CN111249174A - Double-shell-core structure composition and preparation method thereof - Google Patents
Double-shell-core structure composition and preparation method thereof Download PDFInfo
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- CN111249174A CN111249174A CN202010112551.2A CN202010112551A CN111249174A CN 111249174 A CN111249174 A CN 111249174A CN 202010112551 A CN202010112551 A CN 202010112551A CN 111249174 A CN111249174 A CN 111249174A
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- fat
- hyaluronic acid
- active substance
- soluble active
- oil
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
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- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
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- A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns
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- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/56—Compounds, absorbed onto or entrapped into a solid carrier, e.g. encapsulated perfumes, inclusion compounds, sustained release forms
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
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Abstract
The present application provides a composition of a double shell-core structure and a method for preparing the same, the composition comprising a core containing a fat-soluble active substance, an inner shell surrounding the core and formed of phospholipids and cholesterol, and an outer shell surrounding the inner shell and comprising hyaluronic acid. The preparation method comprises the following steps: mixing the fat-soluble active substance with the oil substance to obtain a fat-soluble active substance oil-soluble mixture; mixing phospholipid, cholesterol, positive charge regulator and oil-soluble mixture of fat-soluble active substances to obtain encapsulated fat-soluble active substance core-shell nano-bodies; adding a surfactant into a hyaluronic acid aqueous solution to obtain surfactant modified hyaluronic acid; adding hyaluronic acid modified by a surfactant into the core-shell nano-body encapsulating the fat-soluble active substance to obtain the composition containing the fat-soluble active substance with a double-shell-core structure. The application ensures the stability, high content, high activity and the like of the fat-soluble active substance by effectively encapsulating and transporting the fat-soluble active substance.
Description
Technical Field
The application relates to the technical field of compositions, in particular to a composition with a double-shell-core structure and a preparation method thereof.
Background
Astaxanthin belongs to a fat-soluble pigment and is one of the carotenoids with the most economic value. The astaxanthin oil is insoluble in water, sensitive to external conditions, easy to oxidize, poor in stability, easy to lose activity, not beneficial to human body absorption, difficult to be directly used in cosmetics to play the effects of resisting oxidation, removing free radicals and the like. How to improve the stability of astaxanthin oil and promote its efficient utilization in skin is still a hot point of research.
Hyaluronic acid molecules maintain a high water content within their structural skeleton, and when the stratum corneum is exposed to water, the tissue swells, the stratum corneum barrier unravels, and a pathway is formed for the molecules to enter the skin. Hyaluronic acid and hyaluronic acid derivatives can hydrate the stratum corneum, open up a permeation path and promote transdermal delivery. The structural hydrophobic plaque domain of hyaluronic acid may interact with lipid components in the stratum corneum during penetration, disrupting the skin barrier, and increasing the skin permeability of hyaluronic acid and its derivatives. Hyaluronic acid receptors on skin resident cells such as epidermal keratinocytes and dermal fibroblasts facilitate transdermal delivery of hyaluronic acid and its derivatives. The hyaluronic acid with small molecular weight can enter the dermis due to strong permeability, so that the water storage capacity of the dermis is improved, but the film forming capacity is poor, and the moisture on the surface layer of the skin cannot be locked; hyaluronic acid with large molecular weight has strong film forming property but poor permeability. Cosmetics with different effects can be effectively improved only by selecting proper molecular weight hyaluronic acid to be combined with certain specific receptors on cell surfaces, and meanwhile, the action time of the active ingredients in vivo is prolonged, the bioavailability is improved, and the curative effect is improved.
Disclosure of Invention
Based on the defects that astaxanthin oil in the prior art is sensitive to external conditions, is easy to oxidize, has poor stability, is easy to lose activity, is not beneficial to human body absorption, is difficult to be directly used in cosmetics to exert oxidation resistance, remove free radicals and the like, the application aims to provide a composition with a double-shell-core structure and a preparation method thereof.
Specifically, the present application relates to the following aspects:
1. a composition of a double shell-core structure, comprising a core containing a fat-soluble active substance, an inner shell formed of a phospholipid and cholesterol surrounding the core, and an outer shell comprising hyaluronic acid surrounding the inner shell.
