KR101087734B1 - Method for Purification of Saponin from Soapberry, Dichloro Methane Fraction of Soapberry, and Cosmetic Composition for Hair Comprising the Same - Google Patents

Abstract

The present invention relates to a method for purifying saponin from a patient tree, a dichloromethane fraction of a patient tree, and a hair cosmetic composition comprising the same. Doing; The skin or seed of the patient-free tree is refluxed for 3 to 5 hours at a temperature of 60 to 80 ° C. in the presence of at least one alcohol selected from the group consisting of C ₁ to C ₅ lower alcohols, or a mixture of the alcohol and water. Extracting to obtain a saponin crude extract having a saponin content of 30 to 40% by weight; And obtaining a dichloromethane fraction of the crude saponin extract obtained above, wherein the saponin content in the fraction is 25 to 35% by weight.

In addition, the dichloromethane fraction of the patient-free tree of the present invention is at least one alcohol selected from the group consisting of C ₁ to C ₅ lower alcohol, or the bark of the patient-free tree extracted with reflux using a mixture of the alcohol and water as a solvent or The saponin crude extract of the seedling is fractionated with dichloromethane, characterized in that the saponin content is 25 to 35% by weight or more. The hair cosmetic composition containing the dichloromethane fraction of the patient-free tree has excellent antibacterial effect, improves the quality of the hair, prevents itching and dandruff of the scalp, prevents static electricity and hair loss, and is usefully used in the industrial field of the hair cosmetic composition. Can be.

Patient tree, saponin, dandruff, antibacterial, rind

Description

Method for Purification of Saponin from Soapberry, Dichloro Methane Fraction of Soapberry, and Cosmetic Composition for Hair Comprising the Same}

The present invention is a method for purifying saponin from a non-patient tree, fractions from a non-patient tree and excellent antimicrobial effect, including the same, improving the quality of the hair, preventing itching and dandruff of the scalp, antistatic and hair loss of the hair cosmetic composition It is about.

The scientific name of the patient-free tree is Sapindus mukorossi, English name Soapberry tree, and the main distribution areas are Jeju, Taiwan, South China, India, and Indonesia on the southwest coast of the Korean peninsula. It is known to bloom in June and to produce a yellowish brown color in October. The patient-free tree is a natural surfactant that begins to be named Soapberry because it foams just by rubbing it by hand. Seeds that have been peeled from the patient's tree in autumn are stored cold in wet sand or buried in open-air with wet sand, and then sown in spring to germinate. The peeled rind (fruit bark) was used as a soap substitute, and the seed was also used as a material for making beads, and was sown and raised mainly near temples. The disease-free tree is a tree that means no patient, and in China, it is called the water-free water. In the book, San Hai-King, it is possible to defeat demons centered on Taoist believers. It is said to have been widely used in the name of 'non-hwan' because of its elimination of womb and worry.

It is known that the saponin of bark of the patient tree contains sapinloside A, B, C, D, etc., and LD50 (mg / kg) for the mice of sapinloside A ~ E is 1625 when in oral and subcutaneous injection. 659, known as 270 when injected intravenously or intraperitoneally. Under normal (0.04mg / kg) normal rabbits do not affect blood pressure, but subcutaneous injection of subcutaneous injections is known to reduce blood pressure by 25%. However, it is known that there is no change in the content of cholesterol in the blood. Early saponin (starting on day 40) in rabbits fed cholesterol-treated experimental atherosclerosis may lower saponin levels, lower blood cholesterol levels and increase phosphatidylcholine (lecithin), leading to lower blood pressure. Doha Herbal Metabolism (Plant), Younglim Temple p291-292, 1998).

On the other hand, human hair is contaminated by sebum secreted from the contaminants or the scalp itself in contact with the surrounding atmosphere, and the hair cleaning composition such as shampoo is used to remove such contaminants or sebum. However, since most of the active ingredients of hair cleaning compositions such as shampoos are made of chemical components such as surfactants and silicones, in the case of sensitive skin, seborrheic dermatitis or inflammatory diseases may occur, which may be a major cause of hair loss. In addition, there is a problem indicative of side effects such as causing dandruff and itching due to skin keratin. Therefore, there has been an effort to solve this problem by using natural materials.

