WO2024152095A1 - Premix and process for preparing a cosmetic composition, cosmetic composition, method for improving the touch sensitivity of a surface, method for photoprotection of a surface and use of the premix - Google Patents

Abstract

The present invention pertains to the fields of cosmetology and related sciences. More specifically, the invention relates to a premix for preparing a cosmetic composition, a process for preparing a cosmetic composition and a cosmetic composition with improved sensory characteristics. As well as a method for improving the touch sensitivity of a surface and a method for photoprotecting a surface. The premix and composition of the invention comprise microparticles and/or submicroparticles of Niobium and provide advantageous and surprising effects. In one embodiment, the premix and composition of the invention additionally comprise niobium nanoparticles.

Description

Invention Patent Descriptive Report

PREMIX AND PROCESS FOR PREPARING A COSMETIC COMPOSITION, COSMETIC COMPOSITION, METHOD FOR IMPROVING TOUCH SENSITIVITY OF A SURFACE, METHOD FOR PHOTOPROTECTING A SURFACE AND USE OF PREMIX

Field of Invention

[0001] The present invention is located in the fields of Cosmetology and related Sciences. More specifically, the invention relates to a premix for preparing a cosmetic composition, a process for preparing a cosmetic composition and a cosmetic composition with improved sensory characteristics. As well as a method for improving the touch sensitivity of a surface and a method for photoprotecting a surface. The premix and composition of the invention comprise Niobium microparticles and/or submicroparticles and provide advantageous and surprising effects. In one embodiment, the premix and composition of the invention additionally comprise Niobium nanoparticles.

Background of the Invention

[0002] The acceptability of cosmetic products on the market depends, among other factors, on the pleasure and well-being they are capable of providing to the consumer. In this sense, the sensorial properties of the product are very important in influencing positive emotions in the user. The perception of the quality of the cosmetic product and its superiority over others of the same nature is often related to the dry touch provided, its smell, its color, texture, freshness, spreadability, quick drying, softness, oily and/or sticky sensation after application, among other sensory properties.

[0003] Cosmetic products that have good sensory properties and also have more than one function, such as photoprotection, blurring imperfections (blur effect), among others, also stand out in the market.

[0004] In this context, among the physical photoprotectors available on the market, titanium dioxide is the most commonly used, followed by zinc oxide and hydroxyapatite. Although it is the most common physical sunscreen, titanium dioxide presents problems such as: a whitish appearance on the skin, pasty sensation, poor spreadability, incompatibility with some cosmetic vehicles. Furthermore, Titanium Dioxide was banned from use in the European community, for use in the food industry, as it is an ingredient with carcinogenic potential.

[0005] Another factor for the acceptability of the cosmetic product is its environmental impact. Therefore, Industries must be concerned with the relationship between beauty products, their sensory characteristics and their impacts on the environment and consumer health, and look for increasingly sustainable options.

[0006] The present invention provides an alternative to these problems.

[0007] Patent document JP2003267850A discloses the use of a powder dispersion (Premix) that includes nanoparticles in a cosmetic composition, more specifically, a sunscreen. On the other hand, said document does not disclose a premix or a composition with the specific characteristics of the present invention.

[0008] Patent document WO2021 121647A1 discloses the use of a complex metal material, applicable in cosmetic compositions, such as sunscreens that present an improvement in the UV absorption process. On the other hand, said document only discloses a series of examples in a generic way, without specific tests and does not disclose a premix or a composition with the specific characteristics of the present invention.

[0009] Patent document W02007133808A2 discloses the use of nanoparticles in cosmetic compositions. However, said document does not disclose a premix or a composition with the specific characteristics of the present invention. [0010] The article Ali et al. (01/2022) (Use of niobium oxide nanoparticles as nanofillers in PVP/PVA blends to enhance UV-visible absorption, opto-linear, and nonlinear optical properties) reveals improvement of UV absorption properties with the use of niobium pentoxide nanoparticles. On the other hand, said document does not disclose a premix or a composition with the specific characteristics of the present invention.

[0011] The article Singh et al. (2014) (Enhanced sun protection of nano-sized metal oxide particles over conventional metal oxide particles: An In-vitro comparative study) reveals a systematic and detailed study of cosmetics containing metal oxides on a nanometric scale. The study presents an in vitro method to determine the sun protection factor of sun cream samples containing zinc oxide and titanium dioxide. All formulated cosmetics were thermally stable, with a pH ranging from 7.9 to 8.2. Cosmetics that contained titanium nanoparticles or zinc oxide showed better spreadability. On the other hand, it only discusses the effect of titanium oxides and zinc oxides and does not disclose a premix or a composition with the specific characteristics of the present invention.

[0012] The article Lyu et al. (08/2022) (Nanoparticles in sunscreen: exploration of the effect and harm of titanium oxide and zinc oxide) presents the use of nanoparticles in a sunscreen. On the other hand, it only discusses the effect of titanium oxides and zinc oxides and does not disclose a premix or a composition with the specific characteristics of the present invention.

[0013] From what can be seen from the researched literature, no documents were found anticipating or suggesting the teachings of the present creation/secret/invention. The invention now revealed has, in the eyes of the inventors, novelty and inventive activity compared to the state of the art.

Summary of the Invention

[0014] The invention provides a premix for preparing a cosmetic composition, the use of the premix for preparing a cosmetic composition, a process for preparing a cosmetic composition and a cosmetic composition with improved sensory characteristics.

[0015] As explained in the following examples, the premix of the present invention presents very promising and surprising results in relation to softness/sensitivity to touch, in addition to promising results as a physical photoprotector.

[0016] In a first object, the present invention presents a premix for preparing a cosmetic composition, comprising one or more excipients and Niobium microparticles, Niobium submicroparticles or combinations thereof. Preferably, the premix comprises niobium submicroparticles.

[0017] In a second object, the present invention presents a process for preparing a cosmetic composition, comprising a step of mixing said premix in cosmetic excipients.

[0018] In a third object, the present invention presents a cosmetic composition, comprising one or more excipients and Niobium microparticles, Niobium submicroparticles or combinations thereof. Preferably, the composition comprises niobium submicroparticles.

[0019] In a fourth object, the present invention presents a method for improving the touch sensitivity of a surface comprising at least one step of applying the cosmetic composition, as defined above, to at least one surface

[0020] In a fifth object, the present invention presents a method of photoprotecting a surface comprising at least one step of applying the cosmetic composition, as defined above, to at least one surface.

[0021] In a sixth object, the present invention presents the use of the premix as defined herein to prepare cosmetic composition for photoprotection against UV radiation from the surface of an individual's skin and to improve sensitivity to touch upon application to the surface. [0022] The premix can be made in solid, semi-solid or liquid form. An example of a liquid form is a stable colloidal suspension that presents a downstream advantage to those who add it to a cosmetic formulation. This advantage is materialized in the reduction of mixing times, regardless of the base, as these differ from TÍO2 and other available materials that are supplied in dry powder, as these require an expensive and laborious dispersion step when incorporating them into the final cosmetic mix. [0023] In the context of the present invention, the expressions “Niobium microparticles”, “Niobium submicroparticles” and “Niobium nanoparticles” cover various chemical entities containing Niobium, including metallic Niobium, oxides, hydrates, hydrides, carbides, or niobium nitrides. Niobium, iron Niobium or Niobium alloyed with other metals or transition metals, or combinations thereof. It also includes Niobium pentoxide (Nb20s), NbC and NbO.

