Search Results (78)

Olive leaves, the main byproducts of olive cultivation, are characterized by a plethora of bioactive metabolites with significant nutritional value. Their main pentacyclic triterpenes, Oleanolic Acid (OA) and Maslinic Acid (MA), are two high added-value compounds with remarkable activities. This study aimed to develop an efficient methodology for extracting and purifying OA and MA, utilizing Supercritical Fluid Extraction (SFE) and Centrifugal Partition Chromatography (CPC)—two modern, scalable, and green techniques. A total of 21 g of olive leaves were subjected to SFE using supercritical CO₂ and ethanol as co-solvent. The extraction employed a step gradient mode, starting with 100% CO₂ and incrementally increasing ethanol (0–10% w/w) every 20 min. Fractions rich in OA and MA (500 mg) were further purified via CPC, utilizing pH zone refining to exploit the protonation and deprotonation properties of acidic triterpenes. The biphasic solvent system consisted of n-hexane, ethyl acetate, ethanol, and water (8:2:5:5 v/v/v/v), with trifluoroacetic acid added to the stationary phase and triethylamine added to the mobile phase. This two-step process yielded 89.5 mg of OA and 28.5 mg of MA with over 95% purity, as confirmed by HPLC-ELSD and ¹H-NMR. Moreover, purified compounds and SFE fractions exhibited promising elastase and collagenase inhibition, highlighting them as dermocosmetic agents. Full article

Background: The Quantitative Analysis of Multi-components by Single-marker (QAMS) method has been developed as an alternative to the External Standards Method (ESM) for the quality control of medicinal herbs. Objectives: In this study, QAMS was developed to determine saponins in the raw materials of Panax vietnamensis using HPLC-PDA/ELSD. Methods: The method was developed and validated. The relative conversion factors F_x were calculated based on the linear regression for HPLC-PDA and the logarithm equation for HPLC-ELSD. The Standard Method Difference (SMD) was determined to indicate the difference in the results of QAMS and EMS. Results: Relative conversion factors (F_x) were determined for each detector to quantify five saponins (ginsenoside Rb₁, Rd, Rg₁, majnoside R2, and vina-ginsenoside R2) in VG root. The F_x values were calculated based on the ratio of the slopes of the regression equations of a single standard and an external standard. For HPLC-PDA, G-Rb1 was used as a single standard with the F_x values of 1.00 (G-Rb₁), 1.08 (G-Rd), 1.32 (G-Rg₁), and 0.04 (M-R2). For HPLC-ELSD, G-Rb₁ was used for determining the content of G-Rg₁ and G-Rb₁ with the F_x values of 1.00 (G-Rb₁) and 0.95 (G-Rg₁), while M-R2 was used for quantitating M-R2 and V-R2 with F_x of 1.00 (M-R2) and 1.05 (V-R2). An SMD value less than 5.00% confirms the close alignment of the QAMS method with ESM. Conclusions: The QAMS method proved to be a feasible and promising method for the quality control of P. vietnamensis. Full article

A high-performance liquid chromatography with evaporative light scattering detection (HPLC-ELSD) method was developed and validated for analyzing fermentable and reducing sugars in brewing matrices. The method exhibited detection limits of 2.5–12.5 mg/L and quantification limits of 12.0–30.0 mg/L. Linearity was achieved for all sugars, fitted with a quadratic calibration model (R² = 0.9998). Precision metrics revealed relative standard deviations (RSDs) below 2% for repeatability and below 6% for intermediate precision. Recovery rates between 86 and 119% confirmed robustness and minimal matrix interference. Application to brewing samples highlighted variability in sugar profiles, with sucrose concentrations in wort ranging from 3.5 to 22.0 g/L and maltose and maltotriose in finished beers between 0.80 and 1.50 g/L and 1.10–2.50 g/L, respectively. Batch variability analysis showed that brewing conditions had a greater impact on sugar concentrations than malt batch origin, with maltose variation reaching 34.6%. This HPLC-ELSD method provides a robust and reliable tool for sugar analysis in brewing, offering valuable insights into fermentation dynamics and batch consistency. Its application to industrial contexts underscores its potential for improving quality control and optimizing brewing processes. Full article

