JPH09227334A - Amber ingredient-containing agent - Google Patents

Abstract

(57) [Summary] [Objective] The object of the present invention is to cultivate a new application for amber, which has conventionally had only very limited applications such as decorative crafts and jewelry.
"Composition component obtained by melting amber""Residual composition component obtained by removing low-boiling substances from molten amber""Low-boiling substance extracted from amber""Low-boiling substance extracted from composition components obtained by melting amber" By discovering a new effect as an active ingredient such as antibacterial, antioxidant, deodorant, hand / skin roughening, anti-inflammatory, etc., these are blended as is or in various products with oils and surfactants,
It is to open up new uses of amber by solving various problems that it has. SOLUTION: The composition component of amber obtained by melting an amber by applying external energy is used as an active ingredient, and by melting, a part or all of the amber constituent is modified. And produced various effective actions and effects including antibacterial properties.

Description

Detailed Description of the Invention

[0001]

FIELD OF THE INVENTION The present invention is an amber component-containing agent such as an amber melt composition component or its low boiling point extract made from amber, a low boiling point extract of amber or a melt composition component of an extraction residue.
The present invention relates to agents that are active ingredients against antibacterial, antioxidant, deodorant, rough hands and skin, anti-inflammatory and the like.

[0002]

BACKGROUND OF THE INVENTION Amber is mainly a resin of pine plants (mainly C ₄₀
In H ₆₄ 0 ₄₎ of the fossil, including succinic acid by representatives of organic minerals. It is amorphous and has a nodule or drop shape, and exhibits a shell-like cross section and is brittle. Mohs hardness 2-3, density 1.05-1.
It is transparent or translucent at 10 g / cm ³ , has a yellowish (= amber) color with a fat gloss, and may have a white or red color. It fluoresces with ultraviolet rays, and when it rubs it becomes negatively charged and adsorbs fine powder. When heated, it softens at 120 to 150 ° C and melts at 250 to 300 ° C. It is slightly soluble in ethanol, diethyl ether or benzene. Currently,
It is only used for decorative crafts, jewelry, insulating materials, or as an incense for shavings. In particular, those containing complete fossils such as insects, fruits and leaves are especially prized as decorative crafts and gems.

[0003]

DISCLOSURE OF THE INVENTION The present invention is to solve the problem of developing a new application to amber which has been used only for a limited number of purposes such as decorative crafts and jewelry. More specifically, "composition component obtained by melting amber""composition component of residue obtained by removing low-boiling substance from molten amber""low-boiling substance extracted from amber""low-boiling substance extracted from composition component obtained by melting amber" By finding new effects as an active ingredient such as antibacterial, antioxidant, deodorant, hand / skin roughening, anti-inflammatory, etc., these are blended in various products as they are or with oils and fats and surfactants. The solution task is to open up new uses of amber by solving various problems that it has. For example, the active ingredient derived from amber according to the present invention acts as a preservative or a shelf life improver based on its antibacterial property for food and various cosmetic products and ointments,
For oils and fats, it works as an antioxidant for oils and fats due to its antioxidant property, as a deodorant for laundry detergents, and as a hand and skin roughening inhibitor for kitchen detergents. Was newly found. Examples of products containing this active ingredient include creams, milky lotions, and beauty essences containing oils and fats, and other uses include ointments containing oils and fats and surfactants, lubricating oils, engine oils, detergents. Widely applicable to shampoo, conditioner, etc.

