KR102659680B1 - Organo-Ilite composite powder, manufacturing method thereof, and cosmetic composition comprising the same - Google Patents

Abstract

The present invention relates to illite powder; and polyvinylpyrrolidone coated on the surface of the illite powder; and a method for producing the same, wherein the organic-illite composite powder according to the present invention is used as a powder material for a cosmetic composition. When used, color control can be possible without using coloring pigments, and excellent spreadability and biological stability can be secured. When using organic-illite complex powder as a carrier to support functional substances, whitening, wrinkle improvement, moisturizing, etc. Various effects can be achieved.

Description

Organic-Ilite composite powder, manufacturing method thereof, and cosmetic composition comprising the same {Organo-Ilite composite powder, manufacturing method thereof, and cosmetic composition comprising the same}

The present invention relates to an organic-illite composite powder, a method for producing the same, and a cosmetic composition containing the same.

Illite is a mineral that accompanies sedimentary or hydrothermal alteration rocks and is a very important non-expandable clay mineral along with kaolin mineral and smectite.

The general definition of illite that is currently widely used is "the particle size is 2~4 ㎛ or less, similar to mica, the d-spacing is 10 Å, and chemically, it is smaller than muscovite, considering its crystal chemical characteristics." It is more abundant in Si ⁴⁺ , Mg ²⁺ and H ₂ O, but the content of tetrahedral Al ³⁺ and interlayer K ⁺ is lower. The general chemical composition is K _0.8-0.9 (Al, Fe, Mg). ₂ (Si, Al) ₄ O ₁₀ (OH) ₂ . The average charge per unit cell of illite is 0.8, a value intermediate between smectite and mica.

It has been discovered that excellent quality illite is buried in greater abundance in Yeongdong-gun, North Chungcheong Province, Korea compared to other regions (including domestic and overseas). Although the potential for growth is great, in Korea, the excellent properties of the mineral are not being utilized because simple mining and crushing are then sold mainly by small-scale operators.

In particular, a lot of effort is being made at home and abroad to develop eco-friendly well-being materials such as air and water pollution prevention, but the usability and safety of illite, which has excellent performance, has not been secured, so research using illite minerals existing in the region is limited. There is no systematic technological development taking place.

Currently, product development using illite includes soap and shampoo, which are household items that utilize the adsorption efficiency of illite, and for cosmetics, serums and skins using illite eluate, and sunscreen using inorganic materials have been developed.

However, the dark ocher color, which is a unique color of Illite, is an inorganic powder, so its direct use in BB cream or foundation is limited. It is a basic inorganic material for color cosmetics that uses coloring pigments in white powder, and can be directly applied to the color of the raw material itself. It is difficult to use and the mineral itself does not feel smooth, making it difficult to use as a cosmetic material.

Meanwhile, Republic of Korea Patent Publication No. 10-1332268 is presented as a similar prior document.

Republic of Korea Patent Publication No. 10-1332268 (2013.11.18)

In order to solve the above problems, the present invention provides an organic-illite composite powder that can control color without using coloring pigments when used as a powder material for cosmetic compositions and can secure excellent spreadability and biological stability, and its The purpose is to provide a manufacturing method and a cosmetic composition containing the same.

In addition, an organic-illite composite powder that can achieve various effects such as whitening, wrinkle improvement, or moisturizing when carrying functional substances by using the organic-illite composite powder as a carrier, a method of manufacturing the same, and a cosmetic composition containing the same The purpose is to provide.

However, the above object is illustrative, and the technical idea of the present invention is not limited thereto.

One aspect of the present invention for achieving the above object is illite powder; and polyvinylpyrrolidone coated on the surface of the illite powder. It relates to an organic-illite composite powder comprising a.

In the above aspect, the average particle diameter of the illite powder may be 0.1 to 20 ㎛.

In one aspect, the specific surface area of the illite powder may be 1 to 100 m2/g, the pore volume may be 0.01 to 0.1 cm3/g, and the average pore size may be 1 to 100 nm.

