WO2017003080A1 - Dispersion solution containing solid lipid microparticles of surfactant-free system, and cosmetic composition using same - Google Patents

Abstract

The present invention relates to a dispersion solution containing solid lipid microparticles of a surfactant-free system, and a cosmetic composition using the same, and provides: a dispersion solution containing solid lipid microparticles having improved temperature stability and an excellent appearance quality in accordance with the remarkable deterioration of thermal behavior of the solid lipid microparticles in a specific combination; and a cosmetic composition using the same.

Description

Dispersion containing solid lipid fine particles of surfactant-free system and cosmetic composition using same

The present invention relates to a dispersion comprising a solid lipid microparticles of a surfactant-free system and a cosmetic composition using the same, and to a dispersion comprising a solid lipid microparticles having high stability and excellent appearance quality even at high temperatures and a cosmetic composition using the same.

Solid lipid nanoparticles (SLNs) and nanostructures lipid carriers (NLCs) have been developed as alternative carrier systems for emulsions, liposomes, and polymeric nanoparticles and are active It can increase the chemical stability of ingredients, increase skin hydration through occlusive effect, increase the bioavailability of active ingredients in skin, and physical stability of topical preparations. Due to the advantage that can increase, has recently gained great popularity in the cosmetic field. However, since the SLN and NLC are too stable to take a long time to release the drug, there is a need for a method that can effectively release the drug in order to overcome this, and when applied to the oil-in-water formulation, Due to the imbalance of the wax-lipid combination, it is difficult to secure stability.

Accordingly, in order to improve the above-described problems, the present inventors search for a dispersion containing solid lipid particles of a specific combination with a small change in structure according to temperature change, and when the crystal melting temperature and the recrystallization temperature satisfy a specific range, The present invention has been completed by discovering that dispersions containing solid lipid particulates with excellent stability can be prepared.

It is an object of the present invention to provide a cosmetic composition having a function of excellent appearance differentiation and improved skin moisturizing effect by using a dispersion including solid lipid microparticles having a high temperature stability.

In order to solve the object of the present invention, the present invention provides a dispersion comprising solid lipid microparticles including wax, lipids and oils, and satisfying the following formulas 1 and 2

[Equation 1]

40 <Tm ₁ <80

[Equation 2]

28 <Tm ₂ <55

 [Equation 1 or 2,

Tm ₁ is the maximum temperature value of the crystal melting temperature at heating;

Tm ₂ is the maximum temperature value of the recrystallization temperature at reduced temperature]

In another aspect, the present invention provides a cosmetic composition that is excellent in high temperature stability including a dispersion that satisfies the formula 1 and formula 2.

Although the dispersion including the solid lipid particles according to the present invention is a surfactant-free system, it has excellent emulsion stability and excellent formulation stability according to temperature, so that it can be effectively applied to a water gel base, and excellent skin stability and trouble generation are minimized. It has the advantage of being able to.

In addition, the dispersion containing the solid lipid particles according to the present invention effectively inhibits coalescence or aggregation, which not only has a differentiated appearance, but also provides excellent moisture with a smooth application while melting at skin temperature, and is excellent when applied to the skin. Occlusion effect has the advantage of providing a high moisturizing power and skin suppleness.

In addition, the dispersion containing the solid lipid particles according to the present invention has the advantage of providing a high moisture feeling of the solubilization formulation and the oiliness of the emulsified formulation, moisturizing sustainability at the same time.

The cosmetic composition using the dispersion including the solid lipid fine particles according to the present invention has a function of enhancing or decreasing skin absorption by a change in phase, thereby providing a cosmetic composition with optimized skin absorption tendency.

FIG. 1 shows an analysis result using differential scanning calorimetry (DSC) of solid lipid particles in Example 1 composition.

Figure 2 shows the analysis results using differential scanning calorimetry (DSC) of the solid lipid particles in the composition of Example 7.

FIG. 3 shows an analysis result using differential scanning calorimetry (DSC) of solid lipid particles in Example 9 composition.

Figure 4 shows the analysis results using differential scanning calorimetry (DSC) of the solid lipid particles in the composition of Example 10.

Figure 5 shows the results of analysis using differential scanning calorimetry (DSC) of the solid lipid particles in the composition of Example 11.

