Search Results (117)

Background: Carbamazepine (CBZ) and aripiprazole (ARI), frequently detected in medical facility effluents, are resistant to conventional wastewater treatment. However, a systematic comparison of their electrolytic degradation product profiles under different electrode conditions using an identical operating platform has not been previously reported. Methods: CBZ and ARI in NaCl solutions were subjected to electrolytic oxidation using the Eleca^® system with either a boron-doped diamond (BDD) or a metal electrode. Residual drugs were quantified by LC-MS/MS and pseudo-first-order degradation kinetics were calculated. Transformation products were characterized by LC/PDA/HRMS/MS based on accurate mass measurements, MS/MS fragmentation, chromatographic behavior, and UV absorption. Radical scavenger experiments using methanol and tert-butanol were conducted to investigate reactive species’ contributions to degradation. Results: Both drugs were rapidly degraded under all conditions, with the metal electrode consistently exhibiting higher apparent pseudo-first-order rate constants than the BDD electrode. The metal electrode generated hydrophobic intermediates apparently retaining aromatic skeletons (consistent with partial oxidation), whereas the BDD electrode yielded more polar, low-molecular-weight products consistent with more extensive skeletal fragmentation (deep oxidation). Scavenger experiments suggested a greater relative contribution of hydroxyl radicals (•OH) under BDD electrode conditions. Transformation products were transiently detected but eliminated by prolonged electrolysis. Conclusions: Electrode material critically determines the degradation pathway, reactive species distribution, and product profile. Structural analysis of the tentatively identified transformation products suggests loss of pharmacophore integrity in several intermediates; however, residual pharmacological risk has not been experimentally validated and requires biological sassays for confirmation. Furthermore, the observed disappearance of the parent compounds does not demonstrate complete mineralization, detoxification, or environmental safety, as total organic carbon measurements and ecotoxicological assays were not performed. This study provides the first comparative characterization of transformation products of recalcitrant psychotropic drugs under metal vs. BDD electrode electrolysis, offering mechanistic insights for pharmaceutical wastewater treatment optimization. Full article

Background/Objectives: Hypericum perforatum L. is a medicinal plant containing diverse specialized metabolites, including flavonoids, naphthodianthrones, phloroglucinols, and phenolic acids. However, the relationship between its quantitative flavonoid composition and extract-level anti-inflammatory activity remains insufficiently characterized. This study aimed to profile the chemical constituents of H. perforatum extract (HPE), quantify selected flavonoid markers, and relate these data to nitric oxide (NO) inhibitory activity in LPS-stimulated RAW 264.7 macrophages. Methods: HPE was chemically characterized by LC–MS/MS, and selected flavonoid constituents were quantified using HPLC/PDA analysis. Cell viability and NO production were evaluated in RAW 264.7 macrophages using MTT and Griess assays, respectively. Results: LC–MS/MS profiling tentatively identified 36 compounds in HPE, with flavonoid-related metabolites representing the largest portion of the annotation list. Multiple quercetin-derived glycosides and conjugates were detected, indicating a flavonoid-rich phenolic profile. HPLC/PDA analysis showed that hyperoside (2) was the most abundant quantified marker at 12.44 mg/g extract, followed by rutin (1, 9.18 mg/g), quercetin (4, 6.64 mg/g), and avicularin (3, 5.55 mg/g), whereas amentoflavone (5) was detected only at trace level. At non-cytotoxic concentrations, HPE significantly suppressed LPS-induced NO production, iNOS protein expression, and the mRNA expression of the pro-inflammatory cytokines Tnf and Il6 in RAW 264.7 macrophages. Compounds 1–4 also reduced NO production and iNOS protein expression, although their effects on cytokine mRNA expression differed among compounds. Conclusions: HPE exhibited anti-inflammatory potential in LPS-stimulated macrophages, as shown by inhibition of NO production, downregulation of iNOS protein expression, and reduced Tnf/Il6 mRNA expression. However, extract-equivalent comparison indicated that the extract-level response could not be directly assigned to any single quantified flavonoid marker. The broader flavonoid-rich phenolic matrix may provide a plausible context for this response, but additive or synergistic interactions among constituents were not directly demonstrated and require further validation. Full article

