JP2014218479A - Hair restorer for scalp - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a hair restorer for scalp which can be suitable for continuous daily use, having an excellent restorable effect from mulberry bark extract.SOLUTION: A hair restorer for scalp contains an effluent obtained by extracting an extract from mulberry bark with ethanol, hydrous ethanol, methanol, hydrous methanol, acetone, or hydrous acetone; dissolving the extract concerned in hydrous ethanol with ethanol concentration of 63-67% to allow synthetic adsorption resin which consists of styrene divinylbenzene copolymer having no ion exchange group and which has a porous structure with pores having a most frequent radius of 50-500 Å to adsorb; and eluting the adsorbing component concerned in ethanol or hydrous ethanol with ethanol concentration of 90% or more.

Description

  The present invention is a hair growth agent for scalp comprising a hair cycle conversion promoting component contained in mulberry white skin extract as an active ingredient, and the feeling of use that can be suitably used for daily continuous use is remarkable. The present invention relates to an improved scalp hair restorer.

Hair is an important factor that affects the appearance of human beings, but in modern society, an increasing number of people suffer from alopecia due to aging, changes in dietary habits, social stress, and the like.
There are many types of alopecia, but the main ones include androgenetic alopecia, diffuse alopecia (alopecia seen in women), and alopecia areata (transient).
Of these, transient alopecia areata is often completely cured by dermatological treatment, but the former two are intractable and difficult to treat.
“Male pattern baldness” has a strong genetic factor, and its cause is considered to be mainly due to male hormones, peripheral circulation disorders, and the like. Moreover, although not the main cause, abnormal sebum secretion, excessive occurrence of dandruff, malnutrition, etc. are also considered to have an effect.
Moreover, “diffuse alopecia” seen in women is thought to be caused by insufficient blood flow to the hair follicle, excessive hair care due to hair washing, brushing, and the like.

About 90% of normal human hair is in a growth period (a period when hair grows), and about 10% is in a resting period (a period when hair growth stops and falls off).
Alopecia is a condition caused by the suppression of hair follicle cell proliferation and the entry of hair that should originally be in the growth phase into the resting phase.
Therefore, the present inventors consider that a substance that promotes the proliferation of hair follicle cells or a substance that converts resting hair into growing hair can be an effective hair restorer in order to improve alopecia, As a result of repeated studies, it was found that the mulberry bark extract has an effect of promoting hair cycle conversion from the resting stage to the growing stage (see, for example, Patent Document 1).

However, in addition to ingredients that promote hair cycle conversion, mulberry white skin extract has a strong ripening-like unpleasant odor, which is extremely difficult to use on a daily basis as a hair restorer. Met.
In addition, the hair feels rough after use (smoothness is lost) and becomes soft (loss of stiffness), and there are many problems in the feeling of use as a hair restorer.
Moreover, the hair cycle conversion promoting component in the mulberry white skin extract has not been specified, and it has been extremely difficult to specifically separate the hair cycle conversion promoting component and the component that inhibits the feeling of use.

Japanese Patent No. 3505200

Nishinichi Dermatology vol.58 (1996) No.4 p619-624

  An object of the present invention is to solve the above-mentioned problems and to provide a hair growth agent for scalp that has excellent hair growth action derived from mulberry white skin extract and can be suitably used for daily continuous use.

  As a result of extensive studies, the present inventors dissolved the mulberry bark extract in water-containing ethanol in a specific ethanol concentration range and then adsorbed it onto a specific type of synthetic adsorption resin, and eluted the adsorbed component. It has been found that the hair cycle conversion promoting component can be specifically recovered by separating the hair cycle conversion promoting component and the component inhibiting the feeling of use of the scalp hair restorer very easily and safely.

The present invention has been made based on these findings.
In the present invention according to [Claim 1], an extract is obtained from mulberry bark using a solvent shown in (A) below; the extract is dissolved in hydrous ethanol having an ethanol concentration of 63 to 67%. It is made to adsorb | suck to the synthetic | combination adsorption resin shown to the following (B) in the state made into the ;; The hair growth agent for scalp containing the eluate obtained by eluting the said adsorption component with the solvent shown to the following (C) .
(A): Ethanol, hydrous ethanol, methanol, hydrous methanol, acetone, or hydrous acetone.
(B): A synthetic adsorption resin comprising a styrene-divinylbenzene copolymer having no ion exchange group and having a porous structure having pores with a most frequent radius of 50 to 500 mm.
(C): ethanol or hydrous ethanol having an ethanol concentration of 90% or more.
The present invention according to [Claim 2] is an eluate containing the components shown in the following (D) and (E) and substantially free of the components shown in the following (F). The hair growth preparation for scalp according to claim 1.
(D): β-tocophenol.
(E): For the extract obtained by extracting from the mulberry bark using the solvent shown in (A) above, using a column shown in (G) below at a flow rate of 0.9 mL / min and a column temperature of 45 ° C. A component contained in a peak detected at a measurement wavelength of 210 nm during a retention time of 22 to 28 minutes when developed by high-performance liquid chromatography under the condition of moving from hydrous methanol having a methanol concentration of 60% to 100% methanol.
(F): For the extract obtained by extracting from the mulberry bark using the solvent shown in (A) above, using a column shown in (G) below at a flow rate of 0.9 mL / min and a column temperature of 45 ° C. A component contained in a peak detected at a measurement wavelength of 210 nm during a retention time of up to 19 minutes when developed by high performance liquid chromatography under the condition of moving from hydrous methanol having a methanol concentration of 60% to 100% methanol.
(G): A column packed with an octadecylsilylated silica gel carrier shown in (H) below, having a column inner diameter of 4.6 mm and a column length of 25 cm.
(H): Octadecylsilylated silica gel having a carbon content of 15% (w / w) having a structure represented by the following structural formula (1) on the surface, which is a spherical support having an average pore size of 8 nm and an average particle size of 5 μm Carrier.