[0004]

[Means for Solving the Problems] The amber ingredient-containing agent of "claim 1" is characterized in that "the amber composition ingredient obtained by melting external amber by applying external energy is an active ingredient". . Amber itself did not show any action and effect as described in the conventional example, and only a decorative effect was mainly expected, but by melting, it changed to part or all of the amber constituents. Occurs, which produces effective actions and effects in various industries including antibacterial properties.
Due to the above-mentioned actions and effects, oils and fats are added to the melt as it is or the coolant as it is or in the molten state, and further other chemicals and chemical agents are added to these, for example, an external preparation (for example, ship Agents, cosmetics, quasi-drugs, pharmaceuticals), deodorant fragrances, cleaning agents (clothes and kitchen detergents), hair protectants, hair growth agents, whitening agents, antiatopic agents, Zensoku remedies, antioxidants Can be used as

Here, as the external energy source for melting amber, heating, electromagnetic waves, ultrasonic waves and the like can be mentioned. As a means of adding external energy to amber to melt it, simple heating may be used, but if ultrasonic waves and electromagnetic waves (high-frequency microwave) are used together with heating, the energy added per unit time is higher than in the case of heating alone. Since the amount increases, it melts at a temperature several tens of degrees lower. Also, in the case of heating, the melting temperature will vary depending on the amber's origin, etc.
It is about 380 ° C. Since some or all of the heated amber is modified by heating and exhibits a unique action / effect that has not been seen so far, the cooled product may be used as it is for the above-mentioned application, but in the molten state. Surfactant or high temperature oily substance in amber (for example, high boiling point oil, animal or vegetable oil that can be used as the base or additive, squalene, squalane, ester, wax, paraffins, silicone oil, fluorine oil) , Polyoxyethylene, polypropylene, and derivatives thereof) may be added to uniformly dissolve them. The boiling point of the high boiling point oil is at least 120 ° C. or higher, and it is important that the amber composition component and the high boiling point oil are uniformly dissolved. This point is the same in other cases.

[0006] The amber component-containing agent of "claim 2" is "an organic solvent-soluble component is extracted and removed with an organic solvent from the amber composition components obtained by melting external amber by applying external energy, and the residue is externally extracted. The residual composition component obtained by melting by applying energy is used as an active ingredient ”, which is used as it is or together with oils and fats or surfactants or together with other medicinal components, to obtain the antibacterial effect. Due to various industrially effective actions and effects such as sex, for example, external preparations (eg, ship agents, cosmetics, quasi drugs, pharmaceuticals), deodorants added to detergents, hair protectants, hair growth agents ,Whitening,
Anti-atopic agent, skin activating agent (for example, wrinkle spreading agent)
It can be used as an antioxidant. The organic solvent used for the extraction here is, for example, ethanol, ether, acetone, toluene, ethyl acetate, cellosolves and the like. The same applies to other embodiments below.

The amber ingredient-containing agent of "claim 3" is characterized in that "a low boiling point substance extracted from amber is used as an active ingredient", and the amber ingredient-containing agent of "claim 4" is "external". The low boiling point substance extracted from the composition component of amber obtained by adding energy and melting is used as an active ingredient ”. These also exhibit effective actions and effects in various industries including the above-mentioned antibacterial properties, and by using with a surfactant or an oily substance or with other medicinal components, an external preparation (for example, a ship agent, cosmetics, It can be used as a quasi drug, a drug), a detergent, and an aromatic agent (aromatherapy, deodorant, phytoncide agent).

[0008]

EXAMPLES Examples of the present invention will be described in detail below. The embodiment according to the present invention includes 4) of A), B), C1) and C2).
There are various types, and as comparative examples, an example using amber powder and a case of no addition (control) are shown. First, the manufacturing method of each example will be described, and then each effect will be described.

Example A) 100 g of Dominica amber is melted by heating in an oil bather (= oil bath) while applying ultrasonic waves of 28 kHz and 100 W while stirring in a nitrogen stream. To melt amber, you can simply heat it,
When ultrasonic waves or high-frequency microwaves are applied while heating, they are melted at a temperature lower by several tens of degrees Celsius for the above reason. After melting, cool to 180 ° C, then 200g of squalane.
In addition, it melt | dissolves and it cools, and an example of the oil-and-fat agent containing the amber composition component of Claim 1 is manufactured.

