WO2016013772A1 - Production method for hydrogel mask having outstanding skin-improving effect while comprising large oil fraction, and hydrogel composition produced by means of the method - Google Patents
Production method for hydrogel mask having outstanding skin-improving effect while comprising large oil fraction, and hydrogel composition produced by means of the method Download PDFInfo
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- WO2016013772A1 WO2016013772A1 PCT/KR2015/006378 KR2015006378W WO2016013772A1 WO 2016013772 A1 WO2016013772 A1 WO 2016013772A1 KR 2015006378 W KR2015006378 W KR 2015006378W WO 2016013772 A1 WO2016013772 A1 WO 2016013772A1
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- hydrogel
- pit
- water
- oil
- hydrogel composition
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
- A61K8/06—Emulsions
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
Definitions
- the present invention relates to a method for producing a hydrogel and a hydrogel composition prepared through the same, and more particularly, to a method for preparing a hydrogel composition through a phase inversion temperature (PIT) emulsification process and a hydrogel composition prepared through the same. It is about.
- PIT phase inversion temperature
- hydrogel mask sheets developed in the past were mostly composed of water-soluble components, and even if the oil-soluble components were formulated, the level of the use of the suspension for the purpose of differentiation or a slight feeling of improvement was improved. In addition, when a large amount of useful components are formulated, the useful components are separated, viscoelasticity is lowered, and the adhesion of the skin is lowered.
- Phase inversion temperature emulsi fying system (PIT) emulsification is called the phase-in-phase emulsification system, and when the temperature rises, the degree of hydration of the non-ionic surfactant hydrophilic part decreases, and HLB (hydrophi lic l ipophi lic balance) is used.
- Emulsification method In general, the surfactant is a hydrophilic and lipophilic balance in the aqueous solution at a specific temperature, which is called the phase inversion temperature of the surfactant. At the phase temperature, the curvature of water in the hydrophilic part changes from positive to negative, and the association number of the surfactant becomes infinite.
- the surfactant phase coexists with the oil phase and the water phase and exists in a transparent gel state as a bi-cont inuous phase.
- E how to get the emulsion.
- This method is a new technology that makes it possible to produce fine nanoemulsion dogs easily only by the composition of a surfactant, without having to pass through the reaction chamber under high pressure or strong dispersion that consumes a lot of energy.
- emulsifying common oil Levels of emulsions are reaching large particles.
- the PIT emulsification system it is not difficult to obtain a nano-sized fine emulsion, thereby making it possible to effectively produce excellent contents.
- W / 0 emulsification phase is formed by increasing activity of hydrophobic group which is an alkyl chain in the range of 80 ⁇ 951, and bicontiguous phase appears in the range of 61 ⁇ 69 ° C. You can get status. As a general molding equipment, there is a limit to quenching high temperature contents uniformly at all times and the cost burden is high. However, it was confirmed that this can be done by utilizing the conditions of quenching through the shell during the forming process of the hydrogel mask.
- Korean Patent No. 10-1240254 relates to a hydrogel sheet mast and a method for preparing the same, and comprises a small amount of an encapsulated effective ingredient separately prepared by a phase-transfer emulsification method during the preparation of the hydrogel to prepare a hydrogel sheet mast. It describes a method for improving the moisturizing power and skin flexibility by depositing a small amount on the outside of the hydrogel, but the present invention maximizes the skin efficacy as well as technical value by gelling the entire hydrogel composition using the PIT emulsification method.
- the manufacturing process of the hydrogel is accompanied by a heating process of 90 ° C or more, so as to simply add the ingredients encapsulated by the phase-transfer emulsification method during weeding, as described in the registered patent (10-1240254) capsules by high temperature conditions
- the stability of the chip may be broken or deformed, making it difficult to expect the actual effect.
- the phase transition emulsification method is a generic term for all emulsification methods that have a form that is changed during manufacture from oil-in-water (0 / W) to water-in-oil (W / 0) or water-in-water (W / 0) to oil-in-water (0 / W). I say that.
- the PIT emulsion was manufactured by the PIT emulsification method.
- the PIT emulsion is sensitive to external temperature since the PIT emulsion is made by an emulsification method using a specific temperature range. Therefore, stable emulsion can be formed through proper temperature conditions and stable prescription design.
- the present inventors have diligently studied to overcome the problems of the prior art, the hydrogel manufacturing method through the phase inversion temperature (PIT) emulsification process, containing the oil through the PIT method in the hydrogel was difficult to contain oil By facilitating easy to penetrate the skin of the active ingredient in the nano-emulsion state, it was confirmed that the effect can be further improved, and completed the present invention.
- PIT phase inversion temperature
- Patent Document 0001 K 10-1240254 ⁇
- the main object of the present invention is to facilitate the incorporation of oil through the PIT method in the hydrogel, which was difficult to contain oil, thereby facilitating the skin inversion temperature (PIT) emulsification process of the active ingredient in the nano-emulsion state. It is to provide a method for producing a hydrogel through.
- PIT skin inversion temperature
- Another object of the present invention is to provide a hydrogel composition prepared using a hydrogel manufacturing method through the phase inversion temperature (PIT) emulsification process.
- PIT phase inversion temperature
- 'impregnation' of the present invention refers to the inclusion of a PIT emulsion between the network structure of the gelled product.
- the term 'aqueous portion' of the present invention is generally referred to as an aqueous portion composed only of components dissolved in water at the time of manufacture.
- the term 'oil phase' of the present invention is generally referred to as an oil phase portion composed only of components dissolved in oil.
- the water phase portion is 50 to 60% by weight of the purified water included in the water phase portion, including more than 5 to 10% by weight of the content of purified water included in the oil phase portion of the present invention, respectively the water phase portion and the oil phase portion It was said.
- the water phase part of this invention is a name of the manufacturing part which mixes purified water, a water-soluble gelling polymer, and polyhydric alcohol
- an oil phase part is a name of the manufacturing part which produces 0 / W emulsion dog by PIT emulsification.
- the PIT nanoemulsion used to impregnate oil inside hydrogels having a gel network structure in the present invention is a great discovery.
- the strength of the gel was weakened and the loading itself was impossible.
- the PIT nano emulsion was able to impregnate the inside of the hydrogel, and it was confirmed that the superior efficacy effect can be obtained by the successful completion of the present invention.
- the characteristic feature highlighted in the present invention is not possible by simple blending after forming the hydrogel, but the temperature at which the water-soluble gelling polymer and the aqueous phase are mixed to gel (60 to 10 CTC).
- gelling and PIT emulsion are prepared by heating / stirring at a temperature (60 to 95 ° C.) to form a PIT emulsion at the oil phase and the oil phase, the gel phase and the PIT emulsion are mixed to form a PIT emulsion.
- PIT emulsions are stably impregnated in the gelation while cooling to a temperature range of 60 to 80 ° C.
- PIT emulsions are stably present in the gelled network structure, and the PIT emulsions stably do not lose their original state.
- Emulsion can be prepared (in the present invention, the 'hydrogel composition of the entire PIT emulsification The 'says Expressed). This hydrogel manufacturing process is the first found in the present invention, and this characteristic part has made it possible to realize the actual hydrogel to industrialization.
- the polyhydric alcohol in the step a) may be used any polyhydric acid conventionally used, preferably glycerin, butylene glycol, dipropylene glycol, propylene glycol, nucleic acid diol, 1 , 2-hexanediol, 1,2-pentanedi is characterized in that at least one selected from the group consisting of propanediol and 1,2-octanedi.
- the other additive in step a) may include any other additives conventionally added to make a hydrogel, preferably methylparaffin, propylparaben, phenoxyethanol glyceryl caprylate, and ethylsilyl glycerin It is characterized in that at least one selected from the group consisting of skin conditioning agent consisting of caprylic / capric glycerides and natural extracts.
- the nonionic surfactant in step b) may be any nonionic surfactant conventionally used, preferably glyceryl monostearate, cetes 10-30, ceteares 10-30 and ste And at least one selected from the group consisting of Ares 10 30.
- PIT emulsions can be made under the use of nonionic surfactants.
- hydrogels prepared by the general emulsification method do not form gels properly, even though nonionic surfactants are used. It was confirmed.
- the emulsified particle size is large. It can be seen that it is possible to prepare a stable hydrogel that is formed and does not cause high cloudiness or breakage (see Comparative Example 1-2, Fig. 9).
- the oily skin softener in step b) is characterized in that at least one selected from the group consisting of hydrocarbon-based oil, silicone-based oil, ester-based oil and natural oil.
- Hydrocarbon oils include Mineral Oil, Isododecane and Squalane, and silicone oils may be selected from Dimethicone, Cyclopentasi loxane and Trisi loxane.
- esters include Octyldodecyl Myristate, Di isostearyl Malate, Isopropyl Myristate, and natural oils are Macadamia nut oi l and Sunf lower oi l. Ol ive oi l may be selected from, but is not limited thereto.
- the PIT emulsion in step c) is characterized in that it has an average particle size of 100 ⁇ 500nm.
- the water-soluble polymer is cellulose, konjac, locust bean gum, carob bean gum, alginate, chitosan, starch, pectin, allyl, guar gum, mannan, poloronig arabic gum, flu Ran, collagen, gellan gum, xanthan gum, carrageenan, sclerotium gum and agar is characterized in that at least one selected from the group consisting of.
- the present invention provides a hydrogel composition prepared according to the above production method.
- the hydrogel composition prepared by applying the PIT emulsification method is compared with the particles of the hydrogel composition prepared by the general emulsification method, whereas the particles prepared by the general emulsification method have a unit size.
- PIT Emulsification The prepared particles were confirmed to have a ran unit size.
- the hydrogel composition of the present invention is superior to the control.
- the hydrogel composition prepared by the PIT emulsification method can provide a better effect than the hydrogel composition prepared by the conventional general emulsification method, and these compositions are prepared together in the form of a mask sheet that adheres to the skin. In this case, it can be seen that the effect can be maximized (see Experimental Example 2-3 and FIGS. 11-13).
- the composition contains from 0.1 to 10% by weight of gelling polymer, 0.1 to 30% by weight of polyhydric alcohol, 0.1 to 20% by weight of nonionic surfactant, and 0.1 to 30% by weight of skin softener, based on the total weight of the composition. It features.
