KR100593706B1 - W/S type hydrous cosmetic products with no preservatives and their manufacturing methods by using silicon crosspolymer combinations. - Google Patents

Abstract

Preservatives commonly used in cosmetics are added to prevent the deterioration of the product and to maintain its purity during its use or preservation, and to protect the cosmetics from microorganisms such as bacteria and fungi, such as parabens, imidazolidinyl ureas, and diazolyses. Chemical preservatives, such as dinil urea and phenoxyethanol, are used. However, these chemical preservatives are inevitably used, although the side effects of causing toxicity, skin irritation, allergy, etc. are larger than other cosmetic ingredients. The present invention relates to a W / S type water-based cosmetic composition having a preservative effect without adding a preservative by using a silicone crosslinked polymer combination having a low irritation and safe skin. That is, it is a cosmetic composition that can contain more water phases by using silicone cross-linked polymers as a silicone-based functional cosmetic composition in combination, and is safe from microorganisms such as bacteria or mold without preservatives, and can be preserved for a long time. In addition, the silicone crosslinked polymers used and the cosmetic composition of the present invention did not respond to skin irritation patch experiments in humans and proved to be safe for human body. The W / S type water-based cosmetic composition is dimethicone / vinyl dimethicone crosspolymer (Dimethicone / vinyl dimethicone crosspolymer), Dimethicone copolyol crosspolymer (Lamethyone copolyol crosspolymer), Lauryl dimethicone / copolyol crosspolymer (Lauryl dimethicone / copolyol crosspolymer), decamethyl cyclopentasiloxane, and glyceryl polyacrylate dimethicone copolyol.

Antiseptic, Preservative, Preservative-free, Sensitive Skin, Skin Irritation, Skin Toxicity, Allergy, Functional Cosmetic, Silicone, Silicone Cross-linked Polymer, Atopy Skin, Bacteria, Mold, Preservative Test, W / S Type

Description

W / S type hydrous cosmetic composition with no preservatives using silicone crosslinked polymer combination and its manufacturing method {W / S type hydrous cosmetic products with no preservatives and their manufacturing methods by using silicon crosspolymer combinations.}

Figure 1a ~ g] is a photograph of the antiseptic results of the W / S type aqueous cosmetic composition prepared according to the present invention with respect to bacteria and fungi and other composition compositions. Eye A is a cosmetic composition according to the present invention, Eye B is a comparative example 7 in [Table 5] below Eye C is a comparative example 1 in [Table 4] below, Eye D is a comparative example 6 in [Table 3] The photograph of the preservation test result by the composition of the. The photographic order of the drawings is listed by the date of preservative inspection.

It is antiseptic to prevent the decay of animals and plants by the action of microorganisms, and the agent added for this purpose is a preservative. In cosmetics, preservatives are generally added to prevent the deterioration of the product and to maintain its purity during its use or preservation. To protect the cosmetics from microorganisms such as bacteria and fungi, paraben, imidazolidinyl urea, diazoly Most of chemical preservatives such as dinil urea and phenoxyethanol are used. However, these chemical preservatives have higher side effects such as toxicity, skin irritation, and allergy than other cosmetic ingredients, but there are few alternatives for preservation in the present technology, which is inevitably used. The present invention protects the cosmetics from microorganisms such as bacteria and fungi without using such preservatives, and can be stored for a long time and has a low skin irritation and is a W / S type cosmetic composition that can be safely used for acne, sensitivity, and atopic diseases. .

Human skin is affected by many factors that exist in everyday life. The skin around the eyes is one of the thinnest parts of human skin, and the amount of moisture and fat is less than that of other parts, and natural sebaceous membrane is not formed. In addition, people with atopic dermatitis are sensitive to almost every body, such as skin folds, face, neck, arms and legs. When using a cosmetic composition added with chemical preservatives to such a sensitive skin and around the eyes, the cosmetic composition applied to inflammation due to acne, skin irritation, allergies, toxicity may be caused. The water-containing products are water-containing formulations that have excellent moisturizing effect and have a good feeling of use, and thus are widely used in cosmetic formulations. Using chemical preservatives to prevent the invasion of microorganisms can cause skin problems, allergies and skin irritation. Common chemical preservatives such as phenoxyethanol, imidazolidinyl urea, and parabens are reported to cause irritation and inflammation on the skin, and when they get into the eyes. The present invention is a silicone-based functional cosmetic composition using a variety of silicone cross-linked polymers in combination to function more water and protect the cosmetics from microorganisms such as bacteria and fungi without adding a preservative, and a safe cosmetic composition that can be stored for a long time to be.