Example B) 100 g of Dominican amber is heated at 280 ° C. in an oil bath while stirring in a nitrogen stream. After that, it is cooled to 50 ° C or lower, and anhydrous ethanol 500
Add ml and reflux for 3 hours. The residue after extraction with the ethanol layer is washed with ethanol, heated and melted again, 180 ° C
Squalane (200 g) is added to the residue cooled to dissolve, and the mixture is cooled to produce an example of the amber component-containing agent according to claim 2.

Example C1): 100 g of Lithuanian amber
Crushed to 300 mesh or less, and anhydrous ethanol 50
After adding 0 ml and refluxing for 5 hours, the liquid obtained by filtration is steam-distilled to produce an example of the amber component-containing agent according to claim 3. It is a low boiling point liquid substance.

Example C2): 100 g of Dominica amber is heated at 280 ° C. in an oil bath while stirring in a nitrogen stream. After that, it is cooled to 50 ° C or below, and anhydrous ethanol 5
Add 00 ml and reflux for 3 hours. The extracted ethanol layer is concentrated under reduced pressure and steam distilled to produce an example of the amber component-containing agent according to claim 4. It is a low boiling point liquid substance.

Next, the action and effect of the amber component-containing agent containing the amber-derived active ingredient shown in Examples A, B, C1 and C2 will be examined. (1) Experimental data of the antibacterial activity of the amber component-containing agent containing an active ingredient derived from amber (see Table 1). Here, the minimum inhibitory concentration (hereinafter MI
C) ppm was measured to test its antibacterial activity. The fungus used is Gram-positive Staphylococcus aureus (S. aureu
s), gram-negative E. coli, and fungus A. niger. The "amber powder" used as a comparative example in Table 1 was one having a 300 mesh pass, and the amber-derived active ingredients shown in the comparative example and Examples A, B, C1 and C2 were both 0.1% by weight. Lauromacrogol was emulsified in HLBI 4.0 and used.

Table 1 S. aureus E. coli A. niger amber powder>8000>8000> 8000 Example A 400 800 1600 Example B 1600 1600 3200 Example C1 400 400 800 Example C2 100 100 200

According to Table 1, the "amber powder" used as a comparative example did not show any action or effect as an antibacterial activity. On the other hand, all of Examples A, B, C1 and C2 showed an antibacterial effect. In particular, Example C2 showed the strongest antibacterial activity. From now on, the properties of the amber can be changed by heat-melting the amber or by heat-melting the extraction residue, or a new action and effect which has not been available in the past can be exhibited, or the amber can be trapped in the amber by extraction. It is recognized that it was possible to bring out the properties that were not previously known. According to this, Examples A, B, C1,
The active ingredient represented by C2 can be used as a natural food additive for antibacterial action and as a shelf life improver or preservative.

Further, by utilizing its antibacterial property, it can be used as a preservative for ointments, creams, emulsions, beauty essences, rinses and the like. Table 2 shows the test results. In this test, the cosmetic / medical base cream of the formula in parentheses (cetyl alcohol: 10% by weight, lauromacrogol HLB 14.0: 5% by weight, squalane: 5% by weight, da-tocopherol: 0. 02% by weight, purified water ... balance, total 100% by weight, and serum base (10
Double solution sodium hyaluronate: 5% by weight, 10 times solution hydrolyzed elastin: 5% by weight, glycerin: 10% by weight,
Vitamin C: 0.5% by weight, vitamin B1: 0.005% by weight, vitamin B2: 0.01% by weight, 10 times liquid collagen: 30% by weight, purified water: balance, total 100% by weight)
On the other hand, aspergillus niger (A. niger), which is a kind of black mold, was inoculated to 5 × 10 ⁶ / ml, and a storage test was conducted on each sample under the conditions of 37 ° C., humidity 90% by weight, and 30 days. I went. As a result, as shown in Table 2, molds did not occur in Examples A, B, C1 and C2, but molds occurred in the control (no addition) and the amber powder, and there was no antibacterial action. Was recognized. Table 2
In, x indicates that mold is generated, and ◯ indicates that mold is not generated.

