A nanobionic bicontinuous phase microencapsulate and method of making the same

Abstract

The application belongs to the technical field of cosmetic manufacturing, and discloses a nano-bionic double-continuous-phase microcapsule package and a preparation method thereof, which comprises the following steps: respectively performing constant-temperature water bath dissolution on an oil phase mixture and a mixture, uniformly stirring, homogenizing to a nano-scale stable and uniform state, taking active substances to be wrapped, dissolving the active substances with squalane, adding again, and adding an aqueous phase mixture to perform high-pressure homogenization. By wrapping the water-insoluble active substances into water-soluble ones, the stability of light- and heat-sensitive active ingredients can be improved, the skin irritation of part of the active ingredients can be reduced, the action time can be prolonged, the transdermal absorption is good, the skin biocompatibility is good, and the safety is higher.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of cosmetic manufacturing, and more particularly to a nano-bionic double-continuous-phase microcapsule and a preparation method thereof. BACKGROUND

[0002] Double-continuous-phase refers to a multi-layer emulsion formed by dispersing one emulsion in another continuous phase. Common multi-emulsions are mainly divided into two categories: water-in-oil-in-water (W / O / W) and oil-in-water-in-oil (O / W / O).

[0003] Microcapsules are microcapsules in which solid, liquid or gaseous particles are encapsulated in a semi-permeable or sealed capsule membrane with a diameter of 1-500 microns by using certain technical methods, innovative processes and specific equipment, using natural or synthetic polymer materials. The substances in the microcapsules can be isolated from the environment and are more stable. Under appropriate conditions and means, the encapsulated substances can achieve controlled release.

[0004] At present, the effective components of cosmetics are various, some of which have remarkable effects, but also have application problems such as poor compatibility, crystallization, inactivation, difficult emulsification and stability, irritation, and poor transdermal absorption, making it difficult to achieve its own efficacy. Therefore, in the field of cosmetic manufacturing technology, the double-continuous-phase microcapsule encapsulation technology is introduced to improve the stability of the effective components, reduce the irritation to the skin, and prolong the action time, which is a problem to be solved at present. SUMMARY

[0005] In order to solve the above problems, the present application provides a nano-bionic double-continuous-phase microcapsule and a preparation method thereof.

[0006] The nano-bionic double-continuous-phase microcapsule and the preparation method thereof provided by the present application adopt the following technical scheme:

[0007] A nano-bionic double-continuous-phase microcapsule preparation method, comprising the following steps:

[0008] Step 1: Take squalane, dipalmitoyl hydroxyproline, glycosphingolipids and glycolipids and mix to obtain an oil phase mixture A;

[0009] Step 2: Take hyaluronic acid and collagen, add pure water and mix to obtain a water phase mixture A;

[0010] Step 3: The oil phase mixture A and the water phase mixture B obtained in steps 1 and 2 are respectively dissolved in a constant temperature water bath, and then the water phase mixture A is added to the oil phase mixture A at a uniform speed after stirring with a magnetic stirrer, and the initial emulsion A is obtained after secondary stirring;

[0011] Step 4: The initial emulsion A prepared in step 3 is added to a high-pressure homogenizer, and is homogenized to a nano-sized stable and uniform state to obtain a transparent oily inclusion as material A for standby;

[0012] Step 5: Take ultrapure water, hydrogenated phosphatidylcholine, heat and dissolve in a water bath, and magnetically stir for 15 min to obtain water phase mixture B;

[0013] Step 6: Take the active substance to be encapsulated, dissolve in squalane, and then add the material A prepared in step 4, and continue to stir uniformly to obtain oil phase mixture B;

[0014] Step 7: The oil phase mixture B obtained in step 6 is added to the water phase mixture B obtained in step 5, and continues to stir for 15 min to obtain an initial emulsion B;

[0015] Step 8: The initial emulsion B prepared in step 7 is added to a high-pressure homogenizer to obtain a bicontinuous phase microcapsule inclusion emulsion with a particle size of 100-200 nm.

[0016] Further, the oil phase mixture A in step 1 comprises, by weight fraction: squalane 50-85 parts, dipalmitoyl hydroxyproline 1-5 parts, glycosphingolipid 1-5 parts, and glycolipid 1-5 parts.

[0017] Further, the water phase mixture A in step 2 comprises, by weight fraction: pure water 5-25 parts, hyaluronic acid 1-5 parts, and collagen 1-5 parts.

