KR20130076465A - Method for production of cosmetic composition containing the powder of captured siegesbcekia glabrescens makin - Google Patents
Method for production of cosmetic composition containing the powder of captured siegesbcekia glabrescens makin Download PDFInfo
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- KR20130076465A KR20130076465A KR1020110145061A KR20110145061A KR20130076465A KR 20130076465 A KR20130076465 A KR 20130076465A KR 1020110145061 A KR1020110145061 A KR 1020110145061A KR 20110145061 A KR20110145061 A KR 20110145061A KR 20130076465 A KR20130076465 A KR 20130076465A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
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- 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
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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Abstract
The present invention (A) using carbon dioxide as the supercritical fluid, obtaining a rare supercritical fluid extract under the pressure of 200 ~ 500bar, extraction temperature 40 ~ 60 ℃ conditions; (B) mixing the rare supercritical fluid extract with betacyclodextrin to prepare an inclusion complex; (C) spray-drying the inclusion complex to produce rare inclusion powder; And (D) adding the rare inclusion powder to a water-soluble cosmetic base.
Description
The present invention relates to a cosmetic composition, and more particularly, to a method for producing a cosmetic composition comprising a rare clath inclusion powder obtained by supercritical fluid extraction method containing beta cyclodextrin as a natural preservative.
Antiseptic means a drug that prevents the decay of a substance, that is, to prevent the decay of animals and plants by the action of microorganisms, and preservatives are defined as a drug added for preservation for the purpose of preservation. Generally, preservatives are added to prevent the deterioration of food, cosmetics, wood, pharmaceuticals, etc. and to maintain their purity while using or preserving them. Therefore, it is essential that preservatives are harmless to the human body and that the addition should not impair the quality (Narmandakh Jugee et al. 3, A Study of the Patch Test Results with Preservative Antigens for Patients with Suspected Cosmetic Contact Dermatitis, Korean Journal of Dermatology 2010; 48 (2): 109-114).
As a conventional cosmetic preservative, chemical preservatives have been mainly used, and among them, paraben is known as a chemical preservative. Recently, a problem has been raised that parabens may accumulate in the skin, and it is also known to cause breast cancer. As such, many problems regarding human stability have been raised with respect to chemical preservatives. Therefore, research on natural preservatives obtained from natural products in consideration of human safety aspects is urgently required.
Siegesbeckia glabrescens Makino is distributed in Korea, Japan, Taiwan, and China, and is a perennial herb of Asteraceae that grows near fields or fields. Young leaves, the main raw material of the Food & Drug Administration's raw material classification, are listed as edible raw materials, and outposts are widely used for medicinal purposes. Rupture mainly inhibits swelling of joints and lowers blood pressure in animals. In addition, it can be used in combination with donkeys for dysentic arthritis, and its efficacy against jaundice hepatitis has also been confirmed. In addition, civilian juice is used to detoxify poisonous snakes and insects, and it is also effective for treating paralysis and paraplegia.
The main components of the rare extracts are orientalide, pubetalin, darutin, darutoside, and campesterol. Enzyme inhibitory activity of protein tyrosine phosphatase 1B (PTP1B) of terpenes has been reported to confirm the therapeutic potential of diseases such as obesity and diabetes (Kim S. et al., J. Enzyme inhib. Med. Chem. 2006 , 21 (4); 379-383.), MCF-7, MDA-MB-231, human-derived breast cancer cells, induced cell death (Jun SY. Et al., Oncol Rep., 2006, 15 (6)). 1461-1467).
On the other hand, the main components of the rare are a lot of components having hydrophobic properties, when extraction using water as a solvent, extraction of the potent component does not occur smoothly, or precipitation occurs largely. As an alternative, ethanol or an ethanol-containing aqueous solution is widely used as a solvent, but there is an increase in manufacturing cost and tariff. In addition, there is a problem that the inclusion of the cyclodextrin is difficult to dissolve during low solubility and powdering process. Therefore, when a rare extract having a hydrophobic characteristic is added to the water-soluble cosmetic formulation, there is a problem that the solubility is not effectively completed the formulation.
An object of the present invention is to provide a method for producing a cosmetic composition containing a natural preservative harmless to the human body in order to solve the problems of the prior art.
In addition, an object of the present invention is to provide a method of increasing the solubility of the rare extract while increasing the extraction efficiency of the hydrophobic component when adding the rare extract to the water-soluble cosmetic formulation.
