Search Results (35)

Extensive research on amphibians has focused on areas such as morphological and molecular taxonomy, ecology, embryology, and molecular phylogeny. However, the structure and biotechnological potential of egg jelly—which plays a protective and nutritive role for embryos—have remained largely unexplored. This study presents, for the first time, a detailed physicochemical analysis of the egg jelly of Pelophylax ridibundus, an amphibian species, using Fourier Transform Infrared Spectroscopy, Thermogravimetric Analyzer, X-ray Diffraction, and elemental analysis. The carbohydrate content was determined via High-Performance Liquid Chromatography analysis, and the protein content was identified using Liquid Chromatography-Tandem Mass Spectrometry analysis. Additionally, it was revealed that this jelly exhibits a significant cytotoxic effect on melanoma cells (viability < 30%) while showing no cytotoxicity on healthy dermal fibroblast cells (viability > 70%). Consequently, this non-toxic, biologically derived, and cultivable material is proposed as a promising candidate for cancer applications, paving the way for further research in the field. Full article

Kefir, a fermented milk product produced using kefir grains, is a symbiotic consortium of bacteria and yeasts responsible for driving the fermentation process. In this study, an in-depth analysis of kefir’s lipid profile was conducted, with a focus on its phospholipid (PL) content, employing liquid chromatography with high-resolution mass spectrometry (LC-HRMS). Nearly 300 distinct polar lipids were identified through hydrophilic interaction liquid chromatography (HILIC) coupled with electrospray ionization (ESI) and Fourier-transform orbital-trap MS and linear ion-trap tandem MS/MS. The identified lipids included phosphatidylcholines (PCs), lyso-phosphatidylcholines (LPCs), phosphatidylethanolamines (PEs) and lyso-phosphatidylethanolamines (LPEs), phosphatidylserines (PSs), phosphatidylglycerols (PGs), and phosphatidylinositols (PIs). The presence of lysyl-phosphatidylglycerols (LyPGs) was identified as a key finding, marking a lipid class characteristic of Gram-positive bacterial membranes. This discovery highlights the role of viable bacteria in kefir and underscores its probiotic potential. The structural details of minor glycolipids (GLs) and glycosphingolipids (GSLs) were further elucidated, enriching the understanding of kefir’s lipid complexity. Fatty acyl (FA) composition was characterized using reversed-phase LC coupled with tandem MS. A mild epoxidation reaction with meta-chloroperoxybenzoic acid (m-CPBA) was performed to pinpoint double-bond positions in FAs. The dominant fatty acids were identified as C18:3, C18:2, C18:1, C18:0 (stearic acid), C16:0 (palmitic acid), and significant levels of C14:0 (myristic acid). Additionally, two isomers of FA 18:1 were distinguished: ∆9-cis (oleic acid) and ∆11-trans (vaccenic acid). These isomers were identified using diagnostic ion pairs, retention times, and accurate m/z values. This study provides an unprecedented level of detail on the lipid profile of kefir, shedding light on its complex composition and potential nutritional benefits. Full article

In this work, mesoporous silicas with two types of mesoporous structures were synthesized and functionalized with sulfonic acid groups: MCM-41-SO₃H (honeycomb-like hexagonal structure) and MSU-2-SO₃H (three-dimensional porous structure with wormhole pores). The synthesized materials were characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscopy, nitrogen adsorption–desorption, Fourier-transform infrared spectroscopy, ²⁹Si solid-state nuclear magnetic resonance spectroscopy, and elemental analysis. The obtained functionalized materials were evaluated as sorbents for strong cation-exchange solid-phase extraction (SPE) to determine their efficiency in the adsorption and desorption of tropane alkaloids (atropine and scopolamine). The loading solvents, loading volume, analyte concentration, and elution volume were studied, using 50 mg of both materials. Analyses were carried out by ultra-high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry. The synthesized MCM-41-SO₃H material presented the highest recovery efficiency and has proven to be a promising sorbent for strong cation-exchange SPE of atropine and scopolamine in aqueous media. The high degree of functionalization of MCM-41-SO₃H and the high accessibility of the sulfonic groups for the target analytes, due to the regularity and uniformity of their pores, maximize the contact between the alkaloids and the sorbent, favoring efficient adsorption. Full article

