Search Results (355)

Reliable analytical methods are essential for the assessment, effective quality control, and guarantee of consistent and reproducible performance of chemical profiles of non-psychoactive low-THC Cannabis sativa L. samples and their products. An integrated analytical approach was applied for the first time to evaluate low-THC C. sativa products on the Serbian legal market using chemometrics combined with five complementary techniques: ultraviolet–visible spectroscopy (UV–Vis), high-performance thin-layer chromatography (HPTLC), portable Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR) and gas chromatography–mass spectrometry (GC–MS). HPTLC rapidly differentiated key cannabinoids with R_F at 0.39 and 0.61, while GC–MS enabled comprehensive identification of major cannabinoids (CBG and CBD). Spectroscopic fingerprints provided characteristic UV–Vis absorption maximum (215, 235, and 275 nm), Raman (1700, 1550, 1517, 1224, 1096 cm⁻¹) and FTIR marker bands (615, 1059, 1288, 1620, 2932 cm⁻¹), supporting robust monitoring. Principal component analysis (PCA) across all five techniques revealed two major distinct sample clusters and identified the most influential analytical signals. The combined separation, spectroscopic, and multivariate approach is proven to be effective for systematic cannabinoid content assessment, authentication, and chemical profiling within a process-oriented context, thus enabling effective quality control in the cultivation process by targeting compounds of interest. Full article

Urban forest management practices generate substantial amounts of twig biomass that is commonly treated as waste, despite its potential as a source of bioactive compounds. Biological and chemical properties of methanolic extracts of 19 urban forest tree and shrub species were assessed using a multidisciplinary approach combining high-performance thin-layer chromatography (HPTLC) and HPTLC-DPPH bioautography with spectrophotometric determination of radical scavenging activity (RSA), total phenolic content (TPC), inhibition assays of skin aging-related enzymes (tyrosinase and elastase), and testing against skin pathogens Staphylococcus aureus and Pseudomonas aeruginosa. The results revealed marked differences in biological activity among extracts, driven primarily by specific phytochemical profiles. Torminalis glaberrima (Gand.) Sennikov & Kurtto (108.8 ± 6.6 μmol TE/mL) and Paliurus spina-christi Mill. (106.6 ± 1.6 μmol TE/mL) exhibited the highest RSA, correlating with elevated TPC. Acer campestre L. (51.6 ± 9.1%) showed the strongest elastase inhibition. The most pronounced tyrosinase inhibition was observed for Torminalis glaberrima (39.0 ± 3.5%), indicating a significant contribution of TPC. In contrast, the strongest antibacterial activity was recorded for Acer platanoides L. and Carpinus betulus L., despite their lower TPC values, suggesting the contribution of non-phenolics. Phenolic zones (R_F 0.10, 0.28, 0.57, 0.58) were identified as putative markers of the observed bioactivities. Overall, twigs emerge as an underexplored source with considerable potential for natural cosmetics development, warranting further investigations. Full article

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

This study evaluated activities of crude extracts from different parts of the tree of heaven (Ailanthus altissima (Mill.) Swingle) collected in Slovenia and Hungary, using effect-directed analyses based on hyphenation of high-performance thin-layer chromatography (HPTLC) and nine in vitro assays performed in situ on chromatographic plates after the separation. HPTLC separation combined with a set of four antibacterial assays, two antifungal assays, and three enzyme inhibitor assays to evaluate the extracts of 15 plant parts: young shoots, young leaves, mature leaves, yellow leaves, petioles of leaves, petioles of male inflorescences, petioles of fruits, female inflorescences, young fruits, male inflorescences, mature male inflorescences, bark of 1–2-year branches, bark of 2-year branches, bark of tree trunk, and bark of roots. Antibacterial activities against Gram-positive bacteria (Bacillus subtilis, Rhodococcus fascians) and Gram-negative bacteria (Aliivibrio fischeri, Pseudomonas syringae pv. maculicola (Psm)), as well as inhibition of enzymes α-glucosidase, lipase, and acetylcholinesterase, were observed for all extracts. Extracts differed in their antifungal activities. Extracts of young shoots, mature leaves, petioles of leaves, and bark of roots showed antifungal activity against plant pathogens Fusarium avenaceum and Bipolaris sorokiniana. Extracts of yellow leaves, male inflorescences, bark of 1–2-year branches, and bark of tree trunks were only active against F. avenaceum, whereas extracts of young leaves were only active against B. sorokiniana. This study is the first to report that A. altissima extracts exhibit (1) antifungal activity against F. avenaceum and B. sorokiniana; (2) antibacterial activity against A. fischeri, Psm, R. fascians, and B. subtilis (except leaves, bark of branches and bark of tree trunks); and (3) inhibitory activity toward lipase, α-glucosidase (except bark of tree trunks), and acetylcholinesterase (except bark of tree trunks). Full article