It is also an object of the present invention to provide extraction conditions of rare extract having properties suitable for use in cosmetic formulations.
In order to achieve the above object, the present invention (A) using carbon dioxide as a supercritical fluid, obtaining a rare supercritical fluid extract under the pressure of 200 ~ 500bar, extraction temperature 40 ~ 60 ℃ conditions; (B) mixing the rare supercritical fluid extract with betacyclodextrin to prepare an inclusion complex; (C) spray-drying the inclusion complex to produce rare inclusion powder; And (D) adding the rare inclusion powder to a water-soluble cosmetic base.
In addition, the present invention provides a method for producing a cosmetic composition, characterized in that to obtain a rare supercritical fluid extract under the conditions of the pressure 200 bar, extraction temperature 60 ℃ in the step (A).
In addition, the present invention provides a method for producing a cosmetic composition, characterized in that the inclusion ratio of betacyclodextrin: rare in step (B) is 100: 3 ~ 100: 6.
The present invention also provides a method for producing a cosmetic composition, wherein the rare inclusion powder is an off-white powder.
The present invention also provides a method for producing a cosmetic composition, characterized in that the rare inclusion powder is used as a natural preservative.
Hereinafter, a method for preparing a cosmetic composition containing a natural preservative using the rare extract of the present invention will be described in detail for each step.
(A) obtaining a rare supercritical fluid extract
This step is to obtain a rare supercritical fluid extract using the supercritical fluid extraction method.
Supercritical fluid extraction is an extraction method that combines the principles of solvent extraction and distillation. Its advantages include high dissolving power, rapid mass transfer and heat transfer, low viscosity, and rapid penetration into micropores due to high diffusion coefficients. There is this. In addition, since supercritical fluid extraction can be set under conditions of high density by manipulating pressure and temperature, it is possible to obtain high purity natural active ingredients with excellent selectivity, such as fractionation and separation. Since the solubility and density change with the change of pressure, the activity of the extract may also vary. In addition, since it is extracted at a relatively low temperature, there is an advantage that can prevent the loss of the natural active ingredient by heat.
In the present invention, carbon dioxide is preferably used as a supercritical fluid, and the rare water is extracted under conditions of a pressure of 200 to 500 bar and an extraction temperature of 40 to 60 ° C. Preferably flowing carbon dioxide gas at a flow rate of 55 ~ 58g / min under a pressure of 200bar, extraction temperature 60 ℃ to obtain a rare supercritical fluid extract. When the above conditions are satisfied, chlorophyll is hardly eluted to obtain a rare supercritical fluid extract having a pale off-white appearance.
In addition, when the above conditions are satisfied, the rare supercritical fluid extract can be obtained with good yield while maintaining the rare antiseptic power without the use of a cosolvent such as alcohol, chlorinated hydrocarbon, hexane, acetone. Therefore, the use of an organic solvent is unnecessary, and thus a cosmetic composition that is environmentally friendly and stable to the human body can be prepared.
(B) preparing an inclusion complex
This step is to prepare a clathrate complex by mixing the rare supercritical fluid extract obtained in step (A) with dextrin.
Rare supercritical fluid extracts extracted using supercritical fluid extraction may be added to cosmetic compositions, but there are limitations to solvents applicable to cosmetics, resulting in 1,3-butylene glycol ) Or water-soluble solvents such as propylene glycol, which are difficult to dissolve. Therefore, in the present invention, the rare supercritical fluid extract is included in the dextrin to improve the solubility problem of the rare supercritical fluid extract.
At this time, the preferred dextrin may be gamma cyclodextrin, beta cyclodextrin, it is more preferable to use beta cyclodextrin from the economic point of view.
In addition, when the rare supercritical fluid extract is included in dextrin, distilled water is added to the mixture of the rare supercritical fluid extract and dextrin, followed by stirring at 50 to 60 ° C. At this time, the inclusion ratio of the dextrin and the rare supercritical fluid extract is preferably 100: 3 to 100: 6, more preferably 100: 3. When the inclusion ratio is satisfied, excellent dispersion efficiency can be produced in a stable powder in the following step.
(C) preparing a rare inclusion powder
This step is to prepare a rare inclusion powder by spray drying the inclusion complex prepared in step (C).
After manufacturing the clathrate composite at the optimum clathrate ratio, if a stable powdering process is secured, mass production is possible, and thus the cosmetic material can be easily manufactured and manufactured.
