Polymeric Compounds Research Articles

Thin Films of a Complex Polymer Compound for the Inhibition of Iron Alloy Corrosion in a H3PO4 Solution.

The etching of iron alloy items in a H3PO4 solution is used in various human activities (gas and oil production, metalworking, transport, utilities, etc.). The etching of iron alloys is associated with significant material losses due to their corrosion. It has been found that an efficient way to prevent the corrosion of iron alloys in a H3PO4 solution involves the formation of thin complex compound films consisting of the corrosion inhibitor molecules of a triazole derivative (TrzD) on their surface. It has been shown that the protection of iron alloys with a mixture of TrzD + KNCS in a H3PO4 solution is accompanied by the formation of a thin film of coordination polymer compounds thicker than 4 nm consisting of TrzD molecules, Fe2+ cations and NCS-. The layer of the complex compound immediately adjacent to the iron alloy surface is chemisorbed on it. The efficiency of this composition as an inhibitor of iron alloy corrosion and hydrogen bulk sorption by iron alloys is determined by its ability to form a coordination polymer compound layer, as experimentally confirmed by electrochemical, AFM and XPS data. The efficiency values of inhibitor compositions 5 mM TrzD + 0.5 mM KNCS and 5 mM TrzD + 0.5 mM KNCS + 200 mM C6H12N4 at a temperature of 20 ± 1 °C are 97% and 98%, respectively. The kinetic parameters of the limiting processes of hydrogen evolution and permeation into an iron alloy in a H3PO4 solution were determined. A significant decrease in both the reaction rate of hydrogen evolution and the rate of hydrogen permeation into the iron alloy by the TrzD and its mixtures in question was noted. The inhibitor compositions 5 mM TrzD + 0.5 mM KNCS and 5 mM TrzD + 0.5 mM KNCS + 200 mM C6H12N4 decreased the total hydrogen concentration in the iron alloy up to 9.3- and 11-fold, respectively. The preservation of the iron alloy plasticity in the corrosive environment containing the inhibitor under study was determined by a decrease in the hydrogen content in the alloy bulk.

Fabricating Effective and Recyclable Cadmium‐based Coordination Polymer for Selective Synthesis of 1,5‐Benzodiazepines

AbstractMetal coordination polymers are widely applied in the synthesis of heterocyclic compounds due to the advantages of highly dispersed metal active sites, low cost and strong designability. Herein, employing the 9‐benzyl‐3,6‐di(1H‐pyrazol‐1‐yl)‐9H‐carbazole (BPC) as a ligand, the cadmium‐coordinated polymer compound (Cd‐BPC) was facilely prepared by solvothermal method and characterized by energy dispersive spectrometer (EDS), flourier‐transform infrared spectroscopy (FT‐IR), scanning electron microscope (SEM), transmission electron microscopy (TEM) and X‐ray photoelectron spectrometry (XPS). Employing the Cd‐BPC polymer as a catalyst, 1,5‐benzodiazepine derivatives were produced with relatively high yields through the reaction of o‐phenylenediamine with ketones, and o‐phenylenediamine with alcohols. Additionally, Cd‐BPC could be reused for at least 5 times without significant decrease.

Recent Study of Separation and Identification of Micro- and Nanoplastics for Aquatic Products.

Micro- and nanoplastics (MNPs) are polymeric compounds widely used in industry and daily life. Although contamination of aquatic products with MNPs exists, most current research on MNPs focuses on environmental, ecological, and toxicological studies, with less on food safety. Currently, the extent to which aquatic products are affected depends primarily on the physical and chemical properties of the consumed MNPs and the content of MNPs. This review presents new findings on the occurrence of MNPs in aquatic products in light of their properties, carrier effects, chemical effects, seasonality, spatiality, and differences in their location within organisms. The latest studies have been summarized for separation and identification of MNPs for aquatic products as well as their physical and chemical properties in aquatic products using fish, bivalves, and crustaceans as models from a food safety perspective. Also, the shortcomings of safety studies are reviewed, and guidance is provided for future research directions. Finally, gaps in current knowledge on MNPs are also emphasized.