- the content of the skin softener (oil) is out of the above range, it does not feel the effect when less than 0.1 weight 3 ⁇ 4 »and the gel breakage occurs when more than 30% by weight is possible to form a hydrogel having a commodity value.
- the water-soluble gelling polymer if it is out of the above range, it is difficult to mold in a gel state if less than 0.1 weight 3 ⁇ 4>, and if it is more than 10% by weight, the molding is difficult due to the high viscosity.
- polyhydric alcohol the elasticity of the gel is lowered when less than 0.1 weight 3 ⁇ 4, and the increase in effect is ineffective because the increase is more than 30% by weight.
- non-unsaturable surfactants when the content is 0.1 wt% or less or 20 wt% or more, problems may occur in the formation of suitable emulsified particles and stabilization of the formulation.
- the composition is characterized in that the formulation of the mask sheet form.
- Hydrogel composition using the PIT emulsification method according to the invention is water and By providing oil at the same time, it can satisfy the nutrition and moisture of the skin at the same time, and can be manufactured in a small particle size simply without special manufacturing equipment, thereby making an economical and effective hydrogel.
- Example 1 and 2 is a view showing the form of the hydrogel prepared according to the preparation method of Example 1 of the present invention.
- 3 and 4 is a view showing the form of the hydrogel prepared according to the preparation method of the present invention Example 2.
- FIG 5 and 6 are views showing the form of the hydrogel prepared according to the preparation method of the present invention Example 3.
- FIG 7 and 8 are views showing the form of the hydrogel prepared according to the preparation method of Comparative Example 1 of the present invention.
- FIG. 9 is a view showing the form of the hydrogel prepared according to the preparation method of Comparative Example 2 of the present invention.
- FIG. 10 is a view showing the results of particle size comparison between the general emulsification method and the PIT emulsification method of Experimental Example 1 of the present invention.
- FIG. 10 is a view showing the results of particle size comparison between the general emulsification method and the PIT emulsification method of Experimental Example 1 of the present invention.
- Figure 11 is a view showing the form of the hydrogel prepared according to the preparation method of Experimental Example 3 of the present invention (from the left control, macadam i aoi, dimethicone (6cs), octyldodecyl myristate).
- Example 14 is a view showing the form of the hydrogel prepared according to the preparation method of Example 3, showing the results of Experimental Example 4.
- Example 15 is a view showing the form of the hydrogel prepared according to the preparation method of Example 2, showing the results of Experimental Example 4 (from the left control, macadamia oi l, dimethicone, octyldodecyl myristate). [Form for implementation of invention]
- the key point is to design the preparation method to be consistent with the PIT production temperature and the dissolution temperature of the hydrogel. More specifically, the temperature at which the composition of the aqueous phase portion shown in Table 1 is dissolved is in the range of 70 ⁇ 90 ° C., in order to encapsulate the nanoemulsion inside the hydrogel, the preparation silver of the PIT nanoemulsion should be the same.
- Example 3 Preparation of hydrogel through PIT emulsification process according to the type of water-soluble gelling polymer, the type of oil and the content of oil phase
- Comparative Example 1 Preparation of a hydrogel through the PIT emulsification process containing no oil and no silver surfactant
- Example 1 The composition of Example 1 was prepared in the same manner as in Preparation Example 1 except for the oil phase part (oil nonionic surfactant, Cetearyl Alcohol).
- oil phase part oil nonionic surfactant, Cetearyl Alcohol.
- Example 2 It was carried out in the same composition as in Example 1, but prepared by the general emulsification method, not the PIT emulsification method.
- the water-soluble gelling polymer and polyalcohol were dissolved in the aqueous phase and then emulsified by heating / dissolving the non-silver surfactant and the oil-based skin softener in a separate oil phase.
- the contents manufacturing is completed, the contents are discharged and gelated by cooling the contents using a cooler.
- the emulsifier using the PIT emulsification method was prepared in Example 1, and the particle size was measured.
- the emulsifier used in the emulsion system using the general emulsification method is commonly used a combination of polysorbate -60 and glyceryl monostearate as the most commonly used surfactant (Table 5), the production method It proceeded similarly to Example 1.
- the concentration was tested to the same concentration as the total concentration of the surfactant using the PIT emulsification method.
- Example 1 Using Example 1 and Comparative Example 1, and attached to the face for 20 minutes for each of 15 men and women each 30 minutes, the feeling and stimulation test was carried out. As a result, as shown in Table 6, Example 1 can be seen that compared to Comparative Example 1 in the overall evaluation items such as skin moisturizing and flexibility, stimulation. In particular, much improved improvement was found in skin moisturizing and suppleness, which contained oils with similar levels of oil content as commonly produced emulsion dogs. Expected to increase flexibility
- Example 2 Based on the results confirmed through Experimental Example 2, the test was conducted to improve the moisturizing power and moisture to obtain more objective data.
- the oil the same vegetable oil (Macadamia oil), silicone oil (Dimethic e 6cs) and ester oil (Octyldodecyl Myristate) were used in the same amount.
- Moisturizing power is calculated using the average value measured three times.
- Test subjects 18 healthy adult women and 12 males (average 25 years old)
- Example 2 The hydrogel prepared in Example 2 was observed by leaving it exposed to air. As a result, as can be seen in Figures 14 and 15, there is a difference in speed depending on the type of oil, but it can be seen that the impregnated emulsion inside the gel exits the outside of the gel and the gel becomes more transparent. This confirmed that the active ingredient in the hydrogel can be easily eluted from the matrix and transferred to the skin along with the dihydrate.
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Abstract
The present invention relates to a hydrogel composition using a phase inversion temperature (PIT) emulsification process and to a production method for same. More specifically, the invention relates to a method wherein a water-based moiety comprising a water-soluble gelling polymer, purified water, a polyhydric alcohol and other additives is heated/stirred at between 60 and 100°C and, in a separate container, an oil-based moiety comprising a nonionic surfactant and an oily skin-softening agent is heated to between 60 and 95°C, and then the water-based moiety and the oil-based moiety are mixed and cooled to a temperature range at which the water-based moiety gells, namely between 60 and 80°C, and at the same time a PIT emulsion is stably impregnated into the gelled article, cooling takes place via a cooler, and a hydrogel is moulded. The present invention makes it possible to achieve more effective skin penetration of active ingredients in the nano-emulsion state, and thus to enhance the effects thereof, by using the PIT emulsification method to make it easier to include oil fractions in hydrogels in which it has previously been difficult to include oil fractions.
Description
【명세서】 【Specification】
【발명의 명칭】 [Name of invention]
다량의 유분을 포함하면서 피부개선효과가 우수한 하이드로겔 마스크의 제조방법 및 이를 통하여 제조된 하이드로겔 조성물 Method for producing a hydrogel mask comprising a large amount of oil and excellent skin improvement effect and the hydrogel composition prepared through this
【기술분야】 Technical Field
본 발명은 하이드로겔 제조방법 및 이를 통하여 제조된 하이드로겔 조성물에 관한 것으로, 더욱 구체적으로는 PIT(Phase inversion temperature)유화 공정을 통한 하이드로겔 (Hydrogel ) 조성물의 제조방법 및 이를 통해 제조된 하이드로겔 조성물에 관한 것이다. The present invention relates to a method for producing a hydrogel and a hydrogel composition prepared through the same, and more particularly, to a method for preparing a hydrogel composition through a phase inversion temperature (PIT) emulsification process and a hydrogel composition prepared through the same. It is about.
【배경기술】 Background Art
점차 현대인들은 기본적인 노화의 요인 외에도 오염된 외부환경과 생활 속 스트레스, 메이크업 제품의 사용빈도 확대에 따른 심각한 피부 손상에 시달리고 있다. 이를 극복하기 위해 로션, 크림, 에센스 등 다양한 스킨케어 제품의 사용과 피부과 치료 등을 활용하고 있다. 하지만 일반적인 스킨케어 제품의 사용으로는 피부 조직의 특성상 피부침투의 한계가 있어, 즉각적인 피부 개선을 기대하기가 어렵다. 이에 고가의 피부과 치료 및 약물 치료와 같은 비교적 위험한 시술에까지 이르게 된다. 따라서 피부침투가 효과적이면서도 비교적 안전하고 저렴한 형태의 기초 화장품이 필요하다. Increasingly, modern people are suffering from severe skin damage caused by contaminated external environment, stress in daily life, and increasing use of makeup products. To overcome this problem, we use various skin care products such as lotions, creams, essences, and dermatology treatments. However, the use of general skin care products has a limitation of skin penetration due to the nature of the skin tissue, it is difficult to expect immediate skin improvement. This leads to relatively dangerous procedures such as expensive dermatological treatments and drug treatments. Therefore, there is a need for a basic cosmetic that is effective and relatively safe and inexpensive skin penetration.
최근 들어 다양한 형태의 시트를 적용한 마스크시트의 개발과 소비가 활발하다. 시트지를 활용하여 내용물의 피부흡수를 효과적으로 높여주면서도 비교적 가격이 저렴한 것이 장점이기 때문이다. 일반적인 시트타입뿐만 아니라, 하이드로겔, 바이오셀를로오츠 등 그 범위도 확대되고 있다. 그 중 하이드로겔의 웅용분야는 다양하다. 화장품뿐만 아니라 피부미용과 의료 분야에서도 다양하게 적용되고 있다. 대부분의 하이드로겔은 겔상태를 유지하면서 지지체인 하이드로겔 속에 함유되어 있는 약물이 피부 쪽으로 서서히 방출되도록 조절하는
가능을 이용한 것이다. 종래의 하이드로겔의 핵심 성분은 겔을 형성하고 유지하는 기능을 가진 다양한 겔화 고분자가 주로 사용된다. 기존에 개발된 다수의 하이드로겔 마스크시트의 조성은 대부분 수용성 성분들로 구성되어 았으며, 유용성 성분이 배합되었다 하더라도 외관의 차별화를 목적으로 하는 현탁제의 용도나 약간의 사용감을 개선하는 수준이었다. 또한 다량의 유용성분을 배합할 경우 유용성 성분이 분리되고 점탄성이 떨어지며, 피부의 부착력이 떨어지는 등의 다양한 문제점들올 가지고 있다. In recent years, the development and consumption of mask sheets to which various types of sheets are applied is active. This is because it is advantageous that the sheet is relatively inexpensive while effectively increasing the skin absorption of the contents. In addition to the general sheet type, the range of hydrogels, biocells and the like is also expanding. Among them, the grand field of hydrogel is various. In addition to cosmetics, it is widely applied in skin care and medical fields. Most hydrogels maintain the gel state and regulate the release of drugs contained in the hydrogel as a support to the skin slowly. It is possible to use. As a core component of the conventional hydrogel, various gelling polymers having a function of forming and maintaining a gel are mainly used. Many of the hydrogel mask sheets developed in the past were mostly composed of water-soluble components, and even if the oil-soluble components were formulated, the level of the use of the suspension for the purpose of differentiation or a slight feeling of improvement was improved. In addition, when a large amount of useful components are formulated, the useful components are separated, viscoelasticity is lowered, and the adhesion of the skin is lowered.