In the present invention, the inclusion complex is powdered by using a spray dryer (BUCHI SWITZERLAND, BUCHI Mini Spray Dryer B-290), stability of powdering, appearance of powder suitable for cosmetic materials (off-white powder), high yield Inclusion powder can be prepared.
At this time, preferred spray drying conditions are as follows.
Inlet: 150 ℃
Outlet: 90 ~ 100 ℃
Aspirator (%): 100
Pump (%): 10
Nozzle Claner: 0
(D) adding rare clathrate powder to the water-soluble cosmetic base
This step is a step of preparing a cosmetic composition by adding the rare inclusion powder prepared in step (C) to a water-soluble cosmetic base.
In the water-soluble cosmetic composition, a solvent having water solubility is used as a base, and water, alcohol, and the like of the water-soluble solvent are used. However, the water-soluble cosmetic composition of the present invention is not only completely water-soluble composition, but also comprises an oil phase, and includes an emulsion (emulsion) and the like which shows some water solubility.
According to the present invention, a cosmetic composition containing a natural preservative can be prepared using a rare inclusion powder.
In addition, according to the present invention Bacillus by using rare inclusion powder subtilis , Staphylococcus aureus , Esherichia coli , Pseudomonas aeruginosa , Candida albicans , Aspegillus Cosmetic compositions having excellent antimicrobial activity against niger can be prepared.
In addition, according to the present invention, a rare extract showing relatively low water solubility can be effectively dissolved and added to the water-soluble cosmetic composition.
In addition, according to the present invention it is possible to manufacture a cosmetic composition in an economical way by reducing the cost of tariffs and the like by not using ethanol while effectively maintaining a rare antiseptic force through a supercritical fluid extraction method.
Moreover, according to this invention, a cosmetic composition can be manufactured using the rare inclusion powder which has a characteristic (off-white powder) suitable for a cosmetic material.
1 is a graph showing a change in extraction yield of rare water according to supercritical fluid extraction conditions.
Hereinafter, the configuration of the present invention will be described in detail through the following examples and experimental examples. However, the scope of the present invention is not limited only to the following examples, and includes variations of similar technical ideas.
Example One : Supercritical Using fluid extraction Rare Preparation of extract
In this embodiment, a supercritical fluid extraction device (OSA-SCCO-S-100-500) was used for supercritical fluid extraction.
1 kg of pulverized rare flakes were put into an extraction tank, and extracted at 40, 50, and 60 ° C. for 120 minutes at a pressure of 200, 300, 400, or 500 bar to obtain an extract. At this time, CO 2 gas was flowed at a flow rate of 55 to 58 g / min.
The results of checking the extraction trend according to the conditions of the supercritical fluid temperature and pressure are shown in Table 1 and FIG. 1.
According to this, the pressure showed the highest extraction yield at 300 bar, the temperature showed the highest extraction yield at 40 ℃.
On the other hand, as a result of visual inspection, it showed a pale off-white appearance almost no chlorophyll elution at 200 bar, 60 ℃ conditions. To this end, a rare supercritical fluid extract extracted at 200 bar and 60 ° C. was used.
Example 2 : Included Rare Supercritical Fluid extracts ( Enclosure Complex)
In this example, the clathrate complex was prepared using a rare supercritical fluid extract and dextrin obtained by removing the chlorophyll prepared in Example 1.
After adding the rare supercritical extract of Example 1 to 100 g of maltodextrin, gamma cyclodextrin, and betacyclodextrin to the dry weight of 1, 3, and 6% by dry weight, the rare supercritical extract and dextrin were mixed. Distilled water was added three times the total dry weight and mixed for 24 hours using a stirrer at 50 ~ 60 ℃. When the mixing was completed, the presence of precipitates was visually checked to remove distilled water using a rotary vacuum concentrator under conditions where no precipitate was formed, and then the inclusion complexes were recovered.
The inclusion results according to the inclusion ratio of the rare supercritical fluid extract and dextrin are shown in Table 2 below.
Dextrin: Rare
According to Table 2, in the case of inclusion using maltodextrin, precipitation was formed regardless of the inclusion ratio of maltodextrin and the rare supercritical fluid extract.
On the other hand, in the case of inclusion using gamma cyclodextrin and betacyclodextrin, it was confirmed that no precipitation was formed at various inclusion ratios. Considering the unit price, beta-cyclodextrin may be advantageous. In the following, beta-cyclodextrin was used to determine inclusion conditions with rare supercritical fluid extracts.