Anticorrosion and Supercapacitor Applications of Polypyrrole Coated Graphite Nanocomposites

The present investigation reports the successful incorporation of Graphite into the PPy matrix via a chemical in-situ polymerization technique. Obtained composites were thoroughly studied by using powder X-ray diffraction (PXRD), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FT-IR). The corrosion inhibition response of the composites on mild steel (MS), treated in acid media was analysed through atomic absorption spectroscopy (AAS), impedance, Tafel diagram (potentiodynamic polarization) and scanning electron microscopy (SEM) techniques. The results have revealed better inhibitory properties of these composites in the premeditated acid media. The Tafel and impedance curves revealed the dependency of polymer compounds on the corrosion protection of MS steel. The surface of MS is examined through the SEM technique (before and after corrosion). The synthesized materials were further studied for supercapacitor applications using electrochemical Cyclic Voltammetry (CV) and Galvanostatic Charging and Discharging studies (GCD) measurements. The supercapacitor and corrosion properties can be further optimized to develop effective PPy/G structures.

Saw marks in bone: A preliminary empirical study to inform decision making and best practice

Forensic toolmark examiners compare marks between those observed on an item/surface and those made by a reference implement, such as a particular tool or weapon, to provide an opinion of the likelihood of common origin. It is widely accepted that such comparison opinions need to be underpinned by empirical research, and this study aimed to add to the knowledge base relied upon when developing and comparing saw marks in bone, a substrate encountered in body dismemberment cases. Porcine bones were used as a human proxy; they were either fresh with residual soft tissue and bodily fluids present (‘wet’) to replicate dismembered bones shortly post-mortem, or processed to remove soft tissue and moisture content (‘dry’) to represent cases of dismemberment after an extended period of decomposition and exposure. The bones were cut using one implement of each of five classes: hand saw, mitre saw, reciprocating saw, oscillating saw, and serrated knife. They were cut, either completely through (except for serrated knife), giving two surfaces per cut to examine, or to a depth up to 3 mm (false starts). Five replicates per combination of bone condition, saw, and cut type gave 130 bone samples. These were then cleaned and cast using Isomark Silicone Polymer Compound or Mikrosil, giving 260 cast samples. All bone and cast samples were photographed, examined for various class characteristic markers, and specific markers measured. No significant differences between Isomark and Mikrosil casts were observed when compared side-by-side, demonstrating suitability of both materials for casting of saw marks on bone. Although saw marks presented more class characteristic markers on dry than wet bones, calculations of tooth distances and measurements of kerf width (KW) from marks did not significantly differ between bone conditions, with exception of the reciprocating saw that produced false start marks with significantly larger minimum KW on wet than dry samples. Further analysis supported that tooth distances on marks made by hand and oscillating saws are sufficiently accurate for the determination of saw teeth per inch (TPI). However, one tooth distance on marks made by reciprocating saws did not accurately represent TPI. Finally, examination of presence or absence of class characteristic markers on each saw mark demonstrated consistent variation between saw classes. These results enabled the development of exclusion-based decision trees, and a reference database (available on request), for use by toolmark examiners in their evaluation of saw types based on class characteristic markers observed in cut bone.

Functionalized Calixarenes as Promising Antibacterial Drugs to Face Antimicrobial Resistance.

Since the discovery of polyphenolic resins 150 years ago, the study of polymeric compounds named calix[n]arene has continued to progress, and those skilled in the art perfectly know now how to modulate this phenolic ring. Consequently, calix[n]arenes are now used in a large range of applications and notably in therapeutic fields. In particular, the calix[4]arene exhibits multiple possibilities for regioselective polyfunctionalization on both of its rims and offers researchers the possibility of precisely tuning the geometry of their structures. Thus, in the crucial research of new antibacterial active ingredients, the design of calixarenes finds its place perfectly. This review provides an overview of the work carried out in this aim towards the development of intrinsically active prodrogues or metallic calixarene complexes. Out of all the work of the community, there are some excellent activities emerging that could potentially place these original structures in a very good position for the development of new active ingredients.