This study investigates the potential reuse of Prunus spinosa (blackthorn) seeds, a food industry by-product. Traditionally discarded, these seeds are now being explored for their bioactive compounds. In this work, seeds were used as raw material for supercritical CO₂ extraction. Two distinct extracts were obtained at low and high pressure (SFE90 and SFE200) and both extracts presented an aqueous phase (WE90 and WE200). SFE90 analysis by GC/MS allowed us to identify benzaldehyde and fatty acids (mainly oleic and linoleic acids). The fatty acid profile of SFE200, determined by HPLC-DAD/ELSD, showed that oleic and linoleic acids were predominant in supercritical oil. The phytochemical composition of the water extracts, analyzed via LC-DAD-ESI-MS, revealed that higher pressure enhanced the recovery of specific flavonols and anthocyanins, while lower pressure preserved various polyphenolic subclasses. WE90 was rich in 3-feruloylquinic acid and cyanidin-3-O-rutinoside, whereas WE200 was rich in caffeic acid hexoside 2 and dihydro-o-coumaric acid glucoside. Benzaldehyde was individuated in WE90 and WE200 by HPLC-DAD analysis. Cytotoxicity assays demonstrated that WE90, WE200 and SFE200 had anticancer effects on SH-SY5Y neuroblastoma cells, while all extracts did not remarkably affect the viability and morphology of human skin keratinocytes (HaCaT cells). These results suggest that P. spinosa seed extracts have potential nutraceutical and pharmaceutical applications. Full article

Selenium–polysaccharides possess antioxidant properties, making them promising materials for functional foods, pharmaceuticals, and clinical applications. This study examines the incorporation of selenium into polysaccharides via mycelial biosynthesis and its effects on structure and antioxidant activity. Polysaccharides obtained from Lentinula edodes-submerged cultures grown in Se-supplemented and non-supplemented media were analysed for Se content (RP-HPLC/FLD), structure (FT-IR, HPLC, and HPGPC-ELSD), and antioxidant activity (DPPH scavenging, reducing power, and Fe²⁺ chelation). Two low-molecular-weight Se–heteropolysaccharides (Se-FE-1.1 and Se-FE-1.2) containing ~80 and 125 µg/g Se were isolated, primarily composed of glucose, mannose, and galactose with β-glycosidic linkages. Se incorporation into polysaccharides selectively enhanced their antioxidant activity in the DPPH radical scavenging assay, with minimal effects observed in iron chelation and reducing power assays. Crude Se–polysaccharides displayed the highest antioxidant activity, suggesting an additional contribution from protein components. Our findings demonstrate that Se is effectively incorporated into polysaccharides, altering monosaccharide composition while preserving glycosidic linkages. The selective enhancement of radical scavenging suggests that selenium plays a specific role in antioxidant activity, primarily influencing radical scavenging mechanisms rather than interactions with metal ions. Further research is needed to clarify the mechanisms of selenium incorporation, the nature of its bonding within the polysaccharide molecule, and its impact on biological activity. Full article

The aerial parts (Herba Saniculae) and the underground parts (Radix Saniculae) of Sanicula europaea (sanicle) have been used traditionally in Austrian folk medicine to treat wounds. Interestingly, in the Austrian vernacular, “Radix Saniculae” can also refer to the underground parts of Cardamine enneaphyllos. This ambiguity can lead to mistakes in using these two plants and, importantly, adulterations. The present work aims to shed light on using Radix Saniculae as a wound-healing agent. Thus, the main components in the aerial and the scarcely investigated underground parts of Sanicula europaea were identified and compared to the underground parts of Cardamine enneaphyllos. For this purpose, different analytical techniques were employed: TLC, HPLC-DAD/ELSD, UHPLC-ESI-MS, and GC-MS. The main components in both Sanicula and Cardamine plant extracts were saccharides. Both parts of Sanicula europaea showed similar compositions: hydroxycinnamic acid derivatives and triterpene saponins. In contrast, the underground parts of Cardamine enneaphyllos contain two glucosinolates and their breakdown products. These findings suggest the same wound-healing activity for the underground parts of Sanicula europaea as was already found for its aerial parts. The glucosinolates detected in Cardamine enneaphyllos substantiate its use in wound healing. Nevertheless, the presented analytical methods allow for easy discovery of adulterations. Full article

