JP2003160502A - Production method of active fraction obtained from pyroligneous acid and utilization thereof - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To obtain an active fraction contained in a crude pyroligneous acid by eliminating its harmful components. <P>SOLUTION: The crude pyroligneous acid is firstly extracted with benzene followed by extraction with a weak alkali buffer solution to obtain an acid fraction. The residual benzene solution is then mixed with a strong alkali solution to obtain an alkali soluble phenol fraction and finally a neutral fraction as benzene solution. The acid and phenol fractions are isolated by re-extraction with benzene after neutralization with a hydrochloric acid. <P>COPYRIGHT: (C)2003,JPO

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention removes biologically harmful components contained in crude wood vinegar and crude bamboo vinegar (collectively referred to as wood vinegar in the present invention) to obtain active ingredients (acidic fraction) in wood vinegar. , Phenol fraction, Neutral fraction) and cosmetics using this as raw material (prevention of skin troubles due to sunburn, cleaning, hair, foundation, makeup, fragrance, nails, lips, oral cavity, bathing, tooth brushing) Pathogens such as worms, insect bites, athlete's foot, medicinal products for repairing skin troubles such as grass rash, quasi drugs, Staphylococcus aureus, MRSA (mesitillin-resistant Staphylococcus aureus), salmonella, O-157, etc. The present invention relates to health foods, soft drinks, and other foods that use the prevention of germs (bactericidal action) on sex microorganisms.

[0002]

2. Description of the Related Art Wood vinegar is a dry-distilled liquid produced by cooling the smoke generated when carbonizing (dry-distilling) bamboo such as bark, trees, bamboo, Menso bamboo and bamboo grass such as bear bamboo and chishima bamboo grass. . Although its chemical composition may vary depending on the type of raw material,
In addition to water, typical ones are acetic acid, propionic acid, phenol, cresols, formaldehyde, methanol and the like, which amount to 180 to 200 kinds.

As mentioned above, the wood vinegar solution contains a large amount of formaldehyde and methanol as biohazardous components. Therefore, unless they are removed, they cannot be used as raw materials for cosmetics, pharmaceuticals, quasi drugs, pharmaceuticals, and foods.

Wood vinegar has been used as an antiseptic for foods, for adding aroma to smoked products, and as a bactericidal agent in gardening because of its unique aroma and bactericidal action. further,
It is empirically known to be effective in treating diabetes, improving kidney function, treating liver damage, and the like. However, the wood vinegar solution (including products marketed as distilled wood vinegar solution these days) contains formaldehyde and methanol which are biotoxic components, and at the same time has an unpleasant odor.

[0005] Conventionally, research and development of a cosmetic raw material base (cosmetic raw material) using wood vinegar has been carried out, and as a result, it has succeeded in producing a high-quality wood vinegar having the formaldehyde and methanol removed from the wood vinegar (Patent No. 3002166). Issue 3002
No. 170), the use of this product as a cosmetic base has been approved by the Ministry of Health and Welfare, and cosmetics containing this product are commercially available.

[0006] This high-quality wood vinegar solution is Staphylococcus aureus, MR
Although it has a strong antibacterial action and an antioxidant action against SA, Pseudomonas aeruginosa, Trichophyton, etc., it has an unpleasant odor, so it is used in areas other than cosmetics, such as food additives and health drinks. There was a difficulty in doing so.

[0007]

SUMMARY OF THE INVENTION Therefore, the object of the present invention is to remove biohazardous substances such as formaldehyde and methanol contained in wood vinegar and unpleasant odors and to have an antioxidative ability to "body-friendly". It is to provide food ingredients such as "health drinks using natural ingredients".

[0008]

[Means for Solving the Problems] The present inventors have earnestly studied the use of the above-mentioned wood vinegar solution, and finally arrived at the present invention.