In the above embodiment, the organic-illite composite powder may be prepared by adding illite powder to a polyvinylpyrrolidone solution with a concentration of 1 to 100 mM and stirring, wherein the weight average of the polyvinylpyrrolidone is The molecular weight may be 1,000 to 100,000 g/mol.

In addition, another aspect of the present invention includes the steps of a) grinding illite to produce illite powder; and b) adding the illite powder to a polyvinylpyrrolidone solution and stirring it. It relates to a method of producing an organic-illite composite powder, including.

In another aspect, the concentration of the polyvinylpyrrolidone solution may be 1 to 100 mM.

In another aspect, the weight average molecular weight of polyvinylpyrrolidone may be 1,000 to 100,000 g/mol.

In another aspect, the manufacturing method may further include treating the illite powder with acid after step a).

In another aspect, the acid may have an acid dissociation equilibrium constant of -3 to 1 pKa.

In another aspect, the acid treatment may be performed at a temperature of 80 to 150°C for 1 to 24 hours.

In addition, another aspect of the present invention relates to a cosmetic composition containing the above-described organic-illite composite powder.

When using the organic-illite composite powder according to the present invention as a powder material for a cosmetic composition, color control can be possible without using coloring pigments, excellent spreadability and biological stability can be secured, and the organic-illite composite powder can be used as a powder material for cosmetic compositions. When used as a carrier to carry functional substances, it has the advantage of achieving various effects such as whitening, wrinkle improvement, or moisturizing.

Figure 1 is an actual photograph comparing the color of illite powder according to experimental conditions before and after acid treatment.
Figure 2 is a field emission scanning electron microscopy (FE-SEM) image measuring the surface shape of illite according to grinding test conditions.
Figure 3 shows the results of PSA (Particle size analyzer) measuring the size of illite powder according to grinding test conditions.
Figure 4 is an isotherm graph of nitrogen adsorption of illite according to experimental conditions before and after acid treatment.
Figure 5 shows PSA results measuring the particle size of organic-illite composite powder according to PVP coating to improve spreadability.
Figure 6 is a nitrogen adsorption isotherm graph of organic-illite composite powder according to PVP coating to improve spreadability.
Figure 7 is a FE-SEM image of the organic-illite composite powder before (a) and (b) after PVP coating to improve spreadability.
Figure 8 shows FT-IR data of illite, PVP, and organic-illite composite powder.
Figure 9 is a graph showing the change in skin moisture measurement values before and after product application.
Figure 10 shows the results of evaluating antioxidant capacity according to PVP@Illite concentration.
Figure 11 shows the cytotoxicity test results.

Hereinafter, the organic-illite composite powder according to the present invention, its manufacturing method, and the cosmetic composition containing the same will be described in detail. The drawings introduced below are provided as examples so that the idea of the present invention can be sufficiently conveyed to those skilled in the art. Accordingly, the present invention is not limited to the drawings presented below and may be embodied in other forms, and the drawings presented below may be exaggerated to clarify the spirit of the present invention. At this time, if there is no other definition in the technical and scientific terms used, they have the meaning commonly understood by those skilled in the art to which this invention pertains, and the gist of the present invention is summarized in the following description and attached drawings. Descriptions of known functions and configurations that may be unnecessarily obscure are omitted.

One aspect of the present invention is illite powder; and polyvinylpyrrolidone coated on the surface of the illite powder. When the organic-illite composite powder according to the present invention is used as a powder material for a cosmetic composition, a coloring pigment is produced. Color control can be possible without the use of There is an advantage to being able to do it.

In one example of the present invention, the illite powder is obtained by pulverizing the illite raw material several times to finer particles, and the average particle diameter may be 0.1 to 20 ㎛, more preferably 0.5 to 10 ㎛, more preferably 1 to 5 ㎛. It may be ㎛. In this range, it has excellent dispersibility and can provide a soft and smooth texture when added to cosmetics.