Systematic Study of Vibrational Spectra of Octahedral Rhenium Clusters {Re6S8-xBrx}Bry (x = 0, 1, 2, 3, 4) with Mixed Sulfur/Bromine Inner Ligands

A series of rhenium compounds with the octahedral cluster core {Re6S8-xBrx} (x = 0–4): with molecular and polymeric structure were obtained. In these compounds the cluster core composition varies monotonically, the geometry of the cluster and the rhenium coordination polyhedron are retained unchanged, while the symmetry of the cluster changes. The vibrational spectra (Raman and IR) were recorded and analyzed for compounds with all possible S/Br ratios in the cluster core. The group vibrations of clusters were attributed with the use of DFT calculations of vibrational spectra. It is shown that the set of main characteristic bands is retained in both ionic and polymeric compounds regardless of the composition and the symmetry of the cluster core while the observed vibration frequencies of these bands depend on the S/Br ratio in the cluster core. In particular, the group Re–S stretching vibrations (A1g(S8) and T2g(S8) modes) shifted to higher frequencies with the increase in the number of Br atoms in the cluster. The difference in the connectivity in polymeric compounds leads to an increase in the number of bands in the spectra and to the disappearance of the A1g(Br) modes.

Photoluminous Response of Biocomposites Produced with Charcoal.

Due to the possible effects of global warming, new materials that do not have a negative impact on the environment are being studied. To serve a variety of industries and outdoor applications, it is necessary to consider the impact of photoluminosity on the performance of biocomposites in order to accurately assess their durability characteristics and prevent substantial damage. Exposure to photoluminosity can result in adverse effects such as discoloration, uneven surface, loss of mass, and manipulation of the intrinsic mechanical properties of biocomposites. This study aims to evaluate general charcoal from three pyrolysis temperatures to understand which charcoal is most suitable for photoluminosity and whether higher pyrolysis temperatures have any significant effect on photoluminosity. Porosity, morphology, Fourier transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy of charcoal were analyzed. Charcoal obtained at a temperature of 800 °C demonstrates remarkable potential as a bioreinforcement in polymeric matrices, attributable to its significantly higher porosity (81.08%) and hydrophobic properties. The biocomposites were characterized for flexural strength, tensile strength, scanning electron microscopy (SEM), FTIR, and x-ray diffraction (XRD). The results showed an improvement in tensile strength after exposure to photoluminosity, with an increase of 69.24%, 68.98%, and 54.38% at temperatures of 400, 600, and 800 °C, respectively, in relation to the treatment control. It is notorious that the tensile strength and modulus of elasticity after photoluminosity initially had a negative impact on mechanical strength, the incorporation of charcoal from higher pyrolysis temperatures showed a substantial increase in mechanical strength after exposure to photoluminosity, especially at 800 °C with breaking strength of 53.40 MPa, and modulus of elasticity of 4364.30 MPA. Scanning electron microscopy revealed an improvement in morphology, with a decrease in roughness at 800 °C, which led to greater adhesion to the polyester matrix. These findings indicate promising prospects for a new type of biocomposite, particularly in comparison with other polymeric compounds, especially in engineering applications that are subject to direct interactions with the weather.

New Ethynylphenylborasilsesquioxanes-Their Reactivity and Behavior during Thermal Decomposition.

In this paper, a new type of borasilsesquioxanes was synthesized through a condensation process, and its reactivity in catalytic hydrosilylation reactions with silanes, siloxanes, and silsesquioxanes was investigated. The obtained compounds were mostly obtained in >90% yield. They were fully characterized using spectroscopic (1H, 13C, 29Si NMR) and spectrometric (MALDI-TOF-MS) methods. The next stage of the research involved studying the thermogravimetric properties of the borasilsesquioxanes. By analyzing the different stages of decomposition using spectroscopic techniques (NMR, ATR-FTIR, Raman) and microscopic imaging, it was found that the structure of the borasilsesquioxanes changed during the pyrolysis process and polymer compounds were formed.