The present invention is characterized by the W / S-type water-based cosmetic composition using a silicone crosslinked polymer combination that does not add a preservative in order to not irritate sensitive skin, skin around the eyes, acne skin and the like. The W / S type water-based cosmetic composition is 1 to 20% by weight of dimethicone / vinyl dimethicone crosspolymer, 1 to 20% by weight of dimethicone copolyol crosspolymer, lauryl dimethicone 1-20% by weight of lauryl dimethicone / copolyol crosspolymer, 0.1-5% by weight of decamethyl cyclopentasiloxane, Glyceryl polyacrylate dimethicone copolyol 1 It is characterized by containing ~ 20% by weight.

Example 1

It was prepared according to the composition shown in Table 1 below, the preparation method is as follows. The component B phase is well stirred beforehand. Mix the components of phase A and warm them to 85 ℃ in a water bath in a water bath. The Agi mixer is used to add a small amount of phase A to phase B at 2000 rpm for 15 minutes to produce a highly viscous W / S type aqueous cosmetic composition.

Examples 2-6

It was prepared in the same manner as in Example 1, and its composition is shown in the following [Table 1].

Examples 7-12

It was prepared in the same manner as in Example 1, and its composition is shown in the following [Table 2].

Comparative Example 1

In order to compare with the case of the Example was prepared with a difference in the components of the Example.

A manufacturing method is the same as the manufacturing method of an Example. The component B phase is well stirred beforehand. Mix the components of phase A and warm them to 85 ℃ in a water bath in a water bath. The Agi mixer was used to add a small amount of phase A to phase B at a speed of 2000 rpm for 15 minutes to prepare a high viscosity W / S type cosmetic composition. The composition is shown in the following [Table 3].

Comparative Examples 2 to 6

It was prepared in the same manner as in Comparative Example 1 and its composition is shown in the following [Table 3].

Comparative Examples 7 to 8

It was prepared in the same manner as in Comparative Example 1 and its composition is shown in the following [Table 4].

Test Example

1) Antiseptic test

In order to evaluate the antiseptic ability against bacteria, 50 g of cosmetics of Examples 1 to 12 and Comparative Examples 1 to 8 were Escherichia coli, Pseudomonas aeruginosa, and Staphylococcus aurea. Mixed fungi such as Staphylococcus aureus, Enterobactor cloaca, were added and mixed at an initial concentration of 10 ⁶ / ml per sample. From 0, 1, 3, 7, 14, 21, 28, etc., from the date of measurement, the measurement and the number of bacteria shall be calculated according to the general viable cell counting method of the microbial contamination test method.

In order to evaluate the room buoyancy for fungal the Examples 1 to 12 and Comparative Examples 1 to 8 10 The mixed inoculum of Candida albicans (Candida albicans), Aspergillus and this (Aspergillus niger) in the cosmetic 50g of ⁵ / After adding and mixing to ml, it was kept for 5 weeks in a 25 ℃ incubator, and 0, 1, 3, 7, 14, 21, 28 days, etc., from the day of inoculation of the inoculated cells, and the hyphae Observe spore development.

Detailed preservative test methods are described below.

1. Reagent Preparation

1) Strain used for test

Bacteria-Escherichia coli (ATCC: 8739), Pseudomonas aeruginosa (ATCC: 99027), Staphylococcus aureus (ATCC: 6538),

Enterobactor cloaca (ATCC: 13047)

Fungi-Aspergillus niger (ATCC: 16404) Candida albicans (ATCC: 10231)

2. Preparation of fungi

1) Bacteria

① Dispense Tryptic soy broth 7ml into test tube and sterilize for 15 minutes at 121 ℃ in autoclave.

② Inoculate each strain stored in the liquid medium.

③ Vortex the test tube inoculated with the strain for about 3 seconds and incubate in 37 ℃ incubator for 16 ~ 24 hours.

④ After diluting so that the number of cultured bacteria solution to 10 ⁶ / ml, mix and prepare in sterile container.

2) Aspergillus niger (ATCC: 16404)

① Sterilize Sabouraud dextrose agar in autoclave at 121 ℃ for 15 minutes and pour into Peptri dish to harden.

② Incubate spores of Aspergillus niger in hardened Sabouraud dextrose agar in a single inoculation 25 ℃ incubator for 3-7 days.

③ Collect only the spores from the incubator and incubate them so that the number of spores is 10 ⁵ / ml.

3) Candida albicans (ATCC: 10231)

① After dispensing 7ml seeds of Sabouraud dextrose broth into test tube, sterilize at 121 ℃ for 15 minutes in autoclave.

