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This study aimed to enhance the ultrasonic-assisted extraction (UAE) yield of seawater Arthrospira platensis polysaccharides (APPs) and investigate its structural characteristics and bioactivities. The optimization of UAE achieved a maximum crude polysaccharides yield of 14.78%. The optimal extraction conditions were a liquid–solid ratio of 30.00 mL/g, extraction temperature of 81 °C, ultrasonic power at 92 W and extraction time at 30 min. After purification through cellulose DEAE-52 and Sephadex G-100 columns, two polysaccharide elutions (APP-1 and APP-2) were obtained. APP-2 had stronger antioxidant and immunoregulatory activities than APP-1, thus the characterization of APP-2 was conducted. APP-2 was an acidic polysaccharide consisting of rhamnose, glucose, mannose and glucuronic acid at a ratio of 1.00:24.21:7.63:1.53. It possessed a molecular weight of 72.48 kDa. Additionally, APP-2 had linear and irregular spherical particles and amorphous structures, which contained pyranoid polysaccharides with alpha/beta glycosidic bonds. These findings offered the foundation for APP-2 as an antioxidant and immunomodulator applied in the food, pharmaceutical and cosmetic industries. [ABSTRACT FROM AUTHOR]

This overview provides insights into organic and metal–organic polymer (OMOP) catalysts aimed at processes carried out in the liquid phase. Various types of polymers are discussed, including vinyl (various functional poly(styrene-co-divinylbenzene) and perfluorinated functionalized hydrocarbons, e.g., Nafion), condensation (polyesters, -amides, -anilines, -imides), and additional (polyurethanes, and polyureas, polybenzimidazoles, polyporphyrins), prepared from organometal monomers. Covalent organic frameworks (COFs), metal–organic frameworks (MOFs), and their composites represent a significant class of OMOP catalysts. Following this, the preparation, characterization, and application of dispersed metal catalysts are discussed. Key catalytic processes such as alkylation—used in large-scale applications like the production of alkyl-tert-butyl ether and bisphenol A—as well as reduction, oxidation, and other reactions, are highlighted. The versatile properties of COFs and MOFs, including well-defined nanometer-scale pores, large surface areas, and excellent chemisorption capabilities, make them highly promising for chemical, electrochemical, and photocatalytic applications. Particular emphasis is placed on their potential for CO2 treatment. However, a notable drawback of COF- and MOF-based catalysts is their relatively low stability in both alkaline and acidic environments, as well as their high cost. A special part is devoted to deactivation and the disposal of the used/deactivated catalysts, emphasizing the importance of separating heavy metals from catalysts. The conclusion provides guidance on selecting and developing OMOP-based catalysts. [ABSTRACT FROM AUTHOR]

Polysaccharides from cyanobacteria are extensively reported for their complex structures, good biocompatibility, and diverse bioactivities, but only a few cyanobacterial species have been exploited for the biotechnological production of polysaccharides. According to our previous study, the newly isolated marine cyanobacterium Cyanobacterium aponinum SCSIO-45682 was a good candidate for polysaccharide production. This work provided a systematic study of the extraction optimization, isolation, structural characterization, and bioactivity evaluation of polysaccharides from C. aponinum SCSIO-45682. Results showed that the crude polysaccharide yield of C. aponinum reached 17.02% by hot water extraction. The crude polysaccharides showed a porous and fibrous structure, as well as good moisture absorption and retention capacities comparable to that of sodium alginate. A homogeneous polysaccharide (Cyanobacterium aponinum polysaccharide, CAP) was obtained after cellulose DEAE-52 column and Sephadex G-100 column purification. CAP possessed a high molecular weight of 4596.64 kDa. It was mainly composed of fucose, galactose, and galacturonic acid, with a molar ratio of 15.27:11.39:8.64. The uronic acid content and sulfate content of CAP was 12.96% and 18.06%, respectively. Furthermore, CAP showed an in vitro growth inhibition effect on human hepatocellular carcinoma (HepG2) cells. The above results indicated the potential of polysaccharides from the marine cyanobacterium C. aponinum SCSIO-45682 as a moisturizer and anticancer addictive applied in cosmetical and pharmaceutical industries. [ABSTRACT FROM AUTHOR]

Olive mill wastewater (OMW) poses a significant environmental challenge and health concern in olive-producing countries, including Jordan. Surfactant micelles are frequently employed as solubilizing agents to enhance the water solubility of chemical compounds. This study aims to leverage the sodium dodecyl sulfate (SDS) micelles in a multi-step process to detoxify OMW for agricultural and industrial uses and reduce its impact. The OMW was treated in multiple steps: screening, coagulation with different chemicals, and distillation with different surfactants. The treatment steps were monitored using LC–MS, GC–MS, ICP–MS, chemical oxygen demand contents, and total phenolic compounds. The detoxification of OMW was evaluated using standard germination assays, MTT assays using tissue culture, and toxicity assays using fluorescence bacteria. Following the treatment, the seed growth rate improved significantly from 0% to 100%. The GC–MS revealed a substantial decrease in pollutants. The concentration of polyphenols was reduced to 2.5%, while the COD level decreased to 35%. The toxicity in bacteria was significantly reduced in a time-dependent manner, and the toxicity in human cells decreased by 95%. Additionally, between 50% and 95% of metals in OMW were removed. The multi-step SDS-based approach successfully detoxified the OMW and enhanced water quality, which would pave the road for its direct application in industry and agriculture. [ABSTRACT FROM AUTHOR]

A condensation reaction of salicylic acid with formaldehyde in the presence of sulfuric acid led to the synthesization of the bis(2-hydroxy-3-carboxyphenyl)methane (BHCM) ligand, which was subsequently allowed to bind with nickel (II) ions. In light of the information obtained from the elemental analyses (C, H, and M), spectral (IR, MS, 1H-NMR, and UV–Vis) and thermal and magnetic measurements, the most likely structures of the ligand and complex have been identified. It has been suggested that the BHCM coordinates in a tetradentate manner with two Ni(II) ions to produce an octahedral binuclear complex. The SEM and TEM morphology of the compounds showed spherical shapes. An X-ray diffraction analysis indicated a considerable difference in the diffraction patterns between BHCM (crystalline) and Ni–BHCM (amorphous), and the Scherrer equation was used to calculate the crystallite size. Some optical characteristics were estimated from UV–Vis spectra. The ligand and its nickel(II) complex underlie the range of semiconductors. It was verified that for human lung (A-549) cancer, the BHCM compound displayed a significant barrier to the proliferation test in noncancerous cells (human lung fibroblasts, WI-38), which was also undertaken. To demonstrate the binding affinities of the chosen compounds (BHCM and Ni–BHCM) in the receptor protein's active site [PDB ID: 5CAO], a molecular docking (MD) study was carried out. [ABSTRACT FROM AUTHOR]

Heterostructures of visible light-absorbing semiconductors were prepared through the growth of ZnIn2S4 crystallites in the presence of CdS nanostructures. A variety of hybrid compositions was synthesized. Both reference samples and heterostructured materials were characterized in detail, regarding their morphology, crystalline character, chemical speciation, as well as vibrational properties. The abovementioned physicochemical characterization suggested the absence of doping phenomena, such as the integration of either zinc or indium ions into the CdS lattice. At specific compositions, the growth of the amorphous ZnIn2S4 component was observed through both XRD and Raman analysis. The development of heterojunctions was found to be composition-dependent, as indicated by the simultaneous recording of the Raman profiles of both semiconductors. The optical band gaps of the hybrids range at values between the corresponding band gaps of reference semiconductors. The photocatalytic activity was assessed in both organic dye degradation and hydrogen peroxide evolution. It was observed that the hybrids demonstrating efficient photocatalytic activity in dye degradation were rather poor photocatalysts for hydrogen peroxide evolution. Specifically, the hybrids enriched in the CdS component were shown to act efficiently for hydrogen peroxide evolution, whereas ZnIn2S4-enriched hybrids demonstrated high potential to photodegrade an azo-type organic dye. Furthermore, scavenging experiments suggested the involvement of singlet oxygen in the mechanistic path for dye degradation. [ABSTRACT FROM AUTHOR]