In addition, the specific surface area of the illite powder may be 1 to 100 m2/g, the pore volume may be 0.01 to 0.1 cm3/g, and the average pore size may be 1 to 100 nm, but the grinding of the illite powder The particle characteristics of illite powder can be controlled depending on the presence or absence of a post-acid treatment process. As an example, in the case of acid-treated illite powder, the specific surface area may be 10 to 100 m2/g, the pore volume may be 0.03 to 0.1 cm3/g, the average pore size may be 1 to 20 nm, and further. Specifically, for example, the specific surface area may be 30 to 50 m2/g, the pore volume may be 0.03 to 0.08 cm3/g, and the average pore size may be 3 to 10 nm. As the acid-treated illite powder has a larger specific surface area and pore volume, it is advantageous for carrying functional substances when used as a carrier, and can provide various effects such as whitening, wrinkle improvement, or moisturizing. As another example, in the case of illite powder that has not been treated with acid, the specific surface area may be 1 to 10 m2/g, the pore volume may be 0.01 to 0.03 cm3/g, and the average pore size may be 25 to 100 nm. , more specifically, for example, the specific surface area may be 1 to 5 m2/g, the pore volume may be 0.01 to 0.025 cm3/g, and the average pore size may be 30 to 50 nm.

In addition, the color of the organic-illite composite powder can be adjusted differently depending on whether an acid treatment process is performed after pulverizing the illite powder. As shown in Figure 1, the illite powder before acid treatment is somewhat darker in color and has a color similar to that of foundation No. 23 when compared to cosmetics, while the acid-treated illite powder becomes brighter in color and has a color similar to foundation number 13. can be shown.

On the other hand, the organic-illite composite powder according to an example of the present invention is illite powder in a polyvinylpyrrolidone solution at a concentration of 1 to 100mM, more preferably 3 to 50mM, more preferably 5 to 20mM. It may be manufactured by adding and stirring. In this range, polyvinylpyrrolidone can be effectively coated on the surface of illite powder.

At this time, polyvinylpyrrolidone is a non-ionic polymer that is biocompatible and non-toxic. By coating polyvinylpyrrolidone on the surface of illite powder, the spreadability and spreadability of the organic-illite composite powder can be improved. . Preferably, the weight average molecular weight of the polyvinylpyrrolidone may be 1,000 to 100,000 g/mol, more preferably 3,000 to 50,000 g/mol, and even more preferably 5,000 to 30,000 g/mol. Within this range, the surface of ELIVE powder can be well coated, and the desired level of spreadability and spreadability can be secured.

In addition, another aspect of the present invention relates to a method for producing the above-described organic-illite composite powder, specifically comprising: a) pulverizing illite to produce illite powder; and b) adding the illite powder to the polyvinylpyrrolidone solution and stirring it.

As a pretreatment, the mined illite exists as soil in a natural state and contains various organic matter (insects, tree roots, fragments, etc.), so a sieve vibrator is used to remove this and equalize the particle size. The illite can be separated. Thereafter, the illite that has been sieved to a thickness of 400 to 500 ㎛ is heat treated at 500 to 800° C. to completely remove remaining organic substances.

Afterwards, the illite can be pulverized and powdered to a desired size. The equipment used is a disk mill and a jet mill. In the case of the disk mill, the grinding method is performed in a dry state, and like a typical millstone, two pieces of zirconia ceramic disks are rotated. It is designed to crush samples, and in the case of a jet mill, it is pulverized dry and uses the kinetic energy of the fluid to supply materials into a jet stream generated by compressed air or water vapor ejected from a high-pressure nozzle to prevent collisions between particles or with walls. It has a principle of crushing.

First, the illite is first pulverized to a size of 100 to 250 ㎛ using disk mill equipment, and then secondary pulverized to have an average particle size of 0.1 to 20 ㎛ using a jet mill. , primary crushing and secondary crushing can be performed more than once.

Next, finely ground illite powder can be added to the polyvinylpyrrolidone solution and stirred to coat the surface of the illite powder with polyvinylpyrrolidone.