The present invention according to [Claim 3] is described in claim 1 or 2, wherein the hair-restoring agent has the characteristics shown in the following (I) to (L) when used by applying to the scalp externally. It is related with the hair restorer for scalp.
(I): A feature that promotes the action of converting resting hair into anagen hair.
(J): A feature that does not give an unpleasant odor to hair.
(K): A feature that maintains the slipperiness of hair.
(L): A feature that maintains the elasticity of hair.
The present invention according to [Claim 4] is the scalp according to any one of Claims 1 to 3, wherein the synthetic adsorption resin according to (B) is a synthetic adsorption resin having pores having a radius of 200 to 300 mm. It relates to a hair restorer.
The present invention according to [Claim 5] is the hair growth for scalp according to any one of claims 1 to 4, wherein the ethanol concentration when the extract is dissolved in hydrous ethanol is 64 to 66%. It relates to the agent.
The present invention according to [Claim 6] relates to a hair cosmetic composition, a hair styling composition, or a hair washing composition comprising the hair growth agent for scalp according to any one of claims 1 to 5.
The present invention according to [Claim 7] is to extract an extract from mulberry bark using a solvent shown in (A) below; the extract is dissolved in hydrous ethanol having an ethanol concentration of 63 to 67% Adsorbed on the synthetic adsorption resin shown in the following (B); and eluting the adsorbed component in the solvent shown in (C) below; and containing the obtained eluate; The present invention relates to a method for producing a hair restorer for scalp.
(A): Ethanol, hydrous ethanol, methanol, hydrous methanol, acetone, or hydrous acetone.
(B): A synthetic adsorption resin comprising a styrene-divinylbenzene copolymer having no ion exchange group and having a porous structure having pores with a most frequent radius of 50 to 500 mm.
(C): ethanol or hydrous ethanol having an ethanol concentration of 90% or more.
The present invention according to [Claim 8] is used to produce a hair growth agent for scalp by extracting from mulberry white skin using a solvent shown in (A) below; In a state dissolved in 63-67% water-containing ethanol, it is adsorbed on the synthetic adsorption resin shown in (B) below; the adsorbed component is eluted with the solvent shown in (C) below; And a method for improving the feeling of use of the hair growth agent for scalp.
(A): Ethanol, hydrous ethanol, methanol, hydrous methanol, acetone, or hydrous acetone.
(B): A synthetic adsorption resin comprising a styrene-divinylbenzene copolymer having no ion exchange group and having a porous structure having pores with a most frequent radius of 50 to 500 mm.
(C): ethanol or hydrous ethanol having an ethanol concentration of 90% or more.

The present invention makes it possible to separate the 'hair cycle conversion-promoting component' and the 'component inhibiting the feeling of use as a scalp hair restorer' contained in the mulberry white skin extract by an extremely easy and safe method. And
The present invention is a scalp which has no intense sensation-like unpleasant odor when the conventional mulberry white skin extract is directly blended with a hair-growth agent, and has improved hair loss, softening, etc. after use. It is possible to provide a hair restorer.
Thereby, this invention makes it possible to provide the hair growth agent for scalp which has the outstanding hair growth effect | action by the hair cycle conversion promotion effect | action and can be used everyday.

In Experiment 3, it is a figure which shows the result of having analyzed the mulberry bark extract (the extract obtained by extracting with 70% EtOH and then treating with diethyl ether) by HPLC. In Experiment 5, it is a figure which shows the result of having analyzed the mulberry bark extract (the extract obtained by extracting with 70% EtOH and then treating with ethyl acetate) by HPLC. (A) In Experiment 6, it is a figure which shows the result of having analyzed the mulberry white bark extract (liquid which extracted 70% EtOH and prepared EtOH concentration 65%, and passed through the synthetic adsorption resin column) by HPLC. (B) In Experiment 6, it is a figure which shows the result of having analyzed the HPLC of the purified mulberry bark extract (liquid eluted with 99% EtOH from the synthetic adsorption resin column). (A) In Test Example 7, a photograph image of a liquid color of mulberry white skin extract (unpurified product). (B) A photographic image of the liquid color of the purified mulberry bark extract.

Hereinafter, the present invention will be described in detail.
The present invention is a hair restorer comprising a hair cycle conversion promoting component contained in mulberry white skin extract as an active ingredient, and the feeling of use that can be suitably used for daily continuous use is significantly improved. The present invention relates to a hair growth agent for scalp.

[material]
The present invention uses mulberry white skin as a raw material. Here, mulberry bark refers to the root bark of a plant belonging to the genus Morus. Here, as plants of the genus Mulberry, for example, M.lhou (logwa), M.bombycis (Yamagwa), M.laevigata (Nagamiguwa), M.tiliaefolia (Keguwa), M.boninensis (Ogasawa raguwa), M. Examples include serrata (red mulberry), M.rubra (red mulberry), M.alba (karaya magwa, mugwa, white mulberry), M.nigra (kuromiguwa), M.mesozygia (black mulberry).
Among these, in particular, it refers to the root bark of M. alba and M. lhou.

  The raw material of mulberry bark is desirably used for extraction after being appropriately shredded or pulverized. Further, it may be used for extraction after being ground, crushed, powdered or the like.

[Extract]
In the present invention, it is necessary to obtain an extract (mulberry bark extract: crude extract) from the mulberry bark raw material using an extraction solvent.
Here, as the extraction solvent, one or more hydrophilic organic solvents selected from ethanol, methanol, and acetone or an aqueous solution thereof (hydrous organic solvent) can be used. Preferably, an organic solvent aqueous solution (aqueous organic solvent) having an organic solvent concentration of 65 to 99%, preferably 68 to 95%, more preferably 70 to 90% is used as the extraction solvent.
The amount of the extraction solvent used is 5 to 20 times, preferably 8 to 15 times the amount of the extraction solvent relative to the mulberry bark raw material (weight).

The extraction time is 1 day or more, preferably 2 days or more, more preferably 3 days or more, further preferably 5 days or more, particularly preferably 7 days or more when performed at room temperature (10 to 30 ° C.). desirable. The upper limit is within 14 days, preferably within 10 days.
When the extraction is performed under heating conditions (for example, 40 to 80 ° C.), 0.5 to 48 hours, preferably 1 to 24 hours, more preferably 1.5 to 12 hours, further preferably 2 to 10 hours, and particularly preferably 3 to 8 hours. It is preferable to carry out over time.
The extraction operation may be left still, but it is desirable to perform stirring and mixing.
Moreover, when using methanol or hydrous methanol as an extraction solvent, it is desirable to carry out by heating and refluxing at a high temperature.

After the extraction, concentration or the like may be performed to remove the hydrophilic solvent or moisture, and then liquid-liquid extraction may be performed using a lipophilic organic solvent. Here, as the lipophilic organic solvent, ethyl acetate, diethyl ether, benzene, toluene, xylene, or the like can be used.
The amount of the lipophilic organic solvent used is 0.1 to 3 times, preferably 0.2 to 2 times, more preferably 0.3 to 1 times the amount of the raw mulberry bark (weight). The operation may be performed after stirring and mixing.
As the distribution operation, for example, liquid-liquid countercurrent distribution is appropriate. When the organic solvent layer is collected, and the solvent is distilled off and dried, a component having a hair restoring action is obtained.

