JP2004315391A - Olive fruit extract and method for producing the same - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To obtain an olive fruit extract which exhibits excellent physiological activities, and to provide a method for producing the same. <P>SOLUTION: The olive fruit extract is characterized by being obtained by the extraction of olive fruits with a mixture of 1,3-butylene glycol with water. A cosmetic is compounded with the olive fruit extract. The method for producing the olive fruit extract comprises extracting harvested olive fruits or oil-squeezed olive fruit residues with the mixture of 1,3-butylene glycol with water. The olive fruit extract has highly more excellent hyaluronidase activity-inhibiting action, esterase activity-inhibiting action, active oxygen-scavenging action, collagen degradation-depressing action, and the like, than those of conventional extracts. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

表１から解るように、本発明のオリーブ果実抽出物を配合したハンドクリームは、従来品を越える著しい美肌作用を奏する。
【００３１】
試験例６：オリーブ果実抽出物配合ボディーソープの製造
以下の基本成分に加え、実施例１のオリーブ果実抽出物をその他の成分の合計に対して２重量％配合して、ハンドクリームを得た。
基本成分：
ラウリル硫酸アンモニウム ８％
ポリオキシエチレンラウリルエーテル硫酸ナトリウム ２％
椰子油脂肪酸アミドプロピルベタイン ７％
椰子油脂肪酸モノエタノールアミド ４％
エデト酸２ナトリウム ０．２％
安息香酸ナトリウム ０．２％
クエン酸 ０．２％
水 残部
こうして製造したボディーソープおよびオリーブ果実抽出物を含まない以外は同一の組成を有するボディーソープを被験者に１日１回使用させ、１０日後の皮膚の変化を潤い、張りおよび艶の３項目について観察した。
結果を表２に示す。表２の結果は、それぞれの項目について改善された被験者の数を示す。
【表２】

表２から解るように、本発明のオリーブ果実抽出物を配合したボディーソープは、従来品を越える著しい美肌作用を奏する。
【００３２】
【発明の効果】
本発明によれば、１，３−ジブチルエーテルで抽出することにより、ヒアルロニダーゼ活性阻害作用、エラスターゼ活性阻害作用、活性酸素消去作用、コラーゲン分解抑制作用等について、従来品と比較して格段に優れたオリーブ果実抽出物を提供することができる。係るオリーブ果実抽出物は、特に軟膏、クリーム、乳液、懸濁液、溶液等の外用薬に好ましく配合することができる。
【図面の簡単な説明】
【図１】図１は、本発明のオリーブ果実抽出物の製造方法を図示する流れ図である。[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to an olive fruit extract that is extracted from olive fruits and exhibits excellent physiological activity, and a method for producing the same.
[0002]
[Prior art]
Olives are plants of the Oleaceae family that originate from the Mediterranean coast, and have been cultivated for food and oil for a long time. The olive fruit usually grows from about October and becomes pale green, and when it has purple-red spots, it is a time suitable for processing into green pickles. Then, around November, the whole will become so-called live olives, which have a purple-black color, and will be suitable for salting. Ripe olive fruits around December contain about 15 to 30% of oil, and olive oil is pressed from the olive fruits at this time. The olive fruits and olive oil thus obtained are known to have various excellent effects such as reduction of arteriosclerosis, stomach ulcer and constipation, strengthening of bones, prevention of aging, and beautiful skin effect.
[0003]
Above all, olive oil is a vegetable oil containing various active ingredients such as oleic acid, provitamin A, vitamin B, vitamin Ks, polyphenols and the like. Effects of cancer and polyphenols on cancer development and promotion of bone formation based on provitamin A, vitamin D and vitamin K have been reported. Olive oil also has beautiful skin effects such as reducing rough skin, keeping the skin healthy, moisturizing the skin, protecting the skin, and preventing the skin from drying out, and is used in cosmetics and external medicines. ing.
[0004]
Further, as an olive fruit extract obtained from olive fruits, those obtained by extracting fruits and / or seeds of olive plants with water and / or an organic solvent are known (for example, see Patent Document 1). It has been reported that this extract has an active oxygen scavenging effect, a melanin production inhibitory effect and a tumor cell growth inhibitory / killing effect, and the solvent used for extraction imparts safety to the human body for the resulting extract. From the viewpoint of increasing the effect and increasing the action, it is considered desirable to use a mixed solvent of water and alcohol.