More specifically, the concentration of the polyvinylpyrrolidone solution may be 1 to 100mM, more preferably 3 to 50mM, and even more preferably 5 to 20mM. In this range, polyvinylpyrrolidone can be effectively coated on the surface of illite powder.

Solvents for the polyvinylpyrrolidone solution include alcohol-based solvents such as ethanol, isopropyl alcohol, butyl alcohol, 2-methoxyethanol, and 2-butoxyethanol; Ketone-based solvents such as acetone; Acetate-based solvents such as ethyl acetate and butyl acetate; and amine-based solvents such as N-methylpyrrolidone, pyrimidine, and pyrrolidine; It may be any one or two or more mixed solvents selected from the group consisting of, etc.

At this time, the stirring temperature may be room temperature, about 15 to 35 ℃, and the stirring time may be 24 to 60 hours, but it is not necessarily limited thereto, and polyvinylpyrrolidone can be sufficiently coated on the surface of the illite powder. It is sufficient if the conditions exist.

In addition, as described above, the polyvinylpyrrolidone may have a weight average molecular weight of 1,000 to 100,000 g/mol, more preferably 3,000 to 50,000 g/mol, and even more preferably 5,000 to 30,000 g/mol. It may have a weight average molecular weight. Within this range, the surface of ELIVE powder can be well coated, and the desired level of spreadability and spreadability can be secured.

Meanwhile, as described above, the method for producing an organic-illite composite powder according to an example of the present invention further includes the step of treating the illite powder with acid after step a) to control the particle characteristics and color of the illite powder. can do.

At this time, the particle characteristics of the illite powder may vary depending on the type of acid used. An acid suitable for the present invention may have an acid dissociation equilibrium constant of -3 to 1 pKa, specifically, for example, nitric acid (-1.3 pKa ) can be. The concentration may be 0.1 to 5 M, and more preferably 0.5 to 3 M. In this range, illite powder with a larger specific surface area can be obtained.

In addition, the acid treatment may be performed at a temperature of 80 to 150°C for 1 to 24 hours, and more preferably at a temperature of 100 to 130°C for 3 to 12 hours. Under these conditions, the illite powder is sufficiently treated with acid to obtain illite powder having a specific surface area of 10 to 100 m2/g, a pore volume of 0.03 to 0.1 cm3/g, and an average pore size of 1 to 20 nm. Illite powder having a specific surface area of 30 to 50 m2/g, a pore volume of 0.03 to 0.08 cm3/g, and an average pore size of 3 to 10 nm can be obtained.

Finally, another aspect of the present invention relates to a cosmetic composition containing the above-described organic-illite composite powder. At this time, the cosmetic composition can use the organic-illite complex powder as an extender and color pigment, and can be used, for example, in color cosmetics such as powder foundation, liquid foundation, cushion foundation, or sunscreen. Alternatively, when functional substances are carried using illite powder as a carrier, various effects such as whitening, wrinkle improvement, or moisturizing can be achieved, and it can be used in skin care cosmetics such as skin, lotion, essence, cream, or pack.

At this time, the organic-illite composite powder may be added in an amount of 1 to 20% by weight of the total weight of the cosmetic composition, but is not necessarily limited thereto, and the content may vary depending on the use of the cosmetic composition, and other components They may also be composed of ingredients commonly used in the industry depending on the purpose of the cosmetic composition.

Hereinafter, the organic-illite composite powder according to the present invention, its manufacturing method, and the cosmetic composition containing the same will be described in more detail through examples. However, the following examples are only a reference for explaining the present invention in detail, and the present invention is not limited thereto, and may be implemented in various forms.

Additionally, unless otherwise defined, all technical and scientific terms have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention pertains. The terminology used in the description herein is merely to effectively describe particular embodiments and is not intended to limit the invention. Additionally, the unit of additives not specifically described in the specification may be weight percent.

1. Preparation of illite powder

Illite materials were mined in a new mining area owned by Yeongdong-gun, North Chungcheong Province. After physically optimizing grinding conditions for processing and purification, an acid treatment process was introduced to improve specific surface area and control color.

