KR102136226B1 - Extraction method of cosmetic raw materials using sous-vide method - Google Patents

Abstract

The present invention relates to a method for extracting cosmetic raw materials and, more specifically, to a method for extracting cosmetic raw materials using a sous vide method to prevent a natural extract from being changed. To this end, according to the present invention, the method comprises: a first step of washing and drying raw botanical materials; a second step of finely cutting the washed and dried raw botanical materials; a third step of adding a solvent of 5 to 100 times of the total weight of the raw botanical materials to the finely cut raw botanical materials and putting the mixture in a closed vessel to perform vacuum-packaging; a fourth step of aging the vacuum-packed raw botanical materials at 0 to 10°C for 2 to 7 days; a fifth step of extracting the aged raw botanical materials for 2 to 7 days to produce a botanical extract; and a sixth step of filtering the botanical extract.

Description

Extraction method of cosmetic raw materials using the Subid method {EXTRACTION METHOD OF COSMETIC RAW MATERIALS USING SOUS-VIDE METHOD}

The present invention relates to a method for extracting a cosmetic raw material, and more particularly, to a method for extracting a cosmetic raw material using a Subid extraction method.

Free radicals, called free radica, are produced during the process by which oxygen from your breath produces and converts energy. Free radicals are very aggressive chemicals in our body that damage healthy cells and, as a result, are involved in inflammation, wrinkles, and aging. Antioxidants act to remove free radicals and are still the most popular representative material in cosmetics. Antioxidants are mainly found in plants. Antioxidants from these plants can be obtained through various extraction methods such as hot water extraction, reflux extraction, low temperature extraction, ultrasonic extraction, and supercritical extraction. Is becoming.

Sous-vide extraction method is one of the vacuum low-temperature extraction methods, and it is a method of extracting completely without destroying the antioxidant components or other effects of vegetable raw materials. Sous-vide extraction method is a process that extracts at a low temperature after extracting at a low temperature after aging the plant after putting the plant raw material in a container and vacuum-packing it. It can solve problems such as decreased efficacy and decreased anti-wrinkle efficacy.

Republic of Korea Registered Patent Publication No. 10-1998374

The present invention is to solve the above problems, and an object of the present invention is to provide a method for extracting a cosmetic raw material using a souvide extraction method.

The above and other objects and advantages of the present invention will become apparent from the following description of preferred embodiments.

The object is a first step of washing and drying the vegetable raw material; A second step of rinsing the washed and dried vegetable raw materials; A third step of adding a solvent of 5 to 100 times the total weight of the vegetable raw material to the shredded vegetable raw material, and packaging the product in a sealed container under vacuum; A fourth step of maturing the vacuum-packed vegetable raw material at 0-10°C for 2-7 days; A fifth step of extracting the aged vegetable raw material for 2 to 7 days to produce a vegetable extract; And a sixth step of filtering the vegetable extract; can be achieved by a method of extracting cosmetic raw materials comprising.

At this time, the vegetable raw material, may be at least any one selected from the group consisting of sea grapes, myrtle, centella, and calendula.

In addition, the extraction of the fifth step may be to extract the aged vegetable raw material at 30 ~ 60 ℃.

According to the present invention, it is possible to effectively extract the active ingredient from the vegetable raw material. Specifically, it is possible to produce an extract that can prevent the variation of the natural extract and improve the antioxidant effect and anti-aging effect, so it has an effect that can be used as a raw material for functional cosmetics.

Particularly, problems such as variation of raw material components and decomposition of active components, which are disadvantages of the conventional hot water extraction method, have been improved, and can have an effect of obtaining an active component without an organic solvent removal step, and preserve the intrinsic fragrance of vegetable raw materials. It has the advantage of being able to.

However, the effects of the present invention are not limited to the above-mentioned effects, and other effects not mentioned will be clearly understood by those skilled in the art from the following description.

1 is a view schematically showing a method of extracting cosmetic raw materials according to an embodiment of the present invention.
2 is a view showing the antioxidant effect of Examples and Comparative Examples.
3 is a view showing the polyphenol content of Examples and Comparative Examples.
4 is a view showing the results of cytotoxicity experiments of Examples and Comparative Examples.
5 is a view showing the anti-wrinkle effect of Examples and Comparative Examples.

Hereinafter, the present invention will be described in detail with reference to examples and drawings of the present invention. These examples are only provided by way of example to illustrate the present invention in more detail, it will be apparent to those skilled in the art that the scope of the present invention is not limited by these examples. .

In addition, unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the art to which the present invention belongs, and in case of conflict, the present specification including definitions. The description will take precedence.

