CN112175733A - Method for preparing vanilla essential oil extract and cosmetic composition containing vanilla essential oil extract - Google Patents
Method for preparing vanilla essential oil extract and cosmetic composition containing vanilla essential oil extract Download PDFInfo
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- CN112175733A CN112175733A CN202010384982.4A CN202010384982A CN112175733A CN 112175733 A CN112175733 A CN 112175733A CN 202010384982 A CN202010384982 A CN 202010384982A CN 112175733 A CN112175733 A CN 112175733A
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- essential oil
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- oil extract
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
Abstract
The present invention relates to a method for manufacturing a vanilla essential oil extract and a cosmetic composition including the vanilla essential oil extract, and more particularly, to a method for manufacturing a vanilla essential oil extract having excellent pharmacological activity and significantly improved skin stability and a cosmetic composition including the vanilla essential oil extract manufactured by the method thereof. To this end, a method for producing an extract of vanilla essential oil is characterized by comprising: a first step of mixing vanilla essential oil and powdered adsorbent and adsorbing the vanilla essential oil to the powdered adsorbent; a second step of adding a solvent to the vanilla extract adsorbed on the powdered adsorbent and mixing the resulting mixture to produce a vanilla extract mixture; and a third step of filtering the vanilla oil mixture to obtain vanilla oil extract.
Description
Cross Reference to Related Applications
This application claims priority and benefit from korean patent application No.10-2019-0079260, filed on year 07, 02, 2019, which is incorporated herein by reference for all purposes as if fully set forth herein.
Technical Field
The present invention relates to a method for manufacturing a vanilla essential oil extract and a cosmetic composition including the vanilla essential oil extract, and more particularly, to a method for manufacturing a vanilla essential oil extract having excellent pharmacological activity and significantly improved skin stability and a cosmetic composition including the vanilla essential oil extract manufactured by the method thereof.
Background
Medicinal plants, including vanilla plants, have long been used for therapeutic purposes due to their high pharmacological activity and weak toxicity. This physiological activity is based on a class of phenolic compounds called phytochemicals (phytochemicals) or alkaloids (David o. kennedy, Advanced in nutrition, 2011). Generally, essential oils obtained by performing soxhlet extraction, squeeze extraction, cold-dip extraction, warm-dip extraction, or supercritical extraction processes on aromatic vanilla plants using an organic solvent are the main means of aromatherapy (korean laid-open patent No. 0038962, korean registered patent No. 1437221). Essential oils, which have been widely used as preservatives in the process of making mummy in ancient egypt, are used in various ways with the unique effects of various plants as substances capable of providing a cure to humans, and are particularly widely used for various infectious diseases including skin diseases. These essential oils are known to have pharmacological functions due to aromatic volatile components and eugenol and phenylpropanoid, lignan, ephedrine, caffeine, indole, aminobutyric acid (GABA), curcumin, coumarin and terpene components in addition to the essential oil components.
Currently, the fragrance and components of essential oils are also used in the field of skin management to improve the skin condition, and studies on essential oils having antibacterial and antioxidant effects are conducted to use essential oils for problematic skin management. In particular, majorana has been reported to have three times or more antibacterial effects against Staphylococcus aureus (Staphylococcus aureus) compared with the same concentration of phenol, and thyme, cinnamon bark, oregano, and the like have been reported to have extremely high antibacterial effects (j.v. loveti, j.chem. ecol., 1989). Further, it has been reported that essential oils have antioxidant effects because mice coated with lavender generate less active oxygen after UVB irradiation and are rapidly eliminated by active oxygen detoxification enzymes (r.h. whitemarker, Science, 1971).
However, it has been reported that essential oils having high antibacterial power also include components that may irritate the skin among the essential oil components. In the case of cinnamon bark oil, it has been reported that cinnamaldehyde (cinnamyl aldehyde) which accounts for 50% or more of the total composition of essential oil components has a strong antibacterial activity, but may cause irritation to the skin and cause allergic reactions.
