KR102544469B1 - Cosmetic Additives Composition and Manufacturing Method of the Same - Google Patents

Abstract

The present invention relates to a cosmetic additive composition and a manufacturing method thereof, and more specifically, to a cosmetic additive composition containing glycoside derivatives, xylose, polyol and anhydro polyol, and a manufacturing method thereof. According to the production method of the present invention, the additive composition containing the functional glycoside derivatives with high efficiency can be easily manufactured and can be used in a variety of cosmetic formulations without restrictions.

Description

Cosmetic additive composition and manufacturing method {Cosmetic Additives Composition and Manufacturing Method of the Same}

The present invention relates to a cosmetic additive composition and a manufacturing method thereof, and more particularly, to a cosmetic additive composition comprising a glycoside derivative, xylose, polyol and anhydro polyol, and a manufacturing method thereof It is about.

The skin acts as a protection and barrier against the external environment and it is important to ensure a sufficient level of skin moisturization to preserve the skin's suppleness, softness, elasticity and/or appearance. In particular, the stratum corneum, the outermost region of the epidermis, delays water loss occurring in the deep layer of the epidermis, protects it from mechanical attack, and constitutes the first line of defense against UV rays.

In general, the decrease in moisturizing level can be prevented through moisturizing agents, and various moisturizing agents with improved effects or formulations have recently been developed. Recently, various glycoside derivatives are known to be effective in moisturizing, whitening, and treating inflammation. In one embodiment, Korean Patent Publication No. 10-2083970 discloses a composition for skin whitening containing a monoterpene glycoside compound derived from natural products, and Korean Patent Publication No. 10-2206536 discloses dicotomines or beta-sitosterol-3. A composition for preventing, improving or treating dermatitis containing -O-glycoside is disclosed.

In particular polyol glycosides can be prepared by reacting a polysaccharide, such as starch, with a polyol, such as a straight-chain or branched-chain aliphatic compound containing from 2 to 20 carbon atoms and containing at least two hydroxyl groups. This process is generally carried out under high pressure conditions at temperatures generally above 120° C. in the presence of at least one acid catalyst. Polysaccharides are hydrolyzed to give oligosaccharides and monosaccharides, which react with polyols in an acetalization reaction to produce polyol glycosides.

However, these methods have high energy-consuming operating conditions, and the obtained polyol glycosides exhibit poorly controlled glycosidic structures, and their often dark color makes them unsuitable for use in preparing cosmetic and/or pharmaceutical compositions. do.

Korean Patent Publication No. 10-2083970 Korean Patent Publication No. 10-2206536

The present invention is to solve the problems of the prior art as described above, and a cosmetic additive composition for skin moisturizing containing a glycoside derivative as an active ingredient and a method for preparing a high-purity glycoside derivative-containing additive with high efficiency and not derived from natural products. is intended to provide

In order to achieve the above object, the present invention provides a cosmetic additive composition comprising a glycoside derivative, xylose, polyol and anhydro polyol.

Preferably, the glycoside derivative is xylityl glucoside, and the polyol and anhydro polyol are preferably xylitol and anhydroxylitol.

On the other hand, in order to achieve the above object, the present invention includes a mixing step of preparing a mixed solution by uniformly dispersing sugar in a polyol; a heating step of heating the mixed solution under an acid catalyst; A catalyst removal step of removing the catalyst from the reaction mixture; And adding xylose to the mixture from which the catalyst has been removed.

At this time, the heating step is preferably performed at 100 to 110 ° C. for 3 to 7 hours, and the acid catalyst is preferably sulfuric acid.

According to the production method of the present invention, an additive composition containing a functional glycoside derivative with high efficiency can be easily prepared and can be used without limitation in various cosmetic formulations.

1 is a graph showing the results of experimental examples comparing the moisturizing power of Examples of the present invention and Comparative Examples.
Figure 2 is a comparative photograph showing the presence or absence of color change when silver ions are added to Examples of the present invention and Comparative Examples.

