JP2000256123A - Production of thistle extract - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain the subject extract which is useful in compositions of preparation for external use for skin or compositions of bath preparation by contacting an extract solvent solution from a thistle group plant with a synthetic adsorbent and removing the adsorbate from the above adsorbent to effect decoloring the extract while holding its lipolytic activity. SOLUTION: This extract is obtained by contacting an extract solvent solution such as ethanol solution from a thistle group plant such as Cirsium nipponicum var incomptum with a synthetic adsorbent, preferably a styrene- divinylbenzene-based synthetic adsorbent, acrylic ester-based synthetic adsorbent or methacrylic acid ester-based synthetic adsorbent, and then removing the adsorbate from the above adsorbent. The amount of the above adsorbent to be used is preferably 0.1-6.0 wt. times based on the solid amount in the solution to be treated. An adsorbent treatment operation is performed preferably under ordinary pressure to 50 atomospheric pressure and at room temperature to 40 deg.C temperature, and in the case of a batch method, the treatment time is preferably 1-24 h.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] The present invention relates to a method for producing a thistle extract having excellent lipolytic activity and improved color, and a skin external preparation composition and a bath composition containing the extract. .

[0002]

2. Description of the Prior Art Thistle extract has a lipolytic activity and is excellent in suppressing, preventing and improving obesity (JP-A-8-301780).
issue). However, since thistle extract is dark brown, there is a problem in that when it is added to the composition for external use on skin and the composition for bath, the color of the composition becomes darker. In addition, in order to obtain a thistle extract which has been bleached to a color that can be blended in an amount capable of exhibiting lipolytic activity to the external composition for the skin and the bath preparation composition by the activated carbon treatment usually used for decolorization, the activated carbon is extracted. Although it was necessary to use the solid content in the content more than 1 weight, there was a problem that the lipolytic activity of the thistle extract treated with 1 weight of activated carbon was lost. Accordingly, an object of the present invention is to provide a method for producing a decolorized thistle extract while retaining lipolytic activity.

[0003]

Means for Solving the Problems The present inventors have found that the use of a synthetic adsorbent can improve the color of thistle extract while maintaining lipolytic activity.

[0004] That is, the present invention provides a method for producing a thistle extract characterized by contacting a solvent extract of a thistle plant with a synthetic adsorbent to remove adsorbed substances to the adsorbent. is there. The present invention also provides a skin external preparation composition and a bath composition containing the thistle extract obtained by the above treatment.

[0005]

BEST MODE FOR CARRYING OUT THE INVENTION The thistle plant may be any of the thistle plants, but is preferably a thistle plant, a genus Athisium plant, and a genus Thistle plant. Plants are particularly preferred. Nambu thistle, stone thistle, silk thistle, yoshino thistle, horsetail thistle, and mountain thistle are more preferable.

[0006] Thistle family plants include leaves, flower heads,
Seeds, stems, roots and whole plants can be used as raw materials. Among them, it is preferable to use a dried above-ground part which is easy to collect.

As the extraction solvent for thistle plant of the present invention, lower alcohols such as methanol, ethanol and propanol, polyhydric alcohols such as propylene glycol and butylene glycol, and water are used alone or as a mixture of two or more. be able to.

The solvent extract of thistle plants used for the treatment with the synthetic adsorbent can be used as it is, or the solvent extract can be concentrated and then treated. If a precipitate is formed by this concentration, it is desirable to remove the precipitate before performing the synthetic adsorbent treatment.

The synthetic adsorbent required for the present invention includes:
Styrene-divinylbenzene-based, acrylate-based and methacrylate-based synthetic adsorbents are preferred, but styrene-divinylbenzene-based synthetic adsorbents are preferred. The operation of removing the adsorbed substance from the solvent extract using a synthetic adsorbent may be any of a batch method and a column method. The amount of the adsorbent used is 0.001 of the solid content in the solution to be treated.
５０50-fold weight is usually used, but preferably 0.1-
It is good to make it 6 times by weight. The processing operation is performed at normal pressure to 5
The treatment can be carried out at 0 atm, and the treatment temperature is usually from 0 ° C to 100 ° C, preferably from room temperature to 40 ° C. The processing time of the batch method is usually from 10 minutes to 1 month, but preferably from 1 hour to 24 hours.