[0024] It is worth mentioning that in addition to Nb2Ü5, the product may contain other Nb polymorphs such as NbO and NbÜ2 and these same crystalline phases in the amorphous state, in combinations and proportions between them. Example: a premix can be prepared with Nb2Ü5 98% + NbÜ2 2%, partially crystalline and amorphous. In this case, 66% of this composition is crystalline. For another composition, the premix can be prepared with Nb2Ü587% + NbÜ2 13%. In this case, 95% of this composition is in the amorphous state.

[0025] Niobium Pentoxide, due to its physicochemical characteristics, is demonstrated as an excellent alternative to Titanium Dioxide. In the present invention, the evaluation of UVA and UVB photoprotection carried out with a premix containing microparticles and/or submicroparticles and, optionally, Niobium nanoparticles showed advantages over products containing Titanium Dioxide, zinc oxide and nano hydroxyapatite. The product of the invention presented advantages in relation to cosmetic sensorial, with photoprotective benefits, among others.

[0026] These and other objects of the invention will be immediately valued by those skilled in the art and by companies with interests in the segment, and will be described in sufficient detail for reproduction in the following description.

Brief Description of Figures

[0027] The following figures are displayed:

[0028] Figure 1 illustrates the results of the particle size distribution analysis for the sample with a processing time of 1 h in counting frequency (%) per diameter (nm).

[0029] Figure 2 illustrates the results of the particle size distribution analysis for the sample with a processing time of 3h in counting frequency (%) per diameter (nm).

[0030] Figure 3 illustrates the results of the particle size distribution analysis for the sample with a processing time of 6h in counting frequency (%) per diameter (nm).

[0031] Figure 4 illustrates the results of the particle size distribution analysis for the sample with a processing time of 12h in counting frequency (%) per diameter (nm).

[0032] Figure 5 illustrates the results of the particle size distribution analysis for the sample with a processing time of 6h in percentage (%) of numerical density by size class (pm).

[0033] Figure 6 illustrates the results of the particle size distribution analysis for the sample with a processing time of 6h in percentage (%) of volumetric density by size class (pm).

[0034] Figure 7 illustrates the results of the particle size distribution analysis for the sample with a processing time of 12h in percentage (%) of numerical density by size class (pm).

[0035] Figure 8 illustrates the results of the particle size distribution analysis for the sample with a processing time of 12h in percentage (%) of volumetric density by size class (pm).

[0036] Figure 9 shows a comparative result between the curves obtained as described in example 1 for Pentoxide nanoparticle samples of Niobium with a processing time of 6h, making a comparison between the numerical distribution and the volumetric distribution.

[0037] Figure 10 shows a comparative result between the curves obtained as described in example 1 for Niobium Pentoxide nanoparticle samples with a processing time of 12h, making a comparison between the numerical distribution and the volumetric distribution.

[0038] Figure 1 1 shows a comparative result between the numerical density curves (%) obtained as described in example 1 for Niobium Pentoxide nanoparticle samples with processing time of 6h and 12h, making a comparison between the numerical distribution for a processing time of 6h and the numerical distribution for a processing time of 12h.

[0039] Figure 12 shows a comparative result between the volumetric density curves (%) obtained as described in example 1 for samples of Niobium Pentoxide nanoparticles with processing times of 6h and 12h, making a comparison between the volumetric distribution for processing time of 6h and volumetric distribution for a processing time of 12h.

[0040] Figure 13 shows the comparative result between all samples/products subjected to UVA and UVB tests. Shown are: A) Lotion LN10 6h 5%; B) Lotion LN10 6h 10%; C) Lotion LN10 12h 5%; D) Lotion LN10 12h 10%; E) Zinc Oxide Lotion 5%; F) Nano hydroxyapatite lotion 5%; G) Titanium dioxide lotion 5%.

[0041] Figure 14 shows the comparative result between samples/products applied at 5% and subjected to UVA and UVB tests. Shown are: A) Lotion LN10 6h 5%; B) Lotion LN10 12h 5%; C) Zinc Oxide Lotion 5%; D) Nano hydroxyapatite lotion 5%; E) Titanium dioxide lotion 5%.

[0042] Figure 15 shows the comparative result between the samples/products LN 10 6h and 12h applied at 5% and 10% and subjected to UVA and UVB tests. Shown are: A) Lotion LN10 6h 5%; B) Lotion LN10 12h 5%; C) Lotion LN10 6h 10%; D) Lotion LN10 12h 10%.

[0043] Figure 16 presents a comparative graph of all formulations tested in the present invention.

Detailed Description of the Invention

[0044] The invention provides a premix for preparing a cosmetic composition, use of the premix in preparing a cosmetic composition, a process for preparing a cosmetic composition and a cosmetic composition with improved sensory characteristics.

[0045] In a first object, the present invention presents a premix for preparing a cosmetic composition, comprising one or more excipients and Niobium microparticles, Niobium submicroparticles or combinations thereof. Preferably, the premix comprises niobium submicroparticles.

[0046] In one embodiment, said premix additionally comprises Niobium nanoparticles.

[0047] Without the desire to be linked to theory, it is understood that said premix of the present invention benefits from the packaging of larger particles and the covering power of nanometric ones in order to achieve the technical effect of better sensitivity to touch.

[0048] In one embodiment, said premix comprises at least approximately 80% Niobium particles. In one embodiment, said particles may comprise Niobium microparticles and/or Niobium Submicroparticles and, optionally, Niobium nanoparticles. This high concentration of said particles facilitates the process of preparing cosmetic compositions by distributing them to other ingredients/excipients.

[0049] In the context of the present invention, the expressions “Niobium particles”, “Niobium microparticles”, “Niobium submicroparticles” and “Niobium nanoparticle” cover various chemical entities containing Niobium, including Niobium metal, oxides, hydrates, hydrides , carbides, or nitrides of Niobium, iron Niobium or Niobium alloyed with other metals or transition metals, or combinations thereof. It also includes Niobium pentoxide (Nb20s), NbC and NbO.

[0050] It is worth mentioning that in addition to Nb2Ü5, the product may contain other Nb polymorphs such as NbO and NbÜ2 and these same crystalline phases in the amorphous state, in combinations and proportions between them. Non-limiting example: a premix can be prepared in Nb2Ü5 98% + NbÜ2 2%, partially crystalline and amorphous. In this case, 66% of this composition is crystalline. For another composition, the premix can be prepared with Nb2Ü5 87% + NbC 13%. In this case, 95% of this composition is in the amorphous state.

[0051] In one embodiment, the premix described here has improved sensory effects. In one embodiment, said improved sensory effect is touch sensitivity.

[0052] The premix can be made in solid, semi-solid or liquid form. In this last form, the premix can be made with a stable colloidal suspension and therefore present a subsequent advantage for those who add it to a cosmetic formulation. This advantage is materialized in the reduction of mixing times, regardless of the base, as these differ from TÍO2 and other available materials that are supplied in dry powder, as these require an expensive and laborious dispersion step when incorporating them into the final cosmetic mix.

[0053] In a second object, the present invention presents a process for preparing a cosmetic composition, comprising a step of mixing said premix in cosmetic excipients.

[0054] In a third object, the present invention presents a cosmetic composition, comprising one or more excipients and Niobium microparticles, Niobium submicroparticles or combinations thereof. Preferably, the composition comprises niobium submicroparticles.

[0055] In one embodiment, the cosmetic composition additionally comprises niobium nanoparticles.

[0056] In one embodiment, the composition comprises up to approximately 10% by weight of Niobium particles. Alternatively, compositions containing Niobium particles contain up to approximately 5% by weight of said particles. In one embodiment, said particles may comprise Niobium microparticles and/or Niobium Submicroparticles and, optionally, Niobium nanoparticles.