기초 화장품으로 피부 침투를 용이하게 하기 위해서는 화장료의 입자 크기를 작게 할수록 유리하다. 화장료의 형태를 크게 가용화와 유화로 나눌 수있는데, 이를 하이드로겔 제형에 적용시 몇 가지 문제점이 있다. 가용화 타입의 경우 조성의 대부분이 수용성 성분으로 구성되어 피지막으로 구성된 피부조직의 최외각 층을 침투하기가 어렵고 피부가 필요로 하는 유분의 제공이 용이하지 않다는 단점이 있다. 유화타입의 경우는 다량의 유분을 함유 가능하여, 피부에 층분한 영양을 부여할 수는 있으나 입자크기가 비교적 커서 피부 흡수 및 하이드로겔 내부에 안정한 로딩이 용이하지 않을 수 있다는 점과 과량의 유분을 사용시 겔 형성의 문제점 및 제형의 불안정성 등과 같은 기술적인 문제가 있다. 이러한 제형적 한계를 극복하기 위해 리포좀과 같은 다양한 공법과 소재를 이용한 화장료들이 개발되었으나, 비용적 한계 극복과 안전한 피부 적용이라는 관점에서 여전히 어려운 과제로 남아있다. In order to facilitate skin penetration into the basic cosmetics, the smaller the particle size of the cosmetic is advantageous. Forms of cosmetics can be divided into solubilization and emulsification largely, there are some problems when applied to the hydrogel formulation. In the case of the solubilization type, most of the composition is composed of water-soluble components, so it is difficult to penetrate the outermost layer of skin tissue composed of the sebaceous membrane, and it is not easy to provide oil required by the skin. In the case of emulsification type, it can contain a large amount of oil, so that it can give a good nutrition to the skin, but the particle size is relatively large so that it is not easy to absorb the skin and stable loading inside the hydrogel. There are technical problems such as problems of gel formation and formulation instability in use. In order to overcome these formulation limitations, cosmetics using various methods and materials, such as liposomes, have been developed, but still remain difficult in view of overcoming cost limitations and safe skin application.
PIT유화시스템 (Phase inversion temperature emulsi fying system)이란 전상온도 유화라고 일컬으며, 온도가 상승하면 비이온 계면활성제 친수부의 수화 정도가 하락되고, HLB(hydrophi l ic l ipophi l ic balance)가 변하는 것을 이용한 유화방법이다. 일반적으로 계면활성제는 특정한 온도의 수용액상에서 친수성과 친유성이 균형을 이루게 되는데, 이 온도를 계면활성제의 전상온도 (phase inversion temperature)라 한다. 전상온도에서는 친수부의 물에 대한 곡률이 양에서 음으로 변화하며 계면활성제의 회합수는 무한대가 된다. 이때는 계면활성제상이 유상 및 수상과 공존하며 바이컨티니어스상 (bi-cont inuous phase)인 투명한 겔 상태로 존재하게 되고, 이때 유화하면 작은 나노 입자의
에:멀젼을 얻을 수 있는 방법이다. 이 방법은 에너지가 많이 소모되는 강한 분산이나, 고압력 하에 반웅 챔버를 통과하지 않고도 계면활성제의 조성만으로도 쉽게 미세 나노에멀견의 제작이 가능한 신기술이라 할 수 있다. 일반적인 오일을 유화하여 사용할 경우 대부분
수준의 큰 입자의 에멀견에 이르고 있다. 이에 반하여 PIT유화시스템을 이용할 경우 어렵지 않게 나노 사이즈의 미세 에멀젼을 얻을 수 있기 때문에 보다 효과적으로 우수한 내용물을 만들 수 있다. PIT 유화는 80~951 범위에서 알킬체인인 소수기의 활성이 강해져서 W/0 유화상이 형성되고, 서서히 넁각하여 61~69°C 범위에서 바이컨티니어스상이 나타나며, 이때 급넁각하여 원하는 나노에멀견 상태를 얻을 수 있다. 일반적인 성형 설비로는 고온의 내용물을 항시 균일하게 급냉 하기에 한계가 있고, 비용적인 부담도 높다. 그러나 하이드로겔 마스크의 성형 과정 중에 넁각기를 통한 급냉의 조건을 활용하여 이를 수행할 수 있음을 확인하였다. Phase inversion temperature emulsi fying system (PIT) emulsification is called the phase-in-phase emulsification system, and when the temperature rises, the degree of hydration of the non-ionic surfactant hydrophilic part decreases, and HLB (hydrophi lic l ipophi lic balance) is used. Emulsification method. In general, the surfactant is a hydrophilic and lipophilic balance in the aqueous solution at a specific temperature, which is called the phase inversion temperature of the surfactant. At the phase temperature, the curvature of water in the hydrophilic part changes from positive to negative, and the association number of the surfactant becomes infinite. In this case, the surfactant phase coexists with the oil phase and the water phase and exists in a transparent gel state as a bi-cont inuous phase. E: how to get the emulsion. This method is a new technology that makes it possible to produce fine nanoemulsion dogs easily only by the composition of a surfactant, without having to pass through the reaction chamber under high pressure or strong dispersion that consumes a lot of energy. When emulsifying common oil Levels of emulsions are reaching large particles. On the contrary, when the PIT emulsification system is used, it is not difficult to obtain a nano-sized fine emulsion, thereby making it possible to effectively produce excellent contents. In PIT emulsification, W / 0 emulsification phase is formed by increasing activity of hydrophobic group which is an alkyl chain in the range of 80 ~ 951, and bicontiguous phase appears in the range of 61 ~ 69 ° C. You can get status. As a general molding equipment, there is a limit to quenching high temperature contents uniformly at all times and the cost burden is high. However, it was confirmed that this can be done by utilizing the conditions of quenching through the shell during the forming process of the hydrogel mask.
한국등록특허 10-1240254호는 하이드로겔 시트마스트 및 이의 제조 방법에 관한 것으로, 상전이 유화법으로 별도 제조한 캡슐화된 유효성분을 하이드로겔의 제조과정 중에 소량 함유시켜 하이드로겔 시트마스트를 제조하여 유효성분을 하이드로겔 외부에 소량 침적시켜 보습력 및 피부유연성을 향상시키는 방법에 대해 기재하고 있으나 본 발명은 하이드로겔 조성물 전체를 PIT 유화법을 이용하여 겔화함으로써, 피부 효능은 물론 기술적 가치를 극대화하였다. 일반적으로 하이드로겔의 제조과정은 90°C 이상의 가온 공정이 수반되기 때문에, 상기 등록특허 (10-1240254)와 같이 단순히 제초 중에 상전이 유화법으로 캡술화한 성분을 첨가하는 경우 고온의 조건에 의해 캡슐의 안정성이 깨지거나 변형되어 실제의 효과를 기대하기 어려울 수 있다. 상전이 유화법은 수중유형 (0/W)을 유중수형 (W/0)으로 또는 유중수형 (W/0)을 수중유형 (0/W) 형태로 제조 중에 변경되는 형태를 가지는 모든 유화방법을 총칭하는 것을 말한다. Korean Patent No. 10-1240254 relates to a hydrogel sheet mast and a method for preparing the same, and comprises a small amount of an encapsulated effective ingredient separately prepared by a phase-transfer emulsification method during the preparation of the hydrogel to prepare a hydrogel sheet mast. It describes a method for improving the moisturizing power and skin flexibility by depositing a small amount on the outside of the hydrogel, but the present invention maximizes the skin efficacy as well as technical value by gelling the entire hydrogel composition using the PIT emulsification method. In general, the manufacturing process of the hydrogel is accompanied by a heating process of 90 ° C or more, so as to simply add the ingredients encapsulated by the phase-transfer emulsification method during weeding, as described in the registered patent (10-1240254) capsules by high temperature conditions The stability of the chip may be broken or deformed, making it difficult to expect the actual effect. The phase transition emulsification method is a generic term for all emulsification methods that have a form that is changed during manufacture from oil-in-water (0 / W) to water-in-oil (W / 0) or water-in-water (W / 0) to oil-in-water (0 / W). I say that.
본 발명에서 사용한 기술은 PIT 유화법으로 PIT 유화물을 제조하였는데, 특히 PIT 유화물은 특정 온도 범위를 이용한 유화방법으로 만들어지므로 외부의 온도에 민감하다. 따라서 적정 온도 조건과 안정적인 처방설계를 통해서 안정적인 유화물이 형성될 수 있다.
이에, 본 발명자들은 상기 종래기술들의 문제점들을 극복하기 위하여 예의 연구노력한 결과, PIT(Phase inversion temperature) 유화공정을 통한 하이드로겔 제조방법은, 유분을 함유하기 어려웠던 하이드로겔에서 PIT 용법을 통해 유분의 함유를 용이하게 함으로써 나노 에멀견 상태의 유효성분의 피부 침투가 용이해져 그 효과를 더욱 향상시킬 수 있음을 확인하고, 본 발명을 완성하게 되었다. In the technique used in the present invention, the PIT emulsion was manufactured by the PIT emulsification method. In particular, the PIT emulsion is sensitive to external temperature since the PIT emulsion is made by an emulsification method using a specific temperature range. Therefore, stable emulsion can be formed through proper temperature conditions and stable prescription design. Accordingly, the present inventors have diligently studied to overcome the problems of the prior art, the hydrogel manufacturing method through the phase inversion temperature (PIT) emulsification process, containing the oil through the PIT method in the hydrogel was difficult to contain oil By facilitating easy to penetrate the skin of the active ingredient in the nano-emulsion state, it was confirmed that the effect can be further improved, and completed the present invention.
