KR20100090533A - Method of extracting for sea silt extract and whitening functional cosmetic composition containing the extract - Google Patents

Abstract

PURPOSE: A cosmetic composition for skin whitening containing Boryung mud extract is provided to maximize whitening effect and mud efficacy. CONSTITUTION: A method for manufacturing Boryung mud extract comprises: a step of mixing the mud and purified water in a weight ratio of 1:5 and stirring for 40-80 minutes; a step of removing supernatant after placing and repeating above steps; a step of mixing mud and purified water in a weight ratio of 1:5 and stirring for 40-60 minutes at room temperature; a step of maintaining for 12-20 hours in a refrigerator to remove salt; a step of mixing mud and purified water in a weight ratio of 1:2 and stirring for 40-60 minutes; a step of placing in the refrigerator for 40-60 minutes; a step of maintaining in the refrigerator for 12-20 hours; a step of filtering; a step of performing preservation treatment using 1,3-butyleneglycol; and a step of disinfecting. The composition contains 80-98 wt% of mud extract, 1-10 wt% of Broussonetia kazinokii extract, and 1-10 wt% of arbutin.

Description

Extraction method of Boryeong acid mud extract and whitening functional cosmetic composition containing the extract {METHOD OF EXTRACTING FOR SEA SILT EXTRACT AND WHITENING FUNCTIONAL COSMETIC COMPOSITION CONTAINING THE EXTRACT}

The present invention relates to an extraction method for obtaining an extract from a mud and a whitening functional cosmetic composition prepared using the obtained extract.

Mud (MUD) generally contains a large amount of various active ingredients, such as natural minerals to prevent skin aging, and rich in minerals that give vitality and elasticity to the skin to make young and fresh skin. In addition, there are colloidal ingredients (colloids) and crystalline ingredients can be used in physical therapy methods such as sand steaming or sauna, and has an excellent effect on the treatment of trauma due to antibacterial and fungicidal action.

In addition, by activating the cell activity by the release of far-infrared radiation, capillary expansion, blood circulation and metabolism promotion, various wastes in the skin is discharged out of the body to make each cell of the body healthy and vigorous.

Due to the nature of the mud, various cosmetic-related technologies using mud have been studied. As an example, a cosmetic raw material mud manufacturing composition that emits far-infrared energy of Korea Patent Publication No. 2002-0087590 (2002.11.23), Korea Publication Mud pack composition of Patent No. 2001-0090063 (October 18, 2001), color cosmetic composition for body painting containing mud of Korean Patent Publication No. 2003-0060426 (2003.07.16), Korean Patent Publication No. 2004 -0022868 Mud color cream composition containing mud of (2004.03.18), cosmetic composition containing mud and herbs and black fine powder of the Republic of Korea Patent Registration 10-0515956 (2005.09.13), Republic of Korea Patent Publication No. 2004-0067377 Numerous patented technologies have been disclosed, including mud extracts and cosmetic compositions containing herbal oils (July 30, 2004).

In the present invention, mud, especially Boryeong acid mud, Boryeong acid mud is Na 1.47%, Mg 0.71%, Al 8.89%, Si 31.52%, K 3.61%, Ca 0.70%, Ti 0.54%, Fe 4.46%, O It has a composition of 48.10%. In addition, it has a far-infrared ray-generating effect compared to the general mud, and it is known to help skin soothing, blemishes, acne, and help skin regeneration and blood circulation.

As such, the technology using Boryeong acid mud, which has a higher effect of far-infrared rays than that of general mud, uses cosmetic ingredients having skin moisturizing effect and cell growth effect from Boryeong acid mud of Korea Patent Publication No. 2001-0079027 (2001.08.22). Extraction method and skin cosmetic composition containing the Boryeong acid mud of the Republic of Korea Patent Publication No. 1998-0034570 (1998.08.05).

The present invention is characterized by a cosmetic composition having a whitening effect, the use of arbutin is important to achieve the whitening effect. However, in the prior art, there is little method for arbutin to be properly used with mud, and there is little use of arbutin, or even if it is used, its use is inadequate and the whitening effect cannot be exhibited.

In addition, cosmetics made using conventional Boryeong acid mud stayed in a product line that is only a general concept rather than maximizing the efficacy of the mud. For this reason, cosmetics made using conventional Boryeong acid mud have high added value as a cosmetic for consumers. It could not be created.

