KR20130014150A - Liposome collecting kaempferitrin and coating carrageenan and method of the same - Google Patents

Abstract

PURPOSE: A liposome containing kaempferitrin and coated with carrageenan is provided to enhance dispersion stability in a formulation and to develop a natural organic UV protection agent. CONSTITUTION: A method for preparing a liposome which contains kaempferitrin and is coated with carrageenan comprises: a step of dissolving phospholipid in a lipid solvent; a step of drying the mixture by vacuum at reduced pressure and forming a phospholipid membrane; a step of dissolving kaempferitrin in a buffer for preparing a solution and adding the solution and carrageenan to a phospholipids membrane; a step of treating by ultrasonic waves and encapsulating kaempferitrin in a liposome; a step of removing uncapsulated kaempferitrin by washing; and a step of forming a film on the liposome surface using the carrageenan. The phospholipid includes phospholipid, phosphatidyl choliine, lipid, lecithin, or cholesterol. A cosmetic composition for blocking UV rays contains the liposome as an active ingredient.

Description

Liposome coated with carrageenan and coated with carrageenan and its preparation method {Liposome Collecting Kaempferitrin and Coating Carrageenan and Method of The Same}

The present invention relates to liposomes in which capperitrin is trapped and coated with carrageenan, and more particularly, liposomes which have a sunscreen effect to increase the surface stability of particles to minimize skin absorption of active substances. And, by coating a carrageenan derived from the nature outside the liposomes to increase the stability of the material to increase the duration of UV protection is trapped capritririn, characterized in that the liposomes coated with carrageenan, its preparation method and active ingredient It relates to a sunscreen cosmetic composition containing.

Kaempferitrin is a dicotyledonous plant native to Africa and India. It is a flavonoid-based substance present in large quantities of horseshoe, a perennial herb of Mallow family, and has anti-inflammatory effects (Food chemistry, 117: 444, 2009). Effect (Bioc. Biop. Res. Comm., 380: 39, 2009), and the like, and the Korean Patent No. 10-0815476 discloses Kenaf ( Hibiscus cannabbinus L., Malvaceae) extract and isolated therefrom It is known that new camphorol compounds have excellent effects on antioxidants and antibacterial properties.

In general, liposomes are nano-sized (1 μm or less) capsules as phospholipids and mediators, and they can contain both lipophilic and hydrophilic functional materials, so they are suitable for living organisms similar to human skin cells. It is a substance that, when added to a hydrophilic formulation, remains suspended and has surface stability. Looking at the examples of previous studies of natural sunscreen, coffee oil, jujube fruit extract, aloe extract, etc. are known to be effective in the sunscreen effect, but the study applying the capture technology or emulsification technology for stability in the formulation is inorganic ultraviolet Except in the case of using a blocking material, there is no situation.

Therefore, the present inventors liposomes the camphorritin extracted from natural plants to increase the stabilization and skin surface sustainability, and as a result of the effort to manufacture a cosmetic composition having a sunscreen effect, as a result, the camphortrit having a sunscreen effect is collected Carrageenan is coated on the liposomes to confirm that it is effective in blocking the sun based on the improved dispersion stability to complete the present invention.

An object of the present invention is to liposome the sunscreen to increase the surface stability of the particles by increasing the surface stability of the particles by liposomes, and to increase the stability of the material by coating the carrageenan derived from the nature outside the liposomes The present invention provides a liposome that collects camphortrin to increase its duration, a preparation method thereof, and a sunscreen cosmetic composition containing the same as an active ingredient.

In order to achieve the above object, the present invention comprises the steps of (a) mixing the phospholipids dissolved in a lipid solvent; (b) vacuum drying to form a phospholipid membrane; (c) adding an aqueous solution and carrageenan prepared by dissolving campertrin in a buffer to the resulting phospholipid membrane, followed by sonication to capture campertrin into liposomes; (d) washing and removing non-captured camphortrins other than liposomes; And (e) forming a film with carrageenan on the washed liposome surface to obtain a coated liposome, thereby providing a method for producing a liposome that is trapped and coated with carrageenan.

The present invention also provides a liposome having an ultraviolet blocking function, which is prepared by the above method, in which camphoritrin is collected and coated with carrageenan.