That is, the present invention is a method for producing an effective fraction from a wood vinegar, which comprises fractionating a crude wood vinegar by the following steps. Step 1: Add a water-insoluble organic solvent to the crude wood vinegar,
Mix, transfer the active ingredient of the crude wood vinegar to the organic solvent,
A step of obtaining an organic solvent extract. Step 2: pH 8.0 in the organic solvent extract obtained in Step 1.
~ 8.5 buffer is added and mixed to extract soluble matter in the buffer, and the resulting buffer extract is acidified with an acid,
Next, a step of adding a non-water-soluble organic solvent, mixing them, obtaining an organic solvent extract again, drying and then removing the organic solvent to obtain an acidic fraction of wood vinegar. Step 3: An alkaline aqueous solution having a pH of 12 to 14 is added to the organic solvent extract after extraction with the buffer solution of Step 2, and mixed to extract a soluble component in the alkaline aqueous solution, and the obtained alkaline aqueous solution extract is acidified. To acidify, then add a water-insoluble organic solvent and shake to obtain an organic solvent extract again,
After drying, a step of removing the organic solvent to obtain a phenol fraction of wood vinegar. Step 4: A step of drying the organic solvent extract after the alkaline aqueous solution extraction of Step 3 and then removing the organic solvent to obtain a neutral fraction of wood vinegar. Is.

The present invention also relates to the acidic fraction of wood vinegar, the phenolic fraction of wood vinegar and the neutral fraction of wood vinegar produced as described above, and cosmetics, pharmaceuticals and quasi drugs containing these fractions as active ingredients. It is a product or food.

[0011]

BEST MODE FOR CARRYING OUT THE INVENTION In the present invention, first, a non-water-soluble organic solvent is added to and mixed with a wood vinegar solution, and an active ingredient is extracted into the organic solvent phase to obtain an extraction raw material for each fraction in the following steps. (Step 1).

The wood vinegar used here is a crude wood vinegar obtained by carbonization of various trees and their bark, bamboo shoots, Moso bamboo,
It is a crude bamboo vinegar obtained by dry-distilling Chishima bamboo grass, bear bamboo grass, etc., and it can be used even if it is produced by any commonly used production method. A wood vinegar solution obtained from an ordinary charcoal kiln can be preferably used. The wood vinegar usually has chemical components as shown in Table 1 described below, and generally has a pH of 2 containing 1.7 to 2.5% by weight of the total amount of solid components and volatile components. A brownish-brown aqueous solution with a sourness of 3 to 2.5 and a smoky smell. In the present invention, the pH may be adjusted to about 1 with an inorganic acid such as hydrochloric acid if necessary.

As the water-insoluble organic solvent used here,
Anything that does not mix freely with water can be used, but petroleum ether with low polarity, diethyl ether,
Hexane, benzene and the like are preferable, and benzene is more preferable. An appropriate amount of the organic solvent used is 100 to 600 parts by weight with respect to 100 parts by weight of the wood vinegar solution, and when benzene is used as the organic solvent, it is preferably 200 to 500 parts by weight.

A wood vinegar solution and an organic solvent are mixed and then allowed to stand to separate an organic solvent phase and an aqueous phase. The active ingredient is extracted in the obtained organic solvent phase. If necessary, the organic solvent extract obtained here is dried with anhydrous sodium sulfate or the like, and then subjected to the following steps.

The mixing is usually carried out at room temperature, and the time is sufficient for the active ingredient to be extracted into the organic solvent phase, which is appropriately determined depending on the mixing temperature and the amount of extraction solvent used.

The pH of the organic solvent extract obtained in step 1
After adding 8.0 to 8.5 of the buffer solution and thoroughly mixing it, the mixture was left to stand, the buffer solution phase was collected, the buffer solution extract was neutralized with an acid, and then the water-insoluble organic solvent was added again. After sufficiently mixing, then the aqueous solution phase and the organic solvent phase are separated, the organic solvent phase is collected and, if necessary, dried over anhydrous sodium sulfate or the like, and then the organic solvent is distilled off to obtain an acidic fraction of wood vinegar ( Step 2).

