JP2008150336A - Rose antioxidation substance - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To eliminate the defects of a rose oil or a rose water extracted from a rose flower comprising easy oxidation, degradation and fragrance loss with time. <P>SOLUTION: Based on the new findings made by the inventors that the extracted rose oil or rose water contains tannic acid and yeast, the inventors have found that a rose antioxidation substance having excellent fragrance, sterilizing effect and antiseptic effect can be produced by fermenting, aging and purifying a rose oil and a rose water taking advantage of the action of the tannic acid and yeast. The rose antioxidation substance has high stability and high safety to human body and is usable as an antioxidation agent for cosmetics, drinks, foods, drugs, and quasi-drugs. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention ferments, matures and purifies rose oil and rose water, which are substances extracted from rose flowers, which can be used in the fields of preservatives, fragrances, cosmetics, beverages, foods, pharmaceuticals, quasi drugs, etc. The present invention relates to a rose antioxidant substance comprising the obtained composition as an active ingredient.

  In general, in the process of production, processing, and storage of cosmetics, foods, pharmaceuticals, quasi-drugs, etc., chemically synthesized antiseptics and fungicides such as parabens are used to prevent deterioration of quality due to decay. There are many. However, conventional antiseptics that have been chemically synthesized do not decompose even if they enter the skin or human body, so if they are used for a long period of time, they will disrupt the cycle of the body and cause side effects such as functional disorders and diseases in the skin and body. There is a harmful effect that occurs. Therefore, use tends to be avoided from the viewpoint of safety, and there is an increasing expectation for preservatives derived from natural products, in particular, plant-based preservatives that function continuously in the living body. However, no biodegradable preservatives that are friendly to humans and the earth have been found to have sufficient antioxidant activity and bactericidal performance.

  Antioxidants contained in foods such as flavonoids, caffeic acid derivatives, sesaminol and phytic acid are currently attracting attention and expected as natural antioxidants, but tannins such as polyphenols are also substances with high antioxidant activity. R & D is being conducted as Polyphenol is a general term for plant components that have multiple phenolic hydroxy groups (hydroxy groups bonded to aromatic rings such as benzene and naphthalene rings) in the molecule. It is a flavonoid that is a pigment component of plants and an astringent component of tea. It is well known that catechins and tannins such as gallic acid and cinnamic acid are also members of this group. Specific health functions of polyphenols include antioxidant activity, plaque-generating enzyme inhibitory activity, antibacterial / antiviral activity, serum cholesterol elevation inhibitory effect, blood pressure regulating effect, α-amylase inhibitory effect (blood glucose level regulating effect), body Inhibition of fat accumulation, improvement of intestinal microflora, deodorizing action, polyphenol has been recognized as an effect for food for specified health use, and is also based on medicine and nutrition (Non-Patent Document 1) .

Conventionally, as a proof of the antibacterial action of the aromatic components of rose oil, the antibacterial activity of rose oil (Rose Otto Oil) and its main components, citronellol and geraniol, was confirmed by Staphylococcus.
aureus, Escherichia coli, Candida albicans, Aspergillus
fumigatus), soaked a 5% ethyl acetate solution of rose oil in a paper disk (diameter 8 mm), air-dried, cultured in Muller Hinton (bacteria) or RPM1640 medium (fungus) and measured. The measured values of staphylococci 17 mm, Escherichia coli 0 mm, Candida 22 mm, and Aspergillus 37 mm have been proven (Non-patent Document 2).

In addition, as a method for showing the bactericidal efficacy of conventional rose oil and its aromatic components,
According to the measured value of the carboxylic acid coefficient measured using typhosus, Eberth), rose oil 7.0, Geraniol 11.5, Linalool 7.0, Eugenol 14.4, phenylethyl alcohol It can be seen that (Pheyl-ethyl-alcohol) 9.0 and β-ionone 2.2 have strong bactericidal properties (Non-patent Document 3).