FIG. 6 shows the results of analysis using differential scanning calorimetry (DSC) of solid lipid particles in the composition of Example 12.

FIG. 7 shows an analysis result using differential scanning calorimetry (DSC) of solid lipid particles in Example 13 composition.

FIG. 8 shows an analysis result using differential scanning calorimetry (DSC) of solid lipid particles in Comparative Example 1 composition.

9 is a photograph confirming the restoring force of the dispersion prepared in Example 7 and Comparative Example 1.

The dispersion including the solid lipid fine particles of the surfactant-free system according to the present invention and the cosmetic composition using the same are described below, but unless otherwise defined in the technical terms and scientific terms used at this time, the present invention generally includes The person skilled in the art has a general understanding, and in the following description, descriptions of well-known functions and configurations that may unnecessarily obscure the subject matter of the present invention will be omitted.

Conventional solid lipid nanoparticles (SLN) and nanostructured lipid carriers (NLC) are susceptible to changes in temperature over time when applied to cosmetic compositions, and therefore, recrystallization of waxes or lipids at low temperatures is difficult. It occurs at the high temperature or the melting of the wax or lipids has a problem of poor stability, such as poor usability, viscosity of the formulation, turbidity in the formulation.

Accordingly, the present applicant has further intensified research on the structural change according to the temperature change of each component included in the solid lipid microparticles through DSC, and as a result, the thermal stability of the solid lipid microparticles in certain combinations significantly lowers the stability. It has been found that the eggplant can be prepared a dispersion, the dispersion satisfies the following formulas 1 and 2, and includes solid lipid particles having a wax, a lipid and an oil.

[Equation 1]

40 <Tm ₁ <80

[Equation 2]

28 <Tm ₂ <55

[Equation 1 or 2,

Tm ₁ Is the maximum temperature value of the crystal melting temperature at heating;

Tm ₂ is the maximum temperature value of the recrystallization temperature at reduced temperature]

The solid lipid microparticles according to an embodiment of the present invention may give a visual cognitive effect through appearance discrimination and visualization in which skin active ingredients are absorbed as a stable dispersion having a stable stability, and as a conventional surfactant as a surfactant-free system. It can minimize the skin irritation or troubles caused, it can be applied to sensitive skin products.

As used herein, the term "lipid" refers to a single-chain lipid, and may be one or more selected from linear saturated alcohols and linear saturated fatty acids, but is not limited thereto.

In addition, the term "full width at half maximum" of the present invention means the range of temperature change (ΔT) based on the half height with respect to the peak of the melting temperature and recrystallization temperature by DSC analysis. do.

In the case of the warm-up crystal melting temperature (Tm ₁ ) according to the present invention, it shows a soft coating feeling while melting at the skin temperature, preferably in the range of the following Equation 3 in terms of imparting an excellent moisture and moisture to the skin But it is not limited thereto.

[Equation 3]

40 <Tm ₁ <80

In addition, in the case of the recrystallization temperature (Tm ₂ ) at the time of temperature reduction according to the present invention, the improved high temperature stability, and due to the fast recovery force may be in the range of the following Equation 4 preferably in terms of transparency of the trauma, but is not limited thereto. no.

[Equation 4]

28 <Tm ₂ <40

The crystal melting temperature and the recrystallization temperature of the dispersion according to an embodiment of the present invention each have one peak, it is advantageous that the dispersion of the crystal melting temperature and recrystallization temperature range is low. The low dispersion of the crystal melting temperature and the recrystallization temperature range may mean that the structural change according to the temperature change is small, and thus the low temperature and high temperature stability of the solid lipid particles may be remarkably improved.

In this aspect, more preferably, the full width at half maximum (ΔT m ₁ ) of the crystal melting temperature at heating is in the range of 1 to 5 ° C. or at the full width at the temperature of recrystallization at low temperature. half maximum, △ T m ₂ ) is a low dispersion that satisfies the range of 1 to 5 ℃ is good in terms of stability of the high dispersion according to the temperature change, the resilience of the solid lipid particles when the temperature is lowered to room temperature at a high temperature (above 45 ℃) In this excellent aspect, the half-height width value of the recrystallization temperature at low temperature must satisfy the range of 1 to 5 ° C.

