KR101769935B1 - Method for producing Broussonetia plant extracts, the extracts produced thereby, and the cosmetic composition containing the same - Google Patents

Abstract

The present invention relates to a method for producing a mackerel extract, a mackerel extract, and a cosmetic composition comprising the same. More particularly, the present invention relates to a method for extracting mackerel or an extract thereof by ultra high pressure, supercritical or oil extraction method, , Anti-aging, anti-wrinkle, moisturizing and elasticity improvement effect, a mackerel extract prepared thereby, and a cosmetic composition containing the same.

Description

TECHNICAL FIELD The present invention relates to a method for producing a mulberry extract, a mulberry extract prepared by the same, and a cosmetic composition containing the extract,

The present invention relates to a method for producing a mackerel extract, a mackerel extract, and a cosmetic composition containing the same. More particularly, the present invention relates to a method for extracting mackerel or an extract thereof by ultra high pressure, supercritical or oil extraction method, , Anti-aging, anti-wrinkle, moisturizing and elasticity improvement effect, a mackerel extract prepared thereby, and a cosmetic composition containing the same.

The mackerel has been used as a raw material for papermaking and has various medicinal properties. It has effects on tonic, acupuncture, acupuncture, species, waxing and diuretic, removing wind, clearing blood It is said to be effective for declining eyesight.

Ultra high pressure technology is artificially applying a pressure of 1 GPa, that is, about 10,000 atm or more. It is used for diamond synthesis and metal processing, and has recently been applied to extract natural products.

A supercritical fluid refers to a fluid at a point where it can not distinguish a liquid from a gas by reaching a state beyond a certain high temperature and high pressure limit. The density of the molecules is close to the liquid, but the viscosity is low and close to the gas, the diffusion is fast and the thermal conductivity is high, which is useful for the chemical reaction. The use of such a supercritical fluid is supercritical extraction.

The inventors of the present invention have studied a method for increasing the content of active ingredient in the extract of Mulberry tree. As a result, they found that when extracting mulberry with an ultra high pressure, supercritical or oil extraction method, the effect of improving whitening, antiaging, anti wrinkle, moisturizing and elasticity is excellent Thereby completing the present invention.

Accordingly, it is an object of the present invention to provide a method for producing a mulberry extract for increasing the content of an active ingredient in a mulberry extract.

It is also an object of the present invention to provide a cosmetic composition comprising a mulberry extract prepared by the above method.

In order to achieve the above object, the present invention provides a method for producing a mulberry extract comprising a step of extracting at least one selected from the group consisting of roots, stems, leaves, flowers and fruits of Mulberry tree by ultra high pressure, supercritical or oil extraction method .

In addition, the present invention provides a cosmetic composition comprising the extract of Mulberry Mackerel prepared by the above method.

The extract of mulberry leaves extracted by the method of the present invention was excellent in whitening, anti-aging, anti-wrinkle, moisturizing and elasticity improving effects due to the increase of active ingredients.

1 is a cross-sectional view of an ultra high pressure machine used in the present invention.
2 is a photograph of the ultra-high pressure machine used in the present invention.

Hereinafter, the present invention will be described in more detail.

The present invention relates to a method for producing a mulberry extract by ultra high pressure, supercritical or oil extraction method. More particularly, the extraction method according to the present invention is characterized in that at least one of roots, stems, leaves, flowers and fruits of mulberry is added with water or C1 to C5 lower alcohol, and the active ingredient is added at 10 to 90 DEG C for 4 to 24 hours Extracting; And extracting the extract with an ultrahigh pressure, supercritical or oil extraction method. The ultrahigh pressure, supercritical or oil extraction method may be performed simultaneously with or sequentially with the extraction step, and the extraction process using a lower alcohol may be omitted You may.

In one embodiment of the present invention, the extract of Mulberry can be prepared using ultra high pressure technology. For example, roots, stems, leaves, flowers or fruits of mulberry can be extracted at 20 to 50 DEG C under a pressure of 50 to 300 MPa for 10 to 20 minutes under ultra-high pressure, preferably at 25 to 35 DEG C for 70 to 200 High-pressure treatment is carried out at a pressure of Mpa for 10 minutes to 15 minutes.