The above thistle extract includes, in addition to the solution obtained by this adsorbent treatment operation, those obtained by concentrating the solution. Further, in addition to the decolorizing method using the synthetic adsorbent, a decolorizing treatment using activated carbon that is 0.2% by weight or less of the solid content of the extract, which is the amount of activated carbon whose lipolytic activity hardly decreases, May be implemented.

The thistle extract of the present invention is used by blending it with a skin external preparation such as cream, milky lotion and cosmetics, and a bath preparation. When the product of the present invention is added to a skin external preparation, 0.0
It is preferable to add so as to be 1 to 20% by weight (hereinafter, simply indicated by "%"). When added to a bath agent, the concentration in the bath water is preferably 0.001 ppm to 200 ppm, more preferably 0.01 ppm to 100 ppm.

[0012]

Example 1 (Preparation 1 of thistle extract) To 1 kg of the above-ground part of dried milk thistle (Cirsium nipponicum var incomptum), 10 L of 50% ethanol was added, and the mixture was heated and extracted, followed by filtration to obtain a solvent extract. To the residue, 8 L of 50% ethanol was added again, and the mixture was filtered after warm extraction. The obtained solvent extracts were combined and concentrated to obtain a 600 mL aqueous solution. The precipitated insolubles were removed by centrifugation and subsequent filtration to obtain an aqueous solution containing 21% w / v solids. The aqueous solution was mounted on Diaion HP20 (styrene-divinylbenzene-based synthetic adsorbent, Mitsubishi Chemical), 600 mL (0.36 kg weight) column chromatography, and eluted with 1.2 L of water. The obtained aqueous solution is concentrated again,
Make up to 980 mL of aqueous solution. The solid content in the obtained aqueous solution was 10 w / v%.

Example 2 (Preparation 2 of thistle extract) Thistle extract described in Example 1 (500 mL, solid content: 50 g)
Was added with activated carbon (5 g), and the mixture was heated and stirred. After removing the activated carbon, the obtained solution is concentrated and dried, and as a powder extract,
46 g of thistle extract was obtained.

Comparative Example 1 (Thistle Solvent Extract) 1 L of 50% ethanol was added to 100 g of the above-ground portion of dried milk thistle (Cirsium nipponicum var incomptum), extracted with warming, and filtered to obtain a solvent extract. 50% for residue
Ethanol (800 mL) was added again, and the mixture was filtered after warm extraction. The obtained solvent extracts were combined, concentrated and dried to obtain 132 g of a thistle solvent extract as a dark brown syrup.

Comparative Example 2 (Production of Thistle Extract Decolorized with Activated Carbon Only) To 50 g of thistle extract described in Comparative Example 1 was added 500 mL of water, heated and dissolved, and the insoluble matter was removed by centrifugation. 39 g of activated carbon was added to 480 mL (39 g of solid content) of the obtained aqueous solution, and the mixture was heated and stirred. After removing the activated carbon, the obtained solution was concentrated and dried to obtain 37 g of thistle extract as a powder extract.

Test Example 1 (Color test of thistle extract) A 10% ethanol solution containing 1% of solid content was prepared,
The color was determined visually.

[0017]

[Table 1]

Test Example 2 (Test for Lipolysis Acceleration Activity of Thistle Extract) Rodbell method [Rodbell, M .; , J. et al. Bio
l. Chem. 239, 375 (1964)], male Wistar rats (body weight 150-200 g).
Free adipocytes were prepared from 6 epididymal adipose tissues using a collagenase solution. The cells were incubated at 37 ° C. in Hank's buffer containing bovine serum albumin adjusted to a test substance concentration of 100 μg / mL at 37 ° C.
After incubation for a time, released glycerol was measured by an enzymatic method (F-kit glycerol; using Boehringer Mannheim). Table 2 shows the results.