Recently, research and development of shampoos having a protective function and a nutrition supply function for the scalp and hair have been actively conducted. In particular, various methods for producing shampoos have been proposed by adding extracts of plants obtainable from nature to shampoo raw materials (raw materials in which additives such as surfactants and bubble enhancers are mixed).

However, the shampoo or rinse composition including most of the natural material is often included selectively only one or two natural material according to the purpose, there has been a technical difficulty because the extraction or purification method of the natural material is not easy.

Accordingly, the inventors of the present invention have completed the present invention while repeatedly researching a natural cosmetic material, especially a hair cosmetic composition containing saponin, and a method for purifying saponin at a high concentration from a patient tree for the preparation thereof.

Accordingly, an object of the present invention is to provide a method for purifying high concentrations of saponin from a patient tree. It is also an object of the present invention to provide a fraction having a high saponin content from the patient tree. In addition, an object of the present invention is to provide a hair cosmetic composition comprising the fraction.

In order to achieve the above object, the present invention provides a method for purifying saponin from a patient tree, a dichloromethane fraction of the patient tree, and a hair cosmetic composition comprising the same.

Saponin purification method from the patient tree according to an embodiment of the present invention comprises the steps of preparing a bark or seed of the patient tree;

The bark of the patient-free tree is extracted under reflux for 3 to 5 hours at a temperature of 60 to 80 ° C. in the presence of at least one alcohol selected from the group consisting of C ₁ to C ₅ lower alcohols, or a mixture of the alcohol and water. Obtaining a saponin crude extract having a saponin content of 30 to 40% by weight; And

Obtaining a dichloromethane fraction of the obtained saponin crude extract,

Saponin content in the fractions is characterized in that 25 to 35% by weight.

At this time, the saponin content in the saponin crude extract may be preferably 35 to 36% by weight. In addition, the saponin content in the dichloromethane fraction of the saponin crude extract may preferably be 29 to 32% by weight. As described above, by extracting reflux in the presence of a lower alcohol or a mixture of the alcohol and water, a saponin crude extract containing a high concentration of saponin was obtained.

At this time, at least one alcohol selected from the group consisting of C ₁ to C ₅ lower alcohols, or a mixture of the alcohol and water can be selected and used without limitation, preferably methanol or butanol More preferably 95% methanol. The saponin content in the saponin crude extract of the aquatic bark extracted with 95% methanol as described above can be obtained at a high concentration of 30 to 40% by weight, and a high concentration of saponin extract from the apiary bark or the seedling.

At this time, it is preferable that the method of obtaining the saponin crude extract from the bark or seedling of the non-patient tree is reflux extraction. In addition, the extraction temperature at the time of extraction is a temperature range of at least the boiling point of the solvent of one or more alcohols selected from the group consisting of C ₁ to C ₅ lower alcohols used for extraction to enable reflux extraction, or a mixture of the alcohol and water It is preferable to proceed at. As said temperature, Preferably it is 60-80 degreeC according to an extraction solvent. The time required for reflux extraction is preferably 3 to 5 hours. If the extraction time is less than 3 hours, the extraction is not sufficient, and when the extraction time exceeds 5 hours, the degree of extraction increases with increasing extraction time. Do.

Meanwhile, as described above, the saponin content in the crude saponin extract extracted by the above method is 30 to 40% by weight, and the saponin content in the fraction fractionated with dichloromethane is 25 to 35% by weight. Preferably the saponin content in the saponin crude extract may be 35 to 36% by weight, the saponin content in the dichloromethane fraction may be 29 to 32% by weight.

As described above, in the case of extracting saponin from the bark or bark according to the purification method of the embodiment of the present invention, it may contain at least 30% by weight saponin in the crude saponin extract, 25% by weight in the fraction of dichloromethane The saponin can be contained.

  Saponin purification method from the patient tree according to the embodiment according to the embodiment, the step of concentrating the fraction of dichloromethane under reduced pressure to 50 to 100 atm; And centrifuging the saponin fraction concentrated under reduced pressure as described above at 2000 to 4000 rpm.