2. The composition according to claim 1, wherein the fat-soluble active substance is one or more selected from astaxanthin oil, ceramide, retinol, coenzyme Q10, and vitamin E.
3. A method for preparing a composition of a double shell-core structure comprising:
mixing the fat-soluble active substance with the oil substance to obtain a fat-soluble active substance oil-soluble mixture;
mixing phospholipid, cholesterol, positive charge regulator and the oil-soluble mixture of the fat-soluble active substance to obtain an encapsulated fat-soluble active substance core-shell nano body;
adding a surfactant into a hyaluronic acid aqueous solution to obtain surfactant modified hyaluronic acid;
adding the surfactant modified hyaluronic acid into the encapsulated fat-soluble active substance core-shell nano-body to obtain the composition containing the fat-soluble active substance with a double shell-core structure.
4. The process according to claim 3, wherein the fat-soluble active substance is one or more selected from astaxanthin oil, ceramide, retinol, coenzyme Q10 and vitamin E.
5. The production method according to item 3 or 4, wherein the mass ratio of the oil substance to the fat-soluble active substance is 3:1 to 25: 1.
6. The method according to claim 3 or 4, wherein the mass ratio of the phospholipid to the fat-soluble active substance is 1:5 to 2: 1.
7. The method according to claim 3 or 4, wherein the mass ratio of the cholesterol to the fat-soluble active substance is 1:12 to 1: 2.
8. The production method according to item 3 or 4, wherein the mass ratio of the surfactant to the hyaluronic acid is 1:16 to 1: 5.
9. The production method according to item 3 or 4, wherein the surfactant is added to the aqueous hyaluronic acid solution to obtain a surfactant-modified hyaluronic acid, and the method comprises:
adding a surfactant into a hyaluronic acid aqueous solution, homogenizing at 45-60 ℃ and 2000-10000 rpm for 3-30 min, and uniformly dispersing;
homogenizing and circulating for 2-5 times under 450-1200 bar to obtain the hyaluronic acid modified by the surfactant.
10. The method according to item 3 or 4, wherein the mass ratio of hyaluronic acid to the fat-soluble active substance in the surfactant-modified hyaluronic acid added is 1:4 to 3: 1.
11. The production method according to claim 3 or 4, wherein the oil-based substance is one or more of hemp oil, squalane, rice bran oil, olive oil, almond oil, jojoba oil, avocado oil, shea butter, tea seed oil, grape seed oil, wheat germ oil, peanut oil, mineral oil, higher fatty alcohol, higher fatty acid, palmitic acid or myristic acid ester, caprylic acid glyceride, and capric acid glyceride.
12. The method according to claim 3 or 4, wherein the phospholipid is one or more selected from egg yolk lecithin, hydrogenated egg yolk phospholipid, soybean lecithin, cephalin, dicetyl phosphate, dimyristoyl phosphatidylcholine, dilauroyl phosphatidylcholine, dioleoyl phosphatidylcholine, and distearoyl phosphatidylcholine.
13. The method according to claim 3 or 4, wherein the cholesterol is one or more of egg yolk cholesterol, egg white cholesterol, serum cholesterol, and gallbladder cholesterol.
14. The method according to item 3 or 4, wherein the hyaluronic acid is one or more selected from the group consisting of:
hyaluronic acid with molecular weight of 5 KDa-15 KDa;
hyaluronic acid with molecular weight of 15 KDa-50 KDa;
hyaluronic acid with molecular weight of 50 KDa-100 KDa; and
hyaluronic acid with molecular weight more than 100 KDa.
15. The method according to claim 3 or 4, wherein the positive charge regulator is one or more of quaternary ammonium salt-18, polyquaternium-7, phosphatidylethanolamine, and polyquaternium-39.
16. The production method according to item 3 or 4, wherein the average particle diameter of the nanobody is 150 to 1000 nm.
17. The production method according to item 3 or 4, wherein the surfactant is one or more of hydroxypropyl cellulose (HPC), Sodium Dodecyl Sulfate (SDS), dodecahydroxystearic acid, and 1-ethyl-3- [ 3-dimethylamino) propyl ] -carbodiimide (EDC).
