The present technology describes the process of obtaining a material containing nanostructured reactive molecules based on niobium compounds, the products obtained and their use as a chemical/biological barrier on surfaces. The nanostructured hybrid material can be used as a component of cosmetic products, intensifying its effectiveness and time of action. In addition, it can be incorporated into different surfaces, including fabrics, maintaining its action against bacteria and viruses. It can also be applied in the form of a gel or liquid spray. Niobium nanoparticles combined with quaternary ammonium compounds for sprays and with methylene blue dye to form sanitizing gels showed high efficiency in deactivating the coronavirus, with stability and prolonged activity.
Brazil holds more than 90% of the world's exploitable reserves of niobium and is still its largest producer and exporter. In this way, the development of new products for use in different industrial sectors can become a topic of strategic importance for the development, not only of the state of Minas Gerais, but also for the country. This development may mean a technological increase in the products generated from Brazilian ore, implying an increase in added value and the consequent generation of jobs in the country.
In the context of technology development, it is observed that niobium-based systems have played an important role in several reactions, being able to act as an active phase, dopant and also as a reactional support. Special characteristics, such as redox property, photosensitivity, high acidity and strong metal-support interaction have made these systems, especially oxyhydroxide, niobium oxide, phosphate and pentoxide, present high performance in the most varied types of reaction. In order to increase its activity, many studies report the modification of Nb2O5 with phosphoric acid, resulting in niobium phosphate. In some cases, NbCl5 is also used as a precursor. The scientific literature also reports several studies highlighting the use of niobium compounds in oxidation reactions, including organic pollutants present in industrial effluents or in glycerol cleavage reactions.
Quaternary ammonium compounds, such as hexadecyltrimethylammonium bromide (CTAB), are membrane active agents, that is, the predominant sites of action are the cytoplasmic membrane in bacteria or the plasma membrane in yeast. Surface active agents or surfactants have two regions in their molecular structure: a hydrophobic (supporting) group and a hydrophilic (polar) group. Cationic agents, such as quaternary ammonium compounds, are the most useful antiseptics and disinfectants, and are also known as cationic surfactants. CTAB serves as an important surfactant in the DNA extraction buffer system to remove membrane lipids and promote cell lysis. CTAB has been shown to have potential use as an anticancer agent, promoting apoptosis of tumor cells from head and neck cancers (Emma Ito, Kenneth W. Yip, David Katz, Sonali B. Fonseca, David W. Hedley, Sue Chow, G. WeiXu, Tabitha E. Wood, Carlo Bastianutto, Aaron D. Schimmer, Shana O. Kelley, Fei-Fei Liu. Potential Use of Cetrimonium Bromide as an Apoptosis-Promoting Anticancer Agent for Head and Neck Cancer. Molecular Pharmacology, 76, 2009, 969-983).
Quaternary ammonium salts have known antibacterial properties and their hydrophobic carbon chain can deactivate viruses by reacting with their lipid barrier, with activity already demonstrated in the deactivation of the coronavirus (Franklin Dexter, FASA, Michelle C. Parra, Jeremiah R. Brown, Randy W. Loftus. Perioperative COVID-19 Defense: An Evidence-Based Approach for Optimization of Infection Control and Operating Room Management, Anesthesia & Analgesia, 2020) (Nancy Baker, Antony J. Williams, Alexander Tropsha, Sean Ekins. Repurposing Quaternary Ammonium Compounds as Potential Treatments for COVID-19, Pharm Res, 37, 2020, 104) (Maria L. S. O. Lima, Ramon K. S. Almeida, Francine S. A. da Fonseca, Caroline C. S Gonçalves. A química dos saneantes em tempos de COVID-19. Você sabe como funciona? Quim. Nova, 43, 2020, 668-678).
Patent document U.S. Pat. No. 8,337,872, entitled “Method of inhibiting the transmission of influenza virus”, from 2006, relates to the method of inhibiting the transmission of the influenza virus. Antimicrobial compositions with rapid and persistent antiviral efficacy against influenza viruses, including avian influenza viruses, are disclosed. Antimicrobial compositions contain a disinfectant alcohol, an organic acid and water, wherein the composition has a pH of about 5 or less and the non-volatile components of the composition are capable of forming a barrier film or layer on a treated surface.
