAE for this purpose seems to be more efficient with a view of obtaining of a highly potent extract in a much shorter time. Full article

Chamomile tea is a popular beverage and herbal remedy with various health benefits, including antioxidant and antimicrobial activities and beneficial effects on metabolism. In this study, we investigated the inhibitory activities of secondary metabolites from Matricaria chamomile L. against COX2, an enzyme involved in inflammation and linked to cancer development. The cytotoxicity of the compounds was also evaluated on a panel of 60 cancer cell lines. Myricetin, one of the COX2-inhibiting and cytotoxic compounds in chamomile tea, was further studied to determine a proteomic expression profile that predicts the sensitivity or resistance of tumor cell lines to this compound. The expression of classical mechanisms of anticancer drug resistance did not affect the responsiveness of cancer cells to myricetin, e.g., ATP-binding cassette (ABC) transporters (ABCB, ABCB5, ABCC1, ABCG2), tumor suppressors (p53, WT1), and oncogenes (EGFR, RAS), whereas significant correlations between myricetin responsiveness and GSTP expression and cellular proliferation rates were observed. Additionally, Kaplan–Meier survival time analyses revealed that high COX2 expression is associated with a worse survival prognosis in renal clear cell carcinoma patients, suggesting a potential utility for COX2 inhibition by myricetin in this tumor type. Overall, this study provides insight into the molecular modes of action of chamomile secondary metabolites and their potential as cancer-preventive or therapeutic agents. Full article

Identifying novel phytochemical secondary metabolites following classical pharmacognostic investigations is tedious and often involves repetitive chromatographic efforts. During the past decade, Ultra-High Performance Liquid Chromatography-Quadrupole Time of Flight-Tandem Mass Spectrometry (UHPLC-QToF-MS/MS), in combination with molecular networking, has been successfully demonstrated for the rapid dereplication of novel natural products in complex mixtures. As a logical application of such innovative tools in botanical research, more than 40 unique 3-oxy-, 3, 6-dioxy-, and 3, 6, 27-trioxy-steroidal saponins were identified in aerial parts and rhizomes of botanically verified Smilax sieboldii. Tandem mass diagnostic fragmentation patterns of aglycones, diosgenin, sarsasapogenin/tigogenin, or laxogenin were critical to establishing the unique nodes belonging to six groups of nineteen unknown steroidal saponins identified in S. sieboldii. Mass fragmentation analysis resulted in the identification of 6-hydroxy sapogenins, believed to be key precursors in the biogenesis of characteristic smilaxins and sieboldins, along with other saponins identified within S. sieboldii. These analytes’ relative biodistribution and characteristic molecular networking profiles were established by analyzing the leaf, stem, and root/rhizome of S. sieboldii. Deducing such profiles is anticipated to aid the overall product integrity of botanical dietary supplements while avoiding tedious pharmacognostic investigations and helping identify exogenous components within the finished products. Full article

The lichen Cetraria islandica (L.) Ach. has been used in traditional and modern medicines for its many biological properties such as immunological, immunomodulating, antioxidant, antimicrobial, and anti-inflammatory activities. This species is gaining popularity in the market, with interest from many industries for selling as medicines, dietary supplements, and daily herbal drinks. This study profiled the morpho-anatomical features by light, fluorescence, and scanning electron microscopy; conducted an elemental analysis using energy-dispersive X-ray spectroscopy; and phytochemical analysis was performed using high-resolution mass spectrometry combined with a liquid chromatography system (LC-DAD-QToF) of C. islandica. In total, 37 compounds were identified and characterized based on comparisons with the literature data, retention times, and their mass fragmentation mechanism/s. The identified compounds were classified under five different classes, i.e., depsidones, depsides, dibenzofurans, aliphatic acids, and others that contain simple organic acids in majority. Two major compounds (fumaroprotocetraric acid and cetraric acid) were identified in the aqueous ethanolic and ethanolic extracts of C. islandica lichen. This detailed morpho-anatomical, EDS spectroscopy, and the developed LC-DAD-QToF approach for C. islandica will be important for correct species identification and can serve as a useful tool for taxonomical validation and chemical characterization. Additionally, chemical study of the extract of C. islandica led to isolation and structural elucidation of nine compounds, namely cetraric acid (1), 9′-(O-methyl)protocetraric acid (2), usnic acid (3), ergosterol peroxide (4), oleic acid (5), palmitic acid (6), stearic acid (7), sucrose (8), and arabinitol (9). Full article

