Search Results (66)

Knowledge about the composition (volatile and non-volatile) and functionality of natural extracts from Mediterranean plants serves as a basis for their further application. In this study, five selected plants were used for the extraction of plant metabolites. Leaves and flowers of Critmum maritimum, Rosmarinus officinalis, Olea europea, Phylliera latifolia and Mellisa officinalis were collected, and a total of 12 extracts were prepared. Extractions were performed under microwave-assisted conditions, with two solvent types: water (W) and a hydroalcoholic (ethanolic) solution (HA). Detailed extract analysis was conducted. Phenolics were analyzed by detecting individual bioactive compounds using high-performance liquid chromatography and by calculating total phenolic and total flavonoid content through spectrophotometric analysis. Higher concentrations of total phenolics and total flavonoids were obtained in the hydroalcoholic extracts, with the significantly highest total phenolic and flavonoid values in the rosemary hydroalcoholic extract (3321.21 mg_GAE/L) and sea fennel flower extract (1794.63 mg_QE/L), respectively; and the lowest phenolics in the water extract of olive leaves (204.55 mg_GAE/L) and flavonoids in the water extracts of sea fennel leaves, rosemary, olive and mock privet (around 100 mg_QE/L). Volatile organic compounds (VOC) were detected using HS-SPME/GC–MS (Headspace Solid-Phase Microextraction coupled with Gas Chromatography-Mass Spectrometry), and antioxidant capacity was estimated using DPPH (2,2-diphenyl-1-picrylhydrazyl assay) and FRAP (Ferric Reducing Antioxidant Power) methods. HS-SPME/GC–MS analysis of samples revealed that sea fennel had more versatile profile, with the presence of 66 and 36 VOCs in W and HA sea fennel leaf extracts, 52 and 25 in W and HA sea fennel flower extracts, 57 in rosemary W and 40 in HA, 20 in olive leaf W and 9 in HA, 27 in W mock privet and 11 in HA, and 35 in lemon balm W and 10 in HA extract. The lowest values of chlorophyll a were observed in sea fennel leaves (2.52 mg/L) and rosemary (2.21 mg/L), and chlorophyll b was lowest in sea fennel leaf and flower (2.47 and 2.25 mg/L, respectively), while the highest was determined in olive (6.62 mg/L). Highest values for antioxidant activity, determined via the FRAP method, were obtained in the HA plant extracts (up to 11,216 mg_AAE/L for lemon balm), excluding the sea fennel leaf (2758 mg_AAE/L) and rosemary (2616 mg_AAE/L). Considering the application of these plants for fresh fish preservation, antimicrobial activity of water extracts was assessed against Vibrio fischeri JCM 18803, Vibrio alginolyticus 3050, Aeromonas hydrophila JCM 1027, Moraxella lacunata JCM 20914 and Yersinia ruckeri JCM 15110. No activity was observed against Y. ruckeri and P. aeruginosa, while the sea fennel leaf showed inhibition against V. fisheri (inhibition zone of 24 mm); sea fennel flower was active against M. lacunata (inhibition zone of 14.5 mm) and A. hydrophila (inhibition zone of 20 mm); and rosemary and lemon balm showed inhibition only against V. fisheri (inhibition zone from 18 to 30 mm). This study supports the preparation of natural extracts from Mediterranean plants using green technology, resulting in extracts rich in polyphenolics with strong antioxidant potential, but with no clear significant antimicrobial efficiency at the tested concentrations. Full article

This paper reviews the research progress on ionogels in flexible pressure sensors. Ionogels comprise solid carrier networks and ionic liquids (ILs) dispersed therein and have good non-volatility, high conductivity, thermal stability, a wide electrochemical window, and mechanical properties. These characteristics give ionogels broad application prospects in wearable electronic devices, intelligent robots, and healthcare. The article first introduces the classification of ionogels, including the classification based on ILs and solid carrier networks. Then, the preparation methods and processing technologies of ionogels, such as the direct mixing method, in situ polymerization/gel method, and solvent exchange method, are discussed. Subsequently, the article expounds in detail on the properties and modification methods of ionogels, including toughness, conductivity, hydrophobicity, self-healing, and adhesiveness. Finally, the article focuses on the application of ionogels in flexible pressure sensors and points out the challenges faced in future research. The language of this mini-review is academic but not overly technical, making it accessible to even researchers new to the field and establishing an overall impression of research. We believe this mini-review serves as a solid introductory resource for a niche topic, with large and clear references for further research. Full article