The present invention also provides a sunscreen cosmetic composition containing the liposome as an active ingredient.

By coating carrageenan on the liposomeized camphortririn of the present invention, by improving the dispersion stability in the formulation and inhibiting skin penetration to the maximum, by increasing the duration of the active substance on the surface of the skin by developing a natural organic sunscreen having a high UV protection index It provides a natural organic sunscreen and external skin composition having an effective sunscreen ability by securing the stabilization technology in the formulation of camphortrin, and overcomes the side effects and disadvantages of the inorganic sunscreen.

1 shows a TEM image of liposomeized camphortrin.

Unless otherwise defined, 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. In general, the nomenclature used herein is well known and commonly used in the art.

In the present invention, the camphortririn having a sunscreen effect is trapped in the liposomes to maximize the formulation stability on the skin surface of the sunscreen material to increase the duration of the sunscreen, carrageenan forms a coating film on the liposome surface UV by UV It provides a sunscreen cosmetic composition that maximizes the oxidative stability of the blocking material to improve the disadvantages of existing natural sunscreens.

In one aspect, the present invention comprises the steps of (a) mixing the phospholipids dissolved in a lipid solvent; (b) vacuum drying to form a phospholipid membrane; (c) adding an aqueous solution and carrageenan prepared by dissolving campertrin in a buffer to the resulting phospholipid membrane, followed by sonication to capture campertrin into liposomes; (d) washing and removing non-captured camphortrins other than liposomes; And (e) forming a film with carrageenan on the washed liposome surface to obtain a coated liposome, and to a method for producing a liposome that is trapped and coated with carrageenan.

Carrageenan (carrageenan) in the present invention is a natural polysaccharide of a polymer obtained by hot water extraction from Irish moss of red algae, the basic structure is galactose polymer, κ-carrageenan, λ-carrageenan, ι-carrageenan and roughly divided into six types. Although all consist of residues of galactose, the bond state and the number of bonds of a sulfate group differ. Carrageenan has the ability to thicken or gelate solutions even in small amounts in the water phase and is widely used as a jelly, stabilizer and dispersant for pharmaceuticals and cosmetics.

In the present invention, the phospholipid may be selected from the group consisting of phospholipid, phosphatidyl choline, lipid, lecithin and cholesterol, wherein the lipid solvent is chloroform, ether, acetone, alcohol, chloroform and It may be characterized in that it is selected from the group consisting of carbon disulfide.

In an embodiment of the present invention, the lecithin and cholesterol mixture is dissolved in chloroform, and then transferred to a vacuum vacuum flask, and vacuum reduced until the organic solvent evaporates and concentrated under reduced pressure at 40 ° C. or lower for 6 hours to thin the surface of the vacuum flask. Phospholipid membranes were formed. Thereafter, dissolve 1% of camphortrin in PBS buffer, and then add carrageenan at 0.5%, 1%, and 2%, respectively, and sonicate until the phospholipid membrane formed on the flask wall is dissolved under warming conditions. Liposome was obtained to give sample 1.

In the present invention, the carrageenan solution is added to the liposome in step (e) and vacuum reduced at 40 to 60 ° C. and 20 to 100 hPa, and the carrageenan is coated on the surface of the liposome by repeating until a solvent other than carrageenan evaporates. can do.

In another embodiment of the present invention, the obtained liposomes were washed with PBS buffer and then centrifuged to settle the liposomes for 15 minutes, and then the supernatant was removed. This washing step was repeated three times to obtain purely liposome-formulated camphortririn, and for coating of carrageenan, 0.5% carrageenan aqueous solution was added to the obtained liposome and placed in a reduced pressure flask and vacuumed to 20 hPa at 60 ° C warming conditions. The solvent was evaporated under reduced pressure to obtain camphortririn-containing liposome sample 2 having carrageenan coated on the liposome wall.

In the present invention, step (e) is to wash the liposomes with a carrageenan solution, obtain a liposome and freeze, and then wash it again with PBS buffer to obtain a liposome coated with carrageenan in a hydrogel state. can do.