【선행기술문헌】 Prior Art Documents
【특허문헌】 [Patent literature]
(특허문헌 0001) K 10-1240254 Β (Patent Document 0001) K 10-1240254 Β
【발명의 상세한 설명】 [Detailed Description of the Invention]
【기술적 과제】 [Technical problem]
따라서, 본 발명의 주된 목적은 유분을 함유하기 어려웠던 하이드로겔에서 PIT 용법을 통해 유분의 함유를 용이하게 함으로써 나노 에멀견 상태의 유효성분의 피부 침투를 더욱 용이하게 하는 PIT(Phase inversion temperature) 유화공정을 통한 하이드로겔 제조방법을 제공하는 데 있다. Therefore, the main object of the present invention is to facilitate the incorporation of oil through the PIT method in the hydrogel, which was difficult to contain oil, thereby facilitating the skin inversion temperature (PIT) emulsification process of the active ingredient in the nano-emulsion state. It is to provide a method for producing a hydrogel through.
본 발명의 다른 목적은 상기 PIT(Phase inversion temperature) 유화공정을 통한 하이드로겔 제조방법을 이용하여 제조된 하이드로겔 조성물을 제공하는데 있다. Another object of the present invention is to provide a hydrogel composition prepared using a hydrogel manufacturing method through the phase inversion temperature (PIT) emulsification process.
【기、술적 해결방법】 【Technical Solution】
하기 단계를 포함하는 PIT(Phase inversion temperature)유화공정을 통한 하이드로겔 (Hydrogel ) 조성물 제조방법을 제공한다. It provides a method for producing a hydrogel (Hydrogel) composition through a phase inversion temperature (PIT) emulsification process comprising the following steps.
a) 별도의 용기에 수용성 겔화 고분자, 정제수, 다가알코올 및 기타첨가제를 포함하는 수상부를 60 내지 100°C로 가온 /교반 하는 단계; a) warming / stirring the aqueous phase containing water-soluble gelling polymer, purified water, polyhydric alcohol and other additives in a separate container at 60 to 100 ° C .;
b) 별도의 용기에 비이온성 계면활성제 및 오일성 피부유연화제를 포함하는 유상부를 60 내지 95°C로 가온 /교반하여 PIT유화물을 제조하는 단계 ;
c) 상기 a)의 겔화물에 b)의 PIT 유화물을 투입하고 60 내지 80°C로 냉각시키며 겔화물 내부로 PIT유화물을 함침시키는 단계; 및 b) preparing a PIT emulsion by heating / stirring the oil phase including the nonionic surfactant and the oily skin softener in a separate container at 60 to 95 ° C .; c) injecting the PIT emulsion of b) into the gelation of a), cooling to 60 to 80 ° C. and impregnating the PIT emulsion into the gelation; And
d) 넁각기를 통해 하이드로겔을 넁각시킨 후 성형하는 단계. d) engraving the hydrogel through granulation and then molding.
본 발명의 상기용어 '함침' 은 겔화물의 네트워크 구조 사이에 PIT 유화물을 내포시키는 것을 뜻한다. The term 'impregnation' of the present invention refers to the inclusion of a PIT emulsion between the network structure of the gelled product.
본 발명의 상기용어 '수상부' 는 일반적으로 제조시에 물에 용해되는 성분들로만 구성된 것을 수상부라 한다. 본 발명의 상기용어 '유상부' 는 일반적으로 오일에 용해되는 성분들로만 구성된 것을 유상부라고 한다. 그러나, 본 발명에서 수상부는 수상부에 포함되는 정제수의 함량이 50 내지 60 중량 %로 본원발명의 유상부에서 포함되는 정제수의 함량인 5 내지 10중량 %보다 더 많은 함량을 포함하여 각각 수상부 및 유상부라고 하였다. 또한, 본 발명의 수상부는 정제수와 수용성 겔화 고분자, 다가알코올을 흔합하는 제조부의 명칭이며, 유상부는 PIT유화를 실시하여 0/W 에멀견을 제조하는 제조부의 명칭이다. The term 'aqueous portion' of the present invention is generally referred to as an aqueous portion composed only of components dissolved in water at the time of manufacture. The term 'oil phase' of the present invention is generally referred to as an oil phase portion composed only of components dissolved in oil. However, in the present invention, the water phase portion is 50 to 60% by weight of the purified water included in the water phase portion, including more than 5 to 10% by weight of the content of purified water included in the oil phase portion of the present invention, respectively the water phase portion and the oil phase portion It was said. In addition, the water phase part of this invention is a name of the manufacturing part which mixes purified water, a water-soluble gelling polymer, and polyhydric alcohol, and an oil phase part is a name of the manufacturing part which produces 0 / W emulsion dog by PIT emulsification.
본 발명에서 겔 네트워크 구조를 가진 하이드로 겔 내부에 오일을 함침 시키기 위해 사용된 PIT 나노 에멀젼은 대단한 발견이다. 일반 유화물은 하이드로겔에 함침 시킬 경우, 겔의 강도가 약해지고, 겔 내부에 로딩자체가 불가능했다. 그러나 PIT 나노 유화물은 하이드로겔 내부에 함침이 가능하였으며, 이를 성공함으로써 월등한 효능효과를 얻을 수 있음을 확인하고 본원발명을 완성하였다. 하이드로겔 내부에 함침이 가능한 이유로, 본 발명에서 특징적으로 강조하는 부분은 하이드로겔을 형성한 후에 단순배합에 의하여 가능하게 하는 것이 아니라, 수용성 겔화고분자와 수상부가 흔합하여 겔화하는 온도 (60 내지 10CTC )와 유상부에서 PIT 유화물을 만드는 온도 (60 내지 95°C )에서 각각 가온 /교반하여 겔화물과 PIT 유화물을 제조한 후, 상기 겔화물과 PIT 유화물을 흔합하여 PIT 에멀젼을 만들 때, 수상부가 겔화되는 온도 범위인 60 내지 80°C로 냉각시키면서 PIT 유화물이 겔화물에 안정하게 함침되어 PIT 유화물이 네트워크 구조를 하고 있는 겔화물에 안정하게 존재하게 되면서 PIT 유화물이 본래의 상태를 잃어버리지 않고 안정적으로 PIT 에멀견올 제조할 수 있는 것이다 (이러한 상태를 본원발명에서는 '하이드로겔 조성물 전체를 PIT 유화한다. ' 라고
표현하였다) . 이러한 하이드로겔 제조공정은 본원발명에서 최초로 발견한 조¾으로, 이와 특징적인 부분을 실제 하이드로겔을 공업화에 이르기까지 실현 가능케 하였다. The PIT nanoemulsion used to impregnate oil inside hydrogels having a gel network structure in the present invention is a great discovery. When the common emulsion was impregnated into the hydrogel, the strength of the gel was weakened and the loading itself was impossible. However, the PIT nano emulsion was able to impregnate the inside of the hydrogel, and it was confirmed that the superior efficacy effect can be obtained by the successful completion of the present invention. Because of the possibility of impregnation inside the hydrogel, the characteristic feature highlighted in the present invention is not possible by simple blending after forming the hydrogel, but the temperature at which the water-soluble gelling polymer and the aqueous phase are mixed to gel (60 to 10 CTC). After gelling and PIT emulsion are prepared by heating / stirring at a temperature (60 to 95 ° C.) to form a PIT emulsion at the oil phase and the oil phase, the gel phase and the PIT emulsion are mixed to form a PIT emulsion. PIT emulsions are stably impregnated in the gelation while cooling to a temperature range of 60 to 80 ° C. PIT emulsions are stably present in the gelled network structure, and the PIT emulsions stably do not lose their original state. Emulsion can be prepared (in the present invention, the 'hydrogel composition of the entire PIT emulsification The 'says Expressed). This hydrogel manufacturing process is the first found in the present invention, and this characteristic part has made it possible to realize the actual hydrogel to industrialization.
좀 더 상세하게 기술하면 PIT유화물인 경우에 95 °C이상에서는 W0 유화로 전상이되고, 서서히 냉각하는 과정에서 60~85°C범위에서 바이컨티니어스층이 형성되기 때문에 하이도로겔에 쉽게 함침이 가능함을 알 수 있었다. 이 공정으로 할 경우에만 하이드로겔 내부로 나노유화물의 함침이 가능하였으며, 그러하지 않은 경우와 일반 유화물을 단순히 배합하는 공정에서는 하이드로겔 내부에 오일을 함침하는 것이 불가능하였다. In more detail, in case of PIT emulsification, it becomes phase change by W0 emulsification above 95 ° C, and it is easily impregnated into high road gel because bi-continuous layer is formed in the range of 60 ~ 85 ° C during the slow cooling process. It was found possible. Only in this process was it possible to impregnate the nanoemulsion into the hydrogel, it was not possible to impregnate the oil into the hydrogel in the case of not blending with the general emulsion if not.
본 발명에 있어서, 상기 a) 단계에서 다가알코올은 종래에 사용되어진 어떠한 다가을코을도 사용될 수 있으며, 바람직하게는 글리세린, 부틸렌글라이콜, 디프로필렌글라이콜, 프로필렌글라이콜, 핵산디올, 1,2-헥산디올, 1 ,2-펜탄디을 프로판디올 및 1 ,2-옥탄디을로 구성된 그룹에서 선택되는 하나 이상인 것을 특징으로 한다. - 본 발명에 있어서, a) 단계에서 기타첨가제는 종래에 하이드로겔을 만들기 위해 첨가되는 어떠한 기타첨가제가 포함될 수 있으며, 바람직하게는 메칠파라핀, 프로필파라벤, 페녹시에탄올 글리세릴카프릴레이트, 에칠핵실글리세린, 카프릴릭 /카프릭글리세라이드 및 천연 추출물로 이루어진 피부컨디셔닝제로 구성된 그룹에서 선택되는 하나 이상인 것을 특징으로 한다. In the present invention, the polyhydric alcohol in the step a) may be used any polyhydric acid conventionally used, preferably glycerin, butylene glycol, dipropylene glycol, propylene glycol, nucleic acid diol, 1 , 2-hexanediol, 1,2-pentanedi is characterized in that at least one selected from the group consisting of propanediol and 1,2-octanedi. In the present invention, the other additive in step a) may include any other additives conventionally added to make a hydrogel, preferably methylparaffin, propylparaben, phenoxyethanol glyceryl caprylate, and ethylsilyl glycerin It is characterized in that at least one selected from the group consisting of skin conditioning agent consisting of caprylic / capric glycerides and natural extracts.