Amomum villosum L. is a perennial herbaceous belonging to the ginger family. Due to its unique aroma, it is widely used in alcoholic beverages and food processing. Unfortunately, issues with bitterness and sourness occur, which affect the taste and quality of processed products. In this study, the non-volatile sour and bitter substances in Amomum villosum L. were systematically isolated, purified, and characterized through a combination of chromatographic separation techniques and ultra-performance liquid chromatography–quadrupole time-of-flight mass spectrometry (UPLC/Q-TOF-MS). The results indicate that three sour compounds (DL-malic acid, protocatechuic acid, and p-hydroxybenzoic acid) and one bitter compound (catechin) were identified for the first time in Amomum villosum L. The in vitro anti-tumor activity was screened and determined using Cell Counting Kit-8 (CCK-8) assays, a 5-Ethynyl-2′-deoxyuridine (EdU) staining experiment, and scratch assays. The results reveal that the bitter substance of catechin (25–100 μg/mL) exhibited significant inhibitory effects, which inhibited the proliferation and migration of human non-small cell lung cancer A549 cells through dose-dependent mechanisms. This investigation also reveals the influence of different traditional extraction solvents on the degree of bitterness and sourness in Amomum villosum extracts, providing a theoretical basis for improving the quality and pharmacological utilization of Amomum villosum extracts. Full article

In this work, the development of FDCA-based polyester resins for coil coatings in industrial environment is presented. The goal of our research was to prepare industrial coatings made from renewable materials with the same performance as the standard coating. Resins with 1%–41% of FDCA on polymer were synthesized and then used in a formulation for primer. Resins were characterized by the determination of non-volatile matter, acid value, hydroxyl value, glass transition temperature, and measurement of viscosity, color and molecular weight. Coatings were characterized by the determination of viscosity, density, non-volatile matter, adhesion, T-test, MEK test, reverse impact, and pencil hardness, as well as the measurement of gloss. FTIR measurements confirmed successful incorporation of FDCA into the polymer. The results showed that resins with up to 31% of FDCA on polymer can be used to prepare coil coating where the properties of resins comply with the requirements and are comparable to the properties of standard resin. Resins had non-volatile matter between 59.0 and 60.1%, an acid value up to 4.6 mg KOH/g, a hydroxyl value of 22.0–24.9 mg KOH/g and viscosity at 23 °C between 6100 and 7500 mPa.s. Nevertheless, with the increase in FDCA in the formulation, discoloration of the resin occurred and incompatibility with the solvents was observed, while up to 10 °C lower glass transition temperatures and up to 28% lower molecular weights of the resins were determined. For coatings prepared from FDCA-based resins, the properties improved or were comparable to the properties of coating prepared from standard resin. Adhesion improved with higher content of FDCA in the resin from 2 Gt to 0 Gt, while all coatings had gloss at 60° of 39%–41%, a reverse impact of 10 J and a pencil hardness of H/2H. T-bend test results varied between 2 T and 0.5 T and the results of the MEK test showed resistance > 100 DR. Full article

The members of the genus Helichrysum Mill. are notable for producing a diverse range of structurally intricate secondary metabolites, being the focus of current phytochemical research. Their importance is recognized as several species hold significant ethnopharmacological value, being traditionally used to address ailments in human systems, such as respiratory, gastrointestinal, and urinary conditions, among others. This study used liquid chromatography coupled with high-resolution mass spectrometry results to present the phytochemical composition of non-volatile secondary metabolites in 11 Greek Helichrysum taxa (species and subspecies). For the first time, their total polyphenol content is comparatively assessed and an overview of the non-volatile compounds for five Endangered or Critically Endangered Greek Endemic Helichrysum taxa are presented herein. Almost all of the studied Helichrysum taxa differed significantly in the mean values of their polyphenolic content, except for H. doerfleri and H. heldreichii. A particular emphasis was placed on extracting polyphenols from a cultivated genotype of H. amorginum using aqueous pressurized liquid extraction as an alternative to the traditional organic solvent extraction method. Analysis by high-performance liquid chromatography revealed that this method increased the concentration of neochlorogenic acid and astragalin, compared to other extraction conditions. These findings highlight the potential of alternative extraction techniques for obtaining natural products from sustainably managed phytogenetic sources. Full article