As a corrosion inhibitor for mild steel in a molar hydrochloric acid medium, we investigated the potential of Eucalyptus globulus essential oil (EuEO). Through electrochemical impedance spectroscopy (EIS), potentiodynamic polarization curves, and theoretical methods, including DFT/B3LYP 6-31G (d, p) and Monte Carlo simulations, the interactions between the EuEO components and the steel surface were analyzed. D-Allose, Betulinaldehyde, and Uvaol were identified as the major active compounds in the GC-MS analysis. The experimental results showed that EuEO reached an inhibitory efficiency as high as 97% at a 1 g/L concentration. The findings suggest that EuEO operates as a mixed-type inhibitor, reducing both cathodic and anodic reactions, as well as building up a protective coating on the steel surface. Simulations also confirmed that EuEO molecules function as electron donors and acceptors, enhancing corrosion resistance. [ABSTRACT FROM AUTHOR]

Polyamorphic transformations driven by high-energy mechanical ball milling (nanomilling) are recognized in a melt-quenched glassy alloy of tetra-arsenic triselenide (As4Se3). We employed XRPD analysis complemented by thermophysical heat-transfer and micro-Raman spectroscopy studies. A straightforward interpretation of the medium-range structural response to milling-driven reamorphization is developed within a modified microcrystalline model by treating diffuse peak-halos in the XRPD patterns of this alloy as a superposition of the Bragg-diffraction contribution from inter-planar correlations, which are supplemented by the Ehrenfest-diffraction contribution from inter-atomic and/or inter-molecular correlations related to derivatives of thioarsenide As4Sen molecules, mainly dimorphite-type As4Se3 ones. These cage molecules are merely destroyed under milling, facilitating the formation of a polymerized network with enhanced calorimetric heat-transfer responses. Disruption of intermediate-range ordering, due to weakening of the FSDP (the first sharp diffraction peak), accompanied by an enhancement of extended-range ordering, due to fragmentation of structural entities responsible for the SSDP (the second sharp diffraction peak), occurs as an interplay between medium-range structural levels in the reamorphized As4Se3 glass alloy. Nanomilling-driven destruction of thioarsenide As4Sen molecules followed by incorporation of their remnants into a glassy network is proved by micro-Raman spectroscopy. Microstructure scenarios of the molecular-to-network polyamorphic transformations caused by the decomposition of the As4Se3 molecules and their direct destruction under grinding are recognized by an ab initio quantum-chemical cluster-modeling algorithm. [ABSTRACT FROM AUTHOR]

In this study, the optimal microwave-assisted sol-gel synthesis parameters for achieving TiO2 nanoparticles with the highest specific surface area and photocatalytic activity were determined. Titanium isopropoxide was used as a precursor to prepare the sol (colloidal solution) of TiO2. Isopropanol was used as a solvent; acetylacetone was used as a complexation moderator; and nitric acid was used as a catalyst. Four samples of titanium dioxide were synthesized from the prepared colloidal solution in a microwave reactor at a temperature of 150 °C for 30 min and at a temperature of 200 °C for 10, 20, and 30 min. The phase composition of the TiO2 samples was determined by X-ray diffraction analysis (XRD) and Fourier-transform infrared spectroscopy (FTIR). Nitrogen adsorption/desorption isotherms were used to determine the specific surface area and pore size distributions using the Brunauer–Emmett–Teller (BET) method. The band-gap energy values of the TiO2 samples were determined by diffuse reflectance spectroscopy (DRS). The distribution of Ti and O in the TiO2 samples was determined by SEM-EDS analysis. The effects of adsorption and photocatalytic activity of the prepared TiO2 samples were evaluated by the degradation of ciprofloxacin (CIP) as an emerging organic pollutant (EOP) under UV-A light (365 nm). The results of the photocatalytic activity of the synthesized TiO2 nanoparticles were compared to the benchmark Degussa P25 TiO2. Kinetic parameters of adsorption and photocatalysis were determined and analyzed. It was found that crystalline TiO2 nanoparticles with the highest specific surface area, the lowest energy band gap, and the highest photocatalytic degradation were the samples synthesized at 200 °C for 10 min. The results indicate that CIP degradation by all TiO2 samples prepared at 200 °C show a synergistic effect of adsorption and photocatalytic degradation in the removal process. [ABSTRACT FROM AUTHOR]

With the global population on the rise, an escalating interest exists in environmentally sustainable and friendly protein sources. Insects have emerged as multifaceted resources, viewed not only as potential food items, but also as sources of traditional medicines and proteins. This study utilized response surface methodology (RSM) to ascertain the optimal extraction conditions for proteins from Musca domestica used in toad feeding, denoted as MDPs-T. The yield of MDPs-T was elevated to 18.3% ± 0.2% under these optimized conditions. Subsequently, the particle size, ζ-potentials, and structures of MDPs-T were analyzed and compared with the proteins derived from Musca domestica fed on a normal diet (MDPs-ND). This comparative analysis utilized a range of advanced techniques, involving UV spectroscopy, Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), high-performance gel permeation chromatography (HPGPC), and scanning electron microscopy (SEM). The outcomes have revealed a marginal disparity in the physical and chemical properties between MDPs-T and MDPs-ND. Derosination led to a reduction in the particle size of the MDPs by 10.98% to 62.81%. MDPs-T exhibited a higher proportion of low-molecular-weight components relative to MDPs-ND. Additionally, in a comparative analysis of amino acids, MDPs-T displayed a greater abundance of essential and total amino acids relative to MDPs-ND. Consequently, MDPs-T holds potential as a valuable food supplement for human consumption or as a nutrient-rich feed supplement for animals. [ABSTRACT FROM AUTHOR]

A wide range of nano-objects is found in many applications of our everyday life. Recognition of their peculiar properties and ease of functionalization has prompted their engineering into multifunctional platforms that are supposed to afford efficient tools for the development of biomedical applications. However, bridging the gap between bench to bedside cannot be expected without a good knowledge of their behaviour in vivo, which can be obtained through non-invasive imaging techniques, such as positron emission tomography (PET). Their radiolabelling with [18F]-fluorine, a technique already well established and widely used routinely for PET imaging, with [18F]-FDG for example, and in preclinical investigation using [18F]-radiolabelled biological macromolecules, has, therefore, been developed. In this context, this review highlights the various nano-objects studied so far, the reasons behind their radiolabelling, and main in vitro and/or in vivo results obtained thereof. Then, the methods developed to introduce the radioelement are presented. Detailed indications on the chemical steps involved are provided, and the stability of the radiolabelling is discussed. Emphasis is then made on the techniques used to purify and analyse the radiolabelled nano-objects, a point that is rarely discussed despite its technical relevance and importance for accurate imaging. The pros and cons of the different methods developed are finally discussed from which future work can develop. [ABSTRACT FROM AUTHOR]

Polysaccharides from cyanobacteria are extensively reported for their complex structures, good biocompatibility, and diverse bioactivities, but only a few cyanobacterial species have been exploited for the biotechnological production of polysaccharides. According to our previous study, the newly isolated marine cyanobacterium Cyanobacterium aponinum SCSIO-45682 was a good candidate for polysaccharide production. This work provided a systematic study of the extraction optimization, isolation, structural characterization, and bioactivity evaluation of polysaccharides from C. aponinum SCSIO-45682. Results showed that the crude polysaccharide yield of C. aponinum reached 17.02% by hot water extraction. The crude polysaccharides showed a porous and fibrous structure, as well as good moisture absorption and retention capacities comparable to that of sodium alginate. A homogeneous polysaccharide (Cyanobacterium aponinum polysaccharide, CAP) was obtained after cellulose DEAE-52 column and Sephadex G-100 column purification. CAP possessed a high molecular weight of 4596.64 kDa. It was mainly composed of fucose, galactose, and galacturonic acid, with a molar ratio of 15.27:11.39:8.64. The uronic acid content and sulfate content of CAP was 12.96% and 18.06%, respectively. Furthermore, CAP showed an in vitro growth inhibition effect on human hepatocellular carcinoma (HepG2) cells. The above results indicated the potential of polysaccharides from the marine cyanobacterium C. aponinum SCSIO-45682 as a moisturizer and anticancer addictive applied in cosmetical and pharmaceutical industries.

This study aimed to enhance the ultrasonic-assisted extraction (UAE) yield of seawater Arthrospira platensis polysaccharides (APPs) and investigate its structural characteristics and bioactivities. The optimization of UAE achieved a maximum crude polysaccharides yield of 14.78%. The optimal extraction conditions were a liquid–solid ratio of 30.00 mL/g, extraction temperature of 81 °C, ultrasonic power at 92 W and extraction time at 30 min. After purification through cellulose DEAE-52 and Sephadex G-100 columns, two polysaccharide elutions (APP-1 and APP-2) were obtained. APP-2 had stronger antioxidant and immunoregulatory activities than APP-1, thus the characterization of APP-2 was conducted. APP-2 was an acidic polysaccharide consisting of rhamnose, glucose, mannose and glucuronic acid at a ratio of 1.00:24.21:7.63:1.53. It possessed a molecular weight of 72.48 kDa. Additionally, APP-2 had linear and irregular spherical particles and amorphous structures, which contained pyranoid polysaccharides with alpha/beta glycosidic bonds. These findings offered the foundation for APP-2 as an antioxidant and immunomodulator applied in the food, pharmaceutical and cosmetic industries.