Table 2 Cream base Serum base control × × Amber powder 2000ppm × × Example A 3000ppm 〇 〇 Example B 6000ppm 〇 〇 Example C1 1500ppm 〇 〇 Example C2 400ppm 〇 〇

Next, the antioxidant effect of Examples A, B, C1 and C2 was tested using soybean oil. As an experimental example, the active ingredients of Examples A, B, C1 and C2 were used, as Comparative Example 1, 300 mesh pass amber powder, and as Comparative Example 2 d.
-A-Tocopherol is used, control (no addition) soybean oil, 100ppm, 300ppm,
Using soybean oil added with 1,000 ppm and 2,000 ppm as a test oil, an oven test at 60 ° C. ± 2 ° C. was performed.
The change with time of peroxide value (hereinafter referred to as POV) was measured. The results are shown in graphs 1 to 6 shown in Table 3. Graph 1 relates to amber powder of 300 mesh pass, Graph 2 is da-tocopherol, Graph 3 is Example A, Graph 4 is Example B, Graph 5 is Example C1,
Graph 6 relates to Example C2.

It was found that the amber powder shown in graph 1 of Table 2 accelerates the oxidation of the soybean test oil and deteriorates the fats and oils in the test oil. On the other hand, Examples A, B, C1 and C2 all showed antioxidant performance. In particular, Example B was the strongest and showed a stronger antioxidant performance than the commonly used natural antioxidant da-tocopherol (vitamin E). In addition, da-tocopherol has a maximum of 300 ppm,
If the amount is more than 1,000 ppm, there is a drawback that the oxidation is promoted, contrary to the case of the control (no addition). This is said to be due to autooxidation of tocopherols.
On the other hand, it was found as an experimental result that in Examples A, B, C1 and C2, the effect tended to become stronger as the concentration increased.

[0020]

[Table 3]

Next, the deodorant function of the detergents of Examples A, B, C1 and C2 is 20% by weight of a natural detergent, coconut oil fatty acid hydrolyzed collagen sodium solution (a liquid detergent, shampoo, body soap, etc. can also be applied. ) Was added with 0.5% by weight of the active ingredient of each of Examples A, B, C1 and C2, and a sensation test for odor removal was conducted by 11 panelists. In Table 3, the odor when 0.1 ml of the cleaning agent was added to 1 ml of the aqueous solution containing the odorous substance of 0.1 ppm each was shown by the five-level evaluation. A control (no addition) was used as a comparative example. According to Table 3, in the case of the control (no addition), 1 ml of an aqueous solution containing 0.1 ppm of odorous substance gives off a strong malodor, while Examples A, B and C
It was demonstrated that C1 and C2 had almost no odor.

Table 4 Ammonia Trimethylamine Hydrogen sulfide Methyl mercaptan Control 5.0 5.0 5.0 5.0 5.0 Example A 0 0 1.2 2.4 Example B 0 0 2.6 2.2 Example C1 2 .2 3.2 1.2 1.1 2.2 Example C2 0 1.2 1.1 1.1 1.1

Another deodorant test and the deodorant power when vaporized were measured. (See Table 5) In this case Example C
1. Dissolve the active ingredient of C2 in absolute ethanol and
A weight% solution was prepared, which was evaporated into the test space at a rate of 1 ml / m ³ , and the same sensitivity test was conducted to evaluate whether or not the bad odor of 0.01 ppm could be eliminated. The panelists averaged 11 people. Tobacco odor adopted as an odor substance was 5 mild seven / m ³ . A control (no addition) was used as a comparative example. Table 5 clearly shows that the deodorizing effects of Examples C1 and C2 are large and the deodorizing power is large even in the gas phase. From the above, the active ingredient derived from amber exhibits a strong deodorizing power both in the gas phase and in the liquid phase.