First, the illite was sieved using a sieve shaker to remove organic matter, the particle size was uniformized to about 425 ㎛, and then heat treated (calcination) in an electric furnace at 700°C for 3 hours.

Next, 2 kg of illite is first pulverized to 150-200 ㎛ using a disk mill equipment while maintaining a speed of 400 rpm, and then ground to an average of 3 ㎛ using a jet mill equipment. It was secondaryly pulverized twice to have the following size. At this time, it was pulverized once at a speed of 4,000 rpm and twice at a speed of 2,000 rpm.

The size of the pulverized particles was confirmed using FE-SEM (Field emission scanning electron microscopy) and PSA (Particle size analyzer).

As shown in Figures 2 (FE-SEM) and 3 (PSA), it can be confirmed that the illite was finely powdered through secondary grinding, and this was quantified and shown in Table 1 below.

1st crushing
(D-1) Secondary crushing - 1 time
(J-1_1) Secondary crushing - 2 times
(J-1_2) Average particle diameter (㎛) 190.645 4.5293 2.8221

Next, for the acid treatment process, 200 ml of 1 M nitric acid and 20 g of illite powder were added to a round flask and stirred at 120°C for 6 hours. After the experiment was completed, filtration and washing were repeated more than 5 times to remove the acid and obtain the material, and then dried at room temperature for 2 days.

The specific surface area of illite powder before and after acid treatment was measured with a specific surface area meter, and the results are shown in Figure 4 and Table 2. As a result, the specific surface area of the illite powder (J-1_2) before acid treatment was 2.2 ㎡/g, and the specific surface area of the illite powder (HJ-I_2) after acid treatment was 44.97 ㎡/g, which was approximately 22 times greater through acid treatment. It was confirmed that it had a high specific surface area.

specific surface area
(㎡/g) pore volume
(㎤/g) average pore size
(㎚) Before acid treatment (J-I_2) 2.2101 0.0181 32.822 After acid treatment (HJ-I_2) 44.4273 0.0527 4.7475

In addition, the RGB values of illite powder before acid treatment (J-1_2) and illite powder after acid treatment (HJ-I_2) are R:239 G:227 B:215 and R:229 G:203 B:176, respectively. As shown in Figure 1, when comparing the RGB values of commercially available powder cosmetics, foundations No. 23 and 13 can be compared.

2. Production of organic-illite composite powder

Surface modification was performed to improve the applicability and spreadability of illite powder (HJ-I_2).

50 g of illite powder (HJ-I_2) was added to a 10 mM polyvinylpyrrolidone solution (in ethanol, PVP weight average molecular weight 10,000 g/mol) and complexed at a speed of 480 rpm for 48 hours at room temperature. , filtration and washing were repeated more than 5 times and dried at room temperature for 2 days to obtain an organic-illite composite powder.

The size of the organic-illite composite powder was 2.93 ㎛, which was not much different than before polyvinylpyrrolidone (PVP) coating (Figure 5), but in the case of specific surface area measurement, the specific surface area was reduced to 0.24 ㎡/g due to coating. This was confirmed (Figure 6). These results appear to be the result of a decrease in the specific surface area of illite as the polymer PVP is coated. In addition, in FE-SEM measured to confirm the shape of the particles, it was observed that the surface was smooth compared to the surface roughness of illite before coating (Figure 7, a - before coating, b - after coating).

To improve spreadability, FT-IR analysis before and after PVP coating showed that for illite powder, Si-O-Al 540 cm ^-1 , Al-OH 460 cm ^-1 , Si-O 1100 cm ^-1 , -OH 3400 cm ^-1. Each peak was confirmed at ¹ . In the case of organic-illite composite powder, -CH ₂ bending vibration peak and OH vibration peak at 1400 cm ^-1 , C=O vibration at 1660 cm ^-1 , and OH vibration peak at 3400 cm ^-1 were confirmed by PVP. , it was found that the coating was well done (Figure 8).

