A new carvotacetone sphaeranthone A and four known compounds 3-angeloyloxy-5-[2″,3″-epoxy-2″-methylbutanoyloxy]-7-hydroxycarvotacetone (2), 3-angeloyloxy-5-[3″-chloro-2″-hydroxy-2″-methylbutanoyloxy]-7-hydroxycarvotacetone (3), chrysosplenol D (4), and 3-O-methylquercetin (5) were isolated from leaves of Sphaeranthus africanus growing in Vietnam. Their chemical structures were elucidated by extensive 1D and 2D NMR analysis and high-resolution mass spectroscopy as well as comparisons in literature. Compounds 1-3 were evaluated for the alpha-glucosidase inhibition. They showed moderate activity with IC50 values of 103 ± 1.7, 146.8 ± 2.5, 49 ± 0.8 µg/mL, respectively.
Poly(beta-amino ester) (P beta AE)-based polymers hold promise for bacterial gene transfer due to their ability to form stable complexes with genetic material and facilitate efficient delivery into bacterial cells. These polymers are easily modified to improve uptake and protect DNA or RNA from degradation, providing a safer, more controlled alternative to traditional methods like chemical transformation or electroporation. In this study, we evaluated the gene transformation efficiency of cationic P beta AE polymer, which was synthesized through an aza-Michael addition reaction between piperazine and poly(ethylene glycol) diacrylate. Competent cells from E. coli strain DH5 alpha were prepared with the optimized method using Ca2+ and Mg2+ ions. Different concentrations of the polymer were mixed with pRSET-EmGFP before transforming into competent cells through the heat shock method. Transformed cells were checked on medium containing ampicillin, and by using colony PCR, transformation efficiency was calculated. Based on our findings, we observed a successful transformation of the EmGFP gene in case of having the polymer. Furthermore, the P beta AE at high concentrations (20-100 ng mu L-1) increased transformation efficiency more than twice as compared to the case of no polymer added. In conclusion, P beta AE can effectively increase transformation efficiency.
Hydrogels are notable for their outstanding absorbent qualities, satisfactory compatibility with biological systems, ability to degrade, and inherent safety, all of which contribute to their high demand in the field of biomedicine. This study focuses on the fabrication of hydrogels using environmentally friendly cellulosic material. Cellulose hydrogel beads were prepared by physical cross-linking in a NaOH/urea medium. Furthermore, nano polydopamine was integrated into the hydrogel matrix as functional polymers and α-mangostin was employed as an active pharmaceutical ingredient. The physicochemical properties were comprehensively analyzed using Fourier-transform infrared spectrometer, 13C cross-polarization/magic angle spinning nuclear magnetic resonance, thermogravimetric analysis, and scanning electron microscope. The drug delivery properties, including water content, swelling ratio, and drug release profiles, were evaluated. In vitro cytotoxicity against MC3T3-E1 cells was assessed using sulforhodamine B staining. All test hydrogels exhibited inhibitory activity against the growth of MC3T3-E1 cells. These results indicated the potential use of these hydrogels as a drug delivery carrier for α-mangostin in the treatment of ankylosing spondylitis.
Ciprofloxacin imprinted polymers have garnered significant attention due to the high demand for application in the monitoring of antibiotics. This study focuses on the synthesis and selective adsorption properties of ciprofloxacin imprinted polymers. The polymers were synthesized via precipitation polymerization technique. Optimal condition was achieved using acetonitrile:water (8:2, v/v) and a molar ratio of ciprofloxacin:acid methacrylic:ethylene glycol dimethacrylate of 1:6:30. Physicochemical characterization utilizing FT-IR, TGA-DSC, SEM, and N2 adsorption isotherm confirmed the desired properties of the polymer. Adsorption properties (kinetic, pH, and isotherm) indicated selective adsorption of ciprofloxacin onto the imprinted polymer with an imprinting factor of 1.34 and adsorption capacity up to 11.6 mg g-1. These findings underscore the potential of the ciprofloxacin imprinted polymer as a stationary phase for solid-phase extraction columns.