A condensation reaction of salicylic acid with formaldehyde in the presence of sulfuric acid led to the synthesization of the bis(2-hydroxy-3-carboxyphenyl)methane (BHCM) ligand, which was subsequently allowed to bind with nickel (II) ions. In light of the information obtained from the elemental analyses (C, H, and M), spectral (IR, MS, 1H-NMR, and UV–Vis) and thermal and magnetic measurements, the most likely structures of the ligand and complex have been identified. It has been suggested that the BHCM coordinates in a tetradentate manner with two Ni(II) ions to produce an octahedral binuclear complex. The SEM and TEM morphology of the compounds showed spherical shapes. An X-ray diffraction analysis indicated a considerable difference in the diffraction patterns between BHCM (crystalline) and Ni–BHCM (amorphous), and the Scherrer equation was used to calculate the crystallite size. Some optical characteristics were estimated from UV–Vis spectra. The ligand and its nickel(II) complex underlie the range of semiconductors. It was verified that for human lung (A-549) cancer, the BHCM compound displayed a significant barrier to the proliferation test in noncancerous cells (human lung fibroblasts, WI-38), which was also undertaken. To demonstrate the binding affinities of the chosen compounds (BHCM and Ni–BHCM) in the receptor protein’s active site [PDB ID: 5CAO], a molecular docking (MD) study was carried out.

The ultrasonic-assisted extraction (UAE) method was employed to separate Cinnamomum camphora proanthocyanidin-rich extracts (PCEs). This extraction process was optimized by the Box–Behnken design, and the optimal conditions, on a laboratory scale, were as follows: an ethanol concentration of 75%, a liquid-to-solid ratio of 24 mL/g, an ultrasonic time of 39 min, and an ultrasonic power of 540 W. Under the obtained conditions, the PCE yield extracted by UAE was higher than that from heat reflux extraction and soaking extraction. An ultra-performance liquid chromatography–tandem mass spectrometry analysis was employed to characterize the phloroglucinolysis products of the C. camphora PCEs, by which epigallocatechin, catechin, epicatechin, and (−)-epigallocatechin-3-O-gallate were identified as the terminal units; epigallocatechin, epicatechin, and (−)-epigallocatechin-3-O-gallate were recognized as extension units. The C. camphora PCEs possessed higher anti-ultraviolet activity in vitro compared with the commercially available sunscreen additive of benzophenone with respect to their ethanol solutions (sun protection factor of 27.01 ± 0.68 versus 1.96 ± 0.07 at a concentration of 0.09 mg/mL) and sunscreens (sun protection factor of 17.36 ± 0.62 versus 14.55 ± 0.47 at a concentration of 20%). These results demonstrate that C. camphora PCEs possess an excellent ultraviolet-protection ability and are promising green sunscreen additives that can replace commercial additives. [ABSTRACT FROM AUTHOR]

In total, three related substances (RS) associated with sotalol hydrochloride (STHCl) were herein identified with a novel gradient high-performance liquid chromatography (HPLC) protocol. Further characterization of these substances was then performed via liquid chromatography–mass spectroscopy (LC–MS/MS) and nuclear magnetic resonance (NMR) approaches. For these analyses, commercial STHCl samples were used for quantitative HPLC studies and the degradation of STHCl under acidic (1M HCl), alkaline (1M NaOH), oxidative (30% H2O2), photolytic (4500 Lx), and thermal stress conditions (100 °C) was assessed. This approach revealed this drug to be resistant to acidic, alkaline, and high-temperature conditions, whereas it was susceptible to light and oxidation as confirmed through long-term experiments. The putative mechanisms governing RS formation were also explored, revealing that RS3 was derived from the manufacturing process, whereas RS2 was generated via oxidation and RS1 was generated in response to light exposure. The cytotoxicity of these RS compounds was then assessed using MTT assays and acute toxicity test. Overall, this study provides details regarding the characterization, isolation, quantification, and toxicological evaluation of STHCl and associated RS compounds together with details regarding the precise, specific, and reliable novel HPLC technique, thus providing the requisite information necessary to ensure STHCl purity and safety. [ABSTRACT FROM AUTHOR]

The leaves of Psidium guajava L. are an agro-industrial by-product with an outstanding content of polyphenolic compounds; however, there are many factors which can affect the phytochemical profile when valuing this type of plant material, such as temperatures and extraction times involving in the extraction methods applied. In this context, this study analyzed the impact of different extraction methods (Soxhlet, maceration and ultrasound-assisted extraction) on the phytochemical profile (FTIR and UPLC-MS) and the antioxidant activity (ABTS, FRAP and Folin–Ciocalteu) of guava leaf extracts. A yield of phenolic compounds per gram of guava leaf was obtained within the range of 16 to 45 mg/g; on the other hand, the I C 50 values determined with the ABTS assay ranged between 78 ± 4 to 152 ± 12 µg/mL. The methanolic extract obtained by Soxhlet was the one with the best reducing power, both in the FRAP assay and in the Folin–Ciocalteu assay. Finally, bioactive compounds such as quercetin, kaempferol and avicularin were identified in the guava leaf extract. It was concluded that the purification of polyphenolics compounds improves the antioxidant capacity, and that the extraction method greatly influences the phytochemical profile and activity of the extracts. [ABSTRACT FROM AUTHOR]

Heterostructures of visible light-absorbing semiconductors were prepared through the growth of ZnIn2S4 crystallites in the presence of CdS nanostructures. A variety of hybrid compositions was synthesized. Both reference samples and heterostructured materials were characterized in detail, regarding their morphology, crystalline character, chemical speciation, as well as vibrational properties. The abovementioned physicochemical characterization suggested the absence of doping phenomena, such as the integration of either zinc or indium ions into the CdS lattice. At specific compositions, the growth of the amorphous ZnIn2S4 component was observed through both XRD and Raman analysis. The development of heterojunctions was found to be composition-dependent, as indicated by the simultaneous recording of the Raman profiles of both semiconductors. The optical band gaps of the hybrids range at values between the corresponding band gaps of reference semiconductors. The photocatalytic activity was assessed in both organic dye degradation and hydrogen peroxide evolution. It was observed that the hybrids demonstrating efficient photocatalytic activity in dye degradation were rather poor photocatalysts for hydrogen peroxide evolution. Specifically, the hybrids enriched in the CdS component were shown to act efficiently for hydrogen peroxide evolution, whereas ZnIn2S4-enriched hybrids demonstrated high potential to photodegrade an azo-type organic dye. Furthermore, scavenging experiments suggested the involvement of singlet oxygen in the mechanistic path for dye degradation.

Polyamorphic transformations driven by high-energy mechanical ball milling (nanomilling) are recognized in a melt-quenched glassy alloy of tetra-arsenic triselenide (As4Se3). We employed XRPD analysis complemented by thermophysical heat-transfer and micro-Raman spectroscopy studies. A straightforward interpretation of the medium-range structural response to milling-driven reamorphization is developed within a modified microcrystalline model by treating diffuse peak-halos in the XRPD patterns of this alloy as a superposition of the Bragg-diffraction contribution from inter-planar correlations, which are supplemented by the Ehrenfest-diffraction contribution from inter-atomic and/or inter-molecular correlations related to derivatives of thioarsenide As4Sen molecules, mainly dimorphite-type As4Se3 ones. These cage molecules are merely destroyed under milling, facilitating the formation of a polymerized network with enhanced calorimetric heat-transfer responses. Disruption of intermediate-range ordering, due to weakening of the FSDP (the first sharp diffraction peak), accompanied by an enhancement of extended-range ordering, due to fragmentation of structural entities responsible for the SSDP (the second sharp diffraction peak), occurs as an interplay between medium-range structural levels in the reamorphized As4Se3 glass alloy. Nanomilling-driven destruction of thioarsenide As4Sen molecules followed by incorporation of their remnants into a glassy network is proved by micro-Raman spectroscopy. Microstructure scenarios of the molecular-to-network polyamorphic transformations caused by the decomposition of the As4Se3 molecules and their direct destruction under grinding are recognized by an ab initio quantum-chemical cluster-modeling algorithm.