Table 5 Trimethymethylmethylammonium ruamine Hydrogen sulphide Lcaptan Tobacco control 5.0 5.0 5.0 5.0 5.0 5.0 Example C1 1 2 2 3 1 Example C2 0 0 1 2 1

The cleaning components contained in the detergent tend to roughen the hands. Sodium lauryl sulphate, which is particularly hemolytic,
It is a causative substance for rough hands, as described in the cosmetic material standard commentary (Yakuji Nippo). The effect of the amber component-containing agent of the present invention on hand roughness was tested in the following. Eight housewives were asked to use a detergent containing 20% by weight of sodium lauryl sulfate (the remainder being purified water) as a kitchen detergent for 7 days each, and a rough hand survey was conducted. Each of the kitchen detergents was added with 0.5% by weight of the active ingredients of Examples A, B, C1 and C2, a control (no addition) as a comparative example, and an amber powder as a comparative example 2. The evaluation was carried out on a 5-point scale. << Evaluation criteria >> 1. Obviously, my hands were rough, and I had symptoms such as a rash, redness, and itching. 2. The skin was dry, the fat was removed and the hands were rough. 3. I felt my hands rough when my hands were dry. 4. I felt a slight dry and rough hand. 5. I didn't feel rough at all. In addition, 0.5% of the active ingredient of Examples A, B, C1 and C2 was further applied to a person with rough hands using a control (additive-free) kitchen detergent containing 20% by weight of sodium lauryl sulfate.
The condition of the hands was examined after having been continuously used with the kitchen detergent added by weight%.

Table 6 Mean values of rough hands, using controls Mean values of recovered humans control 1.6 --- Amber powder 1.7 1.3 Example A 3.8 3.6 Example B 4.2 4.1 Example C1 2.0 2.3 Example C2 2.4 2.0

With the control (no active ingredient added) kitchen detergent, rash, itch, dryness, dryness, and other rough ages were clearly observed. Amber powder also had rough hands. However, in Examples A, B, C1 and C2, the presence of the active ingredient alleviated the degree of rough hands, and particularly in Example B, peeling and mildening had a great effect.

Next, people who had rough hands using a control kitchen detergent were further asked to use Examples A, B, C1 and C2 and the amber powder-containing detergent as a comparative example for one week before evaluation. As a result, in the case of the amber powder, the deterioration was further aggravated, but in Examples A, B, C1 and C2, the improvement of hand roughness was observed. Moreover, in Examples A and B, inflammation such as redness was reduced and a remarkable anti-inflammatory effect was also exhibited.

Next, the test results for hemolytic toxicity will be described. Like hemorrhage, hemolysis is an index of toxicity to cells, and its relation to chakra is also discussed.
Therefore, hemolytic toxicity in Examples A, B, C1 and C2 was measured. Control was used as Comparative Example 1, and amber powder was used as Comparative Example 2.

Table 7Incomplete hemolysis concentration Control 5ppm Amber powder 5ppm Example A 15 ppm Example B 30 ppm  Example C1 10 ppm Example C2 10 ppm

The control (no active ingredient added) sodium lauryl sulfate shows hemolytic activity at only 5 ppm.
Amber powder is not as effective as the control,
All of Examples A, B, C1 and C2 are effective, and Example B is 30 ppm, which is 6 times milder. From this, it can be seen that each Example has lower cytotoxicity than Comparative Examples 1 and 2, and it is also correlated with less rough hands.

Next, the whitening effect will be described. 1000 of Examples A, B, C1 and C2 were added to a melanin pigment producing medium.
A sample mixed at a concentration of ppm is used as the test medium of the present invention,
As Comparative Example 1, a control (non-added) medium was prepared, and as Comparative Example 2, a sample in which amber powder was mixed at a concentration of 1000 ppm was prepared, and the inhibition rate of tyrosinase that synthesizes a melanin pigment was measured according to a standard method of in vitro. I investigated the effect. Table 8 shows the results.