본 발명에 있어서, 상기 b) 단계에서 비이온성 계면활성제는 종래에 사용되어진 어떠한 비이온성 계면활성제일 수 있으며, 바람직하게는 글리세릴모노스테아레이트, 세테스 10~30, 세테아레스 10-30 및 스테아레스 10 30로 구성된 그룹에서 선택되는 하나 이상인 것을 특징으로 한다. In the present invention, the nonionic surfactant in step b) may be any nonionic surfactant conventionally used, preferably glyceryl monostearate, cetes 10-30, ceteares 10-30 and ste And at least one selected from the group consisting of Ares 10 30.
일반적으로 비이온 계면활성제 사용하에 PIT유화물을 만들 수 있으며, 본 발명의 실시예에 따르면 비이온 계면활성제를 사용하더라도 일반적인 유화방법으로 제조한 하이드로겔은 겔 형성이 제대로 되지 않아 부서지는 현상이 발생하는 것을 확인하였다. 이러한 결과로 볼 때, 비이온성 계면활성제를 함유하여 PIT 유화방법으로 제조한 하이드로겔의 경우, 유화 입자사이즈가 크게
형성되어 백탁현상이 높거나 부서지는 현상이 발생하지 않는 안정한 하이드로겔을 제조할 수 있음을 알수 있다 (비교예 1-2, 도 그 9 참조) . In general, PIT emulsions can be made under the use of nonionic surfactants. According to an embodiment of the present invention, hydrogels prepared by the general emulsification method do not form gels properly, even though nonionic surfactants are used. It was confirmed. As a result of this, in the case of the hydrogel containing the nonionic surfactant prepared by the PIT emulsification method, the emulsified particle size is large. It can be seen that it is possible to prepare a stable hydrogel that is formed and does not cause high cloudiness or breakage (see Comparative Example 1-2, Fig. 9).
본 발명에 있어서, 상기 b) 단계에서 오일성 피부유연화제는 탄화수소계오일, 실리콘계오일, 에스테르계오일 및 천연오일로 구성된 그룹에서 선택되는 하나 이상인 것을 특징으로 한다. 탄화수소계 오일은 Mineral oi l , Isododecane , Squalane이 있으며, 실리콘계 오일은 Dimethicone, Cyclopentasi loxane, Trisi loxane에서 선택될 수 있다. 또한, 에스테르계은 Octyldodecyl Myristate , Di isostearyl Malate, Isopropyl Myristate가 있으며, 천연오일은 Macadamia nut oi l , Sunf lower oi l . Ol ive oi l에서 선택될 수 있으나 이에 한정된 것은 아니다. In the present invention, the oily skin softener in step b) is characterized in that at least one selected from the group consisting of hydrocarbon-based oil, silicone-based oil, ester-based oil and natural oil. Hydrocarbon oils include Mineral Oil, Isododecane and Squalane, and silicone oils may be selected from Dimethicone, Cyclopentasi loxane and Trisi loxane. In addition, esters include Octyldodecyl Myristate, Di isostearyl Malate, Isopropyl Myristate, and natural oils are Macadamia nut oi l and Sunf lower oi l. Ol ive oi l may be selected from, but is not limited thereto.
본 발명에 있어서, 상기 c) 단계에 PIT 에멀젼은 100~500nm 평균입자크기를 갖는 것을 특징으로 한다. In the present invention, the PIT emulsion in step c) is characterized in that it has an average particle size of 100 ~ 500nm.
본 발명에 있어서, 상기 a) 단계에서 수용성 고분자는 셀를로오스, 곤약, 로커스트콩 검, 캐럽콩 검, 알기네이트, 키토산, 전분, 팩틴, 알길, 구아검, 만난, 폴루로니그 아라비아 검, 플루란, 콜라겐, 젤란검, 잔탄검, 카라기난, 스클레로튬검 및 한천으로 구성된 군으로부터 선택되는 하나 이상인 것을 특징으로 한다. In the present invention, in the step a), the water-soluble polymer is cellulose, konjac, locust bean gum, carob bean gum, alginate, chitosan, starch, pectin, allyl, guar gum, mannan, poloronig arabic gum, flu Ran, collagen, gellan gum, xanthan gum, carrageenan, sclerotium gum and agar is characterized in that at least one selected from the group consisting of.
본 발명의 실시예에 따르면, 수용성 겔화 고분자 및 오일의 종류와 함량을 변화하여 하이드로겔을 제조하였을 때, 현탁도에 약간의 차이가 있으나 유액타입의 하이드로겔이 잘 만들어지는 것을 확인할 수 있었다. 이러한 결과로 볼 때, 본원발명에서 제시한 수용성 겔화 고분자 및 오일 (피부유연화제)을 사용하여도 PIT 유화공정을 통해 안정한 하이드로겔을 제조할 수 있음을 알 수 있다 (실시예 2-3 , 도 3-6 참조) . According to the embodiment of the present invention, when the hydrogel was prepared by changing the type and content of the water-soluble gelling polymer and oil, there was a slight difference in suspension, but it was confirmed that the hydrogel of the emulsion type was well made. From these results, it can be seen that a stable hydrogel can be prepared through the PIT emulsification process even using the water-soluble gelling polymer and oil (skin softener) shown in the present invention (Example 2-3, FIG. 3-6).
본 발명의 다른 양태에 따르면, 본 발명은 상기 제조방법에 따라 제조된 하이드로겔 조성물을 제공한다. According to another aspect of the present invention, the present invention provides a hydrogel composition prepared according to the above production method.
본 발명의 실험예에 따르면, PIT 유화공법을 적용하여 제조한 하이드로겔 조성물은 일반유화법으로 제조된 하이드로겔 조성물의 입자와 비교하였을때, 일반 유화법으로 제조된 입자는 단위의 크기를 갖는 반면에 PIT유화법으로
제조된 입자는 ran 단위의 크기를 갖는 것을 확인하였다. 이러한 결과로 볼 때, 하이드로겔 조성물에 PIT 유화공법을 적용할 경우, 나노 사이즈로 제조된 조성물이 보다 효과적으로 피부 각질충의 흡수를 도와 효과를 극대화시킬 수 았음을 의미한다 (실험예 1 및 도 10 참조) . According to the experimental example of the present invention, the hydrogel composition prepared by applying the PIT emulsification method is compared with the particles of the hydrogel composition prepared by the general emulsification method, whereas the particles prepared by the general emulsification method have a unit size. To PIT Emulsification The prepared particles were confirmed to have a ran unit size. As a result, when the PIT emulsification method is applied to the hydrogel composition, it means that the composition prepared in the nano size was able to more effectively help the absorption of the keratin of the skin and maximize the effect (see Experimental Example 1 and FIG. 10). ).
본원발명의 실험예에 따르면, 사용감, 자극테스트 및 보습력, 수분 개선 테:스트를 확인한 결과, 본원발명의 하이드로겔 조성물이 대조군보다 뛰어난 효과를 확인할 수 있었다. 이러한 결과로 볼 때 PIT 유화공법으로 제조된 하이드로겔 조성물은 기존의 일반 유화법으로 제조된 하이드로겔 조성물보다 보다 뛰어난 효과를 제공할 수 있으며, 이러한 조성물은 피부에 밀착시켜 주는 마스크시트 형태로 함께 제조할 경우 그 효과를 극대화할 수 있음을 알 수 있다 (실험예 2-3 및 도 11-13 참조) . According to the experimental example of the present invention, as a result of confirming the feeling of use, stimulation test and moisturizing power, test of moisture improvement, it was confirmed that the hydrogel composition of the present invention is superior to the control. As a result, the hydrogel composition prepared by the PIT emulsification method can provide a better effect than the hydrogel composition prepared by the conventional general emulsification method, and these compositions are prepared together in the form of a mask sheet that adheres to the skin. In this case, it can be seen that the effect can be maximized (see Experimental Example 2-3 and FIGS. 11-13).
본 발명에 있어서, 상기 조성물은 조성물 총 중량 대비 겔화 고분자 0.1 내지 10 중량 ¾», 다가알코을 0.1 내지 30중량 ¾, 비이온성 계면활성제 0.1 내지 20중량 % 및 피부유연화제 0.1 내지 30중량 % 함유하는 것을 특징으로 한다. In the present invention, the composition contains from 0.1 to 10% by weight of gelling polymer, 0.1 to 30% by weight of polyhydric alcohol, 0.1 to 20% by weight of nonionic surfactant, and 0.1 to 30% by weight of skin softener, based on the total weight of the composition. It features.
피부유연화제 (오일)의 함량이 상기 범위를 벗어날 경우, 0.1중량 ¾» 미만 시 효과를 느끼지 못하며 30중량 % 초과시 겔이 부서지는 현상이 발생되어 상품가치가 있는 하이드로겔의 성형이 블가능하다. 수용성 겔화 고분자의 경우에서도 상기 범위를 벗어날 경우, 0.1중량 ¾> 미만이면 겔 상태로 성형이 어렵고, 10중량 % 초과이면 점도가 너무 높아 제조 시 성형이 어렵다. 또한, 다가알코올의 경우 0.1중량 ¾ 미만이면 겔의 탄력성이 떨어지고, 30증량 % 이상이면 효과상승이 미미하여 비효율적이다. 비이은성 계면활성제의 경우도 0.1중량 % 이하이거나 20중량 % 이상이면 적합한 유화입자의 형성 및 제형의 안정화에 문제가 생길 수 있다. If the content of the skin softener (oil) is out of the above range, it does not feel the effect when less than 0.1 weight ¾ »and the gel breakage occurs when more than 30% by weight is possible to form a hydrogel having a commodity value. Even in the case of the water-soluble gelling polymer, if it is out of the above range, it is difficult to mold in a gel state if less than 0.1 weight ¾>, and if it is more than 10% by weight, the molding is difficult due to the high viscosity. In addition, in the case of polyhydric alcohol, the elasticity of the gel is lowered when less than 0.1 weight ¾, and the increase in effect is ineffective because the increase is more than 30% by weight. In the case of non-unsaturable surfactants, when the content is 0.1 wt% or less or 20 wt% or more, problems may occur in the formation of suitable emulsified particles and stabilization of the formulation.