On the other hand, the dichloromethane fraction of the non-patient tree according to another embodiment of the present invention is one or more alcohols selected from the group consisting of lower alcohols of C ₁ to C ₅ , or a non-patient tree reflux extracted with a mixture of the alcohol and water as a solvent The extract of skin is fractionated with dichloromethane and saponin content is 25 to 35% by weight. More preferably, the saponin content is 29 to 32% by weight. At this time, it is preferable that the alcohol solvent used for reflux extraction as mentioned above is methanol or butanol. More preferably 95% methanol can be used. The saponin content of the saponin crude extract of the apiary bark or seedling extracted with 95% methanol as described above is 30% by weight or more, so that a high concentration of saponin crude extract can be obtained from the apiary tree. The saponin content in the crude extract is 30 to 40% by weight, preferably 35 to 36% by weight. In addition, the dichloromethane fraction obtained by fractionating the crude saponin extract with dichloromethane was confirmed that the saponin content is 25 to 35% by weight, preferably 29 to 32% by weight.

The present invention provides a hair cosmetic composition comprising the dichloromethane fraction according to another embodiment. At this time, the hair cosmetic composition according to the embodiment of the present invention may be produced as a product such as shampoo, hair conditioner, hair tonic, hair cream, etc. which are commonly used according to the embodiment. The composition of these products may contain various bases and additives suitable for the formulation of the product.

When used in the form of a hair cleanser composition, such as a shampoo or hair conditioner, it may be provided in a form comprising a hair cosmetic composition containing 1 to 5% by weight of the dichloromethane fraction of the patient-free tree. Products applied to hair in the form of rinsing with water such as shampoo and hair conditioner contain less than 1% by weight of the hair cosmetic composition according to the above embodiments, which exhibit an antimicrobial effect. When the itch elimination effect becomes insignificant and includes more than 5% by weight, there is no significant difference in the effect increase due to the excess content.

In this case, when used in the form of a hair cleaning composition, such as a shampoo or hair conditioner, selected from the group consisting of surfactants, oils, moisturizers, thickening / formulation stabilizers, pH adjusters, dispersion stabilizers, sunscreens, fragrances and preservatives It may include one or more additives. Preferably, in the case of shampoos, silicone oil, silicone gum, ammonium lauryl sulfate, polyoxyethylene lauryl ammonium sulfate, cocamide die, glycol stearate, lauramid lepofilbetaine, and lauroampocarboxyglycinate It may further include. In addition, the hair conditioner may further include myristic acid isopropyl, liquid paraffin, dimethicone, cetearyl alcohol, ketones, flavoring, and citric acid.

On the other hand, the hair cosmetic composition according to the embodiments of the present invention may be provided in the form of a hair cosmetic composition containing 1 to 5% by weight of the dichloromethane fraction of the non-patient tree. If the product is used without washing with water after applying to the hair, such as hair tonic and hair cream applied to the hair, when the hair cosmetic composition according to the above embodiments exhibits an antimicrobial effect, When the anti-dandruff and scalp removal effect of the scalp is insignificant, and contains more than 5% by weight, there is no significant difference in the increase of the effect due to the excess content.

According to the method for purifying saponin from the tree of the patient of the present invention, it is possible to obtain a purified dichloromethane fraction containing saponin of high saponin content, the hair cosmetic composition comprising the dichloromethane fraction obtained according to the excellent antibacterial effect It is excellent in the improvement of the quality of the hair, prevention of itching and dandruff of the scalp, antistatic and hair loss of the hair, and can be usefully used in the industrial field of the hair cosmetic composition.

Hereinafter, the configuration and effect of the present invention through the specific embodiments of the present invention will be described in more detail. However, the following examples are only intended to more clearly understand the invention, the scope of the invention is not limited to the following examples. Hereinafter, the present invention will be described in detail through examples of the present invention.

[Example]

1. Preparation of the Dichloromethane Fraction of the Patientless Tree

Seeds and rinds were separated from fruitless trees from November 2007 to March 2008 near the Forest Resources Research Institute of San Je-ri, Sanpo-myeon, Naju-si, Jeollanam-do. The peeled peel was dried for 15 days until the tissue of the peel became hard in the shade to reduce the moisture content. The dry peel was pulverized with a grinder to prepare a peel of the patient tree. The photograph of the skin used for the experiment is shown in FIG. 1.