As a traditional Chinese medicine (TCM), Allii Macrostemonis Bulbus (AMB) is a key herb for the treatment of thoracic paralytic cardiac pain, but its quality evaluation method has not yet been fully clarified. In this study, chromatographic fingerprints of AMB were developed using solid-phase extraction–high-performance liquid chromatography–evaporative light scattering detection (SPE-HPLC-ELSD) to evaluate the quality of AMB from various origins and processing methods. This was achieved by employing chemical pattern recognition techniques and verifying the feasibility and applicability of the quality evaluation of AMB through the quantitative analysis of multi-components via a single-marker (QAMS) method. Through the analysis of the fingerprints of 18 batches of AMB, 30 common peaks were screened, and 6 components (adenosine, syringin, macrostemonoside T, macrostemonoside A, macrostemonoside U, and macrostemonoside V) were identified. Moreover, three differential markers (macrostemonoside A, macrostemonoside T, and macrostemonoside U) were screened out using chemometrics techniques, including principal component analysis (PCA), hierarchical cluster analysis (HCA), and orthogonal partial least squares discriminant analysis (OPLS-DA). Subsequently, a QAMS method was established for macrostemonoside T and macrostemonoside U using macrostemonoside A as an internal reference. The results demonstrate the method’s accuracy, reproducibility, and stability, rendering it suitable for the quality evaluation of AMB. This study provides a theoretical basis for drug quality control and the discovery of quality markers for AMB. Full article

Accessing plant resources to extract compounds of interest can sometimes be challenging. To facilitate access and limit the environmental impact, innovative cultivation strategies can be developed. Forskolin is a molecule of high interest, mainly found in the roots of Coleus forskohlii. The aim of this study was to develop aeroponic cultivation methods to provide a local source of Coleus forskohlii and to study the impact of abiotic stress on forskolin and bioactive metabolite production. Three cultivation itineraries (LED lighting, biostimulant, and hydric stress) along with a control itinerary were established. The forskolin content in the plant roots was quantified using HPLC-ELSD, and the results showed that LED treatment proved to be the most promising, increasing root biomass and the total forskolin content recovered at the end of the cultivation period threefold (710.1 ± 21.3 mg vs. 229.9 ± 17.7 mg). Statistical analysis comparing the LED itinerary to the control itinerary identified stress-affected metabolites, showing that LEDs positively influence mainly the concentration of phenolic compounds in the roots and diterpenes in the aerial parts of Coleus forskohlii. Moreover, to better define the phytochemical composition of Coleus forskohlii cultivated in France using aeroponic cultivation, an untargeted metabolomic analysis was conducted using UHPLC-HRMS/MS analysis and molecular networks on both the root and aerial parts. This study demonstrates that aeroponic cultivation, especially with the application of an LED treatment, could be a very promising alternative for a local source of Coleus forskohlii leading to easy access to the roots and aerial parts rich in forskolin and other bioactive compounds. Full article

This study aimed to investigate variations in the phytochemical compound contents and antioxidant potential of the ethanol rhizome extracts of Smilax china L., belonging to the Liliaceae family, from different parts of Korea, namely Uiwang (Mt. Gamnamugol), Gyeonggi Province (SC1); Geochang, Gyeongnam Province (SC2); Yeongwol, Gangwon Province (SC3); and Chungju, Chungbuk Province (SC4). The phenolic and flavonoid contents, radical scavenging activity, and proximate composition of the ethanol extracts from the rhizome samples were determined. The total polyphenol content (TPC) of the extracts ranged between 13.6 and 67.5 mg tannic acid equivalent/g. TPC analysis showed that TPC was higher in SC2 than in SC3, SC4, or SC1. Among the rhizome samples, the SC3 rhizomes had the highest total flavonoid content (TFC) (5.2 mg quercetin equivalents/g). Additionally, SC2 showed the highest radical scavenging activity against DPPH and ABTS⁺ radicals. Chemical characterization using UPLC/UV revealed that the extracts contained compounds such as apiin, kaempferol-3-rutinoside, and chlorogenic acid. Specifically, in SC2, chlorogenic acid was the dominant compound, which supported the levels observed in the UPLC/UV and HPLC/ELSD investigations. Dioscin, another phytochemical, was detected in SC2, SC3, and SC4, indicating the diversity of compounds among the rhizome extracts. Variations in the phytochemical content and antioxidant activity were observed in the extracts from the different regions, underlining the role of geographical variation in the functional characteristics of S. china. The observed differences could have important implications for the medicinal use of S. china extracts in applications such as anti-inflammatory treatments, diabetes management, and potential anticancer therapies. This study underscores the critical need to consider geographical origin when sourcing and utilizing S. china for therapeutic purposes, as it may significantly impact its bioactive profile and efficacy. Full article