In order to clearly describe the proposed invention in the drawings, parts irrelevant to the description are omitted, and like reference numerals are assigned to similar parts throughout the specification. And, when it is said that a part "includes" a certain component, this means that other components may be further included instead of excluding other components unless otherwise specified. In addition, "part" described in the specification means one unit or block that performs a specific function.

In each step, the identification code (first, second, etc.) is used for convenience of explanation. The identification code does not describe the order of each step, and each step does not explicitly describe a specific order in the context. It may be carried out differently from the above-described order. That is, each step may be performed in the same order as specified, or may be performed substantially simultaneously, or in the reverse order.

1 is a view schematically showing a method of extracting cosmetic raw materials according to an embodiment of the present invention. Referring to Figure 1, a method of extracting a cosmetic raw material according to an embodiment of the present invention includes a first step of washing and drying the vegetable raw material; A second step of rinsing the washed and dried vegetable raw materials; A third step of adding a solvent of 5 to 100 times the total weight of the vegetable raw material to the shredded vegetable raw material, and packaging the product in a sealed container under vacuum; A fourth step of maturing the vacuum-packed vegetable raw material at 0-10°C for 2-7 days; A fifth step of extracting the aged vegetable raw material for 2 to 7 days to produce a vegetable extract; And a sixth step of filtering the vegetable extract. The present invention is a method of extracting a cosmetic ingredient using a Subid method for extracting an active ingredient from a vegetable raw material in a vacuum state, which can effectively extract the active ingredient from the vegetable raw material. Specifically, it is possible to produce an extract that can prevent the variation of the natural extract and improve the antioxidant effect and anti-aging effect, so it can have an effect that can be used as a raw material for functional cosmetics. Particularly, problems such as variation of raw material components and decomposition of active components, which are disadvantages of the conventional hot water extraction method, have been improved, and can have an effect of obtaining an active component without an organic solvent removal step, and preserve the intrinsic fragrance of vegetable raw materials. Can have the advantage of being able to.

The first step is a step of washing and drying the vegetable raw material. The vegetable raw material generally means a vegetable raw material capable of producing a vegetable extract for application to cosmetics, and may be selected and used according to the purpose of use of the cosmetic, and is not particularly limited. Specifically, it may be any one selected from the group consisting of sea grapes, gruel, centella, and calendula, but it is only described as an example for explaining a method for extracting cosmetic raw materials using the Subid method, and other herbs, fruits, etc. It is also possible to use various vegetable raw materials.

After the vegetable raw material is washed and dried, various methods can be used within a range that does not damage the vegetable raw material. For example, freeze drying, spray drying, or hot air drying may be used, and drying of the vegetable raw material is preferably 1 to 10% by weight of 100% by weight.

In the second step, the vegetable raw material is shredded. Here, the slicing is used as a concept including both cutting and grinding. Only after crushing the vegetable raw material, it is immersed in a solvent to effectively extract the active ingredient. For example, the vegetable raw material may be cut to a size of 0.01 mm to 2 cm or pulverized to a powder state of about 50 mesh or more, and may be finely cut to an appropriate size according to the properties of the vegetable raw material used.

The third step is a step of adding a solvent of 5 to 100 times the total weight of the vegetable raw material to the shredded vegetable raw material, and packaging the product in a sealed container under vacuum. At this time, the solvent used may be variously selected according to the nature of the vegetable raw material, and the hot water extract, reflux extract, supercritical extract and ultrasonic extract or bifida fermented product, kefir fermented product, which is first extracted using the vegetable raw material, including purified water Microbial fermentation products, such as microbial culture, ethanol, propanediol, butylene glycol, propylene glycol, hexanediol, octanediol, decandiol, organic solvents may be used, but is not limited thereto.

The fourth step is a step of aging the vacuum-packed vegetable raw material at 0-10°C for 2-7 days. A aging process is required so that the active ingredient can be extracted well, and the aging conditions can be variously adjusted according to the solvent selected in the third step. For example, it is also possible to mature in an open or closed tank, or in a dark or light condition.

The fifth step is a step of producing a vegetable extract by extracting the aged vegetable raw material for 2 to 7 days. At this time, extraction is preferably performed at 30 ~ 60 ℃. In the case of less than 30°C, the active ingredient from the vegetable raw material may not be sufficiently soluble in the solvent, and when it exceeds 100°C, there is a concern that a problem occurs in the sealed container.

The sixth step is a step of filtering the vegetable extract. Unnecessary impurities and bacteria contained in the extract can be removed. Filtration can use a variety of methods. For example, it may be filtered using a filter paper having a pore of about 0.1 ~ 2μm, but is not limited thereto.