[0018] Further, in step 3, the temperature of the constant temperature water bath is 45°C.

[0019] Further, the stirring speed in step 3 is 500-600 rmp, and the stirring time is 15 min twice.

[0020] Further, the water phase mixture B in step 5 comprises, by weight fraction: ultrapure water 60-85 parts, and hydrogenated phosphatidylcholine 1-5 parts.

[0021] Further, the oil phase mixture B in step 6 comprises, by weight fraction: squalane 5-10 parts, and material A 5-15 parts.

[0022] Further, the active substance in step 6 includes at least one of HPR, ceramide, resveratrol, and rose essential oil.

[0023] The application also provides a nano-bionic bicontinuous phase microcapsule inclusion prepared according to the above method.

[0024] In summary, the application includes at least one of the following beneficial technical effects:

[0025] (1) By wrapping the water-insoluble active into water-soluble, promoting penetration, prolonging release time, directional release, it can improve the stability of light and heat sensitive active ingredients, reduce the irritation of some active ingredients to the skin, and prolong the action time;

[0026] (2) Due to its unique special structure of continuous phase molecular layer / inner and outer water phase (middle oil phase), it can realize the common delivery of fat-soluble active ingredients and water-soluble active ingredients, and provide an ideal solution for the problems of poor skin penetration of active peptides, poor stability and difficult combination use;

[0027] (3) It has good transdermal absorption and good skin biocompatibility, and is safer;

[0028] (4) The small particles in the dispersed phase can be uniformly distributed on the skin surface and gradually released over time, achieving a lasting skin care effect. BRIEF DESCRIPTION OF DRAWINGS

[0029] Figure 1 The particle size average distribution diagram of the microcapsule encapsulated body emulsion prepared in Example 1 of the present application;

[0030] Figure 2 The particle size average distribution diagram of the microcapsule encapsulated body emulsion prepared in Example 2 of the present application;

[0031] Figure 3 The particle size average distribution diagram of the microcapsule encapsulated body emulsion prepared in Example 3 of the present application. DETAILED DESCRIPTION

[0032] The technical solutions in the embodiments of the present application will be described clearly and completely in combination with the drawings in the embodiments of the present application; obviously, the described embodiments are only part of the embodiments of the present application, not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0033] In the embodiments, the experimental methods used are conventional methods, and the materials, reagents, etc. used are commercially available unless otherwise specified.

[0034] Example 1:

[0035] A preparation method of a nano-bionic bicontinuous phase microcapsule encapsulated body, comprising the following steps:

[0036] Step 1: Mix squalane 65 parts, dipalmitoyl hydroxyproline 3 parts, glycosphingolipid 2 parts and glycolipid 3 parts by weight fraction to obtain oil phase mixture A;

[0037] Step 2: Take hyaluronic acid 3 parts and collagen 2 parts by weight fraction, add pure water 22 parts to mix, obtain water phase mixture A;

[0038] Step 3: The oil phase mixture A and water phase mixture B obtained in steps 1 and 2 respectively are dissolved in a constant temperature water bath at 45℃, stirred with a magnetic stirrer at 500-600rmp for 15min, then the water phase mixture A is added to the oil phase mixture A at a uniform speed, stirred for another 15min to obtain the initial emulsion A;

[0039] Step 4: The initial emulsion A prepared in step 3 is added to a high-pressure homogenizer, and is homogenized to a nano-sized stable and uniform state to obtain a transparent oily inclusion body as material A for standby;

[0040] Step 5: Take ultrapure water 65 parts, hydrogenated phosphatidylcholine 5 parts by weight fraction, heat and dissolve in a water bath, and stir with a magnetic stirrer for 15min to obtain water phase mixture B;

[0041] Step 6: Take the active substance HPR 5 parts to be wrapped, dissolve with squalane 10 parts, then add the material A 15 parts prepared in step 4, and continue to stir uniformly to obtain the oil phase mixture B;

[0042] Step 7: The oil phase mixture B obtained in step 6 is added to the water phase mixture B obtained in step 5, and stirred for another 15min to obtain the initial emulsion B;

[0043] Step 8: The initial emulsion B prepared in step 7 is added to a high-pressure homogenizer to obtain a bicontinuous phase microcapsule inclusion emulsion with a particle size of 100nm-200nm.