This study investigates the chemical composition, nutritional, and biological properties of extracts obtained from A. melanocarpa berries using different extraction methods and solvents. Hydrodistillation and supercritical fluid extraction with CO₂ allowed us to isolate fruit essential oil (HD_EX) and fixed oil (SFE_EX), respectively. A phenol-enriched extract was obtained using a mild ultrasound-assisted maceration with methanol (UAM_M). The HD_EX most abundant component, using gas chromatography-mass spectrometry (GC/MS), was italicene epoxide (17.2%), followed by hexadecanoic acid (12.4%), khusinol (10.5%), limonene (9.7%), dodecanoic acid (9.7%), and (E)-anethole (6.1%). Linoleic (348.9 mg/g of extract, 70.5%), oleic (88.9 mg/g, 17.9%), and palmitic (40.8 mg/g, 8.2%) acids, followed by α-linolenic and stearic acids, were the main fatty acids in SFE_EX determined using high-performance liquid chromatography coupled with a photodiode array detector and an evaporative light scattering detector (HPLC-DAD/ELSD). HPLC-DAD analyses of SFE_EX identified β-carotene as the main carotenoid (1.7 mg/g), while HPLC with fluorescence detection (FLU) evidenced α-tocopherol (1.2 mg/g) as the most abundant tocopherol isoform in SFE_EX. Liquid chromatography-electrospray ionization-MS (LC-ESI-MS) analysis of UAM_M showed the presence of quercetin-sulfate (15.6%, major component), malvidin 3-O-(6-O-p-coumaroyl) glucoside-4-vinylphenol adduct (pigment B) (9.3%), di-caffeoyl coumaroyl spermidine (7.6%), methyl-epigallocatechin (5.68%), and phloretin (4.1%), while flavonoids (70.5%) and phenolic acids (23.9%) emerged as the most abundant polyphenol classes. UAM_M exerted a complete inhibition of the cholesterol oxidative degradation at 140 °C from 75 μg of extract, showing 50% protection at 30.6 μg (IA₅₀). Furthermore, UAM_M significantly reduced viability (31–48%) in A375 melanoma cells in the range of 500–2000 μg/mL after 96 h of incubation (MTT assay), with a low toxic effect in normal HaCaT keratinocytes. The results of this research extend the knowledge of the nutritional and biological properties of A. melanocarpa berries, providing useful information on specific extracts for potential food, cosmetic, and pharmaceutical applications. Full article

Background: Food waste is a global and growing problem that is gaining traction due to its environmental, ethical, social, and economic repercussions. Between 2022 and 2027, the worldwide papaya market is expected to have a huge increase, meaning a growth in organic waste, including peels and seeds. Thus, this study evaluated the potential use of peels and seeds of two mature papaya fruits as a source of bioactive compounds, converting these by-products into value-added products. Proximate analysis (AOAC methods), mineral content (ICP-MS), free sugars (HPLC-ELSD), fatty acid composition (GC-FID), vitamin E profile (HPLC-DAD-FLD), and antioxidant activity (DPPH and FRAP assays) were evaluated. Results: Both by-products showed high total protein (20–27%), and dietary fiber (32–38%) contents. Papaya peels presented a high ash content (14–16%), indicating a potential application as a mineral source. 14 fatty acids were detected, with α-linolenic acid (30%) as the most abundant in the peels and oleic acid (74%) in the seeds. Both by-products showed high antioxidant activity. Conclusion: Papaya by-products display great potential for industrial recovery and application, such as formulation of new functional food ingredients. Full article

Bacillus megaterium is particularly known for its abundance in soils and its plant growth promotion. To characterize the metabolites excreted by this specie, we performed successive liquid/liquid extractions from bacteria culture medium with different polarity solvents (cyclohexane, dichloromethane, ethyl acetate and butanol) to separate the metabolites in different polarity groups. The extracts were characterized regarding their total phenolic content, the amount of reducing sugar, the concentration of primary amines and proteins, their chromatographic profile by HPLC-DAD-ELSD and their chemical identification by GC-MS. Among the 75 compounds which are produced by the bacteria, 19 identifications were for the first time found as metabolites of B. megaterium and 23 were described for the first time as metabolites in Bacillus genus. The different extracts containing B. megaterium metabolites showed interesting agronomic activity, with a global inhibition of seed germination rates of soya, sunflower, corn and ray grass, but not of corn, compared to culture medium alone. Our results suggest that B. megaterium can produce various metabolites, like butanediol, cyclic dipeptides, fatty acids, and hydrocarbons, with diverse effects and sometimes with opposite effects in order to modulate its response to plant growth and adapt to various environmental effects. These findings provide new insight into bioactive properties of this species for therapeutic uses on plants. Full article