Eruca vesicaria subsp. sativa (rocket) sprouts are a rich source of bioactive compounds used in cosmetics. Phytochemical profiling (LC-PDA-MS/MS) of 5-day-old sprouts identified 26 metabolites, mainly glucosinolates (e.g., glucoraphanin and glucoerucin) and flavonol glycosides of quercetin and kaempferol. The extracts exhibited strong antioxidant activity in DPPH^•, ABTS^•+, and ferric-reducing assays and moderate, dose-dependent inhibition of skin-degrading enzymes: tyrosinase, elastase, and collagenase, suggesting anti-wrinkle and skin-brightening effects. Cytotoxicity assays on human BJ skin fibroblasts demonstrated that the rocket sprout extracts were non-cytotoxic at concentrations up to 125 µg/mL, with low-dose treatments enhancing the cell viability. Hemocompatibility tests confirmed safety, with <2% hemolysis observed. The incorporation of these compounds into model emulsions yielded stable formulations over 90 days. These findings support the novelty of rocket sprout extracts as functional/nutricosmetic ingredients with relevance to both food and skin health. Full article

Background: Skin aging is driven by oxidative stress and ultraviolet (UV) exposure, leading to extracellular matrix degradation and loss of skin elasticity. This study aimed to identify the most biologically active Citrus species using a bioassay-guided approach and evaluate its potential for dermal applications. Methods: Hydroalcohol extracts and ethyl acetate fractions of Citrus sinensis, Citrus aurantifolia, and Citrus reticulata leaves were screened for antioxidant, enzyme-inhibitory, and polyphenol content. The most active fraction was characterized by UPLC-PDA and LC–MS/MS, formulated into Span-based nanovesicles, and evaluated for physicochemical properties and drug release. Biological activity was assessed using an in vitro scratch wound-healing assay on human dermal fibroblasts and a UVA-induced photoaging mouse model, supported by molecular dynamics simulations. Results: The ethyl acetate fraction of C. aurantifolia (CAE) exhibited the highest biological activity among the tested samples. This fraction showed potent antioxidant activity (DPPH IC₅₀ = 3.53 ± 0.05 µg/mL), marked inhibition of elastase (91.3%), collagenase (92.0%), and tyrosinase (80.2%), and a high total flavonoid content (110.49 mg rutin equivalents/g). Phytochemical profiling of CAE tentatively identified fourteen compounds, predominantly flavonoids, with hesperidin (30.4 mg/g) as a major constituent. The optimized nanovesicles (184 ± 0.9 nm, PDI 0.10, EE% 75.0%) enabled sustained hesperidin release. CAE and CAEnp enhanced fibroblast migration and accelerated wound closure at 24 h (p < 0.05). In vivo, CAEnp improved UVA-induced histopathological alterations and modulated oxidative stress-related markers by reducing p62/SQSTM1 by 28.7%, Keap1 expression to 21% compared with the CAE-treated group, and enhancing Nrf2, ARE, and NQO1 expression by 54.1%, 28.3%, and 57%, respectively. Molecular dynamics simulations supported stable hesperidin binding to elastase and suggested possible modulation of collagenase flexibility. Conclusions: The polyphenol-rich leaf fraction from C. aurantifolia, identified through comparative bioassay-guided fractionation, demonstrated antioxidant, enzyme-inhibitory, wound-healing, and photoprotective effects, particularly after nanoformulation. These findings support its potential for further development as a natural topical anti-aging candidate. Full article