In one embodiment, before filtering, it is possible to effectively remove impurities and bacteria, and to improve the biocompatibility of the filtered extract, it can be mixed with zwitter ionic material and polylysine.

Since zwitter ionic material is a biocompatible material due to its low protein adsorption property, when applied as a biomaterial, it can prevent inflammation and impart stability to cells or medicines. That is, it is possible to prevent side effects such as allergies when using the human body. For example, the zwitter ionic material may be any one selected from the group consisting of phosphoryl choline, phosphoryl ethanolamine, phosphoryl serine, sulfobetaine, carboxybetaine, and combinations thereof, but sulfobe It is preferable to use others.

Polylysine (polylysine) is a polymer of the amino acid lysine (lysine), synthesized by polymerization, desorption of an N-carboxy amino acid anhydride protecting an ε-amino group, or found in nature by aerobic culture of microorganisms. Polylysine exhibits an α-helix structure when the ε-amino group is positively charged at pH 11 or higher, an irregular structure at pH 11 or lower, and a β structure at pH 11. The polylysine may be epsilon poly-L-lysine. Epsilon poly-L-lysine is a substance known to be safe for humans, such as used as food preservatives for many years in the United States and Japan. Polypeptide, a linear polymer of about 3,000 to about 10,000 Daltons in which the lysine-alpha-carboxyl group and the epsilon-amino group are connected by peptide bonding. Is a substance. When mixed by adding epsilon poly-L-lysine, it is possible to effectively remove bacteria and the like, as well as inhibit the growth of microorganisms, thereby improving the preservation effect of the extract.

The zwitter ionic material and polylysine are preferably included in an amount of 0.1 to 5% by weight, respectively, based on 100% by weight of the total extract. When included in an amount of less than 0.1% by weight, the biocompatibility improving effect, bacteria removal effect and preservation effect are insignificant, and when it is included in excess of 5% by weight, the filtration cost may increase, which is undesirable.

When a cosmetic composition is prepared using the cosmetic raw material produced by the present invention, the cosmetic composition may be prepared by including a stabilizer, a solubilizing agent, conventional adjuvants such as vitamins, pigments and fragrances, and a carrier, and additional effects It may further include a skin absorption accelerator to promote.

The formulation of the cosmetic composition may be prepared in any formulation conventionally prepared in the art, for example, the cosmetic composition may be a lotion, emulsion, skin, toner, lotion, essence, sunscreen, cream, makeup base, foundation, It may be formulated as a powder, pack, gel, shampoo, rinse, spray, makeup remover and detergent, but is not limited thereto.

When the formulation is a paste, cream or gel, animal oil, vegetable oil, wax, paraffin, starch, tracant, cellulose derivative, polyethylene glycol, silicone, bentonite, silica, talc or zinc oxide may be used as a carrier component.

When the formulation is a powder or a spray, lactose, talc, silica, aluminum hydroxide, calcium silicate or polyamide powder can be used as a carrier component, and particularly in the case of a spray, additionally chlorofluorohydrocarbon, propane/butane or Propellants such as dimethyl ether.

When the formulation is a solution or emulsion, a solvent, solubilizer or emulsifier is used as a carrier component, such as water, ethanol, isopropanol, ethyl carbonate, ethyl acetate, benzyl alcohol, benzyl benzoate, propylene glycol, 1,3- Fatty acid esters of butyl glycol oil, glycerol aliphatic esters, polyethylene glycol or sorbitan.

When the formulation is a suspension, liquid diluents such as water, ethanol or propylene glycol as carrier components, ethoxylated isostearyl alcohol, suspensions such as polyoxyethylene sorbitol esters and polyoxyethylene sorbitan esters, microcrystalline cellulose, Aluminum metahydroxide, bentonite, agar or trakant, etc. can be used.

Hereinafter, the configuration of the present invention and its effects will be described in more detail through specific examples and comparative examples. However, this example is intended to illustrate the present invention in more detail, and the scope of the present invention is not limited to these examples.