Cecina de León is a traditional Spanish dry-cured beef product whose surface, as in other similar meat products, becomes heavily colonised by fungi during ripening, raising concerns related to possible mycotoxin contamination. This study aimed to characterise the mycobiota associated with cecina and its production environment, with particular emphasis on mycotoxigenic Penicillium species. Seventy-eight cecina samples and 26 air samples were collected from meat-processing plants and local markets in the province of León (Spain) and analysed for fungal counts, water activity and pH. A total of 101 mould isolates and 16 yeasts were recovered, with Penicillium accounting for 88% of all moulds. Sixteen Penicillium species were identified using a polyphasic approach integrating macro- and micromorphological analysis, extrolite production, molecular markers (BenA, CaM and ITS), and MALDI-TOF MS. Mycotoxin screening by HPTLC and HPLC-PDA targeted cyclopiazonic acid, ochratoxin A, patulin, citrinin, griseofulvin and mycophenolic acid, revealing that 51% of the Penicillium isolates were mycotoxin producers, mainly P. commune. The proposed polyphasic strategy, including MALDI-TOF MS as a rapid complementary tool, offers a practical framework for the surveillance of fungal communities and mycotoxin risk in meat-processing environments. Full article

Phlomis L., with more than 100 species belonging to the Lamiaceae family, is a genus encompassing a diverse group of plants known for their rich phytochemical profiles and important medicinal properties. Phlomis kurdica Rech. fil. is a member of this genus widely distributed in the Middle East, especially in Iran, Iraq and Türkiye. In traditional medicine, Phlomis species have been employed in the treatment of various disorders, particularly skin conditions such as wound healing, as well as diabetes, hemorrhoids, inflammation, and gastric ulcers. The purpose of this study was to investigate the biological activities of Phlomis kurdica on skin-related enzymes and to evaluate its phytochemical properties using HPTLC, LC-MS/MS. Additionally, an emulgel formulation was developed with methanolic extract of the plant and characterized in terms of spreadability, textural profile analysis, pH, viscosity, and content quantification determination. In vitro release and rheology studies were carried out following the characterization investigations. According to our investigations, P. kurdica may be a useful component of wrinkle prevention and skin-regenerating products. Full article

Hydrogen peroxide (H₂O₂) regulates plant metabolism. This study examined its effect on the biosynthesis of specialized metabolites in Baccharis conferta, a medicinal plant rich in phenolics and terpenes. Plants were elicited with 25 µM and 250 µM H₂O₂. Phenolic changes were evaluated by total phenolic content (TPC), total flavonoid content (TFC), phenylalanine ammonia-lyase (PAL) activity, and LC-MS analysis of flavonoids and hydroxycinnamic acids. Meanwhile, terpene changes were evaluated by HPTLC, total terpene content (TTC), and expression of the 1-deoxy-D-xylulose-5-phosphate synthase (Bco-DXS1) gene. H₂O₂ markedly modulated both pathways. Phenolic metabolism was activated, particularly under 25 µM H₂O₂, with PAL activity increasing by 52%, TPC by 42%, and TFC by 50% relative to the control. Chemical analysis revealed that five compounds, including chlorogenic acid, differed significantly across treatments. Gene expression analysis showed that 25 µM H₂O₂ upregulated Bco-DXS1 and increased TTC, whereas 250 µM H₂O₂ repressed gene expression but still enhanced terpene accumulation. Overall, these results suggest that moderate H₂O₂ levels function as a signaling molecule in B. conferta, simultaneously boosting phenolic and terpene pathways. This highlights controlled H₂O₂ elicitation as an effective biotechnological approach to increase the production of valuable metabolites in medicinal plant cultures. Full article