Hereinafter, the present invention will be described in detail with reference to embodiments and drawings of the present invention. These examples are only presented as examples to explain the present invention in more detail, and it will be apparent to those skilled in the art that the scope of the present invention is not limited by these examples. .

In addition, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of skill in the art to which this invention belongs, and in case of conflict, this specification including definitions of will take precedence.

In order to clearly explain the proposed invention in the drawings, parts irrelevant to the description are omitted, and similar reference numerals are attached to similar parts throughout the specification. And, when a certain component is said to "include", this means that it may further include other components without excluding other components unless otherwise stated. Also, a “unit” described in the specification means one unit or block that performs a specific function.

In each step, the identification code (first, second, etc.) is used for convenience of description, and the identification code does not describe the order of each step, and each step does not clearly describe a specific order in context. It may be performed differently from the order specified above. That is, each step may be performed in the same order as specified, may be performed substantially simultaneously, or may be performed in the reverse order.

In order to achieve the above object, the present invention provides a cosmetic additive including a glycoside derivative, a polyol and anhydro polyol, and may further include xylose.

The glycoside derivative is preferably a polyol glycoside in order to increase skin moisturizing ability, and the content thereof is preferably 65 to 75 parts by weight of the total composition in order to exert sufficient functional effects.

The polyol may be erythritol, xylitol, sorbitol, or the like, preferably xylitol. In addition, the sugar component of the glycoside is glucose, dextrose, sucrose, fructose, idose, gulose, galactose, maltose, isomaltose, maltotriose, lactose, cellobiose, mannose, Ribose, xylose, arabinose, lyxose, allose, altrose, dextran, or talose may be used, preferably glucose.

Various combinations of the polyol glycoside obtained by reacting the polyol component and the sugar component are possible, but preferably, Xylityl Glucoside may be used, and erythritol glucoside or sorbitol glucoside may be used. In addition, it is preferable that the average degree of polymerization of the sugar component is 1 to 3.

On the other hand, the polyol and anhydropolyol are by-products generated in the process of producing polyol glycosides, and the content thereof is preferably 1 to 5 parts by weight of the total weight. Overall functional effectiveness is reduced.

The polyol and anhydropolyol may vary depending on the type of polyol glycoside produced. In one embodiment, when the polyol glycoside produced is xylityl glucoside, the polyol and anhydropolyol are xylitol and anhydroxylitol can be

On the other hand, the present invention may further include xylose to improve the overall moisturizing function. All commercially available xylose may be used as the xylose, but in a preferred embodiment, xylose-containing saccharides obtained from natural products such as cornstalks may be used.

Specifically, the xylose-containing saccharide is obtained by grinding corncobs; Steam explosion pre-treatment of the pulverized cornstalks; Acid hydrolyzing the pretreated biomass to obtain a saccharification solution; Neutralizing the acid hydrolysis saccharification solution and filtering to remove precipitates; and desalting the filtered saccharified solution by electrodialysis.

Hereinafter, looking at each step in detail, cornstalks are preferably pulverized to a length of 2 to 3 cm in order to maximize the xylose acquisition efficiency. It is preferable to first pre-treat the pulverized cornstalk by steam explosion in order to increase the effect of hydrolysis thereafter. The steam explosion consists of a steam generator for generating steam, a reactor into which steam generated from the corncob and steam generator flows, and a receiving chamber for receiving materials ejected from the reactor. When cornstalks are introduced into the reactor, steam generated by the steam generator is introduced into the reactor until the temperature within the reactor reaches 200°C (1.6 MPa). Thereafter, after the cornstalks are exposed to steam for about 5 to 10 minutes, the valve is opened to allow the cornstalks inside the reactor to be exploded and introduced into the receiving chamber. Thereafter, the cornstalk introduced into the receiving chamber is separated from the liquid portion through a filtration process.