Also, thymol (thymol) and carvacrol (carvacrol) components included in essential oil components of thyme and oregano are classified as causing irritation to skin and mucous membrane in spite of their potent antibacterial properties, and thus are recommended to be used at low concentrations (kangargin, korean forestry energy council, 1999).
Also, it is difficult to extract such plant nutrient components from essential oils due to low solubility and low content. Therefore, a method of improving the solubility of a medicinal ingredient using an organic solvent, a method of producing the medicinal ingredient in the form of an ionized salt, a method of adjusting pH, a technical method of solubilizing a poorly soluble component using a molecular transporter such as a liposome, a microemulsion, or cyclodextrin, and the like have been disclosed (korean registered patent No. 1495036, korean registered patent No. 1897147). However, these techniques change the physical and chemical properties of the pharmaceutical ingredient or exhibit selective solubilization phenomena, and, due to structural limitations, active ingredients cannot be obtained in a form that is easily formulated.
As described above, there is a further need to develop a novel extraction method that reduces skin allergy toxicity of vanilla plants, is safe because it does not irritate the skin, and can produce an extract in a form that is easy to formulate.
[ Prior art documents ]
[ patent document ]
(patent document 0001) Korean registered patent publication No. 10-1495036
(patent document 0002) Korean registered patent publication No. 10-1897147
Disclosure of Invention
The present invention has been made to solve the above-mentioned problems, and an object of the present invention is to provide a method for producing a vanilla essential oil extract having excellent pharmacological activity and extremely improved skin stability, and a cosmetic composition comprising the vanilla essential oil extract produced by the method.
These and other objects and advantages of the present invention will become apparent from the following description describing preferred embodiments.
Said object is achieved by a method for the manufacture of an extract of essential oil of vanilla, comprising: a first step in which vanilla essential oil and a powdered adsorbent are mixed to adsorb the vanilla essential oil to the powdered adsorbent; a second step of adding a solvent to the vanilla essential oil adsorbed on the powdered adsorbent and mixing to produce a vanilla oil mixture; and a third step, wherein the vanilla essential oil extract is obtained by filtering the vanilla essential oil mixture.
The vanilla essential oil in the first step may be at least one essential oil selected from the group consisting of lemon grass, thyme, lemon, orange, lime, bergamot, sage, rosemary, parsley, mugwort, dandelion, ginseng, mint, lavender, daisy, calendula, garlic, dill, ginkgo biloba, primula, rose, elderberry, cypress, chamomile, grapefruit, eucalyptus, and peppermint.
The powder adsorbent in the first step may be at least one selected from talc, sericite, cyclodextrin and silica.
The solvent in the second step may be at least one selected from purified water, ethanol, glycerol, propylene glycol, dipropylene glycol, butylene glycol, and pentylene glycol.
The vanilla oil mixture in the second step may include vanilla essential oil 1.0 wt% to 90.0 wt%, powdered adsorbent 0.1 wt% to 50.0 wt%, and solvent 0.01 wt% to 90.0 wt%, relative to the total 100 wt%.
And, the object is achieved using a cosmetic composition comprising the vanilla essential oil extract manufactured by the method as an effective ingredient.
The vanilla essential oil extract may be included in an amount of 0.1% to 30% by weight, relative to the total 100% by weight of the cosmetic composition.
The cosmetic composition may be in the form of at least one of a solubilized product, an emulsified product, and a dispersed product.
Drawings
Fig. 1 is a view schematically illustrating a method of manufacturing a vanilla essential oil extract according to one embodiment of the present invention.
Fig. 2 is a graph illustrating the results of high performance liquid chromatography of example 1 and comparative example 1.
Detailed Description
The present invention is described in detail below with reference to embodiments of the present invention and the accompanying drawings. It will be apparent to those skilled in the art that these embodiments are merely exemplary for more specific description of the invention, and that the scope of the disclosure is not limited to these embodiments.
Also, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and in case of conflict, the descriptions in this specification, including definitions, are to be given priority.
In the drawings, portions irrelevant to the description are omitted to clearly explain the proposed invention, and like reference numerals are used for like portions throughout the specification. Also, when a portion "includes" an element, unless otherwise stated to the contrary, it means that other elements may be further included without excluding other elements. Also, "section" described in the specification means one unit or block for performing a specific function.
