KR102130319B1 - Method for preparing micro fiber using nature-derived polysaccharide and cosmetic composition comprising micro fiber prepared therefrom - Google Patents

Abstract

The present invention relates to a method for producing microfibers using natural-derived polysaccharides, and more specifically, i) dissolving natural-derived polysaccharides in a solvent, and ii) injecting the natural-derived polysaccharide solution obtained in step (i) into a syringe. And iii) connecting the syringe infused with the naturally-derived polysaccharide solution to the pump, then stirring the coagulation solvent to flow the naturally-derived polysaccharide solution to make microfibers, and iv) drying the microfibers obtained in step (iii) above. It is related with the manufacturing method of the microfiber containing.
In addition, the present invention relates to a cosmetic composition comprising microfibers produced by the above method.

Description

Method for manufacturing microfibers using natural derived polysaccharides and cosmetic composition comprising microfibers produced thereby{METHOD FOR PREPARING MICRO FIBER USING NATURE-DERIVED POLYSACCHARIDE AND COSMETIC COMPOSITION COMPRISING MICRO FIBER PREPARED THEREFROM}

The present invention relates to a method for producing microfibers using natural-derived polysaccharides, and more specifically, i) dissolving natural-derived polysaccharides in a solvent, and ii) injecting the natural-derived polysaccharide solution obtained in step (i) into a syringe. And iii) connecting a syringe infused with a natural-derived polysaccharide solution to a pump, and then stirring the coagulation solvent to flow the natural-derived polysaccharide solution to make microfibers, and iv) drying the microfibers obtained in step (iii) above. It is related with the manufacturing method of the microfiber containing.

In addition, the present invention relates to a cosmetic composition comprising microfibers produced by the above method.

Fiber is basically a material that looks like an elongated thread. Fabric fibers, natural fibers, and synthetic fibers are largely present. Fabric fibers are fabrics for elongated linear materials that have some strength and flexibility. Natural fiber refers to fibers obtained from natural organisms and minerals, also called natural fibers, and refers to fibers made of natural materials. Synthetic fibers are polymer materials made of fibers by chemically synthesizing a series of long molecules that form fibers using petroleum, coal, air, and water as starting materials. Among them, natural and synthetic fibers are widely used in the medical and cosmetic industries. As materials used for medical purposes, catgut, polyglycolic acid, polydioxanone, silk, polyester, polypropylene, polyamide, and the like are made of yarn. Most of these threads are used for lifting procedures to remove sutures or wrinkles during surgery.

In the cosmetic industry, cosmetics are manufactured using polysaccharides. Polysaccharide refers to a saccharide composed of two or more monosaccharides that form a molecule through a glycosidic bond. The molecular weight varies from thousands to millions. These include hypotonic polysaccharides such as starch and glycogen, and structural polysaccharides such as cellulose and chitin. In addition, pullulan, hyaluronic acid, etc. are also included in the polysaccharide as natural ingredients. Polysaccharides as natural-derived ingredients have adhesive strength and viscosity, and can be applied to skin care, hair care, cleansing products, etc. as a stabilizer, and can be applied to various emulsion products such as body products due to their excellent feeling of use. As an example of a cosmetic using polysaccharides, Korean Patent Publication No. 10-2014-0091449 discloses a face mask having a collagen-containing nanofiber layer. In addition, natural-derived polysaccharides have been applied to the pharmaceutical industry due to their ability to form a film and adhesion. It is used in many formulations to improve the shape or stability of the drug by adding sugar-coated tablets or powders.