In another embodiment of the present invention, the obtained liposomes were washed with PBS buffer and centrifuged to subside the liposomes, and then the supernatant was removed. This washing step was repeated three times to obtain purely liposome-formulated camphortrin, and the aqueous solution of carrageenan was added to the liposome-formulated camphortrin, followed by stirring and centrifugation for 1 minute using a voltex mixer to remove the supernatant. Liposome Sample 3 was obtained, and dried at 60 ° C or higher.

In the present invention, step (e) may be characterized by spraying the carrageenan solution to the liposome as a whole, lyophilized or dried to obtain a liposome coated in a hydrogel state.

In another embodiment of the present invention, the obtained liposomes were washed with PBS buffer and centrifuged to settle the liposomes for 15 minutes, and then the supernatant was removed. This washing step was repeated three times to obtain pure liposomes of camphoritrine. Thereafter, a 0.5% carrageenan aqueous solution was sprayed onto the prepared liposome-ized camphortririn so that the carrageenan solution was entirely buried, and then lyophilized to obtain sample 4.

In another aspect, the present invention relates to a liposome having an ultraviolet blocking function, which is prepared by the above-described method, wherein the camphortrin is collected and coated with carrageenan.

In one embodiment of the present invention, a cream containing liposomes and uncoated camphortrin and a cream containing samples 1 to 4 prepared above were analyzed and the SPF index was analyzed. The SPF index of creams containing trine was 3.2, while the SPF index of liposome-formed and creamy camphortrin-containing creams was 4.9-9.4.

In another aspect, the present invention relates to a sunscreen cosmetic composition containing the liposome as an active ingredient.

In the present invention, by liposome-forming the camphortririn having a sunscreen effect, and coating the carrageenan to increase the dispersion stability in the formulation and inhibit the skin penetration to the maximum to increase the duration of the active substance on the skin surface to increase the UV block index Organic sunscreens can be developed.

Hereinafter, the present invention will be described in more detail with reference to Examples. These examples are only for illustrating the present invention, it will be apparent to those skilled in the art that the scope of the present invention is not to be construed as limited by these examples.

Example 1 Preparation of Liposomes Containing Camparytrin

Kaempferitrin was prepared by separating and purifying kaempferitrin, an active ingredient, by ultra-high pressure salting process after extracting the leaves of ibiscus cannabinus L. using an organic solvent, and using a material having a purity of 95% or more.

0.5 g of lecithin and cholesterol mixture was dissolved in 10 ml of chloroform, and then transferred to a vacuum flask, and vacuum reduced to 20 hPa until the organic solvent evaporated, and concentrated under reduced pressure at 40 ° C. or lower for 6 hours to form a thin phospholipid on the surface of the vacuum flask. A film was formed. After dissolving 1% of camphortrin in PBS buffer, carrageenan was added at 0.5%, 1%, and 2%, respectively, and sonication was performed until the phospholipid membrane formed on the wall of the flask was dissolved under heating conditions (50 ° C). Was subjected to liposome formation of sample to obtain Sample 1.

Example 2 Preparation of Carrageenan-Coated Camperritin-Containing Liposomes by Pressure Reduction Method

The liposome obtained in Example 1 was washed with PBS buffer, and then the liposome was allowed to settle for 15 minutes at 5000 rpm (4,400 g) using a centrifuge, and then the supernatant was removed. This washing step was repeated three times to obtain pure liposomes of camphoritrine.

For the coating of carrageenan, 10 ml of 0.5% carrageenan aqueous solution was added to the obtained liposome and placed in a vacuum flask under reduced pressure to 20 hPa under 60 ° C. warming condition. Liposomal Sample 2 was obtained.

Example 3: Carrageenan-Coated Campertrins by Immersion Method for producing liposomes containing

The liposomes obtained in Example 1 were washed with PBS buffer, and then the liposomes were allowed to settle for 15 minutes at 5000 rpm (4,400 g) using a centrifuge to remove the supernatant. This washing step was repeated three times to obtain pure liposomes of camphoritrine.

5 ml of carrageenan solution was added to the liposome-formulated camphortrin, followed by stirring for 1 minute using a voltex mixer and centrifugation at 5000 rpm (4,400 g) for 15 minutes to remove the supernatant to obtain the deposited liposome sample 3, It dried at 60 degreeC or more.