Geisha coffee (Coffea arabica L. cv. Geisha) is internationally recognized for its exceptional sensory quality; however, its functional properties and bioactive composition remain insufficiently explored. This study evaluated the phytochemical profile, antioxidant capacity, vascular bioactivity, and toxicological safety of an aqueous extract of roasted Geisha coffee (AErGC) from the Chiriquí highlands, Panama. The chemical composition was determined using HPLC-PDA. Antioxidant activity was assessed using DPPH, ABTS, and lipid peroxidation assays. Vascular effects were studied in rat aortic rings, and safety was evaluated through Artemia salina and a single-dose acute oral toxicity model in rats (OECD 423). Chemical characterization was performed by HPLC-PDA, revealing notably elevated levels of caffeine (69.5 ± 6.4 mg/g) and 5-O-caffeoylquinic acid (74.5 ± 6.9 mg/g). The extract exhibited strong free radical scavenging capacity, with an IC₅₀ value of 14.7 ± 4.9 µg/mL in the DPPH assay, and inhibited lipid peroxidation by 72.71 ± 1.63% at 15.6 µg/mL. In endothelium-intact rings, AErGC induced a concentration-dependent vasorelaxant effect, reaching a maximum relaxation of 70.84 ± 2.9%. Toxicological results showed an LC₅₀ > 1000 µg/mL in A. salina and an oral LD₅₀ > 2000 mg/kg, classifying the extract as Category 5 (low toxicity). These findings highlight Panamanian Geisha coffee as a promising functional beverage with antioxidant and vascular protective properties, supporting its potential as a nutraceutical. Full article

Optimizing the extraction of bioactive compounds from Solidago sp. is essential for the development of plant-derived products with therapeutic and nutraceutical potential. Microwave-assisted (MW) and thermal maceration (TM) extraction of S. canadensis aerial parts were comparatively investigated to maximize total flavonoid content (TFC). The obtained extracts were subsequently freeze-dried for storage prior to chemical and biological analyses. Extraction conditions were optimized using a Box–Behnken design. Chemical characterization was performed by FTIR, HPLC-PDA, LC-MS/MS, and GC-MS, enabling detailed profiling of phenolic compounds and terpenoids. Antioxidant capacity was assessed using the DPPH radical scavenging assay, while cytotoxic activity was evaluated against HepG2, HCT-8, and HT-29 tumor cell lines, with HEK-293 cells used as a non-tumorigenic control cell line. Multivariate analysis (PCA) was applied to establish relationships between phytochemical composition and biological responses. Higher TFC values were obtained using MW extraction, whereas TM extracts exhibited greater antioxidant activity. Both extract types induced selective cytotoxic effects against tumor cell lines, while maintaining negligible toxicity toward normal HEK-293 cells. PCA revealed distinct clustering patterns between MW and TM extracts and confirmed a strong association between phenolic composition and bioactivity. The combination of optimized extraction, freeze-drying, and integrated chemical–biological evaluation produced S. canadensis extracts with well-defined phytochemical profiles and biological activity, supporting their potential use in nutraceutical, and pharmaceutical applications. Full article

Phthorimaea operculella is a globally distributed pest of solanaceous crops and represents one of the most critical constraints on potato production worldwide. The overuse of chemical insecticides has led to widespread resistance in pest populations, making entomopathogenic fungi a promising alternative strategy for sustainable agricultural pest management. In this study, a fungal strain designated ML-2 was isolated from naturally infected P. operculella larvae collected from a potato field in Yunnan province, China. Through morphological characteristics and ITS sequence analysis, strain ML-2 was identified as M. robertsii. The growth rate and sporulation yield on PDA and SDAY media were assessed, the virulence of ML-2 against eggs, larvae, and pupae of P. operculella were determined using the dipping method, and the data were analyzed via the time-concentration-mortality (TCM) model. The results showed that there were no significant differences in the growth rate of strain ML-2 on the two culture media (p > 0.05), whereas the sporulation yield on PDA medium was significantly higher than that on SDAY medium (p < 0.01). The highest corrected cumulative mortality rates for P. operculella larvae and pupae were 94.50% and 83.07% on day 7 after inoculation, respectively, while the highest cumulative mortality rate for eggs was relatively low at only 20.28%. Additionally, at a concentration of 1 × 10⁸ spores/mL, the LT₅₀ values of strain ML-2 against P. operculella larvae and pupae were 2.34 days and 2.72 days, respectively. On day 7 post-inoculation, the LC₅₀ values for larvae and pupae were 3.24 × 10⁷ conidia/mL and 9.64 × 10⁵ conidia/mL, respectively. In conclusion, M. robertsii ML-2 exhibits high potential as a candidate biopesticide and can be used in the sustainable integrated management of P. operculella. Full article