The ecological transition is leading industry towards the use of materials of natural origin, which are often proposed for food contact materials as a sustainable solution to reduce plastic use. They are perceived as safe by consumers; however, a strict control on potential contaminants able to migrate to food and beverages is necessary to assess safety. Thus, the development of analytical methods for the detection and the identification of potentially occurring harmful substances is strongly encouraged, and the combination of different techniques can be a solution to obtain complementary information. In this work, GC-MS, HPLC-MS, ATR-IR and ESEM have been exploited with the aim of monitoring both volatile and non-volatile compounds, and to control surface composition and morphology. Extraction with solvent and migration experiments with simulants were performed on 11 commercial samples, including plates, caps, and wooden coffee stirrers. Global and specific migration studies were carried out, and possible differences before and after use were explored. Analysis after solvent extraction confirmed the presence of additives, and of Non-Intentionally-Added Substances (NIAS) that were also found in migration studies. Data on morphological characterisation were useful to control the item composition, and to check the stability of the materials after repeated use. Full article

Background/Objectives: Essential oils (EOs) have been exploited by humans for centuries, but many sources remain poorly investigated, mainly due to the low yields associated with conventional extraction. Recently, new techniques have been developed, like solvent-free microwave extraction (SFME), able to enhance efficiency and sustainability. The use of Papaver rhoeas L. in traditional medicine has led researchers to investigate non-volatile fractions, but there are little data available on EOs. Methods: In the present work, we prepared EOs from the petals and leaves of P. rhoeas by SFME. GC/MS analysis of EOs revealed the presence of 106 compounds belonging to 13 different classes. Isomers of the different alkenes were identified thanks to an alkylthiolation reaction. Results: The results highlighted a predominance of saturated and unsaturated hydrocarbons, alcohols, and esters that might suggest a specific relationship with pollinators. Each population has been compared using PCA, heatmap, and barplot tools, highlighting differences in terms of composition by both comparing leaves and flowers and hill and lowland samples. Furthermore, cantharidin, a metabolite usually produced by insects, was detected in the flowers, possible present for attractiveness purposes. Conclusions: These results could contribute to ensuring a better understanding of the pollination process and of the biological activities of EOs from P. rhoeas. Full article

Spilanthol is a major N-alkylamide constituent of Acmella oleracea (L.) R.K. Jansen with diverse pharmacological properties. We recently showed the applicability of NADES (natural deep eutectic solvents) for the green extraction of spilanthol. However, the purification of targets from NADES poses a challenging step due to their non-volatility. A simple green method to retrieve spilanthol with minimal instrumental effort was devised, fractioning NADES (choline chloride/methylurea, choline chloride/1,2-propanediol, choline chloride/citric acid) and dry ethanolic extracts by SPE on C18 material, eluting merely with ethanolic solutions. The relative distribution of spilanthol and organic adulteration in SPE fractions were detected by HPLC-DAD, followed by scale-up, quantification and purity determination in an NMR-based approach. Isocratic elution with 52% ethanol (v/v) proved suitable in all experiments. The three purest 10 mL fractions combined yielded 12.21 mg spilanthol at 71.65% purity from NADES extract ChCl/P (choline chloride/1,2-propanediol, molar ratio 1:2, +20% m/m water). Ethanolic extract samples showed purities ranging from 77.27 to 80.27% in combined raw fractions. For all samples, purity increased by removing non-soluble substances from organic solutions. Pooled NADES extract fractions showed 89.71% in final samples, ethanolic extracts 87.25 to 91.93%. The highest purities of individual fractions per extract were 89.23 to 94.15%. This cheap and simple purification process is promising to acquire spilanthol for research purposes or as a sample preparation step before HPLC on a semi-preparative to preparative scale, as the substance is highly priced and scarcely available on the market. Organic solvents can be reused, and preliminary scale-up possibilities are shown. Full article

In this study, fully aromatic polyether sulfones were developed, bearing blue, yellow, and orange–red π-conjugated semiconducting units. Carbazole-, anthracene-, and benzothiadiazole-based fluorophores are copolymerized with a diphenylsulfone moiety. A diphenylpyridine comonomer was additionally utilized, acting as both a solubilizing unit and a weak blue fluorescent group. Using this rationale, fluorescent polyarylethers with high molecular weights, up to 70 kDa, were developed, showing film formation ability and high thermal stability, while preserving excellent solubility in common organic, nonvolatile, and nonchlorinated solvents. Fine-tuning of the emission color was achieved through subtle changes of the comonomers’ type and ratio. Single-chromophore-bearing copolymers emitted in the blue or the yellow region of the visible spectrum, while the dual-chromophore-bearing terpolymers emitted throughout the visible spectrum, resulting in white light emission. Solutions of 20 wt% in polar aprotic solvents at ambient conditions allowed the deposition of fluorescent copolyethers and printing from non-chlorinated solvents. All polyethers were evaluated for their structural and optoelectronic properties, and selected copolymers were successfully used in the emitting layer (EML) of organic light-emitting diode (OLED) devices, using either rigid or flexible substrates. Remarkable color stability was displayed in all cases for up to 15 V of bias voltage. The Commission Internationale de L’Eclairage (CIE) of the fabricated devices is located in the blue (0.16, 0.16), yellow (0.44, 0.50), or white region of the visible spectrum (0.33, 0.38) with minimal changes according to the ratio of the comonomers. The versatile methodology toward semiconducting polyethersulfones for polymer light-emitting diodes (PLEDs) developed herein led to the scaled-up production of luminescent polymers of up to 25 g of high-molecular-weight single batches, demonstrating the effectiveness of this approach as a straightforward tool to facilitate the synthesis of flexible and printable EMLs for large-area PLED coverage. Full article