18. The preparation method according to item 3 or 4, wherein the step of obtaining the encapsulated core-shell nano-sized body of the fat-soluble active substance comprises performing high-pressure homogenization treatment, and then obtaining the encapsulated core-shell nano-sized body of the fat-soluble active substance, wherein the pressure during the high-pressure homogenization treatment is 450-1200 bar, and the cycle number is 2-10 times.
19. The method according to item 3 or 4, wherein the aqueous hyaluronic acid solution has a pH of 3 to 6.
20. A fat-soluble active substance-containing composition of a double shell-core structure, which is the composition produced by the production method described in any one of items 3 to 19. The composition prepared by the application effectively encapsulates and transports the fat-soluble active substance through the modified hyaluronic acid, so that the problem of poor solubility of the fat-soluble active substance in water is solved, and the stability, high content, high activity and the like of the fat-soluble active substance are ensured.
Detailed description of the invention
Unless defined otherwise, technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. Although methods and materials similar or equivalent to those described herein can be used in experimental or practical applications, the materials and methods are described below. In case of conflict, the present specification, including definitions, will control, and the materials, methods, and examples are illustrative only and not intended to be limiting. The present application is further described with reference to the following specific examples, which should not be construed as limiting the scope of the present application.
Provided herein is a composition of a double shell-core structure, which includes a core containing a fat-soluble active material, an inner shell formed of phospholipid and cholesterol surrounding the core, and an outer shell comprising hyaluronic acid surrounding the inner shell. By a double shell-core structure is meant a structure comprising a core, and inner and outer shells. Wherein the core contains liposoluble active substances, the inner shell is composed of phospholipid and cholesterol, and the outer shell contains hyaluronic acid. The phospholipid and cholesterol in the inner shell are closely arranged to tightly wrap the active substances such as fat-soluble active substances, thereby forming a protective film to prevent the active substances such as fat-soluble active substances from deteriorating due to external substances such as air and other adverse factors. The inner shell is composed of phospholipids and cholesterol, has a structure similar to that of the skin, and easily enters the stratum corneum. After entering the stratum corneum, the active epidermis is mostly water-soluble tissues, so the hyaluronic acid molecules of the second shell structure, namely the outer shell, have good hydrophilicity and are easy to transport with active substances, and in addition, hyaluronic acid receptors on keratinocytes promote the transdermal delivery of hyaluronic acid and derivatives thereof, so that the active substances are efficiently delivered to the basal layer and the dermis layer of the skin. With the action of active substances on different skin layers, the double-shell-core structure also begins to be decomposed, nutrients such as hyaluronic acid and phospholipid are absorbed, and active substances such as fat-soluble active substances begin to be released continuously. Thus, the synergistic effect of hyaluronic acid and the monolayer inclusion can effectively deliver fat-soluble active substances such as fat-soluble active substances to each layer of skin.
A method for preparing a composition of a double shell-core structure provided herein comprises:
mixing the fat-soluble active substance with the oil substance to obtain a fat-soluble active substance oil-soluble mixture;
mixing phospholipid, cholesterol, positive charge regulator and the oil-soluble mixture of the fat-soluble active substance to obtain an encapsulated fat-soluble active substance core-shell nano body;
adding a surfactant into a hyaluronic acid aqueous solution to obtain surfactant modified hyaluronic acid;
adding the surfactant modified hyaluronic acid into the encapsulated fat-soluble active substance core-shell nano-body to obtain the composition containing the fat-soluble active substance with a double shell-core structure.
Wherein the fat-soluble active substance is one or more selected from astaxanthin oil, ceramide, retinol, coenzyme Q10, and vitamin E.