In addition, regarding the safety of rose oil, it has been announced that GRAS certification “indicates that the US Pharmaceutical Agency has been certified as the safest flavor since 1965” has been confirmed. Absolute Rose Dome (Rosa Centifolia), Otto Rose Bulgaria (Rosa Damascena), Otto Rose Morocco (Rosa Centilolia), Otto Rose Turkey (Rosa
Damascena) was stimulated with 5 g / kg of oral toxic LD50 rats and 2.5 g / kg of cost toxic LD50 rats (of which the cost toxic LD50 rats> 8 g / kg uncertain in this absolute rose dome study). When the phototoxicity was examined, all items were proved to be “no irritation” in the 48-hour closed patch test for irritation. In addition, all items have been proved to be “no stock solution” in phototoxicity. Accordingly, it has been confirmed that it is safe to apply a rose oil concentration of 100% to the skin (Non-Patent Document 4).

  In traditional folk medicine and folk remedies, it has been said that rose has a tonic effect, a tranquilizing effect, an intestinal regulating action, an improvement of gynecological diseases, and a soothing action on the mucous membranes of the eyes and skin. Has been recognized and widely used. However, in the effect and support, there are many parts for which the relationship between specific active ingredients and their functions has not yet been demonstrated. Rose water has been drunk for a long time, and rose oil has been used as a raw material for high-quality perfumes and high-quality foods. However, conventional rose water and rose oil are unstable because they are easily oxidized and the fragrance is easily deteriorated.

For this reason, rose water (aromatic distilled water) that has been generally marketed domestically in the past is often in an already oxidized state, has the drawbacks of musty and perishable, few fragrant ones, chemical synthesis Many cases are adjusted with antiseptics. As described above, there has never been a product that is a natural product but does not oxidize, does not rot, and has a good aroma.
Kunio Nakagawa, “Health Functional Functional Food Tokuho Foods for Specified Health”, Bookman, May 1999, pp. 143-144 Inoue Shigeharu, “Microorganisms and Fragrances”, Fragrance Journal, August 2002, p. 189, Table 4-1. Horiguchi Hiroshi, “Bacterial and Fungicidal Chemistry”, Sankyo Publishing, published on January 10, 1982, pages 4-9 Katsuyuki Hamada and Miyako Ishiuchi, “Rose no Parfum”, Kouryudo Co., Ltd. April 2005, p.234, Anpei Mikami aromatopia No. 28 1998

  Rose oil and rose water extracted from rose flowers have the drawbacks of being easily oxidized, decayed, and fragrance easily over time. An object of the present invention is to provide a rose antioxidant substance that has solved these drawbacks.

  As a means to solve this problem, using rose oil collected from rose oil and rose water extracted by steam distillation method, etc., using the action of tannic acid and yeast, Provided is a rose antioxidant obtained by fermentation, aging and purification.

  The rose antioxidant of the present invention is not only excellent in fragrance, bactericidal power and antiseptic effect, but also has high stability and safety to the human body, so it is added to cosmetics, beverages, foods, pharmaceuticals and quasi drugs Can be provided as an antioxidant.

The present inventors discovered and confirmed that tannic acid and yeast were newly contained in the substance extracted from the rose flower. Thereafter, it was found that a rose antioxidant obtained by fermentation, ripening and purification using tannic acid and yeast has a strong antioxidant action and a bactericidal action by an aroma component, and exhibits an excellent antiseptic effect. Tannic acid and yeast have been conventionally known to be contained in rose flower components, but the present inventors have also found that tannic acid and yeast are contained in the extracted rose oil and rose water. I found it included.
Furthermore, even after passing through the extraction process of steam distillation, it was confirmed that the yeast in the rose was alive and contained in rose oil and rose water, and these yeasts (Saccharomyces cerevisiae: Saccharomyces cerevisiae) ) Succeeded in enhancing the stability of the extract by fermenting the extract. Until now, it has not been confirmed that tannic acid is contained in rose oil or rose water extracted by the steam distillation method using high temperature, and that yeast is alive. By containing tannic acid, it is thought that yeast is protected, and it leads to fermentation and ripening.