As a corrosion inhibitor for mild steel in a molar hydrochloric acid medium, we investigated the potential of Eucalyptus globulus essential oil (EuEO). Through electrochemical impedance spectroscopy (EIS), potentiodynamic polarization curves, and theoretical methods, including DFT/B3LYP 6-31G (d, p) and Monte Carlo simulations, the interactions between the EuEO components and the steel surface were analyzed. D-Allose, Betulinaldehyde, and Uvaol were identified as the major active compounds in the GC-MS analysis. The experimental results showed that EuEO reached an inhibitory efficiency as high as 97% at a 1 g/L concentration. The findings suggest that EuEO operates as a mixed-type inhibitor, reducing both cathodic and anodic reactions, as well as building up a protective coating on the steel surface. Simulations also confirmed that EuEO molecules function as electron donors and acceptors, enhancing corrosion resistance.

In this study, the optimal microwave-assisted sol-gel synthesis parameters for achieving TiO2 nanoparticles with the highest specific surface area and photocatalytic activity were determined. Titanium isopropoxide was used as a precursor to prepare the sol (colloidal solution) of TiO2. Isopropanol was used as a solvent; acetylacetone was used as a complexation moderator; and nitric acid was used as a catalyst. Four samples of titanium dioxide were synthesized from the prepared colloidal solution in a microwave reactor at a temperature of 150 °C for 30 min and at a temperature of 200 °C for 10, 20, and 30 min. The phase composition of the TiO2 samples was determined by X-ray diffraction analysis (XRD) and Fourier-transform infrared spectroscopy (FTIR). Nitrogen adsorption/desorption isotherms were used to determine the specific surface area and pore size distributions using the Brunauer–Emmett–Teller (BET) method. The band-gap energy values of the TiO2 samples were determined by diffuse reflectance spectroscopy (DRS). The distribution of Ti and O in the TiO2 samples was determined by SEM-EDS analysis. The effects of adsorption and photocatalytic activity of the prepared TiO2 samples were evaluated by the degradation of ciprofloxacin (CIP) as an emerging organic pollutant (EOP) under UV-A light (365 nm). The results of the photocatalytic activity of the synthesized TiO2 nanoparticles were compared to the benchmark Degussa P25 TiO2. Kinetic parameters of adsorption and photocatalysis were determined and analyzed. It was found that crystalline TiO2 nanoparticles with the highest specific surface area, the lowest energy band gap, and the highest photocatalytic degradation were the samples synthesized at 200 °C for 10 min. The results indicate that CIP degradation by all TiO2 samples prepared at 200 °C show a synergistic effect of adsorption and photocatalytic degradation in the removal process.

The (R)-(6-Methoxyquinolin-4-yl)[(1S,2S,4S,5R)-5-vinylquinuclidin-2-yl]methanol (quinine)-tetraphenylborate complex was synthesized by reacting sodium tetraphenyl borate with quinine in deionized water at room temperature through an ion-pair reaction (green chemistry) at room temperature. The solid complex was characterized by several physicochemical methods. The formation of ion-pair complex between bio-active molecules and/or organic molecules is crucial to comprehending the relationships between bioactive molecules and receptor interactions. The complex under study was examined for antimicrobial activity. All theoretical calculations were carried out in vacuum and water using the B3LYP level 6–311G(d,p) levels of theory. The theoretical computation allowed for the prediction and visualization of ionic interactions, which explained the complex's stability. The results of energy optimization showed that the Q-TPB complex is stable with a negative complexation energy. The obtained geometries showed that the boron (B−) and nitrogen (N+) in piperidine of the two molecules tetraphenylborate and quinine are close to each other, which makes it possible for ions to interact. The modest energy gap between HOMO and LUMO showed that the compound was stable. The computation of the electron transitions of the two models by density functional theory (TD-DFT) in the solvent at the theoretical level B3LYP/6–311G(d,p) allowed for the detection of three UV/visible absorption bands for both models and the discovery of a charge transfer between the host and the guest. The UV absorption, infrared, and H NMR are comparable with the experimental part. [ABSTRACT FROM AUTHOR]

A new certified reference material (CRM) of D-mannitol (GBW(E) 100681) has been developed in this study. We describe the preparation, structure determination, characterization, homogeneity study, stability study, as well as uncertainty estimation. The main component was 99.91% ± 0.01%. The moisture content of the candidate CRM was 0.036% ± 0.002%, as measured by Karl Fischer titration. The nonvolatile and volatile impurities in the candidate CRM were all much less than 0.01%, which was determined by the ICP–MS and headspace GC–FID methods, respectively. The purity of the D-mannitol CRM was 99.9% ± 1.1% (k = 2), as measured by the two independent approaches involving the mass balance method (MB) and quantitative nuclear magnetic resonance technique (qNMR). The D-mannitol CRM was stable during the monitoring period for each temperature. It is stable for up to 48 months at room temperature and 28 days at 50 °C. The uncertainty was evaluated by combining the contributions from characterization, homogeneity, and stability. The developed D-mannitol CRM would effectively support method validation and proficiency testing, as well as effectively guarantee the accuracy, reliability, and comparability of results. [ABSTRACT FROM AUTHOR]

With the global population on the rise, an escalating interest exists in environmentally sustainable and friendly protein sources. Insects have emerged as multifaceted resources, viewed not only as potential food items, but also as sources of traditional medicines and proteins. This study utilized response surface methodology (RSM) to ascertain the optimal extraction conditions for proteins from Musca domestica used in toad feeding, denoted as MDPs-T. The yield of MDPs-T was elevated to 18.3% ± 0.2% under these optimized conditions. Subsequently, the particle size, ζ-potentials, and structures of MDPs-T were analyzed and compared with the proteins derived from Musca domestica fed on a normal diet (MDPs-ND). This comparative analysis utilized a range of advanced techniques, involving UV spectroscopy, Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), high-performance gel permeation chromatography (HPGPC), and scanning electron microscopy (SEM). The outcomes have revealed a marginal disparity in the physical and chemical properties between MDPs-T and MDPs-ND. Derosination led to a reduction in the particle size of the MDPs by 10.98% to 62.81%. MDPs-T exhibited a higher proportion of low-molecular-weight components relative to MDPs-ND. Additionally, in a comparative analysis of amino acids, MDPs-T displayed a greater abundance of essential and total amino acids relative to MDPs-ND. Consequently, MDPs-T holds potential as a valuable food supplement for human consumption or as a nutrient-rich feed supplement for animals.

A wide range of nano-objects is found in many applications of our everyday life. Recognition of their peculiar properties and ease of functionalization has prompted their engineering into multifunctional platforms that are supposed to afford efficient tools for the development of biomedical applications. However, bridging the gap between bench to bedside cannot be expected without a good knowledge of their behaviour in vivo, which can be obtained through non-invasive imaging techniques, such as positron emission tomography (PET). Their radiolabelling with [18F]-fluorine, a technique already well established and widely used routinely for PET imaging, with [18F]-FDG for example, and in preclinical investigation using [18F]-radiolabelled biological macromolecules, has, therefore, been developed. In this context, this review highlights the various nano-objects studied so far, the reasons behind their radiolabelling, and main in vitro and/or in vivo results obtained thereof. Then, the methods developed to introduce the radioelement are presented. Detailed indications on the chemical steps involved are provided, and the stability of the radiolabelling is discussed. Emphasis is then made on the techniques used to purify and analyse the radiolabelled nano-objects, a point that is rarely discussed despite its technical relevance and importance for accurate imaging. The pros and cons of the different methods developed are finally discussed from which future work can develop.