In one embodiment of the present invention, the ultra-high pressure apparatus having the configuration shown in FIGS. 1 and 2 may be used for ultra-high pressure treatment, but the present invention is not limited thereto. 1, the ultra-high pressure machine includes a cylinder portion, a processing chamber for containing the pressurized material of the sealer portion, a pressurizing piston, a water circulation jacket for regulating the temperature outside the cylinder, And an oil pump. In the Lab scale, the HHP has a maximum pressure of 600 MPa, a working volume of about 0.6 L, and an industrially applicable degree is a pilot-scale (Pilot-scale) UHP plant (35 L) with a maximum pressure of 2,000 Mpa and a working volume of up to 35 liters.

Also, in one embodiment of the present invention, a mulberry extract can be prepared using supercritical technology. At this time, as the supercritical fluid, carbon dioxide, nitrogen, nitrous oxide, methane, ethylene, propane and propylene can be used, and supercritical carbon dioxide is preferably used. This is because carbon dioxide in the supercritical fluid has a critical pressure of 73.8 bar and a critical temperature of 31.1 ° C., which makes it generally easy to make supercritical conditions, is not toxic to carbon dioxide itself and is inexpensive.

The supercritical extraction condition is preferably added by applying a supercritical fluid under a pressure of 70 to 200 bar at 20 to 40 ° C. When the extraction temperature is higher than 20 ° C, the extraction efficiency is increased. When the extraction temperature is higher than 40 ° C, the extraction efficiency is high, but the extraction efficiency is not increased as compared with the lower extraction efficiency. In addition, the extraction efficiency is increased when the air pressure is 70 bar or more, and the extraction efficiency is not increased when the air pressure is 200 bar or less.

Also, in one embodiment of the present invention, a mulberry extract can be prepared through an oil extraction method. For example, vegetable oil such as soybean oil and sesame oil may be added to the root, stem, leaf, flower or fruit of mulberry tree and extracted for 2 to 12 hours at 40 to 70 ° C and 2 to 10 bar pressure.

The present invention also relates to a cosmetic composition comprising 0.0001 to 90% by weight, preferably 0.001 to 50% by weight, of the mackerel extract prepared according to the above method, based on the total weight of the composition. The cosmetic composition according to the present invention is characterized by whitening, anti-aging, anti-wrinkle, moisturizing or improving elasticity.

Hereinafter, the present invention will be described more specifically with reference to examples and test examples. It is to be understood that the scope of the present invention is not limited to these embodiments and that variations, substitutions, and insertions conventionally known in the art can be carried out, And this is included in the scope of the present invention.

[Example 1] Preparation of ultra high pressure extract

After the ultra-high pressure machine was set up, ultra-high pressure treatment was prepared, and the processing chamber portion was filled with water. Then, the mackerel prepared above was packed in a vacuum pack, and a pressure of 50 MPa or more And treated at a temperature of 50 DEG C or lower for 1 minute or longer, cooled at room temperature, and dried in a drier to obtain a mulberry extract.

[Example 2] Preparation of supercritical extract

1 kg of mulberry leaves and roots were washed with clean water and then dried. Then, carbon dioxide was supplied to the extraction tank by using a high pressure gas pump. When the pressure reached 75 bar, the supply of carbon dioxide was stopped. Using a temperature controller, the temperature inside the extraction tank was raised to 40 ° C at a rate of 2 ° C / min through a hot wire wrapping the outside of the extraction tank. The temperature and pressure of the extraction tank were maintained at 34 ° C and 74 bar for 30 minutes while partially discharging the carbon dioxide using a pressure regulator attached to the outlet of the extraction tank. Then, the high-pressure gas pump was restarted and carbon dioxide was continuously supplied to the extraction tank at a flow rate of 2 L / min. At the same time, the extract was released using a pressure regulator attached to the outlet side, and the temperature and pressure of the extraction bath were kept constant at 34 ° C and 74 bar. While the temperature of the pressure regulator was maintained at 40 ° C, the effluent discharged through the pressure regulator was transferred to solid dry ice due to pressure and temperature drop. The extracted extract was decompressed at normal pressure to release carbon dioxide into the atmosphere, and the extract of the mulberry tree was collected into a collector. The above procedure was carried out for 4 hours to obtain a mulberry extract.