In the case of rose oil, about 1 kilogram of oil can be extracted from 3 to 4 tons of flowers, and about 1 to 2 tons of rose water can be extracted. In spite of such a large amount of rose components, it is common practice to add synthetic preservatives and synthetic fragrances to improve stability immediately after extraction. The function and effect of the material should be lost. The inventors have succeeded in increasing the stability of these extracts by fermenting them without adding additives.
And as a means for solving the above-mentioned problems, the present inventors have found that a composition obtained by fermenting and ripening this rose oil and rose water and refining it becomes an excellent rose antioxidant with high safety. .

In practicing the present invention, it is first necessary to extract rose oil and rose water from rose flowers. Although the distillation method using the steam extraction method is shown below, the present invention is not limited by the distillation method, and any extraction method can be used as long as an extract suitable for fermentation can be obtained.
Rose extraction begins with the collection of roses. The roses to be collected are preferably healthy flowers that are grown in accordance with the natural rhythm in a good natural environment. With no pesticides, aiming for organic cultivation, go to pick flowers at dawn from May to June when healthy flowers bloom. All the way of picking flowers is collected manually without damaging the flowers. Pick the flowers by dawn from 9am, place them in a well-ventilated hemp bag and transport them to the factory from 9am to 11am. At this time, the flowers to be carried must also be carefully selected. The crushed flowers and the flowers with heat have already decayed, and the fragrance is oxidized and deteriorated. The collected flowers that have not decayed are selected and extracted by spring distillation using spring water. The steam distillation method in the present invention is a well-known technique and does not characterize the present invention. Thereafter, about 1 kilogram of rose oil is extracted from 3 to 4 tons of flowers, and about 1 to 2 tons of rose water can be collected. The numerical values of the weight of these rose oil and rose water vary depending on the annual rose harvest and variety, and are not limited thereto. Rose oil and rose water after extraction are conventionally boiled and sterilized, and added with chemically synthesized substances and preservatives, but in the present invention, without boiling and sterilization in the process until purification, Carry as it is. At this time, it is desirable to carry with an aluminum container, a PET bottle, and a glass container.

Next, fermentation, ripening and refining methods for rose oil are described below. First, when rose oil extracted by the steam distillation method is put in a sealed container and kept at a temperature of 25 to 35 degrees in an anaerobic state, it naturally ferments in 4 to 6 weeks. As fermentation progresses, the pH value decreases, and alcohol, amylase, carbon dioxide and nitrogen compounds are decomposed by the action of active enzymes (tannase and polyphenase) in rose oil, and the composition of rose oil changes. Thereafter, stearoptene contained in rose oil is purified by natural filtration and exclusive. While being anaerobic, the temperature is gradually decreased about every 4 weeks while being divided into 20 degrees to 13 degrees, 13 degrees to 8 degrees, 8 degrees to 4 degrees, 4 degrees to 0 degrees, 0 degrees to -5 degrees and several times. While aging, repeat the natural filtration in the meantime and repeat the purification. After aging by lowering the temperature to −5 ° C., it is naturally thawed and returned to room temperature, and the temperature is lowered again by about 5 ° C. from room temperature, followed by repeated aging and natural filtration. After completion of ripening, the temperature is lowered to −20 ° C. to stop fermentation, and the rose antioxidant in the present invention is completed. The time required for completion is approximately 6 months to 1 year, but the temperature control until the completion of aging and the determination of the aging period are finally determined based on the analytical value of tannic acid, the hydrogen ion concentration and sensory evaluation. In addition, the temperature and period of fermentation, ripening, and refining in the present invention have different properties each time depending on the state of rose oil as a raw material and the like, and are not limited to the above examples. Table 1 below shows the composition of the rose oil composition obtained through the processes of fermentation, ripening and purification.