3. Moisturizing performance evaluation

First, a test product in which 15 g of illite powder coated with PVP (PVP@HJ-I_2) was mixed with 85 g of glycerin, and 15 g of illite powder not coated with PVP (HJ-I_2) was mixed with 85 g of glycerin. Control products were prepared separately.

Using the above test and control products, the moisturizing effect was evaluated by measuring moisture in 20 healthy adult women aged 20 to 55 years. Moisture was measured on the forearm using a Corneometer (Skin O Mat, Cosmomed Medical Beauty GmbH, Germany), and the average value was calculated using three values. The test product was applied to the selected test area (1.5 cm At each measurement, the test area was lightly wiped with kimwipes and measured. Corneometer consists of measuring the capacitance of current transmitted through a probe in contact with the skin. Moisture content and electrostatic load capacity are proportional to each other, so the higher the moisture, the higher the measured value, and the measurement coefficient is Arbitrary unit (A.U.).

The amount of moisture change was calculated according to the formula below, and the results are shown in Table 3 below.

Moisture change (%) = (│Measured value after product application - Measured value before product application│/Measured value before product application) × 100

(A.U.) test product control product Before application 30 minutes after application Before application 30 minutes after application One 38.4 55.7 38.3 53.6 2 52.4 84.2 52.7 81.2 3 41.2 58.5 41.4 56.3 4 49.3 62.6 49.2 61.6 5 40.6 58.5 40.6 52.3 6 42.3 59.1 42.6 54.1 7 34.5 63.2 34.5 56.2 8 37.3 59.6 37.5 55.8 9 29.6 35.2 29.6 43.2 10 35.5 49.4 35.2 43.6 11 33.5 59.8 33.8 56.4 12 41.6 63.6 41.3 57.5 13 37.8 53.3 37.4 48.7 14 37.3 62.6 37.6 53.5 15 40.1 57.6 40.6 54.8 16 31.4 54.2 31.3 54.6 17 47.6 66.4 47.5 64.8 18 44.1 68.8 44.6 61.6 19 46.5 74.7 46.6 69.2 20 43.8 59.7 43.2 53.4 average 40.24 60.34 40.28 56.62 Standard Deviation 5.97 9.70 6.00 8.44 moisture change - 49.95% - 40.58%

Referring to Table 3 and Figure 9, it was confirmed that the moisture content of the application area of the test product and the control product was statistically significantly improved 30 minutes after application of the product compared to before application of the product.

Compared to the area where the test product was applied, the area where the test product was applied showed a statistically significant immediate moisturizing improvement effect 30 minutes after application, and an immediate moisturizing improvement effect of 49.95% 30 minutes after application compared to before using the product. indicated.

In addition, there were no adverse reactions to the test product such as erythema, edema, scaling, itching, stinging, burning, stiffness, or tingling. The presence or absence of other adverse reactions was closely observed, and no adverse skin events occurred due to the test product during the test period.

4. Antioxidant performance evaluation

The DPPH (2,2-Diphenyl-1-Picrylhydrazyl) solution used in the antioxidant experiment was dissolved in 50% by volume methanol (in deionized water) to make 10 mM. A solution prepared at 10 mM was diluted and used at 200 μM.

PVP-coated illite powder (PVP@Illite, HJ-I_2) and L-ascorbic acid were dispensed at 100 ㎕ each in a 96 well plate. 100 ㎕ of DPPH was added to the dispensed area. The blank solution was prepared by adding 100 ㎕ of methanol to 100 ㎕ of PVP@Illite, and the control solution was prepared by adding 100 ㎕ of DPPH solution to 100 ㎕ of solvent. After reacting for 30 minutes in an incubator at 37°C, the reaction was measured at 520 nm using an ELISA reader.

Antioxidant activity (DPPH scavenging activity, %) was calculated according to the following equation, and the results are shown in Table 4 below.