The pretreated cornstalk is then subjected to an acid hydrolysis process. In an embodiment, acid hydrolysis is performed by adding 100 to 1,000 g of a 0.2 to 5.0% sulfuric acid solution to 100 g of pretreated cornstalk at a reaction temperature of 100 to 200 ° C and a reaction pressure of 0 to 10 kgf / cm2 at 10 to 50 rpm. While stirring, it can be carried out by reacting for 0.5 to 10 hours.

After the acid hydrolysis reaction, the pH 1.0 ~ 2.0 acid hydrolyzate is adjusted to pH 3.0 ~ 7.0 with calcium carbonate, and then stirred under conditions of temperature 60 ~ 90 ℃, time 30 ~ 120 minutes, and acid hydrolyzate Sulfate ions in the solution react with calcium ions to precipitate in the form of calcium sulfate. After removing the precipitated calcium sulfate using a filter cloth, the filtered reaction solution is desalted with an electrical conductivity of 1,000 μS/cm or less using an electrodialysis device. The electrodialysis device includes an ion exchange membrane, an electrode plate, a flow control pump, and a rectifier.

Additionally, the demineralized reaction solution may be passed through a strong acid cation exchange resin, a weak base anion exchange resin, a mixed resin, etc. to remove inorganic salts and ionic substances, and the saccharification solution containing the xylose component thus obtained may be used as it is, It may be used through drying and powdering processes.

In a preferred embodiment, the additive composition comprises 1 to 10 parts by weight of xylose or a saccharide containing xylose and 1 to 5 parts by weight of xylitol, based on 100 parts by weight of Xylityl Glucosides. And it is preferable to include 0.1 to 5 parts by weight of anhydroxylitol (anhydroxylitol).

On the other hand, the above additive composition may be prepared by various methods, but in order to minimize by-products and obtain a glycoside compound with a certain structure, a mixing step of preparing a mixed solution by uniformly dispersing sugar in a polyol; a heating step of heating the mixed solution under an acid catalyst; A catalyst removal step of removing the catalyst from the reaction mixture; and adding xylose to the mixture from which the catalyst has been removed. Each step is described in detail below.

The polyol and sugar used in the mixing step are as described above, and in a preferred embodiment, xylitol and glucose may be used. The molar ratio of the polyol to the sugar is preferably 3:1 to 1:2, and more preferably a molar ratio of 1:1 may be used to minimize by-products.

When the mixing process is completed, polyol glycosides can be prepared by heating under an acid catalyst, and polyols and anhydropolyols as by-products are formed in this process. Preferably, the heating step is performed at 100 to 110° C. for 3 to 7 hours.

The acid catalyst may be sulfuric acid, phosphoric acid, hypophosphorous acid, polyphosphoric acid, hydrochloric acid, nitric acid, or sulfonic acid, preferably sulfuric acid. The acid catalyst is preferably used in an amount of 0.1 to 2 parts by weight based on 100 parts by weight of the mixed solution.

The reaction-completed mixture goes through a catalyst removal step. The acid may be removed through a neutralization reaction by mixing sodium hydroxide, but preferably, the catalyst is removed using an ion exchange resin to adjust the color. it is desirable

When acid is removed through neutralization, acidic anions can interact with various inorganic materials to form color changes or precipitates. It can be prevented.

At this time, the ion exchange resin used can be used without limitation as long as it is an anion-based ion exchange resin, and for example, a homogeneous strong alkaline anion exchange resin, a weak alkaline anion exchange resin (MA-12, MA-12OH, MA-10, MA -15, etc.) can be used.

Finally, xylose or xylose-containing saccharides may be added to the composition from which the catalyst is removed for a skin moisturizing effect. The prepared composition can be used in various formulations and application forms after finally undergoing a dehydration reaction.

Hereinafter, the configuration of the present invention and its effects will be described in more detail through specific manufacturing examples and examples. However, these examples are for explaining the present invention in more detail, and the scope of the present invention is not limited to these examples.