Sambucus sibirica, a deciduous shrub from the Adoxaceae family, is a traditional Kazakh medicine used in Xinjiang, China. Its branches, leaves, and fruits are used to treat fractures, rheumatoid arthritis, and nephritis. To advance research on S. sibirica, we conducted studies on its microscopic identification, chemical composition, and biological activity. The cross-sectional features of the branches, leaves, and fruits were observed under a microscope, revealing different types of ducts, cork cells, non-glandular hairs, oil droplets, stone cells, scale hairs, and star-shaped hairs in the S. sibirica powders. Fourier transform infrared spectroscopy (FTIR) was used to characterize the presence of specific chemical groups, revealing similarities and differences between different parts. Thin-layer chromatography (TLC) confirmed that chlorogenic acid was present in the branches, leaves, and fruits, whereas rutin was more prominent in the leaves. The total flavonoid contents were determined by a photocolorimetric approach and resulted in values of 7419.80, 5193.10, and 3629.10 μg·g⁻¹ (dry weight) for the leaves, branches, and fruits, respectively. Further qualitative and quantitative analyses via ultra-performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry (UPLC-QqQ-MS/MS) identified rutin, chlorogenic acid, quercetin, isoquercetin, and astragalin, with contents ranging from 1.00 to 4535.60 μg·g⁻¹ (dry weight). Antioxidant tests revealed that the branches, leaves, and fruits of S. sibirica presented antioxidant properties, with the leaves demonstrating the highest activity, followed by the branches and fruits. These results align with the results of the quantitative analysis. This study provides valuable insights into the microscopic features, chemical composition, and antioxidant activity of S. sibirica, laying the foundation for its pharmacognosy research and quality standards and offering a reference for its future development and utilization. Full article

The chemical compounds found in propolis vary according to plant sources, species, and geographical regions. To date, Indonesian propolis has not yet become standardized in terms of its chemical constituents. Thus, this study aimed to identify the presence of marker compounds and determine whether different classes of Indonesian propolis exist. In this study, yields, total polyphenol content (TPC), total flavonoid content (TFC), and antioxidants were measured. Identification of chemical compounds was carried out with Fourier-transform infrared (FTIR) spectroscopy and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Metaboanalyst 6.0 was employed in conducting principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA) using the results of the FTIR and LC-MS/MS. The propolis with the highest TFC, TPC, and antioxidant activity was Geniotrigona thoracica from North Sumatra. The results of propolis compound mapping based on region with discriminant analysis revealed that types of propolis from Java have similar characteristics. Then, based on species, the types of propolis from Tetragonula laeviceps and Heterotrigona itama have special characteristics; the samples from these species can be grouped according to similar characteristics. In conclusion, 10 potential marker compounds were identified in Indonesian propolis, enabling regional and species-specific varieties of Indonesian propolis to be classified based on chemical composition mapping. Full article

The main goal of this study was to assess the bioactive and polysaccharide compositions, along with the antioxidant and antibacterial potentials, of five seaweeds collected from the northeastern coast of Algeria. Through Fourier transform infrared spectroscopy analysis and X-ray fluorescence spectroscopy, the study investigated the elemental composition of these seaweeds and their chemical structure. In addition, this study compared and identified the biochemical makeup of the collected seaweed by using cutting-edge methods like tandem mass spectrometry and ultra-high-performance liquid chromatography, and it searched for new sources of nutritionally valuable compounds. According to the study’s findings, Sargassum muticum contains the highest levels of extractable bioactive compounds, showing a phenolic compound content of 235.67 ± 1.13 µg GAE·mg⁻¹ and a total sugar content of 46.43 ± 0.12% DW. Both S. muticum and Dictyota dichotoma have high concentrations of good polyphenols, such as vanillin and chrysin. Another characteristic that sets brown algae apart is their composition. It showed that Cladophora laetevirens has an extracted bioactive compound content of 12.07% and a high capacity to scavenge ABTS⁺ radicals with a value of 78.65 ± 0.96 µg·mL⁻¹, indicating high antioxidant activity. In terms of antibacterial activity, S. muticum seaweed showed excellent growth inhibition. In conclusion, all five species of seaweed under investigation exhibited unique strengths, highlighting the variety of advantageous characteristics of these seaweeds, especially S. muticum. Full article