The buffer used here has a pH of 8.0 to 8.0.
8.5, carbonate buffer, phosphate buffer,
Known as acetate buffer and the like. Of these, carbonate buffer is preferable. If the pH is out of this range,
The acid fraction of the wood vinegar solution to be obtained in this step 2 cannot be sufficiently obtained, or the components of the phenol fraction of the wood vinegar solution obtained in the next step 3 are mixed. The amount of the buffer solution used varies depending on the concentration of the salt, the type of the buffer solution, etc., but normally 5 to 20 parts by weight is suitable for 100 parts by weight of the organic solvent extract of the raw material.

An inorganic acid such as hydrochloric acid or sulfuric acid, or an organic acid such as acetic acid is used to neutralize the buffer solution thus obtained. Of these, hydrochloric acid and acetic acid are preferable because they can be easily processed later. The degree of neutralization is pH 7.5 or less so that the extracted wood vinegar acidic fraction can be sufficiently extracted into the next organic solvent,
The pH is preferably set to 6.8 to 7.0.

The neutralized buffer extract is extracted again with a water-insoluble organic solvent. The solvent used here may be the same as that used in step 1 or may be different. In addition,
As the type of solvent, the solvent used in step 1 can be used. The amount used is 100 to 100 parts by weight of the buffer extract.
600 parts by weight is suitable, usually 200 to 500 parts by weight.

The obtained organic solvent extract is dried over anhydrous sodium sulfate if necessary, and then the organic solvent is distilled off under reduced pressure or atmospheric pressure to obtain an acidic fraction of wood vinegar. The anhydrous sodium sulfate used for drying here depends on the water content in the organic solvent extract, but usually 1 to 10% by weight is sufficient with respect to the organic solvent extract.

The acid fraction of wood vinegar obtained here is odorless,
Colorless, usually 0.0 per 100 parts by weight of raw wood vinegar
It is from 03 to 0.005 parts by weight.

In step 2, the organic solvent phase which is the buffer extraction residual liquid is dried with anhydrous sodium sulfate or the like if necessary, and then an alkaline aqueous solution having a pH of 12 to 14, preferably sodium hydroxide aqueous solution, potassium hydroxide aqueous solution or the like. An alkaline aqueous solution is added and mixed well, and then an alkaline aqueous solution phase and an organic solvent phase are separated. The alkaline aqueous solution extract is sampled, neutralized with an acid, and again mixed with a non-water-soluble organic solvent and thoroughly mixed, and then the organic solvent phase is sampled and, if necessary, dried over anhydrous sodium sulfate, etc. The organic solvent is distilled off under pressure to obtain a phenolic fraction of wood vinegar (step 3).

The alkaline aqueous solution used here has a pH of
12 to 14, usually an aqueous solution of lithium hydroxide, sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or the like, and preferably an aqueous sodium hydroxide solution. There is no problem if the pH is out of this range, but it is preferable that the pH is in this range. The amount of the alkaline aqueous solution used varies depending on the pH, the type of the alkali, etc.
5 to 20 parts by weight is suitable with respect to parts by weight.

An inorganic acid such as hydrochloric acid or sulfuric acid or an organic acid such as acetic acid is used to neutralize the alkaline aqueous solution extract thus obtained. Preferably, since the subsequent treatment is easy,
Hydrochloric acid and acetic acid. The degree of neutralization is adjusted so that the extracted wood vinegar phenolic fraction can be sufficiently extracted into the next organic solvent.
It is preferable that the pH is H7.5 or less, preferably pH 6.8 to 7.0.

The neutralized aqueous alkaline solution extract is extracted again with a water-insoluble organic solvent, and the solvent used here may be the same as that used in step 1 or may be different. As the kind of solvent, the solvent used in step 1 can be used without any problem. The amount used is appropriately 100 to 600 parts by weight, and usually 200 to 500 parts by weight, per 100 parts by weight of the neutralized aqueous alkaline solution.