This study developed and validated a stability-indicating high-performance thin-layer chromatography (HPTLC) method for the identification and quantification of gentamicin sulphate in an ointment formulation using silica gel 60 F254 HPTLC plates as the stationary phase and methanol: chloroform: ammonia solution (25%) (1:1:1, v/v/v) as the mobile phase. An ideal solvent ratio, chloroform: methanol (9:1, v/v), was used to dissolve the ointment sample before analysis. According to the guidelines of the International Council for Harmonisation (ICH), the HPTLC method was validated, demonstrating specificity by separating all three bands of gentamicin sulphate without interference from ointment excipients and/or degradation products resulting from photolytic, photolytic and oxidative, oxidative, acidic, and alkaline stress conditions. The findings of the study also revealed that the method has high levels of linearity within the range of 50–300 ng/band (R² ≥ 0.99), with detection and quantification limits of 7.10 ng, and 21.53 ng, respectively. Additionally, the method does not require any sample pre-treatment, such as extraction from the ointment base, making it simple and convenient for the quality control of gentamicin ointments. Full article

Polyphenols are key dietary bioactive compounds, reducing oxidative stress and neurodegeneration. This study investigated the in vitro antioxidant and neuroprotective potential of some edible fruits (apricots, plums, figs) and vegetable (parsley) extracts related to their phytochemical profile. Plum extract exhibited the strongest antioxidant capacity (ABTS IC₅₀ 1.733 ± 0.079 mg/g; DPPH IC₅₀ 1.593 ± 0.069 mg/g; FRAP 23.161 ± 1.094 mM Fe²⁺), linked to its high chlorogenic and caffeic acids content. Parsley displayed the most potent AChE inhibition (IC₅₀ 0.825 ± 0.026 mg/g), associated with an elevated flavonoids level (TFC 12.874 ± 0.534 mg QE/g) and the presence of ferulic and vanillic acids. Apricot was characterized by notable gallic, syringic, and chlorogenic acids, supporting moderate neuroprotective potential. Figs showed weaker radical scavenging ability but provided a balanced profile of protocatechuic, caffeic, and syringic acids. Correlation analysis revealed specific compound–activity associations, including syringic and vanillic acids with DPPH scavenging capacity, p-coumaric acid with TPC, and gallic/ferulic acids with AChE inhibition. Effect-directed HPTLC confirmed chlorogenic acid as a major contributor to the antioxidant capacity. To our knowledge, this is the first study to comparatively integrate spectrophotometric antioxidant assays, UHPLC-based quantitative phenolic profiling, effect-directed HPTLC bioautography, and AChE inhibition analysis across three edible fruits and one vegetable frequently co-consumed in Mediterranean-type diets, enabling a cross-species compound–activity correlation framework. These species exhibit distinct but complementary phytochemical and biofunctional profiles. Their combined use may support the formulation of functional foods with synergistic antioxidant and neuroprotective benefits. Full article