Antioxidant capacity (%) = 1-(A _s - A _b )/A _c × 100

(A _s : Absorbance of sample solution, A _b : Absorbance of blank solution, A _c : Absorbance of control solution)

Sample concentration (ppm) Antioxidant ability (%) One 100 1.60 2 200 11.98 3 500 15.25 4 1000 18.58 5 2000 24.17

Referring to Table 4 and Figure 10, as a result of measuring the antioxidant power, when PVP@Illite was used as a stock solution and diluted to 100 ppm, 200 ppm, 1000 ppm, and 2000 ppm, the antioxidant power was observed at a concentration of 100 ppm. However, it began to show activity above 200 ppm, and it was confirmed that the highest antioxidant activity appeared at a concentration of 2000 ppm.

5. Safety evaluation (cytotoxicity, genotoxicity)

1) Cytotoxicity test (MTT assay):

As the concentration of PVP-coated illite powder (PVP@Illite, HJ-I_2) increased, the effect on L929 cells was evaluated. The absorbance of the control group, which was untreated with the test substance, and the treated group were measured and compared. To ensure the accuracy of the test, the results were repeated three times and the results were treated as average values.

As a result of the test, as shown in Figure 11, Illite showed a cell viability of 108% at a high concentration of 50 mg/ml, and at concentrations lower than that, it showed a cell viability of over 90%, confirming that it had no cytotoxicity.

2) Genotoxicity test (AMES test):

This test was conducted in accordance with the Ministry of Food and Drug Safety's toxicity test standards (Ministry of Food and Drug Safety, 2014), and the strains used were histidine-auxotrophic strains (TA98, TA100, TA1535, TA1537) of Salmonella typhimurium and tryptophan of Escherichia coli . A total of 5 strains were used as the auxotrophic strain (WP2uvrA).

As a result of the test, no other abnormalities were observed on all plates during colony counting, and no colonies due to microbial contamination were found on the plates to confirm the sterility of the test substance and S9 mixture. The results of investigating the number of revertant colonies for five strains are presented in Tables 5 and 6. The viable cell count of the strains used in the experiment was 1.0~1.2×10 ⁹ /ml, and according to the preliminary experiment results, all samples were performed at the highest concentration of 5,000 ㎍/ml. It was found that there was no significant difference in the number of revertant colonies compared to the negative control group in the test concentration range for both application and non-application of metabolic activation system. Mutation was determined to be positive if the number of revertant colonies was twice that of the negative control group, so it was found that the test concentration of Illite did not cause revertant mutations.

Test
strain Treated
chemical With S9 mixture Without S9 mixture Dose (㎍/㎖) cloony number/plate Dose (㎍/㎖) cloony number/plate TA98 illite Negative control 32±2 Negative control 18±5 312.5 30±7 312.5 17±1 625 28±2 625 18±10 1250 32±8 1250 18±9 2500 33±10 2500 18±4 5000 31±3 5000 16±2 TA100 illite Negative control 190±13 Negative control 193±10 312.5 181±5 312.5 197±6 625 200±19 625 186±29 1250 198±6 1250 186±15 2500 180±5 2500 186±18 5000 185±15 5000 195±15 TA1535 illite Negative control 11±3 Negative control 20±4 312.5 13±2 312.5 22±5 625 12±3 625 17±3 1250 16±4 1250 18±3 2500 11±4 2500 18±5 5000 11±4 5000 18±8 TA1537 illite Negative control 12±2 Negative control 14±1 312.5 14±5 312.5 15±2 625 11±3 625 11±5 1250 9±1 1250 13±3 2500 10±3 2500 11±5 5000 13±1 5000 8±2 Positive control TA98 2-AA 0.5 72±12 TA100 1.0 154±12 TA1535 2 17±2 TA1537 2 10±3 TA98 4NQQ 0.5 68±15 TA100 4NQQ 0.5 400±14 TA1535 SA 0.5 86±12 TA1537 9-AA 50 33±2

(Reverse mutation assay using Salmonella typhimurium treated with illite)

Test
strain Treated
chemical With S9 mixture Without S9 mixture Dose (㎍/㎖) cloony number/plate Dose (㎍/㎖) cloony number/plate WP2uvrA illite Negative control 57±1 Negative control 78±4 312.5 51±2 312.5 81±11 625 86±8 625 79±7 1250 87±11 1250 85±3 2500 85±5 2500 72±7 5000 74±7 5000 55±8 Positive control WP2uvrA 2-AA 6.0 187±12 4NQQ 0.5 114±6

(Reverse mutation assay using E.coli treated with illite)

3) Acute oral toxicity test (requested to external testing agency):

When PVP-coated illite powder (PVP@Illite, HJ-I_2) was orally administered to experimental female mice, the potential toxicity of illite was evaluated.