From the 21st century onwards, not only women but also men are interested in skin beauty, and people undergoing treatment and people seeking functional cosmetics are rapidly increasing. Accordingly, many functional cosmetics have been developed, and the number of people visiting the hospital for skin treatment is increasing. Lifting procedure for wrinkle improvement is a procedure that inserts into the skin using a thread that has excellent biocompatibility. Thread lifting is a procedure that shortly inserts a thread into the subcutaneous layer to promote collagen production and elasticity to the skin, and a thread that pulls sagging facial flesh. It is divided into a procedure to insert a long. Mainly, polydioxanone is used to lift the thread, which promotes collagen production in the dermal layer as the wound caused by thread insertion heals itself, and the principle of spreading skin wrinkles as cells are regenerated around the injected thread. All. However, polydioxanone is a synthetic polymer, and has excellent biocompatibility, which may cause side effects. Recently, cosmetics were developed by focusing on lifting procedures using a melting thread. This is a cosmetic made by dissolving a thread made of a natural ingredient in a functional ampoule to be used.It is a technology in which the thread is dissolved in an ampoule to reverse the formulation, and the ampoule with a whitening and wrinkle improvement function turns into a gel mask to help absorption into the skin. , It is a cosmetic that simultaneously improves skin brightness, moisture, keratin, and elasticity. However, the yarns currently being used are synthetic polymers or yarns derived from natural ingredients, but synthetic polymers require synthetic steps, which increases the cost and does not have better biocompatibility than natural derived ingredients, which can cause side effects. In addition, yarns made of natural-derived ingredients have excellent biocompatibility, but there are disadvantages of high cost of materials.

Republic of Korea Patent Publication No. 10-2014-0091449

Accordingly, the present invention is to provide a method capable of manufacturing microfibers at a low cost through a relatively simple manufacturing process using natural derived polysaccharides having excellent biocompatibility.

In addition, another object of the present invention is to provide a cosmetic composition comprising microfibers produced by the above method.

The present invention to solve the above problems,

i) naturally occurring polysaccharides are dissolved in a solvent;

ii) the natural-derived polysaccharide solution obtained in step (i) is injected into a syringe;

iii) connect the syringe infused with the naturally-derived polysaccharide solution to the pump, then stir the coagulation solvent and flow the naturally-derived polysaccharide solution to make microfibers;

iv) A method for producing a microfiber comprising drying the microfiber obtained in the step (iii).

In addition, in order to achieve the above another object, the present invention provides a cosmetic (cosmetic) composition comprising a micro fiber produced by the method.

Hereinafter, the present invention will be described in detail.

In the present invention, i) a naturally occurring polysaccharide is dissolved in a solvent; ii) the natural-derived polysaccharide solution obtained in step (i) is injected into a syringe; iii) connect the syringe infused with the naturally-derived polysaccharide solution to the pump, then stir the coagulation solvent and flow the naturally-derived polysaccharide solution to make microfibers; iv) A method for producing a microfiber comprising drying the microfiber obtained in the step (iii).

In step (i) of the method for producing microfibers according to the present invention, the naturally occurring polysaccharide is dissolved in a solvent.

Examples of the naturally occurring polysaccharide that can be used in the present invention include, but are not limited to, pullulan, cellulose, hyaluronic acid, inulin, dextrin, starch, chitin, chitosan, chondroitin sulfate, collagen, proteoglycan, and mixtures thereof. In the present invention, the naturally-derived polysaccharide is preferably dissolved in a solvent at a concentration of 5 to 20% by weight, more preferably 6 to 18% by weight, and more preferably 7 to 15% by weight. When the naturally-derived polysaccharide is dissolved in a solvent of less than 5% by weight or more than 20% by weight, there may be a problem in formation of microfibers. Examples of the solvent in the present invention include, but are not limited to, water, formamide, dimethyl sulfoxide, acetic acid and mixtures thereof.