[Example]

Vegetable raw materials including sea grapes, gruel, centella, and calendula were prepared and washed, followed by hot air drying until the mass of moisture reached 5% by weight of the total weight. The dried vegetable raw material was cut into 0.1-1 cm size using a mixer. 50% of the weight of the vegetable raw material was added to the solvent, and then packed in a sealed container and vacuum packed. It was then aged at 4°C. After that, it was immersed in water in a sealed container. Finally, the filtrate was obtained by filtration using a filter paper having a filter size of 1.0 μm (see Table 1). The solvent used was purified water, 1,3-butylene glycol, fermented product, and in the case of fermented product, Bifidobacterium longum cultured in BL (BD) medium for 5 days was used. Examples 1 to 15 were prepared with different aging periods, solvents, extraction temperatures and extraction periods, and in the case of Example 16, the same preparation as Example 6 was performed, but sulfobetaine and epsilon poly-L-lysine were prepared before filtration. 2% by weight of the total weight before each filtration and mixed for 10 minutes and then filtered.

division Extraction method ferment menstruum Extraction temperature Extraction period Example 1 Subid 5 days Purified water 60℃ 5 days Example 2 Subid 5 days Purified water 60℃ 3 days Example 3 Subid 5 days Purified water 80℃ 5 days Example 4 Subid 5 days Purified water 80℃ 3 days Example 5 Subid 3 days Purified water 60℃ 5 days Example 6 Subid 5 days 1,3-BG 60℃ 5 days Example 7 Subid 5 days 1,3-BG 60℃ 3 days Example 8 Subid 5 days 1,3-BG 80℃ 5 days Example 9 Subid 5 days 1,3-BG 80℃ 3 days Example 10 Subid 3 days 1,3-BG 60℃ 5 days Example 11 Subid 5 days Fermentation 60℃ 5 days Example 12 Subid 5 days Fermentation 60℃ 3 days Example 13 Subid 5 days Fermentation 80℃ 5 days Example 14 Subid 5 days Fermentation 80℃ 3 days Example 15 Subid 3 days Fermentation 60℃ 5 days Example 16 Subid 5 days 1,3-BG 60℃ 5 days

[Comparative example]

Vegetable raw materials including sea grapes, gruel, centella, and calendula were prepared and washed, followed by hot air drying until the mass of moisture reached 5% by weight of the total weight. The dried vegetable raw material was cut into 0.1-1 cm size using a mixer. After adding 50 times the weight of the vegetable raw material, the mixture was stirred and extracted at 60°C for 5 days. Finally, the filtrate was obtained by filtration using a filter paper having a filter size of 1.0 μm (see Table 2).

division Extraction method ferment menstruum Extraction temperature Extraction period Comparative Example 1 Hydrothermal - Purified water 60℃ 5 days Comparative Example 2 Hydrothermal 5 days Purified water 60℃ 5 days Comparative Example 3 Hydrothermal - Purified water 80℃ 5 days Comparative Example 4 Hydrothermal 5 days Purified water 80℃ 5 days

[Experimental Example 1: Antioxidant effect analysis]

Free radical scavenging activity was analyzed using DPPH (2,2-Diphenyl-1-picrylhydrazyl) reagent. As a control, ascorbic acid was used. After adding ethanol to Examples 1-16 and Comparative Examples 1-4 to 0.1 mM DPPH and reacting in the dark for 30 minutes, absorbance at 520 nm was measured, and this is shown in FIG. 2.

[Equation 1]

Free radical scavenging activity (%) = 100-Sample material added group absorbance / control absorbance X 100

Next, in order to measure the total polyphenol content, ₂ ml of a 7% Na ₂ CO ₃ (Sodium carbonate, Sigma-Aldrich) solution was mixed with 0.1 ml of the samples of Examples 1 to 16 and Comparative Examples 1 to 4 and 3 After 1 minute, 0.1 ml of 1 N of Folin-Ciocalteu's phenol reagent (Sigma-Aldrich) was added to react for 30 minutes at room temperature, and absorbance was measured at 750 nm. Gallic acid was used as a standard. As for the calibration curve for quantification, the standard substance, gallic acid, was dissolved by concentration, and then treated in the same way as a test substance or a comparative substance.

As a result, it was confirmed that all of Examples 1 to 16 had better effects in the polyphenol content and antioxidant analysis than Comparative Examples 1 to 4, and it was confirmed that Example 11 was the most effective.

[Experimental Example 2: Cytotoxicity Analysis]

After counting using CCD986sk (ATCC) fibroblasts, the cells were dispensed at a concentration of 6 X 10 ³ cells/well in a 96-well plate. After incubation for 24 hours, DMEM containing Examples 1-16 and Comparative Examples 1-4 were added to each well at a total concentration of 5%, and 10% fetal bovine serum and 5% penicillin/streptomycin were added to the fibroblasts. The cells were cultured for 24 hours in a 37°C, 5% CO ₂ incubator using 100 μl of medium. Then, the supernatant was removed, and a mixture of DMEM medium and WST solution (EZ-cytox) in a weight ratio of 9:1 was added, and then reacted for 2 hours in a 37°C, 5% CO ₂ incubator, and absorbance at 450 nm. Was measured. The degree of cytotoxicity (cell viability) was expressed as a percentage (%) based on the absorbance intensity of the control group using a solvent such as a test substance and a comparative substance, and this is shown in FIG. 4.