Acoustical properties of a 3D printed honeycomb structure filled with nanofillers: Experimental analysis and optimization for emerging applications

The novelty of this research lies in the successful fabrication of a 3D-printed honeycomb structure filled with nanofillers for acoustic properties, utilizing an impedance tube setup in accordance with ASTM standard E 1050-12. The Creality Ender-3, a 3D printer, was used for printing the honeycomb structures, and polylactic acid (PLA) material was employed for their construction. The organic, inorganic, and polymeric compounds within the composites were identified using fourier transformation infrared (FTIR) spectroscopy. The structure and homogeneity of the samples were examined using a field emission scanning electron microscope (FESEM). To determine the sound absorption coefficient of the 3D printed honeycomb structure, numerous samples were systematically developed using central composite design (CCD) and analysed using response surface methodology (RSM). The RSM mathematical model was established to predict the optimum values of each factor and noise reduction coefficient (NRC). The optimum values for an NRC of 0.377 were found to be 1.116 wt% carbon black, 1.025 wt% aluminium powder, and 3.151 mm distance between parallel edges. Overall, the results demonstrate that a 3D-printed honeycomb structure filled with nanofillers is an excellent material that can be utilized in various fields, including defence and aviation, where lightweight and acoustic properties are of great importance.

Polyphenols in Plants: Structure, Biosynthesis, Abiotic Stress Regulation, and Practical Applications (Review).

Phenolic compounds or polyphenols are among the most common compounds of secondary metabolism in plants. Their biosynthesis is characteristic of all plant cells and is carried out with the participation of the shikimate and acetate-malonate pathways. In this case, polyphenols of various structures are formed, such as phenylpropanoids, flavonoids, and various oligomeric and polymeric compounds of phenolic nature. Their number already exceeds 10,000. The diversity of phenolics affects their biological activity and functional role. Most of their representatives are characterized by interaction with reactive oxygen species, which manifests itself not only in plants but also in the human body, where they enter through food chains. Having a high biological activity, phenolic compounds are successfully used as medicines and nutritional supplements for the health of the population. The accumulation and biosynthesis of polyphenols in plants depend on many factors, including physiological-biochemical, molecular-genetic, and environmental factors. In the review, we present the latest literature data on the structure of various classes of phenolic compounds, their antioxidant activity, and their biosynthesis, including their molecular genetic aspects (genes and transfactors). Since plants grow with significant environmental changes on the planet, their response to the action of abiotic factors (light, UV radiation, temperature, and heavy metals) at the level of accumulation and composition of these secondary metabolites, as well as their metabolic regulation, is considered. Information is given about plant polyphenols as important and necessary components of functional nutrition and pharmaceutically valuable substances for the health of the population. Proposals on promising areas of research and development in the field of plant polyphenols are presented.

The Role of Chemically Innocent Polyanions in Active, Chemically Fueled Complex Coacervate Droplets.

Complex coacervation describes the liquid-liquid phase separation of oppositely charged polymers. Active coacervates are droplets in which one of the electrolyte's affinity is regulated by chemical reactions. These droplets are particularly interesting because they are tightly regulated by reaction kinetics. For example, they serve as a model for membraneless organelles that are also often regulated by biochemical transformations such as post-translational modifications. They are also a great protocell model or could be used to synthesize life-they spontaneously emerge in response to reagents, compete, and decay when all nutrients have been consumed. However, the role of the unreactive building blocks, e.g., the polymeric compounds, is poorly understood. Here, we show the important role of the chemically innocent, unreactive polyanion of our chemically fueled coacervation droplets. We show that the polyanion drastically influences the resulting droplets' life cycle without influencing the chemical reaction cycle-either they are very dynamic or have a delayed dissolution. Additionally, we derive a mechanistic understanding of our observations and show how additives and rational polymer design help to create the desired coacervate emulsion life cycles.