In one embodiment of the present invention, in step (i), in addition to the naturally occurring polysaccharide, layered double hydroxide (LDH) is dissolved in a solvent together. LDH is a biomaterial adsorption material, and the composition is represented by the structural formula of [M ²⁺ _1-x M ³⁺ _x (OH) ₂ ] ^x+ (A ^n- ) _x/n · mH ₂ O. In the above structural formula, M ²⁺ and M ³⁺ are metal cations, and A ^n- represents an anion located between layers, and M ²⁺ = Ca ^{2 +} , Mg ^{2 +} , Mn ^{2 +} , Fe ^{2 +} , Co ^{2 +,} Zn ^{2 +} or the like, such as a ^{M 3+ = Al 3 +, Fe} 3 +, Ti 3+, a n- is Cl ^- or the _{^{like, CO 3 2-, SO 4 2-}} , -, Br -, NO 3 In the fixed composition state, 0.2≦x≦0.33, and m is generally 0.5-4. The anions located between the layers of the LDH structure can be easily replaced, so that not only biopolymers having a negative charge such as DNA from halogen ions, but also biomaterials such as collagen tripeptides and solid nanoparticles containing Ag, Au, Pt, etc. are intercalated. It can be intercalated. When LDH is additionally dissolved in a solvent together with a naturally-derived polysaccharide to produce microfibers, LDH is adsorbed onto the surface of the fibers to provide efficacy according to various intercalated materials. LDH in the present invention is preferably dissolved in a solvent at a concentration of 30 to 60% by weight.

In the step (ii) of the method for producing a microfiber according to the present invention, the natural-derived polysaccharide solution obtained in the step (i) is injected into a syringe. The syringe that can be used in this step is not particularly limited as long as there is no problem in compatibility with the naturally-derived polysaccharide solution.

In the step (iii) of the method for manufacturing microfibers according to the present invention, a syringe in which a natural polysaccharide solution is injected is connected to a pump, and then a coagulation solvent is stirred while flowing a natural derived polysaccharide solution to make microfibers.

Examples of the coagulant in the present invention include ethanol, methanol, acetone, tetrahydrofuran, dichloromethane, and mixtures thereof, but are not limited thereto. In the present invention, the concentration of the coagulation solvent can be used in various ranges of 1 to 100% by volume. The stirring speed of the coagulation solvent in the present invention is preferably 2 to 20 rpm, more preferably 3 to 15 rpm, and more preferably 3 to 12 rpm. If the stirring speed of the coagulation solvent is less than 2 rpm, the fiber shape may not be properly formed, and natural-derived polysaccharides may be entangled with each other. If the stirring speed exceeds 20 rpm, the natural-derived polysaccharide may break before solidification to form a fiber. . In the present invention, the rate of flowing the naturally-derived polysaccharide solution into the coagulant solvent is preferably 0.3 to 100 μl/min, more preferably 0.5 to 80 μl/min, and more preferably 0.7 to 50 μl/min. In the present invention, if the rate at which the naturally-derived polysaccharide solution flows into the coagulant is less than 0.3 μl/min or exceeds 100 μl/min, there may be a problem in the formation of the fiber shape.

In step (iv) of the method for manufacturing a microfiber according to the present invention, the microfiber obtained in step (iii) is dried. Drying of the microfiber can be performed by various methods known in the art, for example, drying at room temperature or vacuum drying.

According to one aspect of the invention, the diameter of the produced microfibers is less than 1 mm. According to another aspect of the present invention, various cosmetic cosmetic ingredients (whitening, wrinkles, moisturizing, sunscreen, etc.) or various bio encapsulations (eg, liposomes, nanoemulsions, nanoporous) on microfibers Substances, etc.).

In addition, the present invention provides a cosmetic composition comprising microfibers prepared according to the above method.

In the present invention, the cosmetic composition may be formulated into various products such as lotion, emulsion, body lotion, cream, essence, ampoule, BB cream, and hydrogel patch, but is not limited thereto. In the present invention, the cosmetic composition may include various amounts of microfibers depending on formulation needs, and for example, may include microfibers in an amount of 0.02 to 40% by weight.

The present invention is excellent in biocompatibility and can produce microfibers at low cost using natural derived polysaccharides that can reduce side effects on the human body, and the microfibers produced according to the present invention are excellent in coatability, adhesion, and moisture retention. It can be applied to various fields, and in particular, it can provide excellent skin improvement efficacy according to natural derived polysaccharides when used in cosmetic compositions.