<Production Example>

Example

1 molar equivalent of xylitol was introduced into a reactor equipped with a stirrer and then melted at 100°C. While stirring at 100° C., 1 mole of glucose was slowly added to the reactor. Then, a 98 wt% sulfuric acid solution was added in a weight ratio of 0.9% of the weight of the mixed solution.

The reaction medium was reacted by placing it under a partial vacuum of 1.5-3 x 10 ⁴ Pa and holding at 100° C. for 6 hours. After the reaction medium was cooled to a temperature of 95° C., the pH of the mixture was brought to 7 using an ion exchange resin. Then, an example was prepared by additionally adding 0.3 molar equivalent of xylose.

comparative example

1 molar equivalent of xylitol was introduced into a reactor equipped with a stirrer and then melted at 100°C. 0.3 molar equivalent of glucose was slowly added to the reactor while stirring at 100°C. Then, a 98% by weight sulfuric acid solution was added in a weight ratio of 0.9% of the weight of the mixed solution.

The reaction medium was reacted by placing it under a partial vacuum of 1.5-3 x 10 ⁴ Pa and holding at 100° C. for 6 hours. A comparative example was prepared by cooling the reaction medium to a temperature of 95° C. and neutralizing it by adding 48% sodium hydroxide, pH 9, to bring the pH of the mixture to 7.

Examples (% by weight) Comparative Example (% by weight) Xylityl Glucoside 71.6 65.99 xylitol 2.6 3.57 anhydroxylitol 1.3 15.2 Xylose 4.3 - Others (including water) balance balance

As can be seen from the table above, it can be seen that the compositions of Examples have a high content of xylityl glucoside and a small content of by-products.

<Experimental Example 1>

Moisturizing compositions were prepared with the additives of Examples and Comparative Examples of the present invention in the composition ratios shown in Tables 2 and 3 below. (Example DJ-NXG, Comparative Example DJ-XG) After that, skin moisturizing power was measured using a coneometer, and then compared with the graphs in Tables 4 and 5 and FIG. 1. The coneometer experiment was conducted as follows.

After washing the left and right sides of the human body with soap for 10 subjects, the skin was acclimatized under constant temperature and humidity conditions (20±2, relative humidity 40±2℃). Seven test sites were determined as rectangles of 4X3 cm 2 on the left and right sides of the inner side of the lower arm, and the skin surface capacitance was repeatedly measured three times using a Corneometer (CM825). After measurement, samples containing 0, 1, 3, 5, 10, 20% of DJ-XG and DJ-NXG, respectively, which are substances that give skin moisturizing power, as shown in Tables 2 and 3 below, randomly in 7 test sites. 24 μl (2 mg/cm 2 ) was applied.

DJ-XG DJ-XG DJ-XG DJ-XG DJ-XG DJ-XG EDTA-2Na 0.02 0.02 0.02 0.02 0.02 0.02 BiophilicH 2.0 2.0 2.0 2.0 2.0 2.0 D-M 0.20 0.20 0.20 0.20 0.20 0.20 D-P 0.05 0.05 0.05 0.05 0.05 0.05 Germall
115 0.20 0.20 0.20 0.20 0.20 0.20 Sepigel
305 1.00 1.00 1.00 1.00 1.00 1.00 DJ-XG 0.00 1.00 3.00 5.00 10.00 20.00 DI Water 96.53 95.53 93.53 91.53 86.53 76.53

DJ-NXG DJ-NXG DJ-NXG DJ-NXG DJ-NXG DJ-NXG EDTA-2Na 0.02 0.02 0.02 0.02 0.02 0.02 BiophilicH 2.0 2.0 2.0 2.0 2.0 2.0 D-M 0.20 0.20 0.20 0.20 0.20 0.20 D-P 0.05 0.05 0.05 0.05 0.05 0.05 Germall
115 0.20 0.20 0.20 0.20 0.20 0.20 Sepigel
305 1.00 1.00 1.00 1.00 1.00 1.00 DJ-NXG 0.00 1.00 3.00 5.00 10.00 20.00 DI Water 96.53 95.53 93.53 91.53 86.53 76.53