[0057] In one embodiment, the cosmetic composition as described above presents improved sensory properties. In one embodiment, said sensory property is an improved touch sensitivity upon application to a surface.

[0058] In one embodiment, the cosmetic composition additionally has photoprotection power.

[0059] In a fourth object, the present invention presents a method for improving the touch sensitivity of a surface comprising at least one step of applying the cosmetic composition, as defined above, to at least one surface.

[0060] In a fifth object, the present invention presents a method of photoprotecting a surface comprising at least one step of applying the cosmetic composition, as defined above, to at least one surface.

[0061] In a sixth object, the present invention presents the use of the premix as defined herein to prepare cosmetic composition for photoprotection against surface UV radiation of an individual's skin and to improve sensitivity to touch upon application to the surface.

[0062] Niobium Pentoxide nanoparticles have a particle size distribution profile dependent on processing time.

[0063] Definitions of:

[0064] Microparticles: refers to particles with d10 to d100: 26.2 to 144 pm. [0065] Submicroparticles: refers to particles with d10 to d100: 0.3 to 5.2 pm. [0066] Nanoparticles: refers to particles with d10 to d100: 0.17 to 0.63 pm. [0067] Sensory characteristics/effects/properties: refer to attributes of the product such as color, smell, texture, freshness, irritability, spreadability, quick drying, dry touch, sensitivity to touch. The premix and cosmetic composition can provide a soft focus effect, also called blur effect, which is a soft coverage effect that uniforms the surface and reflects light so that we do not notice imperfections. Thus, the aforementioned premix is useful as a general makeup primer.

[0068] Cosmetic composition: refers to a preparation consisting of synthetic or natural substances, for external use on different parts of the human body, with the main objective of cleaning them, perfuming them, altering their appearance, correcting their odor and /or protect them or keep them in good condition. This composition can be made into various liquid, semi-solid or solid cosmetic forms. Non-limiting examples are: emulsions (creams, lotions, gel-cream), suspensions, gels, ointments, solutions, sticks, powders, aerosols, among others.

[0069] Excipients: refers to any compound in a formulation that is not the active ingredient or compound. These excipients are used in formulations to adjust different parameters, such as viscosity, active solubility, formulation stability, homogenization, etc., being available in the most diverse classes: preservatives, chelators, antioxidants, emulsifiers, gelling agents, clarifiers, surfactants, pH, vehicles, humectants, emollients, lubricants, among others. Non-limiting examples that can be used in the context of the present patent application are listed below: capric/caprylic triglyceride, undecane, tridecane, propanediol, cetyl potassium phosphate, glycerin, cetyl alcohol, xanthan gum, hydroxyacetophenone, 1,2 hexanediol, caprylyl glycol, disodium edta, tocopheryl acetate, sodium hydroxide, water.

[0070] The search for cosmetic products is growing, as are the requirements for their acceptability on the market. The premixes and compositions of the present invention have improved sensory characteristics, in addition to a photoprotective effect and blur effect, and can be used in a wide range of products. cosmetics, such as primers.

[0071] It is one of the objects of the invention to provide a premix and a cosmetic composition that provides a soft focus effect, also called a blur effect, which is a soft coverage effect that uniforms the surface and reflects light so that we do not notice imperfections. Said premix is useful as a general makeup primer.

[0072] In one embodiment, the premix can be prepared in a stable colloidal suspension and therefore presents a subsequent advantage for those who add it to a cosmetic formulation. This advantage is materialized in the reduction of mixing times, regardless of the base, as these differ from TÍO2 and other available materials that are supplied in dry powder, as these require an expensive and laborious dispersion step when incorporating them into the final cosmetic mix.

[0073] One of the objects of the invention is a skin photoprotective cosmetic composition.

[0074] In the context of the present invention, the term “individual” should be understood as a human or animal. In one embodiment, the individual can be understood as a human being.

[0075] In one embodiment, the composition is composed of particles dispersed in an oily phase comprising said ingredients/excipients.

Examples

[0076] Example 1 - Sensory analysis

[0077] The sensory evaluation by the participants was carried out immediately after applying the product, after 15 minutes, 1 hour, 24 hours, 1 week, 2 weeks and 4 weeks. Participants rated sensitivity to touch. The following ordinal rating scale was used: 0=none, +=minimal, ++=moderate, +++=high. The samples evaluated contained Niobium submicroparticles or the absence of Niobium submicroparticles. [0078] Table 1 below shows that compositions containing Niobium submicroparticles have improved touch sensitivity compared to compositions without these particles.

[0079] Table 1 - Sensory analysis results

[0080] Example 2 - Analysis of microparticles, submicroparticles and used in the examples

[0081] Particle size distribution analysis was carried out for Niobium Pentoxide nanoparticle samples with processing time (grinding) of 1 h, 6h and 12h (in the case of 6h and 12h, called LN10 6h and 12h, respectively ), which were used in the following examples. [0082] The data show an exponential decay in crystallinity (%) and crystallite size (nm), with the crystallite size (nm) appearing to reach an apparent plateau after 6 hours of grinding. The reduction in crystallinity presents a behavior similar to the size of the crystallite, however, it still presents a significant variation throughout the exposure of niobium pentoxide particles to high energy grinding. Regarding crystallinity, around 61% of monoclinic phase can be observed for the sample subjected to 1 h of grinding, around 41% of monoclinic phase can be observed for the sample subjected to 6h of grinding and around 26% of monoclinic phase for the sample subjected to 12h of grinding. More details about the process for obtaining nanoparticles can be found in patent application BR1 12023003019 of the inventors of the present application.

[0083] The samples with more amorphous characteristics (eg, the 12h sample) showed an even more significant improvement in improving the properties of the cosmetic composition (having a degree of crystallinity of about 26%). On the other hand, significant effects were also observed for samples that were subjected to 1 h and 6 h of grinding (having a degree of crystallinity of around 41 % and 61 %, respectively).

[0084] Figure 1 illustrates the results of analyzing the particle size distribution for the sample with a processing time of 1 h in counting frequency (%) per diameter (nm).

[0085] Figure 2 illustrates the results of analyzing the particle size distribution for the sample with a processing time of 3h in counting frequency (%) per diameter (nm).

[0086] Figure 3 illustrates the results of the particle size distribution analysis for the sample with a processing time of 6h in counting frequency (%) per diameter (nm).

[0087] Figure 4 illustrates the results of the particle size distribution analysis for the sample with a processing time of 12h in counting frequency (%) per diameter (nm).

[0088] Table 2 below shows the parameters of the particle size distribution analysis (numerical distribution) for the Niobium Pentoxide nanoparticle sample with a processing time of 6h.

[0089] Table 2 - Analysis parameters for 6h sample.

[0090] Table 3 shows the results of the particle size distribution analysis (numerical distribution) for the Niobium Pentoxide nanoparticle sample with a processing time of 6h. [0091] Table 3 - Analysis results for 6h sample

[0092] Figure 5 illustrates the results of the particle size distribution analysis for the sample with a processing time of 6h in percentage (%) of numerical density by size class (pm).

[0093] Table 4 details the data that served as the basis for the graph in figure 5.

[0094] Table 4 - Data from figure 5 on analysis for a 6h sample (numerical %)

[0095] Table 5 below shows the parameters of the particle size distribution analysis (volumetric distribution) for the Niobium Pentoxide nanoparticle sample with a processing time of 6h.

[0096] Table 5 - Analysis parameters for 6h sample

[0097] Table 6 shows the results of the particle size distribution analysis (volumetric distribution) for the Niobium Pentoxide nanoparticle sample with a processing time of 6h.