Example 3, 4: using spray drying Rare Enclosure Preparation of powder
In the present embodiment, the inclusion complex having the inclusion ratio (beta cyclodextrin: rare supercritical fluid extract) of 100: 3 and 100: 6 is used under conditions where beta cyclodextrin can be stably included with the rare supercritical fluid extract. A rare inclusion powder was prepared.
A spray dryer (BUCHI SWITZERLAND, BUCHI Mini Spray Dryer B-290) was used for spray drying, and spray drying was performed under the conditions shown in Table 3 below.
The powdered result of applying the spray dryer using the inclusion complex is shown in Table 4 below.
(dextrin: draw = 100: 3)
(dextrin: draw = 100: 6)
According to Table 4, the two inclusion ratios did not show a big difference in the stability and properties of the powdering (chlorophyll-free color), yield. According to this, it is possible to mix, inclusion and powder at both inclusion ratios of 100: 3 and 100: 6, so that the mass production process can be applied according to the formulation development.
Experimental Example 1: Standard test method for indicator component setting and content analysis GC Indicator component quantification using
In the present experimental example, the content of linoleic acid, the index component in the rare supercritical fluid extract and the rare inclusion powder, was confirmed using GC.
500mg of methyl linoleic acid was precisely weighed and dissolved in 100ml of iso-octane to make 5000ppm.
About 0.5 g of the sample was placed in a 50 mL test tube, 5 mL of 0.5 N methanolic NaOH was added, and then sufficiently voltexed, and then heated at 121 ° C. for 15 min in a sterilizer and left at room temperature. 4 mL of 14% BF 3 (in methanol) was added and 10 mL of saturated NaCl solution was added thereto. A 0.2 mL filter was used for 20 mL syringes, left to separate layers, and the upper iso-octane layer was taken and used as a sample solution. Instrument analysis was performed under the GC conditions of Table 5 below.
The linoleic acid content as an indicator component in the rare supercritical fluid extract and the rare inclusion powder is shown in Table 6 below.
(dextrin: rare = 100: 3)
(dextrin: rare = 100: 6)
According to the Table 6, the linoleic acid as an indicator component in the rare supercritical fluid extract was found to be about 3430ppm, and when the inclusion ratio was 100: 3, the linoleic acid content was about 104ppm, and the inclusion ratio was In case of 100: 6, the linoleic acid content was found to be 115ppm.
From this, it was judged that the dispersion efficiency was different depending on the inclusion ratio of dextrin and rare supercritical extract, and the optimum inclusion ratio was found when the inclusion ratio of dextrin: rare extract was 100: 3.
In summary, the conditions for producing the final clathrate powder finally confirmed are as follows.
Supercritical Fluid Extraction Condition: 200bar, 60 ℃
Inclusion rate (dextrin: rare) = 100: 3
Drying method: Spray drying
Appearance: Off-white powder
Experimental Example 2 : Rare Enclosure Antibacterial Functionality of Powder Investigation (validation of rare inclusion powder sign)
In the present experimental example, the microbial growth inhibition minimum concentration (MIC: Minimum Inhibitory Concentration) was measured to confirm the antimicrobial activity of the rare inclusion powder prepared by the method of Example 3.
6 major contaminant microorganisms in cosmetics (( Bacillus as Gram-positive bacteria) subtilis KCTC 1021, Staphylococcus aureus KCTC 1927, Esherichia as Gram-negative bacteria coli KCTC 2593, Pseudomonas aeruginosa KCTC 2004, Candida as Yeast albicans KCTC 7965, Aspegillus fungus niger KCTC 6317)) was incubated and used in the experiment, and calculated by converting the amount of rare flakes contained in the powder, and then adding the sample to the 96-well plate so that the maximum concentration of the rare flakes was 1.5% (w / v). Samples were added to each well by dilution concentration via a 2-step dilution method.
Six microorganisms were inoculated in each well to which the sample was treated to a concentration of 1 × 10 6 CFU / ml, and incubated at 37 ° C., and when the culture was completed, absorbed at 595 nm using an ELISA reader. By measuring the growth degree of the cultured microorganism, and the result of calculating the concentration of the effect is shown in Table 7 below.
According to Table 7, antimicrobial activity was confirmed in the sample in which the rare inclusion powder was added at a concentration of 0.3 to 1% (w / v).
Experimental Example 3: Rare Enclosure Powdered Cosmetic Safety and stimulus assessment
In this Experimental Example, in order to evaluate the safety and stimulation of rare clathrate powder prepared by the method of Example 3 on the human body, the first human body test (Human patch test) to 20 healthy adult men and women Stimulation tests and cumulative stimulation tests were performed.
