KR101000537B1 - Collagen patch base and fabrication method thereof - Google Patents

Abstract

The present invention relates to a collagen patch base and a method for preparing the same, and more specifically, a) dispersing collagen in a solvent, b) repeatedly performing a freeze-thaw method on the dispersion solution obtained above. , And c) collagen patch base prepared by the step of performing the final freeze drying and a method for producing the same.

The collagen patch base is cross-linked by repeatedly performing freeze-thaw without using a cross-linking agent that is harmful to the skin, and aids in hydrating the skin with excellent hydration properties of the collagen component, and is also stimulated by skin affinity and sensitivity. It is effective for soothing skin.

Collagen, freeze thawing, freeze drying, patch base

Description

Collagen patch base and its manufacturing method {COLLAGEN PATCH BASE AND FABRICATION METHOD THEREOF}

The present invention relates to a collagen patch base and a method for preparing the same, and more specifically, the collagen patch base is prepared by repeatedly performing a freeze-thaw method without using a crosslinking agent that is harmful to the skin. The present invention relates to a collagen patch base that helps to hydrate skin with excellent hydration properties, and is effective in calming skin irritated by skin affinity and sensitive skin, and a method of preparing the same.

Today, the cosmetics industry is developing rapidly, and the pack and mask products that can achieve more fundamental skin improvement effects after functional cosmetics are in the spotlight. With the development of technology, a disposable mask pack has been developed which is convenient to use because it does not require any complicated preparation procedure unlike existing products, and various types of packs such as whitening and wrinkle packs and sleeping packs are available depending on the function. It is appearing one after another.

The pack mask functions to keep the skin moisturized and supple due to the occlusive effect of the pack mask, which is applied to the stratum corneum of the skin simultaneously with the supply of moisture, a moisturizer and an emollient agent. At the same time, it has an excellent cleansing effect by removing contamination of the skin surface during drying and peeling.

Packs and masks have various effects, such as moisturizing, nourishing, keratin care, and skin elasticity, depending on their efficacy. Collagen is widely used due to its effects.

Collagen is a structural protein that makes up our body's matrix. In the skin, collagen is the most important component of the dermis. If collagen is oxidized, the matrix becomes less flexible and the skin becomes less elastic and wrinkles occur. The use of these collagen-based cosmetics directly increases the moisturizing effect on the skin, helping to produce new oxidized collagen. The newly created collagen drives skin elasticity to make the skin smooth and shiny.

The effect of collagen on the skin comes from the chemical structure and function of collagen. The collagen is a biological natural high molecular material, a protein of fibrous structure most present in the body of humans and mammals, long chains are formed in parallel with each other to have a strong structure.

Like all other fibrous proteins (elastin, elastin, keratin, muscle proteins), collagen is insoluble in water and performs adhesion and structural functions in living organisms. Thus, in addition to connective tissues such as tendons, ligaments, cartilage, bones and teeth, they also hold cells together as important fibrous tissues of the skin and blood vessels. After all, collagen plays a very important role in the development of embryos, organ formation, cell division and wound healing.

For example, innately lacking collagen in bones tends to weaken bones and lead to fractures (bone dysplasia). As you grow older, the amount of collagen in your skin decreases or deteriorates, causing you to lose elasticity, wrinkles and sagging.

Today, animal-derived collagen is used both as a physiologically active substance and as a carrier for the active substance, depending on the extraction and preparation method. As a bioactive substance, collagen is blended into water-soluble traditional cosmetic preparations (serums, concentrates, aftershaves, etc.) as well as formulations in gel or emulsion forms (wrinkle creams, lotions, sunscreens, various packs), and various research and development. Low-collagen support or delivery system functions shine.

The technology for producing or applying cosmetic collagen is already well known all over the world.

However, the present invention is to propose an insoluble collagen patch base that does not dissolve in water, but is not immersed in a solution state in the collagen or non-woven fabric dissolved in water.

The insoluble collagen patch base is derived from the field of medicine used as a cell support, not from the cosmetic field, and related papers are published in a medical journal, and are applied as a collagen wound coating agent and a collagen hemostatic band.

US Patent Application No. 1982-382133 mentions that collagen can be prepared into a suspension of an aqueous organic acid solution and then lyophilized to obtain a porous natural collagen sheet.

Korean Patent Laid-Open No. 2000-0007983 proposes to obtain a biological tissue including an enhanced collagen layer by applying acid treatment for crosslinking of collagen and to apply it to artificial skin.