[0098] Table 6 - Analysis results for 6h sample

[0099] Figure 6 illustrates the results of the particle size distribution analysis for the sample with a processing time of 6h in percentage (%) of volumetric density by size class (pm).

[0100] Table 7 details the data that served as the basis for the graph in figure 6.

[0101] Table 7 - Data from figure 6 on analysis for a 6h sample (% volumetric)

[0102] Table 8 below shows the parameters of the particle size distribution analysis (numerical distribution) for the Niobium Pentoxide nanoparticle sample with a processing time of 12h.

[0103] Table 8 - Analysis parameters for 12h sample.

[0104] Table 9 shows the results of the particle size distribution analysis (numerical distribution) for the Niobium Pentoxide nanoparticle sample with a processing time of 12h.

[0105] Table 9 - Analysis results for 12h sample

[0106] Figure 7 illustrates the results of the particle size distribution analysis for the sample with a processing time of 12h in percentage (%) of numerical density by size class (pm).

[0107] Table 10 details the data that served as the basis for the graph in figure 7.

[0108] Table 10 - Data from figure 7 on analysis for 12h sample (numerical %)

[0109] Table 11 below shows the parameters of the particle size distribution analysis (volumetric distribution) for the Niobium Pentoxide nanoparticle sample with a processing time of 12h.

[0110] Table 11 - Analysis parameters for 12h sample.

[0111] Table 12 shows the results of the particle size distribution analysis (volumetric distribution) for the Niobium Pentoxide nanoparticle sample with a processing time of 12h.

[0112] Table 12 - Analysis results for 12h sample

[0113] Figure 8 illustrates the results of the particle size distribution analysis for the sample with a processing time of 12h in percentage (%) of volumetric density by size class (pm).

[0114] Table 13 details the data that served as the basis for the graph in figure 8.

[0115] Table 13 - Data from figure 8 on analysis for 12h sample (% volumetric)

[0116] Example 3 - Comparison of particle size distribution analyzes

[0117] Figure 9 shows a comparative result between the curves obtained as described in example 1 for Niobium Pentoxide nanoparticle samples with a processing time of 6h, making a comparison between the numerical distribution and the volumetric distribution.

[0118] Figure 10 shows a comparative result between the curves obtained as described in example 1 for Niobium Pentoxide nanoparticle samples with a processing time of 12h, making a comparison between the numerical distribution and the volumetric distribution.

[0119] Figure 1 1 shows a comparative result between the numerical density curves (%) obtained as described in example 1 for Niobium Pentoxide nanoparticle samples with processing time of 6h and 12h, making a comparison between the numerical distribution for a processing time of 6h and the numerical distribution for a processing time of 12h.

[0120] Figure 12 shows a comparative result between the volumetric density curves (%) obtained as described in example 1 for samples of Niobium Pentoxide nanoparticles with processing times of 6h and 12h, making a comparison between the volumetric distribution for a processing time of 6h and the volumetric distribution for a processing time of 12h.

[0121] Example 4 - Assessment of UVA and UVB Protection Factor

[0122] The determination of the UVA Protection Factor (FPUVA), using a spectrophotometric method, was initially described by B. L. Diffey and J. Robson and later modified and adapted by COLIPA for the evaluation of skin protection against UVA rays conferred by a product. The method described in this example consists of evaluating the UVA protection provided by a product using a spectrophotometric method, using a substrate suitable for applying the sample. The test is based on measuring the transmittance of UV radiation by the sample that is applied to an appropriate substrate with controlled roughness. Samples are exposed to determined and controlled levels of UV radiation using an irradiation source specified by the COLIPA method. Due to possible variations in interlaboratory results, the in vivo FPS is used for the mathematical adjustment of the radiation transmission spectra through a multiplication coefficient C.

[0123] The sunscreen sample is exposed to an irradiation dose proportional to the initial UVA Protection Factor (FPUVAO), calculated using the transmittance data of the unexposed sample. The final UVA Protection Factor (FPUVA) is calculated using the adjusted transmittance data of the sample exposed to UV radiation. The method consists of measuring the UV radiation flux through the product, expressed in terms of transmittance, and comparing it with the initial UV radiation flux of the substrate without product according to the spectrophotometric principle (Eq. 1) below:

T(À) = I / IO, where À is the wavelength (Eq. 1)

[0124] Absorbance at a given wavelength À is related to Transmittance by (Eq. 2): A(A) = -log(T(A) (Eq. 2)

[0125] The absorbance values are multiplied by different irradiances and action spectra so that correlations can be sought with biological responses obtained by in vivo methods. To calculate the FPS, the following are used: Irradiation source. Spectral irradiance generated by the ultraviolet l(A) source. Spectrum of action related to skin response. Spectrum of action related to Erythema that expresses the relationship between the cutaneous/subcutaneous reaction and the light energy E(A) (as defined by the CIE “Commission Internationale de I’Eclairage). To calculate the FPUVA: Irradiation source. Spectral irradiance generated by the ultraviolet l(A) source. Spectrum of action related to skin response. Spectrum of action related to Persistent Pigment Darkening (PPD) that expresses the relationship between the cutaneous/subcutaneous reaction and light energy in the region of 320-400nm P(A). I(A), E(A) and P(A) are known and their values are tabulated. The UVA Protection Factor (FPUVA) is determined by following the following steps:

[0126] Step 1: Measurement of the in vitro Absorbance A0(A) of the product spread on the PMMA substrate prior to any UV irradiation.

[0127] Step 2: Mathematical adjustment of the initial UV spectrum using the “C” coefficient to achieve an in vitro FPS equal to the in vivo FPS of the test sample. Then the initial UVA Protection Factor (FPUVAO) is calculated using A0(A) and C. [0128] Step 3: A single UV dose is calculated, proportional to the FPUVAO. (D = FPUVAO x 1.2 J.cm-2).

[0129] Step 4: UV irradiation of the sample according to the calculated dose D.

[0130] Step 5: Measure the in vitro Absorbance of the product after UV exposure. Obtaining the second UV absorption spectrum - Data from A(A).

[0131] Step 6: Mathematical adjustment of the second spectrum (spectrum after exposure to UV irradiation) according to the same “C” coefficient previously determined in Step 2. Then the in vitro UVA Protection Factor (FPUVA) is calculated.

[0132] In the present example, one of the objectives is to evaluate the behavior of a sunscreen regarding its effectiveness in UVA protection using the protocol based on the ISO 24443:2012 Determination of sunscreen UVA photoprotection in vitro.

[0133] In this example, the products tested are as shown in tables 13-18 below.

[0134] Table 14 - Lotion LN10 004 12 H5 10%

[0135] Table 15 - Lotion LN10 004 6 H5%

[0136] Table 16 - Zinc Oxide Lotion 5%

[0137] Table 17- Nano hydroxyapatite lotion 5%

[0138] Table 18 - Titanium Dioxide Lotion 5%

[0139] Table 19 - Lotion LN10 004 12 H5%

[0140] A sample of each product was stored and kept in IPelin® for a period of 1 month from the end of the tests. Product Application - Substrate Test: the substrate is a material to which the sample is applied. It must be non-fluorescent, photostable, non-reactive and compatible with all ingredients in a formulation. Furthermore, it must distribute the product in a way similar to what occurs on human skin and, therefore, must have a textured face. For this method, PMMA plates (poly-methyl meta-acrylate HD6 - Helioplate) with a textured substrate side were used. Each product was applied to a substrate in drops evenly distributed along the plate, at a rate of 1.3 mg/cm ² . Then, the products were spread in a standardized way with a finger protected by a disposable latex finger until a uniform film was obtained. The samples were then dried at room temperature for at least 30 minutes in the dark before taking the reading. A PMMA plate with 5 mg of glycerin spread on it was used to record the spectrophotometer baseline.