[Example 3] Production of oil extract

1 kg of mulberry leaves and roots were washed with clean water and then dried in 10 ℓ of soybean oil. The extract was extracted with a condenser at 50 ° C. for 2 hours under a pressure of 2 to 4 bar for 4 hours and filtered through a filter paper. This extract was concentrated under reduced pressure to 70 ° C in a distillation apparatus equipped with a cooling condenser to obtain an extract of mulberry leaves.

[Comparative Example 1]

1 kg of mulberry leaves and roots were washed with clean water and then placed in 10 ℓ of water. The extract was boiled in an extractor equipped with a condenser for 5 hours, filtered through a 300-mesh filter cloth, and allowed to stand at 5 to 15 ° C. for 5 days. Filter 2 with filter paper. The extract was concentrated under reduced pressure to 80 ° C in a distillation apparatus equipped with a cooling condenser to obtain 71.3 g (dry weight).

[Example 4]

The mulberry extract prepared in Comparative Example 1 was subjected to ultrahigh pressure treatment in the same manner as in Example 1.

[Example 5]

The mulberry extract prepared in Comparative Example 1 was subjected to supercritical extraction in the same manner as in Example 2.

[Example 6]

The extract of the mulberry extract prepared in Comparative Example 1 was subjected to oil extraction in the same manner as in Example 3.

Test Example 1: Effect of tyrosinase inhibition

The tyrosinase enzyme was extracted from Mushroom and was obtained from Sigma (SIGMA). First, the substrate, tyrosine, is dissolved in distilled water to make a 0.3 mg / ml solution. The solution is put into a test tube in an amount of 1.0 ml. Then, 1.0 ml of potassium phosphate buffer solution (0.1 mol concentration, pH 6.8) and 0.7 ml of distilled water .

The extracts of Examples 1 to 6 and Comparative Example 1 were mixed at an appropriate concentration in an ethanol solution, and 0.2 ml of each of the extract samples prepared was added to the reaction solution and reacted in a thermostatic chamber at 37 ° C for 10 minutes. At this time, the control group was prepared by adding 0.2 ml of the solvent instead of each extract, and ascorbic acid was used as the positive control group. 0.1 ml of tyrosinase solution of 2500 units / ml was added to the reaction solution, and the mixture was reacted in a 37 ° C thermostat for 10 minutes. The reaction tube was immersed in ice water to quench the reaction, and the absorbance at 475 nm was measured with a photoelectron spectrometer. The results are shown in Table 1 below. The tyrosinase inhibitory effect of each extract was calculated by the following formula (1).

Test substance Inhibition rate of tyrosinase (%) Control group (no addition) 0 Ascorbic acid 52 Example 1 45 Example 2 42 Example 3 38 Example 4 66 Example 5 69 Example 6 54 Comparative Example 1 32

From the results shown in Table 1, it can be seen that the extracts of Examples 1 to 6 prepared by ultra-high pressure, supercritical and oil extraction methods had a high inhibitory effect on tyrosinase and thus had excellent whitening effect.

[Test Example 2] Evaluation of inhibition of melanin formation using B16 / F10 melanoma cells

A sample containing 0.001% by weight of each of Examples 1 to 6 and Comparative Example 1 and kojic acid was added to the culture medium of B16 / F10 melanoma cells (Korean Cell Line Bank) at a constant concentration as a test substance and cultured for 3 days The culture was removed, washed with PBS, and the cells were lysed with 1N NaOH and absorbance was measured at 405 nm. Cells to which the test substance was not added were used as a control group, and the melanin formation inhibition degree of each test substance was measured by comparing with the melanin content in the control group. The inhibition rate of melanin production was calculated according to Equation (2), and the results are shown in Table 2.

Test substance Melanin inhibition rate (%) Control group (no addition) 0 Kojic acid 53 Example 1 56 Example 2 52 Example 3 58 Example 4 67 Example 5 69 Example 6 54 Comparative Example 1 41

From the results shown in the above Table 2, it was found that the extracts of Examples 1 to 6 prepared by ultra-high pressure, supercritical and oil extraction methods had a high inhibitory effect on melanin production and excellent whitening effect.