Organotin (IV) dithiocarbamate has recently received attention as a therapeutic agent among organotin (IV) compounds. The individual properties of the organotin (IV) and dithiocarbamate moieties in the hybrid complex form a synergy of action that stimulates increased biological activity. Organotin (IV) components have been shown to play a crucial role in cytotoxicity. The biological effects of organotin compounds are believed to be influenced by the number of Sn-C bonds and the number and nature of alkyl or aryl substituents within the organotin structure. Ligands target and react with molecules while preventing unwanted changes in the biomolecules. Organotin (IV) dithiocarbamate compounds have also been shown to have a broad range of cellular, biochemical, and molecular effects, with their toxicity largely determined by their structure. Continuing the investigation of the cytotoxicity of organotin (IV) dithiocarbamates, this mini-review delves into the appropriate method for synthesis and discusses the elemental and spectroscopic analyses and potential cytotoxic effects of these compounds from articles published since 2010. [ABSTRACT FROM AUTHOR]

The significance of nanomaterials in biomedicines served as the inspiration for the design of this study. In this particular investigation, we carried out the biosynthesis of calcium oxide nanoparticles (CaONPs) by employing a green-chemistry strategy and making use of an extract of Ficus carica (an edible fruit) as a capping and reducing agent. There is a dire need for new antimicrobial agents due to the alarming rise in antibiotic resistance. Nanoparticles' diverse antibacterial properties suggest that they might be standard alternatives to antimicrobial drugs in the future. We describe herein the use of a Ficus carica extract as a capping and reducing agent in the phyto-mediated synthesis of CaONPs for the evaluation of their antimicrobial properties. The phyto-mediated synthesis of NPs is considered a reliable approach due to its high yield, stability, non-toxicity, cost-effectiveness and eco-friendliness. The CaONPs were physiochemically characterized by UV-visible spectroscopy, energy-dispersive X-ray (EDX), scanning-electron microscopy (SEM), X-ray diffraction (XRD), and Fourier-transform infrared spectroscopy (FTIR). The biological synthesis of the calcium oxide nanoparticles revealed a characteristic surface plasmon resonance peak (SPR) at 360 nm in UV-Vis spectroscopy, which clearly revealed the successful reduction of the Ca2+ ions to Ca0 nanoparticles. The characteristic FTIR peak seen at 767 cm−1 corresponded to Ca-O bond stretching and, thus, confirmed the biosynthesis of the CaONPs, while the scanning-electron micrographs revealed near-CaO aggregates with an average diameter of 84.87 ± 2.0 nm. The antibacterial and anti-biofilm analysis of the CaONPs showed inhibition of bacteria in the following order: P. aeruginosa (28 ± 1.0) > S. aureus (23 ± 0.3) > K. pneumoniae (18 ± 0.9) > P. vulgaris (13 ± 1.6) > E. coli (11 ± 0.5) mm. The CaONPs were shown to considerably inhibit biofilm formation, providing strong evidence for their major antibacterial activity. It is concluded that this straightforward environmentally friendly method is capable of synthesizing stable and effective CaONPs. The therapeutic value of CaONPs is indicated by their potential as a antibacterial and antibiofilm agents in future medications. [ABSTRACT FROM AUTHOR]

Engineering research has been expanded by the advent of material fusion, which has led to the development of composites that are more reliable and cost-effective. This investigation aims to utilise this concept to promote a circular economy by maximizing the adsorption of silver nanoparticles and silver nitrate onto recycled chicken eggshell membranes, resulting in optimized antimicrobial silver/eggshell membrane composites. The pH, time, concentration, and adsorption temperatures were optimized. It was confirmed that these composites were excellent candidates for use in antimicrobial applications. The silver nanoparticles were produced through chemical synthesis using sodium borohydride as a reducing agent and through adsorption/surface reduction of silver nitrate on eggshell membranes. The composites were thoroughly characterized by various techniques, including spectrophotometry, atomic absorption spectrometry, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy, as well as agar well diffusion and MTT assay. The results indicate that silver/eggshell membrane composites with excellent antimicrobial properties were produced using both silver nanoparticles and silver nitrate at a pH of 6, 25 °C, and after 48 h of agitation. These materials exhibited remarkable antimicrobial activity against Pseudomonas aeruginosa and Bacillus subtilis, resulting in 27.77% and 15.34% cell death, respectively. [ABSTRACT FROM AUTHOR]

Thymoquinone (TQ) is a quinone derived from the black seed Nigella sativa and has been extensively studied in pharmaceutical and nutraceutical research due to its therapeutic potential and pharmacological properties. Although the chemopreventive and potential anticancer effects of TQ have been reported, its limited solubility and poor delivery remain the major limitations. In this study, we aimed to characterize the inclusion complexes of TQ with Sulfobutylether-β-cyclodextrin (SBE-β-CD) at four different temperatures (293–318 K). Additionally, we compared the antiproliferative activity of TQ alone to TQ complexed with SBE-β-CD on six different cancer cell lines, including colon, breast, and liver cancer cells (HCT-116, HT-29, MDA-MB-231, MCF-7, SK-BR-3, and HepG2), using an MTT assay. We calculated the thermodynamic parameters (ΔH, ΔS, and ΔG) using the van't Holf equation. The inclusion complexes were characterized by X-ray diffraction (XRD), Fourier transforms infrared (FT-IR), and molecular dynamics using the PM6 model. Our findings revealed that the solubility of TQ was improved by ≥60 folds, allowing TQ to penetrate completely into the cavity of SBE-β-CD. The IC50 values of TQ/SBE-β-CD ranged from 0.1 ± 0.01 µg/mL against SK-BR-3 human breast cancer cells to 1.2 ± 0.16 µg/mL against HCT-116 human colorectal cancer cells, depending on the cell line. In comparison, the IC50 values of TQ alone ranged from 0.2 ± 0.01 µg/mL to 4.7 ± 0.21 µg/mL. Overall, our results suggest that SBE-β-CD can enhance the anticancer effect of TQ by increasing its solubility and bioavailability and cellular uptake. However, further studies are necessary to fully understand the underlying mechanisms and potential side effects of using SBE-β-CD as a drug delivery system for TQ. [ABSTRACT FROM AUTHOR]

Echinacea purpurea is a perennial plant that belongs to the Asteraceae family. It has a wide range of applications mainly in the treatment and prevention of inflammations in the respiratory system. The current study aimed to perform a phytochemical characterization of purple coneflower (Echinacea purpurea) roots and their extracts (water, 40%, 50%, 60% ethanol, and 60% glycerol). Phytochemical characterization was carried out by gravimetric, spectrophotometric, and chromatographic methods. Echinacea roots were characterized by a low lipid (0.8%) content. In contrast, carbohydrates (45%) and proteins (20%) occupied a large part of the dry matter. Amongst the extracts, the highest yield was obtained using water as a solvent (53%). Water extract was rich in protein and carbohydrates as fructans (inulin) were the most abundant carbohydrate constituent. The most exhaustive recovery of the phenolic components was conducted by extraction with 40% ethanol and 60% glycerol. It was found that water is the most suitable extractant for obtaining a polysaccharide-containing complex (PSC) (8.87%). PSC was composed mainly of fructans (inulin) and proteins with different molecular weight distributions. The yield of PSC decreased with an increasing ethanol concentration (40% > 50% > 60%) but the lowest yield was obtained from 60% glycerol extract. The obtained results showed that Echinacea roots contained a large amount of biologically active substances—phenolic components and polysaccharides and that glycerol was equally efficient to ethanol in extracting caffeic acid derivatives from purple coneflower roots. The data can be used for the preparation of extracts having different compositions and thus easily be incorporated into commercial products. [ABSTRACT FROM AUTHOR]

Cadmium sulfide nanoparticles (CdS NPs) have been employed in various fields of nanobiotechnology due to their proven biomedical properties. They are unique in their properties due to their size and shape, and they are popular in the area of biosensors, bioimaging, and antibacterial and anticancer applications. Most CdS NPs are generally synthesized through chemical, physical, or biological methods. Among these methods, biogenic synthesis has attracted more attention due to its high efficiency, environmental friendliness, and biocompatibility features. The green approach was found to be superior to other methods in terms of maintaining the structural characteristics needed for optimal biomedical applications. The size and coating components of CdS NPs play a crucial role in their biomedical activities, such as anticancer, antibacterial, bioimaging, and biosensing applications. CdS NPs have gained significant interest in bioimaging due to their desirable properties, including good dispersion, cell integrity preservation, and efficient light scattering. Despite these, further studies are necessary, particularly in vivo studies to reduce NPs' toxicity. This review discusses the different methods of synthesis, how CdS NPs are characterized, and their applications in the biomedical field. [ABSTRACT FROM AUTHOR]

Myo-inositol polyalcohol is a characteristic component of natural and concentrated grape musts (CMs), and Regulation (EU) no. 1308/2013 prescribes its presence as a marker of the authenticity of rectified concentrated must (RCM). Other polyalcohols besides myo-inositol, such as scyllo-inositol or minor sugars, could be considered authenticity markers, but an extensive search in the literature yielded no exhaustively investigated study of their concentration variability in genuine products. The aim of this study was to create an extensive national data bank of minor carbohydrates profiles and investigate the impact of the geographical origin and the different vintages on the concentration of these compounds; to this end, 450 authentic Italian grape musts of different varieties were sampled and analyzed during the harvest season in 2019, 2020, and 2021. The grape musts from the Italian wine-growing areas CII and CIIIb had myo- and scyllo-inositol contents always higher than 756 and 39 mg/kg of sugar, respectively. Conversely, also considering other mono- and disaccharides, sucrose, sorbitol, lactose, maltose, and isomaltose showed contents always lower than 534, 1207, 390, 2222, and 1639 mg/kg of sugar, respectively. The general applicability to the CM and RCM of the proposed authenticity thresholds, established in the must, was demonstrated by studying the influence of must concentration on the myo- and scyllo-inositol content. Inter-laboratory comparison experiments were also conducted to harmonize and characterize laboratory methods and validate the analytical dataset. Based on the obtained results, the text of the EU legislation (Reg. (EU) 1308/2013), which defines the characteristics of the must and the CRM product, should be revised. [ABSTRACT FROM AUTHOR]