[Equation 2]

Cell viability (%) = sample material added group absorbance / control absorbance X 100

As a result, it was confirmed that both Examples 1 to 16 and Comparative Examples 1 to 4 had no cytotoxicity.

[Experimental Example 3: Anti-wrinkle effect analysis (Prcollagen)]

After counting using CCD986sk (ATCC) fibroblasts, the cells were dispensed at a concentration of 1.5 X 10 ⁴ cells/well in a 24-well plate. After incubation for 24 hours in DMEM medium containing 10% fetal calf serum and 5% penicillin/streptomycin, it was cultured for 24 hours after replacement with Serum free media (DMEM with% penicillin/streptomycin). Examples 1 to 16 and Comparative Examples 1 to 4 were mixed with Serum free media and cultured for 48 hours after treatment. All incubations were performed in a 37° C., 5% CO ₂ incubator. The culture was collected and the amount of collagen secreted in the culture was measured using an ELISA kit (Procollagen type C-peptide EIA kit, Takara).

[Equation 3]

Procollagen production (%) = sample processing production / control production X 100

As a result, it was confirmed that the effects of increasing the amount of Procollagen production were superior to those of Comparative Examples 1 to 4 in Examples 1 to 16, and it was confirmed that Example 11 was the most effective.

[Production example]

Lotions and creams could be prepared using the product of Example 11. The specific method is as follows.

[Production Example 1: Lotion]

3.0 parts by weight of propylene glycol, 0.1 parts by weight of carboxy polymer, and preservative trace and residual amount of purified water were mixed and stirred at 80 to 85°C and then added to the production unit to act as an emulsifier, 1.0 parts by weight of polysorbate 60, sorbitan Sesquioleate 0.5 parts by weight, liquid paraffin 10.0 parts by weight, sorbitan stearate 1.0 parts by weight, lipophilic monostearic acid glycerin 0.5 parts by weight, stearic acid 1.5 parts by weight, glyceryl stearate/PEG-400 stearate 1.0 parts by weight, triethanol 0.2 parts by weight of the amine was heated to 80 to 85° C., and then emulsified. After the emulsification is completed, heat is cooled to 50°C with stirring using a stirrer, and then a trace amount of fragrance is added, and after cooling to 45°C, a trace amount of dye is added, and Example 11 is added at 35°C, cooled to 25°C, and aged. Ordered.

[Production Example 2: Cream]

0.3 parts by weight of carboxy polymer, 5.0 parts by weight of butylene glycol, 3.0 parts by weight of glycerin and the remaining amount of purified water were mixed and stirred at 80 to 85° C. and then added to the production unit to act as an emulsifier, 2.0 parts by weight of stearic acid, cetyl alcohol 2.0 parts by weight, glyceryl monostearate 2.0 parts by weight, polyoxyethylene sorbitan monostearate 0.5 parts by weight, sorbitan sesquioleate 0.5 parts by weight, glyceryl monostearate/glyceryl stearate/polyoxyethylene stearate 1.0 part by weight, 1.0 part by weight of wax, 4.0 part by weight of liquid paraffin, 4.0 part by weight of squalane, 4.0 part by weight of caprylic/capric triglyceride was heated to 80 to 85° C., and then 0.5 part by weight of triethanolamine was added to emulsify. . After the emulsification was finished, the mixture was cooled to 35°C with stirring using a stirrer, and then Example 11 was added to cool to 25°C and aged.

In this specification, only a few examples of various embodiments performed by the present inventors are described, but the technical spirit of the present invention is not limited to or limited thereto, and can be variously implemented by a person skilled in the art.

Claims (3)

A first step of washing and drying vegetable raw materials;
A second step of rinsing the washed and dried vegetable raw materials;
A third step of adding a solvent of 5 to 100 times the total weight of the vegetable raw material to the shredded vegetable raw material, and vacuum-packing it in a sealed container;
A fourth step of maturing the vacuum-packed vegetable raw material at 0-10°C for 3-5 days;
A fifth step of extracting the aged vegetable raw material for 3 to 5 days to produce a vegetable extract; And
Including the sixth step of filtering the vegetable extract;
The third stage solvent is a fermentation product of Bifidobacterium longum cultured in BL(BD) medium for 5 days,
The extraction of the fifth step is characterized in that it is performed at 60 ~ 80 ℃, the extraction method of cosmetic raw materials using the Subid method. The method of claim 1, wherein the vegetable raw material,
Method of extracting a cosmetic raw material, characterized in that at least one selected from the group consisting of sea grapes, hair, bottle grass and calendula. delete

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