In the present study, a self-designed colorimetric box equipped with a smartphone as an emerging analytical approach was designed to determine the total phenolic contents (TPCs) in coffee. The formed blue complex between the phenolic compounds and Folin-Ciocalteu reagent was measured its color intensities using RGB (red, green, blue) color system. Different parameters related to the photo capturing were investigated, i.e., the distance between the smartphone and sample holder, constant illumination inside the box, and the reaction time. The method performance based on three color channels (R, G, and B) was evaluated and agreed with Appendix F of AOAC (2016). Different sensitivities among three color channels were achieved, and the linear ranges were wide, from 10.0 mg GAE L -1 up to 120.0 mg GAE L -1 for the B channel, which was compatible with various coffee types (GAE: gallic acid equivalent). No statistical difference between the smartphone-based methods and standard Ultraviolet-visible (UV-Vis) was observed by t-test ( P = 95%). Various advantages were obtained, e.g., simplicity, portability, low-cost operation, and easy accessibility for producers and consumers to test for the raw materials, intermediate and final products. The proposed method was applied to several specific roasted ground coffee products from Lam Dong Province (Vietnam) in the context of the limited scientific data on the internal composition of Vietnamese coffee. The results demonstrate that the TPCs depend on coffee varieties, i.e., Robusta exhibits higher TPCs than Arabica, and roasting levels during the processing, i.e., dark mode generally performs the lowest TPCs, due to the thermal decomposition and formation of different phenolic compounds by Millard reactions.
The objective of this study was to evaluate the antioxidant, anti-skin-aging, anti-inflammatory, and anti-acetylcholinesterase activities of the hexane (n-hex), AcOEt, BuOH, MeOH, and aqueous extracts from R. oligophlebia roots. The total phenolic and flavonoid contents (TPC and TFC) were determined using Folin-Ciocalteu and AlCl3 colorimetric assays. The antioxidant capacity was examined by reducing power (RP), ferric reducing antioxidant power (FRAP), ABTS⋅+ , and DPPH⋅+ radical cation assays. All extracts potentially exhibited antioxidant activity with IC50 values ranging from 2.93 to 5.73 μg/mL for ABTS⋅+ and from 5.69 to 7.65 μg/mL for DPPH⋅+ except the n-hex extract. The BuOH, MeOH, and aqueous extract possess promising anti-skin-aging activities, as observed by an attenuation of UV-A toxicity on human keratinocytes. We proposed that these anti-skin-aging properties are possibly due to direct scavenging activity against reactive oxygen species and upregulate cellular antioxidant machinery. Moreover, we found that the antioxidant capacity was well correlated with anti-inflammatory capacity against nitric oxide (NO) production in terms of the n-hex, AcOEt, and BuOH extracts with IC50 values from 23.21 to 47.1 μg/mL. In contrast, these activities were found to be poorly correlated with AchE activity. To the best of our knowledge, this is the first report of the antioxidant, anti-skin-aging, anti-inflammatory, and anti-acetylcholinesterase activities of the extracts of R. oligophlebia roots. These findings indicated that this species could be a potential source of natural antioxidant, anti-aging, and anti-inflammatory agents. Consequently, it may be suggested as a medicinal plant that prevents diseases related to oxidative stress and inflammatory responses.
Increasing electronic waste (e-waste) generation is cause for great concern in the environment, for which our current society has developed various management policies, although it brings many economic opportunities through recycling and resource recovery activities. The recovery of gold from e-waste is of great importance for economic value and sustainability, as gold contained in e-waste can be manyfold that in primary gold deposits. Hydrometallurgy has succeeded in recovering gold from e-waste using different technical approaches owing to its mild operation, affordability, and low gas emission. However, it is still challenging to develop a complete technology for widespread application due to the complexity of e-waste and very low content of gold. Conventional leaching of gold may not satisfy environmental regulations, while alternative methods still require much effort to scale up their applications. Gold separation has attracted interest in the development of biomaterials for the effective, economical, and environmentally safe adsorption of gold. The phytochemical adsorption of gold has efficiently reduced gold ions to metallic gold, whereas gold-imprinted adsorbents have shown high selectivity toward gold species. The use of low-cost bio-adsorbents derived from agricultural by-products has been shown as a simple recovery option for gold by calcination. This review provides direction for future research toward selecting sustainable and efficient hydrometallurgical approaches for the recovery of gold from e-waste.