In the steps, identification symbols (first, second, etc.) are used only for convenience of description and do not describe the order of the steps, and the steps may be performed in an order different from the described order unless a specific order is explicitly described in the context. In other words, the steps may be performed in the same order as described, may be performed substantially simultaneously with the described order, or may be performed in the reverse order of the described order.
Fig. 1 is a view schematically illustrating a method of manufacturing a vanilla essential oil extract according to one embodiment of the present invention. Referring to fig. 1, a method for manufacturing an extract of vanilla extract according to an embodiment of the present invention includes: a first step of mixing vanilla essential oil and powdered adsorbent to make vanilla essential oil adsorbed on the powdered adsorbent; a second step of adding a solvent to the vanilla essential oil adsorbed on the powdery adsorbent and mixing the resulting mixture to produce a vanilla oil mixture; and a third step of filtering the vanilla oil mixture to obtain vanilla oil extract. Here, the essential oil refers to natural plant oil extracted from aromatic medicinal plants and having inherent fragrance and healing effects of sterilization, sedation, relaxation, etc. at high concentration, and the vanilla essential oil refers to essential oil extracted from vanilla plants.
The present invention can efficiently extract aromatic volatile components and water-insoluble plant nutrient components having pharmacological activity from vanilla extract without using the conventional general extraction method (organic solvent and physical methods such as heating, pressurizing, ultrasonic treatment) and using the continuous partition phenomenon between the powder adsorbent of the stationary phase and the extraction solvent of the mobile phase, thereby making it possible to produce vanilla extract having excellent pharmacological activity and significantly improved skin stability. Further, the extracted components have the effect of being stably dispersed in the extract and being used in cosmetic compositions of various uses and formulations.
Generally, essential oils, which are used as main properties for directional treatment, can be obtained from aromatic vanilla plants by means of organic solvents through the processes of soxhlet extraction, squeeze extraction, cold-dip extraction, warm-dip extraction or supercritical extraction. However, when the vanilla essential oil itself is simply used as it is, although some of the softening action is exhibited outside the living body, there are problems that the effect is not satisfactory in nature and toxic allergy to the skin is caused when the essential oil is applied to a skin external preparation. Further, the vanilla essential oil has a problem that essential oil components such as limonene, terpene, camphor, phenyl ethanol are not easily used as cosmetics, and has a disadvantage that unsaturated components such as oleic acid are easily oxidized or deteriorated to make it difficult to obtain stable cosmetics. In order to solve the problems as described above, the present invention manufactures the vanilla essential oil extract using a continuous partition process after mixing a powder adsorbent of a stationary phase and an extraction solvent of a mobile phase, thereby having not only excellent pharmacological effects but also effects for use in various cosmetic compositions as external skin preparations.
The first step is a step of mixing vanilla essential oil and powdered adsorbent to make vanilla essential oil adsorbed on the powdered adsorbent, and first, vanilla essential oil is mixed with powdered adsorbent of stationary phase and adsorbed. At this time, at least one selected from lemongrass, murraya paniculata, lemon, orange, lime, bergamot, sage, rosemary, parsley, mugwort, dandelion, basil, ginseng, mint, lavender, daisy, calendula, garlic, dill, ginkgo tree, primrose, rose, elderberry, cypress, chamomile, grapefruit, eucalyptus, and peppermint may be used as the vanilla essential oil. Also, at least one selected from talc, sericite, cyclodextrin and silica may be used as the powder adsorbent (powdered adsorbent), but is not limited thereto.
The second step is a step of adding vanilla extract oil adsorbed on the powder adsorbent to dissolve and mix to manufacture vanilla extract oil mixture, namely a step of adding vanilla extract oil adsorbed on the stationary phase powder adsorbent to extraction solvents of various polarities of the mobile phase to mix. At this time, the extraction solvent may be at least one selected from the group consisting of purified water, ethanol, glycerol, propylene glycol, dipropylene glycol, butylene glycol, and pentylene glycol, but is not limited thereto.