[0005]
[Patent Document 1]
JP 2001-181197 A
[Problems to be solved by the invention]
As described above, olive fruits contain various active ingredients that have beneficial effects on living organisms (these are generally referred to as “olive extracts”). However, the efficiency of separating and purifying these active ingredients from olive fruits and further concentrating them is currently low. There is a need for more efficient extraction of active ingredients from olive fruits, and to obtain olive fruit extracts in a form that is advantageous for incorporation into foods, beverages, pharmaceuticals, and topical medicines. large.
[0007]
The present invention has been made in view of the above problems, and an object thereof is to efficiently extract an active ingredient contained in olive fruits, and as a result, an olive fruit extract exhibiting excellent physiological activity. And a method of manufacturing the same.
[0008]
[Means for Solving the Problems]
The present inventors have conducted intensive studies, and as a result, by extracting olive fruits, particularly with a mixture of 1,3-dibutylene glycol and water, a hyaluronidase activity inhibitory effect, an elastase activity inhibitory effect, an active oxygen scavenging effect, collagen The present inventors have found that an olive fruit extract having remarkably superior properties as compared with conventional products can be obtained with respect to the decomposition inhibitory action and the like, and based on this, the present invention has been completed.
[0009]
Therefore, the present invention
Olive fruit extract obtained by extracting olive fruit with a mixture of 1,3-butylene glycol and water,
A cosmetic comprising the olive fruit extract, and an olive fruit extract obtained by extracting a collected olive fruit or olive fruit cake after oil extraction with a mixed solution of 1,3-butylene glycol and water. It relates to a manufacturing method.
[0010]
BEST MODE FOR CARRYING OUT THE INVENTION
Next, the present invention will be described in more detail with reference to the drawings. FIG. 1 is a flowchart illustrating one embodiment of the method for producing an olive fruit extract of the present invention.
[0011]
In the production of the olive fruit extract of the present invention, first, an olive fruit, which is a raw material of the olive fruit extract, and a mixture of 1,3-butylene glycol, which is an extraction solvent, and water are charged into an extraction container. There are various varieties of olives, such as Misson, Manzanillo, Nevadiro Blanco, Picual, Hojiblanca, Arbequina, and Niconica abraña Cranica abraña Mánica bráná zánánánánica or Manica nilica. ), Gordal, Francoisio, Moroiolo, Leccino, Corlatina, Ascolana Terena, etc., and the average of the fruits in each of these varieties. The weight and oil content are different, and the suitable applications are different from those for fruit processing, oil, To have. However, the olive fruit extract of the present invention can be produced from any variety of olives.
Also, the olive fruit as a raw material may be olive fruit cake after olive oil has been pressed, or frozen olive fruit may be used.
[0012]
As the extraction solvent, a 100% 1,3-butylene glycol solvent containing no other auxiliary solvent can be used. However, the extraction solvent can be a mixed solvent composed of water and 1,3-butylene glycol. When a mixed solvent is employed, its concentration is, for example, 30% by volume.
[0013]
After charging the olive fruit and the extraction solvent in the extraction container, extraction is then performed. The extraction can be performed at a slightly higher temperature than room temperature to promote the extraction action. For example, when the extraction temperature is 50 to 60 ° C., the extraction time is about 5 hours.
[0014]
After completion of the extraction, the olive fruit and the extract are separated. The separation of olive fruits can be performed by filtration. The obtained filtrate may be diluted to several times the whole amount if it is convenient for the subsequent solid content separation.
[0015]
Next, filtration is performed again to further separate the solid content contained in the extract. Prior to the solid content separation, it is preferable to add an adsorbent such as diatomaceous earth to the liquid to be filtered to adsorb and separate fine solid content. The amount of the adsorbent is not particularly limited, but is, for example, 10% by volume based on the liquid to be filtered.
[0016]
After the solid content is separated in this way, the obtained filtrate is sterilized. Sterilization can be performed by ordinary heat sterilization, and for example, pasteurization that is maintained at 80 to 90 ° C. for about 1 hour is preferable. Although high-temperature sterilization employing a temperature exceeding 100 ° C. can shorten the sterilization time, it is not a preferable method because it causes decomposition of the active ingredient contained in olive fruits.