[Dissolution in water-containing ethanol with specific ethanol concentration]
In the present invention, after the extraction, it is necessary to make the extract dissolved in water-containing ethanol having an ethanol concentration of 63 to 67%. Here, the lower limit of the ethanol concentration in the hydrous ethanol is 63% or more, preferably 63.5% or more, more preferably 64% or more, and further preferably 64.5% or more. When the ethanol concentration is low, removal of contaminants with high water solubility is not sufficient, and the usability as a scalp hair restorer is unfavorable.
The upper limit of the ethanol concentration in the hydrous ethanol is 67% or less, preferably 66.5% or less, more preferably 66% or less, and still more preferably 65.5% or less. When the ethanol concentration is high, the hair cycle conversion promoting component (active ingredient) tends to flow out without being adsorbed by the synthetic resin, and the titer as a scalp hair restorer is unfavorable.
Considering these points, the ethanol concentration is preferably 63 to 67%, preferably 63.5 to 66.5%, more preferably 64 to 66%, still more preferably 64.5 to 65.5%, and most preferably about 65%. is there.
In the dissolving operation in the water-containing ethanol, it is necessary to accurately adjust the ethanol concentration.

  The amount of hydrous ethanol is 5 to 20 times, preferably 8 to 15 times the amount converted to the raw mulberry bark (weight).

Here, when a solvent other than ethanol is used in the above extraction operation, or when liquid-liquid extraction using a lipophilic organic solvent is performed, these solvents are removed by concentrating to dryness, etc. An operation for adding a solvent having an ethanol concentration is required.
In this regard, it is preferable to use ethanol or hydrous ethanol as the extraction solvent used in the extraction operation.

[Adsorption to synthetic adsorption resin and recovery]
-Synthetic adsorption resin In this invention, after making it the state melt | dissolved in the said water-containing ethanol, operation which makes the said solution contact the synthetic adsorption resin of a specific structure, and adsorbs a part of said melt | dissolution component is performed.
Here, as a synthetic adsorption resin, a styrene-divinylbenzene copolymer having no ion exchange group (see structural formula (2): 'n' and 'm' in the structural formula are positive integers indicating the degree of polymerization) It is necessary to use a synthetic adsorption resin consisting of

As the most frequent radius of the pores of the synthetic adsorption resin, it is necessary to use 50 to 500 mm, preferably 200 to 300 mm.
The average particle size of the synthetic adsorption resin is 0.2 to 1 mm, preferably 0.25 to 0.8 mm. As the particle size distribution, it is desirable to use particles having a particle size of 0.25 mm or more, 80% or more, more preferably 85% or more, and still more preferably 90% or more.
Specific examples of such synthetic resins include Diaion HP-20 (manufactured by Mitsubishi Chemical Corporation).

-Adsorption treatment In the adsorption treatment to the synthetic adsorption resin, it is desirable to equilibrate the resin before adsorption. Specifically, it is desirable to wash the synthetic adsorption resin with water-containing ethanol having the same ethanol concentration as the water-containing ethanol solution (rinsing, column passage, etc.).

The adsorption treatment may be performed by bringing the “synthetic adsorption resin” and the “solution obtained by dissolving the extract into water-containing ethanol” into contact with each other. Specifically, it is desirable to carry out in such a mode that the synthetic adsorption resin is packed in a column and the aqueous ethanol solution is passed through the column.
Further, even when the synthetic adsorption resin is not packed in the column, it can be performed by immersing the synthetic adsorption resin in the solution.
The amount of the synthetic adsorption resin (capacity) used is 0.1 times or more, preferably 0.2 times or more, more preferably 0.4 times or more, still more preferably 0.5 times or more of the mulberry bark raw material (weight), Particularly preferably, the amount is 0.8 times or more, more preferably 1 time or more. If the amount of the synthetic adsorption resin used is too small, the adsorption may not occur sufficiently, which is not preferable. Although there is no restriction | limiting in particular as an upper limit of usage-amount, when economical consideration is considered, it is 10 times or less with respect to mulberry skin raw material (weight), Preferably it can mention 5 times or less.
After passing through the column, it is desirable to perform washing treatment (rinsing, column passage, etc.) with water-containing ethanol having the same ethanol concentration as the water-containing ethanol solution.

-Recovery treatment Recovery of the active ingredient from the synthetic adsorption resin can be eluted using hydrous ethanol having a high ethanol concentration. Here, the ethanol concentration is preferably 90% or more, preferably 95% or more, more preferably 98% or more, still more preferably 99% or more, and particularly preferably 99.5% or more. Most preferably, 100% ethanol is used.
When the ethanol concentration is low, separation of the hair cycle conversion promoting component (active component) from the synthetic adsorption resin from the resin is not sufficient, and the titer as a hair restorer is unfavorable.

When adopting an aspect in which the synthetic adsorption resin is packed and adsorbed, it is possible to collect the eluate containing the active ingredient by passing ethanol or hydrous ethanol through the column.
Moreover, even if it is a case where the aspect which does not fill a column is employ | adopted, it is possible to collect | recover the active ingredients eluted in the immersion liquid by immersing synthetic adsorption resin in the said extract solution.

  The amount of ethanol or water-containing ethanol used is desirably 0.5 times or more, preferably 1 time or more, more preferably 2 times or more of ethanol or water-containing ethanol with respect to the synthetic adsorption resin (volume). If the amount used is too small, the active ingredient cannot be sufficiently recovered, which is not preferable. In addition, the upper limit of the amount used is 40 times or less, preferably 30 times or less, more preferably 20 times or less, even more preferably 10 times or less, particularly preferably in consideration of the effort to concentrate the active ingredient. The amount is desirably 5 times or less.

The column eluate obtained here is recovered as a purified mulberry bark extract. Here, when solid residue or dust floats in the solution, it is desirable to remove it by filtration or the like.
In addition, the column eluate may be dried by performing a drying treatment. As a drying process, it can carry out by the reduced-pressure drying process using an evaporator etc., for example.
The dried product can be redissolved using a hydrophilic organic solvent or a hydrous hydrophilic organic solvent of 65% or more. Here, as the hydrophilic organic solvent or the hydrous hydrophilic organic solvent, ethanol or hydrous ethanol is suitable.

[Purified Mulberry Bark Extract]
The purified mulberry bark extract obtained in the above step (the column eluate, dried product, redissolved solution, etc.) contains many hair cycle conversion promoting components without disappearing, and the feeling of use as a hair restorer It is a composition in which the content of contaminant components that lower the content is significantly reduced.

-Hair cycle conversion promoting component The purified mulberry bark extract contains at least two components having a hair cycle conversion promoting activity. Here, the hair cycle conversion promoting action refers to the action of converting resting hair to anagen hair. As the final effect of promoting the hair cycle conversion promoting action, hair growth (hair growth, hair nourishment) is significantly promoted.