In this study, a highly efficient magnetic molecularly imprinted polymer nanocomposite material was prepared using multi-walled carbon nanotubes as carriers. The characterization of the obtained nanocomposite material was conducted using Fourier transform infrared spectroscopy, a vibrating sample magnetometer, a thermogravimetric analyzer, a scanning electron microscope, and a transmission electron microscope. The adsorption properties of the nanocomposite material were evaluated through adsorption experiments, including static adsorption, dynamic adsorption, and selective recognition studies. The prepared nanocomposite material, serving as a selective adsorbent, was applied in magnetic solid-phase extraction. Subsequently, the derivatized samples were analyzed for glucose in fish serum using liquid chromatography–tandem mass spectrometry. Under optimal conditions, the detection limit was 0.30 ng/mL, the quantitation limit was 0.99 ng/mL, satisfactory spiked recovery rates were obtained, and the relative standard deviation was less than 1.1%. Using 2-deoxy-D-ribose as the template molecule and a structural analog of glucose allowed us to eliminate the potential template leakage in qualitative and quantitative analyses, effectively avoiding the issues of false positives and potential quantitative errors, compared to traditional methods. A method for detecting glucose levels in fish serum based on molecularly imprinted polymer technology has been successfully developed to determine the stress and health levels of fish. Full article

A novel co-bonded octyl and pyridine silica (OPS) sorbent was prepared and applied for the solid phase extraction (SPE) of cyclopiazonic acid (CPA, a type of mycotoxin) in feed and agricultural products for the first time. A simple mixed-ligand one-pot reaction strategy was employed for OPS sorbent preparation. Nitrogen adsorption–desorption measurements, elemental analysis (EI), thermal gravimetric analysis (TGA), and Fourier transform infrared spectroscopy (FT-IR) analysis demonstrated the successful immobilization of octyl and quaternary ammonium groups onto the surface of silica gel. The large specific surface area, high-density functional groups, and mixed-mode anion-exchange characteristics of these silica particles made them the ideal material for the efficient extraction of CPA. Additionally, the OPS sorbents displayed excellent batch-to-batch reproducibility, satisfactory reusability, and low cost. The SPE parameters were optimized to explore the ionic and hydrophobic interactions between CPA and the functional groups, and the ultra-high performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry (UPLC-MS/MS) parameters were optimized to obtain a desirable extraction efficiency and high sensitivity to CPA. Meanwhile, the OPS sorbent presented a satisfactory extraction selectivity and low matrix effect. Under the optimized conditions, our developed CPA detection method was used to determine CPA level in rice, wheat flour, corn flour, peanut, and feed samples, exhibiting a lower detection limit, better linearity, higher sensitivity, and satisfactory extraction recovery rate than previously reported methods. Therefore, our method can be preferentially used as a method for the detection of CPA in agricultural products and feeds. Full article

Flavonoids are important secondary metabolites found in Juglans mandshurica Maxim., which is a precious reservoir of bioactive substances in China. To explore the antitumor actions of flavonoids (JMFs) from the waste branches of J. mandshurica, the following optimized purification parameters of JMFs by macroporous resins were first obtained. The loading concentration, flow rate, and loading volume of raw flavonoid extracts were 1.4 mg/mL, 2.4 BV/h, and 5 BV, respectively, and for desorption, 60% ethanol (4 BV) was selected to elute JMFs-loaded AB-8 resin at a flow rate of 2.4 BV/h. This adsorption behavior can be explained by the pseudo-second-order kinetic model and Langmuir isotherm model. Subsequently, JMFs were identified using Fourier transform infrared combined with high-performance liquid chromatography and tandem mass spectrometry, and a total of 156 flavonoids were identified. Furthermore, the inhibitory potential of JMFs on the proliferation, migration, and invasion of HepG2 cells was demonstrated. The results also show that exposure to JMFs induced apoptotic cell death, which might be associated with extrinsic and intrinsic pathways. Additionally, flow cytometry detection found that JMFs exposure triggered S phase arrest and the generation of reactive oxygen species in HepG2 cells. These findings suggest that the JMFs purified in this study represent great potential for the treatment of liver cancer. Full article

