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OBJECTIVE: Resveratrol-piperazine cocrystals have been obtained by ultrasound (US) and microwave-assisted (MW) techniques, using the solution and slurry-based methods, to study the influence of the synthesis method on the resulting cocrystal properties, and scalability of the processes. The potential of these cocrystals is represented by the unique properties of their components, resveratrol, and piperazine, which could be also used in veterinary practice. Resveratrol has antimicrobial, antiviral and anticarcinogenic properties, while piperazine can be used in the treatment of parasitic infections. METHODS: The influence of ultrasound and microwave-assisted treatment was studied by varying synthesis parameters such as reaction time, temperature, and US or MW power. The main advantage of using these methods is represented by shorter synthesis time compared to conventional methods, resulting in the direct formation of the cocrystals. RESULTS: All samples were obtained in high purity, above 97%. Cocrystal yield correlated positively with ultrasound reaction time, while temperature was not found to influence the microwave synthesis yield up to 50°C, in the case of solution-based methods. MW and US-assisted solution-based methods lead to yields between 52.9 and 68.1%. In the case of the slurry-based method, a minimum reaction time of 5 min leads to the formation of cocrystals with high purity. The resveratrol-piperazine cocrystal's solubility and in vitro antibacterial activity were also evaluated, showing promising results. CONCLUSIONS: Ultrasound and microwave-assisted techniques offer a viable alternative for synthesizing resveratrol-piperazine cocrystals with short reaction times, high yield, and purity, suitable for scalable resveratrol-piperazine cocrystals.

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The 1:1 resveratrol-piperazine cocrystal was successfully synthesized and scaled-up to 300 g scale with the mechanochemical method, as a result of investigating key process parameters, namely the solvent and the grinding time. The use of water, ethanol or ethanol-water mixtures and reaction times up to 50 min were evaluated relative to the dry grinding process. Cocrystal formation and purity were monitored through X-ray diffraction and calorimetry measurements. The dry grinding resulted in an incomplete cocrystal formation, while the use of water or water-ethanol mixture yielded a monohydrate solid phase. Pure ethanol was found to be the optimal solvent for large-scale cocrystallization, as it delivered cocrystals with high crystallinity and purity after 10-30 min grinding time at the laboratory scale. Notably, a relatively fast reaction time (30-60 min) was sufficient for the completion of cocrystallization at larger scales, using a planetary ball mill and a plant reactor. Also, the obtained cocrystal increases the aqueous solubility of resveratrol by 6%-16% at pH = 6.8. Overall, this study highlights the potential of solvent-assisted mechanochemical synthesis as a promising new approach for the efficient production of pure resveratrol-piperazine cocrystals.

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(1) Background: Oxidative stress plays a pivotal role in the pathogenesis of various diseases, including neurodegenerative disorders, cardiovascular diseases, cancer, and diabetes, highlighting the pressing need for effective antioxidant interventions. (2) Methods: In this study, we aimed to develop and characterise two novel antioxidant formulations, F3 and F4, as therapeutic interventions for oxidative stress-related conditions. (3) Results: The physicochemical characterisation, preformulation analysis, formulation, preparation of filling powders for capsules, capsule content evaluation, and antioxidant activity assessment of the two novel antioxidant formulations were assessed. These formulations comprise a combination of well-established antioxidants like quercetin, biotin, coenzyme Q10, and resveratrol. Through comprehensive testing, the formulations' antioxidant efficacy, stability, and potential synergistic interactions were evaluated. (4) Conclusions: The findings underscore the promising potential of these formulations as therapeutic interventions for oxidative stress-related disorders and highlight the significance of antioxidant interventions in mitigating their progression.

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The removal of pharmaceutical contaminants from wastewater has gained considerable attention in recent years, particularly in the advancements of hydrogel-based adsorbents as a green solution for their ease of use, ease of modification, biodegradability, non-toxicity, environmental friendliness, and cost-effectiveness. This study focuses on the design of an efficient adsorbent hydrogel based on 1% chitosan, 40% polyethylene glycol 4000 (PEG4000), and 4% xanthan gum (referred to as CPX) for the removal of diclofenac sodium (DCF) from water. The interaction between positively charged chitosan and negatively charged xanthan gum and PEG4000 leads to strengthening of the hydrogel structure. The obtained CPX hydrogel, prepared by a green, simple, easy, low-cost, and ecological method, has a higher viscosity due to the three-dimensional polymer network and mechanical stability. The physical, chemical, rheological, and pharmacotechnical parameters of the synthesized hydrogel were determined. Swelling analysis demonstrated that the new synthetized hydrogel is not pH-dependent. The obtained adsorbent hydrogel reached the adsorption capacity (172.41 mg/g) at the highest adsorbent amount (200 mg) after 350 min. In addition, the adsorption kinetics were calculated using a pseudo first-order model and Langmuir and Freundlich isotherm parameters. The results demonstrate that CPX hydrogel can be used as an efficient option to remove DCF as a pharmaceutical contaminant from wastewater.