Die Rolle von unreaktiven Polyanionen in aktiven, chemisch regulierten komplexen Koazervaten

AbstractKomplexe Koazervation beschreibt die Flüssig‐Flüssig‐Phasentrennung entgegengesetzt geladener Polymere. Aktive Koazervate sind Tröpfchen, in denen die Affinität eines der Elektrolyte durch chemische Reaktionen gesteuert wird. Diese Tröpfchen sind besonders interessant, weil ihre Eigenschaften durch die Reaktionskinetik streng reguliert werden. Sie dienen beispielsweise als Modell für membranlose Organellen, die häufig auch durch biochemische Transformationen, wie z. B. posttranslationale Modifikationen, gesteuert werden. Sie sind auch ein gutes Modell für Protozellen oder könnten zur Synthese von künstlichem Leben verwendet werden – sie entstehen spontan als Reaktion auf Reagenzien, konkurrieren und zerfallen, sobald alle Nährstoffe verbraucht sind. Allerdings ist die Rolle der unreaktiven Bausteine, z. B. der Polymere, bisher kaum verstanden. Mit unserer Arbeit zeigen wir die wichtige Rolle des unreaktiven Polyanions unserer chemisch betriebenen Koazervattropfen. Wir zeigen, dass das Polyanion den Lebenszyklus der resultierenden Tröpfchen drastisch beeinflusst, ohne den chemischen Reaktionszyklus selbst zu beeinflussen – entweder sind sie sehr dynamisch oder lösen sich nur verzögert auf. Darüber hinaus leiten wir den Mechanismus dahinter ab und zeigen, wie Additive und rationales Polymerdesign dazu beitragen können, die gewünschten Lebenszyklen von Koazervatemulsionen zu erzeugen.

Tubular PEM electrolysis cells with a 3D-printed oxygen electrode and ALD catalyst coating

Polymer electrolyte membrane electrolysis (PEMEL) is a technology with a major role in linking the hydrogen production to renewable energy resources with a volatile behaviour such as wind and solar. High amounts of precious metals and a labour intensive production also make it a cost intensive technology. A tubular cell design has the potential to reduce production costs by co-extrusion of cells which feature a reduced sealing length. For the inner half cell, additive manufacturing (AM) of titanium offers a high degree of freedom for the electrode design to reach a high electric conductivity and active surface area. In combination with atomic layer deposition (ALD) of iridium catalyst a porous transport electrode (PTE) can be fabricated. Using planar test cell results and model based PTE design, this study demonstrates the feasibility of a tubular PEMEL cell consisting of an additively manufactured, iridium coated anode PTE in the inner half cell, an extruded membrane and a platinum coated graphite felt cathode PTE in the outer half cell. The outer titanium current collector can be replaced by an extruded graphite polymer compound current collector to reduce the amount of titanium without performance losses. The cell is operated at 60 °C in 1 mol L−1 sulphuric acid and experimentally characterized by polarization curves and electrochemical impedance spectroscopy (EIS). At 2.0 V cell potential a current density of ≈450mAcm−2 was reached corresponding to an iridium mass specific current density >1500Ag−1 which is significant larger than literature values.

Multifactorial Assessment of the Bioenergetic Potential of Residual Biomass of Pinus spp. in a Rural Community: From Functional Characterization to Mapping of the Available Energy Resource