Combining plant-derived bioactives could produce effective anti-inflammatory interventions for myofascial inflammation. This study evaluated in vitro synergy and computational mechanisms of curcumin–evodiamine activity against TNF-α, IL-1β, iNOS and COX-2, with frontier molecular orbital analysis to inform putative mechanisms. Evodiamine and curcumin were identified/quantified by HPLC–PDA and LC–MS (λmax 226 nm and 426 nm; RT 8.61 and 9.53 min; [M−H]⁻m/z 302.2 and 367.2). Purities were 98.08 ± 1.92% and 98.04 ± 1.86%. Noncytotoxic concentrations in RAW264.7 cells were determined, then LPS-stimulated cells were treated with evodiamine (0.01 µM), curcumin (0.01 µM) and a 1:1 mixture (0.001 µM). Molecular docking against TNF-α, IL-1β, iNOS and COX-2 and HOMO–LUMO calculations were performed. Curcumin and the combination significantly reduced TNF-α and NO; curcumin and the combination reduced IL-1β, whereas evodiamine alone showed limited effects. Docking predicted stronger binding for curcumin and evodiamine than ibuprofen across targets (e.g., curcumin ΔG −10.18 kcal·mol⁻¹ for TNF-α; evodiamine ΔG −10.02 kcal·mol⁻¹ for COX-2). Frontier orbital energies indicated differing electronic profiles (ibuprofen ΔE 8.62 eV; evodiamine 9.65 eV; curcumin 9.89 eV), suggesting complementary reactivity. The curcumin–evodiamine combination exhibits in vitro anti-inflammatory activity with supportive docking and orbital data, providing mechanistic rationale for further development. Full article

The rising demand for sustainable and circular approaches in the agro-industrial sector has generated interest in repurposing herbal tea residues as sources of high-value bioactive compounds. This work focusses on recovering phytochemicals from Rosa canina L. peel and seed dust (by-products of processing of herbal tea in filter tea bags) using green extraction techniques. Two environmentally friendly technologies were used: ultrasound-assisted extraction (UAE) with a sonotrode and subcritical fluid extraction (SBFE). The extracts were qualitatively profiled using (HR) LC-ESI-QToF-MS/MS and quantified using HPLC-PDA. Both by-products contained phenolic substances, including gallic acid derivatives, ellagic acid, and flavonoids such as quercetin and quercetin-3-O-glucoside (only in the peel). Additionally, Folin–Ciocalteu’s assay was used to determine Total Phenolic content (TP). The extraction efficiency was considered in terms of phenolic compound recovery and total phenolic content obtained under the respective experimental conditions. The maximum TP for SBFE was reported in samples extracted with ethanol–water (48:52) at 180 °C, producing 3876.67 GAE mg/L for peel and 1648.57 GAE mg/L for seeds. In the UAE, extraction with ethanol–water (48:52) for 10 min yielded the maximum TP of 2773.81 GAE mg/L for peel and 957.86 GAE mg/L for seeds. These findings highlight the potential of R. canina infusion by-products as long-term sources of bioactive compounds for use in nutraceutical, cosmetic, and pharmaceutical industries. Full article