The hair cycle conversion promoting action component is a column in which an octadecylsilylated silica gel carrier is packed with respect to an extract (mulberry bark extract: crude extract) obtained by extracting from the mulberry bark using the extraction solvent. High-performance liquid chromatography (HPLC) using a column with an inner diameter (φ) of 4.6 mm and a column length of 25 cm under the conditions of moving from hydrous methanol with a methanol concentration of 60% to 100% methanol at a flow rate of 0.9 mL / min and a column temperature of 45 ° C. ), It is included in the '8th fraction' and '10th fraction' obtained by fractionation in order of increasing hydrophilicity.
Here, the octadecylsilyl silica gel support is a spherical support having an average pore diameter of 8 nm and an average particle diameter of 5 μm, and has a structure represented by the following structural formula (1) on the surface and a carbon content of 15% (w / w) octadecylsilylated silica gel support.

Here, the component contained in the “eighth fraction” is specifically measured during a retention time of 22 to 28 minutes when developed by high performance liquid chromatography (HPLC) under the above conditions. It is a component contained in a peak detected at a wavelength of 210 nm.
In addition, the component contained in the “10th fraction” specifically refers to a measurement wavelength between retention times of 29 to 34 minutes when developed by high performance liquid chromatography (HPLC) under the above conditions. It is a component contained in the peak detected at 210 nm. The specific compound name of the component contained in the fraction is β-tocophenol.

The purified mulberry bark extract is obtained by recovering most of the hair cycle conversion promoting components contained in the mulberry bark extract (crude extract).
Here, “mostly recovered” specifically means that the total area of peaks detected at a measurement wavelength of 210 nm after the retention time of 22 minutes is included in the mulberry skin extract (crude extract). 80% or more of the total area of the detected peak of the component, preferably 90% or more, more preferably 90% or more.

-Contaminants The purified mulberry skin extract is substantially free of impurities that reduce the feeling of use as a hair growth agent for scalp.
Specifically, the contaminant component is an extract (mulberry bark extract: crude extract) obtained by extracting from the mulberry bark using the extraction solvent and packed with the octadecylsilylated silica gel carrier. Using a column with a column inner diameter (φ) of 4.6 mm and a column length of 25 cm, and moving from hydrous methanol with a methanol concentration of 60% to 100% methanol at a flow rate of 0.9 mL / min and a column temperature of 45 ° C. This refers to a component contained in a peak detected at a measurement wavelength of 210 nm within a retention time of 19 minutes when developed by chromatography (HPLC).

The purified mulberry bark extract has a measurement wavelength of up to 19 minutes, preferably up to 18 minutes, more preferably up to 17 minutes, and even more preferably up to 16 minutes. The component contained in the peak detected at 210 nm is not substantially contained.
Here, “substantially free” means that the total area of detection peaks of the contaminating components contained in the mulberry bark extract (crude extract) is 1/5 or less, preferably 1/10. Hereinafter, the peak is more preferably 1/20 or less.

[Scalp hair restorer]
-Characteristic The hair growth agent for scalp of this invention contains the mulberry white skin extract refinement | purification products (the above-mentioned column eluate, dry matter, redissolved solution, etc.) obtained at the above-mentioned process.
Here, the said hair growth agent for scalp exhibits the remarkable hair growth (hair growth, hair nourishing) effect by applying to the scalp externally by the effect | action of the component which has the said hair cycle conversion promotion effect.

Further, the scalp hair restorer has an excellent feeling of use that can be suitably used for daily continuous use due to the characteristics that the purified mulberry skin extract does not substantially contain the impurities.
(i) Here, as an excellent feeling of use of the hair growth agent for scalp, specifically, there is no unpleasant odor when applied to the scalp externally. In addition, when the mulberry bark extract (crude extract) is directly blended with a hair-growth agent, it is not resistant to daily use due to a strong unpleasant odor like ripening.
(ii) In addition, the scalp hair restorer has the effect of maintaining the slipperiness (smoothness) of the hair without being rough when applied to the scalp externally. Thereby, an action suitable for the case where the entire hair is desired to be physically smooth hair is exhibited. In addition, when a mulberry white skin extract (crude extract) is directly blended with a hair-growth agent, the hair becomes rough and slipperiness (feeling smooth) is lost.
(iii) Furthermore, the scalp hair restorer has the effect of maintaining the elasticity (elasticity when bent) of the hair when applied externally to the scalp. Thereby, an action suitable for the case where it is desired to physically increase the volume of the entire hair is achieved. In addition, when a mulberry white skin extract (crude extract) is directly blended and used in a hair growth agent, the elasticity of the hair is lost and the hair is softened.

-Dosage form The hair restorer for scalp of this invention can melt | dissolve in fats and oils, such as ethanol containing ethanol concentration 65% or more of ethanol, ethanol, and camellia oil, and cream, and can be used as a hair restorer.
The compounded amount of the purified mulberry bark extract is 0.001% (w / w) or more, preferably 0.01 (w / w) or more, more preferably 0.1% (w / w) of the total weight of the hair restorer in terms of solid content. It is preferable to blend in the proportion of w) or more. When the blending amount is too small, the hair-growth effect cannot be sufficiently obtained, which is not preferable.
Examples of the upper limit include 5% (w / w) or less, preferably 2% (w / w) or less.

  Moreover, as another raw material component mix | blended with the said hair restorer, what is applied to a normal hair restorer can be used. For example, hydrocarbons, waxes, fats and oils, esters, higher fatty acids, higher alcohols, surfactants, fragrances, pigments, preservatives, preservatives, excipients, cooling agents, wetting agents, antioxidants , UV protective agents, alcohols, pH adjusters, fragrances and the like can be blended. In addition, keratolytic agents for epidermis, blood circulation promoters, cell activators, local stimulants, and the like, which are other hair-growth active ingredients, can be blended. Moreover, a disinfectant, an anti-inflammatory agent, an antiseborrheic agent, an antidiarrheal agent, etc. can be mix | blended.

  The scalp hair restorer of the present invention can be in any form as long as it can be externally applied to the scalp. For example, it can be in the form of cream, ointment, lotion, etc. as a medicine or quasi drug.

[Cosmetics for hair, hair styling, hair washing]
The hair growth agent for scalp of this invention can be mix | blended as a component of cosmetics for hair, a hair-styling agent, or a hair-washing agent. For example, it can be blended in hair cream, hair tonic, hair lotion, hair liquid, hair conditioner, hair treatment, hair spray, shampoo, rinse, shampoo and rinse.
As content in this case, it is desirable to adjust according to the range of the compounding quantity quoted by the said hair restorer. When the blending amount is too small, the hair-growth effect cannot be sufficiently obtained, which is not preferable.
In addition, the raw material component used for normal manufacture can be mix | blended as another raw material component mix | blended with cosmetics for hair, a hairdressing agent, and a hair-washing agent.

  EXAMPLES Hereinafter, although an Example is given and this invention is demonstrated, the scope of the present invention is not limited by these.

[Test Example 1] “Examination of extraction solvent”
A solvent capable of extracting hair cycle conversion promoting components (F-8 fraction and F-10 fraction shown in the following HPLC analysis) from the raw mulberry bark was examined.