Glycosylation is a critical quality attribute in biotherapeutics, impacting properties such as protein stability, solubility, clearance rate, efficacy, immunogenicity, and safety. Due to the heterogenic and complex nature of protein glycosylation, comprehensive characterization is demanding. Moreover, the lack of standardized metrics for evaluating and comparing glycosylation profiles hinders comparability studies and the establishment of manufacturing control strategies. To address both challenges, we propose a standardized approach based on novel metrics for a comprehensive glycosylation fingerprint which greatly facilitates the reporting and objective comparison of glycosylation profiles. The analytical workflow is based on a liquid chromatography–mass spectrometry-based multi-attribute method. Based on the analytical data, a matrix of glycosylation-related quality attributes, both at site-specific and whole molecule level, are computed, which provide metrics for a comprehensive product glycosylation fingerprint. Two case studies illustrate the applicability of the proposed indices as a standardized and versatile approach for reporting all dimensions of the glycosylation profile. The proposed approach further facilitates the assessments of risks associated with changes in the glycosylation profile that may affect efficacy, clearance, and immunogenicity. [ABSTRACT FROM AUTHOR]

In this study, various techniques, including X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDS) mapping, X-ray photoelectron spectroscopy (XPS), and water-contact-angle goniometry (WCAG), were used to characterize the crystalline structure and morphological properties of terbium-doped cerium magnesium aluminate (Ce0.67Tb0.33MgAl11O19 or CMAT) in powder form. The results demonstrated that CMAT was successfully synthesized with a particle size of less than 5 µm and a fully evident distribution of elements, as revealed by the SEM images. This was further confirmed by the XRD and HRTEM images. XPS analysis confirmed the presence of all necessary components in CMAT. Additionally, WCAG results showed that the contact angle of CMAT was more hydrophilic with a value of 8.4°. To evaluate its performance, CMAT particles were dispersed in a Polyethersulfone (PES) solution and used to modify a PES ultrafiltration membrane through a phase-inversion method. The resulting membranes were characterized by SEM, atomic force microscopy (AFM), thermogravimetric analysis (TGA), WCAG, and permeability performance and fouling experiments. The addition of CMAT to the PES membranes did not have a significant effect on the structure of the SEM images of the top layer and cross-section of surface properties. However, increasing the concentration of CMAT improved the membrane surface roughness in AFM, and the modified membranes had the ability to resist fouling. The addition of CMAT did not lead to significant energy loss, indicating that the heat flux loss observed can indeed be explained by the amount of C-OH on the PES membrane's surface. The contact angle of the membranes became more hydrophilic with increasing concentration of CMAT from PES G0 to PES G7. The PES origin membrane showed a higher permeation than the membranes mixed with CMAT, and the modified membranes with CMAT displayed significant fouling resistance. [ABSTRACT FROM AUTHOR]

Furosemide is a widely used loop diuretic in the treatment of congestive heart failure and edema. During the preparation of furosemide, a new process-related impurity G in the levels ranging from 0.08% to 0.13% was detected in pilot batches by a new high performance liquid chromatography (HPLC) method. The new impurity was isolated and characterized by comprehensive analysis of FT-IR, Q-TOF/LC-MS, 1D-NMR (1H, 13C, and DEPT), and 2D-NMR (1H-1H-COSY, HSQC, and HMBC) spectroscopy data. The possible formation pathway of impurity G was also discussed in detail. Moreover, a novel HPLC method was developed and validated for the determination of impurity G and the other six known impurities registered in the European Pharmacopoeia as per ICH guidelines. The HPLC method was validated with respect to system suitability, linearity, the limit of quantitation, the limit of detection, precision, accuracy, and robustness. The characterization of impurity G and the validation of its quantitative HPLC method were reported for the first time in this paper. Finally, the toxicological properties of impurity G were predicted by the in silico webserver ProTox-II. [ABSTRACT FROM AUTHOR]

The 4-amino-N-[2 (diethylamino) ethyl] benzamide (procainamide)-tetraphenylborate complex was synthesized by reacting sodium tetraphenyl borate with 4-amino-N-[2 (diethylamino) ethyl] benzamide, chloride salt, and procainamide in deionized water at room temperature through an ion-associate reaction (green chemistry) at room temperature, and characterized by several physicochemical methods. The formation of ion-associate complex between bio-active molecules and/or organic molecules is crucial to comprehending the relationships between bioactive molecules and receptor interactions. The solid complex was characterized by infrared spectra, NMR, elemental analysis, and mass spectrometry, indicating the formation of ion-associate or ion-pair complex. The complex under study was examined for antibacterial activity. The ground state electronic characteristics of the S1 and S2 complex configurations were computed using the density functional theory (DFT) approach, using B3LYP level 6-311 G(d,p) basis sets. R2 = 0.9765 and 0.9556, respectively, indicate a strong correlation between the observed and theoretical 1H-NMR, and the relative error of vibrational frequencies for both configurations was acceptable, as well. HOMO and LUMO frontier molecular orbitals and molecular electrostatics using the optimized were used to obtain a potential map of the chemical. The n → π* UV absorption peak of the UV cutoff edge was detected for both configurations of the complex. Spectroscopic methods were structures used to characterize the structure (FT-IR and 1HNMR). In the ground state, DFT/B3LYP/6-311G(d,p) basis sets were used to determine the electrical and geometric properties of the S1 and S2 configurations of the title complex. Comparing the observed and calculated values for the S1 and S2 forms, the HOMO-LUMO energy gap of compounds was 3182 and 3231 eV, respectively. The small energy gap between HOMO and LUMO indicated that the compound was stable. In addition, the MEP reveals that positive potential sites were around the PR molecule, whereas negative potential sites were surrounding the TPB site of atoms. The UV absorption of both arrangements is comparable to the experimental UV spectrum. [ABSTRACT FROM AUTHOR]

Over the centuries, humans have developed different systems to protect surfaces from the influence of environmental factors. Protective paints are the most used ones. They have undergone considerable development over the years, especially at the turn of the 19th and 20th centuries. Indeed, between the two centuries, new binders and pigments have been introduced in the constituent materials of paints. The years in which these compounds have been introduced and spread in the paint market allow them to be defined as markers for the dating of paints and painted artifacts. The present work is focused on the study of the paints of two vehicles of the Frankfurt Museum of Communication, i.e., a carriage and a cart, that was designed for the German Postal and Telecommunications Service roughly between 1880 and 1920. The characterization of the paints was performed through in situ non-invasive techniques, i.e., portable optical microscopy and multispectral imaging, and laboratory non-destructive techniques, i.e., FT-IR ATR spectroscopy and SEM-EDS. The analytical investigation and the comparison with the data reported in the literature allowed us to determine the historicity of the paints, which are all dated before the 1950s. [ABSTRACT FROM AUTHOR]

The ultrasonic-assisted extraction (UAE) method was employed to separate Cinnamomum camphora proanthocyanidin-rich extracts (PCEs). This extraction process was optimized by the Box–Behnken design, and the optimal conditions, on a laboratory scale, were as follows: an ethanol concentration of 75%, a liquid-to-solid ratio of 24 mL/g, an ultrasonic time of 39 min, and an ultrasonic power of 540 W. Under the obtained conditions, the PCE yield extracted by UAE was higher than that from heat reflux extraction and soaking extraction. An ultra-performance liquid chromatography–tandem mass spectrometry analysis was employed to characterize the phloroglucinolysis products of the C. camphora PCEs, by which epigallocatechin, catechin, epicatechin, and (−)-epigallocatechin-3-O-gallate were identified as the terminal units; epigallocatechin, epicatechin, and (−)-epigallocatechin-3-O-gallate were recognized as extension units. The C. camphora PCEs possessed higher anti-ultraviolet activity in vitro compared with the commercially available sunscreen additive of benzophenone with respect to their ethanol solutions (sun protection factor of 27.01 ± 0.68 versus 1.96 ± 0.07 at a concentration of 0.09 mg/mL) and sunscreens (sun protection factor of 17.36 ± 0.62 versus 14.55 ± 0.47 at a concentration of 20%). These results demonstrate that C. camphora PCEs possess an excellent ultraviolet-protection ability and are promising green sunscreen additives that can replace commercial additives.