In a specific embodiment, when the fat-soluble active substance is astaxanthin oil, the present application provides a composition of a double shell-core structure comprising a core containing astaxanthin oil, an inner shell formed of phospholipids and cholesterol surrounding the core, and an outer shell comprising hyaluronic acid surrounding the inner shell. By a double shell-core structure is meant a structure comprising a core, and inner and outer shells. Wherein the core contains astaxanthin oil, the inner shell is composed of phospholipids and cholesterol, and the outer shell contains hyaluronic acid. The phospholipid and cholesterol are closely arranged in the inner shell, and the active substances such as astaxanthin oil and the like are closely wrapped, so that a protective film is formed, and the active substances such as astaxanthin oil and the like are prevented from being deteriorated by adverse factors such as air and the like. The inner shell is composed of phospholipids and cholesterol, has a structure similar to that of the skin, and easily enters the stratum corneum. After entering the stratum corneum, the active epidermis is mostly water-soluble tissues, so the hyaluronic acid molecules of the second shell structure, namely the outer shell, have good hydrophilicity and are easy to transport with active substances, and in addition, hyaluronic acid receptors on keratinocytes promote the transdermal delivery of hyaluronic acid and derivatives thereof, so that the active substances are efficiently delivered to the basal layer and the dermis layer of the skin. With the action of active substances on different skin layers, the double-shell-core structure also begins to decompose, nutrients such as hyaluronic acid and phospholipid are absorbed, and active substances such as astaxanthin oil are released continuously. Thus, liposoluble active substances such as astaxanthin oil and the like are efficiently delivered to each layer of the skin under the synergistic effect of hyaluronic acid and the monolayer inclusion. The prepared composition is effectively encapsulated and transported by the modified hyaluronic acid prawn green oil, so that the solubility of the astaxanthin oil in water is improved, and the stability, high content, high activity and the like of the astaxanthin oil are ensured.
Wherein the oil substance is used for dissolving the fat-soluble active substance to obtain a uniformly dispersed oil-soluble mixture of the fat-soluble active substance. Further, in the preparation of the green oil solution, the heating temperature is 35-85 ℃, and the ultrasonic treatment time is 5-20 min.
After phospholipid, cholesterol and positive charge regulator are mixed with the oil-soluble mixture of the fat-soluble active substance, the cholesterol and the phospholipid are tightly wrapped on a core containing the fat-soluble active substance to obtain an encapsulated fat-soluble active substance core-shell nano body, and the nano body forms a layer of protective film to prevent external substances, such as air and other adverse factors from deteriorating the active substance. The surface of the encapsulated liposoluble active substance core-shell nano-body obtained by adding the positive charge regulator in the preparation process is positively charged. Adding a surfactant into a hyaluronic acid aqueous solution to obtain surfactant modified hyaluronic acid, wherein the surface of the hyaluronic acid is negatively charged. The hyaluronic acid modified by the surfactant is added into the core-shell nano-body for encapsulating the fat-soluble active substance, and the hyaluronic acid modified by the surfactant is negatively charged, so that the core-shell nano-body for encapsulating the fat-soluble active substance is positively charged, and the modified hyaluronic acid is quickly wrapped around the core-shell nano-body for encapsulating the fat-soluble active substance through electrostatic attraction. On the other hand, due to the action of the surfactant, the hydrophilic groups on the modified hyaluronic acid molecules are combined with the hydrophilic functional groups of the phospholipid, thus forming the composition with a double shell-core structure.
Adding a surfactant into a hyaluronic acid aqueous solution to obtain surfactant modified hyaluronic acid, wherein the preparation method comprises the steps of preparing hyaluronic acid into a hyaluronic acid aqueous solution with the pH value of 3-6, adding the surfactant, homogenizing at 45-60 ℃, 2000-10000 rpm for 3-30 min, and uniformly dispersing; homogenizing and circulating for 2-5 times under 450-1200 bar to obtain the hyaluronic acid modified by the surfactant. Wherein the temperature is 45 to 60 ℃, for example, 45 ℃, 50 ℃, 55 ℃ and 60 ℃. 2000 to 10000rpm, for example, 2000rpm, 3000rpm, 4000rpm, 5000rpm, 6000rpm, 7000rpm, 8000rpm, 9000rpm, 10000rpm may be mentioned. 450 to 1200bar, for example, 450bar, 500bar, 600bar, 700bar, 800bar, 900bar, 1000bar, 1100bar, 1200 bar.
In a specific embodiment, the mass ratio of the oil substance to the fat-soluble active substance is 3:1 to 25:1, and may be, for example, 3:1, 5:1, 15:1, 20:1, or 25: 1.
In a specific embodiment, the oil is one or more of hemp oil, squalane, rice bran oil, olive oil, almond oil, jojoba oil, avocado oil, shea butter, tea seed oil, grape seed oil, wheat germ oil, peanut oil, mineral oil, higher fatty alcohols, higher fatty acids, palmitic acid or myristic acid esters, glyceryl caprylate, and glyceryl caprate. For example, it may be hemp oil, squalane or rice bran oil, or any two or three of them.