After weighing the PVP-coated illite powder (PVP@Illite, HJ-I_2), 30 mg/mL (1st, 2nd step) and 200 mg/mL (3rd, 4th step) were added to sterilized distilled water (water for injection) as an excipient. ) was prepared and used at a certain concentration.

Administration was conducted to all animals once daily for up to 14 days after administration of the test substance. The administration method was to inject the test substance preparation into the stomach using a syringe equipped with a sonde for oral administration to experimental animals that had fasted for about 18 hours. It was administered compulsorily once, and the doses are shown in Table 7 below.

army animal number Marie Sue Dosage
(㎎/㎏ BW) Dosage amount
(㎖/kg BW) Route of administration G1 2101-2103 3 300 10 oral- G2 2201-2203 3 300 G3 2301-2303 3 2000 G4 2401-2403 3 2000 ※ G1: 1st step, G2: 2nd step, G3: 3rd step, G4: 4th step, B.W. : Body weight

As a result, no abnormal findings or dead animals were observed during the experiment period, and no changes in body weight were observed due to administration of the test substance.

From the above results, in the single-dose toxicity test for rats - toxicity grading method, Illite is classified as Category 5 or Category 5 according to the internationally recognized and harmonized classification system for chemical substances and mixtures (GHS). It was classified as Unclassified.

Although the present invention has been described through the above-described specific details and limited examples, these are provided only to facilitate a more general understanding of the present invention, and the present invention is not limited to the above-mentioned examples, and the present invention belongs to Those skilled in the art can make various modifications and variations from this description.

Accordingly, the spirit of the present invention should not be limited to the described embodiments, and the scope of the patent claims described later as well as all things that are equivalent or equivalent to the scope of this patent claim shall fall within the scope of the spirit of the present invention. .

Claims (14)

illite powder; And polyvinylpyrrolidone coated on the surface of the illite powder; an organic-illite composite powder comprising,
The illite powder has an average particle diameter of 0.1 to 20 ㎛, a specific surface area of 1 to 100 m2/g, and an average pore size of 1 to 100 nm,
The polyvinylpyrrolidone has a weight average molecular weight of 1,000 to 100,000 g/mol, an organic-illite composite powder. delete delete According to clause 1,
The pore volume of the illite powder is 0.01 to 0.1 cm3/g, an organic-illite composite powder. delete According to clause 1,
The organic-illite composite powder is prepared by adding illite powder to a polyvinylpyrrolidone solution with a concentration of 1 to 100 mM and stirring it. delete a) grinding illite to produce illite powder; and
b) adding the illite powder to a polyvinylpyrrolidone solution and stirring it,
The illite powder has an average particle diameter of 0.1 to 20 ㎛, a specific surface area of 1 to 100 m2/g, and an average pore size of 1 to 100 nm,
A method for producing an organic-illite composite powder wherein the polyvinylpyrrolidone has a weight average molecular weight of 1,000 to 100,000 g/mol. According to clause 8,
A method for producing an organic-illite composite powder, wherein the concentration of the polyvinylpyrrolidone solution is 1 to 100 mM. delete According to clause 8,
The manufacturing method further includes the step of treating the illite powder with acid after step a). According to claim 11,
A method for producing an organic-illite composite powder, wherein the acid has an acid dissociation equilibrium constant of -3 to 1 pKa. According to claim 11,
A method for producing an organic-illite composite powder, wherein the acid treatment is performed at a temperature of 80 to 150° C. for 1 to 24 hours. A cosmetic composition comprising the organic-illite composite powder of any one of claims 1, 4, and 6.