U.S. Pat. No. 9,549,949, from 2008, entitled “Antiviral agent” describes an antiviral agent that contains as an active ingredient a particle of at least one type of iodide composed of iodine and an element shown in Period 4 to Period 6 and Group 8 to Group 15 of the periodic table or at least one type of monovalent copper compound. The antiviral agent can be incorporated into a variety of products. Although niobium is in group 5 of the periodic table, this document presents iodide or iodine compounds in its composition, not referring to quaternary ammonium salts.
The present technology describes a product with a combined action between niobium compounds and quaternary ammonium salts to act as a chemical/biological barrier on surfaces. The material can be used in products in the form of a liquid to protect surfaces, being efficient in deactivating the coronavirus in an intensified way. The mechanism of action of the nanostructured hybrid material proposed in the present technology consists of chemically combining a niobium compound with a high negative charge that accumulates around it several groups of quaternary ammonium salts, promoting an intensification of its action in the deactivation, for example, of the coronavirus. This is because the compound formed by the chemical bond established between niobium and the quaternary ammonium salt concentrates the hydrophobic groups responsible for deactivating the virus, creating a protective layer on the surface on which it was deposited. The synergistic effect between the niobium compound and the CTAB obtained in the present technology was evident with the results of the coronavirus deactivation studies, where the species separately were much less efficient than the nanostructured hybrid material containing Nb-CTAB.
The present technology also describes the product formed by the combination between the nanostructured hybrid material based on niobium and the methylene blue dye, in the form of a gel, obtained by incorporation in alcohol in commercial gel, which showed an excellent performance in reducing the viral charge. The antiviral effect of the product occurs due to the semiconductor property of the niobium compound, which has the ability to act via photocatalytic effect. This makes it possible to use only 0.5% of the Nb-CTAB gel in combination with commercial alcohol gel to act very efficiently in the deactivation of the coronavirus. The reduction in viral load observed was much greater when compared to pure alcohol gel. In addition, the new molecule Nb-methylene blue remains active, even after evaporation of commercial alcohol, providing prolonged action to the proposed product.
The products of this technology have the potential to be used as chemical/biological barriers due to their incorporation into different surfaces. The hybrid material containing the combination of an inorganic material (niobium) and an organic material (CTAB and/or dye) with structural dimensions of nanostructures can be used as a component of cosmetic products, intensifying their effectiveness and time of action. In addition, it can be incorporated into different fabric surfaces, maintaining its action against bacteria and viruses. In addition, it can be incorporated into different fabric surfaces, maintaining its action against bacteria and viruses. It can also be applied in the form of a gel or liquid spray, presenting a synergistic effect with other sanitizing products, such as alcohol and disinfectants, among others.
The present technology describes the process of obtaining a material containing nanostructured reactive molecules based on niobium compounds, the products obtained and their use as a chemical/biological barrier on surfaces. The nanostructured hybrid material can be used as a component of cosmetic products, intensifying its effectiveness and time of action. In addition, it can be incorporated into different surfaces, including fabrics, maintaining its action against bacteria and viruses. It can also be applied in the form of a gel or liquid spray. Niobium nanoparticles combined with quaternary ammonium compounds for sprays and with methylene blue dye to form sanitizing gels showed high efficiency in deactivating the coronavirus, with stability and prolonged activity.
The niobium oligomer-based nanostructured hybrid material contains negatively charged niobium oligomers and organic cations selected from the group comprising quaternary ammonium salts of the didecyldimethylammonium chloride type, hexadecyltrimethylammonium bromide (CTAB), methylene blue, gentian violet and/or fuchsine dye, at concentrations of 10 to 2000 mg/L of quaternary ammonium for concentrations between 100 and 3000 mg/L of niobium.
Negatively charged niobium oligomers can be obtained from niobium oxides, niobium pentoxide, niobic acid and niobium phosphate.
The nanostructured hybrid material based on niobium oligomers can be incorporated into alcohol gel between 10 and 70% m/m, in proportions of 0.1 to 10% by mass of the niobium compound.