② Inoculate each strain stored in the liquid medium.

③ Vortex the test tube inoculated with the strain for about 3 seconds and incubate in 25 ℃ incubator for 48 hours.

④ Dilute so that the number of cultured bacteria solution to 10 ⁵ / ml and mix with Aspergillus niger in a sterile container.

3. sterile water production

Mix 0.85% NaCl and 0.8% Tween 80 in purified water. Dispense 9 ml of the mixed solution into the test tube and place it in an autoclave to sterilize for 15 minutes at 121 ℃.

4. Device and Apparatus

Aseptic box, sterile pipette, Petri dish, medium: Tryptic Soy Agar, Sabouraud Dextrose Agar, alcohol lamp, sterile hard Erlenmeyer flask, sterile funnel, gauze, thermostat: 37 ± 2 ℃, 25 ± 1 ℃

5. Test method

1) Bacteria Antiseptic Test Method

Accurately weigh 49.5 g of the sample to be tested in a clean container with 70% alcohol swab, inoculate 0.5 g of the prepared bacterial solution into the sample, and mix homogeneously with a sterile rod.

Samples inoculated with bacteria were stored for 4 weeks in a 37 ° C incubator and tested for 0, 1, 3, 7, 14, 21, 28, etc. from the day of inoculation. The measurement and the number of bacteria are calculated according to the trial method.

2) Fungal Preservation Test Method

Accurately weigh 49.5 g of the sample to be tested in a clean container with 70% alcohol swab, inoculate 0.5 g of the prepared mixed microbial solution into the sample, and mix homogeneously with a sterile rod.

Samples inoculated with bacteria were stored in a 25 ± 1 ° C incubator for 5 weeks, and then, on the days of inoculation, 0, 1, 3, 7, 14, 21, 28 days, etc. Observe the mycelia and spores.

For samples estimated to have no abnormality after 60 days, the yeast cell count should be determined according to the fungal test method of microbial contamination test.

6. Judgment criteria

1) The emulsification of bacteria in the sample to be tested should be less than 99% of the initial inoculation after 4 weeks.

2) Preservation of the fungus of the sample to be tested should be free from odor or mycelia or spores on the surface after 60 days, and the number of remaining bacteria in yeast should be 90% or less of the initial inoculation.

The antiseptic test results of the cosmetic composition against bacteria are taken at intervals of 1, 3, 7, 14, 21, and 28 days from the date of inoculation of the bacteria, and the number of viable cells is measured and the number of bacteria is calculated according to the test method. The results are shown in the following [Table 5].

Antiseptic test result of the antiseptic composition of the cosmetic composition against the fungus 1g at 0, 1, 3, 7, 14, 21, 28 days intervals from the day of inoculation of the fungus spread on the medium, and the presence of odor at 7 days intervals And the presence of mycelia and spores on the surface of the sample and the results are shown in Table 6 below.

Unit: cfu / ml

TNTC: Too numerous to count

*-: No bad smell, hyphae and spores for 8 weeks

+: Fungus on the walls or lids within 4 weeks

++ Occurs within 4 weeks due to bad smell

+++: Odor and fungus on the entire surface within 4 weeks

As shown in the above table, among the Examples 1 to 12, Comparative Examples 1 to 6, and Comparative Examples 7 and 8, which did not perform any preservative treatment, the results of the antiseptic force test for bacteria showed the antiseptic treatment. In Comparative Examples 7, 8 and Examples 1 to 12 without antiseptic treatment, antiseptic force against bacteria was observed.

The results of the antiseptic test for fungi showed that Examples 1 to 12 without preservatives and Comparative Example 8 with two preservatives showed antiseptic ability against fungi, but Comparative Examples 1 to 6 and one type without preservatives. In Comparative Example 7 using the preservative of the fungal within 4 weeks of the off-flavor and the development of fungi.

Comparative Examples 1 to 6 were prepared by excluding three compositions from the same prescription as Examples 1 to 12. In Comparative Examples 1 to 6, which did not add a preservative, the preservative effect was not shown, and thus, as shown in the above table, dimethicone / vinyl dimethicone crosspolymer and dimethicone copolyol crosspolymer. crosspolymer), Lauryl dimethicone / copolyol crosspolymer, Decamethyl cyclopentasiloxane, Glyceryl polyacrylate dimethicone copolyol (Glyceryl polyacrylate dimethicone copolyol) It can be seen that the complex combination of polymers has an antiseptic effect on bacteria and fungi.

