Rapid Synthesis and Evaluation of Resveratrol-Piperazine Cocrystals by Ultrasound and Microwave Methods.

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.

Mechanochemical Synthesis of Resveratrol-Piperazine Cocrystals.

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.

Coinage Metals Doped ZnO Obtained by Sol-Gel Method-A Brief Review.

ZnO is one of the most studied oxides due to its nontoxic nature and remarkable properties. It has antibacterial and UV-protection properties, high thermal conductivity, and high refractive index. Various ways have been used to synthesize and fabricate coinage metals doped ZnO, but the sol-gel technique has received a lot of interest because of its safety, low cost, and facile deposition equipment. Coinage metals are represented by the three nonradioactive elements of group 11 of the periodic table: gold, silver, and copper. This paper, which was motivated by the lack of reviews on the topic, provides a summary of the synthesis of Cu, Ag, and Au-doped ZnO nanostructures with an emphasis on the sol-gel process and identifies the numerous factors that affect the morphological, structural, optical, electrical, and magnetic properties of the produced materials. This is accomplished by tabulating and discussing a summary of a number of parameters and applications that were published in the existing literature over the previous five years (2017-2022). The main applications being pursued involve biomaterials, photocatalysts, energy storage materials, and microelectronics. This review ought to serve as a helpful reference point for researchers looking into the many physicochemical characteristics of coinage metals doped ZnO, as well as how these characteristics vary according to the conditions under which experiments are conducted.