In a specific embodiment, the mass ratio of the phospholipid to the fat-soluble active substance (e.g., astaxanthin oil) is 1:5 to 2:1, and may be, for example, 1:5, 1:2, 1:1, 1:1.5, or 1: 2.
In a specific embodiment, the mass ratio of the cholesterol to the fat-soluble active substance (e.g., astaxanthin oil) is 1:12 to 1:2, and may be, for example, 1:12, 1:6, 1:4, 1:3, or 1: 2.
In a specific embodiment, the mass ratio of the surfactant to the hyaluronic acid is 1:16 to 1:5, and may be, for example, 1:16, 1:14, 1:12, 1:10, 1:8, or 1: 5.
In a specific embodiment, the mass ratio of the hyaluronic acid to the lipid-soluble active substance (e.g., astaxanthin oil) in the surfactant-modified hyaluronic acid is 1:4 to 3:1, and may be, for example, 1:4, 1:1, 2:1, or 3: 1.
In a specific embodiment, the phospholipid is one or more of egg yolk lecithin, hydrogenated egg yolk phospholipid, soybean lecithin, cephalin, dicetyl phosphate, dimyristoyl phosphatidylcholine, phosphatidylcholine dilaurate, dioleoyl phosphatidylcholine, and phosphatidylcholin distearate.
In a specific embodiment, the cholesterol is one or more of egg yolk cholesterol, egg white cholesterol, serum cholesterol, and gallbladder cholesterol. The positive charge regulator is one or more than two of quaternary ammonium salt-18, polyquaternium-7, phosphatidylethanolamine and polyquaternium-39.
In a specific embodiment, the hyaluronic acid is one or two or more selected from the group consisting of: hyaluronic acid with molecular weight of 5 KDa-15 KDa; hyaluronic acid with molecular weight of 15 KDa-50 KDa; hyaluronic acid with molecular weight of 50 KDa-100 KDa; and hyaluronic acid with molecular weight more than 100 KDa. 5KDa to 15KDa, for example, 5KDa, 10KDa, 15 KDa. 15KDa to 50KDa, for example, 15KDa, 20KDa, 30KDa, 40KDa, 50 KDa. 50kDa to 100kDa may be, for example, 50kDa, 60kDa, 70kDa, 80kDa, 90kDa or 100 kDa. Greater than 100KDa, for example, 200KDa, 300KDa, 400KDa, 500KDa, etc., may be possible. Hyaluronic acid as used herein is produced by Huaxi Biotech, Inc.
In a specific embodiment, the surfactant is one or more of hydroxypropyl cellulose (HPC), Sodium Dodecyl Sulfate (SDS), dodecahydroxystearic acid, 1-ethyl-3- [ 3-dimethylamino) propyl ] -carbodiimide (EDC).
The average particle diameter of the core-shell nano-body for encapsulating the fat-soluble active substance is 150-1000 nm, for example, 150nm, 200nm, 300nm, 400nm, 500nm, 600nm, 700nm, 800nm, 900nm, 1000 nm. Wherein, the average particle size test conditions of the nano bodies are as follows: a Malvern particle sizer (ZetaNano Size 90, Malvern, uk) analyzer was used, the test angle was 90 °, and the test temperature was 25 ℃.
In a specific embodiment, the average particle size of the astaxanthin oil encapsulated core-shell nano-sized particles is 150 to 1000nm, and for example, may be 150nm, 200nm, 300nm, 400nm, 500nm, 600nm, 700nm, 800nm, 900nm, 1000 nm. Wherein, the average particle size test conditions of the nano bodies are as follows: a Malvern particle sizer (ZetaNano Size 90, Malvern, uk) analyzer was used, the test angle was 90 °, and the test temperature was 25 ℃.
The composition with the double-shell-core structure prepared by the application can be further applied to skin care products, such as aqueous cream and spray freeze-dried powder systems.
The following examples of the present application are intended only to illustrate specific embodiments for carrying out the present application and these embodiments are not to be construed as limiting the present application. Other changes, modifications, substitutions, combinations, and simplifications which may be made without departing from the spirit and principles of the present application are intended to be equivalent substitutions and are within the scope of the present application.