Next, the fermentation, ripening and purification methods of rose water are described below. In rose water, natural fermentation starts at room temperature after extraction, but the fermentation is allowed to proceed for 4 weeks by setting the temperature to 15 to 20 degrees in an anaerobic state. Thereafter, the temperature is lowered to 12 to 8 degrees and further aged for 4 weeks, then returned to room temperature and again reduced to 13 to 12 degrees and aged for 4 weeks. In the meantime, natural filtration is performed and aging and purification are repeated. After completion of ripening, the temperature is lowered to −20 ° C. to stop fermentation, and the rose antioxidant in the present invention is completed. The period until completion requires about 1 to 2 months, but the temperature control until the completion of aging and the criteria for determining the aging period are finally determined by sensory evaluation. In addition, the temperature setting and period of fermentation, aging, and refinement | purification in this invention are not limited to this. Table 2 below shows the composition of the rose water composition obtained through the purification process.

  After completion of fermentation, ripening and purification, it was confirmed by analytical tests and sensory evaluation that the amount and aroma of tannic acid contained in the composition comprising rose oil and rose water were increased. In rose water, only a small amount of tannic acid is usually detected. However, in the composition of rose water produced using the inventive technique of Table 2, 0.6 g of tannic acid was detected in 100 g. It can be confirmed that the fermentation technology has improved. Further, at this time, 0.1 ml of lactic acid was detected in 100 ml. In the case of rose oil, the composition of the rose oil produced by using the inventive technique and the conventional rose oil was compared, and the amount of tannic acid detected from the latter was improved as compared with the conventional rose oil. This is because during the fermentation of rose oil, an oxidative enzyme possessed by tannic acid oxidizes and polymerizes with an organic compound in rose oil to form polymerized tannin. Thereafter, the tannic acid that has been oxidatively polymerized by repeated purification becomes condensed tannin, and by aging, the binding strength and stability of the condensed tannic acids are increased. Similarly, in the fragrance of roses, the effect of improving the scent components such as ester, geraniol, and phenylethyl alcohol is recognized. This is because higher alcohols produced after fermentation combine with organic acids during ripening, improving the aromatic components such as esters and terpenes, and polymerizing with geraniol and citronellol, which are conventional aromatic components of roses. This is because the nature increases. The amount of tannic acid contained in the rose antioxidant in the present invention varies depending on the origin of the rose and the quality of the annual harvest in the rose oil and rose water after extraction, and the final result is an analytical value of tannic acid and hydrogen. Judged by ion concentration and sensory evaluation.

In the conventional rose water, the aroma is disturbed within a few weeks, and a rotting odor due to oxidation occurs. Therefore, it is necessary to add a preservative to maintain the quality. On the other hand, rose water fermented and purified through the above process was stable in fragrance over a long period of time, and it was confirmed that it was extremely resistant to spoilage even when the pH value was observed. Usually, it oxidizes as the rot progresses, but rot is suppressed by the antioxidant power of the stable tannic acid, and the pH value is stable.
Similarly, it was confirmed that the rose oil was fermented, matured and refined and had a good fragrance for a long period of time and was resistant to spoilage. The measurement graph of the transition of the pH value is shown in FIG. 1, FIG. 3, and FIG. 5 using the skin lotion, moisturizing cream, and drinking water of the formulation examples given in Example 1, Example 2, and Example 3.

In addition, in order to investigate the antioxidant effect of rose antioxidants consisting of rose oil and rose water, the above-mentioned rose lotion, moisturizing cream, drinking water added to the panel for a certain period of time, Each item was provided and the effect was investigated. These formulation examples are shown in Example 1, Example 2, and Example 3. In each item, using the lotion and moisturizing cream to which the above-mentioned rose antioxidant substance is added, the effect on freckle and freckles by 15 female panels from the 10s to the 40s of Example 4, 10 of Example 5 Acne by 15 female panels from teens to 40s, effect on pimples, effect on pores and sagging by 15 female panels from teens to 40s in Example 6, teens from 40s to 40s All four items of the effects on sensitive skin and atopy by 10 female panels were examined. Furthermore, the effect on constipation by 30 female panels from the teens to the 40s using the drinking water to which the rose antioxidant substance of Example 8 is added, the female panel 30 from the teens to the 40s in Example 9 When we examined all the two items of effects on menstrual cycle by name, it was revealed that each has an effect.

