JPS63264595A - Production of physiologically active substance from cork tree bark - Google Patents

Abstract

PURPOSE:To readily obtain a substance, having excellent humectant effects, anti-inflammatory activity, etc., and useful as a blending component for cosmetics, etc., without a change of color, etc., with time, by adsorbing an extract of Cork tee bark on an adsorbent and eluting the adsorbed substance with water. CONSTITUTION:Cork tree bark which is dried tree bark of Phellodendron amurense and relative species or species of the same genus is extracted with water, hydrous alcohol or various organic solvents and the resultant extract is then brought into contact with an adsorbent in an amount of preferably 10-40 times. The adsorbed extract is subsequently eluted with water in an amount of preferably >=5 times based on the adsorbent to afford the aimed substance. Furthermore, a hydrophobic adsorbent, such as a porous polymer which is a polymer of styrene and divinylbenzene, is preferably used as the adsorbent.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a physiologically active substance from Auronicum spp., which has excellent moisturizing effects and physiologically active effects such as anti-inflammatory activity, and is highly stable.

As is well known, the extract of Aspergillus orientalis is widely used because it has physiologically active effects such as moisturizing properties and anti-inflammatory activity.
When added to cosmetics, this extract gives elasticity and tension to the skin, and is also highly safe, so it is known to be effective in various cosmetics. It is incorporated into oral compositions as an active ingredient for the prevention of periodontal disease (Japanese Patent Application Laid-open No. 57-56415), and the dry-distilled pulverized product of Aspergillus orientalis is incorporated into periodontitis therapeutics as an active ingredient for the treatment of toothache and periodontitis. (Japanese Unexamined Patent Publication No. 61-1222
No. 21), reducing the skin irritation of the surfactant by blending a hydroalcoholic extract of Aspergillus orientalis into a surfactant (Japanese Patent Application Laid-Open No. 60-56911), and adding a large amount of berberine, a physiologically active ingredient, from Aspergillus orientalis. A method for producing an aqueous extract containing the same (Japanese Patent Publication No. 62-5890) and a skin preparation for external use containing the aqueous extract (Japanese Patent Publication No. 62-5891)
(No.), as well as moisturizing cosmetics containing extract of Aspergillus orientalis (No.
Japanese Unexamined Patent Publication No. 60-258104) etc. have been proposed.

The problem that Ming is trying to solve 3: However, if the extract is added to cosmetics as it is, the yellow components such as berberine, which are called biologically active substances in the extract, will discolor or change color due to the influence of the fragrances in the cosmetics. It has the disadvantage of causing decolorization, making it undesirable as a raw material for cosmetics.

Therefore, a method for easily producing physiologically active substances with stable quality and high yield is desired.

An object of the present invention is to provide a method for easily producing a physiologically active substance having stable quality.

In order to solve the problem 1, the inventors of the present invention have conducted intensive studies to achieve the above-mentioned objective, and as a result, after performing a process of treating the extract of Aspergillus orientalis with an adsorbent, especially a hydrophobic adsorbent, it was treated with water. By elution,
Physiologically active substances can be obtained from Auronicum spp. by a simple operation, and even though the yellow component, which is usually considered to be a bioactive ingredient, is removed in the above process, it has excellent moisturizing effect and anti-inflammatory activity. In addition to obtaining effective mucus, this mucus does not denature and lose its viscosity or physiological activity even if it is redissolved in water after freeze-drying, and the yellow substance is removed during the above process. Even when incorporated into cosmetics and external preparations, the color tone does not change or bleach over time, and it has excellent stability. It can also effectively prevent or improve rough hands and skin, and is safe. high, therefore
The present inventors have discovered that this physiologically active substance can be suitably incorporated into cosmetics, external preparations, etc., and have accomplished the present invention.

Accordingly, the present invention provides a method for producing a physiologically active substance from Aspergillus orientalis, which comprises the steps of treating an extract of Aspergillus orientalis with an adsorbent and then eluting it with water to collect the resulting substance.

The present invention will be explained in more detail below.