Example 4 Preparation of Carrageenan Coated Camperritin-Containing Liposomes by Spray Method

The liposomes obtained in Example 1 were washed with PBS buffer, and then the liposomes were allowed to settle for 15 minutes at 5000 rpm (4,400 g) using a centrifuge to remove the supernatant. This washing step was repeated three times to obtain pure liposomes of camphoritrine.

Thereafter, 5 ml of a 0.5% carrageenan aqueous solution was sprayed onto the prepared liposome-ized camphortririn, and then the whole carrageenan solution was buried, followed by lyophilization to obtain Sample 4.

Formulation Example 1 Cream Containing Liposomalized and Uncoated Campertrin

Creams were prepared using liposomed and uncoated camphortrins (Table 1). Among the components, first, the aqueous components of the raw materials 12 to 17 shown in Table 1 were completely dissolved by heating to 80 ° C., and then the raw materials 1 to 11 of Table 1 were heated to 80 ° C., and added to the solution of the raw materials 12 to 17, followed by a homomixer. (Homo Mixer Mark, Primix, Japan) was used to emulsify at 3,000 rpm for 15 minutes. Then, the raw material 18 was thrown in, stirred for 5 minutes, and cooled to room temperature.

Ingredients of the Cream number ingredient Content in unit One Lipophilic monostearate 2.0 2 Stearic acid 1.5 3 Cetearyl Alcohol 2.2 4 Wax 1.0 5 Squalane 3.0 6 Hardened vegetable oil 1.0 7 Sorbitan stearate 0.6 8 Mineral oil 5.0 9 Polysorbate 60 1.5 10 Dimethicone 1.0 11 Trioctanoine 5.0 12 Betaine 3.0 13 Triethanolamine 1.0 14 glycerin 5.0 15 Sodium hiraruronate 3.0 16 Camperritin without liposome coating 2.0 17 Distilled water Balance 18 Preservative, fragrance, pigment a very small amount

Formulation Example 2: Cream Containing Liposomalized and Coated Campertrins

Using Sample 1 obtained in Example 1, a cream was prepared using camparytrin-containing liposomes (Table 2).

Ingredients of the Cream number ingredient Content in unit One Lipophilic monostearate 2.0 2 Stearic acid 1.5 3 Cetearyl Alcohol 2.2 4 Wax 1.0 5 Squalane 3.0 6 Hardened vegetable oil 1.0 7 Sorbitan stearate 0.6 8 Mineral oil 5.0 9 Polysorbate 60 1.5 10 Dimethicone 1.0 11 Trioctanoine 5.0 12 Betaine 3.0 13 Triethanolamine 1.0 14 glycerin 5.0 15 Sodium hiraruronate 3.0 16 Sample 1 2.0 17 Distilled water Balance 18 Preservative, fragrance, pigment a very small amount

Formulation Example 3: Cream Containing Liposomalized and Coated Campertrins

Using Sample 2 obtained in Example 2, a cream was prepared using the liposome containing carrageenan coated camphortrin as shown in the following formulation (Table 3).

Ingredients of the Cream number ingredient Content in unit One Lipophilic monostearate 2.0 2 Stearic acid 1.5 3 Cetearyl Alcohol 2.2 4 Wax 1.0 5 Squalane 3.0 6 Hardened vegetable oil 1.0 7 Sorbitan stearate 0.6 8 Mineral oil 5.0 9 Polysorbate 60 1.5 10 Dimethicone 1.0 11 Trioctanoine 5.0 12 Betaine 3.0 13 Triethanolamine 1.0 14 glycerin 5.0 15 Sodium hiraruronate 3.0 16 Sample 2 2.0 17 Distilled water Balance 18 Preservative, fragrance, pigment a very small amount

Formulation Example 4: Cream Containing Liposome and Coated Campertrin

Using Sample 3 obtained in Example 3, a cream was prepared using liposomes containing carrageenan coated camphortrin as shown in the following formulation (Table 4).