Galleria mellonella is a lepidopteran whose larval stage has shown the ability to degrade polystyrene (PS), one of the most recalcitrant plastics to biodegradation. In the present study, we fed G. mellonella larvae with PS for 54 days and determined candidate enzymes for its degradation. We first confirmed the biodegradation of PS by Fourier transform infrared spectroscopy- Attenuated total reflectance (FTIR-ATR) and then identified candidate enzymes in the larval gut by proteomic analysis using liquid chromatography with tandem mass spectrometry (LC-MS/MS). Two of these proteins have structural similarities to the styrene-degrading enzymes described so far. In addition, potential hydrolases, isomerases, dehydrogenases, and oxidases were identified that show little similarity to the bacterial enzymes that degrade styrene. However, their response to a diet based solely on polystyrene makes them interesting candidates as a potential new group of polystyrene-metabolizing enzymes in eukaryotes. Full article

Currently, ultrashort oligopeptides consisting of fewer than eight amino acids represent a cutting-edge frontier in materials science, particularly in the realm of hydrogel formation. By employing solid-phase synthesis with the Fmoc/tBu approach, a novel pentapeptide, FEYNF-NH₂, was designed, inspired by a previously studied sequence chosen from hen egg-white lysozyme (FESNF-NH₂). Qualitative peptide analysis was based on reverse-phase high performance liquid chromatography (RP-HPLC), while further purification was accomplished using solid-phase extraction (SPE). Exact molecular ion confirmation was achieved by matrix-assisted laser desorption–ionization mass spectrometry (MALDI-ToF MS) using two different matrices (HCCA and DHB). Additionally, the molecular ion of interest was subjected to tandem mass spectrometry (MS/MS) employing collision-induced dissociation (CID) to confirm the synthesized peptide structure. A combination of research techniques, including Fourier-transform infrared spectroscopy (FTIR), fluorescence analysis, transmission electron microscopy, polarized light microscopy, and Congo red staining assay, were carefully employed to glean valuable insights into the self-assembly phenomena and gelation process of the modified FEYNF-NH₂ peptide. Furthermore, molecular docking simulations were conducted to deepen our understanding of the mechanisms underlying the pentapeptide’s supramolecular assembly formation and intermolecular interactions. Our study provides potential insights into amyloid research and proposes a novel peptide for advancements in materials science. In this regard, in silico studies were performed to explore the FEYNF peptide’s ability to form polyplexes. Full article

Per- and polyfluoroalkyl substances (PFAS) are anthropogenic compounds developed for various applications; some are connected to adverse health impacts including immunosuppression and higher susceptibility to some cancers. Current PFAS remediation treatments from aqueous sources include granular activated carbon (GAC) adsorption, membrane separation, and anion-exchange resin (AER) removal. Each has specific disadvantages, hence the need for a new and efficient technology. Herein, acrylamide-based hydrogel composites were synthesized with powdered activated carbon (PAC) and characterized to determine their affinity for PFAS. Physicochemical characterization included Fourier-Transform infrared spectroscopy (FTIR) to identify chemical composition, thermogravimetric analysis (TGA) to confirm PAC loading percentage, and aqueous swelling studies to measure the effect of crosslinking density. FTIR showed successful conversion of carbonyl and amine groups, and TGA analysis confirmed the presence of PAC within the network. Surface characterization also confirmed carbon-rich areas within composite networks, and the swelling ratio decreased with increasing crosslinking density. Finally, sorption of PFAS was detected via liquid chromatography with tandem mass spectrometry (LC-MS/MS), with removal efficiencies of up to 98% for perfluorooctanoic sulfonic acid (PFOS) and 96% for perfluorooctanoic acid (PFOA). The developed hydrogel composites exhibited great potential as advanced materials with tunable levers that can increase affinity towards specific compounds in water. Full article