[0017]
The olive fruit extract of the present invention is obtained by filtering the sterilized liquid again. This final filtration is preferably performed using a fine filter having a cutoff of, for example, 0.5 μm. By such filtration, the amount of solids contained in the olive fruit extract can be reduced to 0.5% or less.
[0018]
The olive fruit extract of the present invention thus produced exhibits many excellent physiological activities, but the most notable ones are an inhibitory action on hyaluronidase activity, an inhibitory action on elastase activity, a scavenging action on active oxygen, and an inhibitory action on collagen degradation. Each of these operations will be briefly described below.
[0019]
-Hyaluronidase activity inhibitory action Hyaluronic acid has functions such as water retention and flexibility, and is important for keeping skin moist. Hyaluronic acid is degraded by its hydrolyzing enzyme, hyaluronidase. By inhibiting the activity of hyaluronidase, it is possible to suppress the degradation of hyaluronic acid and to prevent a decrease in the moisturizing property, lubricity and flexibility of the skin.
[0020]
Elastase activity inhibitory action Elastin is an elastic tissue contained in the skin, and when it is decomposed, the skin gradually loses its elasticity and elasticity. Elastin degradation is carried out by elastase, which is activated by aging and by external and internal stimuli such as ultraviolet rays. Therefore, if the activity of elastin, which is a degrading enzyme of elastin, can be inhibited to suppress the degradation of elastin, the elasticity of the skin can be maintained and the skin can be kept firm and moist.
[0021]
-Reactive oxygen scavenging action Reactive oxygen is one of the external factors that cause skin inflammation and aging, and it also damages internal tissues and causes wrinkles. Therefore, in order to prevent skin aging and inflammation, elimination of active oxygen by an antioxidant or a radical scavenger is useful. Whether or not an active oxygen scavenging effect is exhibited can be determined from the presence or absence of SOD-like activity and other antioxidant tests.
[0022]
-Collagen degradation inhibitory action Collagen is a substance that has an important function in keeping the skin firm and elastic. However, when collagenase, which is a collagen-degrading enzyme, is activated by external stress such as ultraviolet rays or aging in a living body, the amount of collagen in the skin decreases, which causes wrinkles and loosening. If the activity of collagenase can be inhibited, the degradation of collagen can be suppressed and the skin can be kept healthy.
[0023]
The olive fruit extract of the present invention can be in various dosage forms. For example, it can be blended with foods, drinks, pharmaceuticals, and the like that are taken orally. Above all, it exhibits an excellent skin-beautifying effect, and is therefore preferably formulated into an external preparation directly applied to the skin, for example, an ointment, cream, emulsion, suspension, solution or the like. The compounding amount in these is, for example, 1 to 50% by weight.
[0024]
【Example】
The following examples illustrate the invention in more detail, but these examples are not intended to limit the invention to certain embodiments.
[0025]
Example 1: Production of olive fruit extract An olive fruit extract was produced as follows.
Charging: 100 g of frozen olive fruits and 1000 g of a 30% 1,3-butylene glycol aqueous solution were charged in an extraction container.
Extraction: The extraction vessel was heated to maintain the inside at 50-60 ° C. Extraction was performed at this temperature for 5 hours with stirring.
Olive fruit separation: After completion of the extraction, the olive fruit was removed, and 1000 g of a 30% aqueous solution of 1,3-butylene glycol was added to dilute the extract twice.
Solid separation: 200 g of diatomaceous earth (Radiolite # 200) was added to the diluted solution, and the mixture was stirred for 1 hour to adsorb fine solids. Thereafter, the diluent was filtered to separate the solid content and diatomaceous earth.
Sterilization: The filtrate was heated to 80 to 90 ° C. and sterilized by heating for 1 hour with stirring.
Final filtration: The sterilized filtrate was finally filtered using a 0.45 μm cut-off filter.
According to the above procedure, 1541.2 g of an olive fruit extract containing 0.38% of solids was obtained.