[0044] Example 2:

[0045] A preparation method of a nano-bionic bicontinuous phase microcapsule inclusion body, comprising the following steps:

[0046] Step 1: Take squalane 65 parts, dipalmitoyl hydroxyproline 3 parts, glycosphingolipid 2 parts and glycolipid 3 parts by weight fraction, and mix to obtain an oil phase mixture A;

[0047] Step 2: Take hyaluronic acid 3 parts and collagen 2 parts by weight fraction, add pure water 22 parts to mix, obtain water phase mixture A;

[0048] Step 3: The oil phase mixture A and water phase mixture B obtained in steps 1 and 2 respectively are dissolved in a constant temperature water bath at 45℃, stirred with a magnetic stirrer at 500-600rmp for 15min, then the water phase mixture A is added to the oil phase mixture A at a uniform speed, stirred for another 15min to obtain the initial emulsion A;

[0049] Step 4: The initial emulsion A prepared in step 3 is added to a high-pressure homogenizer, and is homogenized to a nano-sized stable and uniform state to obtain a transparent oily inclusion body as material A for standby;

[0050] Step 5: Take 65 parts of ultrapure water and 5 parts of hydrogenated phosphatidylcholine by weight fraction, heat and dissolve in a water bath, and magnetically stir for 15 min to obtain water phase mixture B;

[0051] Step 6: Take 5 parts of active substance ceramide that needs to be encapsulated, and then add 10 parts of squalane, and then add 15 parts of material A prepared in step 4, and continue to stir uniformly to obtain oil phase mixture B;

[0052] Step 7: The oil phase mixture B obtained in step 6 is added to the water phase mixture B obtained in step 5, and continues to stir for 15 min to obtain an initial emulsion B;

[0053] Step 8: The initial emulsion B prepared in step 7 is added to a high-pressure homogenizer to obtain a bicontinuous phase microcapsule inclusion emulsion with a particle size of 100-200 nm.

[0054] Example 3:

[0055] A preparation method of a nano-bionic bicontinuous phase microcapsule inclusion body, comprising the following steps:

[0056] Step 1: Take 65 parts of squalane, 3 parts of dipalmitoyl hydroxyproline, 2 parts of glycosphingolipids, and 3 parts of glycolipids by weight fraction, and mix to obtain oil phase mixture A;

[0057] Step 2: Take 3 parts of hyaluronic acid and 2 parts of collagen by weight fraction, and mix in 22 parts of pure water to obtain water phase mixture A;

[0058] Step 3: The oil phase mixture A and the water phase mixture B obtained in steps 1 and 2 are respectively dissolved in a constant temperature water bath at 45°C, and are stirred at 500-600 rpm by a magnetic stirrer for 15 min. The water phase mixture A is then added to the oil phase mixture A at a uniform speed, and is stirred again for 15 min to obtain an initial emulsion A;

[0059] Step 4: The initial emulsion A prepared in step 3 is added to a high-pressure homogenizer, and is homogenized to a nano-sized stable and uniform state to obtain a transparent oily inclusion body as material A for standby;

[0060] Step 5: Take 65 parts of ultrapure water and 5 parts of hydrogenated phosphatidylcholine by weight fraction, heat and dissolve in a water bath, and magnetically stir for 15 min to obtain water phase mixture B;

[0061] Step 6: Take the active material resveratrol 5 parts by weight, dissolve squalane 10 parts, then add the material A 15 parts prepared in step 4, continue to stir until uniform, to obtain the oil phase mixture B;

[0062] Step 7: Add the oil phase mixture B obtained in step 6 to the water phase mixture B obtained in step 5, continue to stir for 15 min to obtain the primary emulsion B;

[0063] Step 8: Add the primary emulsion B prepared in step 7 to the high-pressure homogenizer to obtain the bicontinuous phase microcapsule emulsion with particle size of 100 nm-200 nm.

[0064] The bicontinuous phase microcapsule emulsion prepared in the above examples is tested for particle size distribution, and some test parameters are shown in Table 1.

[0065] Table 1:

[0066] Example 1 Example 2 Example 3 Scattering angle 90 90 90 Support temperature 25 25 25 Dispersion medium viscosity 0.895 mPa.s 0.896 mPa.s 0.895 mPa.s Transmittance before measurement 19982 18854 17896 Transmittance after measurement 20029 17788 16537 Distribution profile Standard Standard Standard Dispersion Polydispersity Polydispersity Polydispersity Particle size reference Scattered light intensity Scattered light intensity Scattered light intensity Count rate 5950 counts (kCPS) 6554 counts (kCPS) 972 counts (kCPS) Autocorrelation curve intercept 0.994 0.996 0.976

[0067] The obtained particle size average distribution graphs are shown in Figure 1 , Figure 2 and Figure 3 .