Background/Objectives: This study aimed to evaluate the antidiabetic potential of five extracts/sub-extracts and five known cycloartane saponins [astragalosides (AST) I, II, III, IV, and cyclocanthoside E] from Astragalus noeanus (AN), using four specific diabetes-related molecular targets. Methods: Four diabetes-associated in vitro and in silico targets—protein tyrosine phosphatase 1B (PTP1B), dipeptidyl peptidase IV (DPP IV), α-amylase, and advanced glycation end-products (AGEs)—were employed to obtain comprehensive antidiabetic activity profiles. Additionally, the antioxidant and prebiotic capacities of the extracts/sub-extracts were assessed in vitro. A cycloartane saponin was isolated and structurally characterized. Quantitative analyses of total flavonoids, total saponins, and high-performance thin-layer chromatography (HPTLC) were performed to profile the chemical constituents of the plant material. Results: Among the extracts/sub-extracts, the aqueous extract (ANW) exhibited the highest inhibitory effects against all four diabetes-related targets, with inhibition percentages ranging from 83.70% to 93.49%. The methanol extract (ANM) demonstrated significant prebiotic activity comparable to standard controls on two Lactobacillus strains. The chloroform extract (ANC) showed the highest flavonoid content and exhibited the strongest antioxidant activity across all assays. ANM yielded the highest saponin content (3250 mg escin equivalent/g). HPTLC quantification revealed that AST IV was the predominant saponin in ANM (14.28 μg/mg) after cyclocanthoside E (117.27 ± 6.71 μg/mg). Among the saponins, AST IV displayed the most potent inhibition in diabetes-related enzyme assays, surpassing reference drugs acarbose and vildagliptin at equivalent concentrations. AST III also demonstrated considerable activity, ranking just below AST IV. Molecular docking studies identified AST II and AST III as the most promising ligands, exhibiting superior binding affinities and stronger hydrogen bonding and hydrophobic interactions with target proteins. Cyclocanthoside E was isolated from A. noeanus and evaluated for its antidiabetic effects for the first time, with its structure confirmed by NMR and LC-HRMS analyses. Conclusions: This study highlights Astragalus noeanus as a promising source for safe and effective antidiabetic agents. The potent activity of the aqueous extract, along with AST IV and AST III, warrants further investigation through clinical trials to validate their therapeutic potential in diabetes management. Full article

Pine turpentine essential oil (PTEO) obtained from Pinus pinaster Ait. is known to be used in many fields such as medicine, cosmetics, agriculture, and art. The medicinal use of essential oils puts pressure on industry to produce high-quality products. Pure essential oils derived from natural sources are mistakenly recognized as safe on the grounds of their natural origin. Unless they meet international standards, their safety remains questionable. Therefore, in this study, it was aimed to evaluate the quality of 14 different pine turpentine essential oil samples purchased from various sources on the Turkish market, based on the legally recognized pharmacopoeia in Türkiye, the European Pharmacopoeia (EP). As stated in the “Turpentine Oil” monograph, appearance, relative density, refractive index, optical rotation, acid value, peroxide value, fatty oils, and resinified essential oils analyses were performed for each sample. Additionally, phytochemical profiles were analyzed by high performance thin-layer chromatography (HPTLC) and gas chromatography-mass spectrometry (GC-MS). The results revealed that none of the samples were compliant with EP standards. With this in mind, it is found necessary to impose strict regulations on the production of commercial essential oils. Nevertheless, pharmacies emerge as preferable options for obtaining such products. Full article

Two genetically engineered Bacillus subtilis strains, BMV9 and BsB6, were evaluated in terms of culture medium (effect of nutrients on surfactin yield) and potential biotechnological applications of surfactin in agriculture and the petrochemical industry. BMV9 (spo0A3; abrB*; ΔmanPA; sfp+) is, to date, the highest surfactin producer reported scientifically, and BsB6 is a sfp+ laboratory derivative strain that has also demonstrated considerable production potential. To assess their performance, fermentation experiments were conducted in shake flasks using two different culture media, a mineral salt medium and a complex medium, each supplemented with 2% (w/v) glucose. Lipopeptides (surfactin and fengycin) were extracted and quantified at multiple time points (up to 48 h) via high-performance thin-layer chromatography (HPTLC). Optical density, residual glucose, and pH were monitored throughout the cultivation. In parallel, microbial growth in both media were also validated in small-scale cultivation approaches. Antifungal activity of culture supernatants and lipopeptide extracts was tested against two Diaporthe species, key phytopathogens in soybean crops. Given the agricultural relevance of these pathogens, the biocontrol potential of lipopeptides represents a sustainable alternative to conventional chemical fungicides. Additionally, oil displacement tests were performed to evaluate the efficacy of surfactin in enhanced oil recovery (EOR), bioremediation, and related petrochemical processes. High-resolution LC-MS/MS analysis enabled structural characterization and relative quantification of the lipopeptides. Overall, these investigations provide a comprehensive comparison of strain production performance and the associated impact of cultivation media, aiming to define the optimal conditions for economically viable surfactin production and to explore its broader biotechnological applications in agriculture and the petrochemical industry. Full article