 100g (83 skins) of dried dried skins are placed in a reflux extractor equipped with a reflux condenser to return the sublimated solvent back into the extractor by supplying cooling water by tap water or a cooling circulator. 1L was added.

The temperature of the outer jacket of the extractor was fixed at 70 ° C, extracted for 4 hours, and 95% methanol extract was prepared twice. The extract was cooled at room temperature, filtered through a filter paper (Watman No. 2, USA), concentrated under reduced pressure at 100 to 250 atm using a rotary vacuum concentrator (Iella, Japan), and the alcohol component in the filtrate was recovered. Methanol crude extract was prepared. The saponin concentration in the crude extract was 36% by weight. Since the crude extract is not pure saponin, a dichloromethane solvent (concentration, 95%) is added to remove other extracts (polysaccharides and phenolic compounds) extracted by moisture and alcohol of the skin, and saponin component. And other extract components which condensed. Experimental photographs for the fraction of dichloromethane are shown in FIG. 3. The upper layer is a dichloromethane layer.

The dichloromethane soluble part was concentrated under reduced pressure at 70 to 90 atm using a rotary vacuum concentrator (AIELA, Japan) to prepare a saponin fraction. The prepared saponin fraction was removed by centrifugation at 3000 rpm to remove condensation components other than saponins, which were purified and purified by dichloromethane fraction containing pure saponin bark saponin solution. At this time, the saponin concentration of the obtained dichloromethane fraction was 30%, it was confirmed that the pure saponin solution.

2. Preparation of Shampoo and Rinse from the Dichloromethane Fraction Prepared in 1

A shampoo and rinse having the composition shown in Table 1 and Table 2 were prepared from the dichloromethane fraction obtained in 1 above.

Example Shampoo ingredient Compounding cost
(weight%) Dichloromethane Fraction from Untreated Tree Bark 5.0 Silicone oil (100,000cst) 1.5 Silicone sword 1.0 Ammonium Lauryl Sulfate 12.0 Polyoxyethylene lauryl ammonium sulfate 4.0 Cocamide Diei 3.0 Glycolstearate 1.0 Lauramid Le Popilbetaine 3.0 Lauro Ampocarboxyglycinate 3.0 Coloring, fragrance, preservative Quantity Distilled water Balance

Example Rinse (Hair Conditioner) ingredient Compounding cost
(weight%) Dichloromethane Fraction from Agar Bark 5.0 Myristic acid isopropyl 1.0 Liquid paraffin 4.0 Dimethicone (10,000cst) 1.0 Cetearyl alcohol 3.5 Ketonesage 0.02 Spices 1.0 Citric acid 0.01 Distilled water Balance

Comparative Example Preparation of Shampoo and Rinse of Comparative Example

As a comparative example, shampoo (trade name: elastin) and rinse (trade name: elastin) sold by LG Household & Health Care Co., Ltd. were prepared.

In order to test the hair conditioning effect and the antistatic effect, antibacterial effect and scalp cleaning effect of the shampoo and rinse (hair conditioner) according to the above Examples and Comparative Examples was experimented as follows.

[Experimental Example]

1. Hair conditioning effect and antistatic effect

The shampoo and rinse of the comparative example and the shampoo and rinse (hair conditioner) prepared in the above example were used by 10 sensory evaluation specialists, and the hair conditioning effect and the antistatic effect were compared for each, but the 5-point scale method (5 = The best effect; 4 = the effect is very good; 3 = the effect is usually good; 2 = the effect is slightly good 1 = no effect), and the evaluation score was averaged.

As a specific evaluation method, each hair was shampooed and rinsed (hair conditioner), and the hair was dried with a hair dryer, and then the hair conditioner and the hair were combed 20 times to evaluate the hair conditioning effect and the antistatic effect. The results are shown in Table 3 below, respectively.