However, unlike the collagen cell support, which is easily released in water and easily decomposed in the body, collagen pack manufacturing technology, which needs to be stronger in water, is an upgraded technology and requires a long time of know-how and technology accumulation.

Conventionally, physical and chemical methods are used for crosslinking collagen. Physical crosslinking is accomplished by heat drying at about 100 ° C. under vacuum or by UV irradiation. Chemical crosslinking is also effected by acid treatment or by using a crosslinking agent such as glutaraldehyde, diphenylphosphoryl azide, hexamethylene isocyanate, succinimide or carbodiimide.

Such physical crosslinking and chemical crosslinking increase the tensile strength of biological tissues, but they are likely to cure the biological tissues, and the burden of toxic effects on cells and tissues in vivo is unknown although the exact mechanism is not known. It is not preferable because it is holding.

Japanese Patent Application No. 1982-382133 uses fish skin dermis collagen as a raw material and expands it in an acidic aqueous solution, and then prepares a foam sheet through freeze drying and crosslinking to protect wounds such as skin care masks, partial pack materials, and emergency band aids. It is mentioned that ash and hemostatic sheet can be produced.

In addition, Japanese Patent Application No. 2003-001335 discloses physically homogeneous dispersion of collagen-containing tissues and chemical reduction of unsaturated bonds in order to avoid the use of additional drugs or crosslinking agents. A facial mask is manufactured.

This method has the advantage of not using chemicals or crosslinking agents for crosslinking, but uses sodium borohydride to reduce unsaturated bonds, salt and hydrochloric acid to adjust pH, and Chloroform is used as a solvent. If such hydrochloric acid or organic solvent is not sufficiently removed through freeze-drying, it may remain in the facial mask and cause toxicity to the skin.

It is an object of the present invention to provide a method for producing a collagen patch base that performs a crosslinking reaction without using a crosslinking agent that is harmful to skin.

Another object of the present invention is to provide a collagen patch base which is prepared by the above production method to help hydrate skin with excellent hydration properties of collagen ingredients, and also effective in calming skin, sensitive skin stimulated by skin affinity. will be.

The present invention to prepare a collagen patch base,

a) dispersing collagen in a solvent,

b) repeating the freeze-thaw method on the dispersion solution obtained above, and

c) performing lyophilization

It provides a method for producing a collagen patch base comprising a.

The present invention also provides a collagen patch base prepared by the above method.

The collagen patch base prepared according to the present invention is a patch base consisting of pure collagen by performing a crosslinking reaction of collagen without using a separate crosslinking agent. The collagen patch base helps to hydrate the skin with excellent hydration properties of collagen, and is also effective in soothing skin-sensitive skin and sensitive skin, purifying skin tone and promoting new collagen fiber formation. It is effective in alleviating wrinkles.

In the preparation of the collagen patch base according to the present invention, the crosslinking is performed by repeatedly performing the freeze-thaw method without using a chemical agent such as a crosslinking agent for crosslinking of the conventional collagen, thereby providing a patch base composed of pure collagen only. Manufacturing is possible.

First, in step a), collagen used as a raw material is dispersed in a solvent.

As the collagen raw material, it is used by treating collagen directly derived from animals and plants, or using commercially available collagen.

The collagen used in the present invention is not limited by the origin thereof, and collagen of all living species such as mammals, birds and fish can also be used. In addition, collagen produced by cells such as bacteria, fungi, and yeasts can also be used. If it is collagen derived from an organism, it is a mammalian thing, and cell types, such as a bacterium, mold, and yeast, may be collagen derived from the recombinant which manipulated the gene. The chemical structure of collagen is also not particularly limited, and acid soluble collagen, neutral salt soluble collagen, enzyme soluble collagen, alkali solubilized collagen and the like can be used. In this case, any amino acid sequence represented by teropeptide or the like in collagen or saccharides bound to collagen may be removed depending on the purpose of use, and atelocollagen or the like is preferably used.

Preferably, the bovine dermis is pulverized, and then fat is removed, and the one prepared by washing, stirring, centrifugation and concentration is used.

The solvent includes water; Lower alcohols such as methanol, ethanol, propanol and butanol; And a mixed solvent thereof. Preferably, water or a water / ethanol mixed solvent that is harmless to the skin is used.

The solvent is used in an amount that can be sufficiently immersed and dispersed in collagen, and 50 to 1000 g of solvent is used for 1 g of collagen.

At this time, in addition to collagen, various plant, fruit or seaweed extracts are added as necessary. The extract is commonly used in the cosmetic composition, the effect of which is recognized and non-toxic, any one is possible, for example, ginkgo biloba, aloe, green tea, cucumber, tomato, olive, eucalyptus, lavender, rosemary, oatmeal, eochocho , Algae, oranges, and kiwis are available.