1 is a schematic view of a micro fiber manufacturing apparatus.
Figure 2 is a photograph taken with a scanning electron microscope (HITACHI S-4800, Japan) coated with platinum for 45 seconds microfiber prepared using pullulan and collagen in Example 1.
FIG. 3 is a photograph of a microfiber prepared using cellulose and hyaluronic acid in Example 2, taken with a scanning electron microscope.
Figure 4 is a photograph taken with a scanning electron microscope microfibers prepared using inulin and dextrin in Example 3.
FIG. 5 is a photograph of microfibers prepared using starch and chitin in Example 4, taken with a scanning electron microscope.
FIG. 6 is a photograph of a microfiber prepared using chitosan and chondroitin sulfate in Example 5, taken with a scanning electron microscope.
FIG. 7 is a photograph of a microfiber manufactured using collagen and proteoglycan in Example 6 with a scanning electron microscope.
FIG. 8 is a photograph obtained by scanning electron microscopy of microfibers prepared using natural-derived polysaccharides of pullulan and collagen and retinol-gold-containing LDH in Example 7.
9 is a photograph of a cross section of the microfiber prepared in Example 7 taken with a scanning microscope.
10 is a graph showing the results of measuring skin transdermal moisture loss (TEWL) with TEWAMETER TM 250.
11 is a graph showing the results of measuring the moisturizing power using Corneometer CM 850.

Hereinafter, the present invention will be described in more detail through examples. However, the following examples are only illustrative to aid the understanding of the present invention, and the scope of the present invention is not limited thereby.

Example One: Pullulan And production of microfibers using collagen

0.5 g pullulan and 0.5 g collagen were added to 10 ml of water to dissolve completely. After inserting the prepared pullulan solution into a 20 ml syringe, a rubber tube with a diameter of 0.3 mm was connected to the tip of the syringe needle. The syringe was connected to the pump. The 1 liter beaker contained 1 liter of ethanol as a coagulant, and the rubber tube at the tip of the syringe needle connected to the pump was immersed in the coagulant. A stirrer was installed in the beaker and stirred at a speed of 4 to 5 rpm. The syringe pump was turned on in this state to allow the pullulan solution to flow into the beaker. The speed of the syringe pump was 5 μl/min. The produced microfibers were collected and then vacuum dried.

Example 2: Preparation of microfibers using cellulose and hyaluronic acid

Microfibers were prepared in the same manner as in Example 1, except that 0.5 g of cellulose and 0.5 g of hyaluronic acid were used as the naturally occurring polysaccharide, and a mixed solvent of ethanol and acetone was used as a coagulant.

Example 3: Preparation of microfibers using inulin and dextrin

In the same manner as in Example 1, except that 0.5 g of inulin and 0.5 g of dextrin were used as a polysaccharide derived from nature, a mixed solvent of ethanol and tetrahydrofuran was used as a coagulant, and the pumping speed was 10 μl/min. Microfibers were prepared.

Example 4: Preparation of microfibers using starch and chitin

As a natural-derived polysaccharide, 0.5 g of starch and 0.5 g of chitin were used, a mixed solvent of methanol and dichloromethane was used as a coagulant, and the microparticles were prepared in the same manner as in Example 1, except that the pumping speed was 1 µl/min. Fibers were prepared.

Example 5: Preparation of microfibers using chitosan and chondroitin sulfate

Microfibers were prepared in the same manner as in Example 1, except that 0.5 g of chitosan and 0.5 g of chondroitin sulfate were used as the naturally occurring polysaccharide, and a mixed solvent of methanol and acetone was used as a coagulant.

Example 6: Preparation of microfibers using collagen and proteoglycan

In the same manner as in Example 1, except that 0.5 g of collagen and 0.5 g of proteoglycan were used as a natural polysaccharide, and a mixed solvent of acetone and tetrahydrofuran was used as a coagulant, and the pumping speed was 10 μl/min. Microfibers were prepared.