Gemmotherapy, a natural therapy based on bud macerates, has recently gained importance in the field of food supplements. However, two coexisting extraction methods employ a glycerin-based solvent, either in a binary or ternary solvent mixture. The absence of an official method for bud preparation leads to non-standardized bud macerates. Given this context, this study aimed to (i) assess the influence of solvent composition on the chemical profile of olive young shoot macerates obtained using glycerin-based solvents or using different solvent extractions and (ii) to compare the two coexisting traditional bud extraction methods described by Dr Pol Henry and by the European Pharmacopoeia. A comprehensive phytochemical analysis of all macerates was conducted using HPLC-DAD-ELSD-MS², identifying 50 metabolites divided into 7 classes through dereplication. The extracts obtained with the solvent described by the European Pharmacopoeia (ethanol/glycerin) and by Dr Pol Henry (water/ethanol/glycerin) appeared to be the most diversified in terms of metabolite distribution and possessed higher rates of secondary metabolites. These observations reinforce the interest in a glycerin-based solvent mixture for bud extraction in gemmotherapy. In addition, the difference in composition between the two traditional solvents was highlighted. Indeed, iridoids were predominant in both macerates, representing about 50% of the chemical composition, but differences were observed from one macerate to another regarding the proportions of the other chemical classes. This emphasizes the necessity for standardized gemmotherapy macerates. Full article

In this work, dopamine (DA) was polymerized on the surface of CuO nanoparticles (CuO NPs) to form a molecularly imprinted polymer (MIP@PDA/CuO NPs) for the colorimetric detection of astragaloside-IV (AS-IV). The synthesis process of MIP is simple and easy to operate, without adding other monomers or initiators. CuO NPs has high peroxidase (POD)-like activity that can catalyze the oxidation of 3,3′,5,5′-tetramethylbenzidine (TMB) to generate oxidized TMB (OxTMB) in the presence of H₂O₂, having a maximum ultraviolet-visible (UV-Vis) absorption peak at 652 nm. The AS-IV can specifically bind to the surface imprinted cavities and prevent the entry of TMB and H₂O₂, which will lead to the inhibition of the catalytic reaction. Therefore, a new approach based on the POD-like activity of MIP@PDA/CuO NPs for AS-IV detection was developed with a linear range from 0.000341 to 1.024 mg/mL. The LOD and LOQ are 0.000991 and 0.000341 mg/mL, respectively. The developed method can accurately determine AS-IV in Huangqi Granules and different batches of Ganweikang Tablets, which are similar to the results measured by HPLC-ELSD and meet the requirements of Chinese Pharmacopoeia (2020 edition) for the amount of AS-IV in Huangqi Granules. The combination of MIP with CuO NPs not only endows the detection of AS-IV with high selectivity and reliability, but also expands the application of nanozymes in the detection of small-molecule compounds that have weak UV absorption, and do not have reducibility or oxidation properties. Full article

An analytical method was established using high-performance liquid chromatography coupled with diode array and evaporative light scattering detectors (HPLC-DAD-ELSD) with -C₁₈ and -NH₂ column tandem for the simultaneous determination of hydrophobic atractylenolide I, II, III, atractylone and hydrophilic compounds glucose, fructose and sucrose in the dried rhizome of Atractylodes macrocephala Koidz (a natural raw material for health foods, Bai-Zhu aka. in Chinese). The method combines the different separation capabilities of reversed-phase liquid chromatography and hydrophilic interaction liquid chromatography. It can provides a new choice for the simultaneous determination of hydrophilic and hydrophobic compounds in traditional Chinese medicines and health foods. It provided a reference method for the quality control of Bai-Zhu. The results showed that the linear correlation coefficients of the established column tandem chromatographic method were all greater than 0.9990, the relative standard deviation was 0.1–2.8%, and the average recovery was 96.7–103.1%. The contents of atractylenolide I, II, III, atractylone, fructose, glucose, and sucrose in 17 batches of Baizhu were 172.3–759.8 μg/g, 201.4–612.8 μg/g, 160.3–534.2 μg/g, 541.4–8723.1 μg/g, 6.9–89.7 mg/g, 0.7–7.9 mg/g, and 1.2–21.0 mg/g, respectively. Full article