Pterocaulon polystachyum is a species of pharmacological interest for providing volatile and non-volatile extracts with antifungal and amebicidal properties. The biological activities of non-volatile extracts may be related to the presence of coumarins, a promising group of secondary metabolites. In the present study, leaves and inflorescences previously used for the extraction of essential oils instead of being disposed of were subjected to extraction with supercritical CO₂ after pretreatment with microwaves. An experimental design was followed to seek the best extraction condition with the objective function being the maximum total extract. Pressure and temperature were statistically significant factors, and the optimal extraction condition was 240 bar, 60 °C, and pretreatment at 30 °C. The applied mathematical models showed good adherence to the experimental data. The extracts obtained by supercritical CO₂ were analyzed and the presence of coumarins was confirmed. The extract investigated for cytotoxicity against bladder tumor cells (T24) exhibited significant reduction in cell viability at concentrations between 6 and 12 μg/mL. The introduction of green technology, supercritical extraction, in the exploration of P. polystachyum as a source of coumarins represents a paradigm shift with regard to previous studies carried out with this species, which used organic solvents. Furthermore, the concept of circular bioeconomy was applied, i.e., the raw material used was the residue of a steam-distillation process. Therefore, the approach used here is in line with the sustainable exploitation of native plants to obtain extracts rich in coumarins with cytotoxic potential against cancer cells. Full article

Electrospun/sprayed fiber films and nanoparticles were broadly studied as encapsulation techniques for bioactive compounds. Nevertheless, many of them involved using non-volatile toxic solvents or non-biodegradable polymers that were not suitable for oral consumption, thus rather limiting their application. In this research, a novel electrospun lipid–polymer composite (ELPC) was fabricated with whole generally recognized as safe (GRAS) materials including gelatin, medium chain triglyceride (MCT) and lecithin. A water-insoluble bioactive compound, tetrahydrocurcumin (TC), was encapsulated in the ELPC to enhance its delivery. Confocal laser scanning microscopy (CLSM) was utilized to examine the morphology of this ELPC and found that it was in a status between electrospun fibers and electrosprayed particles. It was able to form self-assembled emulsions (droplets visualized by CLSM) to deliver active compounds. In addition, this gelatin-based ELPC self-assembled emulsion was able to form a special emulsion gel. CLSM observation of this gel displayed that the lipophilic contents of the ELPC were encapsulated within the cluster of the hydrophilic gelatin gel network. The FTIR spectrum of the TC-loaded ELPC did not show the fingerprint pattern of crystalline TC, while it displayed the aliphatic hydrocarbon stretches from MCT and lecithin. The dissolution experiment demonstrated a relatively linear release profile of TC from the ELPC. The lipid digestion assay displayed a rapid digestion of triglycerides in the first 3–6 min, with a high extent of lipolysis. A Caco-2 intestinal monolayer transport study was performed. The ELPC delivered more TC in the upward direction than downwards. MTT study results did not report cytotoxicity for both pure TC and the ELPC-encapsulated TC under 15 μg/mL. Caco-2 cellular uptake was visualized by CLSM and semi-quantified to estimate the accumulation rate of TC in the cells over time. Full article

Currently, fennel bulb is becoming a highly demanded and consumed vegetable due to its licorice flavor and health benefits. Although the chemical composition of fennel essential oil has been extensively studied, the nonvolatile bioactive compounds of fennel bulbs have drawn less attention. Here, the phenolic profile and the antioxidant activity in terms of DPPH radical scavenging activity, reducing power, chelating ability of ferrous ions, and inhibition of lipid peroxidation were analyzed using four different fennel hybrid genotypes and three different extraction solvents (methanol, aqueous-methanol, and hot water). Antioxidant activity results revealed significant variation amongst fennel varieties (>3-fold difference for DPPH and reducing power and >2.7-fold for the inhibition of lipid peroxidation), with methanolic extracts exhibiting the highest antioxidant activity. Total phenol content peaked in the aqueous-methanol extracts, exhibiting a 2-fold difference across fennel genotypes. HPLC–PDA/MS analyses identified high levels of caffeic acid derivatives in hot water extracts, particularly in the commercial genotype. The therapeutic benefits associated with these compounds make it reasonable to use detailed phytochemical screening in fennel breeding programs to obtain varieties with new functionalities and thus higher added value. Full article