The process for obtaining the nanostructured hybrid material based on niobium oligomers comprises the following steps:
a. Dissolving the niobium compounds, containing between 1 and 5 g/L of niobium, in oxalic acid or hydrogen peroxide, in concentrations between 10 and 50% m/m;
The niobium compounds described in step “a” are selected from the group comprising their oxides, being niobium oxides, niobium pentoxide, niobic acid and niobium phosphate.
The quaternary ammonium, described in step “b”, is selected from the group comprising didecyldimethylammonium chloride or hexadecyltrimethylammonium bromide (CTAB) and the cationic dye is selected from the group comprising methylene blue, gentian violet or fuchsine dye, which may be added 0.1 to 5% m/m of alcohol gel 10 to 70% m/m after step “c”.
The nanostructured hybrid material based on niobium oligomer can be used in the production of sanitizing compounds, with bactericidal and antiviral activities, preferably against coronaviruses.
The following examples describe aspects of the present technology and should not be considered as limiting.
The compounds in spray form are obtained by the reaction of the niobium oligomer containing 2,000 mg/L of niobium with the quaternary ammonium (CTAB) 100 mg/L. CTAB is dripped into the oligomer solution until the formation of a micelle containing niobium and CTAB chemically bonded to form Nb-CTAB. It is important to point out that the micellar point is obtained before the solution gelling, so that agitation must be observed and the medium gelling should be avoided. The resulting micelle should be kept under gentle agitation at 100 rpm for 10 min.
The sanitizing gel was obtained from the reaction of the methylene blue dye and the niobium compound using equal volumes of the compounds, the dye concentration being 1000 mg/L and the niobium compound concentration of 2,000 mg/L. This material has good sanitizing properties, especially when associated with alcohol gel 70% m/m. In the mixture with alcohol gel 70% m/m, a ratio of 0.5% by mass of the sanitizing gel formed by Nb-methylene blue was prepared.
Strong evidence of the chemical interaction established between the negatively charged species of niobium and CTAB was obtained by RAMAN spectroscopy, where the shifts referring to the established chemical interactions are clearly observed, as shown in
The products were tested in the feasibility study of Enterococcusfaecalis (Ef), Escherichia coli (Ec) and Eikenellacorrodens (Ek) bacteria. For the studies, 100 μL of BHI culture medium and 100 μL of sterile distilled water were added to each well of the culture medium sterility control plate. The microplates are incubated in an oven at 37° C. and after 24 h the first test reading is performed in a microplate reader. After 48 h, a new reading should be performed, ending the test. Readings are taken at a fixed wavelength of 492 nm. The studies in
For viral load reduction studies directly employing the coronavirus, eight parts of the compound were adapted to room temperature (RT) and mixed with one part of the virus suspension. Immediately after incubation for defined periods at room temperature, the mixture was diluted 1:10. After four days of incubation at 37° C. in a CO2 incubator, cells were microscopically examined for virus-specific cytopathogenic effects after 10 min of virus contact with the niobium compound. All tests were performed in triplicate.
Initially, exploratory studies were carried out with different proportions of the compounds and with the materials separately.
Only CTAB promoted a viral load reduction of approximately 30%, while the new molecule Nb-CTAB promoted a 90% reduction in viral load. This result clearly shows the potentiation of the action of the new hybrid molecule formed by the reaction between CTAB and the negatively charged species of niobium, according to the model generated in the present technology.
Another result that deserves to be highlighted is the data referring to the combination of niobium gel containing niobium-methylene blue with alcohol gel. The presence of niobium gel promoted a viral load reduction of 100%, according to the results of the g7 sample in
Materials g3 and S12, which are sprays containing the hybrid niobium compounds in liquid form, also showed the ability to deactivate the coronavirus, although less efficient when compared to material g7. These compounds in liquid form also showed efficiency with prolonged time, being active even after 6 h of deposition on surfaces.
The results obtained indicate that the materials described in the present invention have high potential to be used in the fight against coronavirus and can be used in the form of a spray as a sanitizer and in the form of gel and can be used as a component of an alcohol gel.
Number | Date | Country | Kind |
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BR1020200163620 | Aug 2020 | BR | national |
Filing Document | Filing Date | Country | Kind |
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PCT/IB2021/051685 | 3/1/2021 | WO |