For this reason, the present inventors developed functional cosmetics using boryeong acid mud by using boryeong acid mud and arbutin appropriately, thereby maximizing the efficacy and effect of cosmetics, and recognizing consumers as high value-added products and functional using mud. It solves the problems of the safety of the human skin application of cosmetics, the inhibitory factor of stability due to various inorganic substances in mud, the miscibility with functional raw materials, and the inhibition of efficacy effect. The present invention can be completed.

As described above, the present invention provides a method of extracting boryeong acid mud extract in a suitable state which can be effectively combined with arbutin, a whitening medicine, and the synergistic effect of the functionality of the extract extracted by the extraction method and the efficacy and effect of arbutin. It is an object of the present invention to provide a whitening functional cosmetic composition having a high added value.

In order to achieve the above object, the present invention is mixed with Boryeong acid mud and purified water in a weight ratio 1: 5, stirred at room temperature for 40 minutes to 80 minutes and then left to remove the supernatant, and pretreatment of repeating the process three times Steps,

A salt removal step of mixing the mud and the purified water after the pretreatment step at a weight ratio of 1: 5, stirring for 40 minutes to 60 minutes at room temperature, and refrigerated for 12 hours to 20 hours, and

After the mud and purified water were mixed in a weight ratio of 1: 2, the mixture was stirred at room temperature for 40 minutes to 60 minutes, and then refrigerated for 12 hours to 20 hours to remove suspended matters in the supernatant. A filtration step of filtration under reduced pressure using a filter paper, and the filtered solution;

A method of extracting Boryeong acid mud extract, which is a preservative and sterilization step of preservatively sterilizing the solution obtained through the filtration step using phenobib and 1,3-butylene glycol, and

The extract extracted by the above method is mixed with arbutin to form a whitening cosmetic composition, or the extract is mixed with arbutin and mulberry extract to constitute a whitening cosmetic composition.

First, looking at the whitening cosmetic composition composed of a mixture of mud extract and arbutin, the composition is composed of a mixture of mud extract 80 ~ 98wt%, arbutin 2 ~ 20wt%. When the mud extract is less than 80wt%, the arbutin content is increased to cause oxidation and discoloration of arbutin, crystallization of arbutin, and some hydroquinones occur. In addition, when the content exceeds 98wt%, since the content of arbutin is relatively decreased, the whitening effect is decreased, the mud extract is preferably used within the range of 80 to 98wt% with respect to the total weight of the whitening cosmetic composition.

4-hydroxyphenyl-β-D-glucopyranoside of the arbutin molecular formula C ₁₂ H ₁₆ O ₇ (272.25), which is less than 2 wt%, has a whitening effect of the composition. If it falls, and exceeds 20wt%, the same problem occurs as the amount of mud extract is less than 80wt%, the amount of arbutin is preferably made within the range of 2 to 20wt%.

Next, looking at the whitening cosmetic composition composed of a mixture of mud extract, arbutin and mulberry extract, the composition is composed of a mixture of 80 ~ 98wt% mud extract, 1 ~ 10wt% of mulberry extract, 1 ~ 10wt% arbutin .

When the mud extract is less than 80wt%, the arbutin content increases to cause oxidation and discoloration of arbutin and crystallization of arbutin. And, there is a problem that some hydroquinone occurs. When it exceeds 98wt%, there is a problem that the whitening effect is lowered because the content of arbutin is relatively reduced. Therefore, the mud extract is preferably used in the range of 80 ~ 98wt%.

In addition, when the mulberry extract is less than 1wt%, there is a problem that the whitening effect is lowered, and when the mulberry extract is more than 10wt%, there is a problem in skin irritation and safety, the mulberry extract is 1 ~ 10wt% based on the total cosmetic composition It is preferable to use.

In addition, when the arbutin is less than 1wt%, the whitening effect of the cosmetic composition may be reduced, and when it exceeds 10wt%, the arbutin content increases, so that arbutin is oxidized and discolored, and crystals of arbutin are precipitated, and some hydroquinone is Since there is a problem that occurs, the arbutin is preferably used in the range of 1 to 10wt% based on the total cosmetic composition.

The mulberry extract is a primary filtration step of filtration of stems and roots of the mulberry or the same plant in ethanol for 1 to 3 weeks, and then filtration,

A second filtration step in which activated carbon is added to the filtrate after the first filtration step, mixed and filtered;

After concentrating the filtrate after the second filtration step, it is prepared through the step of putting the ethyl acetate to mix and then take the ethyl acetate layer to dry under reduced pressure.

In addition, the mulberry extract is used in the form of powder or a solution, the solution is prepared by dissolving the powder of the mulberry extract in butylene glycol of 2w / v%.