(1) "Preparation of aqueous ethanol extract"
By immersing 500 g of shredded mulberry skin in 5 L of 70% EtOH at room temperature for 7 days, 70% EtOH soluble components were extracted to obtain 4.4 L of extract.
Next, EtOH was distilled off from the extract to 500 mL, and then 500 mL of diethyl ether, a lipophilic organic solvent, was added and stirred vigorously for 15 minutes, then allowed to stand to separate the diethyl ether layer. I took it.
Diethyl ether was distilled off from the obtained diethyl ether layer and further dried to obtain 9.1 g of a brown dried product. 7.0 g of that was dissolved in 1 L of 70% EtOH, left in a cold place for 3 days, and further filtered to obtain a mulberry bark extract (Sample 1-1).

(2) "Preparation of mulberry bark extract (90% methanol extract)"
200 g of mulberry cuts were heated under reflux with 2 L of 90% MeOH for 2 hours to extract 90% MeOH soluble components.
Next, MeOH of the extract was distilled off, and water was added to 200 mL. To this was added 200 mL of ethyl acetate, a lipophilic organic solvent, and the mixture was stirred for 15 minutes and then allowed to stand to separate the ethyl acetate layer. did.
Ethyl acetate was distilled off from the resulting ethyl acetate layer and further dried to obtain 4.4 g of a brown dried product. 3.0 g of this was dissolved in 600 mL of 70% EtOH, left in a cold place for 3 days, and further filtered to obtain a mulberry bark extract (Sample 1-2).

(3) “Preparation of mulberry bark extract (70% acetone extract)”
By immersing 500 g of mulberry white cut with 5 L of 70% acetone for 3 days at room temperature, 70% acetone soluble components were extracted to obtain 4.5 L of extract.
Next, acetone of the extract was distilled off to make the liquid volume 500 mL, and then 500 mL of toluene, which is a lipophilic organic solvent, was added, stirred vigorously for 15 minutes, and then allowed to stand to separate a toluene layer.
Toluene was distilled off from the obtained toluene layer and further dried to obtain 10.0 g of a light brown dried product. 5.0 g of that was dissolved in 1 L of 70% EtOH, left in a cool place for 3 days, and further filtered to obtain a mulberry bark extract (Sample 1-3).

(4) "Evaluation of hair cycle conversion ability"
With respect to each of the prepared mulberry bark extracts (Sample 1-1 to Sample 1-3), a test for examining the hair cycle conversion ability of rabbits (New Zealand White) was performed as follows.
All the back body hairs of rabbits (New Zealand White) around 24 weeks of age are in the rest period. Therefore, by applying the drug at this time, only the hair of the drug application part having a hair-growth effect grows during the growth period, and a test for clearly determining the hair-growth effect becomes possible.

First, the back of a 20-21 week old rabbit was shaved using an electric clipper, and thereafter it was confirmed that the hair of the same part did not grow (that is, from the growth period to the rest period).
Six rabbits immediately after the back hair was converted to the resting period were selected as one group, the back shaved part was divided into 4 cm square, and each mulberry white skin extract was added to the center part at a rate of 0.2 once a day. Apply mL. This operation was continued until the non-treated portion was converted into a growth period.
As a control, a group to which nothing was applied was reared in the same manner (non-application group).
And the hair growth state about the hair of a test site | part was evaluated, and the result was shown in Table 1. In addition, each code | symbol which shows the evaluation of the hair growth condition in a table | surface is "+++": The hair densification is remarkable, "++": The hair densification is clear, "+": Slight hair growth is recognized, "- ": Indicates that no hair growth is observed.

As a result, it was shown that in the test group to which each mulberry bark extract was applied, the period of conversion from the rest period to the growth period was significantly shortened compared to the non-application group.
From this, it is shown that an extract obtained by extracting mulberry bark with an aqueous ethanol solution, an aqueous methanol solution, or an aqueous acetone solution contains a component (a component having a hair-growth effect) that promotes hair cycle conversion from the resting phase to the growing phase. It was done.

[Test Example 2] “Examination of hair growth effect of mulberry bark extract in humans”
The hair growth action of the mulberry white skin extract (Sample 1-1: 70% EtOH extract) was actually examined for the effect on human alopecia.

(1) “Improvement test of hair loss in male pattern alopecia patients”
Mulberry white skin extract (Sample 1-1: 70% EtOH extract) was applied daily to the scalp for 6 months to 23 male pattern baldness patients aged 38 to 60 years. The number of times of external application to the head was twice a day.
Hair growth was observed after 3 and 6 months. The results are shown in Table 2.

  As a result, it was confirmed that after 3 months, 10 out of 23 people had some soft hair on the hair loss site. After 6 months, 8 out of 23 people had hard hair, 6 had soft hair, and the remaining 9 had lost hair. That is, improvement of the hair growth state of all subjects (100%) was observed by continuous use for 6 months, and new hair was seen in 61.0% of cases, and an extremely good 'hair growth effect' was confirmed.

(2) “Improvement test of hair loss in patients with diffuse alopecia”
Mulberry white skin extract (Sample 1-1: 70% EtOH extract) was applied daily to the scalp for 6 months to 16 patients with diffuse alopecia from 35 to 63 years old. The number of times of external application to the head was twice a day.
Hair growth was observed after 3 and 6 months. The results are shown in Table 3.

  As a result, it was confirmed that after 3 months, 6 out of 16 people had some soft hair on the hair loss site. After 6 months, 6 out of 16 people had hard hair, 4 had soft hair, and the remaining 6 had lost hair. That is, with continuous use for 6 months, improvement in the hair growth state of all subjects (100%) was observed, and in 63.0% of cases, new hair was seen, and an extremely good 'hair growth effect' was confirmed.

[Test Example 3] “Fraction that promotes hair cycle conversion in mulberry white skin extract”
In order to clarify the components contained in the mulberry bark extract (70% EtOH extract), the above-mentioned hair cycle conversion ability was analyzed by HPLC.
The mulberry bark extract (Sample 1-1: 70% EtOH extract) was developed by HPLC (High Performance Liquid Chromatography). As the column, TSKgel ODS-80TM (made by TOSOH, φ4.6mm × L 250mm, packed carrier (average pore diameter 8nm, average particle diameter 5μm, carbon content 15% (w / w), the above structural formula (1)) The measurement conditions were as follows: measurement wavelength: 210 nm, flow rate: 0.9 mL / min., Column temperature: 45 ° C., mobile phase: 60% MeOH → 100% MeOH (22 min) .) → 100% MeOH (22 min.)
As a result, a chromatogram having a peak shown in FIG. 1 was obtained.