In the method for producing a physiologically active substance from Auronicum of the present invention, the raw material, the dried bark of Auronicum amberjack of the Rutaceae family and a related species of the same genus, is mixed with water, a hydrous alcohol such as hydrous methanol, various organic solvents, For example, methanol,
ethanol, acetone.

First, a step of treating this extract with an adsorbent is performed using an extract extracted with chloroform, ethyl acetate, butanol, ether, etc.

In this case, there is no restriction on the extract of Aspergillus orientalis to be used, and an extract obtained by extracting Aspergillus orensis with hydrous alcohol, etc., or its concentrated or dried product dissolved in water may be used, but in particular, an aqueous extract of Aspergillus orensis may be used. It is preferable to use it as it is or to concentrate it in an appropriate amount and treat it with an adsorbent.

Furthermore, various treatment methods and conditions can be selected for the adsorption treatment, but it is particularly preferable to use a hydrophobic adsorbent as the adsorbent. Porous polymer spherical resin obtained by polymerizing monomers can be effectively used, and since this resin has a hydrophobic surface, it has the ability to adsorb large hydrophobic particles of organic matter by van der Waals force. have Specifically, such hydrophobic adsorbent resins include Amberlite XAD-2, XAD-4 (ROHM
(Manufactured by & Bar), Diaion HP-20, HP
-21 (manufactured by E-Ryo Kasei Co., Ltd.), Sepa beads 5P-206,5
P-207 (manufactured by Mitsubishi Kasei Corporation) is exemplified.

In addition, the amount of adsorbent to be used is appropriately selected depending on the amount of Aspergillus asparagus extract to be used, but the amount of adsorbent that can sufficiently adsorb the Aspergillus asparagus extract, that is, at least 5 times the amount of Aspergillus asparagus extract (extracted 500 d of adsorbent for 100 g of material)
In particular, it is desirable that the amount be in the range of 10 to 40 times.

Next, in the present invention, after treating the extract of Aspergillus orientalis by passing it through an adsorbent as described above, the substance eluted from the adsorbent with water is collected.

Here, the elution method can be a conventional method, for example, by gradually passing water through an adsorbent at room temperature, a mucilage aqueous solution having the desired physiologically active action can be obtained.

Note that the amount of water used for elution is 2 times the amount of adsorbent resin.
The amount is preferably 5 times or more, particularly 5 times or more.

The substance thus obtained by elution with water can be used without distilling off the solvent, or after partially or completely distilling off the solvent, depending on the product to be blended.

The substance obtained by the method for producing a physiologically active substance from Auronicum spp. of the present invention has excellent physiologically active effects such as moisturizing effect and anti-inflammatory activity, and can be used in various cosmetics and external preparations to maintain skin moisturizing properties and prevent rough hands and skin. It can be widely used by being incorporated into products to prevent or improve skin irritation, or to prevent dermatitis, etc. Note that when the physiologically active substance of the present invention is blended into various cosmetics and external preparations, the amount of the present invention is 0.01 to 50% of the total product (
% by weight).

Highlights As explained above, according to the method for producing a physiologically active substance from Auronicum oleracea of the present invention, a substance with excellent physiologically active effects such as moisturizing effect and anti-inflammatory activity can be easily obtained. Furthermore, the physiologically active substance obtained by the production method of the present invention does not denature and lose its viscosity or physiological activity even if it is redissolved in water after freeze-drying, and it does not deteriorate when incorporated into cosmetics etc. The color tone does not change over time, it is highly stable, and it is also highly safe, so it can be used as a variety of cosmetics and external preparations to keep the skin moisturized, prevent or improve rough hands and skin, and treat dermatitis, etc. It can be widely used by incorporating it into preventive products.

EXAMPLES The present invention will be specifically explained below with reference to Examples and Experimental Examples, but the present invention is not limited to the Examples below.

〔Example〕

2Ω of Auronicum water extract (equivalent to 200g of Auronicum powder)
was passed through IQ's Amberlite XAD-2 resin (manufactured by Rohm and Haas) and eluted with about 5Q of water to obtain a water-eluted portion. By freeze-drying the obtained aqueous eluate, a white to cream-colored mucous substance was obtained (yield: 10
%).