Examples
The present invention is further illustrated by the following examples, which are intended to be purely exemplary of the invention and are not intended to be limiting.
The experimental methods used in the following examples are all conventional methods, unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1
Weighing 3.0g of hemp oil, placing in a beaker, placing the beaker in a water bath magnetic stirrer, setting the temperature at 70 ℃, rotating at 700rpm, fully mixing for 40min, cooling, and introducing nitrogen for 10min for later use.
Weighing 1.0g of astaxanthin oil, adding the astaxanthin oil into the oil solution under the protection of nitrogen, setting the temperature at 60 ℃, rotating at 700rpm, and fully mixing for 20min to finally obtain a uniform astaxanthin oil-soluble mixture.
Weighing 1.0g of egg yolk lecithin and 0.5g of cholesterol, dissolving in 75ml of water solution, adding 0.2g of phosphatidylethanolamine and 0.1g of octadecanol amine, adding the astaxanthin oil-soluble mixture, stirring at high speed, and homogenizing a sample by using a high-pressure homogenizer at a pressure of 900bar for 4 times in a circulating manner to obtain the encapsulated astaxanthin oil core-shell nano-body.
Weighing 3.0g of hyaluronic acid with the molecular weight of 5KDa, dissolving the hyaluronic acid in 10ml of purified water, and adjusting the pH value to 3-6 to obtain a hyaluronic acid aqueous solution. Adding 0.6g of hydroxypropyl cellulose into the hyaluronic acid aqueous solution, homogenizing at 45 ℃, 10000rpm for 30min, uniformly dispersing, and then homogenizing and circulating for 2 times at 450bar to obtain the hydroxypropyl cellulose modified hyaluronic acid.
Dropwise adding the hydroxypropyl cellulose modified hyaluronic acid into the astaxanthin oil encapsulated core-shell nano-bodies under the stirring of 700rpm, and reacting at the constant temperature of 45 ℃ for 30min to obtain the astaxanthin oil-containing composition with a double-shell-core structure.
Examples 2 to 5
Examples 2-5 were carried out according to the procedure of example 1, varying the molecular weights of the oil-based substances, phospholipids, hyaluronic acid, and the contents of the respective components. The reaction conditions of the different examples are shown in Table 1.
Example 6
The same procedure as in example 1 was repeated except that 1.0g of astaxanthin oil was weighed out in example 1 and that 0.3g of retinol was weighed out. Finally, a retinol-containing composition of a double shell-core structure was obtained.
Comparative example 1
Weighing 5.0g of squalane and 1.0g of rice bran oil, placing the mixture in a beaker, placing the beaker in a water bath magnetic stirrer, setting the temperature at 70 ℃, rotating at 700rpm, fully mixing the mixture for 40min, cooling, and introducing nitrogen for 10min for later use.
Weighing 1.0g of astaxanthin oil, adding the astaxanthin oil into the oil solution under the protection of nitrogen, setting the temperature at 60 ℃, rotating at 700rpm, and fully mixing for 20min to finally obtain a uniform astaxanthin oil-soluble mixture.
Weighing 2.0g of egg yolk lecithin and 0.3g of cholesterol, dissolving in 75ml of water solution, adding 0.2g of phosphatidylethanolamine and 0.1g of octadecanolamine, adding the astaxanthin oil-soluble mixture, stirring at high speed, and then homogenizing a sample by using a high-pressure homogenizer at the pressure of 500bar for 4 times in a circulating manner to obtain the encapsulated astaxanthin oil core-shell nano-body.
Comparative example 2
Weighing 5.0g of squalane and 1.0g of rice bran oil, placing the mixture in a beaker, placing the beaker in a water bath magnetic stirrer, setting the temperature at 70 ℃, rotating at 700rpm, fully mixing the mixture for 40min, cooling, and introducing nitrogen for 10min for later use.
Weighing 1.0g of astaxanthin oil, adding the astaxanthin oil into the oil solution under the protection of nitrogen, setting the temperature at 60 ℃, rotating at 700rpm, and fully mixing for 20min to finally obtain a uniform astaxanthin oil-soluble mixture.