본 발명에 있어서, 상기 조성물은 마스크시트 형태의 제형인 것을 특징으로 한다. In the present invention, the composition is characterized in that the formulation of the mask sheet form.
【유리한 효과】 Advantageous Effects
본 발명에 따른 PIT 유화공법을 이용한 하이드로겔 조성물은 수분과
유분을 동시에 제공함으로써 피부의 영양과 수분을 동시에 만족시킬 수 있으며, 특별한 제조 설비 없이도 간단하게 작은 입자 사이즈로 제조가 가능함으로써 경제적이면서도 효능이 높은 하이드로겔을 만들 수 있다. Hydrogel composition using the PIT emulsification method according to the invention is water and By providing oil at the same time, it can satisfy the nutrition and moisture of the skin at the same time, and can be manufactured in a small particle size simply without special manufacturing equipment, thereby making an economical and effective hydrogel.
【도면의 간단한 설명】 [Brief Description of Drawings]
도 1 및 2는 본원발명 실시예 1의 제조방법에 따라 제조된 하이드로겔의 형태를 보여주는 도면이다. 1 and 2 is a view showing the form of the hydrogel prepared according to the preparation method of Example 1 of the present invention.
도 3 및 4는 본원발명 실시예 2의 제조방법에 따라 제조된 하이드로겔의 형태를 보여주는 도면이다. 3 and 4 is a view showing the form of the hydrogel prepared according to the preparation method of the present invention Example 2.
도 5 및 6은 본원발명 실시예 3의 제조방법에 따라 제조된 하이드로겔의 형태를 보여주는 도면이다. 5 and 6 are views showing the form of the hydrogel prepared according to the preparation method of the present invention Example 3.
도 7 및 8은 본원발명 비교예 1의 제조방법에 따라 제조된 하이드로겔의 형태를 보여주는 도면이다. 7 and 8 are views showing the form of the hydrogel prepared according to the preparation method of Comparative Example 1 of the present invention.
도 9는 본원발명 비교예 2의 제조방법에 따라 제조된 하이드로겔의 형태를 보여주는 도면이다. 9 is a view showing the form of the hydrogel prepared according to the preparation method of Comparative Example 2 of the present invention.
도 10은 본원발명 실험예 1의 일반유화법과 PIT유화법의 입경사이즈 비교에 대한 결과를 나타내는 도면이다. . FIG. 10 is a view showing the results of particle size comparison between the general emulsification method and the PIT emulsification method of Experimental Example 1 of the present invention. FIG. .
도 11은 본원발명 실험예 3의 제조방법에 따라 제조된 하이드로겔의 형태를 보여주는 도면이다 (왼쪽부터 control , macadam i a oi l , dimethicone(6cs) , octyldodecyl myristate) . Figure 11 is a view showing the form of the hydrogel prepared according to the preparation method of Experimental Example 3 of the present invention (from the left control, macadam i aoi, dimethicone (6cs), octyldodecyl myristate).
도 12 및 13은 실험예 3의 제조방법에 따라 제조된 하이드로겔의 보습력 및 수분개선 테트스 결과를 나타내는 도면이다. 12 and 13 are views showing the results of moisturizing power and moisture improvement test of the hydrogel prepared according to the preparation method of Experimental Example 3.
도 14는 실시예 3의 제조방법에 따라 제조된 하이드로겔의 형태를 보여주는 도면이며, 실험예 4의 결과를 나타내는 도면이다. 14 is a view showing the form of the hydrogel prepared according to the preparation method of Example 3, showing the results of Experimental Example 4.
도 15는 실시예 2의 제조방법에 따라 제조된 하이드로겔의 형태를 보여주는 도면이며, 실험예 4의 결과를 나타내는 도면이다 (왼쪽부터 control , macadamia oi l , dimethicone , octyldodecyl myristate) .
【발명의 실시를 위한 형태】 15 is a view showing the form of the hydrogel prepared according to the preparation method of Example 2, showing the results of Experimental Example 4 (from the left control, macadamia oi l, dimethicone, octyldodecyl myristate). [Form for implementation of invention]
이하, 실시예를 통하여 본 발명을 더욱 상세히 설명하기로 한다. 이들 실시예는 단지 본 발명을 예시하기 위한 것이므로, 본 발명의 범위가 이들 실시예에 의해 제한되는 것으로 해석되지는 않는다. 실시예 1: PIT유화공정을 통한 하이드로겔의 제조 Hereinafter, the present invention will be described in more detail with reference to Examples. Since these examples are only for illustrating the present invention, the scope of the present invention is not to be construed as being limited by these examples. Example 1 Preparation of Hydrogel Through PIT Emulsification Process
하기 표 1의 조성으로 하기와 같이 제조하였다. It was prepared as follows in the composition of Table 1.
별도의 유상 용해조에 Mineral oi l , 비이온 계면활성제인 Ceteth-20 , Steareth-20 및 Glyceryl Stearate와 Cetearyl Alcohol , 방부제를 투입하고 70 ~ 85°C로 가온용해 한 후 별도 가온한 정제수를 투입하여 0/W 형태의 PIT 유화물을 제조한다. 여기에 별도의 수상 용해조에서 가온 /용해 한 수용성 겔화고분자, 다가알코을, 기타첨가제 부분올 첨가하고 충분히 가은 교반한다. 그 후, 상기 수상 용해조에 PIT 유화물을 투입한 후, 60~80°C로 넁각시키며 겔화물 (수상부) 내부로 PIT 유화물을 함침 시킨다. 내용물 제조가 완료되면 내용물을 배출하고 냉각기를 이용하여 내용물을 냉각시켜 겔화 한다. 본 발명에서는 PIT 생성온도와 하이드로겔의 용해온도와 일치가 되게 조제공법을 설계하는 것이 핵심 포인트이다. 더욱 상세하게 기술하면, 표 1에 나타낸 수상부의 조성이 용해되는 온도는 70~90°C범위에서 용해되고, 나노유화물을 하이드로겔 내부에 봉입하게 위하여는 PIT 나노유화물의 조제 은도가 동일해야 함으로 유상부에 나타낸 PIT조성으로 할 경우 PIT형성온도가 70~85°C범위에서 선택적으로 나타나는 것을 확인하였다. 이 이론을 근거로 하이드로겔을 제조할 경우 아주 파인한 나노 에멀견이 하이드로겔 내부에 패킹되는 것을 알 수 있었다. 이렇게 할 경우, 하이드로겔이 흐물흐물 거리지 않으며 탄력있고, 촉촉한 고품질의 하이드로겔을 개발할 수 있었다.
【표 1】 To separate oil melting vessel Mineral oi l, nonionic surfactant of Ceteth-20, and Steareth-20, and Glyceryl Stearate and Cetearyl Alcohol, In the preservative and then dissolved by heating at 70 ~ 85 ° C In a separate heating the purified water 0 Prepare PIT emulsions in the form of / W. Here, water-soluble gelled polymer, polyhydric alcohol, and other additive partial oligomers heated / dissolved in a separate aqueous phase dissolving tank are added thereto, and the mixture is stirred well. Then, after the PIT emulsion is added to the aqueous dissolution tank, it is angled at 60 ~ 80 ° C and impregnated the PIT emulsion into the gel (water phase). When the contents manufacturing is completed, the contents are discharged and gelated by cooling the contents using a cooler. In the present invention, the key point is to design the preparation method to be consistent with the PIT production temperature and the dissolution temperature of the hydrogel. More specifically, the temperature at which the composition of the aqueous phase portion shown in Table 1 is dissolved is in the range of 70 ~ 90 ° C., in order to encapsulate the nanoemulsion inside the hydrogel, the preparation silver of the PIT nanoemulsion should be the same. In the case of PIT composition shown in Figure 3, the PIT formation temperature was found to appear selectively in the range of 70 ~ 85 ° C. On the basis of this theory, it was found that very fine nanoemulsion dogs were packed inside the hydrogel when the hydrogel was prepared. In this case, the hydrogel did not linger and was able to develop a high quality hydrogel that was elastic and moist. Table 1
수상부 함량 Water content
Water 62.6 Water 62.6
Xanthan Gum 0.3 Xanthan Gum 0.3
CARRAGEENAN 0.4CARRAGEENAN 0.4
Gellan Gum 0.6 Gellan gum 0.6
Glycerin 1 5 Glycerin 1 5
유상부 (PIT제조부) 함량 Oil phase part (PIT manufacturing part) content
Mineral oil (미네랄오일) 7.0 Mineral oil 7.0
Ceteth-20 1 Ceteth-20 1
Steareth-20 1 Steareth-20 1
Glyceryl Stearate 1Glyceryl Stearate 1
Cetearyl Alcohol 0.5Cetearyl Alcohol 0.5
Phenoxyethanol 0.5 Phenoxyethanol 0.5
Water 10 Water 10
CaCI2 < 0.1 그 결과, 도 1 및 도 2에 나타난 바와 같이, 유백색을 띤 얇고 탄력 있는 제형이 완성됨을 알 수 있다. 실시예 2: 수용성 겔화 고분자의 종류 및 함량에 따른 PIT 유화공정을 통한 하이드로겔의 제조 CaCI 2 <0.1 As a result, as shown in Figure 1 and 2, it can be seen that the milky thin, elastic formulation is completed. Example 2: Preparation of Hydrogel through PIT Emulsification Process According to Kind and Content of Water-Soluble Gelling Polymer
하기 표 2와조성으로 실시예 1의 제조방법과 동일하게 제조하였다.
It was prepared in the same manner as in Preparation Example 1 in Table 2 and the composition.