[0141] Test procedure. Pre-irradiation of the plates. A single dose of irradiation was calculated from the FPUVAO value. Samples were kept below 40°C during exposure to UV radiation.

[0142] Each PMMA plate was read at different locations to ensure that at least 2 cm ² was measured. The PFUVAO or FPUVA of a plate is calculated through the average absorbance of all sites on the same PMMA plate. If the coefficient of variation for absorbance between different sites exceeded 50%, this plate would be rejected and a new plate would be prepared. The product's FPUVAO or FPUVA is the average of the FPUVAO or FPUVA of at least 3 individual boards. If the coefficients of variation between the FPUVAO or FPUVA of the individual plates exceeded 20% then new plates would be prepared until the criterion for the coefficient of variation was reached. Calculation of the critical wavelength: the value of the critical wavelength (Àc) for the test product is defined as that wavelength where the area below the absorbance spectrum for the product irradiated from 290 nm to Àc is 90% of the integral of the absorbance spectrum from 290 nm to 400 nm, and is calculated as follows: a series of absorbance values (dependent on the wavelength increment) are calculated for each of the three plates, separately, on which the test product was applied.

[0143] The results of the products corresponding to tables 14-19 are indicated in tables 20-25 below.

[0144] Table 20a - Lotion Results LN10 004 6 H5 10% (where Àc corresponds to the critical wavelength; DP is the standard deviation):

t-statistic: 3.182446

Number of plates: 4

IC95: 0.918693

% of CI in relation to the mean: 16.7

[0145] The results obtained for the tested standard are shown in table 20b below (standard: S2, UVA-PF specification between 10.7 and 14.7)

[0146] Table 20b - Results for the standard

t-statistic: 3.182446

Number of plates: 4

IC95: 1 .299228

% of CI in relation to the mean: 10.8

[0147] The product LOTION LN10 004 6 H 10%, code IPC.2022.3314, presented an average UVA Protection Factor (FPUVA) equal to 5.5 and critical wavelength equal to 382.8nm.

[0148] Table 21 - Lotion Results LN10 004 06 H 5% (where Àc corresponds to the critical wavelength; DP is the standard deviation):

t-statistic: 3.182446

Number of plates: 4

IC95: 0.795612

% of CI in relation to the mean: 18.7

[0149] The results obtained for the tested standard are those in table 20b.

[0150] The LN10 004 6 H 5% Lotion product, code IPC.2022.3315, presented an average UVA Protection Factor (FPUVA) equal to 4.3 and a critical wavelength equal to 381.3nm.

[0151] Table 22 - 5% Zinc Oxide Lotion Results (where Àc corresponds to the critical wavelength; SD is the standard deviation):

t-statistic: 3.182446

Number of boards: 4 IC95: 0

% of CI in relation to the mean: 0

[0152] The results obtained for the tested standard are those in table 20b.

[0153] The 5% Zinc Oxide Lotion product, code IPC.2022.3316, presented an average UVA Protection Factor (FPUVA) equal to 4.0 and a critical wavelength equal to 381.8nm.

[0154] Table 23 - Results Nano Hydroxyapatite Lotion 5% (where Àc corresponds to the critical wavelength; DP is the standard deviation):

t-statistic: 3.182446

Number of plates: 4

IC95: 0.795612

% of CI in relation to the mean: 24.5

[0155] The results obtained for the tested standard are those in table 20b.

[0156] The product Nano Hydroxyapatite Lotion 5%, code IPC.2022.3317, presented an average UVA Protection Factor (FPUVA) equal to 3.3 and a critical wavelength equal to 374nm.

[0157] Table 24 - Results Titanium Dioxide Lotion 5% (where Àc corresponds to the critical wavelength; DP is the standard deviation):

t-statistic: 3.182446

Number of plates: 4

IC95: 0.918693

% of CI in relation to the mean: 20.4

[0158] The results obtained for the tested standard are those in table 20b.

[0159] The product Titanium Dioxide Lotion 5%, code IPC.2022.3318, presented an average UVA Protection Factor (FPUVA) equal to 4.5 and a critical wavelength equal to 382.8nm.

[0160] Table 25 - Results LOTION LN10 004 12 H 5% (where Àc corresponds to the critical wavelength; DP is the standard deviation):

t-statistic: 3.182446

Number of plates: 4

IC95: 0795612

% of CI in relation to the mean: 18.7

[0161] The results obtained for the tested standard are those in table 20b.

[0162] The product LOTION LN10 004 12 H 5%, code IPC.2022.3316, presented an average UVA Protection Factor (FPUVA) equal to 4.8 and critical wavelength equal to 382nm.

[0163] Example 5 - Assessment of sun protection factor

[0164] The solar spectrum is made up of a series of radiations, and almost all of them can act in a beneficial way. However, when the amount of energy absorbed is greater than the tolerable dose, risks are inevitable. The main solar radiations are: Infrared rays, responsible for the feeling of heat and dehydration of the skin during exposure to the sun; UVA (320-400nm), tans superficially, however, it contributes to premature skin aging, induced by prolonged sun exposure; pass through most common glass. Depending on the thickness of the skin, they can reach dermal tissues, which makes them as dangerous as higher energy wavelengths (UVB). The UVA range can be subdivided into low UVA, from 320-340 nm, responsible for the vast majority of the physiological effects of UVA on the skin, and high UVA, from 340-400 nm, responsible for very small changes in elastic fibers; UVB (290-320 nm) are considered more harmful than UVA radiation. They have little penetration into the skin, but due to their high energy, they are most responsible for immediate damage from solar radiation. and for much of the late damage. They are also responsible for transforming epidermal ergosterol into vitamin D. In excess, they cause erythema (sunburn), premature aging and skin cancer, mainly affecting people with fair skin; UVC (100-290nm), are quite harmful, do not stimulate tanning and cause sunburn and cancer. Some studies have detected a slow destruction of the ozone layer caused by CFCs (chlorofluorocarbons), a family of gases used until recently as a propellant in aerosols and refrigeration. The consequences of this destruction have not yet been fully assessed, but they will undoubtedly greatly affect life on the planet. Tanning is a defense against solar radiation, which stimulates the body to produce melanin, a natural skin pigment, thus reducing the penetration of UVA and UVB radiation. In the first few days of sun exposure, the melanin production mechanism begins to be activated. During this period, sunscreens with higher protection factors should be used, as they will act in a similar way to melanin, filtering UVA and UVB rays. The sun protection factor or SPF is intended to indicate to the consumer the degree of protection provided by the product. The great variability of solar radiation and different skin types force the consumer to know their own skin and define which SPF is best suited to their case. The higher the FPS value, the higher the level of protection. To choose the FPS compatible with a given skin type, one should not take into account the parts of the body most exposed to the sun, such as arms or face, as these regions are in direct and constant contact with the sun and, therefore, respond in a negative way. differently to its effects. SPF measurement methods are based on the appearance of erythema on the skin. It is therefore necessary to standardize the way this erythema is measured. Therefore, minimum erythematic dose (MED) is defined as the amount of energy required to produce the first noticeable erythematic reaction with clearly defined borders, observed between 16-24 hours after exposure to ultraviolet radiation. The minimum erythematogenous dose (MED) depends on the individual's skin type, amount of melanin in the skin, the length and intensity of the incident wave. Individuals can be classified into six groups that are also called phototypes, which are estimated through personal history of burns and tanning, after exposure for 30 to 50 minutes in the midday sun, after a period without exposure. The phototypes have the characteristics described in table 2.