Morphine and codeine are the two principal opiates found in the opium poppy (Papaver somniferum L.) and are therapeutically used for pain management. Poppy seeds with low opiates are primarily used for culinary purposes due to their nutritional and sensory attributes. Intentional adulteration of poppy seeds is common, often combined with immature, less expensive, exhausted, or substituted with morphologically similar seeds, viz., amaranth, quinoa, and sesame. For a safer food supply chain, preventive measures must be implemented to mitigate contamination or adulteration. Moreover, the simultaneous analysis of P. somniferum and its adulterants is largely unknown. Pre- and post-processing further complicate the alkaloid content and may pose a significant health hazard. To address these issues, two independent methods were investigated with eight botanically verified and fifteen commercial samples. Microscopical features were established for the authenticity of raw poppy seeds. Morphine, codeine, and thebaine quantities ranged from 0.8–223, 0.2–386, and 0.1–176 mg/kg, respectively, using LC-QToF. In most cases, conventional opiates have a higher content than papaverine and noscapine. The analytical methodology provided a chemical profile of 47 compounds that can be effectively applied to distinguish poppy seeds from their adulterants and may serve as an effective tool to combat ongoing adulteration. Full article

Elderberry is highly reputed for its health-improving effects. Multiple pieces of evidence indicate that the consumption of berries is linked to enhancing human health and preventing or delaying the onset of chronic medical conditions. Compared with other fruit, elderberry is a very rich source of anthocyanins (approximately 80% of the polyphenol content). These polyphenols are the principals that essentially contribute to the high antioxidant and anti-inflammatory capacities and the health benefits of elderberry fruit extract. These health effects include attenuation of cardiovascular, neurodegenerative, and inflammatory disorders, as well as anti-diabetic, anticancer, antiviral, and immuno-stimulatory effects. Sales of elderberry supplements skyrocketed to $320 million over the year 2020, according to an American Botanical Council (ABC) report, which is attributable to the purported immune-enhancing effects of elderberry. In the current review, the chemical composition of the polyphenolic content of the European elderberry (Sambucus nigra) and the American elderberry (Sambucus canadensis), as well as the analytical techniques employed to analyze, characterize, and ascertain the chemical consistency will be addressed. Further, the factors that influence the consistency of the polyphenolic chemical composition, and hence, the consistency of the health benefits of elderberry extracts will be presented. Additionally, adulteration and safety as factors contributing to consistency will be covered. The role of elderberry in enhancing human health alone with the pharmacological basis, the cellular pathways, and the molecular mechanisms underlying the observed health benefits of elderberry fruit extracts will be also reviewed. Full article

Phytochemical investigation of the aerial parts of Artemisia heptapotamica Poljak led to the isolation of ten known compounds, including four alkyl p-coumarates: octadecyl trans-p-coumarate (1), icosy trans-p-coumarate (2), docosyl trans-p-coumarate (3), and tetracosyl trans-p-coumarate (4), one sesquiterpene lactone: santonin (5), four flavonoids; axillarin (6), quercetin 3-O-methyl ether (7), luteolin (8), and quercetin (9), and one phenolic acid derivative: p-coumaric acid (10). The structures of the isolated compounds were identified by various spectroscopic analyses. Additionally, the antimicrobial activity of the total extract and different fractions was screened, and they exhibited no inhibition of the growth of Candida albicans, C. neoformans, Aspergillus fumigatus, methicillin-resistant Staphylococcus aureus (MRS), E. coli, Pseudomonas aeruginosa, Klebsiella pneumonia, and Vancomycin-resistant Enterococci (VRE) at the tested concentrations ranging from 8 to 200 μg/mL. The identification and tentative characterization of the secondary metabolites were conducted using LC-QToF analysis. This method helps in the putative characterization of sesquiterpene lactones, flavonoids, coumarate derivatives, and aliphatic compounds. The developed method identified 43 compounds, of which the majority were sesquiterpene lactones, such as eudesmanolides, germacranolides, and guaianolide derivatives, followed by flavonoids. The proposed LC-QToF method helps develop dereplication strategies and understand the major class of chemicals before proceeding with the isolation of compounds. Full article