Although the test example and the Example using the rose antioxidant substance which consists of the rose oil and rose water described above are shown below, this invention of this application is not restricted to an Example.

(Test example: Change in transition with temperature and pH value)
In order to investigate the antiseptic effect, lotion, moisturizing cream and drinking water to which rose antioxidants composed of rose oil and rose water of the present invention are added are changed over a period of about two months, and their pH value and temperature change. As shown in FIG. 1, FIG. 3, and FIG. 5, the stability of the pH value is high, and it is not only difficult to oxidize the rose oil and rose water itself, but also the antiseptic effect on the added one. It was revealed to bring about. In the formulation example of the moisturizing cream shown in Table 6, rose oil after fermentation, ripening, and purification exhibits an effect as a preservative with a composition of only 0.03%. This is comparable to the preservative effect of chemical compounds.

(Test example: Changes in pigment due to antioxidant effect using sicon extract)
In order to confirm the antioxidant action of the rose antioxidant substance of the present invention, a chicone extract is added as a natural colorant to a lotion and a moisturizing cream to which a rose antioxidant substance comprising rose oil and rose water is added, and a halogen lamp is added thereto. The tungsten wire was irradiated for about 48 hours, and the degree of change of the dye was examined. Formulation examples of the skin lotion and moisturizing cream are shown in Example 1 and Example 2. Sensory evaluation of whether the lotion and moisturizing cream pigments changed before and after irradiation was evaluated with 2 specialist panels and 3 general panels. Have gained.

(Test example: sensory evaluation of fragrance)
Comparing the sensory evaluation of the fragrance of rose oil and rose water before implementation of the technology of the present invention and the rose antioxidant obtained from the technology of the present invention between the two specialized panels and the three general panels As a result of evaluation, all of the five people evaluated that the scent of rose antioxidant substances consisting of rose oil and rose water after implementation of the technology of the present invention was “improved” compared to before implementation.

Measurement of the pH value of lotion made with 0.03% rose oil, 10% rose water, 1% xanthan gum, 0.1% chicory extract and 88.87% purified water. See FIG. 1 and FIG. In addition, the rose oil and rose water which are mentioned here represent the rose antioxidant substance obtained by this invention technique.

Made with 0.03% rose oil, 10% rose water, 5.77% beeswax, 41% jojoba oil, 41% olive oil, 0.1% sodium hyaluronate, 0.1% shikon extract, 2% silk extract Measurement of the pH value of the moisturizing cream. See FIG. 3 and FIG. In addition, the rose oil and rose water which are mentioned here represent the rose antioxidant substance obtained by this invention technique.

Measurement of the pH value of drinking water made using 25% rose water and 75% purified water. See FIG. 5 and FIG. In addition, the rose oil and rose water which are mentioned here represent the rose antioxidant substance obtained by this invention technique.

In order to confirm the presence or absence of the effect on stains and freckles, the skin lotion of the prescription example given in Example 1 and the moisturizing cream of the prescription example given in Example 2 were applied to a panel of 15 people in their teens to 40s. After 3 days of face washing in the morning and evening, when they were used in the order of lotion and moisturizing cream, the following responses were obtained. This is due to the antioxidant action of the rose antioxidant substance of the present invention due to the stain and adsorption to melanin pigments such as freckles and reduction.

In order to confirm the presence or absence of an effect on acne and pimples, the lotion of the prescription example given in Example 1 and the moisturizing cream of the prescription example given in Example 2 were applied to a panel of 15 females in their teens to 40s. After about 3 months of face washing in the morning and evening, the following answers were obtained when used in the order of lotion and moisturizing cream. This is because the rose antioxidant of the present invention penetrates and sterilizes acne bacteria that cause acne, adsorbs it to excess fat and oxidizes and reduces the skin balance, This is due to the normal return.