This study aims to develop a green and efficient method for synthesizing antimicrobial amino-functionalized microcrystalline celluloses from cotton fibers. Microcrystalline cellulose was prepared by acid hydrolyzing of cellulose. Tosyl cellulose was synthesized by tosylation of cellulose in an eco-friendly medium using NaOH/urea and decyl glucoside surfactant with DSTs of 0.51. Three amino-functionalized cellulose derivatives were synthesized by nucleophilic substitution reaction of tosyl cellulose with 3-aminopropyltrimethoylsilane, ethylenediamine, and triethylenetetramine. The physicochemical properties of investigated celluloses were characterized by Fourier transform infrared spectroscopy, X-ray diffraction analysis, scanning electron microscopy, and thermogravimetric analysis-differential scanning calorimetry. Microcrystalline cellulose with high crystallinity index (81.90
Novel ciprofloxacin composite imprinted materials are synthesized by using co-precipitation polymerization of dual functional monomers (methacrylic acid and 2-vinylpyridine) and polystyrene-co-divinylbenzene. The intermolecular interactions between monomers and template are evaluated by molecular modeling analysis. The physicochemical properties of the obtained polymers are characterized using FT-IR, TGA, and SEM. Batch adsorption experiments are used to investigate adsorption properties (kinetic, pH, and isotherm). These polymers are employed to prepare the solid phase extraction cartridges, and their extraction performances are analyzed by the HPLC-UV method. DFT calculations indicate that hydrogen bonding and π-π stacking are the driving forces for the formation of selective rebinding sites. The obtained polymers exhibit excellent adsorption properties, including fast kinetics and high adsorption capacity (up to 10.28 mg g-1) with an imprinted factor of 2.55. The Scatchard analysis indicates the presence of specific high-affinity adsorption sites on the imprinted polymer. These absorbents are employed to extract CIP in river water with recoveries in the range of 65.97-119.26% and the relative standard deviation of 3.59-14.01%. Furthermore, the used cartridges could be reused at least eight times without decreasing their initial adsorption capacity.
Background . Garcinia is a large genus which has promising bioactivities. However, the properties of many Garcinia species have not been investigated thoroughly. Aim . To determine the antioxidant and antimicrobial capabilities of the extracts from different Garcinia species. Methodology . Six Garcinia species, including Garcinia fusca , Garcinia hopii , Garcinia planchonii , Garcinia nigrolineata , Garcinia gaudichaudii , and Garcinia tinctoria were extracted using n -hexane, ethyl acetate, and methanol, producing n -hexane extract (HE), ethyl acetate extract (EAE), and methanol extract (ME). After that, the total polyphenol content was evaluated using Folin–Ciocalteu assay. DPPH, hydroxyl radical scavenging, and total antioxidant capacity assays were performed to test the antioxidant activity. Subsequently, the antimicrobial activities against Gram-positive ( Staphylococcus aureus , Bacillus subtilis ) and Gram-negative ( Escherichia coli , Pseudomonas aeruginosa ) bacterial strains were assessed using Kirby Bauer and the broth microdilution methods. Results . Many Garcinia extracts contained high total polyphenol content consisting of ME of G. hopii ad G. tinctoria , and EAE of G. planchonii and G. tinctoria . The EAE of G. tinctoria showed effective antioxidant capacity (IC 50 = 1.5 µ g/mL). Additionally, the EAE of G. gaudichaudii was effective against Gram-positive bacteria with minimal inhibition concentration (MIC) of 15.625–25 µ g/mL whereas ME of G. planchonii was effective against both Gram-positive bacteria (MIC = 160 µ g/mL) and Gram-negative bacteria (MIC = 75 µ g/mL). Conclusion . Several extracts of Garcinia species demonstrated valuable antioxidant and antimicrobial properties.
Background: Ciprofloxacin (CIP), an important broad-spectrum fluoroquinolone antibiotic, was often used as a template molecule for the preparation of imprinted materials. In this study, methacrylic acid and 2-vinylpyridine were employed for the first time as dual functional monomers for synthesizing ciprofloxacin imprinted polymers. Methods: The chemical and physicochemical properties of synthesized polymers were characterized using Fourier transform-infrared spectroscopy, thermogravimetric analysis-differential scanning calorimetry, scanning electron microscopy, and nitrogen adsorption-desorption isotherm. The adsorption properties of ciprofloxacin onto synthesized polymers were determined by batch experiments. The extraction performances were studied using the solid phase extraction and HPLC-UV method. Results: The molecularly imprinted polymer synthesized with dual functional monomers showed a higher adsorption capacity and selectivity toward the template molecule. The adsorbed amounts of ciprofloxacin onto the imprinted and non-imprinted polymer were 2.40 and 1.45 mg g−1, respectively. Furthermore, the imprinted polymers were employed as a selective adsorbent for the solid phase extraction of ciprofloxacin in aqueous solutions with the recovery of 105% and relative standard deviation of 7.9%. This work provides an alternative approach for designing a new adsorbent with high adsorption capacity and good extraction performance for highly polar template molecules.