The solid lipid particles according to an embodiment of the present invention may be one containing one or more waxes selected from vegetable waxes, animal waxes, mineral waxes and synthetic waxes, non-limiting example of the wax candelilla Wax, Carnauba Wax, Rice Wax, Cotton Wax, Berry Berry Wax, Chinese Insect Wax, Sugar Cane Wax, Jojoba Wax, Shea Butter, Sunflower Wax, Hydrogenated Vegetable Oil, Hydrogenated Olive Vegetable waxes including oil stearyl esters, hydrogenated olive oil dodecyl esters, and the like; Animal waxes including beeswax, lanolin and the like; Mineral waxes including ozokerite, ceresin wax, microcrystalline wax, multi wax, paraffin wax and the like; Synthetic waxes including polyethylene wax, POE (polyoxyethylene) lanolin alcohol ether wax, POE lanolin alcohol acetate wax, POE cholesterol ether wax, lanolin fatty acid polyethylene glycol wax, POE hydrogenated lanolin alcohol ether wax, and the like; It may be one or more selected from, but not limited to this, it is preferable that the wax corresponding to the temperature range of 50 to 80 ℃ in terms of providing not only the stability of the solid lipid particles but also excellent oiliness and moisturizing sustainability at the same time, more preferably Examples include candelilla wax, carnauba wax, rice wax, berryberry wax, jojoba wax, shea butter, sunflower seed wax, hydrogenated olive oil stearyl ester, hydrogenated olive oil dodecyl ester, and the like. It is preferable to include at least one wax selected from synthetic waxes including vegetable waxes, microcrystalline waxes, mineral waxes including multi waxes, paraffin waxes, and the like.

The oil may be one or more oils selected from hydrocarbon oils, ester oils, triglyceride oils, vegetable oils and silicone oils. Non-limiting examples of the oils include squalane, mineral oil, hydrogenated polydecene ( hydrocarbon-based oils including hydrogenated polydecene), hydrogenated polyisobutene, and the like; Isopropyl palmitate, 2-octyldodecyl myristate, isopropyl myrister, butyloctyl salicylate, cetyl octanoate, cetyl octyl hexanoate, coco caprylate / caprate, decyl cocoate, isostere Ester oils including arylisostearate, pentaerythritol tetraethylhexanoate, dicaprylylcarbonate, and the like; Vegetable oils including castor oil, olive oil, jojoba oil, avocado oil, macadamia oil, meadowfoam seed oil and the like; And oils selected from dimethylpolysiloxane, methylphenylpolysiloxane, decamethylcyclopentasiloxane, methyl chrymethicone, phenyltrimethicone, cyclomethicone, dimethicone, and the like; Vegetable oils including jojoba oil, avocado oil, meadowfoam seed oil, and the like, in terms of excellent usability and low solubility in waxes or lipids; Hydrocarbon-based oils such as squalane, hydrogenated polydecene, hydrogenated polyisobutene, and the like; Ester-based oils including 2-octyldodecyl myristate, cetyl octyl hexanoate, isopropyl myrister, butyloctyl salicylate, pentaerythritol tetraethylhexanoate, dicaprylylcarbonate and the like; One or more oils are good. In this case, when the solubility in wax or lipid in the oil is increased, the melting point of the dispersion is lowered, and when the solubility is lowered, the melting point of the dispersion is increased, and when using the linear hydrocarbon oil as described above, It is preferable to implement a melting point.

In addition, the lipid may be one or more selected from higher fatty alcohols of C10-C30 and higher fatty acids of C10-C30, and has a high solubility in the oil and may be high in C10-C30 in terms of melting at skin temperature and showing a soft coating. Preference is given to using fatty alcohols. At this time, a non-limiting example of the higher fatty alcohol may include one or more lipids selected from cetyl alcohol, stearyl alcohol, cetostearyl alcohol, behenyl alcohol and the like, but is not limited thereto.

The solid lipid microparticles according to one embodiment of the present invention may include 50 to 150 parts by weight of lipids and 100 to 500 parts by weight of oil, based on 100 parts by weight of wax, preferably based on wax 1 The oil should be mixed in a 1: 2 ratio and 1: 5 ratio.