The organic solvent extract obtained here is dried with anhydrous sodium sulfate if necessary, and then the organic solvent is distilled off under reduced pressure or atmospheric pressure to obtain a phenol fraction of wood vinegar. The anhydrous sodium sulfate used for drying here depends on the water content in the organic solvent extract, but usually 1 to 10% by weight is sufficient with respect to the organic solvent extract.

The phenolic fraction of wood vinegar obtained here is
It has a sweet scent and is usually 0.10 to 0.13 parts by weight per 100 parts by weight of the raw wood vinegar.

The organic solvent solution remaining after being extracted with the alkaline aqueous solution of step 3 is dried with anhydrous sodium sulfate or the like, if necessary, and then the organic solvent is distilled off under reduced pressure or atmospheric pressure to obtain a neutral fraction of wood vinegar. Is obtained (step 4). The anhydrous sodium sulfate used for drying here depends on the water content in the organic solvent solution, but usually 1 to 10% by weight is sufficient with respect to the organic solvent solution.

The neutral fraction of wood vinegar obtained here has a odor of stickiness generated when charcoal is burned, and the raw wood vinegar liquor 10
It is 0.06-0.09 part by weight per 0 part by weight.

When each fraction of the present invention is dissolved in a 50% ethyl alcohol aqueous solution or a 50% glycerin aqueous solution, the wood vinegar acid acidic fraction is colorless, odorless and transparent, and the wood vinegar phenolic fraction is pale yellow and sweet. It has a scent and is transparent, and the neutral fraction of wood vinegar is light yellow and transparent, having the odor of stickiness that occurs when charcoal is burned.

Each fraction of the present invention can be used in cosmetics, pharmaceuticals, foods / beverages, etc. by dissolving it in an aqueous solution of ethyl alcohol, an aqueous solution of glycerin, squalane, camellia oil, linoleic acid and the like.

Specifically, each fraction is used by dissolving it in an organic solvent, an oil component, or an aqueous solution depending on the purpose of use. In this case, the amount of liquid to be dissolved is preferably equal to or less than that of the used wood vinegar.

Each fraction is well soluble in warm water, organic solvents such as ethanol, diethyl ether, n-hexane, ethyl acetate, acetone, benzene and the like, and also soluble in jojoba oil, camellia oil, squalane, glycerin, etc. However, it can be used as a raw material for manufacturing cosmetics, pharmaceuticals, foods, or as it is.

Cosmetics (packs, shaving agents, toothpastes, sunscreens, lotions, creams, emulsions, medicated soaps, shampoos, rinses) are manufactured by utilizing the antioxidant and antibacterial effects of these fractions. In that case, an acidic fraction of wood vinegar, a phenolic fraction, and a neutral fraction are appropriately selected and used according to the preference of aroma. In this case, 0.1 part by weight of the fraction is added to 100 parts by weight of the water-soluble liquid or oily liquid and mixed well, and 1 to 10 parts by weight is added to 100 parts by weight of the cosmetic assembly material.

In the case of producing healthy drinking water and specific healthy drinking water by utilizing the antioxidant action and antibacterial action of these fractions, these fractions are appropriately selected and used. In this case, 0.1 to 5 parts by weight of a fraction prepared by adding 100 parts by weight of water to 100 parts by weight of normally produced drinking water is used.

Antioxidant action of these fractions, tannin has been used to repair damaged skin husks by pathogenic microorganisms.
When producing a therapeutic agent for mucosal infections and a therapeutic agent for troubled skin due to grass rash and atopic dermatitis, these fractions are appropriately selected and used. In that case, 0.5 to 5 parts by weight of a water-soluble liquid or ointment pharmaceutical composition 100 parts by weight, 0.1 part by weight of a fraction was added to 100 parts by weight of an aqueous or oily solution and well dissolved. Is added.