In total, three related substances (RS) associated with sotalol hydrochloride (STHCl) were herein identified with a novel gradient high-performance liquid chromatography (HPLC) protocol. Further characterization of these substances was then performed via liquid chromatography–mass spectroscopy (LC–MS/MS) and nuclear magnetic resonance (NMR) approaches. For these analyses, commercial STHCl samples were used for quantitative HPLC studies and the degradation of STHCl under acidic (1M HCl), alkaline (1M NaOH), oxidative (30% H2O2), photolytic (4500 Lx), and thermal stress conditions (100 °C) was assessed. This approach revealed this drug to be resistant to acidic, alkaline, and high-temperature conditions, whereas it was susceptible to light and oxidation as confirmed through long-term experiments. The putative mechanisms governing RS formation were also explored, revealing that RS3 was derived from the manufacturing process, whereas RS2 was generated via oxidation and RS1 was generated in response to light exposure. The cytotoxicity of these RS compounds was then assessed using MTT assays and acute toxicity test. Overall, this study provides details regarding the characterization, isolation, quantification, and toxicological evaluation of STHCl and associated RS compounds together with details regarding the precise, specific, and reliable novel HPLC technique, thus providing the requisite information necessary to ensure STHCl purity and safety.

The leaves of Psidium guajava L. are an agro-industrial by-product with an outstanding content of polyphenolic compounds; however, there are many factors which can affect the phytochemical profile when valuing this type of plant material, such as temperatures and extraction times involving in the extraction methods applied. In this context, this study analyzed the impact of different extraction methods (Soxhlet, maceration and ultrasound-assisted extraction) on the phytochemical profile (FTIR and UPLC-MS) and the antioxidant activity (ABTS, FRAP and Folin–Ciocalteu) of guava leaf extracts. A yield of phenolic compounds per gram of guava leaf was obtained within the range of 16 to 45 mg/g; on the other hand, the IC50 values determined with the ABTS assay ranged between 78 ± 4 to 152 ± 12 µg/mL. The methanolic extract obtained by Soxhlet was the one with the best reducing power, both in the FRAP assay and in the Folin–Ciocalteu assay. Finally, bioactive compounds such as quercetin, kaempferol and avicularin were identified in the guava leaf extract. It was concluded that the purification of polyphenolics compounds improves the antioxidant capacity, and that the extraction method greatly influences the phytochemical profile and activity of the extracts.

Cross-linked enzyme aggregates (CLEAs) represent an effective tool for carrier-free immobilization of enzymes. The present study promotes a successful application of functionalized magnetic nanoparticles (MNPs) for stabilization of cellulase CLEAs. Catalytically active CLEAs and magnetic cross-linked enzyme aggregates (mCLEAs) of cellulase from Trichoderma reesei were prepared using glutaraldehyde (GA) as a cross-linking agent and the catalytic activity and stability of the CLEAs/mCLEAs were investigated. The influence of precipitation agents, cross-linker concentration, concentration of enzyme, addition of bovine serum albumin (BSA), and addition of sodium cyanoborohydride (NaBH3CN) on expressed activity and immobilization yield of CLEAs/mCLEAs was studied. Particularly, reducing the unsaturated Schiff's base to form irreversible linkages is important and improved the activity of CLEAs (86%) and mCLEAs (91%). For increased applicability of CLEAs/mCLEAs, we enhanced the activity and stability at mild biochemical process conditions. The reusability after 10 cycles of both CLEAs and mCLEAs was investigated, which retained 72% and 65% of the initial activity, respectively. The thermal stability of CLEAs and mCLEAs in comparison with the non-immobilized enzyme was obtained at 30 °C (145.65% and 188.7%, respectively) and 50 °C (185.1% and 141.4%, respectively). Kinetic parameters were determined for CLEAs and mCLEAs, and the KM constant was found at 0.055 ± 0.0102 mM and 0.037 ± 0.0012 mM, respectively. The maximum velocity rate (Vmax) was calculated as 1.12 ± 0.0012 µmol/min for CLEA and 1.17 ± 0.0023 µmol/min for mCLEA. Structural characterization was studied using XRD, SEM, and FT-IR. Catalytical properties of immobilized enzyme were improved with the addition of reducent NaBH3CN by enhancing the activity of CLEAs and with addition of functionalized aminosilane MNPs by enhancing the activity of mCLEAs. [ABSTRACT FROM AUTHOR]

Elaeagnus angustifolia (EA) mediated green chemistry route was used for the biofabrication of NiONPs without the provision of additional surfactants and capping agents. The formation of NiONPs was confirmed using advanced different characterization techniques such as Scanning electron microscopy, UV, Fourier transmission-infrared, RAMAN, and energy dispersal spectroscopic and dynamic light scattering techniques. Further, different biological activities of EA-NiONPs were studied. Antibacterial activities were performed using five different bacterial strains using disc-diffusion assays and have shown significant results as compared to standard Oxytetracycline discs. Further, NiONPs exhibited excellent antifungal performance against different pathogenic fungal strains. The biocompatibility test was performed using human RBCs, which further confirmed that NiONPs are more biocompatible at the concentration of 7.51–31.25 µg/mL. The antioxidant activities of NiONPs were investigated using DPPH free radical scavenging assay. The NiONPs were demonstrated to have much better antioxidant potentials in terms of % DPPH scavenging (93.5%) and total antioxidant capacity (81%). Anticancer activity was also performed using HUH7 and HEP-G2 cancer cell lines and has shown significant potential with IC50 values of 18.45 μg/mL and 14.84 μg/mL, respectively. Further, the NiONPs were evaluated against Lesihmania tropica parasites and have shown strong antileishmanial potentials. The EA-NiONPs also showed excellent enzyme inhibition activities; protein kinase (19.4 mm) and alpha-amylase (51%). In conclusion, NiONPs have shown significant results against different biological assays. In the future, we suggest various in vivo activities for EA-NiONPs using different animal models to further unveil the biological and biomedical potentials. [ABSTRACT FROM AUTHOR]

Consumers increasingly prefer and seek functional beverages, which, given their characteristics, provide important bioactive compounds that help prevent and treat chronic diseases. Mead is a traditional fermented alcoholic beverage made from honey solution. The aging process of mead with oak chips is innovative and bestows functional characteristics to this beverage. Thus, in this study, we sought to develop and characterize a novel functional beverage by combining the health benefits of honey with the traditional aging process of alcoholic beverages in wood. Phenolic compounds, flavonoids, and antioxidant capacity were analyzed in mead using oak chips at different toasting levels and aged for 360 days. LC-ESI-QTOF-MS/MS was used to analyze the chemical profile of different meads. Over time, the aging process with oak chips showed a higher total phenolic and flavonoid content and antioxidant capacity. Eighteen compounds belonging to the classes of organic acids, phenolic acids, flavonoids, and tannins were identified in meads after 360 days. Our findings revealed that the addition of oak chips during aging contributed to p-coumaric, ellagic, abscisic, and chlorogenic acids, and naringenin, vanillin, and tiliroside significantly impacted the functional quality of mead. [ABSTRACT FROM AUTHOR]

The extraction, characterization and antioxidant activity of polysaccharides from Choerospondias axillaris leaves were investigated in the present study. Two purified polysaccharide fractions, CALP-1 and CALP-2, were isolated from crude Choerospondias axillaris leaf polysaccharides (CALP) by DEAE-52 cellulose chromatography and Sephadex G-100 column chromatography. The characteristics of CAL-1 and CALP-2 were determined by using High-performance Gel Permeation Chromatography (HPGPC), High-Performance Anion-Exchange Chromatography, HPAEC (HPAEC-PAD) and Fourier transform infrared spectroscopy (FTIR). CALP-1 with molecular weight of 11.20 KDa was comprised of Rhamnose, Arabinose, Galactose, Glucose, Xylose, Mannose and galacturonic acid in a molar ratio of 5.16:2.31:5.50:27.18:1.00:0.76:1.07. CAL-2 with molecular weight of 8.03 KDa consisted of Rhamnose, Arabinose, Galactose, Glucose, and galacturonic acid at a ratio of 1.38:3.63:18.84:8.28:1.45. FTIR revealed that CALP-1 and CALP-2 were acidic polysaccharides. The antioxidant activity of crude CALP, CALP-1 and CALP-2 was evaluated in vitro. The fraction CALP-2 was demonstrated to be of polysaccharide nature containing a large percentage of Galactose but no Xylose and Mannose. The antioxidant activity assays showed that CALP-1 and CALP-2 exhibited antioxidant and scavenging activities on hydroxyl and DPPH radicals in vitro. Compared with pure polysaccharide, crude CALP exhibited stronger anti-oxidant activities. These results will provide a better understanding of Choerospondias axillaris leaf polysaccharide and promote the potential applications of Choerospondias axillaris leaf polysaccharide in the pharmacological field and as a natural antioxidant. [ABSTRACT FROM AUTHOR]