Introduction: Ionic liquids (ILs) have attached many attentions due to their interesting physicochemical properties. However, ionic liquids have several disadvantages including high viscosity, difficult to purify, separate and recycle, and expensive. Therefore, supported ionic liquids (SIL) have been developed to overcome these problems. SIL based on cellulose material was conventionally synthesized by silanization reaction between ionic liquid trialkoxyl silane and hydroxyl groups on the surface of cellulose. However, low reactivity of cellulose hydroxyl groups causes the low efficiency of silanization reaction. With the aim to resolve these problems and improve the reactivity of cellulose silanization reaction, cellulose graft ionic liquid was synthesized and characterized. Methods: Cellulose graft ionic liquid (CL-IL) material was synthesized by silanization reaction. The influence of reaction condition such as IL/CL (w/w) ratio, base catalyst (NH3) and agent coupling tetraethyl orthosilicate (TEOS) on silanization reaction was investigated. The modified CL-IL materials were characterized using FT-IR, TGA, SEM. The ion exchange properties were evaluated via batch adsorption studies to evidence the efficiency of silanization reaction of cellulose. Results: The study indicated that adding TEOS with NH3 catalyst could significantly increase the number of imidazolium groups grafted on cellulose about 75% compared to the conventional approach. CL-IL material is an efficient anion exchange materials displaying fast kinetic adsorption and high capacity adsorption of MO up to 1.4 mmol g-1. Conclusion: High-efficiency of cellulose silanization was obtained by using coupling agent TEOS and base catalyst. Therefore, the silanization reaction can be used for synthesis divers of functional cellulose materials. This approach can be aimed for the design of cheaper and high-performance materials for catalysis, polymer composite and adsorption in water treatment and depollution of industrial wastewater.
Ionosilicas are defined as silica based materials containing covalently tethered ionic groups. These materials, situated at the interface of silica hybrid materials and ionic liquids, have large potential in catalysis, molecular recognition and separation. This paper focuses on applications of ionosilicas as efficient adsorbents of para-aminosalicylate (PAS). Various ionosilica materials containing ammonium groups were synthesized by template directed hydrolysis-polycondensation reactions starting from silylated precursors, among them one particular material bearing an aromatic benzyl group. The different materials were used for the extraction of PAS from aqueous solution, Specifically, we investigated the sorption process of PAS as a function of the porosity of the material, its chemical constitution, and the pH of the suspension. We further investigated the kinetics and enthalpic displacement effects, based on Isotherm Titration Calorimetry (ITC) measurements. We show that for an identical number of ion exchange sites, PAS is more efficiently adsorbed using an ionosilica bearing aromatic groups. We attribute this result to a pi-pi-stacking contribution involving the phenyl groups of the material, which increases the affinity of PAS towards this particular ionosilica material. In general, our study highlights the high potential of ionosilicas in adsorption processes. Here, ionosilicas with tailored properties can be designed for the separation of specific target compounds. This versatility of these adsorbents will be of interest in advanced separation processes for sustainable development applications.
We report ionosilicas with different chemistries, textures, and morphologies and their use as adsorbents for chromium(VI). All studied materials are highly efficient anion exchange materials with adsorption capacities between 1.6 and 2.6 mmol/g. The ion exchange capacity of the materials reaches up to 91% of the theoretical value, that is, the molar amount of ionic groups immobilized within the material, indicating a very high accessibility of the organo-ionic groups. Noticeable differences were found regarding the ion exchange properties in terms of capacity and kinetics according to the used material, in particular, its porosity. High specific surface areas favor the adsorption process and result in high adsorption capacity. However, even a nonporous material displays high adsorption capacity of 1.7 mmol/g. This result can be attributed to the high hydrophilicity of ionosilicas that favors diffusion and mass transfer throughout the material. The adsorption kinetics are fast, as 80-90% of the adsorption capacity is reached after similar to 10 min. Finally, isotherm titration calorimetry evidences the influence of the constitution of the cationic group the displacement enthalpy, in relationship with the steric hindrance of the alkyl groups that surround the cationic center.