[0037]

EXAMPLES The present invention will be further described below with reference to examples. Further, the usefulness of the acidic fraction of wood vinegar, the phenol fraction, and the neutral fraction obtained by the production method of the present invention will be described.

Example 1 Step 1: Production of Fractionated Raw Material The raw material wood is wood vinegar obtained by carbonization (charcoal burning) of driftwood (pine, beech, oak, willow, cedar, etc.) that has flowed into the reservoir (power development stock 100 parts by weight of benzene are added to 100 parts by weight of the company) and mixed well at room temperature. Then, the mixture is allowed to stand to separate the benzene phase and the aqueous phase to obtain a benzene phase.
To 100 parts by weight of this benzene extract, 1.25 parts by weight of anhydrous sodium sulfate was added and thoroughly mixed, and then filtered to obtain a fractionated raw material used in the following examples. The main chemical components of this benzene extract are shown in Table 1. In addition, strong acidic organic acids such as acetic acid, propionic acid, and formic acid contained in the raw wood vinegar are not included.

[0039]

【table 1】

Example 2 Step 2: Preparation of acidic fraction of wood vinegar solution To 100 parts by weight of the benzene extract obtained in Example 1, 10 parts by weight of a 5% sodium hydrogen carbonate aqueous solution (pH 8.5) was added, and the mixture was thoroughly mixed. Mix. After separating the benzene phase and the aqueous phase, the aqueous phase is collected, and 1.25 parts by weight of 1N hydrochloric acid is added to the aqueous phase for neutralization (pH 7.0). After adding 430 parts by weight of benzene to 100 parts by weight of the neutralized aqueous phase and mixing them well, the benzene phase and the aqueous phase are separated and the benzene phase is collected. To 100 parts by weight of this benzene phase, 2 parts by weight of anhydrous sodium sulfate was added and thoroughly mixed, and then filtered. Then, the benzene filtrate is concentrated under reduced pressure to obtain an acidic fraction of wood vinegar. The acidic fraction of wood vinegar obtained here is wood vinegar 1
It was 4 mg per 00 ml. Representative chemical components of this fraction are shown in Table 2.

[0041]

[Table 2]

Example 3 Step 3: Production of phenol fraction of wood vinegar 1.25 parts by weight of anhydrous sodium sulfate was added to 100 parts by weight of the remaining benzene phase extracted with the aqueous sodium hydrogen carbonate solution of Example 2 and mixed well. After that, it is filtered. To the obtained benzene filtrate, 10 parts by weight of 2% aqueous sodium hydroxide solution (pH 14) is added and mixed well. After separating the benzene phase and the aqueous phase, the aqueous phase was collected and 1N hydrochloric acid 1
Add 8 parts by weight to neutralize (pH 7.0). After 400 parts by weight of benzene was added to 100 parts by weight of the neutralized aqueous phase and thoroughly mixed, the benzene phase and the aqueous phase were separated, and the benzene phase was collected. 2.5 parts by weight of anhydrous sodium sulfate was added to 100 parts by weight of the benzene phase, mixed well, and filtered. The obtained benzene filtrate is concentrated under reduced pressure to obtain a wood vinegar phenol fraction. The phenol fraction of the wood vinegar thus obtained was 110 mg per 100 ml of the wood vinegar. Representative chemical components of this fraction are shown in Table 3.

[0043]

[Table 3]

Example 4 Step 4: Preparation of Neutral Fraction of Wood Vinegar Liquid Anhydrous sodium sulfate was added to 100 parts by weight of the remaining benzene phase extracted with the aqueous sodium hydroxide solution of Example 3.
Add 25 parts by weight, mix well, and filter. The benzene filtrate is concentrated under reduced pressure to obtain a wood vinegar neutral fraction. The neutral fraction of wood vinegar obtained here is 6 per 100 ml of wood vinegar.
It was 6 mg. Representative chemical components of this fraction are shown in Table 4.