Next, in step b), the freeze-thaw method of the dispersion solution prepared in the step is repeatedly performed.

The freeze-thaw method freezes the collagen below the freezing point and then thaws it above the freezing point. The freeze-thaw method causes hydrogen bonds between amino acids present in the collagen structure so that a separate crosslinking agent is not added. The degree of crosslinking of collagen can be increased.

In other words, one molecule of collagen has a triple-helical structure in which three long threads, called α-chains, are twisted together, and one α-chain consists of more than 1,000 amino acids (-NH ₂ ). . That is, one collagen molecule contains more than 1,000 amino acids.

In this case, the collagen molecules are aligned with a predetermined direction through freezing, and the aligned collagen molecules are released by thawing, and the amino acid functional groups in the collagen molecule are brought closer to each other, thereby causing crosslinking between the molecules of collagen. .

The degree of crosslinking of the collagen increases with several freeze-thaw methods, and this increase in the degree of crosslinking results in an increase in the strength of the patch base. Therefore, the freeze-thaw method of step b) is performed at least once, preferably 2 to 10 times, more preferably 3 to 5 times, in consideration of the economical aspect of the patch base with appropriate strength.

The freeze-thaw method is performed by freezing the dispersion solution obtained in step a) at -50 to -25 ° C and then thawing at 25 to 45 ° C.

Next, in step c), the collagen crosslinked through the freeze-thaw method is lyophilized to prepare a collagen patch base.

The solvent present in the collagen is sublimated into gaseous vapor through the lyophilization and freeze-drying, so that pores are formed at the position at which the solvent escapes, thereby obtaining light sponge or foam collagen. In addition, since the solvent is removed through lyophilization, physical and chemical changes of the collagen properties are extremely small, and shrinkage and drying of the collagen are hardly generated. In addition, the natural tissue structure of collagen is not destroyed and exists in a porous state.

This freeze drying is performed by leaving the collagen for 1 to 72 hours at -55 to -25 ° C under a pressure of 0.01 to 0.5 Torr. The freeze-drying conditions have a great effect on the quality of the collagen patch base, so close attention is required for its control. Typically, when the freeze-drying speed is high, the diameter of the pores formed in the collagen patch base is reduced, so the cooling treatment conditions are carefully controlled.

The collagen patch base prepared by the above method is obtained in the form of a sponge having a pore and flexibility. Such collagen patch base may be molded into a sheet shape or molded according to the shape of the site used for ease of use.

The average pore diameter of the collagen patch base is 0.3-100 탆, preferably 1-50 탆, and the bulk density is 0.05-1.0 g / cm 3, preferably 0.07-0.5 g / cm 3.

The thickness of such a collagen patch base is 0.01-3.0 mm, preferably 0.05-2.5 mm, in order to enhance the delivery effect of moisture or nutrient components. If the thickness of the patch base is larger than the range, it is difficult to fix the skin, and it is difficult to cover the entire skin. On the contrary, if the patch base is smaller than the range, the mechanical strength is weakened.

The collagen patch base prepared by the present invention has a good moisture content in the form of a sponge or a foam in which a plurality of pores exist, thereby sufficiently supplying moisture into the skin.

Referring to Experimental Example 2 of the present invention, the collagen patch base has a swelling strength of 100 to 200 KPa and a dry strength of 50 to 80 KPa, thereby having excellent mechanical properties. In addition, there is flexibility, and when it adheres to the face or the like, it can be partially stretched and brought into close contact with each other. As a result, the adhesion to the face is further improved.

The collagen patch base is attached to the face, and then massaged several times after contacting the face with air using a sponge or both hands using distilled water, bottled water, or skin.

As a result, it absorbs moisture through the pores in the collagen patch base and swells again upon rehydration. These excellent hydration properties help to supply moisture to the skin, and are also effective in calming the skin and irritated skin, which are stimulated by skin affinity, and specifically have the following effects.

1) Increases firming and maintains moist skin by moisturizing effect of collagen ingredients

2) Collagen ingredients help nourish the skin and help antioxidant and skin vitality

3) Excellent skin affinity helps calm irritated and sensitive skin

4) Helps to cleanse skin tone

5) Restore skin moisture balance

6) active collagen fiber protection

7) Promote new collagen fiber formation

8) Moisturizes deeply into skin, relieves elasticity and wrinkles

Hereinafter, preferred embodiments of the present invention will be described in order to facilitate understanding of the present invention. However, the following examples are merely provided to more easily understand the present invention, and the contents of the present invention are not limited by the examples.