Ingredients of the Cream number ingredient Content in unit One Lipophilic monostearate 2.0 2 Stearic acid 1.5 3 Cetearyl Alcohol 2.2 4 Wax 1.0 5 Squalane 3.0 6 Hardened vegetable oil 1.0 7 Sorbitan stearate 0.6 8 Mineral oil 5.0 9 Polysorbate 60 1.5 10 Dimethicone 1.0 11 Trioctanoine 5.0 12 Betaine 3.0 13 Triethanolamine 1.0 14 glycerin 5.0 15 Sodium hiraruronate 3.0 16 Sample 3 2.0 17 Distilled water Balance 18 Preservative, fragrance, pigment a very small amount

Formulation Example 5: Cream Containing Liposomalized and Coated Campertrins

Using Sample 4 obtained in Example 4, a cream was prepared using the liposome containing carrageenan coated camphortrin as shown in the following formulation (Table 5).

Ingredients of the Cream number ingredient Content in unit One Lipophilic monostearate 2.0 2 Stearic acid 1.5 3 Cetearyl Alcohol 2.2 4 Wax 1.0 5 Squalane 3.0 6 Hardened vegetable oil 1.0 7 Sorbitan stearate 0.6 8 Mineral oil 5.0 9 Polysorbate 60 1.5 10 Dimethicone 1.0 11 Trioctanoine 5.0 12 Betaine 3.0 13 Triethanolamine 1.0 14 glycerin 5.0 15 Sodium hiraruronate 3.0 16 Sample 4 2.0 17 Distilled water Balance 18 Preservative, fragrance, pigment a very small amount

Test Example 1: TEM imaging of liposome-ized camphortririn and in vitro  SPF measurement at

TEM of Sample 1 prepared in Example 1 was taken (FIG. 1), and the UV blocking ability of Samples 1 to 4 prepared in Examples 1 to 4 was tested using an Optometrics turnkey system 290S in vitro SPF measuring apparatus. , A cream prepared using liposomes and uncoated camphortrin as a control group is shown in Formulation Example 1, and a liposomeized camphortrinin is shown as Formulation Examples 2 to 5. As a result, it was confirmed that the SPF index of the cream containing camphortririn prepared by liposomeization and coating was higher than that of the camphorritrin-containing cream without liposomeization and coating (Table 6).

SPF results of kaempferitrin Formulation Example 1 Formulation Example 2 Formulation Example 3 Formulation Example 4 Formulation Example 5 SPF Index 3.2 4.9 8.9 9.2 9.4

The specific parts of the present invention have been described in detail above, and it is apparent to those skilled in the art that such specific descriptions are merely preferred embodiments, and thus the scope of the present invention is not limited thereto. something to do. It is therefore intended that the scope of the invention be defined by the claims appended hereto and their equivalents.

Claims (8)

A method for preparing a liposome coated with carrageenan, wherein the camphoritrine is collected, comprising the following steps:
(a) mixing the phospholipids and dissolving them in a lipid solvent;
(b) vacuum drying to form a phospholipid membrane;
(c) adding an aqueous solution and carrageenan prepared by dissolving campertrin in a buffer to the resulting phospholipid membrane, followed by sonication to capture campertrin into liposomes;
(d) washing and removing the camphortrin that was not collected in the liposomes; And
(e) forming a film with carrageenan on the washed liposome surface to obtain a coated liposome.
The method of claim 1, wherein the phospholipid is at least one selected from the group consisting of phospholipid, phosphatidyl choline, lipid, lecithin and cholesterol.
The method of claim 1, wherein the lipid solvent is selected from the group consisting of chloroform, ether, acetone, alcohol, chloroform and carbon disulfide.
According to claim 1, step (e) is a carrageenan solution is added to the liposome, the vacuum pressure at 40 ~ 60 ℃, 20 ~ 100hPa and repeated until the solvent other than carrageenan evaporates to coat the carrageenan on the liposome surface How to.
The method according to claim 1, wherein step (e) washes the liposomes with a carrageenan solution, obtains and freezes the liposomes, and washes them again with PBS buffer to finally obtain liposomes coated with carrageenan in a hydrogel state. How to.
The method of claim 1, wherein step (e) comprises spraying the carrageenan solution on the liposome as a whole, and lyophilizing or drying it to obtain a liposome coated in a hydrogel state.
A liposome having an ultraviolet blocking function, which is prepared by the method of any one of claims 1 to 7, wherein camphoritrin is collected and coated with carrageenan.
A sunscreen cosmetic composition comprising the liposome of claim 7 as an active ingredient.

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