The aqueous phase of the trauma of the dispersion according to an embodiment of the present invention may further include an aqueous phase thickener for stable dispersion of the solid lipid particles. At this time, the water thickener is not limited as long as it is a substance used to improve the viscosity of the water phase in the art, polyacrylic acid, polyacrylamide, polymethacrylic acid, polyhydroxyethyl methacrylate, polyacrylic acid-polymetha Krylic acid copolymer, polyacrylic acid-polyacrylamide copolymer, polymethacrylic acid-polyacrylamide copolymer, polyethylene glycol, poly (N, N-ethylaminoethyl methacrylate), hyaluronic acid, agar, chitosan, ammonium May include one or more aqueous thickeners selected from acryloyldimethyltorate-VPicopolymers, xanthan gums, celluloses, cellulose ethers, polyvinyl derivatives, alginates and polyacrylates or substituted with hydrophobic groups. It has low emulsifying power, improves stability of formulation and transparency of product, Polyacrylic acid not substituted with a hydrophobic group in view of having a number of restoration properties; Polyacrylamide; And polymethacrylic acid; Copolymers alone or in combination are preferred.

The viscosity of the dispersion according to an embodiment of the present invention is preferably in the range of 10,000 to 50,000 cps, preferably in the range of 10,000 to 30,000 cps in terms of stable dispersibility and excellent spreadability of the solid lipid particles, but is not limited thereto. It is not.

In addition, the average diameter of the solid lipid particles may range from 10 nm to 20 mm, may range from 50 nm to 10 mm, and may range from 100 nm to 10 mm in terms of phase stability and optimum stability according to temperature. However, it is not limited thereto.

The present invention provides a cosmetic composition comprising a dispersion that satisfies the following formula 1 and formula 2.

[Equation 1]

40 <Tm ₁ <80

[Equation 2]

28 <Tm ₂ <55

[Equation 1 or 2,

Tm ₁ Is the maximum temperature value of the crystal melting temperature at heating;

Tm ₂ is the maximum temperature value of the recrystallization temperature at reduced temperature]

The cosmetic composition may contain a dispersion that satisfies the above range, may give a good moisture while melting at the skin temperature, and can provide high moisturizing power and skin suppleness through excellent occlusion effect when applied to the skin. .

In addition, the cosmetic composition may have a function of enhancing or decreasing skin absorption by a change of phase, thereby providing a cosmetic composition with optimized skin absorption tendency.

The cosmetic composition according to an embodiment of the present invention may further include fragrances, pigments, preservatives, fungicides, oxidative stabilizers, pearls and the like within a range that does not inhibit the effect of the dispersion.

Hereinafter, the present invention will be described in more detail based on the following examples. However, the following examples are not intended to limit the invention only.

(Examples 1 to 15 and Comparative Example 1)

The waxes, lipids, and oils were completely dissolved at 85 ° C. according to the compositions of Tables 1 to 2 to form an oil phase, and then a thickener of the following composition was added to form an aqueous phase (water gel base) having a viscosity of 15,000 cps (centi poise). After the addition, the mixture was stirred at room temperature with an azi mixer to prepare a dispersion including solid lipid particles (average diameter: 3 mm).

Raw material name Example One 2 3 4 5 6 7 8 9 10 Wax Multiwax 0.6 - - - 0.6 0.6 0.6 0.6 0.6 Jojoba esters - 0.6 - - - - - - - Sunflower seed wax - - 0.6 - - - - - - Hydrogenated Stearyl Olive Esters - - - 0.6 - - - - - Shea butter - - - - 0.6 - - - - Geology Cetyl alcohol - - - - - - 0.7 0.7 0.7 0.7 CETEARYL ALCOHOL - - - - 0.35 - - - Stearic acid 0.7 0.7 0.7 0.7 0.7 0.35 - - - oil Squalane - - - - - - - 2 - - Hydrogenated Polydecene 2 2 2 2 2 2 2 - - - Pentaerythrityl Tetraethylhexanoate - - - - - - - - 2 - Octyldodecyl Myristate - - - - - - - - - 2 Thickener Cabomer 0.4 - 0.4 0.4 0.4 0.4 0.4 0.4 0.4 Acrylates.C10-30 Alkyl Acrylate Crosspolymer 0.4 0.3 - - - - - - - Ammonium AcryloyldimethyltaurateVP Copolymer 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 Hydroxyethyl Acrylate.Sodium Acryloyldimethyl Taurate Copolymer - 0.2 - - - - - - - Other additives Polyol 20 20 20 20 20 20 20 20 20 20 water To 100 To 100 To 100 To 100 To 100 To 100 To 100 To 100 To 100 To 100