[0165] Table 26 - Skin phototypes according to M. A, Patahak (1983):

[0166] The FPS corresponds to how many MED a person can be exposed to the Sun without developing erythema. Therefore, SPF is defined as the ratio between the amount of ultraviolet energy required to produce an erythematic dose in protected skin in relation to the energy required to produce an erythematic dose in unprotected skin.

[0167] In this example, the objective of the tests is to determine the Static Sun Protection Factor (SPF) of the test products using the Protocol based on the ISO 24444:2019 standard - Cosmetics — Sun protection test methods — In vivo determination of the sun protection factor (SPF).

[0168] The selection of Participants followed the criteria: Number of participants included in the study 03 Phototypes (Fitzpatrick) I to III Sex F and M Age 21 to 46.

[0169] Inclusion criteria: Age 18 to 65 years; phototypes I to III; Male and female; Individual typological angle (ITA ^S ) greater than 28 ^s - determined by colorimetry.

[0170] Non-inclusion/exclusion criteria: Skin marks in the experimental area that interfere with the assessment of possible skin reactions (pigmentation disorders, vascular malformations, scars, increased hairiness, large amounts of ephelides and nevi, sunburn); Active dermatoses (local and disseminated) that could interfere with the study results; Pregnant or breastfeeding women; History of allergic reactions, irritation or intense sensations of discomfort to topical products: cosmetics and medicines; Participants with a history of allergy to the material used in the study; History of atopy; History of pathologies aggravated or triggered by ultraviolet radiation; People with immunodeficiencies; Kidney, heart or liver transplants; Intense sun exposure or tanning session up to 15 days before the initial assessment; Expected intense sun exposure or tanning session during the study period; Plan to take a swim in the sea, swimming pool or sauna during the study; Participants who practice water sports; Use of the following systemic topical medications: immunosuppressants, antihistamines, non-steroidal anti-inflammatory drugs, and corticosteroids up to two weeks before the selection; Treatment with acid vitamin A and/or its derivatives orally or topically up to 1 month before the start of the study; Anticipated vaccination during the study or up to 3 weeks before the study; Be participating in another study; Any condition not mentioned above that, in the investigator's opinion, could compromise the evaluation of the study; History of lack of adherence or unwillingness to adhere to the study protocol; Professionals directly involved in carrying out this protocol and their families.

[0171] Restrictions imposed on participants: Do not undergo aesthetic or dermatological treatments during the study.

[0172] Medications prohibited during the study: Anti-inflammatories; Antihistamines; Immunosuppressants; Acidic vitamin A and derivatives.

[0173] Products containing microparticles and/or submicroparticles and, optionally Niobium Pentoxide nanoparticles.

[0174] Consent of Research Participants. The objective and methodology of the research were explained to the participants and they signed an Informed Consent Form.

[0175] Procedure for determining static (dry) FPS. Multiport 601 equipment with 300 W xenon arc lamp (Solar Light Co Inc); PMA2103 SUV LLG Detector; PMA2100 Photometer/Radiometer. Determination of the Minimum Erythematogenous Dose (MED).

[0176] The minimum erythematogenous dose (MED) is considered to be the amount of radiant energy necessary to produce the least noticeable and undoubted redness, evaluated 16 to 24 hours after exposure. Each participant's MED was determined by a sequence of exposure to ultraviolet light, with intensity (MED/minute) increased in geometric progression, with each exposure graduated with an increase of 12% in relation to the previous one (1.12n). After 16-24 hours of irradiation, a local dermatological examination was carried out to check the spots with the appearance of erythema.

[0177] Determination of static (dry) FPS. On the back (infrascapular region) of each participant, 5.0 x 7.0 cm (35 cm ² ) rectangles, called sites, were marked with a surgical pen. The sites were cleaned with dry cotton. 2 mg/cm ² of the samples under evaluation or the Standard Product were applied to the demarcated sites, spreading them homogeneously with a finger wrapped in a finger. After application, participants waited 15 minutes for it to dry. After drying, the site was irradiated, considering the defined time of the individual MED and the expected SPF of the product. 16-24 hours after irradiation, a local dermatological examination was carried out to determine the SPF.

[0178] FPS Calculation The FPS value is defined by the ratio between the time needed to produce a MED on skin protected with a product containing sunscreen (MEDp) and the time needed to produce a MED on unprotected skin (MEDu). Thus, the FPS is calculated by Eq. 3.

Eq.3

The FPS value was calculated for each participant. For the panel of participants, the average FPS, standard deviation and lower limit of the 95% confidence interval were calculated.

[0179] Tables 27-32 show the results obtained for the product samples in Table 14-19, respectively, and the standard product P2 (PFS 13.7 to 18.5).

[0180] Table 27 - Results for the product samples from Table 14. No. of participants included: 3; Number of participants who completed the study: 3.

[0181] The test product in the table above presented an average static FPS of 15.4. The standard product P2, evaluated concomitantly, presented an average static FPS of 16.0. These results are in accordance with those provided for in Protocol ISO 24444:2019 - Cosmetics — Sun protection test methods — In vivo determination of the sun protection factor (SPF).

[0182] The product LOTION LN10 004 6 H 10%, code IPC.2022.3314, presented an average static FPS of 15.4.

[0183] Table 28 - Results for the product samples from Table 19. No. of participants included: 3; Number of participants who completed the study: 3.

[0184] The test product in the table above presented an average static FPS of 10.3. The standard product P2, evaluated concomitantly, presented an average static FPS of 16.0. These results are in accordance with those provided for in Protocol ISO 24444:2019 - Cosmetics — Sun protection test methods — In vivo determination of the sun protection factor (SPF).

[0185] The product LOTION LN10 004 6 H 5%, code IPC.2022.3315, presented an average static FPS equal to 10.3.

Example 6 - UVA-B SPF effectiveness compared to market filters

[0186] In the present example, a comparative FPS UVA-B efficacy screening was carried out between materials containing microparticles and/or submicroparticles and, optionally, nanoparticles and the market inorganic filters Titanium Dioxide, Zinc Oxide and Nano Hydroxyapatite.

[0187] UVA FPS (320-400 nm) and Static FPS Screening reflects the level of protection against UVB rays (290-320 nm) offered by a cosmetic product after application to dry skin, with a minimum drying time of 15 minutes . Tests were carried out with the aim of identifying the estimated protection factor for each of the samples at concentrations of use similar to those used in the physical photoprotector market.

[0188] UVA rays are characterized by superficially tanning the skin, contributing to its premature aging, induced by prolonged sun exposure. These rays pass through most common glass. Depending on the thickness of the skin, they can reach dermal tissues, which makes them as dangerous as higher energy wavelengths (UVB). A The UVA range can be subdivided into low UVA, from 320-340nm, responsible for the vast majority of the physiological effects of UVA on the skin, and high UVA, from 340-400nm, responsible for very small changes in elastic fibers. UVB rays (290-320nm) are considered more harmful than UVA radiation. They have little penetration into the skin, but due to their high energy, they are largely responsible for immediate damage from solar radiation and a large part of late damage. They are also responsible for transforming epidermal ergosterol into vitamin D. In excess, they cause erythema (sunburn), premature aging and skin cancer, mainly affecting people with fair skin.

[0189] For the study in question, it was decided to carry out comparative tests with micronized titanium dioxide, zinc oxide and Nano hydroxyapatite, both with nanometric particle sizes, at a concentration of 5% (% solids). These ingredients are the physical or inorganic photoprotectors most used on the market. And to understand whether there is a proportional relationship between concentration of use and sun protection factor, LN10 6 and 12 h were also subjected to tests in application at 10% (% solids).