As described above, the whitening functional cosmetic composition containing the extract extracted by the extraction method of Boryeong acid mud extract according to the present invention experimentally analyzed the mutual miscibility and stability between the raw materials of Boryeong mud and functional cosmetics, and the result By applying to solubilized formulations and emulsifier type dispersion formulations based on this, it provides a high value-added functional cosmetics. And as such a high value-added functional cosmetics, it has the effect of increasing the development of the local industry and the recognition of Boryeong mud as a luxury product of consumers.

Detailed description of the technical configuration will be described through an embodiment.

Example 1: Mud Extract

Mud extract (Sea Silt Extract) is prepared through a pre-treatment step, salt removal step, filtration step, preservation and sterilization step sequentially, the pretreatment step is put 100ml of purified water in 500g Boryeong acid mud and stirred for 1 hour at room temperature After allowing to stand, the supernatant is removed and the same process is repeated three times.

In the salt removal step, 50 ml of purified water was added to 250 g of the Boryeong acid mud that had been subjected to a pretreatment step, stirred at room temperature for 1 hour, and then refrigerated and left to stand for 12 hours.

Next, in the filtration step, 100 ml of purified water was added to 200 g of the bored acid mud after the desalination step, and the mixture was stirred at room temperature for 1 hour, then refrigerated and left to stand for 12 hours, and then the suspended solids of the supernatant were removed. Pass through and filter the resulting solution under reduced pressure using filter paper.

Finally, the mud extract is completed by sterilizing the solution obtained through the filtration step using fenobib and 1,3-butylene glycol, followed by sterilization.

Example 2: whitening cosmetic composition (mixing of mud extract and arbutin)

2 g of the dissolved arbutin solution is administered to stir 98 g of the mud extract and stirred for 10 minutes. After stirring is complete, sealed after 400mesh filtration and stored at room temperature.

Arbutin (Arbutin) is represented by the following Formula 1,

4-hydroxyphenyl-β-D-glucopyranoside of the molecular formula C ₁₂ H ₁₆ O ₇ (272.25) of arbutin, containing at least 98.0% of arbutin when quantified do.

1. The appearance of arbutin

Arbutin is a white to pale yellow powder with a slight peculiar smell.

2. Identification Test of Arbutin

When 1 ml of arbutin is added to the solution, 2 ml of anthrone solution is cooled with water.

And when measured according to the potassium bromide purification method of the infrared absorption spectrum measurement method with arbutin, absorption at the wave number of 3,384 cm ^-1 , 3,290 cm ^-1 , 1,514 cm ^-1 , 1,222 cm ^-1 and 1,080 cm ^-1 Indicates.

Moreover, when absorption spectrum is measured by the absorbance measurement method with the aqueous solution of arbutin, absorption maximum is shown by wavelength 283 +/- 2 nm.

3. Melting Point of Arbutin

The melting point of arbutin is 198 to 201 ° C.

4. Purity of Arbutin

In the case of heavy metals, 1.0 g of arbutin is weighed and tested according to the first method. Add 2.0 mL of lead standard solution (20 ppm or less) to the reference solution.

In the case of arsenic, 1.0 g of arbutin is weighed to make a test solution according to the first method, and tested according to the method of using device B (less than 2 ppm).

5. Moisture of Arbutin

The water content of arbutin is 0.5% or less.

6. Arbutin ignition residue

The ignition residue of arbutin is 0.5% or less.

7. Assay of Arbutin

Accurately weigh 40 mg of arbutin, add mobile phase to make 10 ml, and use it as the sample solution. Separately, arbutin standard is dried in a desiccator (reduced pressure, silica gel) for 12 hours, and 40 mg is precisely weighed and operated in the same manner as the sample solution to prepare a standard solution. 20 μl of the sample solution and the standard solution are tested according to the liquid chromatograph method under the following conditions to obtain the arbutin peak areas A _T and A _S of the sample solution and the standard solution.

Amount of arbutin (C ₁₂ H ₁₆ O ₇ ) (mg) = Amount of arbutin standard (mg) × (A _T / A _S )

8. Operating Conditions of Arbutin

The detector is an ultraviolet absorbance photometer (measured wavelength 280 nm), and the column is filled with a octadecylylated silica gel for liquid chromatograph of 5 µm in a stainless tube having an inner diameter of 4.6 mm and a length of 20 cm. The mobile phase is a water, ethanol and acetic acid mixed liquid (95: 5: 1), and a flow rate is 1.0 mL / min.