The chromatogram shown in FIG. 1 was divided into F-1 to F-11 fractions in descending order of water compatibility, and each fraction was dissolved in 70% EtOH to a concentration of 1% (w / w).
Each fraction was subjected to a test for examining the hair cycle conversion ability of rabbits (New Zealand White) in the same manner as described in Test Example 1 (4).
In addition, as a control, a group to which only 70% EtOH was applied (70% EtOH application group) and a group to which nothing was applied (non-application group) were reared in the same manner and subjected to evaluation.

As a result, in the test group to which 'F-8 fraction' and 'F-10 fraction' were applied, the period of conversion from the resting phase to the growth phase was significantly shortened compared to the non-application group. Indicated.
On the other hand, no difference was observed in the remaining F-1 to F-7, F-9, and F-11 fractions compared to the non-application group.
From this, it was shown that the component which accelerates | stimulates the hair cycle conversion contained in mulberry white skin is a component contained in F-8 and F-10. The component contained in F-10 was identified as β-tocophenol.

[Test Example 4] “Usage feeling of mulberry bark extract (unpurified product)”
It was confirmed that the mulberry bark extract contains hair cycle conversion promoting components (F-8 fraction and F-10 fraction). Therefore, the usability when the above mulberry white skin extract (Sample 1-1: 70% EtOH extract) was used as a hair growth agent for scalp was examined.

As a result, the mulberry white skin extract had an unpleasant odor close to a ripe odor and was evaluated as having difficulty in daily continuous use. Moreover, since the hair was rough, it was evaluation that slipperiness worsened.
From this, it was estimated that many of the peaks shown in the chromatograph of FIG. 1 in Test Example 3 contain many components that greatly reduce the feeling of use.

[Test Example 5] “Examination of purification method (liquid-liquid extraction) of hair cycle conversion promoting components”
In order to improve the feeling of use, a liquid-liquid that does not flow out the hair cycle conversion promoting components (F-8 fraction and F-10 fraction) and removes only the components that reduce the feeling of use. The extraction method was examined.

(1) "Examination of ethyl acetate treatment" (comparative example)
The method of Test Example 1 (1) was modified to try to perform “ethyl acetate” treatment instead of “diethyl ether” treatment after 70% EtOH extraction.
1 kg of mulberry cuts were stirred in 10 L of 70% EtOH at 45 ° C. for 4 hours to extract 70% EtOH soluble components and filtered to obtain 8 L of extract.
Next, the extract was concentrated under reduced pressure to 0.5 L, ethyl acetate (0.5 L) was added and extracted with stirring, and the ethyl acetate phase was separated and recovered. Further, ethyl acetate (0.5 L) was again added to the remaining aqueous phase, and the mixture was stirred and extracted again, and the ethyl acetate phase was separated and recovered.
A mixture of these ethyl acetate phases was dried under reduced pressure to obtain a dried product (38 g).
EtOH (2.1 kg) and purified water (0.9 kg) were added and dissolved by stirring, and stored at 4 ° C. for 7 days.
By filtering the solution, a mulberry bark extract (Sample 5-1: EtOH concentration 70%, solid content 1.1% (w / w)) was obtained.

The obtained mulberry bark extract (sample 5-1: ethyl acetate treated product) was subjected to HPLC analysis in the same manner as described in Test Example 3. The obtained chromatogram results are shown in FIG.
As a result, in the chromatogram of FIG. 2, the presence of the F-8 and F-10 fractions was confirmed, but many peaks indicating contaminants were also confirmed.
Therefore, when the ethyl acetate treatment is performed, the impurities (usability-inhibiting components) confirmed in the chromatogram of Fig. 1 (Sample 1-1: treated with diethyl ether in Test Example 1 (1)) are reduced. The effect could not be confirmed at all.

(2) "Examination of n-hexane-methanol treatment" (comparative example)
In the same manner as in the above method (1), except that the liquid-liquid extraction after 70% ethanol extraction was performed using “methanol saturated n-hexane solution” instead of the ethyl acetate treatment, An extract (Sample 5-2: EtOH concentration 70%) was prepared.

The obtained mulberry bark extract (Sample 5-2: n-hexane-methanol treated product) was subjected to HPLC analysis in the same manner as described in Test Example 3.
As a result, when n-hexane-methanol treatment was performed, the presence of the F-10 fraction was confirmed, but it was shown that the F-8 fraction was lost. This is probably because the F-8 fraction is insoluble in n-hexane.

[Test Example 6] “Examination of purification method (synthetic adsorption resin column treatment) of hair cycle conversion promoting component”
Is it possible to remove only the components that reduce the feeling of use without flowing out the hair cycle conversion promoting components (F-8 fraction and F-10 fraction) by purification using a synthetic adsorption resin column? It was investigated.

(1) “Examination of liquid flow through synthetic adsorption resin at 65% EtOH concentration” (Example)
A 50% mulberry shredded product was stirred in 500 mL of 70% EtOH at 45 ° C for 4 hours and filtered to extract 70% EtOH soluble components, and the extract (solid content 0.80% (w / w)), and water was added to prepare “EtOH concentration 65%”.
Next, the extract was passed through a Diaion HP-20 column (φ2.2 cm × L 13 cm, column volume 50 mL: manufactured by Mitsubishi Chemical Corporation) at a flow rate of 100 mL / hr, and the column was 65% EtOH (100 mL). Washed with
Here, the cleaning liquid was collected and dried under reduced pressure to obtain a dried product. 70% EtOH (120 mL) was added thereto and stirred to obtain a dissolved solution (Sample 6-1: solid content 0.44% (w / w)).

  Next, 99% EtOH (150 mL) was passed through the column to elute the adsorbed components, and the eluate was dried under reduced pressure to obtain a dried product (0.58 g). 70% EtOH (120 mL) was added thereto and dissolved by stirring to obtain a purified mulberry bark extract (Sample 6-2: EtOH concentration 70%, solid content 0.48% (w / w)).

The obtained purified mulberry bark extract (sample 6-2) and column passage liquid (sample 6-1) were subjected to HPLC analysis in the same manner as in the method described in Test Example 3. The results of the obtained chromatogram are shown in FIGS. 3 (A) and 3 (B).
As a result, as shown in FIG. 3 (B), in the purified mulberry bark extract (sample 6-2), the presence of the F-8 and F-10 fractions was confirmed, and the chromatogram ( It was confirmed that the impurities confirmed in Sample 1-1: Diethyl ether-treated product of Test Example 1 (1) were significantly reduced. On the other hand, as shown in FIG. 3 (A), it was confirmed that only the impurities were separated in the column passing solution.

(2) “Examination of liquid flow through synthetic adsorption resin at 70% EtOH concentration” (comparative example)
In the purification method (1) above, after extraction of 70% EtOH soluble component of mulberry bark, it was passed through the synthetic adsorption resin with 70% EtOH concentration (and column pretreatment was performed with 70% EtOH. Except for the above, a purified mulberry bark extract (Sample 6-3) was prepared in the same manner as (1) above.
As a result of HPLC analysis, most of the F-8 and F-10 fractions were lost in the purified mulberry bark extract (Sample 6-3).