TABLE 1 reaction conditions of examples and comparative examples
The particle size test was performed on the encapsulated astaxanthin oil core-shell nanobodies prepared in examples 1 to 5, respectively, and the average particle size of the encapsulated astaxanthin oil core-shell nanobodies in each example is shown in table 2. Wherein the test conditions are as follows: a Malvern particle sizer (ZetaNano Size 90, Malvern, uk) analyzer was used, the test angle was 90 °, and the test temperature was 25 ℃.
TABLE 2 average particle diameters shown under the conditions of examples 1 to 6 and comparative example 1
Test examples
The obtained compositions containing astaxanthin oil prepared in the above examples and comparative examples were subjected to facial muscle base solution preparation, and the corresponding facial muscle base solutions were subjected to efficacy tests. The compositions of examples 1 to 6 were formulated according to the formulations shown in tables 3 and 4. The composition of comparative example 1 was formulated according to the formulation of table 5, and the composition of comparative example 2 was formulated according to the formulation of table 6.
Table 3 examples 1-5 facial muscle base fluid formulations
Table 4 example 6 facial muscle base fluid formulation
TABLE 5 facial muscle base solution formulation
Table 6 trial preparation of facial muscle base solution formulation for comparative example 2
Then, the facial muscle base fluid obtained by compounding is subjected to efficacy test.
The test objects are: 13 groups of volunteers, 20 in each group, age 25-45 years, male and female are unlimited.
The test method comprises the following steps: the test was performed as a half-face control, using facial anti-aging moisturizing muscle base solution (prepared in examples 1-6) on one side and a control (comparative example 1 or 2) on the other side, once in the morning and at night. High-resolution pictures are taken before, 2 weeks, 4 weeks and 8 weeks after the samples are used, the water content of the facial cuticle, the transdermal water loss and the skin elasticity are detected, the changes of facial fine lines and glossiness are analyzed, and the average value is obtained by repeating the measurement for 3 times.
The apparatus used was: skin elasticity tester MPA 580(Courage + Khazaka, Germany), skin moisture tester Corneometer CM 825(Courage + Khazaka, Germany), skin moisture loss tester TewameterTM300(Courage + Khazaka, Germany), VISIA CR (Canfield, USA).
The calculation method comprises the following steps: the initial value of the moisture content of facial skin is L0 i(i-1, 2 ….14), after 8 weeks the experimental group was marked L8 i(i-1, 2 …, 14), respectively, mixing L8 i/L0 iRelative facial water values were obtained for 20 volunteers and then averaged to obtain the final average relative skin moisture value. In the same way, the relative data of the percutaneous water loss and the skin elasticity are obtained in sequence.
1. Moisturizing effect of facial muscle base solution
Table 6 shows the influence of the facial muscle foundation liquid on the water content of the skin cuticle of the face and the influence of the transdermal water dispersion amount, and the results show that the facial anti-aging muscle foundation liquid has a certain moisturizing effect, can improve the water content of the skin cuticle and reduce the transdermal water dispersion amount, and has the functions of locking water, moisturizing and improving the barrier; obviously, the water locking and moisturizing effects of the anti-aging and moisturizing composition with the hyaluronic acid modified phospholipid as the shell carrier and the astaxanthin oil as the core are higher than those of a simple mixing system of hyaluronic acid and astaxanthin oil, especially when the sample of example 2 is used, the water content of the stratum corneum is improved by 23.43%, and the transdermal water loss is reduced by 27.48%. Example 5 stratum corneum HAs less water content, probably because HA HAs a higher molecular weight and is less able to penetrate deeper into the skin to function. In conclusion, the hyaluronic acid has the molecular weight of 5-50 KDa, and the liposome has the high-efficiency water replenishing function at 250-650 nm.
TABLE 6 influence of samples on the water content of the stratum corneum of facial skin and the amount of transdermal water dispersion
2. Effects of facial muscle base fluid on skin elasticity
Table 7 shows the effect of the facial muscle foundation on the elasticity of facial skin, and the results show that the facial muscle foundation can improve the skin elasticity, and especially the skin elasticity is improved by 25.27% at 8 weeks with the best effect when the sample of example 2 is used.