[0045]

[Table 4]

Application Example 1 Total Phenolic Amount of Each Fraction Each of the fractions obtained in Examples 2 to 4 was prepared with a 50% aqueous ethanol solution to a concentration of 100 ml of raw wood vinegar, and total phenol was prepared by the Foreign-Dennis method. The quantity was measured. The results are shown in Table 5. The actual measured value of total phenol was highest in the phenol fraction of wood vinegar at 76.8 mg / dl, followed by the neutral fraction of 15.4 mg / dl and the acidic fraction of 3.6 mg / dl.
It was. The total amount of phenol contained in 1 mg of each fraction was calculated from this measured value, and the acidic fraction of wood vinegar was 0.90 m.
g, phenol fraction 0.70 mg, neutral fraction 0.23 m
It was g.

[0047]

[Table 5]

Application Example 2 Tannin content of each fraction Using the sample prepared in Application Example 1, the tannin content of each fraction was measured by the tartaric acid / iron reaction method. The results are shown in Table 6. The measured value is 0.80 m of the phenol fraction of wood vinegar.
The highest value was g / dl, and the acid fraction and the neutral fraction were about 0.4 mg / dl, respectively. When the amount of tannin contained in 1 mg of each fraction was calculated from this measured value, the acidic fraction of wood vinegar was the highest at 0.100 mg, and the phenol fraction and the neutral fraction were 0.007 mg and 0.0 respectively.
The value was almost the same as that of 06 mg, which was less than 1/10 of the acidic fraction.

[0049]

[Table 6]

Application Example 3 The antioxidant polyphenols of each fraction are widely present in the plant kingdom as secondary metabolites, and recent research reports confirm that they have various physiological activities such as antiviral action and antiallergic action. Has been done. Such physiological activity is considered to be due to the antioxidant ability of phenols. Since each fraction of wood vinegar was used as a raw material for foods such as pharmaceuticals, cosmetics and health drinks, the antioxidant ability of each of these fractions was measured. Each fraction was adjusted to 1 mg / dl with a 50% ethanol aqueous solution and used as a measurement sample. The measurement of antioxidant capacity utilizes the fact that the oxide of linoleic acid fades β-carotene,
The anti-fading activity was used as an index. Also,
The value of the antioxidative ability of each fraction sample is the calibration curve (0 mg / dl, 1 mg / dl, 5 mg of butyl hydroxytoluene (BHT) 50% ethanol solution of each concentration prepared in advance.
mg / dl) was used to determine the BHT value (the lower the value of the antioxidant activity expressed by the BHT value, the stronger the antioxidant power). As a control, 50 mg ethanol solution of chlorogenic acid and α-tocopherol (vitamin E) at a concentration of 1 mg / dl was used. Table 7 shows the measurement results of each fraction and the control. The wood vinegar phenolic fraction is chlorogenic acid,
It shows the same antioxidant capacity as α-tocopherol, and the acid fraction and neutral fraction have weaker antioxidant capacity than the phenol fraction,
It has sufficient antioxidant ability.

[0051]

[Table 7]

Application Example 4 Superoxide scavenging ability of each fraction The strength of the antioxidant ability is greatly involved in the onset mechanism of all disease states, and the antioxidant activity using linoleic acid / β-carotene measured in Application Example 3 Noh shows the peroxidation reaction of lipids. Lipid peroxidation is an addition reaction of oxygen to lipids,
For this to occur either lipids or oxygen must be activated. Therefore, ES for each fraction sample
By the R spin trap method, the erasing rate of superoxide (O ₂ ⁻ ) which is a typical oxide substance was examined and compared with the value of α-tocopherol. The sample used was a 50% aqueous ethanol solution adjusted to 1 mg / ml. Table 8 shows the dilution ratios at which the superoxide scavenging rate was 50%. The dilution factor of the wood vinegar acid acidic fraction was the highest at 50 times, followed by the phenol fraction at 11 times and the neutral fraction at 1.2 times, and α-tocopherol was not observed to eliminate superoxide at all.