[0068] The particle size distribution graphs shown in Figure 1 , Figure 2 and Figure 3 are analyzed and calculated, and the results are shown in Table 2.

[0069] Table 2:

[0070]

[0071]

[0072] From the results in Table 2, it can be seen that the average particle size of the bicontinuous phase microcapsule emulsion prepared in the above examples is 100 nm-200 nm, so it has good transdermal absorption, and in the actual application process as a skin care product, the small particles in the dispersed phase can be uniformly distributed on the skin surface, and can be gradually released over time, achieving a lasting skin care effect.

[0073] The above are preferred embodiments of the present application, and do not limit the protection scope of the present application, therefore: any equivalent changes made on the basis of the structure, shape, principle of the present application should be covered within the protection scope of the present application.

Claims

1. A method of preparing a nanobionic bicontinuous phase microencapsulate, characterized in that, The method comprises the following steps: Step 1: mixing squalane, dipalmitoyl hydroxyproline, glycosphingolipids and glycolipids to obtain an oil phase mixture A; Step 2: mixing hyaluronic acid and collagen in pure water to obtain an aqueous phase mixture A; Step 3: separately subjecting the oil phase mixture A and the aqueous phase mixture A obtained in steps 1 and 2 to constant temperature water bath dissolution, and then adding the aqueous phase mixture A into the oil phase mixture A at a uniform speed after stirring with a magnetic stirrer, and then stirring twice to obtain a preliminary emulsion A; Step 4: adding the preliminary emulsion A prepared in step 3 into a high-pressure homogenizer, homogenizing it to a nano-sized stable and uniform state to obtain a transparent oily inclusion as material A for standby; Step 5: heating and dissolving ultrapure water and hydrogenated phosphatidylcholine in a water bath, and stirring with a magnetic stirrer for 15 min to obtain an aqueous phase mixture B; Step 6: dissolving the active substance to be encapsulated in squalane, and then adding the material A prepared in step 4, and continuing to stir uniformly to obtain an oil phase mixture B; Step 7: adding the oil phase mixture B obtained in step 6 into the aqueous phase mixture B obtained in step 5, and continuing to stir for 15 min to obtain a preliminary emulsion B; Step 8: adding the preliminary emulsion B prepared in step 7 into a high-pressure homogenizer to obtain a nano-bionic bicontinuous phase microcapsule inclusion with a particle size of 100-200 nm.

2. A method of preparing a nanobionic bicontinuous phase microencapsulate according to claim 1, wherein, The oil phase mixture A in step 1 comprises, by weight fraction: squalane 50-85 parts, dipalmitoyl hydroxyproline 1-5 parts, glycosphingolipids 1-5 parts, and glycolipids 1-5 parts.

3. A method of preparing a nanobionic bicontinuous phase microencapsulate according to claim 2, wherein, The aqueous phase mixture A in step 2 comprises, by weight fraction: pure water 5-25 parts, hyaluronic acid 1-5 parts, and collagen 1-5 parts.

4. A method of preparing a nanobionic bicontinuous phase microencapsulate according to claim 3, wherein, In step 3, the temperature of the constant temperature water bath is 45℃.

5. A method of preparing a nanobionic bicontinuous phase microencapsulate according to claim 4, wherein, The stirring speed in step 3 is 500-600 rmp, and the stirring time is 15 min for each time.

6. The method of claim 1, wherein the nano-biomimetic bicontinuous phase microencapsulation is prepared by the steps of: The aqueous phase mixture B in step 5 comprises, by weight fraction: ultrapure water 60-85 parts, and hydrogenated phosphatidylcholine 1-5 parts.

7. A method of preparing a nanobionic bicontinuous phase microencapsulate according to claim 6, wherein, The oil phase mixture B in step 6 comprises, by weight fraction: squalane 5-10 parts, and material A 5-15 parts.

8. The method for preparing a nano-bionic dual-phase microcapsule encapsulation according to claim 1, characterized in that, The active substance in step 6 comprises at least one of HPR, ceramide, resveratrol and rose essential oil.

9. The nano-bionic bicontinuous phase microcapsule inclusion prepared by the method according to any one of claims 1-8.

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