Pistacia lentiscus L. is widely reported in the ethnobotanical literature for its use in treating various pathologies, particularly skin disorders such as burns, inflammation, and wounds. These traditional applications suggest broader potential anti-aging activity and support the exploration of simple and sustainable extraction strategies. In this study, an aqueous extract obtained from leaf hydrodistillation residues, representing a by-product of essential oil production, was chemically characterized by LC-ESI-QToF-MS/MS and HPLC-PDA. The analysis identified 32 compounds, including 8 gallic acid derivatives, accounting for 70.7% of the total extract, and 24 flavonol glycosides. High total phenolic and flavonoid contents were associated with strong antioxidant activity, confirmed by the ABTS assay and by a dose-dependent intracellular ROS reduction in keratinocytes. The extract exhibited significant inhibitory activities against key skin-aging-related enzymes, with IC₅₀ of 33.8 µg/mL and 17.4 µg/mL, respectively for tyrosinase and elastase. Notably, strong anti-hyaluronidase activity, IC₅₀ 4.3 µg/mL, is reported here for the first time, while no collagenase inhibition was observed. The cytotoxicity assay demonstrated a favorable safety profile at biologically active concentrations. Overall, these results highlight the bioactivity of the P. lentiscus phenolic phytocomplex and support the valorization of hydrodistillation aqueous residues as a sustainable source of multifunctional bioactive compounds for dermocosmetic applications. Full article

Conventional immunochromatographic assays (ICAs) face limitations in sensitivity and dynamic range, hindering their application in on-site, class-specific screening of sulfonylurea (SU) adulteration in functional foods. To address this, a signal amplification strategy was developed by engineering high-density platinum nanozymes on a mesoporous metal–organic framework (PCN-224). The mesoporous architecture of PCN-224 facilitated high-density and stable loading of catalytically active Pt sites. The established PCN-224@Pt-based ICA achieved detection limits of 0.52–7.94 μg/kg in tea and 0.69–7.02 μg/kg in capsules, with linear ranges of 1.69–513.01 μg/kg and 2.05–716.47 μg/kg, respectively. Compared with traditional colloidal gold immunochromatographic assays (CG-ICAs), sensitivity was improved by up to 57-fold, while the linear detection range was expanded by over 5-fold relative to the previously reported PCN-224@PDA- ICA. The method demonstrated recovery rates of 81.8–119.8% and coefficients of variation between 2.5% and 11.4%. Validation against LC-MS/MS using 20 real samples showed excellent agreement (R² > 0.99). This work not only provides a sensitive and rapid tool for the surveillance of SU adulteration in functional foods but also establishes a generalizable nanozyme design strategy applicable to enhancing the performance of a wide range of ICA-based detection platforms. Full article

Projects integrating Science, Technology, Engineering, and Mathematics (STEM) are essential to interdisciplinary research. This study presents a STEM (Science, Technology, Engineering, and Mathematics) methodology with the primary objective of designing, constructing, and validating a functional cannabinoid extraction device. To inform the device’s drying parameters, the dehydration kinetics of female hemp buds or flowering buds (FHB) were first analyzed using infrared drying at 100 °C for different durations. The plants were cultivated and harvested in accordance with good agricultural practices using Dinamed CBD Autoflowering seeds. The FHB were harvested and prepared by manually separating them from the stems and leaves. Six 5 g samples were prepared, each with a slab geometry of varying surface area and thickness. Two of these samples were ground: one into a fine powder and the other into a coarse powder. Mathematical fits were obtained for each resulting curve using either an exponential decay model or the logarithmic equation $y\left(t\right)=A\left(e^{-kt}\right)+y_0$ calculate the equilibrium moisture (m_E). The Moisture Rate (MR) was calculated, and by modelling with the logarithmic equation, the constant k and the effective diffusivity (Deff) were determined with the analytical solution of Fick’s second law. The Deff values (ranging from 10⁻⁷ to 10⁻⁵) were higher than previously reported. The coarsely ground powder sample yielded the highest k and Deff values and was selected for oil extraction. The device was then designed using Quality Function Deployment (QFD), specifically the House of Quality (HoQ) matrix, to systematically translate user requirements into technical specifications. A 200 g sample of coarsely ground, dehydrated FHB was prepared for ethanol extraction. Chemical results obtained by Liquid Chromatography coupled with Photodiode Array Detection (LC-PDA) revealed the presence of THC, CBN, CBC, and CBG. The extraction device design was validated using previous results showing the presence of CBD and CBDA. The constructed device successfully extracted cannabinoids, including Δ9-THC, CBG, CBC, and CBN, from coarsely ground FHB, validating the integrated STEM approach. This work demonstrates a practical framework for developing accessible agro-technical devices through interdisciplinary collaboration. Full article

