ABSTRACTIntroductionPeels are an abundant but still underutilized waste product in the Citrus fruit industry. They contain coumarins with antiadipogenic potential that could be promising targets in new valorization strategies for Citrus peels.ObjectivesIn this study, these coumarins, that is, citropten, bergamottin, and 5‐geranyloxy‐7‐methoxycoumarin (5G7MC), were investigated in Citrus limon peels of different commercial varieties by HPLC‐DAD after extraction with ethanol and choline chloride‐based natural deep eutectic solvents (NADES) as alternative extraction agents in green natural product extraction.ResultsTarget coumarins were almost exclusively found in the flavedo (exocarp) peel layer and in whole peel samples, but not in the albedo (mesocarp) layer. Flavedo samples from varieties “Verdelli” (ES) and “Lisbon” (ZA) showed particularly high concentrations in ethanolic extracts. When applying NADES extraction, best results for citropten were achieved with malonic acid, 1,2‐propanediol, and citric acid as hydrogen bond donors (HBDs), with higher yields than the reference solvent ethanol. For bergamottin and 5G7MC, promising results were obtained for 1,2‐propanediol as HBD, though lower yields than with ethanol. The possible chlorination of coumarin epoxides byakangelicol and oxypeucedanin was recognized for acidic NADES in LC–MS analysis.ConclusionOverall, C. limon peels proved to be a relevant starting material for valorization through coumarin extraction with ethanol and NADES.

ABSTRACTIntroductionThe metabolome of plants is influenced by various factors, especially environmental, as the season in which they are grown. So, distinct varieties of the identical plant might show an increase or decrease in metabolites. The diversity of content of primary and secondary metabolites can also determine the variation in their biological properties. Due to the current occurrence of various fennel varieties, the crop can now be grown for the entire year.ObjectiveThis work used an integrated approach of LC/MS and NMR analysis to characterize the metabolome of fennel waste of different varieties by multivariate statistical analysis.MethodsThe extracts were investigated by NMR and LC/MS analysis to focus attention on the primary and secondary metabolites. Both LC‐HRMS and NMR data were analyzed by principal component analysis (PCA).ResultsThe 1H‐NMR analysis led to the identification of 15 primary metabolites, such as amino acids, carbohydrates, and organic acid derivatives. The secondary metabolites identified by LC/MS analysis mainly belong to the phenolic, lipid, and fatty acid compounds classes.ConclusionThis integrated approach guarantees a precise and complete overview of the variations in the metabolic expression of the fennel varieties grown in different seasons.

ABSTRACTIntroductionZiziphora clinopodioides subsp. bungeana (Juz.) Rech.f. is used in traditional medicine for various purposes. Previous phytochemical studies focused on phenolic compounds, but triterpenoids were almost overlooked.ObjectiveThe study focused on the isolation of compounds with dual antidiabetic activity from the aerial parts of Z. clinopodioides subsp. bungeana.Materials and MethodsSeparation of CHCl3‐soluble fraction by silica gel column chromatography using different mobile phases and purification of compounds by semi‐preparative HPLC or preparative TLC. The structures of pure compounds were elucidated by 1D and 2D NMR experiments along with HRMS. Compound 1 was additionally identified by the single crystal X‐ray diffraction method. α‐Glucosidase inhibitory assay and GLUT4 expression and translocation in C2C12 myotubes were conducted to evaluate antidiabetic potential of isolated compounds.ResultsThis phytochemical study led to the isolation of 20 compounds, including a unique monoterpene diperoxy dimer (1). Compounds 7 and 9–11 displayed more potent α‐glucosidase inhibitory activity (IC50 45.3–135.3 μM) than acarbose used as a positive control (IC50 264.7 μM), while only pomolic acid (5) increased GLUT4 translocation in C2C12 myotubes in a significant manner.ConclusionExtensive chromatographic separation led to the isolation and identification of a unique monoterpene diperoxy dimer (1) from aerial parts of Z. clinopodioides subsp. bungeana. Some triterpenes inhibited α‐glucosidase, another increased GLUT4 translocation. Although none of the isolated compounds demonstrated dual antidiabetic activity, selected triterpenes proved to be potent antidiabetic agents in vitro.

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No abstract is available for this article.

ABSTRACTIntroductionNutricosmetics derived from Silybum marianum, known for their anti‐inflammatory and hepatoprotective properties, necessitate accurate quantification of silybin, a key bioactive component.ObjectivesThis study aims to develop a novel high‐performance liquid chromatography (HPLC) method with amperometric detection (HPLC‐ECD) for the precise determination of silybin. An ultrasound‐assisted extraction (UAE) procedure is also established for solid sample preparation prior to chromatographic analysis.Materials and MethodsChromatographic separation of silybin was performed on a C18 column and using methanol–0.035 M potassium phosphate (pH 4.0) at 1.0 mL min−1 flow rate as mobile phase in gradient mode. The electrochemical detection (ECD) of silybin was carried out on a glassy carbon electrode (GCE) at +1.10 V versus Ag/AgCl. The UAE procedure for silybin extraction from solid samples was performed by 15 min sonication in an ultrasonic bath (80 kHz and 100% power) at room temperature.ResultsUnder the optimal chromatographic conditions, silybin diastereoisomers (silybin A and silybin B) can be separated from other S. marianum flavonolignans in less than 20 min, with a detection limit (LOD) of 0.060 mg L−1 and a reproducibility (RSD) of 5%. This method was successfully applied to analyze silymarin‐containing products with recoveries close to 100%.ConclusionsThis work presents the first HPLC method for silybin determination using an amperometric detector with a GCE. The LOD is competitive in comparison with previously published HPLC‐DAD methods. This HPLC‐ECD method allows silybin diastereoisomers identification without interferences of other flavonolignans present in silymarin extracts.

ABSTRACTIntroductionExisting methods for morphological, organoleptic, and chemical authentication may not adequately ensure the accurate identification of plant species or guarantee safety. Herbal raw material authentication remains a major challenge in herbal medicine. Over the past decade, DNA barcoding, combined with an orthogonal approach integrating various testing methods for quality assurance, has emerged as a new trend in plant authentication.ObjectiveThe review evaluates DNA barcoding and common alternative testing in plant‐related sectors to enhance quality assurance and accurate authentication.MethodStudies were selected based on their relevance to the identification, quality assurance, and safety of herbal products. Inclusion criteria were peer‐reviewed articles, systematic reviews, and relevant case studies from the last two decades focused on DNA barcoding, identification methods, and their applications. Exclusion criteria involved studies lacking empirical data, those not peer‐reviewed, or those unrelated to the main focus. This ensured the inclusion of high‐quality, pertinent sources while excluding less relevant studies.ResultsAn orthogonal approach refers to the use of multiple, independent methods that provide complementary information for more accurate plant identification and quality assurance. This reduces false positives or negatives by confirming results through different techniques, combining DNA barcoding with morphological analysis or chemical profiling. It enhances confidence in results, particularly in cases of potential adulteration or misidentification of plant materials.ConclusionThis study highlights the persistent challenges in assuring the quality, purity, and safety of plant materials. Additionally, it stresses the importance of incorporating DNA‐based authentication alongside traditional methods, to enhance plant material identification.