[Formulation Examples 1 to 6 and Comparative Formulation Examples 1 to 2]

The nutritional creams of Formulation Examples 1 to 6 and Comparative Formulation Examples 1 to 2 were prepared in a conventional manner according to the composition of Tables 3 and 4 (unit: wt%).

Compounding ingredient Formulation Example 1 Formulation Example 2 Formulation Example 3 Formulation Example 4 Formulation Example 5 Formulation Example 6 Example 1 0.5 - - - - - Example 2 - 0.5 - - - - Example 3 - - 0.5 - - - Example 4 - - - 0.5 - - Example 5 - - - - 0.5 - Example 6 - - - - - 0.5 Wax 10 10 10 10 10 10 Polysorbate 60 1.5 1.5 1.5 1.5 1.5 1.5 Piggy 60 hardened castor oil 2 2 2 2 2 2 Sorbitan sesquioleate 0.5 0.5 0.5 0.5 0.5 0.5 Liquid paraffin 10 10 10 10 10 10 Squalane 5 5 5 5 5 5 Caprylic / capric triglyceride
(Estasan: Uniqema (manufacturer)) 5 5 5 5 5 5 glycerin 5 5 5 5 5 5 Butylene glycol 3 3 3 3 3 3 Propylene glycol 3 3 3 3 3 3 Triethanolamine 0.2 0.2 0.2 0.2 0.2 0.2 Preservatives, coloring and flavoring Suitable amount Suitable amount Suitable amount Suitable amount Suitable amount Suitable amount Purified water Balance Balance Balance Balance Balance Balance

Compounding ingredient Comparative Formulation Example 1 Comparative Formulation Example 2 Comparative Example 1 - 0.5 Wax 10 10 Polysorbate 60 1.5 1.5 Piggy 60 hardened castor oil 2 2 Sorbitan sesquioleate 0.5 0.5 Liquid paraffin 10 10 Squalane 5 5 Caprylic / capric triglyceride
(Estasan: Uniqema (manufacturer)) 5 5 glycerin 5 5 Butylene glycol 3 3 Propylene glycol 3 3 Triethanolamine 0.2 0.2 Preservatives, coloring and flavoring Suitable amount Suitable amount Purified water Balance Balance

[Test Example 3] Skin moisturizing effect

In order to measure the effect of the extract of the mulberry tree according to the present invention on the increase in skin moisturizing power, 160 adult male and female adults of 40 to 50 years of age representing dry skin were divided into 8 groups, and Formulation Examples 1 to 6 and Comparative Formulation Examples 1 to 2 Twice daily for 4 weeks. (24 ° C, relative humidity: 40%) after one week, two weeks, and four weeks after application and before two weeks (six weeks after completion of application) Skin moisture was measured and the results are shown in Table 5 below. Connio meter is a skin moisture analyzer that measures the amount of water present in the skin by measuring the electrical conductivity of the skin. The test result is a percentage of the increment of the measured value after a certain period of treatment based on the coneometer value measured just before the start of the test.

Test substance Moisture growth rate (%) 1 week Two weeks 4 weeks 6 weeks Formulation Example 1 32 36 38 30 Formulation Example 2 33 37 37 29 Formulation Example 3 30 37 40 30 Formulation Example 4 31 40 42 32 Formulation Example 5 31 39 40 31 Formulation Example 6 32 36 38 29 Comparative Formulation Example 1 30 32 32 15 Comparative Formulation Example 2 32 35 38 26

From the results of Table 5, it can be confirmed that the skin moisture increase rate of Formulation Examples 1 to 6 including the extracts of mulberry leaves of Examples 1 to 6 prepared through the ultra-high pressure, supercritical and oil extraction methods according to the present invention is excellent. In addition, even after stopping the application of the nutritional cream of Formulation Examples 1 to 6, the skin moisture was measured similarly to the one week after application, and it was found that the skin moisture was maintained constantly for a certain period of time without applying the example there was.

[Test Example 4] Effect of improving skin wrinkles

In order to measure the effect of the extract of Mulberry Mulberry according to the present invention on the improvement of skin wrinkles, 160 wrinkles of 30 to 50 year olds were compared and evaluated for the improvement of skin wrinkles.