Raw material name Example Comparative Example 1 11 12 13 14 15 Wax Hydrogenated castor oil - - - 0.6 Multiwax 0.6 0.6 0.6 0.6 - - Jojoba esters - - - 0.6 - Geology Cetyl alcohol 0.7 0.7 0.7 - - - CETEARYL ALCOHOL - - 0.7 - - Behenyl alcohol - - - - 0.6 - Stearic acid - - - - - 0.7 oil Squalane - - - - - Hydrogenated Polydecene - - - 2 4 2 Pentaerythrityl Tetraethylhexanoate - - - - - - Octyldodecyl Myristate - - - - - - Cetyl ethyl hexanoate 2 - - - Dicaprylyl Carbonate 2 - - - - MeadowfoamSeed Oil - 2 - - - Thickener Cabomer 0.4 0.4 0.4 0.4 0.4 0.4 Other additives Polyol 20 20 20 20 20 20 water To 100 To 100 To 100 To 100 To 100 To 100

DSC analysis of the solid lipid particles of the solid lipid particle dispersion in Examples 1 to 15 and Comparative Example 1 was carried out under the following conditions and the results are shown in FIGS.

(DSC analysis condition)

DSC was used as CSC (4100DSC, Calorimetry Science Corporation, Lindon, Utah, United States). One pan was used as a reference material without filling a sample, and each sample was filled with a sample of each of the solid lipid fine particles prepared in Examples 1 to 15 and Comparative Example 1, respectively. The reference pan, which did not fill the sample, became the reference material, which was set as the baseline, and the thermal flow of the remaining samples was compared and analyzed. The temperature range to be measured was measured at 5 ° C./min from 25 ° C. to 85 ° C., and the results are shown in FIGS. 1 to 8 and Table 3 below.

Example Comparative Example 1 One 7 9 10 11 12 13 Tm ₁ 42 42.5 42.5 41 37.5 43 38 43 Tm ₂ 35 36 34 32.5 29 33 29 36 ΔTm ₂ 2.5 2.0 1.8 4.8 2.5 3.0 2.0 7.0

As shown in Figures 1 to 7, the solid lipid particles according to the present invention, the crystal melting temperature and the recrystallization temperature each has a single peak crystal melting temperature value, the half-height width of the recrystallization temperature at reduced temperature according to the present invention By having a single peak satisfactory, it was found that the crystallization rate was fast and the resilience of the solid lipid fine particles in the formulation was excellent.

On the contrary, as shown in FIG. 8, in Comparative Example 1, the crystallization temperature had a large range of structural changes according to the temperature, and the recrystallization temperature also had a wide range, indicating that the crystallization rate was slow. .

That is, the solid lipid particles satisfying the formulas 1 and 2 according to the present invention has a low dispersion crystal melting temperature range and recrystallization temperature range by minimizing thermal behavior and suppressing structural changes due to temperature changes, thereby further improving. Emulsification stability and excellent temperature stability can be represented.

In addition, in order to confirm the formulation stability according to the temperature, each of the dispersion prepared in Examples 1 to 15 and Comparative Example 1 was put in a vial having a content of 20 g room temperature (25 ± 2 ℃), cold and thermostat (4 ± 2 ℃ ), High temperature thermostat (45 ± 2 ℃) and cycle chamber (Freeze-Thaw Chamber, cycle from -20 ℃ to 45 ℃ once a day) and store and check the formulation stability of each sample at weekly interval. The results are shown in Table 4 below.