After 6 hours of application, the skin surface capacitance was repeatedly measured three times using a coneometer. At this time, an adaptation period was also performed under constant temperature and humidity conditions. After obtaining the average value of the capacitance measured repeatedly three times, it was used as the moisture content. The initial moisture content before application and the moisture content of the uncoated area were corrected to obtain the moisture change rate, and based on this, the moisturizing power of the sample was judged.

Moisture change rate (%) = │{[(Tdi-Td0)-(Ntdi-NTd0)]/[(Ntdi-NTd0)+Td0]}*100│

(Tdi = nth measurement value of the sample application area, Td0 = before measurement value of the sample application area, NTdi = nth measurement value of the area where the sample is not applied, NTd0 = before measurement value of the area where the sample is not applied)

Using this formula, the results shown in Tables 4 and 5 were obtained, and these results are shown in Figure 1.

DJ-XG Concentration (%) 0 One 3 5 10 20 Skin moisturizing power (%) 5 10 15 20 25 50

DJ-NXG concentration (%) 0 One 3 5 10 20 Skin moisturizing power (%) 5 18 25 38 50 70

As can be seen from the above results, it was confirmed that the moisturizing power of the examples of the present invention was superior to that of the comparative examples.

<Experimental Example 2>

After preparing a solution by mixing 0.5 g of the sample of Comparative Example and Experimental Example and 9.5 g of R.O. water, respectively, 01 g (1%) of AgNO3 solution was added and left at room temperature for 24 hours. The color change of the solution was confirmed and shown in FIG. did

As can be seen in the figure, in the case of the comparative example, it was confirmed that the sulfuric acid anion reacted with the silver ion to take on a dark color, as shown in the reaction formula below, while it was confirmed that there was no color change in the embodiment of the present invention.

Na2SO4 + 2AgNO3 → 2NaNO3 + Ag2SO4

Although the present invention has been described in relation to the preferred embodiments as mentioned above, the technical spirit of the invention is not limited or limited thereto, and can be modified and implemented in various ways by those skilled in the art, of course.

Claims (5)

Includes Xylityl Glucoside, Xylose Containing Saccharides, Xylitol and Anhydroxylitol,
The xylose-containing saccharide may include grinding corncobs; Steam explosion pre-treatment of the pulverized cornstalks; Acid hydrolyzing the pretreated biomass to obtain a saccharification solution; Neutralizing the acid hydrolysis saccharification solution and filtering to remove precipitates; And desalting the filtered saccharification solution by electrodialysis;
Based on 100 parts by weight of Xylityl Glucosides, it contains 1 to 10 parts by weight of xylose-containing saccharide, 1 to 5 parts by weight of Xylitol, and 0.1 to 5 parts by weight of anhydroxylitol. Cosmetic additive composition to be.
delete A method for preparing the cosmetic additive composition of claim 1,
A mixing step of uniformly dispersing glucose in xylitol at a molar ratio of 1:1 to prepare a mixed solution; a heating step of heating the mixed solution at 100 to 110° C. for 3 to 7 hours under a sulfuric acid catalyst; A catalyst removal step of removing the catalyst from the reaction mixture; and adding a xylose-containing saccharide to the mixture from which the catalyst has been removed.
The xylose-containing saccharide may include grinding corncobs; Steam explosion pre-treatment of the pulverized cornstalks; Acid hydrolyzing the pretreated biomass to obtain a saccharification solution; Neutralizing the acid hydrolysis saccharification solution and filtering to remove precipitates; And desalting the filtered saccharification solution by electrodialysis;
Method for producing a cosmetic additive composition, characterized in that the removal of the catalyst is made using an ion exchange resin.
delete delete

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