【표 2】 Table 2
그 결과, 도 3 및 도 4에 나타난 바와 같이, 유백색을 띤 얇고 탄력있는 제형이 완성됨을 알 수 있다. 실시예 3: 수용성 겔화 고분자의 종류, 오일의 종류 및 유상부의 함량에 따른 PIT유화공정을 통한 하이드로겔의 제조 As a result, as shown in Figures 3 and 4, it can be seen that the milky thin, elastic formulation is completed. Example 3: Preparation of hydrogel through PIT emulsification process according to the type of water-soluble gelling polymer, the type of oil and the content of oil phase
하기 표 3의 조성으로 실시예 1의 제조방법과 등일하게 제조하였다.
To the composition of Table 3 was prepared in the same manner as in Example 1.
【표 3] [Table 3]
그 결과, 도 5 및 6에서 나타나는 바와 같이 오일의 종류 및 유상부 함량을 증가시킴에 따라 현탁도는 달라지나 유액타입의 하이드로겔이 잘 만들어 지는 것을 확인할 수 있다. 비교예 1: 오일 및 비이은 계면활성제를 함유하지 않은 PIT 유화공정을 통한 하이드로겔의 제조 As a result, as shown in Figures 5 and 6 as the type of oil and the content of the oil portion increases the suspension degree can be confirmed that the hydrogel of the emulsion type is well made. Comparative Example 1: Preparation of a hydrogel through the PIT emulsification process containing no oil and no silver surfactant
실시예 1의 조성물에서 유상부 (오일 비이온 계면활성제, Cetearyl Alcohol ) 를 제외한 조성물로 실시예 1의 제조방법과 동일하게 제조하였다. The composition of Example 1 was prepared in the same manner as in Preparation Example 1 except for the oil phase part (oil nonionic surfactant, Cetearyl Alcohol).
그 결과, 도 7 및 8에서 나타나는 바와 같이 투명한 형태의 하이드로겔이 만들어지는 것을 확인할 수 있다.
비교예 2: 일반 유화법을 통한 하이드로겔의 제조 As a result, it can be seen that the hydrogel of the transparent form is made as shown in Figures 7 and 8. Comparative Example 2: Preparation of Hydrogel by General Emulsification
실시예 1과 동일한 조성으로 실시하되 PIT 유화법이 아닌 일반 유화 방식으로 제조하였다. 표 4의 조성과 같이, 수상부에 수용성 겔화 고분자 및 다가알코을을 가온용해 한 후 별도의 유상부에서 비이은계면활성제 및 오일성 파부유연화제를 가온 /용해한 것을 투입하여 유화한다. 내용물 제조가 완료되면 내용물을 배출하고 냉각기를 이용하여 내용물을 냉각시켜 겔화 한다. It was carried out in the same composition as in Example 1, but prepared by the general emulsification method, not the PIT emulsification method. As shown in the composition of Table 4, the water-soluble gelling polymer and polyalcohol were dissolved in the aqueous phase and then emulsified by heating / dissolving the non-silver surfactant and the oil-based skin softener in a separate oil phase. When the contents manufacturing is completed, the contents are discharged and gelated by cooling the contents using a cooler.
【표 4] [Table 4]
그 결과, 도 9에서 나타나는 바와 같이 유화 입자사이즈가 크게 형성되어 백탁도가 높고, 겔 형성이 제대로 되지 않아 부서지는 현상이 발생되는 것을 확인 할 수 있다. 실험예 1: 일반유화법과 PIT유화법의 입경사이즈 비교 As a result, as shown in Figure 9 it can be confirmed that the emulsified particle size is formed large, the turbidity is high, the gel formation is not properly formed, the phenomenon of breakage occurs. Experimental Example 1 Comparison of Particle Sizes between General Emulsification and PIT Emulsification
본 발명에서 겔 네트워크 구조를 가진 하이드로 겔 내부에 오일을
함침시킴에 있어서 오일입자의 영향에 대하여 실험하였다. 이 실험은 본 발명의 가술적인 부분을 보다 실증적으로 제안하기 위하여 실험한 결과의 일부를 제안한다. In the present invention, the oil inside the hydrogel having a gel network structure The effect of oil particles on impregnation was tested. This experiment suggests some of the results of the experiment to suggest more empirical part of the present invention.
그러나 이 결과가 본 발명의 전부에 해당하는 것은 아니며, 일부 비교결과를 밝히고자 한다. However, this result does not correspond to all of the present invention, it is intended to reveal some comparison results.
PIT유화법을 사용한 유화제는 실시예 1에서 제조한 것으로 입경 사이즈를 측정하였다. 반면에, 일반 유화법을 이용한 에멀견계에서 사용된 유화제는 일반적으로 가장 많이 사용하고 있는 계면활성제로서 폴리솔베이트 -60과 글리세릴모노스테아레이트를 흔합하여 사용 (하기 표 5)하였으며, 제조 방법은 실시예 1과 동일하게 진행하였다. 또한, 사용농도는 PIT유화법을 이용한 계면활성제의 총 농도와 동일한 농도로 하여 실험하였다. The emulsifier using the PIT emulsification method was prepared in Example 1, and the particle size was measured. On the other hand, the emulsifier used in the emulsion system using the general emulsification method is commonly used a combination of polysorbate -60 and glyceryl monostearate as the most commonly used surfactant (Table 5), the production method It proceeded similarly to Example 1. In addition, the concentration was tested to the same concentration as the total concentration of the surfactant using the PIT emulsification method.
【표 5】Table 5
그 결과, 도 10에 나타낸 바와 같이 PIT유화법을 이용한 에멀전계에서는 미네랄오일의 농도가 3¾일 경우, 평균입경이 87nm 이었고, 5¾일 때의 평균입경은 98nm, 7%일 때의 평균 입경은 105nm로 lOOnm전후로 분포되어 있음을 알 수 있었다. As a result, as shown in FIG. 10, in the emulsion system using the PIT emulsification method, when the mineral oil concentration was 3¾, the average particle diameter was 87 nm, and when the average particle size was 5¾, the average particle diameter was 98 nm and 7%, and the average particle diameter was 105 nm. It can be seen that the distribution before and after lOOnm.
반면, 일반 유화법을 이용한 에멀견계에서는 미네랄오일의 농도가 3%일 경우, 평균입경이 5.2 μ ηι 이었고, 5¾일 때의 평균입경은 9.6 μ ηι, 7%일 때의 평균 입경은 10·5 μ ηι로, 5~10 μ ιη 범위로 아주 큰 입자를 형성하고 있음을 알 수 있었다. On the other hand, in the emulsion system using the general emulsification method, when the mineral oil concentration was 3%, the average particle diameter was 5.2 μ ηι, and when the average particle diameter was 59.6, the average particle diameter was 9.6 μηι and the average particle diameter was 7 · 5. From μ ηι, it can be seen that very large particles are formed in the range of 5 to 10 μ η.
이 결과는 하이드로겔의 내부에 패킹되는 오일의 안정성에도 큰 영향에 기인한다는 것을 부가적으로 알 수 있었다. 일반유화법을 이용한 오일은 하이드로겔 내부에 함침 되었을 때의 안정성이 아주 나빴으며, 겔의 강도도 약해져 쉽게 부서지는 현상이 발생되었다. 그러나 PIT 나노 유화물에서는 하이드로겔내부에 안정하게 로딩되어 있었으며, 안정성, 겔의 강도도 그대로 유지되면서 기본적 성능이 배가되는 것을 알 수 있었다. This result was additionally found to be due to a large effect on the stability of the oil packed inside the hydrogel. The oil using the general emulsification method was very poor when it was impregnated into the hydrogel, and the strength of the gel was also weakened, causing easy breakage. However, the PIT nano emulsions were loaded stably in the hydrogel, and the stability and the strength of the gel were maintained intact, and the basic performance was found to double.
이러한 결과로 보아 하이드로겔의 피부 효능적 측면에서도 월등히 우수한 차별성이 있을 것으로 기대하여 피부 평가에 대한 실험을 추가적으로 수행하였다. 이하 본 발명을 다음의 실시예에 의하여 설명하고자 한다. 그러나 이들은 본 발명의 일실시예로서 이들에 의해 본 발명의 권리범위가 한정되는 것은 아니다. 실험예 2: 사용감 및 피부 자극 테스트 In view of these results, the skin evaluation of hydrogels was expected to be superior to the superiority, and further experiments on skin evaluation were performed. Hereinafter, the present invention will be described by the following examples. However, these are not limited to the scope of the present invention by these as an embodiment of the present invention. Experimental Example 2: Feeling and skin irritation test
상기 실시예 1 및 비교예 1을 사용하여, 남녀 각각 15명씩 30명을 대상으로 얼굴에 20분간 부착하여 사용감 및 자극 테스트를 진행하였다. 그 결과 하기 표 6에 나타나는 바와 같이 실시예 1은 비교예 1에 비해 피부보습 및 유연성, 자극등 전체적인 평가항목에서 좋아진 것을 알 수 있다. 특히 피부보습 및 유연성에서 훨씬 높은 개선 효과를 확인할 수 있었는데, 이것은 일반적으로 제조되는 에멀견과 유사한 함량수준의 유분이 함유되면서 피부의 보습과
유연성을 높여준 것으로 예상된다 Using Example 1 and Comparative Example 1, and attached to the face for 20 minutes for each of 15 men and women each 30 minutes, the feeling and stimulation test was carried out. As a result, as shown in Table 6, Example 1 can be seen that compared to Comparative Example 1 in the overall evaluation items such as skin moisturizing and flexibility, stimulation. In particular, much improved improvement was found in skin moisturizing and suppleness, which contained oils with similar levels of oil content as commonly produced emulsion dogs. Expected to increase flexibility
【표 6】Table 6
평가기준 : 매우우수 (5점 )/우수 (4점 )/보통 (3점 )/불량 (2점 )/매우불량 (1점 ) 실험예 3: 보습력 및 수분개선 테스트 Evaluation criteria: Very good (5 points) / Excellent (4 points) / Normal (3 points) / Poor (2 points) / Very poor (1 point) Experimental Example 3: Moisturizing and moisture improvement test
상기 실험예 2를 통해 확인한 결과를 토대로 좀 더 객관적인 데이터를 얻기 위해 보습력 및 수분개선 테스트를 진행하였다. 실험은 하기 표 7과 동일한 처방에서 오일의 종류만 변경하고 실시예 1과 동일한 제조방법을 통해 제조한 후 진행하였다. 오일은 대표적인 식물성 오일 (Macadamia oi l ) , 실리콘오일 (Dimethic e 6cs) , 에스테르오일 (Octyldodecyl Myristate) 을 각각 동량 사용하였다. Based on the results confirmed through Experimental Example 2, the test was conducted to improve the moisturizing power and moisture to obtain more objective data. The experiment was carried out after the manufacture through the same manufacturing method as in Example 1 only changing the type of oil in the same prescription as in Table 7. As the oil, the same vegetable oil (Macadamia oil), silicone oil (Dimethic e 6cs) and ester oil (Octyldodecyl Myristate) were used in the same amount.