The generation of biomass residues in different productive activities of rural communities in Mexico represents an area of opportunity for the generation of bioenergy for various purposes. Solid biofuels (SBF), for example, are an alternative for the exploitation of these residues. The present study shows a comprehensive proposal for the analysis of residues of Pinus spp. generated by the artisanal sector of a rural community in Mexico. The proposal is based on four stages: a) characterization of the physico-chemical and functional properties of the residues, by Scanning Electron Microscopy (SEM), Infrared (FTIR) and Raman Spectroscopy, Thermogravimetry (TGA-DTG), determining the calorific coefficient and polymeric compounds present by fiber analysis; (b) spatial, temporal and dimensional analysis of the waste generated in the town studied; (c) assessment of the energy potential available in space and time; (d) definition of guidelines for the management of solid biofuels for the community through collection, processing and final disposal centers. The results of the assessment of timber residue from 50 artisan workshops that represent 25% of the total in the community show that the identified heating value of the dry residue ranges from 17.6 MJ/kg to 18.1 MJ/kg, attributed to the presence of polymeric compounds such as cellulose, hemicellulose and lignin, the latter in the order of 28%, which contributes to a high energy potential, and whose compounds were identified by TGA-DTG analysis, FTIR, SEM and fiber analysis. The energy potential was estimated at approximately 7 TJ/year for the analyzed workshops. In which case, the economic savings obtained from unburned firewood would amount to about $20,000 USD/year. As regards the reduction in firewood consumption due to the use of residues for energy purposes, about 350 Tn/year would be mitigated, which would reduce the community’s emissions by more than 76 TnCO2/year. A strategic management proposal was also established, aimed at providing spaces for the collection, processing and final disposal of solid biofuels from wood residues, which in sum represent an energy alternative that is sustainable in environmental, economic and social terms, for the same community.

Structural evolution, synthesis mechanism and thermal conductivity of (La0.2Nd0.2Sm0.2Gd0.2Yb0.2)2Zr2O7 high-entropy ceramic prepared by concurrent chemical coprecipitation method

(La0.2Nd0.2Sm0.2Gd0.2Yb0.2)2Zr2O7 (Ln2Zr2O7) ceramic powders with nanoscale were synthesized by concurrent chemical coprecipitation method. The thermal behaviors and structural evolution of Ln2Zr2O7 precursor were investigated. The synthesis mechanism and thermal conductivity of Ln2Zr2O7 ceramic were also discussed in detail. Results show that a kind of complex polymeric compound containing -[Zr–OH–Zr]- and -[Zr–OH-Ln]- network structure was formed in the as-synthesized Ln2Zr2O7 precursor, which directly transformed to Ln2Zr2O7 crystals through dehydroxylation and structural ordering during the calcination process. The bulk Ln2Zr2O7 ceramics have a lower thermal conductivity of 1.20–1.47 W/(m·K), which can be attributed to the high-entropy effect resulting from the introduction of multiple rare earth elements.

Synthesis of a novel Cu/DPA-MOF/OP/CS hydrogel with high capability in antimicrobial studies.

Today, with the indiscriminate use of antibiotics, we face the resistance of some bacterial strains against some antibiotics. Therefore, it is essential to report and synthesize new compounds with antimicrobial properties. A novel copper/dipicolinic acid-metal-organic framework cross-linked oxidized pectin and chitosan (Cu/DPA-MOF/OP/CS) hydrogel polymer was synthesized under environmental conditions with the controllable process, which uses biodegradable polymer compounds such as pectin and chitosan in its structure. The efficient physicochemical features of the synthesized Cu/DPA-MOF/OP/CS hydrogel using SEM, FT-IR, TGA, BET, XRD, and EDS/mapping were identified and confirmed. The newly synthesized Cu/DPA-MOF/OP/CS hydrogel showed activity against Gram-positive and Gram-negative bacterial strains and fungal species, and significant antibacterial and antifungal properties were observed. In antibacterial activity, the MIC against Gram-positive species was in the range of 16-128mg/mL, the MIC against Gram-negative species was in the range of 64-256mg/mL, and the MIC against fungal species was in the range of 128-512mg/mL. In antimicrobial evaluations, in addition to the MIC test, the MBC test, the MFC test, and the IZD test were performed, and the results were reported. The results were compared with commercial antibiotics in the market. Development of novel nanostructures based on hydrogel polymers with distinctive functionality can affect the performance of these nanostructures in different areas.

Tandem Suzuki Polymerization/Heck Cyclization Reaction to Form Ladder-Type 9,9'-Bifluorenylidene-Based Conjugated Polymer.