The skin condition of both sides of the facial area before the use of the cream was measured. Then, the creams of Formulation Examples 1 to 6 and Comparative Formulation Examples 1 and 2 were used for 3 months for each test subject, and then the same area was re- And the results are shown in Table 6 below. The skin wrinkles were measured with a Visiometer system (C + K company) by removing the wrinkles of the eye tail region with a replica in a constant temperature and humidity chamber at 24 ° C and a relative humidity of 40%. The change amount of the skin wrinkles was calculated according to the following equation (3).

In the equation (3), "Tdi" is the measured site value at D90 and "Tdo" is the measured site value at D0.

Test substance Change in skin wrinkles (%) Formulation Example 1 19 Formulation Example 2 17 Formulation Example 3 16 Formulation Example 4 22 Formulation Example 5 20 Formulation Example 6 18 Comparative Formulation Example 1 2 Comparative Formulation Example 2 12

From the results of Table 6, it can be confirmed that Formulation Examples 1 to 6 containing the extracts of Mulberry tree extracts of Examples 1 to 6 prepared by ultra high pressure, supercritical and oil extraction methods according to the present invention have excellent skin wrinkle improving effect.

[Test Example 5] Confirmation of improving skin elasticity

In order to confirm the skin elasticity improving effect, creams of Formulation Examples 1 to 6 and Comparative Formulation Examples 1 and 2 were divided into eight groups each consisting of 160 persons of 30 to 40 years old women in a group of 20 persons. The experimental method is as follows.

Creams of Formulation Examples 1 to 6 and Comparative Formulation Examples 1 and 2 were each divided into groups and applied once to the face for 12 weeks. Then, skin elasticity meter (Cutometer SEM 575, C + K Electronic Co., Germany) And skin elasticity was measured. The results are shown in Table 7 below. The results in Table 7 are reported as ΔR8 (R8 (left) -R8 (right)) of Cutometer SEM 575, where the R8 value indicates the nature of viscoelasticity.

Test substance Skin elasticity effect Formulation Example 1 0.37 Formulation Example 2 0.38 Formulation Example 3 0.35 Formulation Example 4 0.42 Formulation Example 5 0.41 Formulation Example 6 0.37 Comparative Formulation Example 1 0.12 Comparative Formulation Example 2 0.32

From the results of Table 7, it can be confirmed that the skin elasticity improving effects of Formulation Examples 1 to 6 including the extracts of mulberry leaves of Examples 1 to 6 prepared through the extraction process according to the present invention are excellent.

Therefore, it can be confirmed that the cosmetic composition containing the extract of Mokuba extract of the present invention is very effective for improving skin elasticity.

Claims (10)

Extracting at least one member selected from the group consisting of root, stem, leaf, flower and fruit of mulberry with water or C1 to C5 lower alcohol; And
Extracting the extract obtained by the first extraction with an ultrahigh pressure, supercritical or oil extraction method,
The ultra-high pressure extraction method is characterized in that the treatment is carried out at a temperature of 20 to 50 DEG C at a pressure of 50 to 300 MPa for 10 minutes to 20 minutes,
Characterized in that the supercritical extraction process is carried out using a supercritical fluid at 20 ° C to 40 ° C under a pressure of from 70 to 200 bar,
Wherein the oil extraction method comprises adding vegetable oil and treating the mixture at 40 to 70 DEG C and 2 to 10 bar pressure for 2 to 12 hours. delete delete The method according to claim 1,
Wherein the ultra high pressure extraction method is performed at 25 to 35 DEG C at a pressure of 70 to 200 MPa for 10 minutes to 15 minutes. The method according to claim 1,
Wherein the supercritical extraction is carried out under a pressure of 34 to 40 DEG C and 74 to 200 bar. The method according to claim 1,
Wherein the supercritical fluid is carbon dioxide, nitrogen, nitrous oxide, methane, ethylene, propane or propylene. The method according to claim 1,
Wherein the oil extraction method comprises adding vegetable oil and treating the mixture at 50 DEG C and 2 to 4 bar pressure for 4 to 12 hours. 8. The method of claim 7,
Wherein the vegetable oil is soybean oil or sesame oil. 9. A cosmetic composition comprising a mulberry extract prepared according to any one of claims 1 to 8. 10. The method of claim 9,
Wherein said composition is for whitening, anti wrinkling, moisturizing or improving elasticity.

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