The vanilla essential oil extract can be effectively obtained only by mixing vanilla essential oil, powdered adsorbent and solvent in appropriate amounts, preferably including 1.0% to 90.0% by weight vanilla essential oil, 0.1% to 50.0% by weight powdered adsorbent, and 0.01% to 90.0% by weight solvent, based on 100% by weight total. Also, purified water may be used to adjust the equilibrium, and the solvent may include purified water.
The third step is a step of obtaining a vanilla essential oil extract by filtering the vanilla oil mixture, and although there is no particular limitation on the extraction conditions, it is preferably extracted under conditions of a temperature of room temperature and a number of revolutions of 20rpm to 180rpm for 1 hour to 24 hours.
The vanilla essential oil manufactured by the above-described method may be included as an effective ingredient in a cosmetic composition. The inclusion as the active ingredient means not only that the vanilla extract is added to the composition to exhibit an effect of improving the skin condition when the user uses the cosmetic composition, but also that various other ingredients are added as sub-ingredients for ingredient transfer and stabilization to make various forms. At this time, the vanilla essential oil is preferably included at 0.1% by weight to 30% by weight, relative to the total 100% by weight of the cosmetic composition. When the amount is less than 0.01 wt%, the skin-improving effect is insignificant, and when the amount is more than 30 wt%, the efficiency of the amount of raw materials to be charged is low, which is uneconomical.
The cosmetic composition can be made into various dosage forms, and can be made into at least one of soluble product, emulsified product and dispersed product. The solubilized product is a product in which a small amount of oil component is transparently dissolved in water by a surfactant, the emulsified product is a product in which the oil component is opalescent by the surfactant, and the dispersed product is a product in which fine solid particles are uniformly mixed with water or oil component by the surfactant. Specifically, the formulation may be a cosmetic water, a gel, a water-soluble solution, a cream, an essence, a base cosmetic formulation formed into an oil-in-water (O/W) type or a water-in-oil (W/O) type, a barrier cream of an oil-in-water type or a water-in-oil type, a foundation, a sunscreening cream, a lipstick, a lip gloss, a face powder, a dual use powder cake, an eye shadow, a blush, an eyebrow pencil, or the like.
Hereinafter, the composition of the present disclosure and the effects thereof will be described in more detail by specific examples and comparative examples. However, this embodiment is used to more specifically describe the present disclosure, and the scope of the present disclosure is not limited to these embodiments.
[ examples 1-2]
Vanilla extract was produced by adsorbing lemon grass essential oil on talc as a stationary phase powder adsorbent and then extracting at 50rpm for 1 hour at room temperature using butylene glycol as an extraction solvent (total 100g) (see example 1, table 1). Example 2 (refer to table 2) was prepared by the same method as example 1, except that thyme essential oil was used instead of lemon grass essential oil.
[ Table 1]
[ Table 2]
Comparative examples 1 to 6
Comparative examples 1 and 4 were prepared according to the contents of tables 1 and 2, and extracts were prepared by a general temperature-rising extraction method in which dried leaves of lemon grass and thyme were finely cut and butylene glycol was used as an extraction solvent. Comparative examples 2 and 5 were set as the essential oil itself without the extraction process. Comparative examples 3 and 6 were manufactured according to the contents of said tables 1 and 2, however, comparative examples 3 and 6 were manufactured without using a general temperature-rising extraction method, by mixing butanediol and essential oil at 50rpm for 1 hour, adding purified water, and separately filtering only a purified water layer.
[ examples 3 to 5]
The production was carried out in the same manner as in example 1 except that the content of talc powder used as the powder adsorbent was changed (see table 3).
[ Table 3]
[ examples 6 to 8]
The production was carried out in the same manner as in example 1 except that the content of butanediol in the mobile phase was changed (see Table 4).
[ Table 4]
[ examples 9 to 11]
The same production as in example 1 was carried out except that the kind of the extraction solvent was changed (refer to table 5) to observe the extraction characteristics as the distribution coefficient of the extraction solvent of the mobile phase changes (solubility difference to essential oil).