Evaluation item     Example     Comparative example Hair conditioning effect 4.1 2.8 Antistatic effect 2.2 0.3

2. Paper Disc Test

Paper Disc Test was performed to check the antimicrobial activity against the causative agents of shampoo and rinse prepared in the above Example. First, in order to activate the test strain phytirosporum obale was precultured for 5 days in a Potato dextrose broth (containing 1% corn oil) medium. The culture medium thus prepared was plated on a solid medium (Potato dextrose broth + 1.5% agar) and dried. From the dichloromethane fraction obtained in Example 1, a 10% aqueous saponin solution was prepared, instilled in 40 µl each on a paper disc of 8 mm in diameter, and then placed on a solid medium prepared above. The antimicrobial activity was evaluated by observing the germ growth blocking area around the paper disc and measuring the size of the ring ring. The antimicrobial test results are as shown in FIG. As can be seen in Figure 4, the growth rate of the bacteriophage growth of 10% aqueous solution of the tree bark saponin was 10mm ± 2mm appeared to have an antibacterial effect against the cause of dandruff.

3. Scalp condition observation

After using the shampoo and rinse three times in Examples and Comparative Examples, the condition of the scalp was observed. When the shampoo and rinse (hair conditioner) of the comparative example were used, the pores of the scalp were clogged with silicone oil, but when the shampoo and rinse of the example were used, the periphery of the pores was clean.

As described above, the shampoo and rinse (hair conditioner) of the embodiment have excellent anti-dandruff effect and antistatic effect according to the antimicrobial effect, and improve the quality of the hair when used for a long time, and increase the glossiness of the hair surface to confirm that it is useful. It was. Therefore, by using the hair cosmetic composition according to the present invention, it is possible to expect the effect of improving the hair and prevent hair aging.

1 is a picture of the bark of the tree without a patient used an embodiment of the present invention.

Figure 2 is a photograph of the seed of the tree.

Figure 3 is a photograph of a non-patient bark saponin fraction dichloromethane according to an embodiment of the present invention. The upper layer is the dichloromethane fraction.

Figure 4 is a photograph of the antimicrobial effect test medium against the causative agent of dandruff using saponin bark of the present invention.

Claims (13)

Preparing a rind or seed of a patient tree; The skin or seed of the patient-free tree is refluxed for 3 to 5 hours at a temperature of 60 to 80 ° C. in the presence of at least one alcohol selected from the group consisting of C ₁ to C ₅ lower alcohols, or a mixture of the alcohol and water. Extracting to obtain a saponin crude extract having a saponin content of 30 to 40% by weight; And Obtaining a dichloromethane fraction of the obtained saponin crude extract, Saponin content from the patient tree, characterized in that the saponin content in the fraction is 25 to 35% by weight. The method of claim 1, wherein the alcohol is methanol or butanol. The method of claim 1, further comprising: concentrating the fraction of dichloromethane under reduced pressure at 50 to 100 atmospheres; And The method for purifying saponin further comprising the step of centrifuging the saponin fraction concentrated under reduced pressure as described above at 2000 to 4000 rpm. Bark or seedling of a non-patient tree extracted under reflux for 3 to 5 hours at a temperature of 60 to 80 ° C. using at least one alcohol selected from the group consisting of C ₁ to C ₅ lower alcohols or a mixture of the alcohol and water as a solvent. A dichloromethane fraction of a patient-free tree, characterized in that the saponin content obtained by fractionating the crude saponin extract of dichloromethane is 25 to 35% by weight. The dichloromethane fraction of claim 4, wherein the alcohol solvent is methanol or butanol. A hair cosmetic composition comprising the dichloromethane fraction according to claim 4. The hair cosmetic composition according to claim 6, wherein the dichloromethane fraction comprises 1 to 5% by weight. Shampoo comprising the hair cosmetic composition of claim 6. 9. The shampoo of claim 8 wherein the shampoo is silicone oil, silicone gum, ammonium lauryl sulfate, polyoxyethylene lauryl ammonium sulfate, cocamide die, glycol stearate, lauramid lepofilbetaine, and lauroampocarboxyglycol. A shampoo further comprising sinate. A hair conditioner comprising the hair cosmetic composition of claim 6. 11. The hair conditioner of claim 10, wherein the hair conditioner further comprises myristic acid isopropyl, liquid paraffin, dimethicone, cetearyl alcohol, ketones, flavors, and citric acid. A hair tonic comprising the hair cosmetic composition of claim 6.       A hair cream comprising the hair cosmetic composition of claim 6.

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