Lately, the essential oils industry has been one of the most expanding markets globally. However, the byproducts generated after the distillation of aromatic plants and their transformation to novel high-added value products consist of a major up-to-date challenge. Thus, the scope of the current study is the optimization of ultrasound-assisted extraction (UAE) for the recovery of phenolic compounds from rose (Rosa damascena) post-distillation side streams using Box–Behnken design. In particular, the highest total phenolic content (TPC) was achieved at 71% v/v ethanol–water solution, at 25 min, 40 mL/g dry sample and 53% ultrasound power, while ethanol content and extraction time were the most crucial factors (p-value ≤ 0.05) for UAE. Both solid (RSB) and liquid (LSB) rose side streams exhibited significant antiradical and antioxidant activities. The interpretation of attenuated total reflection-Fourier transform infrared (ATR-FTIR) spectra confirmed the presence of compounds with properties such as phenolic compounds, phenolic amide derivatives, and alcohols in the extracts. Moreover, the flavonoids naringenin, quercetin, and kaempferol were the major phenolic compounds, identified in the extracts by liquid chromatography-tandem mass spectrometry analysis (LC-MS/MS), followed by gallic, protocatechuic, p-hydroxybenzoic, and rosmarinic acids. Furthermore, the LC-MS/MS results pinpointed the effect of factors other than the extraction conditions (harvesting parameters, climatic conditions, plant growth stage, etc.) on the phenolic fingerprint of RSB extracts. Therefore, RSB extracts emerge as a promising alternative antioxidant agent in food products. Full article

This study investigates the ethanolic extract of dried walnut (Juglans regia L.) shells upon hammer milling (HM) and ball milling (BM) grinding processes. Marked differences were observed in the attenuated total reflection Fourier-transform infrared (ATR-FTIR) spectra. The two extracts were investigated by reversed-phase liquid chromatography coupled with electrospray ionization and high-resolution mass spectrometry (RPLC-ESI-HRMS). Following enzymatic digestion, the fatty acids (FAs) were examined, and tandem MS of epoxidized species was applied to establish the C-C double bond position; the most abundant species were FA 18:2 Δ^9,12, FA 18:1 Δ⁹, and FA 18:3 Δ^9,12,15. However, no significant qualitative differences were observed between FAs in the two samples. Thus, the presence of potential active secondary metabolites was explored, and more than 30 phenolic compounds, including phenols, ellagic acid derivatives, and flavonoids, were found. Interestingly, the HM samples showed a high concentration of ellagitannins and hydrolyzable tannins, which were absent in the BM sample. These findings corroborate the greater phenolic content in the HM sample, as evaluated by the Folin–Ciocalteu test. Among the others, the occurrence of lanceoloside A at m/z 391.1037 [C₁₉H₂₀O₉-H]⁻, and a closely related benzoyl derivate at m/z 405.1190 (C₂₀H₂₂O₉-H]⁻), was ascertained. The study provides valuable information that highlights the significance of physical pre-treatments, such as mill grinding, in shaping the composition of extracts, with potential applications in the biorefinery or pharmaceutical industries. Full article

Antibiotic drug residues can adversely affect the human body. Lincomycin is a common veterinary drug that can form residues in foods of animal origin. However, the detection of trace residue levels of lincomycin residues in real samples is challenging. Here, a simple solid phase extraction (SPE) method was developed for the enrichment of lincomycin from cow milk samples before its detection by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The adsorbent used in the SPE was a Cu-based metal-organic framework (Cu-MOF) prepared by the solvothermal synthesis approach. The prepared MOFs were characterized using scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FT-IR), X-ray diffractometry (XRD), differential thermogravimetric analysis (TG-DTA), and N2 adsorption-desorption experiments. The adsorption capacity (adsorption equilibrium, extraction time, pH), and elution solvent parameters were investigated. Under the optimized conditions of the HPLC-MS/MS method, lincomycin was detected in the linear range of 10–200 g/L with a detection limit of 0.013 ng/mL. Commercial milk samples were spiked with lincomycin, and a recovery rate between 92.3% and 97.2% was achieved. Therefore, the current method can be successfully applied for the enrichment and determination of lincomycin from milk samples. Full article