TABLE 7 influence of samples on facial skin elasticity the influence of facial muscle base fluid on facial texture
3. Effects of facial muscle base fluid on skin texture
Table 8 shows the effect of the facial muscle fluid on the skin texture, and the results show that the facial muscle fluid can lighten the facial fine lines and reduce the area of the fine lines with time, especially the area of the fine lines in the same selected area in 8 weeks is reduced by 19.66% by using the sample of example 2, and the effect is the best. The example 4 sample is equivalent to the example 5 sample in effect, and may be too small in inclusion particle size, and the amount of the encapsulated active is relatively small, which is not favorable for the active to exert the effect for a long time.
TABLE 8 Effect of samples on facial skin texture
Comparative example 2 has certain anti-aging and moisturizing effects, but the effect is not obvious compared with other examples. The astaxanthin oil has good anti-aging effect, but has poor stability and is sensitive to light, heat and the like, the stability of the astaxanthin oil can be improved by preparing a shell-core structure, and the structure is similar to a skin phospholipid bilayer structure and can promote the transdermal absorption of active substances. In addition, the hyaluronic acid wrapped outside can not only form a water-retaining barrier for the skin, but also carry active substances into the dermis layer to exert the effect.
In conclusion, the facial muscle base solution has the functions of efficiently moisturizing and moisturizing, has a remarkable effect of fading fine lines, can improve the skin glossiness, and further shows that the composition with the hyaluronic acid modified phospholipid as a shell carrier and the astaxanthin oil as a core has the effects of efficiently resisting aging and moisturizing, in addition, the structure with the hyaluronic acid modified phospholipid as the shell carrier and the retinol as the core also has the effects of efficiently resisting aging and moisturizing, and further shows that the structure with the hyaluronic acid modified phospholipid as the shell carrier and the oil-soluble active substance as the core can be applied to astaxanthin, and also can be applied to any one or more than two of retinol, ceramide, coenzyme Q10, vitamin E and the like.
Claims (10)
1. A composition of a double shell-core structure, comprising a core containing a fat-soluble active substance, an inner shell formed of a phospholipid and cholesterol surrounding the core, and an outer shell comprising hyaluronic acid surrounding the inner shell.
2. The composition according to claim 1, wherein the fat-soluble active substance is one or more selected from astaxanthin oil, retinol, ceramide, coenzyme Q10, and vitamin E.
3. A method for preparing a composition of a double shell-core structure comprising:
mixing the fat-soluble active substance with the oil substance to obtain a fat-soluble active substance oil-soluble mixture;
mixing phospholipid, cholesterol, positive charge regulator and the oil-soluble mixture of the fat-soluble active substance to obtain an encapsulated fat-soluble active substance core-shell nano body;
adding a surfactant into a hyaluronic acid aqueous solution to obtain surfactant modified hyaluronic acid;
adding the surfactant modified hyaluronic acid into the encapsulated fat-soluble active substance core-shell nano-body to obtain the composition containing the fat-soluble active substance with a double shell-core structure.
4. The method according to claim 3, wherein the fat-soluble active substance is one or more selected from astaxanthin oil, retinol, ceramide, coenzyme Q10, and vitamin E.
5. The preparation method according to claim 3 or 4, wherein the mass ratio of the oil substance to the fat-soluble active substance is 3:1 to 25: 1.
6. The method according to claim 3 or 4, wherein the mass ratio of the phospholipid to the fat-soluble active substance is 1:5 to 2: 1.
7. The method according to claim 3 or 4, wherein the mass ratio of the cholesterol to the fat-soluble active substance is 1:12 to 1: 2.
8. The method according to claim 3 or 4, wherein the mass ratio of the surfactant to the hyaluronic acid is 1:16 to 1: 5.
9. The method according to claim 3 or 4, wherein the surfactant is added to the aqueous hyaluronic acid solution to obtain a surfactant-modified hyaluronic acid, and the method comprises:
adding a surfactant into a hyaluronic acid aqueous solution, homogenizing at 45-60 ℃ and 2000-10000 rpm for 3-30 min, and uniformly dispersing;
homogenizing and circulating for 2-5 times under 450-1200 bar to obtain the hyaluronic acid modified by the surfactant.
10. The method according to claim 3 or 4, wherein the mass ratio of hyaluronic acid to the fat-soluble active substance in the surfactant-modified hyaluronic acid is 1:4 to 3: 1.
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