20 healthy males and females were dissolved in 0.3% (w / v) of dilution clathrate powder of Example 3 in a Finn Chamber and added dropwise to 20ul each, which was then placed inside the arm of the human body as a test site. Topped and fixed with tape. In the first skin irritation test, the patch was removed for 24 hours, and then the skin reaction of the test site after 4 hours and 24 hours after removing the patch was determined according to the criteria of Table 8 below, and the results are shown in Table 9 below. It was.
[Stimulus calculation formula]
Stimulus = [{(±) number x 1} + {(+) number x 2} + {(++) number x 3}] / number of subjects
According to the above Table 9, it was confirmed that the cosmetic composition containing the rare inclusion clathrate powder of the present invention does not irritate the human body.
Experimental Example 4 : Rare Enclosure Confirmation of formulation stability of powder Rare Enclosure Determination of Solubility of Powder by Solvent)
In this Experimental Example, the solvent-specific solubility of the rare clathrate powder prepared by the method of Example 3 was confirmed, and the results are shown in Table 10 below.
According to Table 10, it was confirmed that the rare inclusion clathrate powder of the present invention is dissolved up to 2.0% in distilled water.
Example 4 : Rare Enclosure Preparation of lotions containing powders (lotions containing natural preservatives)
In this example, a lotion containing the rare inclusion powder prepared in Example 3 was prepared according to a conventional method, and its components and compositions are shown in Table 11 below.
Example 5: Rare Enclosure Containing powder Skin (skin containing natural preservatives) Manufacturing
In this embodiment, the skin containing the rare inclusion clathrate powder prepared in Example 3 was prepared according to a conventional method, the components and compositions are shown in Table 11 below.
Claims (5)
(B) mixing the rare supercritical fluid extract with betacyclodextrin to prepare an inclusion complex;
(C) spray-drying the inclusion complex to produce rare inclusion powder; And
(D) adding the rare clathrate powder to a water-soluble cosmetic base; a method of producing a cosmetic composition comprising a.
In the step (A)
Process for producing a cosmetic composition, characterized in that to obtain a rare supercritical fluid extract at a pressure of 200 bar, extraction temperature 60 ℃.
In the step (B)
Beta cyclodextrin: The inclusion rate of the rare earth is a manufacturing method of the cosmetic composition, characterized in that 100: 3 ~ 100: 6.
Said rare inclusion powder is a process for producing a cosmetic composition, characterized in that the off-white powder.
The rare inclusion powder is a method for producing a cosmetic composition, characterized in that used as a natural preservative.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2015199516A1 (en) * | 2014-06-27 | 2015-12-30 | 연세대학교 산학협력단 | Composition for improving muscular function or enhancing exercise performance, containing kirenol or hui chum extract |
KR20160034569A (en) * | 2014-09-22 | 2016-03-30 | 수원대학교산학협력단 | Production method of non-pigmented antioxidant extracts, non-pigmented antioxidant extracts produced by the method and cosmetic composition containing the same |
US10507224B2 (en) | 2014-06-27 | 2019-12-17 | Aat Costech Co., Ltd. | Composition including kirenol or siegesbeckia herba extract for muscle function improvement or exercise ability enhancement |
KR20200069743A (en) * | 2018-12-07 | 2020-06-17 | 한국과학기술연구원 | Composition for improving intestinal microbiome comprising siegesbeckia pubescens makino extract |
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2011
- 2011-12-28 KR KR1020110145061A patent/KR20130076465A/en not_active Application Discontinuation
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2015199516A1 (en) * | 2014-06-27 | 2015-12-30 | 연세대학교 산학협력단 | Composition for improving muscular function or enhancing exercise performance, containing kirenol or hui chum extract |
US10507224B2 (en) | 2014-06-27 | 2019-12-17 | Aat Costech Co., Ltd. | Composition including kirenol or siegesbeckia herba extract for muscle function improvement or exercise ability enhancement |
KR20160034569A (en) * | 2014-09-22 | 2016-03-30 | 수원대학교산학협력단 | Production method of non-pigmented antioxidant extracts, non-pigmented antioxidant extracts produced by the method and cosmetic composition containing the same |
KR20200069743A (en) * | 2018-12-07 | 2020-06-17 | 한국과학기술연구원 | Composition for improving intestinal microbiome comprising siegesbeckia pubescens makino extract |
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