[Experimental Example 1] An ointment having the following formulation was prepared using the mucus substance obtained in the example.

White petrolatum 250g Stearyl alcohol 220 Propylene glycol 120 Sodium lauryl sulfate
15 Aurubaku mucus (product of the present invention)
10 paraoxybenzoic acid propyl 0.15
Refined ice balance
Amount: 100.0g The above ointment containing the present invention product and an ointment base having the same formulation as above but not containing the present invention product were used as specimens, and the moisturizing effect of each specimen was measured by the following method.

The test sample was continuously applied to rough skin models (8 models) created by repeatedly washing the inner side of the forearm with soap, and conductive dust was measured using a high-frequency impedance method before and on the second day of application. .

The results are shown in the figure.

Note that 0 on the impedance measurement date on the horizontal axis in the figure indicates immediately before sample application, and 2 indicates the second day of continuous sample application.

Further, in the figure, A indicates a group administered with an ointment containing the product of the present invention, B indicates a group administered with an ointment base, and C indicates no treatment.

As is clear from the figure, the average mold conductivity of the ointment application group containing the present invention product was higher than that of the ointment base application group and the untreated group, confirming that the invention product has an excellent moisturizing effect. .

[Experimental Example 2] Blood was collected from a Wistar female rat weighing 220 g under ether anesthesia, and the collected blood was washed 4 times with phosphate buffer, diluted with the washing solution, and the number of red blood cells was 1 and OX 10.
'cells/mQ, and this was used as a red blood cell suspension.

A hypotonic 0.32N solution containing the mucus substance obtained in the example (product of the present invention) as a specimen was dissolved in 0.2 d of the above red blood cell suspension.
a (10mM phosphate buffer (pH 7,4) containing 4.8
After mixing d and leaving it at room temperature for 30 minutes, 200 Or
Centrifuged at pm for 10 minutes.

The supernatant was collected, the absorbance at a wavelength of 540 nm was measured, and the hemolysis inhibition rate was calculated based on the following formula.

For comparison, the hemolysis inhibition rate was determined in the same manner as described above using a water extract of Laminaria japonica as a specimen.

The results are shown in Table 1.

Table 1 From the results shown in Table 1, it was confirmed that the mucilage substance of the present invention has a high hemolysis suppression rate and is excellent in anti-inflammatory action.

Examples of formulations of the products of the present invention are shown below. Note that all percentages hereinafter indicate weight percentages.

[Formulation example 1] Stearic acid 2.0
% stearyl alcohol 7.
0 reduction lanolin 2
．． 0 squalane 5
．． 0 octyldodecanol 6
．． 0 lipophilic type glyceryl monostearate 2.
0 Auricular mucus (product of the present invention) 1.0 Fragrance 0
．． 3 Preservative Trace amount of propylene glycol 5.0
Total 10
0.0% [Formulation Example 2] dQ-α-tocopherol acetate 0.
2% liquid paraffin 9
．． 0 paraffin
1.0 Isopropyl palmitate
3.0 cetanol
3.0 stearic acid
3.0 Lipophilic glyceryl monostearate
2.0 Butyl paraoxybenzoate
0.1 Methyl paraoxybenzoate 0
．． 2 Amber mucus (product of this invention) 1.0 Flavoring agent Micro-purification Water Balance

[Brief explanation of drawings]

The figure is a graph showing the average type conductivity before and after application of the sample in the evaluation of moisturizing effect. Applicant Lion Co., Ltd. Agent Patent Attorney Takashi Kojima (Ω) Impedance measurement date

Claims (1)

[Scope of Claims] 1. A method for producing a physiologically active substance from Aspergillus orientalis, which comprises performing a step of treating an extract of Aspergillus orientalis with an adsorbent, and then collecting a substance obtained by eluting it with water. 2. The manufacturing method according to claim 1, wherein the adsorbent is a hydrophobic adsorbent.