[0190] Method: For the formulations tested, a standard base was produced, compatible with all applications, as detailed in the clinical test reports. For this base, surfactants and emollients frequently used in photoprotector formulations were listed. The samples with Niobium particles are presented in the form of a suspension in an aqueous medium and for all of them a solids concentration of 20% was considered for the purpose of calculating the percentage of active.

[0191] The results can be summarized in table 29.

[0192] Table 29 - FPUVA, FPUVB and FPS results

* Ultraviolet protection factor A ** Ultraviolet protection factor B *** Sun Protection Factor

[0193] The results are very promising. Figure 13 shows a general overview of the results in which Nano hydroxyapatite at 5% showed the lowest absorption for UVA radiation and LN10 at 10% showed the highest absorption for UVB (static SPF).

[0194] In a comparative way, the results of all active ingredients applied at 5% can be seen in figure 14, in which it is observed that titanium dioxide presents the best result in relation to UVB absorption (FPUVB=13.4 ) and for UVA (FPUVA=4.5), but for UVA the difference is very small (+ 0.2 points of FPUVA) in relation to the LN10 6 and 12h samples, both with FPUVA= 4.3 and this result was superior to Zinc Oxide and Nano Hydroxyapatite.

[0195] In figure 15 it can be seen that among the samples of the LN10 6h and 12h product, the samples applied at 5% showed very similar results, while in the samples applied at 10% a better performance was observed for the LN10 12h. Both LN10 samples presented an FPUVA ratio of at least 1/3 in relation to FPUVB, which complies with Brazilian legislation, RDC N ^s 30, OF JUNE 1 ² , 2012 of Anvisa, which describes the Mercosul Technical Regulation on Protectors Solar in Cosmetics. Based on the data obtained for LN10 12h, there is a strong indication that each percentage point is equivalent to 2 FPUVB points.

[0196] The results obtained allow us to conclude that LN10 12h at a concentration of 10% active was more promising than LN10 6h at 10% active. For the comparative concentration of 5%, both LN 10 samples were only less effective in relation to titanium dioxide, but in relation to zinc oxide and Nano hydroxyapatite they showed slightly superior performance. These results indicate that LN10 is a very promising material as a physical photoprotector. [0197] Example 7 - comparison with micro-sized Niobium particle samples

[0198] For comparison purposes, formulations with micro-sized niobium pentoxide particles (d10 to d100 = 26.2 to 144 pm) were also tested in amounts of 5% and 10% of the composition.

[0199] Table 30 - Sample IPC.2023.1682 - Nb micro particles 5%

[0200] Table 31 - Sample IPC.2023.1683 - Nb micro particles 10%

[0201] Using the same methodology as in example 4, the UVA Protection Factor (FPUVA) of the samples described in tables 30 and 31 was determined.

[0202] Table 32a - Sample results IPC.2023.1682 - Nb micro 5% particles (where Àc corresponds to the critical wavelength; DP is the standard deviation):

t-statistic: 3.18

Number of plates: 4

IC95: 0.795612

% of CI in relation to the mean: 18.72

[0203] The results obtained for the tested standard are shown in table 32b below (standard: S2, UVA-PF specification between 10.7 and 14.7)

[0204] Table 32b - Results for the standard

t-statistic: 3.182446

Number of plates: 4

IC95: 2.002245

% of CI in relation to the mean: 15.7

[0205] The sample IPC.2023.1682 - Nb micro 5% particles presented an average UVA protection factor (FPUVA) equal to 4.25 and a critical wavelength equal to 377.0 nm.

[0206] Table 33a - Sample results IPC.2023.1683 - Nb micro 10% particles (where Àc corresponds to the critical wavelength; DP is the standard deviation):

t-statistic: 3.18

Number of plates: 4

IC95: 0.918693

% of CI in relation to the mean: 10.81

[0207] The results obtained for the tested standard are shown in table 32b below (standard: S2, UVA-PF specification between 10.7 and 14.7)

[0208] Table 32b - Results for the standard

t-statistic: 3.182446 Number of plates: 4 IC95: 2.002245 % of CI in relation to the mean: 15.7

[0209] The sample IPC.2023.1683 - Nb micro 10% particles showed an average UVA protection factor (FPUVA) equal to 8.5 and a critical wavelength equal to 378.0 nm.

[0210] Additionally, using the same methodology as in example 5, the solar protection factor of the samples described in tables 30 and 31 was evaluated.

[0211] Table 34 - Results sample I PC.2023.1682 - Nb micro particles 5% (Table 30). No. of participants included: 10; Number of participants who completed the study: 10.

[0212] The test sample presented an average static FPS of 12.7. The standard product P2, evaluated concomitantly, presented an average static FPS of 15.3. These results are in accordance with those provided for in Protocol ISO 24444:2019 - Cosmetics — Sun protection test methods — In vivo determination of the sun protection factor (SPF).

[0213] Table 35 - Sample results IPC.2023.1683 - Nb micro particles 10% (Table 31). No. of participants included: 10; Number of participants who completed the study: 10.

| Participants ~| | Reference product. | Test product |

[0214] The test sample presented an average static FPS of 23.8. The standard product P2, evaluated concomitantly, presented an average static FPS of 16.2. These results are in accordance with those provided for in Protocol ISO 24444:2019 - Cosmetics — Sun protection test methods — In vivo determination of the sun protection factor (SPF).

[0215] Example 8 - comparison with sub-micro size Niobium particle samples

[0216] For comparison purposes, formulations with sub-micro size niobium pentoxide particles (d10 to d100 = 0.3 to 5.2 pm) in amounts of 5% and 10% of the composition were also tested.

[0217] Table 36 - Sample IPC.2023.1 163 - sub-micro Nb particles 5%

[0218] Table 37 - Sample IPC.2023.1162 - sub-micro Nb particles 10%

[0219] Using the same methodology as in example 4, the UVA Protection Factor (FPUVA) of the samples described in tables 36 and 37 was determined.

[0220] Table 38a - Results sample IPC.2023.1163 - sub-micro 5% Nb particles (where Àc corresponds to the critical wavelength; DP is the standard deviation):

t-statistic: 3.182446

Number of plates: 4

IC95: 2.002245

% of CI in relation to the mean: 15.7

[0221] The results obtained for the tested standard are shown in table 38b below (standard: S2, UVA-PF specification between 10.7 and 14.7)

[0222] Table 38b - Results for the standard

t-statistic: 3.182446

Number of plates: 4

IC95: 2.002245

% of CI in relation to the mean: 15.7

[0223] Sample I PC.2023.1 163 - 5% sub-micro Nb particles presented an average UVA protection factor (FPUVA) equal to 6.5 and a critical wavelength equal to 378.0 nm.

[0224] Table 39a - Sample results IPC.2023.1 162 - sub-micro 10% Nb particles (where Àc corresponds to the critical wavelength; DP is the standard deviation):

t-statistic: 3.18

Number of plates: 4

IC95: 0.795612

% of CI in relation to the mean: 9.09

[0225] The results obtained for the tested standard are shown in table 39b below (standard: S2, UVA-PF specification between 10.7 and 14.7)

[0226] Table 39b - Results for the standard

t-statistic: 3.182446

Number of plates: 4

IC95: 2.002245

% of CI in relation to the mean: 15.7

[0227] The sample IPC.2023.1162 - 10% sub-micro Nb particles presented an average UVA protection factor (FPUVA) equal to 8.75 and a critical wavelength equal to 379.0 nm.