Saponins are valuable health-promoting metabolites. The genus Sechium spp. is a valuable source of such metabolites. Unfortunately, there is no established method for the extraction of saponins from the fruits of this species. Therefore, this research aimed to compare three gravimetric extraction methods for saponins in two Sechium genotypes. The analysis included FT-MIR and HPTLC fingerprinting, as well as spectrophotometric quantification. Independent of the extraction method, bagasse produced higher extraction yields than juice. Among the gravimetric methods, M3 produced the highest yields, while M1 captured the most remarkable diversity and abundance of saponins. The spectrophotometric quantification corroborated the higher total saponin content in bagasse extracts. This data highlights the use of fruit bagasse as the primary source of saponin extraction in Sechium. In addition, we recommend extracting bagasse through M3 for scalable pre-enrichment, while M1 extraction must be used when preserving chemical diversity is critical. Full article

Thin-layer chromatography (TLC) remains a widely used, cost-effective and convenient method to separate small molecules, particularly in the field of natural products and (phospho)lipids. Despite advances in chromatographic methods such as high-performance liquid chromatography (HPLC), TLC retains several advantages, including simplicity and accessibility. However, a critical step is the visualization of the separated lipids on the TLC plate. Although the majority of the regularly used methods were established decades ago, there are still a number of potential pitfalls and widely unknown aspects. This review provides a concise overview about commonly used stationary phases and the solvent systems in TLC analysis of lipids. The main focus is on visualization techniques, spanning from non-specific, destructive (charring by semi-concentrated acids) to specific, non-destructive approaches (e.g., exposition to iodine to monitor unsaturated lipids). The advantages and disadvantages of the different methods will be critically discussed and frequently occurring problems highlighted. Furthermore, the combination of TLC with mass spectrometry (MS) detection will be introduced, covering both extraction-based electrospray ionization MS techniques as well as desorption techniques such as matrix-assisted laser desorption/ionization MS. MS detection, while generally more sensitive and offering molecular specificity, introduces higher technical and financial requirements compared to conventional staining. Nonetheless, the combination of TLC with MS holds significant potential for enhancing lipidomic workflows, particularly in complex biological samples. Full article

The agar diffusion method was used to test the antibacterial activity of 12 plant species against Agrobacterium tumefaciens, the bacterium that is responsible for crown gall disease. Leaf, root, or flower extracts were prepared, but not all parts were used for each of the 12 plants listed. Plant extracts from leaves exhibited higher antibacterial activity than those from flowers and roots. Furthermore, the type of solvent had a significant influence on both the antibacterial activity and the flavonoid and polyphenol content. Acetone and alcohol extracts contained higher contents of these compounds than water extracts. The strongest bacteriostatic effect was of the leaf extracts of eucalyptus (Eucalyptus nicholii L.) and St. John’s wort (Hypericum perforatum L.). Based on HPTLC analysis, eucalyptus extracts contained, among others, chlorogenic acid, hyperoside, and quercetin, while St. John’s wort extracts contained rutin, hyperoside, and quercetin. The tansy leaf extracts (Tanacetum vulgare L.) were also rich in flavonoids and phenolic acids, such as kaempferol-3-glucoside, luteolin, chlorogenic acid, cynarine, and rutin. However, a moderate inhibitory effect against the tested bacterium was found in tansy extracts, as well as hop (Humulus lupulus L.), wormwood (Artemisia absinthium L.), peppermint (Mentha piperita L.), yarrow (Achillea millefolium L.), and nettle (Urtica dioica L.) extracts. The least effective were the root extracts of dandelion (Taraxacum officinale F.H. Wiggers coll.) and valerian (Valeriana officinalis L.), as well as the flower extracts of chamomile (Matricaria chamomilla L.) and marigold (Calendula officinalis L.). Given the lack of effective chemical products and the unavailability of commercially resistant cultivars, the use of plant-based extracts for protecting against crown gall appears to be of particular interest. The preliminary results are promising and suggest that eucalyptus and St. John’s wort extracts are the most promising for controlling A. tumefaciens. Full article