[0026]
Test Example 1: Evaluation of hyaluronidase activity inhibitory action Except that olive fruit extract obtained in Example 1 was replaced with water instead of a 30% 1,3-butylene glycol aqueous solution, the same as Example 1 was used. The olive fruit water extract obtained in the process was evaluated for its hyaluronidase activity inhibitory action. The reason for using water for the extraction is that when the olive fruit extract contains alcohol, it is impossible to measure the hyaluronidase activity.
0.2 mL of olive fruit water extract, 0.1 mL of hyaluronidase solution, Compound 48 / 800.2 mL, and 0.2 mL of potassium hyaluronate solution were mixed and reacted at 37 ° C., followed by 0.3 mL of 0.4N sodium hydroxide. Was added to stop the reaction. Then, the boric acid solution was added and mixed. The resulting solution was heated in a boiling water bath to inactivate the enzyme, cooled to room temperature on ice, added with 6 mL of p-DAB, allowed to stand at 37 ° C for 20 minutes, and then measured for absorbance at 585 nm for hyaluronan. The acid was quantified.
The result was the concentration of the extract required to inhibit the hyaluronidase activity by 50% (IC ₅₀ ), and was 0.318 mg / mL.
The results obtained for the water extract are in themselves good. However, it is known in the prior art that the substance having the ability to inhibit hyaluronidase activity is a polysaccharide such as peptin, and the polysaccharide is generally more efficient using water and 1,3-butylene glycol than ethanol. It is also known that it can be extracted. Therefore, the olive fruit extract of Example 1 is expected to exhibit hyaluronidase activity that is comparable to or higher than the water extract tested in this test example, and that is much better than the ethanol extract.
[0027]
Test Example 2: Evaluation of elastase activity inhibitory action Exactly the same as Example 1 except that instead of the olive fruit extract obtained in Example 1, water was used for extraction instead of an aqueous 30% 1,3-butylene glycol solution. The elastase activity inhibitory effect of the olive fruit water extract obtained in the process was evaluated. The reason why water was used for the extraction was that, as in Test Example 1, when the olive fruit extract contained alcohol, the elastase activity could not be measured.
50 μL of olive fruit water extract, 25 μL of 12 μg / mL human leukocyte-derived elastase (manufactured by ELASTIN PRODUCT CO. INC), and 25 μL of methoxy-succinyl-alanyl-alanyl-propyl valine-p-nitroanilide prepared to 8 mM, were mixed. The reaction was performed at 37 ° C. for 20 minutes. The absorbance at 405 nm of the solution after the reaction was measured, and the amount of nitroaniline produced was quantified.
The result was the concentration of the extract required to inhibit elastase activity by 50% (IC ₅₀ ), and was 11.8 mg / mL.
The results obtained for the water extract are in themselves good. However, it is known in the prior art that the substance having elastase activity inhibitory ability is a polysaccharide such as peptin, and the polysaccharide is generally more efficiently used with water and 1,3-butylene glycol than with ethanol. It is also known that it can be extracted. Thus, the olive fruit extract of Example 1 is expected to exhibit elastase activity that is comparable to or higher than the water extract tested in this test example, and that is significantly better than the ethanol extract.
[0028]
Test Example 3: Evaluation of active oxygen scavenging action The active oxygen scavenging action of a two-fold dilution (solid content 0.19%) of the olive fruit extract obtained in Example 1 was evaluated for both the SOD-like action and the antioxidant test. Was evaluated.
4-1: SOD-like action NBT was reduced by xanthine and O ₂ ⁻ generated by xanthine oxidase, and the amount of formazan produced was quantified by measuring absorbance at 560 nm, and the SOD-like activity was evaluated by the NBT method.
The results showed that the 2-fold dilution of the olive fruit extract obtained in Example 1 had a SOD-like effect of 76.0%.
4-2: Antioxidant test A stable radical having an ultraviolet absorption at 517 nm in a purple color: diphenylpicrylhydrazyl (DPPH) is used, and the disappearance of the purple color of the radical by the action of an antioxidant is measured. Thereby, the active oxygen scavenging action was evaluated.
As a comparison, the same test was carried out when an olive fruit extract produced by extraction with water and an olive fruit extract produced by extraction with ethanol were added.