Example 3: Whitening Cosmetic Composition (Mudd Extract, Arbutin and Mulberry Extract)

5 g of arbutin is completely dissolved by warm stirring with purified water. Then, the dissolved arbutin solution is administered to agitate 90 g of the mud extract and stirred for 10 minutes. To this, 5 g of mulberry extract is administered and stirred for 10 minutes. After 400mesh filtration and store at room temperature sealed.

The mulberry extract (Broussonetia Extract) is a powder obtained by extracting the stems or roots of the mulberry ( Broussonetia kazinoki ) and the same plant (Moraceae) with ethanol and ethyl acetate or 2w / v% butylene glycol solution of the powder. In the functional test of this raw material, the tyrosinase inhibition rate is 48.5 to 84.1%.

1.Production method

The mulberry extract is immersed for 1 to 3 weeks by adding twice the capacity of ethanol to the stems or roots of the mulberry and the same plant, and the mixed filtrate is mixed with 1% of activated carbon and filtered. Take this filtrate, concentrate it, add ethyl acetate, shake it well, mix it, take the ethyl acetate layer, dry it under reduced pressure, and dissolve it in butylene glycol to obtain a 2w / v% solution.

2. Characteristics of Mt.

Its extract is pale yellow to yellow brown viscous liquid or yellowish brown to dark brown crystalline powder with a slight peculiar smell.

3. Confirmation test of mulberry extract

Put butylene glycol in 2 g of the extract, and make 500 ml of the solution. In the case of powder, 1 g of butylene glycol is added to 1 g of this raw material to dissolve, and 1 ml of 100 ml of solution is added. Butylene glycol is added to 100 ml. When the absorption spectrum is measured by the absorbance method with the sample solution, the absorption maximum is shown at the wavelength of 283 ± 2nm. The pH of the mulberry extract is 2.7 ~ 4.7.

4. Functional Test of Methanol Extract

Take the amount of 50mg as the powder of the mulberry extract, add ethanol to dissolve it, take 10ml of the solution into 100ml, and add ethanol to make 100ml as the sample solution.

500 µl of buffer (0.1 M potassium dihydrogen phosphate solution is adjusted to 2 M sodium hydroxide solution to pH 6.8) (10 ml of water in 3 mg of tyrosine standard), 450 µl of water, and Add 50 μl of sample solution, mix, add 50 μl of enzyme solution (Mushroom Tyrosinase (Standard) to make 2 units / μl in buffer), shake and mix for 10 minutes at 37 ℃. After leaving for 500 minutes, 500 μl of the buffer solution, 950 μl of water and 50 μl of ethanol were added thereto, and the absorbance B was measured at a wavelength of 475 nm using a solution obtained by operating in the same manner as the sample solution.

Separately, the absorbance A was measured using 50 μl of ethanol instead of the test solution as the test solution, and the absorbance A was measured. 50 μl of water instead of the enzyme solution was used as the test solution. The absorbance C is measured and the tyrosinase inhibition rate (%) is calculated | required according to following formula (1).

Tyrosinase inhibition rate (%) = [{A- (B-C)} / A] × 100 ---------------- 1)

Here, A: absorbance obtained from blank test solution

          B: absorbance obtained from the sample liquid

          C: Absorbance obtained from the color correction liquid.

Test Example 1: Stability Test of Boryeong Mud Extract and Arbutin

In the case of Boryeong mud extracts, minerals were present, and thus experiments on discoloration and stability of arbutin used as cosmetic whitening ingredients were performed.

Experiments on discoloration and precipitation were carried out by preparing a mixed solution as shown in Table 1 below and incubating each in an incubator at 4 ° C., 25 ° C. and 45 ° C. in a daylight environment. 2 is shown.

As a result, no change occurred at 4 ℃ and 25 ℃ for 10 weeks, and slight discoloration at 8 ℃ at 45 ℃ and daylight. In addition, the pH was 6.32 at 25 ° C.

Table 1. Mixed Solution of Boryeong Mud Extract

 ingredient Ratio (wt%)  Boryeong Mud Extract 90.0  Arbutin 20% liquid mixture (arbutin, purified water) 10.0

Table 2. Observation table by temperature (○: no change, △: slight change, X: change)

condition Early Week 1 2nd week 3rd week 4 weeks Week 5 Week 6 Week 7 Week 8 Week 9 Week 10 4 ℃ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ 25 ℃ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ 45 ℃ ○ ○ ○ ○ ○ ○ ○ ○ △ △ △ daylight ○ ○ ○ ○ ○ ○ ○ ○ △ △ △

Test Example 2: Whitening Solution Stability and Usability Test of Boryeong Mud Extract

Sorbent type arbutin solution was formulated using Boryeong mud extract. Experimental formulations are shown in Table 3.