[ Table 5]
[ example 12]
A cosmetic composition containing example 1 was produced (see table 6). Specifically, the water-soluble components shown in Table 6 were heated and stored at 70 ℃ and the oil-soluble components were added to the mixture to pre-emulsify the mixture, followed by uniformly emulsifying the mixture with a high-speed mixer. Then, after slowly cooling, the mixture was uniformly mixed with the extract of lemon grass essential oil of example 1 to prepare a cream (example 12) formulation.
[ Table 6]
Comparative example 7
The preparation was carried out by the same method as example 10 except that the extract of lemongrass essential oil of example 1 was not added (said table 6).
[ Experimental example 1: measuring changes in the plant nutrient components contained in the extract ]
The qualitative analysis and state comparison of the changes in the production of pharmacologically active ingredients in the extracts of lemongrass essential oil of example 1 and comparative example 1 (temperature-increasing solvent extraction method) were performed by high performance liquid chromatography, and the results are shown in fig. 2. Analysis was performed using a 2695 system from Water as HPLC, Sunfire C18(5 μm,4.6 × 250mm) as column, and Waters 996 diode array detector as detector, under the following analysis conditions: the solvent composition was 2% from Acetonitrile (Acetonitrile) and H2The proportion of O98% starts at 30 minutes to 100% acetonitrile, the analysis time is 40 minutes, the elution quantity is 0.8ml/min and is measured according to gradient conditions.
From fig. 2 in which the production change of the pharmacologically active ingredient in the extract was measured, it was confirmed that the increase in the production and the change in the distribution of the specific ingredient in the region of about 24min were observed in the sample of example 1 as compared with those in comparative example 1.
From the results, it was confirmed that example 1 using the adsorbent and the extraction solvent can change the phytonutrient components that cause pharmacological effects in the skin.
[ Experimental example 2: free radical scavenging rate measurement experiment
In order to measure the radical scavenging rate of the samples obtained from examples and comparative examples, an extract having excellent antioxidant activity, such as green tea extract, was used as a comparative sample under laboratory conditions and the radical scavenging activity was measured using the DPPH method.
The radical scavenging rate due to reducing power is measured in the DPPH method using a radical called a diphenylpicrylhydrazino radical (DPPH; 2,2-Di (4-tert-octylphenyl) -1-piperidinylhydrazyl free chemical). The degree of decrease in absorbance due to reduction of the test substance DPPH was compared with the absorbance of the blank test solution, and the radical clearance was measured at a wavelength of 560 nm.
In order to measure the DPPH radical scavenging rate, samples of examples (1 to 11) and comparative examples (4 to 6) were prepared at concentrations of 0.2%, 0.1%, 0.05%, and 0.005%. The extracts at the concentrations were put into 96-well plates, respectively, and DPPH prepared with 100uM methanol solution was added thereto to make the total volume of the solution 200. mu.l. This was left at 37 ℃ for 30 minutes and then the absorbance was measured at 560 nm.
[ mathematical formula 1]
Radical clearance (%) {100- (B/a) } x100
A: absorbance of control wells not treated with the sample of the present invention
B: absorbance of test set well for processing sample of the present invention
Measurement of radical scavenging Rate according to extraction method
The antioxidant activities of example 1 (lemongrass essential oil extract) and example 2 (thyme essential oil extract) and comparative examples 1 to 6 extracted by different extraction methods are shown in table 7. Examples 1 and 2 using the extraction method according to an embodiment of the present invention show results that the antioxidant activity is similar to or slightly lower than that of green tea extract as a control group. However, comparative examples 1, 2, 4 and 5 using only essential oil or vanilla leaves using a conventional extraction method showed lower antioxidant effect compared to examples, and the essential oil extracts of comparative examples 3 and 6 excluding the adsorbent showed slight antioxidant activity.