Table 8 Suppression rate control 0% Amber powder 2% Example A 81% Example B 92% Example C1 57% Example C2 28%

According to the results of Table 8, Examples A, B, C
In all of 1 and C2, a remarkable inhibitory effect of tyrosinase was observed, but there was almost no effect on amber powder. In particular, Examples A, B, C1 and C2 which were subjected to ultrasonic waves had a strong whitening effect, and Example B having a large amount of non-volatile components showed the strongest effect.

[0035]

EFFECTS OF THE INVENTION The present invention, as described above, uses amber as a raw material, "a composition component obtained by melting amber", "residual composition component obtained by removing low-boiling substances from molten amber", "amber-extracted low-boiling substance". Antibacterial to "Extracted low boiling point substances from composition components obtained by melting amber",
We have found new effects such as anti-oxidation, deodorization, hand and skin roughening, anti-inflammatory, whitening effect, etc. These are various problems that are present as they are or blended with various products with oils and surfactants It was possible to solve the problem, and it was possible to develop a new application of amber.

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[Procedure amendment]

[Submission date] April 17, 1996

[Procedure amendment 1]

[Document name to be amended] Statement

[Name of item to be corrected] 0032

[Correction method] Change

[Correction contents]

Next, the whitening effect will be described. Examples melanin producing enzyme reaction solution A), and a specimen by mixing a B, C1, C2 at a concentration of 1000 ppm. And control (no additive) sample as a comparative example 1, the amber powder to create a mixed analyte at a concentration of 1000ppm as Comparative Example 2, the inhibition rate of tyrosinase to synthesize melanin pigment was measured by a conventional method in Vito b , Examined the whitening effect. Table 8 shows the results.

─────────────────────────────────────────────────── ─── Continuation of front page (51) Int.Cl. ⁶ Identification number Internal reference number FI Technical display location A61K 35/78 ABF A61K 35/78 ABFB ADA ADAB ADZ ADZB A61L 9/01 A61L 9/01 Z C09K 15 / 34 C09K 15/34 (72) Inventor Nouichi Sawaguchi 1-31-15 Yoyogi, Shibuya-ku, Tokyo Inside the Advanced Utilization Research Center for Natural Medicines Co., Ltd. (72) Kazuro Nakao 1-31-15 Yoyogi, Shibuya-ku, Tokyo Incorporated crude drug advanced utilization research institute

Claims (11)

[Claims] 1. An amber ingredient-containing agent, characterized in that the amber composition ingredient obtained by melting external amber by applying external energy is an active ingredient. 2. A residue obtained by extracting an organic solvent-soluble component with an organic solvent from the composition components of amber obtained by melting external amber by applying external energy, and adding external energy to the residue to obtain a residue. An amber ingredient-containing agent, characterized in that a composition ingredient is an active ingredient. 3. An amber component-containing agent, which comprises a low boiling point substance extracted from amber as an active ingredient. 4. An amber ingredient-containing agent, characterized in that a low boiling point substance extracted from a composition component of amber obtained by melting external amber by applying external energy is used as an active ingredient. 5. An amber ingredient-containing agent, wherein the active ingredient according to any one of claims 1 to 4 exhibits antibacterial properties. 6. An amber ingredient-containing agent, wherein the active ingredient according to any one of claims 1 to 4 exhibits antioxidant properties. 7. An amber ingredient-containing agent, wherein the active ingredient according to any one of claims 1 to 4 exhibits deodorant properties. 8. An amber ingredient-containing agent, wherein the active ingredient according to any one of claims 1 to 4 exhibits hand / skin roughening preventive properties. 9. An amber ingredient-containing agent, wherein the active ingredient according to any one of claims 1 to 4 exhibits anti-inflammatory properties. 10. An amber ingredient-containing agent, wherein the active ingredient according to any one of claims 1 to 4 exhibits a whitening effect. 11. The amber component-containing agent according to claim 1, 2 or 4, wherein the external energy is only heating, only electromagnetic waves, or heating and ultrasonic waves or a combination of heating and electromagnetic waves. Amber ingredient-containing agent.