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The present research focuses on the physicochemical and pharmacotechnical properties of new hydrogels obtained using allantoin, xanthan gum, salicylic acid and different concentrations of Aloe vera (5, 10, 20% w/v in solution; 38, 56, 71 wt% in dry gels). The thermal behavior of Aloe vera composite hydrogels was studied using DSC and TG/DTG analyses. The chemical structure was investigated using different characterization methods (XRD, FTIR and Raman spectroscopies) and the morphology of the hydrogels was studied SEM and AFM microscopy. Pharmacotechnical evaluation on tensile strength and elongation, moisture content, swelling and spreadability was also completed. Physical evaluation confirmed that the appearance of the prepared Aloe vera based hydrogels was homogeneous and the color varied from pale beige to deep opaque beige with increasing Aloe vera concentration. All other evaluation parameters, e.g., pH, viscosity, spreadability and consistency were found to be adequate in all hydrogel formulations. SEM and AFM images show that the structure of the hydrogels condensed into homogeneous polymeric solids with the addition of Aloe vera, in accordance with the decrease in peak intensities observed via XRD analysis. These results suggest interactions between the hydrogel matrix and Aloe vera as observed via FTIR and TG/DTG and DSC analyses. Considering that Aloe vera content higher than 10% (w/v) did not stimulate further interactions, this formulation (FA-10) can be used for further biomedical applications.

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In this paper, we conducted a fundamental study concerning the effect of thermal treatment on the structure and morphology of 2 mol% vanadium doped ZnO nanopowders obtained by microwave assisted sol-gel method (MW). The samples were analyzed by DTA, FTIR, XRD, SEM, and UV-Vis spectroscopy. The DTA results showed that above 500 °C, there was no mass loss in the TG curves, and ZnO crystallization occurred. The XRD patterns of the thermally treated powders at 500 °C and 650 °C showed the crystallization of ZnO (zincite) belonging to the wurtzite-type structure. It was found that in the 650 °C thermally treated powder, aside from ZnO, traces of Zn3(VO4)2 existed. FTIR spectra of the annealed samples confirmed the formation of the ZnO crystalline phase and V-O bands. The micrographs revealed that the temperature influenced the morphology. The increase in the annealing temperature led to the grain growth. The SEM images of the MW powder thermally treated at 650 °C showed two types of grains: hexagonal grains and cylindrical nanorods. UV-Vis spectra showed that the absorption band also increased with the increasing temperature of thermal treatment. The MW sample annealed at 650 °C had the highest absorption in ultraviolet domain.

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A facile, green synthesis methodology to obtain zinc oxide nanoparticles using three polysaccharide gums (Acacia gum, Guar gum and Xanthan gum) of biological origin was developed. Subsequently, biosynthesized zinc oxide nanoparticles were incorporated into a sustainable chitosan hydrogel matrix functionalized with propolis extract. This study has revealed that the selected polysaccharides as chelates represents a suitable approach to synthesize ZnO nanoparticles of particular interest with controlled morphology. The formation of ZnO nanoparticles using polysaccharide gums was confirmed by FTIR, XRD, UV-Vis spectroscopy, thermal analysis, SEM, Raman and photoluminescence spectroscopies. The rheological behaviour of obtained hydrogels was evaluated. The AFM studies demonstrate that all synthesized chitosan incorporated ZnO composites hydrogels functionalized with propolis extract exhibit corrugated topographies. The present study highlights the possible incorporation of various guest molecules into hydrogel matrix due to its tuneable morphologies. The obtained hydrogel composites were cytocompatible in L929 fibroblast cell culture, in a range of concentrations between 50 and 1000 µg/mL, as assessed by MTT, LDH and Live/Dead double staining assays. By enhancing the biological properties, these novel green hydrogels show attractive superior performance in a wide concentration range to develop future in vivo suitable natural platforms as effective delivery systems of pharmacologic agents for biomedical applications.

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Nowadays, the use of marine by-products as precursor materials has gained great interest in the extraction and production of chemical compounds with suitable properties and possible pharmaceutical applications. The present paper presents the development of a new immediate release tablet containing calcium lactate obtained from Black Sea mussel shells. Compared with other calcium salts, calcium lactate has good solubility and bioavailability. In the pharmaceutical preparations, calcium lactate was extensively utilized as a calcium source for preventing and treating calcium deficiencies. The physical and chemical characteristics of synthesized calcium lactate were evaluated using Fourier Transform Infrared Spectroscopy, X-ray diffraction analysis and thermal analysis. Further, the various pharmacotechnical properties of the calcium lactate obtained from mussel shells were determined in comparison with an industrial used direct compressible Calcium lactate DC (PURACAL®). The obtained results suggest that mussel shell by-products are suitable for the development of chemical compounds with potential applications in the pharmaceutical domain.

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The present study describes for the first time the synthesis of silica nanoparticles starting from sodium silicate and oleic acid (OLA). The interactions between OLA and sodium silicate require an optimal OLA/OLANa molar ratio able to generate vesicles that can stabilize silica particles obtained by the sol-gel process of sodium silicate. The optimal molar ratio of OLA/OLANa can be ensured by a proper selection of OLA and respectively of sodium silicate concentration. The titration of sodium silicate with OLA revealed a stabilization phenomenon of silica/OLA vesicles and the dependence between their average size and reagent's molar ratio. Dynamic light scattering (DLS) and scanning electron microscopy (SEM) measurements emphasized the successful synthesis of silica nanoparticles starting from renewable materials, in mild condition of green chemistry. By grafting octadecyltrimethoxysilane on the initial silica particles, an increased interaction between silica particles and the OLA/OLANa complex was achieved. This interaction between the oleyl and octadecyl chains resulted in the formation of stable gel-like aqueous systems. Subsequently, olive oil and an oleophylic red dye were solubilized in these stable aqueous systems. This great dispersing capacity of oleosoluble compounds opens new perspectives for future green chemistry applications. After the removal of water and of the organic chains by thermal treatment, mesoporous silica was obtained.