Example 7: Pullulan Containing collagen and retinol-gold LDH Preparation of used microfiber

Mg(NO ₃ ) ₂ , Al(NO ₃ ) ₃ [Mg ₄ Al ₂ (OH) ₁₂ ]CO ₃ ·nH ₂ O layered double hydroxide (LDH) containing carbonate ion (carbonate) , Na ₂ CO ₃ , NaOH and the like were synthesized by co-precipitation. Crystallized LDH nanoparticles were prepared by hydrothermal treatment of the synthesized LDH. The LDH thin film was prepared by placing the washed silicon substrate (100 crystal faces) in a 20 ml 1-butanol solution in which 10 mg of LDH nanoparticles were dispersed and sonicating for about 10 minutes. The following solvent heat (solvothermal) method was used to prepare the retinol-gold-containing LDH thin film. LDH containing 10 mg of retinol-gold, 18 ml of toluene, and 0.5 ml of ethanol were placed in a hydrothermal container with a capacity of 25 ml coated with Teflon, and reacted at 120°C for 48 hours. After completion of the reaction, the LDH thin film containing retinol-gold was washed with ethanol and dried in air.

10 g of retinol-gold containing LDH and 1 g of pullulan were dissolved in 10 ml of water to dissolve completely. After inserting the prepared solution into a 20 ml syringe, a rubber tube with a diameter of 0.3 mm was connected to the tip of the syringe needle. The syringe was connected to the pump. A 1 liter beaker contains 1 liter of methanol as a coagulant, and the rubber tube at the tip of the syringe needle connected to the pump is immersed in the coagulant. The beaker was installed with a stirrer and stirred at 4-5 rpm. The syringe pump was turned on in this state so that a solution of retinol-gold containing LDH and pullulan flowed into the beaker. The speed of the syringe pump was 5 μl/min. The produced microfibers were collected and then vacuum dried.

Example 8 and Comparative Example 1: Preparation of micro-fiber-containing and cosmetic-free lotion

100 g of the microfiber obtained in Example 1 was added to 900 g of water, then dispersed for 5 minutes at a speed of 3,000 rpm with a laboratory mixer, filtered through a 50 mesh stainless metal mesh, and filtered to about 1% by weight. A micro fiber solution was obtained.

Each component was introduced into a container in the composition shown in Table 1 below, dissolved at a temperature of 80° C., and then mixed and cooled for 5 minutes using a homo mixer to defoam and obtain microfiber-containing and non-containing cosmetic water, respectively.

Example 9: Preparation of microfiber containing emulsion

100 g of the microfiber obtained in Example 1 was added to 900 g of water, and then dispersed for 5 minutes at a speed of 3,000 rpm with a vorette repertoire mixer, filtered through a 50 mesh stainless metal mesh, and a microfiber solution of about 1% by weight Got

Each component was introduced into a container in the composition shown in Table 2 below, dissolved at a temperature of 80° C., and then mixed and cooled for 5 minutes using a homo mixer to defoam to obtain an emulsion.

Example 10: Preparation of body lotion containing microfibers

100 g of the microfiber obtained in Example 1 was added to 900 g of water, and then dispersed for 5 minutes at a speed of 3,000 rpm with a vorette repertoire mixer, filtered through a 50 mesh stainless metal mesh, and a microfiber solution of about 1% by weight Got

Each component was introduced into a container with the composition shown in Table 3 below, dissolved at a temperature of 80° C., and then mixed and cooled for 5 minutes using a homo mixer to defoam to obtain a body lotion.

Example 11: Preparation of microfiber containing cream

100 g of the microfiber obtained in Example 1 was added to 900 g of water, and then dispersed for 5 minutes at a speed of 3,000 rpm with a vorette repertoire mixer, filtered through a 50 mesh stainless metal mesh, and a microfiber solution of about 1% by weight Got

Each component was introduced into a container with the composition shown in Table 4 below, dissolved at a temperature of 80° C., and then mixed and cooled for 5 minutes using a homo mixer to defoam to obtain a cream.