In order to confirm the presence or absence of the effect on pores and sagging, the skin lotion of the prescription example given in Example 1 and the moisturizing cream of the prescription example given in Example 2 were applied to a panel of 15 females in their teens to 40s. After about 3 months of face washing in the morning and evening, the following answers were obtained when used in the order of lotion and moisturizing cream. This is because the antioxidant substance of the present invention penetrates into pores and sagging to remove unwanted dirt with the power of adsorbing and reducing dark spots and waste products in the pores, and adjusting the skin balance to prevent pores and face. It can be said that there is also a work that attracts the whole slack.

In order to confirm the presence or absence of the effect on sensitive skin and atopy, the skin lotion of the prescription example given in Example 1 and the moisturizing cream of the prescription example given in Example 2 are applied to a panel of 10 people in their teens to 40s. After about 3 months of face washing in the morning and evening, the following answers were obtained when used in the order of lotion and moisturizing cream. The rose antioxidant substance of the present invention is effective for sensitive skin and symptoms such as atopy, is very gentle to the skin, and reports that the symptoms of atopy have been improved and alleviated have been cited.

In order to confirm the presence or absence of effects on menstrual irregularity and menstrual cycle stability, 100 ml of drinking water of the prescription example given in Example 3 was applied to a total of 30 female panels in their teens to 40s for about 3 months. 10ml of the above-mentioned drinking water was added to the water, and it was drunk three times in the morning and evening, and at the same time the basal body temperature chart was measured every morning and the effect was examined. . This is because the antioxidant substance of the present invention is adsorbed to the active oxygen in the body and oxidized and reduced to improve the circulation of blood and oxygen in the body, the biological clock works normally, and physiological stability and menstrual cycle stability are also improved. It can be said that there is an effect.

In order to confirm the presence or absence of the effect on the improvement of constipation, the drinking water of the prescription example given in Example 3 was applied to 100 ml of water for about three months on a panel of 30 women in their teens to 40s. When 10 ml of the above-mentioned drinking water was added and the drink was taken three times in the morning and evening, and at the same time, the basal body temperature chart was measured every morning and the effect was examined. The following answer was obtained. This is because of the effect of improving constipation brought about by the rose antioxidant of the present invention, by adsorbing and reducing the harmful substances such as gas and nitrogen compounds collected in the intestine to promote the bowel movement. It can be said that there is.

  Rose antioxidant with excellent safety obtained by fermenting, aging and refining substances extracted from rose flowers can be used in cosmetics, beverages, foods, pharmaceuticals, quasi drugs Acts as an antioxidant and preservative. In addition, since the aroma of roses is exhibited even in a small amount of fragrance, natural rose fragrances are emitted without using synthetic fragrances, and production of expensive natural rose products and quality improvements are expected. The potential for future wide-ranging industrial use can be expected.

Measurement graph of pH value of lotion to which rose antioxidant substance composed of rose oil and rose water is added (Example 1). Example 1 pH value of a skin lotion to which a rose antioxidant consisting of rose oil and rose water is added. A measurement graph of pH value of a moisturizing cream to which a rose antioxidant consisting of rose oil and rose water is added (Example 2). PH value of a moisturizing cream to which a rose antioxidant consisting of rose oil and rose water was added (Example 2). The measurement graph of the pH value of the drinking water which diluted the rose antioxidant substance which consists of rose water with purified water (Example 3). PH value of drinking water obtained by diluting rose antioxidant substance consisting of rose water with purified water (Example 3).

Claims (7)

  Rose antioxidant obtained from fermentation, ripening and purification using the newly discovered composition, Tannic acid and yeast, among the substances extracted from rose flowers.   The rose antioxidant substance according to claim 1, wherein the extracted substance is rose oil or rose water.   The antiseptic | preservative characterized by the rose antioxidant substance of Claim 1 or 2 being an active ingredient.   A fragrance comprising the rose antioxidant substance according to claim 1 or 2 as an active ingredient.   The cosmetic according to claim 1 or 2, comprising the rose antioxidant substance as an active ingredient.   The beverage according to claim 1 or 2, comprising the rose antioxidant substance as an active ingredient.   The food according to claim 1 or 2, comprising the rose antioxidant substance as an active ingredient.