Rowanberries (Sorbus aucuparia) are valued for their high content of bioactive compounds. This study examined the effects of sweeteners (sucrose, xylitol, erythritol, steviol glycosides), fruit pulp preparation (fresh vs. steamed), and storage conditions (4 °C and 30 °C, 3 months) on the composition of rowanberry nectars. Polyphenols were quantified using LC-PDA-QTOF/MS and UPLC-PDA-FL, and carotenoids, organic acids, antioxidant capacity (FRAP), and physicochemical properties were also determined. Steaming increased total polyphenol levels in nectars by 13–52%, with the highest values observed in formulations containing steviol glycosides (up to 1833 mg/100 mL). Changes in carotenoid content during storage varied depending on the sweetener type. In steamed nectars with erythritol stored at 4 °C, carotenoid levels remained close to those measured in the corresponding unsweetened steamed sample. Storage influenced turbidity and viscosity in all variants, with the largest viscosity increases recorded in stevia- and erythritol-sweetened nectars. Overall, the combined effects of fruit preparation, sweetener type, and storage determined the final composition and stability of rowanberry nectars. Full article

Small ruminant production under grazing conditions plays a crucial role in the global primary sector economy. However, these animals are highly susceptible to gastrointestinal nematodes (GINs), which significantly impact their health and welfare. Given the increasing resistance to conventional anthelmintics, there is a pressing need to explore sustainable alternatives, such as plant secondary metabolites. This study aimed to identify phenolic compounds with anthelmintic activity from Tithonia diversifolia aerial parts, using Haemonchus contortus as a biological model. Egg hatching inhibition (EHI) and larval mortality assays were used to evaluate the anthelmintic activity of a hydroalcoholic extract (HA-E), an aqueous (Aq-F) and ethyl acetate fraction (EtOAc-F), and eight bioactive subfractions (TdR1-TdR8) obtained from EtOAc-F. The identification of major compounds was performed using HPLC-PDA. The E-HA and EtOAc-F achieved 100% EHI at 40 and 4 mg/mL, respectively. The subfractions TdR2 (EC₉₀ = 0.55 mg/mL), TdR3 (EC₉₀ = 0.12 mg/mL), and TdR4 (EC₉₀ = 0.26 mg/mL) exhibited the highest ovicidal activity. In the larval mortality test, EtOAc-F showed an LC₈₅ of 56.74 mg/mL. The major identified compounds included cinnamates, hydroxycinnamic acids (e.g., caffeic acid and chlorogenic acid), gallates, flavonoids (flavones and flavanones), and coumarins. These findings support the potential of T. diversifolia as a promising natural source for the control of GINs in small ruminants. Full article

Arachidonic acid (AA) is a polyunsaturated fatty acid, an essential component of the brain membrane phospholipids. It is released into the bloodstream in response to various pathological conditions. Its potential as a biomarker for oxidative membrane damage determines the importance of its reliable quantification. Therefore, the aim of the current study was to develop a simple and robust LC-MS method that is easy to implement for routine testing of free arachidonic acid (AA) in human serum. The method included a simple two-step sample preparation procedure based on liquid–liquid extraction and protein precipitation, followed by AA analysis by UPLC coupled with PDA and QDa detectors. The ICH M10 guideline was followed for validation studies. The method demonstrated high selectivity and linearity with R² = 0.9952 for solvent-based and R² = 0.9979 for matrix-matched calibration. The LODs and LOQs were 0.046 µg/mL and 0.133 µg/mL, respectively. The accuracy and precision were between 6 and 14% RSD. No carry-over and matrix interferences were observed. The method was successfully applied to real serum samples, where AA concentrations ranged from 0.82 to 2.69 µg/mL, consistent with data of other studies. This method provides a reliable, reproducible, and rapid alternative for AA quantification in research and routine practice. Full article