[0053]

[Table 8]

Considering this result together with the result of Application Example 3, the inhibitory action on lipid activity is phenol fraction> neutral fraction ≧ acidic fraction, and the action of phenol fraction is chlorogenic acid and α-tocopherol. It is about the same. The scavenging action of superoxide is acidic fraction> phenol fraction> neutral fraction, which is much stronger than α-tocopherol.

Application Example 5 Antibacterial action of each fraction Using each sample prepared by adjusting each fraction to a concentration of 1 mg / ml with a 50% ethanol solution, Staphylococcus aureus, MRSA (Mesicillin-resistant Staphylococcus aureus), Trichophyton Tegrophytes: a kind of fungus causing athlete's foot), Salmonella SG1
X, antibacterial activity against pathogenic E. coli O-157 was investigated.
According to a dilution method of diluting the above stock solution up to 10 times, the antibacterial action of the acid fraction of wood vinegar was the strongest, followed by the phenol fraction and the neutral fraction, depending on the bacterial species. The acid fraction of wood vinegar has the strongest antibacterial action against Staphylococcus aureus, MRSA and Trichophyton, and is a cause of food poisoning, Salmonella S.
No strong antibacterial action was observed against G1X and O-157.

[0056]

According to the production method of the present invention, the antioxidant action,
Each fraction of wood vinegar having antibacterial action can be obtained, and its utilization range is wide. In particular, for the research and development of the intended product (medicines, quasi drugs, cosmetics, health drinks, food additives, etc.), use the acid fraction or phenol fraction obtained here, respectively, or It is desirable to use the two fractions together.

─────────────────────────────────────────────────── ─── Continuation of front page (51) Int.Cl. ⁷ Identification code FI theme code (reference) A61P 17/00 101 A61P 17/00 101 17/16 17/16 F term (reference) 4B018 LB08 LB10 LE05 MD48 ME06 ME09 MF01 4C083 AA111 CC02 CC11 CC13 CC25 CC41 EE12 EE13 EE31 FF01 4C088 AB03 AB12 AC06 CA09 CA15 CA23 ZA89 ZB35 ZC37

Claims (5)

[Claims] 1. A method for producing an effective fraction from a wood vinegar, which comprises fractionating a crude wood vinegar by the following steps. Step 1: Add a water-insoluble organic solvent to the crude wood vinegar,
Mix, transfer the active ingredient of the crude wood vinegar to the organic solvent,
A step of obtaining an organic solvent extract. Step 2: pH 8.0 in the organic solvent extract obtained in Step 1.
~ 8.5 buffer is added and mixed to extract soluble matter in the buffer, and the resulting buffer extract is acidified with an acid,
Next, a step of adding a non-water-soluble organic solvent, mixing them, obtaining an organic solvent extract again, drying and then removing the organic solvent to obtain an acidic fraction of wood vinegar. Step 3: An alkaline aqueous solution having a pH of 12 to 14 is added to the organic solvent extract after extraction with the buffer solution of Step 2, and mixed to extract soluble components in the alkaline aqueous solution, and the resulting alkaline aqueous solution extract is acidified. To acidify, then add a water-insoluble organic solvent and shake to obtain an organic solvent extract again,
After drying, a step of removing the organic solvent to obtain a phenol fraction of wood vinegar. Step 4: a step of drying the organic solvent extract after the alkaline aqueous solution extraction of Step 3 and then removing the organic solvent to obtain a neutral fraction of wood vinegar. 2. An acidic fraction of wood vinegar prepared according to claim 1. 3. A phenolic fraction of wood vinegar prepared according to claim 1. 4. A neutral fraction of wood vinegar prepared according to claim 1. 5. A cosmetic product, a pharmaceutical product, comprising the fraction according to claim 2 as an active ingredient.
Quasi-drugs or food.