(3) “Examination of liquid flow through synthetic adsorption resin at EtOH concentration of 60%” (comparative example)
In the purification method (1) above, after extracting 70% EtOH soluble components of mulberry bark, water was added to prepare “EtOH concentration 60%” and passed through the synthetic adsorption resin (and before the column) A purified mulberry bark extract (sample 6-4) was prepared in the same manner as (1) except that the treatment was performed with 60% EtOH.
As a result of HPLC analysis, the purified mulberry bark extract (sample 6-4) was contaminated by the chromatogram in Fig. 1 (sample 1-1: treated with diethyl ether in Test Example 1 (1)). It was confirmed that the product was not sufficiently removed and the purification was insufficient.

[Test Example 7] “Study on feeling of use of purified mulberry bark extract (evaluation of liquid color and odor)”
As a result of the above study, when purified by passing through synthetic adsorption resin (Diaion HP-20) at an EtOH concentration of 65%, the hair cycle conversion promoting component (F-8 fraction and F-10 fraction) flows out. It has been clarified that other contaminating components can be greatly reduced without the need to do so.
Therefore, the effect of the feeling of use when the purified mulberry skin extract was used as a hair growth agent for scalp was evaluated.

First, about the liquid color and odor of the purified mulberry bark extract of Test Example 6 (1) (Sample 6-2: Column purified product), the mulberry bark extract of Test Example 5 (1) (Sample 5-1: Column) Comparison with the unpurified product). The results are shown in Table 5. FIG. 4 is a photographic image diagram showing the appearance of both liquids.
As a result, although both solutions contain the same hair cycle conversion promoting component (F-8 fraction and F-10 fraction), the 'liquid color' is the unpurified column (Sample 5-1: Fig. 5) It was revealed that the purified column (sample 6-2: Fig. 4B) was much thinner than 4A).
In addition, regarding the “odor”, the unpurified column (Sample 5-1: Fig. 4A) felt an unpleasant odor like a mature rice but the purified column (Sample 6-2: Fig. 4B). There was almost no unpleasant odor and it did not affect the feeling of use.

  From this, it was shown that by purifying the mulberry bark extract using the method of Test Example 6 (1), it was possible to eliminate the problems that were difficult to use on a daily basis, especially due to the unpleasant odor like the ripe odor. It was.

[Test Example 8] “Study on feeling of use of purified mulberry bark extract (evaluation of amount adsorbed on hair)”
When the purified mulberry skin extract was used as a scalp hair restorer, the ease of absorption into hair was evaluated. In addition, the amount absorbed into hair is an important factor that affects how the drug is effective when used as a hair growth agent for scalp.

A hair bundle (2 g, 15 cm) of the same human hair of a Chinese woman (Buelux) was dried by bleaching, perm treatment and ultrasonic cleaning. After performing this process three times in total, it was rinsed with purified water and naturally dried to obtain damaged hair.
After leaving the damaged hair in a constant temperature and humidity environment (55 to 57% (RH) at 15 to 16 ° C) for 3 hours, weigh the weight with a precision electronic pan balance (Ay-220: Shimadzu Corporation). Measured and “initial weight (a)”.
Next, the sample was immersed in a solution of “sample 6-2 (column purified product)”, “sample 5-1 (column unpurified product)” or “70% EtOH” and air-dried overnight. Similarly, after standing for 3 hours in a constant temperature and humidity environment, the weight was measured, and the value was defined as “adsorption weight (b)”.
In addition, in order to calculate the adsorption amount of each sample, the value when treated (control) with 70% EtOH was measured in the same manner.
Then, using the following formula (1), “adsorption amount (c)” (mg / g: mg of extract component adsorption amount per 1 g of hair) when each sample was treated was calculated. This value corresponds to an increase in weight from the weight of the components inside the hair that flowed out by 70% EtOH treatment. The results are shown in Table 6.

  As a result, even when the column purified product (Sample 6-2) was treated, no significant difference was observed in the amount of adsorption to the hair compared to the column purified product (Sample 5-1). From this, it was shown that the amount of adsorption was not suppressed by the column purification step.

[Test Example 9] “Examination of feeling of use of purified mulberry bark extract (evaluation of friction coefficient)”
When the purified mulberry skin extract was used as a hair growth agent for scalp, the effect on the properties (friction coefficient) of the hair surface was evaluated.

40 hairs (hair dried after each sample treatment used in Test Example 8) are arranged at equal intervals between 2 cm above the slide glass, and both ends are fixed with an adhesive, and a friction sensor (friction feeling tester) is placed on the hair. : KES-SE-DC: Kato Tech Co., Ltd.) and the coefficient of friction was measured.
The friction coefficient measurement conditions were SNES: H (force gauge 20 g / V), sliding speed: 1.0 mm / sec., Static friction load: 25 g, friction sensor: silicon sensor, measurement location: 21-22 ° C, 66 % (RH).
Then, the coefficient of friction was measured at three locations and the average value was calculated to calculate “MIU (average coefficient of friction). In addition, as a control, the value treated with 70% EtOH was measured in the same manner. Shown in

As a result, when treated with 70% EtOH as a control, the MIU value was high, and “smoothness of hair (feeling smooth)” was completely lost. On the other hand, when treated with the column purified product (Sample 6-2), the MIU value was significantly lower, which was lower than when treated with the column unpurified product (Sample 5-1). .
From this, it was shown that the hair restorer prepared by purifying the mulberry white skin extract by column method of Test Example 6 (1) has the property of maintaining “easy slipperiness (smooth feeling)”. .

[Test Example 10] “Examination of feeling of use of purified mulberry bark extract (evaluation of bending feeling)”
When the purified mulberry skin extract was used as a hair growth agent for scalp, the effect on hair properties (bending feeling) was evaluated.

50 hairs (hair dried after treatment of each sample used in Test Example 8) between 5 cm on the mount are aligned and fixed uniformly with an adhesive, and a hair strain tester (KES-FB2-S- "2HB value (bending recovery property)" was measured using DC: manufactured by Kato Tech.
The measurement conditions were SNES: 20 g, bending curvature: 1.0, sample size: 5 cm, measurement location: 22 ° C., 55 to 57% (RH).
Then, the average value was calculated by measuring the values at three locations. As a control, the value treated with 70% EtOH was measured in the same manner. The results are shown in Table 8.