【표 7] [Table 7]
-측정 방법: 시험부위에 제품을 30분간 부착하여 흡수시킨 후, 사용 전, 제품 사용 직후 (30분), 2시간, 4시간, 8시간 간격으로 보습력을 측정한다. -Measurement method: After absorbing the product by attaching it to the test area for 30 minutes, measure the moisturizing power every 2 hours, 4 hours, 8 hours before use and immediately after use (30 minutes).
-결과 분석법: 보습력은 3회 측정한 평균값을 이용하여 산출함. -Analysis of results: Moisturizing power is calculated using the average value measured three times.
-시험 대상자: 건강한 성인 여성 18명, 남성 12명 (평균 25세) Test subjects: 18 healthy adult women and 12 males (average 25 years old)
-시험 부위: 팔 (하박 내측, 2 x 2 cm2) -Test site: arm (inner forearm, 2 x 2 cm 2 )
-측정 기기: 보습력 측정 - Corneometer CM 825 -Measuring Instrument: Moisture Measurement-Corneometer CM 825
-시험 물질: 1. Control hydrogel -Test substance: 1. Control hydrogel
2. Macadamia nut oi 1 2.Macadamia nut oi 1
3. Dimethicone(6CS) 3.Dimethicone (6CS)
4. Eutanol GM 그 결과, Control Hydrogel 등 4종 모두 무도포 군에 비해 8시간 까지 높은 피부 보습 효과를 나타냈으며, Macadamia nut oi l과 Eutanol GM은 Control Hydrogel 보다 높은 보습효과를 나타냈다 (도 11 내지 도 13) . 실험예 4: 에멀견 유효성분의 피부 전달 가능 테스트 4. Eutanol GM As a result, all four species including Control Hydrogel showed higher skin moisturizing effect up to 8 hours than the non-coating group, and Macadamia nut oil and Eutanol GM showed higher moisturizing effect than Control Hydrogel (FIG. 11 to FIG. 13). Experimental Example 4: Skin delivery test of the emulsion active ingredient
상기 실시예 2에서 만들어진 하이드로겔을 공기중에 노출시켜 방치하여 관찰하였다. 그 결과, 도 14 및 도 15에서 볼 수 있듯이, 오일의 종류에 따라 속도의 차이는 있으나 겔 내부의 함침된 유화물이 겔 외부로 빠져나와 겔이 점점 투명해지는 것을 확인할 수 있다. 이로써 하이드로겔내에 에말젼 유효성분이 매트릭스로부터 서서히 용이하게 용출되어 이수물과 함께 피부로 전달될 수 있다는 것을 확인하였다.
The hydrogel prepared in Example 2 was observed by leaving it exposed to air. As a result, as can be seen in Figures 14 and 15, there is a difference in speed depending on the type of oil, but it can be seen that the impregnated emulsion inside the gel exits the outside of the gel and the gel becomes more transparent. This confirmed that the active ingredient in the hydrogel can be easily eluted from the matrix and transferred to the skin along with the dihydrate.
Claims
【 ^구항 1】 [^ Clause 1]
하기 단계를 포함하는 PIT(Phase inversion temperature)유화공정올 통한 하이드로겔 (Hydrogel ) 조성물 제조방법: Method for preparing a hydrogel composition through phase inversion temperature (PIT) emulsification process comprising the following steps:
a) 별도의 용기에 수용성 겔화 고분자, 정제수, 다가알코을 및 가타첨가제를 포함하는 수상부를 60 내지 100°C로 가온 /교반 하는 단계; a) warming / stirring the water phase including the water-soluble gelling polymer, purified water, polyhydric alcohol, and the addition additive in a separate container at 60 to 100 ° C .;
b) 별도의 용기에 비이온성 계면활성제 및 오일성 피부유연화제를 포함하는 유상부를 60 내지 95°C로 가온 /교반하여 PIT유화물을 제조하는 단계 ; b) preparing a PIT emulsion by heating / stirring the oil phase including the nonionic surfactant and the oily skin softener in a separate container at 60 to 95 ° C .;
c) 상기 a)의 겔화물에 b)의 PIT 유화물을 투입하고 60 내지 80°C로 냉각시키며 겔화물 내부로 PIT유화물을 함침시키는 단계; 및 c) injecting the PIT emulsion of b) into the gelation of a), cooling to 60 to 80 ° C. and impregnating the PIT emulsion into the gelation; And
d) 냉각기를 통해 하이드로겔을 냉각시킨 후 성형하는단계. d) molding after cooling the hydrogel through a cooler.
【청구항 2】 [Claim 2]
제 1항에 있어서, 상기 a) 단계에서 다가알코올은 글리세린, 부틸렌글라이콜, 디프로필렌글라이콜, 프로필렌글라이콜, 헥산디을, 1 ,2- 핵산디을, 1,2-펜탄디을, 프로판디올 및 1 ,2-옥탄디을로 구성된 그룹에서 선택되는 하나 이상인 것을 특징으로 하는 하이드로겔 조성물 제조방법. According to claim 1, wherein the polyhydric alcohol in step a) glycerin, butylene glycol, dipropylene glycol, propylene glycol, hexanedi, 1,2- nucleic acid di, 1,2-pentanedi, propane Method for producing a hydrogel composition, characterized in that at least one selected from the group consisting of diol and 1,2-octanediol.
【청구항 3】 [Claim 3]
제 1항에 있어서, 상기 a) 단계에서 기타첨가제는 메칠파라핀, 프로필파라벤, 페녹시에탄올 글리세릴카프릴레이트, 에칠핵실글리세린, 카프릴릭 /카프릭글리세라이드 및 천연 추출물로 이루어진 피부컨디셔닝제로 구성된 그룹에서 선택되는 하나 이상인 것을 특징으로 하는 하이드로겔 조성물 제조방법 . The method of claim 1, wherein the other additive in step a) is a group consisting of a skin conditioning agent consisting of methyl paraffin, propyl paraben, phenoxyethanol glyceryl caprylate, ethynyl glycerin, caprylic / capric glyceride and natural extracts Method for producing a hydrogel composition, characterized in that at least one selected from.
【청구항 4】 [Claim 4]
제 1항에 있어서, 상기 b) 단계에서 비이온성 계면활성제는 글리세릴모노스테아레이트, 세테스 10~30, 세테아레스 10~30 및 스테아레스 10~30로
구성된 그룹에서 선택되는 하나 이상인 것을 특징으로 하는 하이드로겔 조성물 제조방법 . The method of claim 1, wherein in step b), the nonionic surfactant is glyceryl monostearate, cetes 10-30, ceteares 10-30 and steares 10-30. Process for producing a hydrogel composition, characterized in that at least one selected from the group consisting of.
【청구항 5】 [Claim 5]
제 1항에 있어서, 상기 b) 단계에서 오일성 피부유연화제는 탄화수소계오일, 실리콘계오일, 에스테르계오일 및 천연오일로 구성된 그룹에서 선택되는 하나 이상인 것을 특징으로 하는 하이드로겔 조성물 제조방법. The method of claim 1, wherein the oil-based skin softener in step b) is at least one selected from the group consisting of hydrocarbon-based oils, silicone-based oils, ester-based oils and natural oils.
【청구항 6】 [Claim 6]
제 1항에 있어서 , 상기 c) 단계에 PIT 에멀견은 100~500nm 평균입자크기를 갖는 것을 특징으로 하는 하이드로겔 조성물 제조방법 . [Claim 2] The method of claim 1, wherein the cit emulsion in step c) has a mean particle size of 100-500 nm.
【청구항 7】 [Claim 7]
제 1항에 있어서, 상기 a) 단계에서 수용성 고분자는 셀를로오스, 곤약, 로커스트콩 검, 캐럽콩 검, 알기네이트, 키토산, 전분, 팩틴, 알길, 구아검, 만난, 플루로니그 아라비아 검, 플루란, 콜라겐, 젤란검, 잔탄검, 카라기난, 스클레로튬검 및 한천으로 구성된 군으로부터 선택되는 하나 이상인 것을 특징으로 하는 하이드로겔 조성물 제조방법 . The method of claim 1, wherein in the step a), the water-soluble polymer is cellulose, konjac, locust bean gum, carob bean gum, alginate, chitosan, starch, pectin, allyl, guar gum, mannan, pluronig arabic gum, Method for producing a hydrogel composition, characterized in that at least one selected from the group consisting of pullulan, collagen, gellan gum, xanthan gum, carrageenan, sclerotium gum and agar.
【청구항 8] [Claim 8]
제 1항의 제조방법에 따라 제조된 하이드로겔 조성물. 【청구항 9】 Hydrogel composition prepared according to the method of claim 1. [Claim 9]
제 8항에 있어서, 상기 조성물은 조성물 총 중량 대비 겔화 고분자 0.1 내지 10 중량 %, 다가알코을 0.1 내지 30중량 비이온성 계면활성제 0.1 내지 20중량 % 및 피부유연화제 0.1 내지 30중량 % 함유하는 것을 특징으로 하는 하이드로겔 조성물.
【청구항 10】 The composition of claim 8, wherein the composition contains 0.1 to 10% by weight of gelling polymer, 0.1 to 20% by weight of polyhydric alcohol, 0.1 to 20% by weight of nonionic surfactant, and 0.1 to 30% by weight of skin softener. Hydrogel composition. [Claim 10]
제 8항에 있어서, 상기 조성물은 마스크시트 형태의 제형인 것을 특징으로 하는 하이드로겔 조성물.
The hydrogel composition of claim 8, wherein the composition is in the form of a mask sheet.
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CN106619321A (en) * | 2017-02-11 | 2017-05-10 | 佛山市芊茹化妆品有限公司 | Face mask containing oily components |
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