[0228] Additionally, using the same methodology as in example 5, the solar protection factor of the samples described in tables 36 and 37 was evaluated.

[0229] Table 40 - Sample results IPC.2023.1163 - sub-micro Nb particles 5% (Table 36). No. of participants included: 3; Number of participants who completed the study: 3.

[0230] The test sample presented an average static FPS of 13.4. The standard product P2, evaluated concomitantly, presented an average static FPS of 16.4. These results are in accordance with those provided for in Protocol ISO 24444:2019 - Cosmetics — Sun protection test methods — In vivo determination of the sun protection factor (SPF).

[0231] Table 41 - Sample results IPC.2023.1162 - submicro Nb particles 10% (Table 37). No. of participants included: 10; Number of participants who completed the study: 10.

[0232] The test sample presented an average static FPS of 23.5. The standard product P2, evaluated concomitantly, presented an average static FPS of 16.4. These results are in accordance with those provided for in Protocol ISO 24444:2019 - Cosmetics — Sun protection test methods — In vivo determination of the sun protection factor (SPF).

[0233] Example 9 - general comparative table

[0234] For comparison purposes, figure 16 shows a comparative graph of all formulations tested in the present invention.

[0235] Table 42 - comparative table of the formulations tested for in vitro UVA protection and for SPF.

[0236] From the results above, for formulations containing 5% by mass of particles when comparing with a composition containing 5% by mass of Titanium Dioxide (which is commonly used in sunscreens), it is possible to observe that particularly better results than dioxide of Titanium were observed for compositions containing 5% niobium pentoxide particles that were subjected to 1 h of grinding, niobium pentoxide particles that were subjected to 6 h of grinding and niobium pentoxide particles that were subjected to 12 h of grinding. Particularly in the case where the solid particles have been dispersed in an oily phase.

[0237] Likewise, particularly expressive results for higher concentrations (e.g. 10% by mass) were observed for compositions containing niobium pentoxide particles that were subjected to 12 hours of grinding. However, very expressive results at high concentrations were also observed for niobium pentoxide particles that were subjected to 1 h of grinding, niobium pentoxide particles that were subjected to 6 h of grinding, as well as particles with micro and sub-micro diameters. For 1h, 6h and 12h particles, particularly in the case where the solid particles were dispersed in an oil phase.

[0238] Particularly for the formulation containing particles with a diameter micro exfoliating effect was observed.

[0239] The results are very promising and demonstrate that Niobium microparticles and/or submicroparticles are very promising materials as a physical photoprotector, in addition to presenting surprising results in relation to softness/sensitivity to touch as shown by sensory testing.

[0240] Example 10 - Cytotoxicity (evaluates cell death when in contact with viable cells)

[0241] According to ISO 10993-5 “Biological evaluation of medical devices, Tests for in vitro cytotoxicity”, the material is considered non-cytotoxic when relative cell viability above 70% is verified. Therefore, at the concentrations analyzed:

[0242] - Within 24 hours of exposure to cells, the compounds NIONE LN 10006-6H and NIONE LN 10006-12H are considered non-cytotoxic from a concentration of 0.78 mg/g;

[0243] - After 48 hours of exposure, the compounds NIONE LN 10006-6H and NIONE LN 10006-12H are considered non-cytotoxic from a concentration of 0.20 mg/g.

[0244] Example 11 - Genotoxicity (evaluates potential damage to cellular DNA when in contact with viable cells)

[0245] Evaluating short-term exposure of the two compounds (6h) with and without metabolic activation (6h), the concentration of 0.0012% of the active niobium compound proved to be genotoxic for both products Nione LN 10006 6h and Nione LN 10006. However, concentrations of 0.0006% and 0.0003% of niobium did not prove to be genotoxic when exposed to cells. Thus, concentrations < 0.0006% of the two products evaluated do not present cellular genotoxicity.

[0246] The depositor, when depositing this request with the competent/guarantor body, seeks and intends to: (i) name the authors/inventors in respect of their respective moral, copyright and property rights related to their works; (ii) unequivocally indicate that it holds the secret of business or industrial and holder of any form of intellectual property that derives therefrom and the depositor desires; (iii) describe in detail the content of the creations and the secret, proving their existence on a physical and legal level; (iv) obtain protection for your spirit creations, as provided for in the Copyright Law; (v) establish the relationship between the examples/concretions and the creative, ornamental, distinctive or inventive concept according to the depositor's cognition and their context, to clearly demonstrate the scope of their protected and/or guardianable intangible asset; (vi) request and obtain additional rights provided for patents, if the applicant chooses to continue with the administrative procedure until the end.

[0247] Any future disclosure or publication of this document does not, in itself, constitute authorization for commercial use by third parties. Even if the content becomes part of the physical world accessible to third parties, the disclosure and publication of this document in accordance with the law does not eliminate the legal status of secret, serving only the spirit of the Law to: (i) serve as proof that the creator created the objects described here and expressed them in a physical medium, which is this report itself; (ii) unequivocally indicate its owner/holder and authors/inventor(s); (iii) inform third parties regarding the existence of the creations and the aforementioned industrial secret, the content for which intellectual protection is required or will be required under the terms of the Law, including patent protection and the date of its deposit, from which it will have rights of priority and the term of patent exclusivity may begin, if applicable; and (iv) assist in the technological and economic development of the country, from the revelation of the creation, if this occurs, and the authorization of the use of the secret solely and exceptionally for the purposes of studies and/or development of new improvements, thus avoiding reinvestment parallel by third parties in the development of the same good.

[0248] It is immediately warned that any commercial use requires authorization from the authors or the possessor/holder and that unauthorized use entails sanctions provided for by law. In this context, given the broad detail according to which the creation, the concept and examples were revealed by the depositor, those skilled in the art will be able, without much effort, to consider other ways of implementing the present creation and/or invention in ways not identical to those merely exemplified above. However, such forms are or may be considered to be within the scope of one or more of the attached claims.

Claims

Claims 1 . Premix for preparing a cosmetic composition characterized by comprising one or more excipients and Niobium microparticles, Niobium submicroparticles or combinations thereof. 2. Premix according to claim 1, characterized in that it additionally comprises niobium nanoparticles. 3. Premix according to claim 1, characterized in that it comprises at least 80% Niobium microparticles and/or Niobium submicroparticles and, optionally Niobium nanoparticles. 4. Process for preparing a cosmetic composition characterized by comprising a step of mixing a premix as defined in claim 1 in cosmetic excipients. 5. Cosmetic composition characterized by comprising one or more cosmetic excipients and Niobium microparticles, Niobium submicroparticles or combinations thereof. 6. Cosmetic composition according to claim 5, characterized in that it additionally comprises niobium nanoparticles. 7. Cosmetic composition according to claim 5, characterized in that it comprises up to approximately 10% by weight of Niobium microparticles and/or Niobium submicroparticles and, optionally Niobium nanoparticles. 8. Cosmetic composition according to claim 5, characterized in that it presents improvement in sensory properties. 9. Cosmetic composition according to claim 8 characterized by the sensory property being a sensitivity to touch upon application to a surface. 10. Method for improving the touch sensitivity of a surface characterized by comprising at least one step of applying the cosmetic composition, as defined in claim 5, to at least one surface. 10. Method of photoprotecting a surface characterized by comprising at least one step of applying the cosmetic composition, as defined in claim 5, to at least one surface. 11 . Use of the premix as defined in claim 1, characterized in that it is to prepare cosmetic composition for photoprotection against UV radiation from the surface of an individual's skin and to improve sensitivity to touch upon application to the surface.