[0019]

[Table 2]

Using the extracts prepared by the methods shown in Examples 1 and 2, skin external preparations such as a paste and foam pack and a bath preparation were prepared according to the following formula.

Example 3 (gel cream) (%) Extract of Example 1 or 2 10 Liquid paraffin suitable amount Squalane 20 microcrystalline wax 5 cetyl isooctanoate 5 polyoxyethylene (20) glycerol tri isostearate 1 Fragrance trace amount Dye trace amount

Example 4 (massage agent containing scrubbing agent) (%) Extract of Example 1 or 2 5 Isoproterenol hydrochloride 1 Polyethylene beads (particle size 20 μm or less 7%, particle size 5000 μm or more 0%) 10 Flow Paraffin 14 2-Ethylhexanoic acid triglyceride 37 Sorbitol 8 Polyethylene glycol (average molecular weight 400) 6 Acylmethyltaurine 6 Polyoxyethylene (60) octyldodecyl alcohol ether 8 Purified water Appropriate amount Fragrance Trace amount

Example 5 (foam pack) (%) Extract of Example 1 or 2 15 Yohimbine hydrochloride 2 1,3-butylene glycol 10 Glycerin 10 Methylparaben 0.2 Potassium hydroxide 0.2 Stearic acid 1 butyl alcohol 2 Polyoxyethylene (60) hydrogenated castor oil 3

Example 6 (Tablet bath agent) (%) Extract of Example 2 14 Amrinone 2 Sodium bicarbonate 20 Sodium carbonate 10 Fumaric acid 30 Polyethylene glycol (average molecular weight 6000) 20 Dextrin Appropriate amount Perfume Trace amount Pigment Trace amount

Example 7 (liquid bath preparation) (%) Extract of Example 1 or 2 20 Triglyceride octoate 33 Octyldodecyl myristate 33 Liquid paraffin Appropriate amount Polyoxyethylene sorbite fatty acid ester (40E.O.) 9 Polyoxy Ethylene sorbite fatty acid ester (20E.O.) 3 Fragrance trace

[0026]

According to the present invention, lipolytic activity is excellent,
In addition, a thistle extract with improved color can be obtained.

Continued on the front page (51) Int.Cl. ⁷ Identification symbol FI Theme coat II (Reference) A61K 35/78 A61K 35/78 T (72) Inventor Yuji Ichii 2606 Kabane-cho, Akabane, Haga-gun, Tochigi Kao Corporation Research In-house (72) Inventor Mori Shinobu 2606 Kabane-cho, Akaga-cho, Haga-gun, Tochigi Prefecture Inside Kao Co., Ltd. Research Institute (72) Inventor Mayumi Sato 2606, Kaiga-cho, Akaga-cho, Haga-gun, Tochigi Pref. AA112 AB032 AB312 AC012 AC022 AC102 AC122 AC132 AC182 AC242 AC292 AC352 AC402 AC422 AC432 AC442 AC482 AC732 AC792 AC852 AD021 AD022 AD091 AD112 AD242 CC05 CC07 CC22 CC25 DD08 DD15 DD16 DD23 DD41 EE03 EE11 4C088 AB27 AC01 AC03 MA04 MA13 MA10 NA06 ZC19 ZC33

Claims (4)

[Claims] 1. A method for producing a thistle extract, which comprises contacting a solvent extract of a thistle plant with a synthetic adsorbent to remove adsorbed substances to the adsorbent. 2. The synthetic adsorbent is a styrene-divinylbenzene synthetic adsorbent, an acrylate synthetic adsorbent, or a methacrylate synthetic adsorbent.
Production method as described. 3. An external preparation composition for skin containing a thistle extract obtained by the production method according to claim 1 or 2. 4. A bath composition containing a thistle extract obtained by the production method according to claim 1 or 2.