[ Table 7]
Measurement of radical scavenging according to degree of adsorption
The antioxidant activities of the essential oil extracts of lemongrass of examples 1 and 3 to 5, which varied according to the content of talc as a powder adsorbent, were compared, and the results thereof are shown in table 8 below. As can be seen from table 8, examples 1 and 4 are the most excellent in antioxidant activity, and example 5, which has the highest talc content, is inferior in antioxidant activity. It can be seen that the extraction efficiency varies depending on the talc content.
[ Table 8]
| Name of sample | Antioxidant Effect (%) |
| Example 1 (12.0% by weight of talc) | 91 |
| Example 3 (Talc powder 3.0 wt%) | 55 |
| Example 4 (Talc powder 6.0 wt%) | 90 |
| Example 6 (talc powder 24.0 wt%) | 80 |
| Green tea extract 0.1 wt% | 92 |
Measurement of radical scavenging Rate according to extraction solvent content
The antioxidant activities of the essential oil extracts of lemongrass of examples 1 and 6 to 8, which varied according to the content of the extraction solvent of the mobile phase, were compared, and the results thereof are shown in table 9. As can be seen from table 9, example 1 using 15.0 wt% of butanediol is the most excellent in antioxidant activity, and the antioxidant effect on the use amount is not significantly increased at the content above.
[ Table 9]
| Name of sample | Antioxidant Effect (%) |
| Example 1 (butanediol 15.0 wt%) | 90 |
| Example 3 (butanediol 0.0 wt%) | 35 |
| Example 4 (butanediol 7.5 wt%) | 58 |
| Example 6 (butanediol 30.0 wt%) | 95 |
| Green tea extract 0.1 wt% | 92 |
Measurement of radical scavenging Rate according to extraction solvent class
The antioxidant activities of the lemongrass essential oil extracts of examples 1 and 9 to 11 according to the kinds of extraction solvents were compared, and the results thereof are shown in table 10. As can be seen from table 10, examples 1 and 9, in which butanediol and ethanol were used as extraction solvents, were the most excellent in antioxidant activity.
[ Table 10]
Example 3: evaluation of cytotoxicity)
Cytotoxicity on skin cells was evaluated for example 1 (lemongrass essential oil extract) and comparative example 2 (lemongrass essential oil). Each well in a 96 well assay plate was plunged with 1X105cells/mL fibroblasts (fibroplast) diluted with cell culture medium (10% FBS in DMEM) and attached for 24 hours. The sample obtained in example 1 was diluted to an appropriate concentration, treated in each well, and then cultured for 24 hours. After 24 hours, the medium was removed, 200. mu.l of a cell culture medium containing a solution of tetramethyltetrazolium blue (MTT; 3- (4, 5-dimethyltetrazol-2 yl) -2, 5-dipehnyltetrazolium bromide) (2.5mg/ml) was put into each well, and then cultured in a CO2 incubator at 37 ℃ for two hours. The medium was removed and 100. mu.l of dimethyl sulfoxide (DMSO) was added thereto. After shaking for 5 minutes to lyse the cells, the absorbance at 565nm was measured on a microplate analyzer. The cell viability (%) was determined as shown in the following equation 2, and the concentration of the agent that did not affect cell survival was determined. The results are shown in table 11 below.
[ mathematical formula 2]
Cell survival rate (%) { (St-Bo)/(Bt-Bo) } x100
And (4) Bo: 565nm absorbance for wells that only underwent chromogenic reaction on cell culture Medium
Bt 565nm absorbance of a well in which a color development reaction was carried out without treating a sample
St: 565nm absorbance of a well for treating a sample and performing a color development reaction
[ Table 11]
| Name of sample | 100% cell viability |
| Example 1(0.1 wt%) | 2.0％ |
| Comparative example 2(0.1 wt%) | 0.2％ |
As can be seen from table 11, the extract of lemongrass essential oil in example 1 showed a cell viability of 100% at a concentration of 2.0 wt%, and was a safe sample with a low possibility of causing skin irritation when considering the concentration generally used in cosmetics. However, the lemongrass essential oil of comparative example 2 showed a cell survival rate of 100% at a concentration of 0.2 wt% or less, showed 10-fold or more higher cytotoxicity than the extract of example 1, and thus was judged to have a high possibility of inducing skin irritation. In other words, it is known that the extract to which the essential oil extract production method according to an embodiment of the present disclosure is applied can significantly reduce the possibility of skin irritation as compared to when used as an essential oil.