Example 12: Preparation of micro fiber containing essence

100 g of the microfiber obtained in Example 1 was added to 900 g of water, and then dispersed for 5 minutes at a speed of 3,000 rpm with a vorette repertoire mixer, filtered through a 50 mesh stainless metal mesh, and a microfiber solution of about 1% by weight Got

Each component was introduced into a container with the composition shown in Table 5 below, dissolved at a temperature of 80° C., and then mixed and cooled for 5 minutes using a homo mixer to defoam to obtain an essence.

Example 13: Preparation of micro fiber ampoules

2 g of the microfiber obtained in Example 1 was placed in a sealed container with a lid, and each component was added to the glass bottle container in the composition shown in Table 6 below. Was made possible.

Example 14: contains microfiber BB Cream (Foundation) Produce

100 g of the microfiber obtained in Example 1 was added to 900 g of water, and then dispersed for 5 minutes at a speed of 3,000 rpm with a vorette repertoire mixer, filtered through a 50 mesh stainless metal mesh, and a microfiber solution of about 1% by weight Got

Each component was introduced into a container in the composition shown in Table 7 below, dissolved at a temperature of 80° C., and then mixed and cooled for 5 minutes using a homo mixer to defoam to obtain a BB cream (foundation).

Example 15: Preparation of microfiber containing hydrogel patch

After making a hydrogel with the composition of Table 8, 3 g of microfibers were added as a matrix.

Experimental Example One: Transdermal moisture Loss ( TEWL ) Measure

After applying the lotion of Example 8 and Comparative Example 1 using TEWAMETER TM 250 (Courage + Khazaka electronic GmbH, Germany), the skin epidermal water loss (TEWL) was measured and the results are shown in FIG. 10. Shown. As can be seen from Figure 10, it was found that the moisturizing power is superior to that of the lotion containing no microfiber.

Experimental Example 2: Measurement of skin moisturizing power

After applying the lotion of Example 8 and Comparative Example 1 with Corneometer CM850 (Courage + Khazaka electronic GmbH, Germany), the moisturizing power was measured and the results are shown in FIG. 11. As can be seen from FIG. 11, it was found that the moisturizing power was superior to that of the lotion containing no microfiber.

Claims (14)

i) 5-20% by weight of naturally occurring polysaccharide, a mixture of pullulan and collagen, dissolved in a solvent selected from the group consisting of water, formamide, dimethylsulfoxide, acetic acid and mixtures thereof;
ii) the natural-derived polysaccharide solution obtained in step (i) is injected into a syringe;
iii) A syringe infused with a naturally-derived polysaccharide solution is connected to a pump, and then a coagulation solvent selected from the group consisting of ethanol, methanol, acetone, tetrahydrofuran, dichloromethane and mixtures thereof is stirred at a rate of 3 to 15 rpm and natural The resulting polysaccharide solution was flowed at a rate of 0.5 to 80 μl/min to make microfibers;
iv) A method for producing microfibers, comprising drying the microfibers obtained in step (iii). delete delete delete The method of claim 1, wherein in step (i), the layered double hydroxide is further dissolved in a solvent. The method of claim 5, wherein the layered double hydroxide is dissolved in a solvent at 30 to 60% by weight. delete The method of claim 1, wherein the concentration of the coagulation solvent is 1 to 100 volumes (v/v)%. delete delete The method of claim 1, wherein the drying in step (iv) is drying at room temperature or vacuum drying. The method of claim 1, wherein the manufactured microfiber has a diameter of less than 1 mm. A cosmetic composition comprising microfibers produced by the method of any one of claims 1, 5, 6, 8, 11 and 12. The cosmetic composition according to claim 13, comprising 0.02 to 40% by weight of microfibers.

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