In this study, a new colistin-functionalized silica gel material (SiO2@NH2@COOH@CST) was synthesized after carboxylation on the surface of amino-modified silica. The main factors affecting the adsorptive properties of the material, such as the types of linkers, the linking methods, the reaction buffers and the particle sizes of carriers, were systematically investigated. The SiO2@NH2@COOH@CST was characterized by means of electron microscopy, Fourier-transform infrared spectroscopy, zeta potential measurements, etc. We demonstrated that the sorbent showed good adsorption of Gram-negative bacteria. The adsorption efficiency of E. coli on SiO2@NH2@COOH@CST was 5.2 × 1011 CFU/g, which was 3.5 times higher than that on SiO2@NH2@COOH, suggesting that electrostatic interactions between SiO2@NH2@COOH@CST and E. coli played a key role. The adsorption was quick, and was reached in 5 min. Both pseudo-first-order and pseudo-second-order kinetic models fit well with the dynamic adsorption process of SiO2@NH2@COOH@CST, indicating that physical adsorption and chemisorption might occur simultaneously during the adsorption process. SiO2@NH2@COOH@CST was successfully applied for the rapid capture of bacteria from water. The synthesized material could be used as a potential means of bacterial isolation and detection. [ABSTRACT FROM AUTHOR]

The current study aims to develop eco-friendly and economical chitosans with a wide range of applications using organic acids for shrimp shells demineralization. Chitosan samples were extracted from shrimp (Parapenaeus longirostris) shells and the demineralization step was performed with three organic acids (citric, acetic, and lactic) and two mineral acids (hydrochloric and sulfuric). The chitosans were characterized by Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), and scanning electron microscopy (SEM). The chitosans' physicochemical properties were also determined. The characteristic bands and functional groups of the chitosans were identified by FTIR spectra. The chitosans' crystallinity order was as follows: ChHCl > ChCitric > ChH2SO4 > ChLactic > ChAcetic. The chitosans' morphological characteristics revealed a smooth surface and fibrous structures with pores. Chitosans extracted by organic acids showed the highest extraction yields. ChHCl and ChCitric had higher degrees of deacetylation values; 83.67% and 81.47%, respectively. The solubility was proportional to the degree of deacetylation. Furthermore, ChH2SO4 and ChCitric had lower molecular weight values; 149 kDa and 183 kDa, respectively. Organic acids are as effective as mineral acids for shrimp shells demineralization. The developed process opens up possibilities to produce chitin and chitosan in a more eco-friendly way and at a lower cost in many industrial sectors. [ABSTRACT FROM AUTHOR]

The (R)-(6-Methoxyquinolin-4-yl)[(1S,2S,4S,5R)-5-vinylquinuclidin-2-yl]methanol (quinine)-tetraphenylborate complex was synthesized by reacting sodium tetraphenyl borate with quinine in deionized water at room temperature through an ion-pair reaction (green chemistry) at room temperature. The solid complex was characterized by several physicochemical methods. The formation of ion-pair complex between bio-active molecules and/or organic molecules is crucial to comprehending the relationships between bioactive molecules and receptor interactions. The complex under study was examined for antimicrobial activity. All theoretical calculations were carried out in vacuum and water using the B3LYP level 6–311G(d,p) levels of theory. The theoretical computation allowed for the prediction and visualization of ionic interactions, which explained the complex’s stability. The results of energy optimization showed that the Q-TPB complex is stable with a negative complexation energy. The obtained geometries showed that the boron (B−) and nitrogen (N+) in piperidine of the two molecules tetraphenylborate and quinine are close to each other, which makes it possible for ions to interact. The modest energy gap between HOMO and LUMO showed that the compound was stable. The computation of the electron transitions of the two models by density functional theory (TD-DFT) in the solvent at the theoretical level B3LYP/6–311G(d,p) allowed for the detection of three UV/visible absorption bands for both models and the discovery of a charge transfer between the host and the guest. The UV absorption, infrared, and H NMR are comparable with the experimental part.

A new certified reference material (CRM) of D-mannitol (GBW(E) 100681) has been developed in this study. We describe the preparation, structure determination, characterization, homogeneity study, stability study, as well as uncertainty estimation. The main component was 99.91% ± 0.01%. The moisture content of the candidate CRM was 0.036% ± 0.002%, as measured by Karl Fischer titration. The nonvolatile and volatile impurities in the candidate CRM were all much less than 0.01%, which was determined by the ICP–MS and headspace GC–FID methods, respectively. The purity of the D-mannitol CRM was 99.9% ± 1.1% (k = 2), as measured by the two independent approaches involving the mass balance method (MB) and quantitative nuclear magnetic resonance technique (qNMR). The D-mannitol CRM was stable during the monitoring period for each temperature. It is stable for up to 48 months at room temperature and 28 days at 50 °C. The uncertainty was evaluated by combining the contributions from characterization, homogeneity, and stability. The developed D-mannitol CRM would effectively support method validation and proficiency testing, as well as effectively guarantee the accuracy, reliability, and comparability of results.

The current study examines the desiccation-resistant Ramlibacter tataouinensis TTB310T as a model organism for the production of novel exopolysaccharides and their structural features. This bacterium is able to produce dividing forms of cysts which synthesize cell-bound exopolysaccharide. Initial experiments were conducted on the enrichment of cyst biomass for exopolysaccharide production under batch-fed conditions in a pilot-scale bioreactor, with lactate as the source of carbon and energy. The optimized medium produced significant quantities of exopolysaccharide in a single growth phase, since the production of exopolysaccharide took place during the division of the cysts. The exopolysaccharide layer was extracted from the cysts using a modified trichloroacetic acid method. The biochemical characterization of purified exopolysaccharide was performed by gas chromatography, ultrahigh-resolution mass spectrometry, nuclear magnetic resonance, and Fourier-transform infrared spectrometry. The repeating unit of exopolysaccharide was a decasaccharide consisting of ribose, glucose, rhamnose, galactose, mannose, and glucuronic acid with the ratio 3:2:2:1:1:1, and additional substituents such as acetyl, succinyl, and methyl moieties were also observed as a part of the exopolysaccharide structure. This study contributes to a fundamental understanding of the novel structural features of exopolysaccharide from a dividing form of cysts, and, further, results can be used to study its rheological properties for various industrial applications. [ABSTRACT FROM AUTHOR]

Auricularia auricula-judae polysaccharide (AAP)-based nanoparticles (NPs) prepared via an anti-solvent precipitation approach were studied. Response surface methodology (RSM) design was carried out on the basis of single factor experiments, using average size and polydispersity index (PDI) as indicators. The optimal preparation conditions were determined to include an AAP concentration of 1 mg/mL, a pH of 8, and an anti-solvent/solvent volume ratio of 6. The average particle sizes of the AAP-NPs, PDI and electrical characteristic (ζ-potential) were found to be 150.27 ± 3.21 nm, 0.135 ± 0.012 and −31.10 ± 0.52 mV, respectively. Furthermore, Fourier transform infrared spectroscopy (FTIR) was used to determine the chemical structure of the AAP-NPs. It was observed that the intensity of AAP-NPs in the wide spectral band of 3000–3750 cm−1 was significantly stronger than that of the AAP, as was the characteristic peak of carboxyl anion, and the characteristic band moved to shorter wavelengths. Subsequent thermogravimetric analysis showed that the antisolvent precipitation method improved the thermal stability of the AAP, while scanning electron microscopy (SEM) and X-ray diffraction (XRD) showed that the morphology of AAP-NPs was uniform and well-distributed, and that their single crystal structures had remained unaffected during the process. Moreover, the DPPH and ABTS scavenging activities of AAP-NPs were increased, and the IC50 values were 0.544 ± 0.241 mg/mL and 0.755 ± 0.226 mg/mL, respectively. [ABSTRACT FROM AUTHOR]