[ Experimental example 4: evaluation of efficacy of cosmetic application
Confirmation of skin elasticity improving Effect
Comparative experiments were performed on the cosmetics of the extract of lemongrass essential oil obtained in example 1 (example 12) and comparative example 7 to evaluate the skin elasticity improvement effect on human subjects.
The cream of example 12 and the cream of comparative example 7 were applied to 20 subjects (ages of 20 to 30 years) twice a day on the right side of the face and on the left side of the face during two consecutive months.
After the end of the experiment, the skin elasticity improvement effect was measured with a skin elasticity measuring instrument (cutometer SEM 575, C + K Electronic co., Germany (Germany)) before the product was used and after two months of use. The experimental results are reported in table 12 below as Δ R7 values for the Cutometer SEM 575. The R7 value refers to the viscoelasticity (viscoelasticity) of the skin. As shown in table 12, it was found that the skin elasticity improvement effect was excellent in the subjects who applied the cream containing the lemongrass essential oil extract.
[ Table 12]
| Experimental products | Skin elasticity effect (Delta R7) |
| Example 12 | 0.38 |
| Comparative example 7 | 0.11 |
n＝20,p<0.05
Confirming the skin wrinkle-improving effect
Comparative experiments were performed on the cosmetic containing the extract of lemongrass essential oil obtained in example 1 (example 12) and comparative example 7 to evaluate the skin wrinkle improvement effect on human subjects.
The cream of example 12 and the cream of comparative example 7 were applied to 20 subjects (ages of 20 to 30 years) twice a day on the right side of the face and on the left side of the face during two consecutive months.
After the experiment was completed, in order to confirm the wrinkle-improving effect of the skin before and after two months of use of the product, a silicon replica (replica) was produced, and the wrinkle state at a specified site was measured with a visibility meter (visiometer: SV60, C + K Electronic Co., Germany) as an image analyzer. The results are shown in table 13 below. The result represents the average of the results obtained by subtracting the parameter values two months before from the respective parameter values two months after. In other words, a negative value indicates a high wrinkle-improving effect. As can be seen from table 13, it was confirmed that the skin wrinkle-improving effect of example 12 containing the lemongrass essential oil extract of example 1 was greatly improved.
[ Table 13]
Confirmation of skin whitening Effect
Comparative experiments were performed on the cosmetics containing the lemongrass essential oil extract obtained in example 1 (example 12) and comparative example 7 to evaluate the skin whitening effect on human subjects.
The cream of example 12 and the cream of comparative example 7 were applied to 20 subjects (ages of 20 to 30 years) twice a day on the right side of the face and on the left side of the face during two consecutive months. After the experiment was completed, the change (L) in the brightness of the color was measured on the skin of the applied part on both left and right sides of the face by an image analyzer and a colorimeter (Minolta CR300), and the effect was classified and measured according to the following scale by objective visual observation by a plurality of experts and subjective visual observation by the subject. The results are shown in table 14 below. At this time, the whitening efficacy degree was evaluated by classifying into the following seven grades.
[ Standard for evaluation of whitening efficacy ]
-3: extreme deterioration
-2: deterioration of
-1: slight deterioration of
0: has no change
1: slightly improved
2: improvements in or relating to
3: is extremely improved
As shown in table 14, it was found that the whitening effect on the facial skin of the subjects to whom the cream containing the lemongrass essential oil extract was applied was excellent.
[ Table 14]
It is known that the vanilla extract, which is extracted by using a powdery adsorbent such as talc as a stationary phase and purified water and butanediol as an extraction solvent, exhibits an antioxidant effect, an effect of removing intracellular active oxygen, an effect of inhibiting the activity of tyrosine enzyme, a whitening effect, an effect of alleviating cytotoxicity due to ultraviolet irradiation, and an inhibitory effect on the expression of inflammatory cytokines due to ultraviolet irradiation, through the above-mentioned various tests.