2) skin irritation test

The skin irritation test was performed on the composition of this invention. The skin irritation test is a test for evaluating the potential of contact dermatitis for the cosmetic composition to ensure the safety of the cosmetic composition and to minimize skin side effects.

1. Test substance preparation

Distilled water, petrolatum, imidazolidinyl urea was tested as a control group of the present invention W / S type hydrous cosmetic composition and composition raw materials.

Water and petrolatum are applied to the skin as it is, while imidazolidinyl urea is 0.3% dissolved in water and applied to the skin. The present invention W / S type hydrous cosmetic composition is also applied to the skin as it is. Dimethicone / vinyl dimethicone crosspolymer, Dimethicone copolyol crosspolymer, Lauryl dimethicone / copolyol crosspolymer, Decamer methyl cyclopentasiloxane Decamethyl cyclopentasiloxane is applied to the skin as it is. Glyceryl polyacrylate dimethicone copolyol is dissolved in 15% petroleum jelly and applied to the skin.

2. Test subject

20 (female: 10, male: 10) test subjects included 3 sensitive skin

3. Site and Period of Test Application

It was attached to the inner side of the upper arm of both arms of the application part for 30 hours.

4. Sample application amount

Make sure that the filter paper on the finn chamber is sufficiently wetted, but the sample is not extracted. (If the Finn chamber volume is 25µl, add 15-18µl.)

5. Judgment of the reaction

Remove the patch after blocking patch for 30 hours, and observe the reaction after 1 hour. Then, observe again 48 hours after the test application.

As shown in the results of [Table 7] below, skin irritation test did not show skin irritation in the distilled water and petrolatum control. In addition, the present invention W / S type water-containing cosmetic composition also did not appear skin irritation. Dimethicone / vinyl dimethicone crosspolymer (Dimethicone / vinyl dimethicone crosspolymer), Dimethicone copolyol crosspolymer, Lauryl dimethicone / copolyol crosspolymer contained in the W / S type water-based cosmetic composition of the present invention Dimethicone / copolyol crosspolymer, Decamethyl cyclopentasiloxane and Glyceryl polyacrylate dimethicone copolyol in 15% vaselin did not show any skin irritation. For the commonly used imidazolidinyl urea, a weak positive response was seen in 3 out of 10 people. This skin irritation test result shows that the present invention W / S type water-containing cosmetic composition and the cosmetic composition raw material do not cause skin irritation.

As described in detail above, the W / S type water-containing cosmetic composition using the silicone cross-linked polymer combination of the present invention enables to protect the cosmetic composition from microorganisms such as bacteria and fungi without long-term chemical preservatives and to preserve it for a long time. As a result of the skin irritation test, it was confirmed that the cosmetic composition containing the preservative was likely to cause irritation to the skin, but the composition according to the present invention was confirmed to have little possibility of causing irritation. Therefore, the present invention overcomes the limitations of functional cosmetics, which have weaknesses to bacteria despite excellent moisturizing power and usability, and thus, manufacture of safe cosmetics without adding chemical preservatives that cause human toxicity, skin irritation, and allergies. Has become possible.

Claims (3)

Dimethicone / vinyl dimethicone crosspolymer 1 ~ 20 wt%, Dimethicone copolyol crosspolymer 1 ~ 20 in preparing W / S type water-based cosmetic composition using silicone crosslinked polymer % By weight, 1-20% by weight of Lauryl dimethicone / copolyol crosspolymer, 0.1-5% by weight of decamethyl cyclopentasiloxane, glyceryl polyacrylate dimethicone copolyol ( Glyceryl polyacrylate dimethicone copolyol) W / S type aqueous cosmetic composition, characterized in that it contains 1 to 20% by weight delete Dimethicone / vinyl dimethicone crosspolymer 1 ~ 20 wt%, Dimethicone copolyol crosspolymer 1 ~ 20 to make W / S type water-based cosmetic composition using silicone crosslinked polymer % By weight, 1-20% by weight of Lauryl dimethicone / copolyol crosspolymer, 0.1-5% by weight of Decamethyl cyclopentasiloxane, glyceryl polyacrylate dimethicone copolyol ( Glyceryl polyacrylate dimethicone copolyol) 1 to 20% by weight and the oil phase containing the silicone cross-linked polymer was uniformly stirred, and then the components of the aqueous phase were mixed, and a small amount of the aqueous phase was added to the gradually stirred oil phase using an Agi mixer. Cosmetic process characterized in that the manufacturing process of high W / S type water-based cosmetic composition Preparation method of water

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