The synthesis of ladder-type 9,9'-bifluorenylidene-based conjugated polymer is reported. Unlike the typical synthetic strategy, the new designed ladder-type conjugated polymer is achieved via tandem Suzuki polymerization/Heck cyclization reaction in one-pot. In the preparation process, Suzuki polymerization reaction occurred first and then the intramolecular Heck cyclization followed smoothly under the same catalyst Pd(PPh3)4. The model reaction proved that the introduction of iodine (I) for this tandem reaction can effectively control the sequential bond-forming process and inhibit the additional competitive side reactions. Thus, small-molecule model compounds could be obtained in high yields. The successes of the synthesized small molecule and polymer compounds indicate that the Pd-catalyzed tandem reaction may be an effective strategy for improving extended π-conjugated materials.

Syntheses and Characterization of Main Group, Transition Metal, Lanthanide, and Actinide Complexes of Bidentate Acylpyrazolone Ligands.

The synthesis of acylpyrazolone salts and their complexes of main group elements, transition metals, lanthanides, and actinides are described and characterized inter alia by means of single-crystal X-ray crystallography, NMR, and IR spectroscopies. The complexes consist of two, three, or four acylprazolone ligands bound to the metal atom, resulting in a structurally diverse set of coordination complexes with (distorted) octahedral, pentagonal-bipyramidal, or antiprismatic arrangements. Several complexes proved to be polymeric in the solid state including heterobimetallic sodium/lanthanide coordination polymers. A selection of the polymeric compounds was analyzed via TG/DTA measurements to establish their stability. The ligands, in turn, were readily synthesized in good yields from commercially available hydrazine hydrochloride salts. These findings demonstrate that acylpyrazolone ligands can form complexes with metals of varying ionic radii, highlighted by their utility in other areas such as analytical and metal organic framework chemistry.

Study of the Influence of the Excipients Used for the Synthesis of Microspheres Loaded with Quercetin: Their Characterization and Antimicrobial Activity

The aim of this study was to determine the potential pharmaceutical applications of quercetin—a natural flavonoid compound with a polyphenolic structure—following its encapsulation in polymeric microspheres resistant to degradation. The microspheres were prepared from natural polymeric compounds (chitosan and sodium alginate) via a complex coacervation method, with the goal of protecting quercetin from the degradation reactions that can affect its bioactivity. After the microspheres were prepared, they were characterized using various analytical methods. The encapsulation efficiency (EE (%)), swelling index (idxSWL%), roughness (measured using confocal laser scanning microscopy—CLSM), and surface morphology (measured using scanning electron microscopy—SEM) were all analyzed. In addition, the release capacity of quercetin from the microspheres (mQrel%) and the antimicrobial activity of the microspheres were evaluated in vitro. Finally, a multivariate statistical analysis (MANOVA, p = 0.05, PCA, and AHC) was conducted. This analysis showed that chitosan–sodium alginate–quercetin microspheres (CAQ-Ms) entrap 86.91 ± 1.10–93.11 ± 0.72% quercetin; in vitro, 71.46 ± 0.25–91.06 ± 0.15% quercetin was released, and the swelling index was higher (6701.29 ± 0.39–10,009.30 ± 1.11%) in the phosphate-buffered solution with a pH of 7.4. The CLSM and SEM analyses showed that the polymer concentration in CAQ-Ms was increased, and the roughness and smoothness of the microspheres were also increased. SEM also showed that the external layer of CAQ-Ms was formed from chitosan and the internal layer was formed from sodium alginate. Antimicrobial tests showed that CAQ-Ms had antibacterial and antifungal effects on the analyzed strains and produced larger inhibition zones between 15.3 and 14.4 mm on Escherichia coli and between 13.3 and 14.2 mm on Candida albicans, and smaller inhibition zones, between 12.4 and 13.6 mm, on Staphylococcus aureus. According to the obtained results, after the multivariate statistical analysis, it can be observed that the best performance was presented by samples P1, P2, and P3. In conclusion, the method used for the formulation of CAQ-Ms was efficient because it enabled an increase in the solubility of quercetin in water and its protection against external and internal degradation in the gastrointestinal tract. This system can be further used to produce new pills for oral administration that are able to reach the small intestine, where they can then release loaded active drugs.