Further, it was confirmed that the extract has an excellent antioxidant activity effect without causing skin allergy irritation as compared with conventional essential oils, and also has a solubilizing ability to stably disperse a plant nutrient component or an alkaloid component including a water-insoluble short chain fatty acid (short chain fatty acid) showing a pharmacological effect in the skin in the extract. Therefore, the vanilla extract can be suitably used for producing cosmetic compositions such as lotions, creams, lotions, masks, powders and the like, which can exhibit excellent effects of external skin preparations such as skin anti-aging effects, whitening effects, weakening effects on skin irritation and the like.
According to the present invention, aromatic volatile components and water-insoluble plant nutrient components having pharmacological activity can be efficiently extracted from vanilla essential oil, whereby vanilla essential oil extract having excellent pharmacological activity and significantly improved skin stability can be produced.
Also, it can solve the problems of skin allergy toxicity and general usability of the existing vanilla essential oil, has excellent physiological activity, and solves environmental problems by minimizing the use of chemical organic solvents in the extraction process.
Further, the extracted components have the effect of being stably dispersed in the extract and being used in cosmetic compositions of various uses and formulations.
However, the effects of the present invention are not limited to the effects mentioned above, and other effects not mentioned should be clearly understood by those of ordinary skill in the art based on the description below.
In the present specification, only a few examples of various embodiments performed by the present inventors have been described, however, the technical idea of the present disclosure is not limited thereto, and may be modified and implemented in various forms by those of ordinary skill in the art.
Claims (8)
1. A method for preparing vanilla essential oil extract comprises:
a first step in which vanilla essential oil and a powdered adsorbent are mixed to adsorb the vanilla essential oil to the powdered adsorbent;
a second step of adding a solvent to the vanilla essential oil adsorbed on the powdered adsorbent and mixing to produce a vanilla oil mixture; and
a third step, wherein the vanilla oil mixture is filtered to obtain vanilla oil extract.
2. The method for manufacturing a vanilla essential oil extract according to claim 1, characterized in that the vanilla essential oil in the first step is vanilla essential oil
At least one essential oil selected from lemongrass, thyme, lemon, orange, lime, bergamot, sage, rosemary, parsley, mugwort, dandelion, basil, ginseng, mint, lavender, daisy, calendula, garlic, dill, ginkgo tree, primrose, rose, elderberry, cypress, chamomile, grapefruit, eucalyptus, and peppermint.
3. The method of claim 1, wherein the powdered adsorbent in the first step is at least one selected from the group consisting of talc, silk, cyclodextrin and silica.
4. The method for producing a vanilla essential oil extract according to claim 1, wherein the solvent in the second step is at least one selected from the group consisting of purified water, ethanol, glycerin, propylene glycol, dipropylene glycol, butylene glycol and pentylene glycol.
5. The method for producing a vanilla essential oil extract according to claim 1, wherein the vanilla essential oil mixture in the second step,
comprises 1.0 to 90.0% by weight of vanilla extract, 0.1 to 50.0% by weight of powdered adsorbent and 0.01 to 90.0% by weight of solvent, relative to the total 100% by weight.
6. A cosmetic composition characterized by comprising, as an active ingredient, a vanilla essential oil extract produced by the process of at least one of claims 1 to 5.
7. The cosmetic composition of claim 6,
comprises from 0.1% to 30% by weight of vanilla essential oil extract, relative to the total 100% by weight of the cosmetic composition.
8. The cosmetic composition according to claim 6, wherein the formulation is at least one of a solubilized product, an emulsified product and a dispersed product.
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| KR102217697B1 (en) * | 2020-10-30 | 2021-02-22 | 바이오닉랩 주식회사 | Aromatherapy composition comprising natural aroma oil |
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| KR101405160B1 (en) * | 2011-10-07 | 2014-06-12 | 김주태 | Method for producing cosmetic beauty water comprising soluble silicate salt and cinnamomum camphora oil |
| KR20130128647A (en) * | 2012-05-17 | 2013-11-27 | 임상덕 | Functional shampoo |
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