The results showed that a two-fold dilution of the olive fruit extract obtained in Example 1 had 75.0% antioxidant properties.
From the above results, it can be seen that the olive fruit extract obtained in Example 1 exerts a high active oxygen scavenging effect in both cases of evaluation by the SOD-like action and the antioxidant test.
[0029]
Test Example 4: Evaluation of collagenase activity inhibitory action The olive fruit extract obtained in Example 1 was evaluated for collagenase activity inhibitory action.
50 μL of the olive fruit extract of Example 1, 50 μL of 0.1 mg / mL collagenase type IV (manufactured by Sigma), and 400 μL of 0.39 mg / mL PZ-peptide (manufactured by BACHEM Fenichemikalian AG) were mixed, and the mixture was added at 37 ° C. The reaction was performed for 30 minutes. The reaction was terminated by adding 1 mL of a 25 mM citric acid solution to the reaction solution. The solution was further extracted by adding 5 mL of ethyl acetate, the ethyl acetate layer was separated by centrifugation, and the absorbance at 320 nm was measured.
The result was 10.4, assuming that the inhibitory action collagen degradation amount when distilled water was added instead of the olive fruit extract was 100. Therefore, the olive fruit extract of Example 1 can inhibit the activity of collagenase and significantly suppress the degradation of collagen.
[0030]
Test Example 5: Production of hand cream containing olive fruit extract In addition to the following basic components, the olive fruit extract of Example 1 was blended at 3% by weight based on the total amount of other components to obtain a hand cream.
Basic ingredients: water, mineral oil, petrolatum, glycerin, hydrogenated polyisobutene, microcrystalline wax, cyclomethicone, lanolin alcohol, paraffin, squalane, jojoba oil, decyl oleate, octyldodecanol, aluminum distearate, magnesium stearate, magnesium sulfate Magnesium, citric acid, benzoate, tocopherol, butylhydroxyanisole, dibutylhydroxytoluene, fragrance.
The hand cream thus prepared and the hand cream having the same composition except that it does not contain the olive fruit extract are applied to the skin of the subject once a day, and after 10 days, the change of the applied area is moistened, and the three items of tension and gloss are applied. Was observed.
Table 1 shows the results. The results in Table 1 show the number of subjects who improved for each item.
[Table 1]

As can be seen from Table 1, the hand cream containing the olive fruit extract of the present invention has a remarkably beautiful skin effect exceeding that of the conventional product.
[0031]
Test Example 6: Production of body soap containing olive fruit extract In addition to the following basic components, the olive fruit extract of Example 1 was blended at 2% by weight based on the total of other components to obtain a hand cream.
Basic ingredients:
8% ammonium lauryl sulfate
Sodium polyoxyethylene lauryl ether sulfate 2%
Coconut oil fatty acid amidopropyl betaine 7%
Coconut oil fatty acid monoethanolamide 4%
Edetate disodium 0.2%
Sodium benzoate 0.2%
0.2% citric acid
Water balance The body soap having the same composition except that the body soap and the olive fruit extract thus produced are not used is used by the test subject once a day. Observed.
Table 2 shows the results. The results in Table 2 show the number of subjects who improved for each item.
[Table 2]

As can be seen from Table 2, the body soap containing the olive fruit extract of the present invention has a remarkably beautiful skin effect exceeding conventional products.
[0032]
【The invention's effect】
According to the present invention, by extracting with 1,3-dibutyl ether, the hyaluronidase activity inhibitory action, elastase activity inhibitory action, active oxygen scavenging action, collagen degradation inhibitory action, etc. are significantly superior to conventional products. An olive fruit extract can be provided. Such an olive fruit extract can be preferably incorporated into an external preparation such as an ointment, a cream, an emulsion, a suspension, or a solution.
[Brief description of the drawings]
FIG. 1 is a flow chart illustrating a method for producing an olive fruit extract of the present invention.

Claims (3)

An olive fruit extract obtained by extracting olive fruits with a mixture of 1,3-butylene glycol and water. A cosmetic comprising the olive fruit extract according to claim 1. A method for producing an olive fruit extract, comprising extracting a collected olive fruit or olive fruit cake after oil extraction with a mixed solution of 1,3-butylene glycol and water.

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