Example 1 Example 5 Example 7 Comparative Example 1 Room temperature (1 week / 2 weeks / 3 weeks / 4 weeks) ◎ / ◎ / ◎ / ◎ ◎ / ◎ / ◎ / ◎ ◎ / ◎ / ◎ / ◎ ◎ / ◎ / ◎ / ◎ Cold and Hot Tub ◎ / ◎ / ◎ / ◎ ◎ / ◎ / ◎ / ◎ ◎ / ◎ / ◎ / ◎ ◎ / ○ / ○ / △ High Temperature Bath ◎ / ○ / ○ / △ ◎ / ○ / △ / △ ◎ / ◎ / ◎ / ◎ △ / △ / × / × Cycle chamber ◎ / ○ / △ / △ ◎ / ○ / △ / △ ◎ / ◎ / ◎ / ◎ ○ / △ / △ / ×

◎: stable; No separation of oil or water and recovery of solid lipid particles

○: relatively stable; There is no separation of oil or water and solid lipid particles are restored but become slightly transparent

△: relatively poor; Oil or water is weakly separated (0.1 cm or less), solid lipid fine particles become transparent

×: very bad; The oil or water is very severely separated and layered (0.1 cm or more), the solid lipid particles become transparent and the trauma becomes opaque.

As shown in Table 4, in the case of the dispersion according to the present invention, it was confirmed that the formulation stability for each temperature compared to Comparative Example 1 is very excellent, as shown in Figure 9, when placed at a high temperature and then turned to room temperature It was found that the shape of the solid lipid particles could be restored to maintain a transparent aqueous gel base. However, in the case of Comparative Example 1, it was found that the formulation stability decreased with temperature, and in particular, that the high temperature stability was remarkably lowered, and when it was put at high temperature and returned to room temperature, the shape of the solid lipid fine particles was dissociated in the aqueous phase without being restored to white water stability. Not only did this fall, but discoloration of the formulation (eg, browning occurred in yellow) occurred.

That is, by using the dispersion containing the solid lipid microparticles having a specific composition according to the present invention, it can have a significantly improved low temperature and high temperature stability compared to the dispersion containing the solid lipid microparticles in the prior art, and have a smooth feeling of use, smooth appearance with excellent appearance quality It is possible to provide an excellent skin cosmetic composition capable of imparting skin feel and improved moisture.

Claims (12)

A dispersion liquid comprising solid lipid fine particles comprising a wax, a lipid and an oil, and satisfying the following Equations 1 and 2 below. [Equation 1] 40 <Tm ₁ <80 [Equation 2] 28 <Tm ₂ <55 [Equation 1 or 2, Tm ₁ is the maximum temperature value of the crystal melting temperature at heating; Tm ₂ Is the maximum temperature of recrystallization temperature at reduced temperature] The method of claim 1, The crystal melting temperature and the recrystallization temperature is characterized in that each having one peak. The method of claim 2, The full width at half maximum (ΔT m ₂ ) of the recrystallization temperature at the time of temperature reduction is 1 to 5 ℃ dispersion. The method of claim 1, Wherein said solid lipid particulates comprise at least one wax selected from vegetable waxes, animal waxes, mineral waxes and synthetic waxes. The method of claim 4, wherein Wherein said lipid is at least one selected from higher fatty alcohols of C10-C30 and higher fatty acids of C10-C30. The method of claim 5, Wherein said oil is at least one oil selected from hydrocarbon oils, ester oils, triglyceride oils, vegetable oils and silicone oils. The method of claim 4, wherein Wherein said solid lipid microparticles comprise 50 to 150 parts by weight of lipid and 100 to 500 parts by weight of oil, based on 100 parts by weight of wax. The method of claim 1, Wherein said dispersion further comprises an aqueous thickener. The method of claim 8, The water thickeners include polyacrylic acid, polyacrylamide, polymethacrylic acid, polyhydroxyethyl methacrylate, polyacrylic acid-polymethacrylic acid copolymer, polyacrylic acid-polyacrylamide copolymer, polymethacrylic acid-poly Acrylamide Copolymer, Polyethylene Glycol, Poly (N, N-Ethylaminoethyl Methacrylate), Hyaluronic Acid, Agar, Chitosan, Ammonium Acryloyldimethyltorate V-Polypolymer, Xanthan Gum, Cellulose, Cellulose Ether, Poly At least one dispersion selected from vinyl derivatives, alginates and polyacrylates. The method of claim 1, The viscosity of the dispersion ranges from 10,000 to 50,000 cps. The method of claim 1, The dispersion of the solid lipid particles has an average diameter of 10 nm to 20 mm. Cosmetic composition containing the dispersion liquid in any one of Claims 1-11.

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