Zanthoxylum oleoresin, a concentrated extract derived from Zanthoxylum bungeanum, is rich in non-volatile, intensely flavorful substances and amide compounds, such as hydroxy-α-sanshool, hydroxy-β-sanshool, and hydroxy-ε-sanshool. The production process of Zanthoxylum oleoresin remains unstandardized, and there is still a lack of research on the precise classification and quantification of its key chemical constituents, as well as the stability of these compounds when produced using different extraction methods. This study utilized preparative liquid chromatography to extract and purify amide compounds from Zanthoxylum oleoresin, successfully isolating three sanshools: hydroxy-α-sanshool, hydroxy-β-sanshool, and hydroxy-ε-sanshool. The stability of three these sanshools under UVB irradiation in different solvents was explored in UVB-simulated sunlight conditions to investigate the degradation or transformation mechanism of Zanthoxylum alkylamides under UVB irradiation. The findings indicate a rapid decrease in the hydroxy-α-sanshool content under UVB ultraviolet light, aligning with the second-order kinetics. This study revealed alterations in the contents of hydroxy-α-sanshool, hydroxy-β-sanshool, and hydroxy-ε-sanshool and the formation of a new compound following exposure to UVB light. This new compound, along with the three sanshools, possesses a uniform m/z 264 and shares similar chemical structures. Further analysis also uncovered that these compounds are capable of undergoing isomerization reactions under UVB irradiation. This demonstrates that UVB irradiation of certain intensities can modify the concentrations and chemical structures of these Zanthoxylum alkylamides. These insights offer crucial guidance for future studies on the processing and preservation of Zanthoxylum alkylamides and their derivatives. Full article

Nanofibrous membranes have gained interest for their small pore size, light weight, and excellent filtration. When produced from high-performance polymers, nanofibrous membranes also benefit from excellent mechanical properties, thermal resistance, and chemical resistance. Electrospinning is a common method of producing high-performance nanofibres. However, there are still major challenges with the dissolution and electrospinning of these polymers, as well as in the performance of the resulting nanofibres, which is often less than what would be expected from a conventional high-performance fibre. This review assesses the state of progress in the electrospinning of five high-performance fibres: meta-aramid (m-aramid), para-aramid (p-aramid), polyamide-imide (PAI), polybenzoxazole (PBO), and polybenzimidazole (PBI). Polymers that can be readily dissolved in organic solvents, such as m-aramid, PAI, and PBI, have been more widely researched for electrospinning compared to those that can only be spun from precursors or dissolved in non-volatile solvents. Major focuses within the literature include optimizing the electrospinning process and improving the mechanical performance of the nanofibres. This review demonstrates a clear need for more standardized characterization methods and consideration for the longevity of the nanofibrous membranes. Future research should also focus on scale-up methods of electrospinning so that the benefits of nanofibres made from high-performance polymers can be leveraged by the industry. Full article

Analytical methods based on the mass balance approach were developed for the purity evaluation of tetracycline hydrochloride, a representative salt compound used in pure veterinary drug analysis. The purity assignment method was used to quantify individual classes of impurities via independent analytical techniques. The mass fraction of the free base or salt form contained in a high-purity organic compound with a hydrochloride salt can be determined. The chloride content by ion chromatography-conductivity detector (IC-CD) and general classes of impurities, including structurally related impurities by liquid chromatography–ultraviolet (LC-UV) detector, water by Karl Fischer (KF) coulometric titration, residual solvents by headspace sampler gas chromatography/mass spectrometry (HS-GC/MS), and non-volatiles by thermogravimetric analyzer (TGA), were considered to calculate the purity of the mass fraction. The chloride content of the salt compound can be considered the main impurity in the mass fraction of the free base in the salt compound. A purity assay using quantitative nuclear magnetic resonance (q-NMR) as a direct determination method was performed to confirm the results of the mass balance method. The assigned purities of the tetracycline free form and its salt form in mass fraction were (898.80 ± 1.60) mg/g and (972.65 ± 1.58) mg/g, respectively, which are traceable to the international system of units (SI). Thus, the procedure for evaluating the purity of the free base and salt forms in the salt compound is newly demonstrated in this study. Full article