Table 3. Boryeong Mud Whitening Solution

ingredient Content (wt%)  Water 78.35  Sea Silt Extract 10.00  Glycerin 3.00  Alcohol 3.00  Butylene Glycol 3.00  Arbutin 2.00  Phenoxyethanol 0.20  Polysorbate 80 0.15  Methylparaben 0.15  Sodium Citrate 0.10  Citric Acid 0.05

Test Example 3: Product Application Experiment of Boryeong Mud Whitening Solution

The experiment was conducted to apply Boryeong mud whitening solution to the existing beauty pack products, Boryeong mud modeling mask pack and mud powder pack. By applying lukewarm water and the developed product, the drying speed and post-drying condition of the pack were compared and evaluated through the double blind method of 10 people. Evaluation items are shown in Table 4 below.

Table 4. Review Items

score 5 4 3 2 One Drying rate Very fast speed moderation Slightly slow Slow Skin condition after drying good Slightly good usually Slightly bad Bad

The results of the evaluation are shown in Table 5 below, and there was no difference in terms of drying speed from the use of conventional lukewarm water, and the skin condition after drying was further improved.

Table 5. Evaluation Results

Evaluation item
Drying speed Skin condition after drying Tepid water Whitening Solution Tepid water Whitening Solution Modeling Mask Pack 3.3 3.2 4.7 5.1 Powder Mask Pack 3.1 3.3 3.8 4.3

Test Example 4: Safety and Analysis of Boryeong Mud Whitening Solution

To determine the safety and efficacy of the experimental Boryeong mud whitening solution, quantitative analysis of lead, arsenic and arbutin was performed. The results are shown in Table 6.

Table 6. Test Results

Inspection items Standard (standard) result Suitability Arbutin 1.8 to 2.2% 2.05% fitness lead 20 ppm 0.00ppm fitness arsenic 10 ppm 0.00ppm fitness

Lead arsenic should be less than 20ppm of lead and less than 10ppm of arsenic in accordance with the 2007-45 Cosmetic Standard and Test Method of Korea Food and Drug Administration. Arbutin solution should be at least 90% of the labeled value according to the functional cosmetic standard and test method of Korea Food & Drug Administration Notification No. 2007-44.

Claims (6)

Boryeong acid mud and purified water were mixed in a weight ratio of 1: 5, stirred at room temperature for 40 minutes to 80 minutes, and then allowed to stand to remove the supernatant, and repeating the above procedure three times, A salt removal step of mixing the mud and the purified water after the pretreatment step at a weight ratio of 1: 5, stirring for 40 minutes to 60 minutes at room temperature, and refrigerated for 12 hours to 20 hours, and Mud and purified water after the desalination step was mixed in a weight ratio of 1: 2 and stirred at room temperature for 40 minutes to 60 minutes, then refrigerated for 12 hours to 20 hours, and the suspension of the supernatant was removed. A filtration step of passing the apparatus and filtration of the liquid from the resulting solution under reduced pressure using a filter paper; Boryeong acid mud extract extraction method characterized in that the solution obtained through the filtration step preservative treatment using fenobib and 1,3-butylene glycol after the antiseptic and sterilization step to sterilize. Whitening cosmetic composition, characterized in that the cosmetic composition formed by adding any one or more components selected from arbutin or mulberry extract to the mud extract extracted by the method of claim 1. The method according to claim 2, Cosmetic composition is a whitening cosmetic composition, characterized in that the mud extract 80 to 98wt%, arbutin 2 to 20wt% of the composition. The method according to claim 2, The cosmetic composition is a whitening cosmetic composition, characterized in that the mud extract is composed of a mixture of 80 ~ 98wt%, 1 ~ 10wt% of mulberry extract, 1 ~ 10wt% arbutin. The method according to claim 4, The mulberry extract is a primary filtration step of filtration of stems and roots of the mulberry or the same plant in ethanol for 1 to 3 weeks, followed by filtration, A second filtration step in which activated carbon is added to the filtrate after the first filtration step, mixed and filtered; Concentrate the filtrate after the second filtration step, and then put the ethyl acetate in the mixture and then take the ethyl acetate layer to obtain a whitening cosmetic composition, characterized in that the manufacturing through the step of drying under reduced pressure. The method according to claim 5, The mulberry extract is in the form of powder or solution, The solution is a whitening cosmetic composition, characterized in that prepared by dissolving the powder in butylene glycol 2w / v%.