As a result, when treated with 70% EtOH as a control, the 2HB value was significantly higher, and “elasticity (recoverability when bent)” was completely lost. On the other hand, when treated with the purified column (sample 6-2), the 2HB value was significantly lower than that when treated with the unpurified column (sample 5-1). .
This indicates that the hair restorer prepared by column purification of mulberry white skin extract by the method of Test Example 6 (1) has the property of maintaining “elasticity (recoverability when bent)”. It has been shown to be suitable for making the hair itself physically volume up.

[Summary of Test Examples 7 to 10]
From the above examination results, the unpleasant odor possessed by the unpurified mulberry bark extract was greatly reduced by purifying the mulberry bark extract using a synthetic adsorption resin. Also, the liquid color is thin and preferable. Moreover, the said refined | purified substance had the property of maintaining the slipperiness (smooth feeling) and elasticity (recoverability when bent) of hair, when used as a hair growth agent for scalp.

From the above, it was shown that the use of the purified mulberry bark extract with a hair growth agent for scalp significantly improved the feeling of use that is extremely important for daily continuous use. .
Furthermore, in addition to the hair-growth effect by the component which has a hair cycle conversion ability, it was shown that it is suitable when maintaining the smoothness of the hair and making the hair itself physically increased in volume.

[Production Example 1] “Preparation of purified mulberry skin extract in hair scalp manufacturing”
Under the conditions clarified by the examination of the above test examples, a purified mulberry skin extract used for the production of a scalp hair restorer was produced on a large scale.

1 kg of mulberry bark shreds were stirred in 10 L of 65% EtOH at 45 ° C. for 4 hours and filtered to extract 65% EtOH soluble components to obtain 8 L of extract. Next, the extract was passed through a Diaion HP-20 column (φ8 cm × L 25 cm, column capacity: 1.26 L, manufactured by Mitsubishi Chemical Corporation) at a flow rate of 1.5 L / hr, and the column was passed through 65% EtOH (2.5 Washed with L). Then, 99% EtOH (4 L) was passed through the column to elute the adsorbed component, and the eluate was dried under reduced pressure to obtain a dried product (18 g). EtOH (2688 mL) was added thereto and dissolved by stirring, purified water (1152 mL) was added and further stirred, and stored at 4 ° C. for 7 days. The resulting solution was then filtered.
As a result, purified mulberry bark extract (EtOH concentration 70%, solid content 0.44% (w / w)) was obtained.

  The present invention is expected to be effectively used as a hair growth agent for scalp that can be used on a daily basis for male pattern alopecia and diffuse alopecia that are conventionally difficult to treat.

Claims (8)

Extract from mulberry bark using the solvent shown in (A) below to obtain an extract; the extract is dissolved in hydrous ethanol having an ethanol concentration of 63-67% and shown in (B) below A hair growth agent for scalp comprising an eluate obtained by adsorbing to a synthetic adsorption resin and eluting the adsorbed component with a solvent shown in (C) below.
(A): Ethanol, hydrous ethanol, methanol, hydrous methanol, acetone, or hydrous acetone.
(B): A synthetic adsorption resin comprising a styrene-divinylbenzene copolymer having no ion exchange group and having a porous structure having pores with a most frequent radius of 50 to 500 mm.
(C): ethanol or hydrous ethanol having an ethanol concentration of 90% or more. 2. The hair restorer for scalp according to claim 1, wherein the eluate is an eluate containing the components shown in the following (D) and (E) and substantially free of the components shown in the following (F).
(D): β-tocophenol.
(E): For the extract obtained by extracting from the mulberry bark using the solvent shown in (A) above, using a column shown in (G) below at a flow rate of 0.9 mL / min and a column temperature of 45 ° C. A component contained in a peak detected at a measurement wavelength of 210 nm during a retention time of 22 to 28 minutes when developed by high-performance liquid chromatography under the condition of moving from hydrous methanol having a methanol concentration of 60% to 100% methanol.
(F): For the extract obtained by extracting from the mulberry bark using the solvent shown in (A) above, using a column shown in (G) below at a flow rate of 0.9 mL / min and a column temperature of 45 ° C. A component contained in a peak detected at a measurement wavelength of 210 nm during a retention time of up to 19 minutes when developed by high performance liquid chromatography under the condition of moving from hydrous methanol having a methanol concentration of 60% to 100% methanol.
(G): A column packed with an octadecylsilylated silica gel carrier shown in (H) below, having a column inner diameter of 4.6 mm and a column length of 25 cm.
(H): Octadecylsilylated silica gel having a carbon content of 15% (w / w) having a structure represented by the following structural formula (1) on the surface, which is a spherical support having an average pore size of 8 nm and an average particle size of 5 μm Carrier.
3. The hair restorer for scalp according to claim 1 or 2, wherein the hair restorer has the characteristics shown in the following (I) to (L) when used by applying to the scalp externally.
(I): A feature that promotes the action of converting resting hair into anagen hair.
(J): A feature that does not give an unpleasant odor to hair.
(K): A feature that maintains the slipperiness of hair.
(L): A feature that maintains the elasticity of hair.   4. The hair growth agent for scalp according to any one of claims 1 to 3, wherein the synthetic adsorption resin described in (B) is a synthetic adsorption resin having pores having a radius of 200 to 300 mm.   The hair growth agent for scalp according to any one of claims 1 to 4, wherein the ethanol concentration when the extract is dissolved in hydrous ethanol is 64 to 66%.   A hair cosmetic, a hair styling agent, or a shampoo comprising the hair growth agent for scalp according to any one of claims 1 to 5. Extract from mulberry bark using the solvent shown in (A) below to obtain an extract; the extract is dissolved in hydrous ethanol having an ethanol concentration of 63-67% and shown in (B) below A method for producing a hair restorer for scalp, comprising: adsorbing to a synthetic adsorption resin; eluting the adsorbed component with a solvent shown in (C) below; and containing the obtained eluate.
(A): Ethanol, hydrous ethanol, methanol, hydrous methanol, acetone, or hydrous acetone.
(B): A synthetic adsorption resin comprising a styrene-divinylbenzene copolymer having no ion exchange group and having a porous structure having pores with a most frequent radius of 50 to 500 mm.
(C): ethanol or hydrous ethanol having an ethanol concentration of 90% or more. In producing a hair growth agent for scalp by extracting from mulberry white skin using the solvent shown in (A) below; the extract was dissolved in hydrous ethanol having an ethanol concentration of 63 to 67%. And adsorbed on the synthetic adsorption resin shown in the following (B); eluting the adsorbed component with the solvent shown in the following (C); and collecting the obtained eluate; A method for improving the feeling of use of the hair growth agent for scalp.
(A): Ethanol, hydrous ethanol, methanol, hydrous methanol, acetone, or hydrous acetone.
(B): A synthetic adsorption resin comprising a styrene-divinylbenzene copolymer having no ion exchange group and having a porous structure having pores with a most frequent radius of 50 to 500 mm.
(C): ethanol or hydrous ethanol having an ethanol concentration of 90% or more.