BACKGROUND: The effective exploitation of biomass for the preparation of fuels and platform chemicals requires the development of novel catalysts and catalyticmethods. In this regard, ionosilicas appear as promising candidates due to their properties and tunability.RESULTS: A novel Pd@ionosilica is prepared by a straightforward ion exchange method based on amorphous ionosilica and sodium tetrachloropalladate. The resulting hybrid material is evaluated as catalyst for the continuous flow reduction of cinnamaldehyde as an exemplary biorefinery case study.CONCLUSION: This work reports the application of metal@ionosilica hybrid materials as catalysts for the continuous flow upgrade of bio-sourced molecules, showing promising results in the case of cinnamaldehyde, here used as exemplary compound. The findings disclosed in this paper provide interesting insights for the development of second generation metal@ionosilica composites for catalytic applications within biorefinery. (C) 2017 Society of Chemical Industry
Ionosilica are mesoporous silica-based hybrid materials containing covalently bound ionic groups. The mixed ionic mineral nature confers particular properties to these materials. Here, we focus on the tailoring of the interfacial properties of ionosilicas. Three materials were synthesized from three different oligosilylated ammonium precursors. Furthermore, anion exchange allowed replacing the halide in the parent ionosilicas by more hydrophobic anions, e.g., thiocyanate (SCN-) and bis(trifluoromethane)sulfonimide (NTf2-). Both the constitution of the ammonium substructure of the precursor and the nature of the counteranion allow controlling the interfacial properties in terms of hydrophilicity and affinity toward different types of solvents. Although all studied ionosilica are highly hydrophilic mesoporous materials, significant differences and clear trends could be observed. As shown via competitive 1-butanol adsorption measurements in the liquid phase and solvent vapor adsorption from the gas phase, the interfacial properties of ionosilicas can be fine-tuned either by the use of more hydrophobic ammonium precursors or the incorporation of hydrophobic anions. We therefore show that ionosilicas combine high porosity, regular architecture on the mesoscopic level with an unmatched chemical versatility, induced by the high variability and the high number of homogeneously distributed ionic species. Ionosilicas appear as highly adaptable materials and can be considered as "designer materials", which are interesting for applications in catalysis, sorption, and separation.
Six 5-arylidene-3-methylrhodanine derivatives were synthesized by the crossed aldolization of aromatic aldehydes with 3- methylrhodanine using 1-butyl-3- methylimidazolium chloride ([BMI]Cl) as phase transfer catalyst in water. The reactions, under microwave irradiation (160 watts) during 10 minutes, afforded the yield of 59–83 %. This is the first time [BMI]Cl was used as phase transfer catalyst in the aldol condensation.
Ammonium based hybrid ionosilicas were prepared from tetrasilylated ammonium precursors. The formed material exhibited high specific surface area together with mesoporosity. Our results indicate that ionosilicas display high exchange capacity for iodide. They were submitted to 10MeV electron irradiation at a total dose of 1.7MGy. Irradiation was shown not to alter the properties of ionosilica: the morphological, textural and surface properties of the material are hardly modified. The sorption properties (sorption capacity and cumulative displacement enthalpy) are similar before and after electron irradiation. This high radiolytical stability confirms that these innovative materials have therefore high potential as anion traps for future applications in decontamination processes or long term storage of radioactive waste.
Ionosilicas, defined as silica based materials containing covalently anchored ionic groups [1], recently emerged as a new family of functional materials. Ionosilicas combine high porosity, regular architecture on the mesoscopic level with an unmatched chemical versatility, induced by the high variability and the high number of incorporated ionic species. Due to their mixed ionic-mineral nature, ionosilicas are situated at the interface of ionic liquids and silica hybrid materials. The first part of this talk will focus on the synthesis of structured ionosilica mesophases. Ionosilicas are obtained under very mild reaction conditions via template directed hydrolysis-polycondensation reactions starting from trialkoxysilylated ionic precursors [2,3]. The formation of structured ionosilica mesophases can only be achieved from suitable surfactant-precursor ion pairs. This approach is particularly appealing as both precursor and surfactant can be modulated, thus allowing a control over chemical constitution and architecture of the formed materials. Ionosilicas can be considered as heterogenized and porous ionic liquid phases. They exhibit tunable interfacial properties in terms of hydrophilicity and water affinity [4]. Ionosilicas represent a real alternative for applications in catalysis and separation. This feature will be illustrated by the unique properties in ion exchange. Ionosilicas efficiently trap anionic metal complexes [5], halides [6] and drugs [7] and therefore have great potential for applications in fields as different as medicine, water treatment or the nuclear fuel management. In summary, ionosilicas represent a very particular class of functional silica based materials displaying unique chemical and physico-chemical properties, together with remarkable surface properties. For this reason, ionosilicas have an outstanding position in the area of silica based materials and are more than simple silica supported ionic liquids.
Mesoporous and nanostructured ionosilica material containing ammonium groups was successfully applied for diclofenac and sulindac adsorption via ion exchange.