Example  One

500 ml of water was added to a reactor maintained at 25 ° C., and 1 g of commercial collagen was added thereto and stirred for 5 hours to disperse collagen to prepare a dispersion solution.

The dispersion solution was poured into a square plate, placed in a freezer at -40 ° C, frozen, and thawed at room temperature (25 ° C). This freeze-thaw method was repeated five times.

After performing the freeze-thaw method, it was placed in a freeze dryer and freeze-dried at −40 ° C. for 1 hour to prepare a collagen patch base in sheet form.

Comparative Example 1

500 ml of water was added to a reactor maintained at 25 ° C., and 1 g of commercial collagen was added thereto and stirred for 5 hours to sufficiently swell the collagen.

In order to crosslink the swelled collagen solution, a polyepoxy compound DENACOL ^™ EX-512 (Nagase Chemical Company, Japan) was added at a concentration of 1% and stirred for about 12 hours for crosslinking.

The crosslinked collagen solution was poured into a square plate, and then freeze-dried at -40 ° C for 7 hours to completely remove the solvent to prepare a collagen patch base in the form of a sheet.

Experimental Example 1: Confirmation of Structure

In order to confirm the structure of the collagen patch base prepared in Example 1 and Comparative Example 1 was measured by a scanning electron microscope.

1 is a scanning electron micrograph of the collagen patch base prepared in Example 1, Figure 2 is a scanning electron micrograph of the collagen patch base prepared in Comparative Example 1.

1 and 2, it can be seen that the collagen patch bases prepared in Example 1 and Comparative Example 1 have a sponge-like sponge form.

Experimental Example 2: Measurement of Physical Properties

In order to investigate the mechanical strength of the collagen patch base according to the number of execution of the freeze-thaw method with the preparation method of Example 1, tensile strength and elongation at swelling and drying were measured.

The thickness of the specimen cut into 3 cm × 1 cm of the collagen patch base was measured, and the cross-sectional area was calculated by multiplying the thickness and the width. Both ends of the specimen were fixed, and the specimen was stretched at room temperature at a rate of 0.5 mm / s using a tensioner, and the tensile strength and the maximum elongation at the fracture point were calculated, and the results obtained are shown in Table 1 below.

division Tensile Strength (KPa) Elongation (%) Example 1 Swelling 120 ± 11 18.2 ± 0.6 When drying  60 ± 1 34.0 ± 1.4 Comparative Example 1 Swelling 140 ± 12 22.7 ± 0.8 When drying  80 ± 2 39.1 ± 1.5

Experimental Example  3: Moisturizing  Measure

Apply the collagen patch bases of Example 1 and Comparative Example 1 to the skin of 20 female subjects, soak them in water and leave them for 20 minutes, and then use the moisture gauge (Corneometer CM820) at 25 ° C for 35% relative humidity. It was. At this time, the massage sheet containing the collagen essence sold in Comparative Example 2 was purchased and used, and the relative value was measured by setting the moisture level to 100 before use.

division Before use After use (relative value) Example 1 100 134 Comparative Example 1 100 128 Comparative Example 2 100 124

Referring to Table 2, it can be seen that the collagen patch base of Example 1 supplies deeper skin than Comparative Example 1 and Comparative Example 2.

Moreover, the collagen patch base of Example 1 does not use any crosslinking agent, and has the advantage of low irritation to the skin, compared to Comparative Example 1 using a crosslinking agent.

Collagen patch base according to the invention can be used as a cosmetic for skin massage.

1 is a scanning electron micrograph of the collagen patch base prepared in Example 1.

Figure 2 is a scanning electron micrograph of the collagen patch base prepared in Comparative Example 1.

Claims (8)

a) dispersing with 50-1000 g of water per 1 g of collagen, b) repeating the freeze-thaw process of freezing the obtained dispersion solution at -50 to -25 ° C, thawing at 25 to 45 ° C 3 to 5 times, and c) a method of preparing a collagen patch base satisfying the following physical properties by performing freeze drying for 1 to 72 hours under a pressure of -55 to -25 ° C and 0.01 to 0.5 Torr: Pore size: 0.3-100 ㎛ Bulk density: 0.05 to 1.0 g / cm 3 Thickness: 0.01 ~ 3.0mm Swelling Strength: 100-200 KPa Drying Strength: 50 ~ 80KPa delete delete delete delete delete delete delete

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