High-moisture-retention face cream and preparation method thereof
By constructing soy lecithin liposomes loaded with squalene and forming a coating of sodium hyaluronate and chitosan on its surface, it solves the problem that it is difficult to improve the skin's long-term moisturizing performance in cosmetics, achieving efficient utilization of compounds and long-term moisturizing effects of face creams.
Patent Information
- Application Number
- CN202510111309.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-23
- Publication Date
- 2025-03-28
AI Technical Summary
Existing cosmetics are difficult to effectively improve the skin's long-term moisturizing properties, and compounds that are difficult to dissolve in water, such as squalene and phytosterols, are less bioavailable.
By constructing liposomes such as squalene-loaded soy lecithin and forming a coating of sodium hyaluronate and chitosan on its surface, combined with electrostatic deposition technology, a sustained-release high-moisturizing cream was prepared.
It has achieved the improvement of the stability and bioavailability of compounds such as squalene, extended the moisturizing effect of the face cream, and improved the stability and biological activity of liposomes.
Smart Images

Figure CN119700563A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of cosmetics, and in particular relates to a highly moisturizing facial cream and a preparation method thereof. Background Art
[0002] The skin is the largest organ in the human body and the first line of defense. The skin is mainly composed of three parts: the epidermis, the dermis, and the subcutaneous tissue. The epidermis is the part of the skin that is in direct contact with the outside world, including the stratum corneum, the clear layer, and the granular layer. The keratin in the stratum corneum can effectively block the infiltration of chemicals and the extravasation of body fluids, and can obtain a certain amount of moisture from the external environment. The dermis is rich in a large number of collagen fibers that maintain skin elasticity. The hyaluronic acid and protein complex in the interfiber matrix can bind a large amount of water. When the hyaluronic acid content decreases, the elasticity of the collagen fibers will be reduced, resulting in dryness, dullness, and increased wrinkles on the skin. In the subcutaneous tissue, the oil secreted by the sebaceous glands helps keep the skin smooth and prevents water evaporation. Therefore, moisturizing is one of the most basic functions of skin care products, which is essential for maintaining skin elasticity and delaying the skin aging process.
[0003] Traditional skin moisturizing solutions often use direct addition of exogenous moisturizers to replenish the surface moisture of the skin, but there are problems such as low utilization rate of active substances and poor stability. The biofilm-like structure of the nano delivery system gives it good biosafety and compatibility. CN111973494 B provides a method for preparing a long-lasting moisturizing cream, in which microcapsule wall materials are prepared by silk fibroin, which slowly dissolves and is filled into the surface of the skin with the release of the core material, thereby improving the skin moisturizing performance, but the particle size of the microcapsule is unknown. CN113262194 B discloses a method for preparing an anti-aging antioxidant liposome cream, which has an outstanding ability to scavenge DPPH free radicals, can effectively improve the dullness of the skin caused by oxidative damage, and achieve brightening and anti-aging effects, but the article does not reflect the preparation process of the liposome and the stability characteristics of the nanoemulsion. CN118161433A discloses the application of tea polyphenols and panthenol composition in a face cream system, which can effectively inhibit the damage of UVB radiation to the skin, but tea polyphenols are sensitive to environmental factors such as temperature, light and pH, and are prone to degradation. Therefore, the preparation of a new nanoemulsion delivery system and its application in sustained-release long-lasting moisturizing cosmetics need to be explored.
[0004] Liposomes are spherical cell-like vesicles formed by self-assembly of phospholipids. They are one of the emerging nanotechnologies. Liposomes have a strong affinity with skin cells and can be used to enhance the delivery of active compounds such as aloe vera, curcumin, resveratrol, coenzyme Q, quercetin, vitamin C and vitamin E in skin care. At the same time, the phospholipids in liposomes are the main components of cell membrane structure, which helps to increase the penetration effect and release of active compounds. However, liposome vesicles are easily affected by the environment such as temperature, pH value and salt ions and aggregate.
[0005] Squalene is a triterpenoid unsaturated hydrocarbon with 6 all-trans double bonds and a molecular formula of C 30 H 50 It is a colorless and odorless liquid oil at room temperature. It is easily oxidized and deteriorated in the air, and emits a special fishy smell. Squalene is similar to human sebum and has a strong affinity. It can form a natural barrier on the skin surface, inhibit the peroxidation of skin lipids, and promote the proliferation of skin basal cells, which helps to delay skin aging, promote cell metabolism and help repair damaged cells. Squalene is mainly derived from the liver of deep-sea fish.
[0006] Phytosterols are a class of steroidal compounds naturally present in plants. They are the general term for plant sterol esters and free plant sterols. Phytosterols are mainly derived from by-products in the processing of vegetable oils.
[0007] However, both squalene and phytosterols are compounds that are poorly soluble in water and have low bioavailability. Nano-delivery is of great significance for improving the solubility and high-value utilization of phytosterols and squalene. Summary of the invention
[0008] The present invention provides a highly moisturizing facial cream and a preparation method thereof to solve the above technical problems.
[0009] The present invention provides a method for preparing a highly moisturizing facial cream, comprising the following steps: (1) Weigh squalane, beeswax, vitamin E, avocado oil, hydrogenated lecithin, isopropyl palmitate, stearyl alcohol, and dimethicone, mix, and heat to obtain phase A; (2) Weigh glycerin, carbomer 940, sodium hyaluronate, xanthan gum, 1,2-hexanediol, and allantoin, add deionized water, mix, and heat to obtain phase B; (3) Take liposomes, cinnamaldehyde, and gardenia essence to obtain phase C; (4) After mixing phase A and phase B, perform the first shear emulsification, cool, mix with phase C, perform the second shear emulsification, and stir to obtain a highly moisturizing facial cream.
[0010] Furthermore, in the phase A of step (1), 0-4 parts of squalane, 2-4 parts of beeswax, 2-4 parts of vitamin E, 0.1-1 parts of avocado oil, 0.1-1 parts of hydrogenated lecithin, 0.1-1 parts of isopropyl palmitate, 1-2 parts of octadecyl alcohol, and 2-4 parts of dimethicone are included; In step (2), in phase B, 5-10 parts of glycerin, 0.1-1 part of Carbopol 940, 0.1-1 part of sodium hyaluronate, 0.08-0.12 part of xanthan gum, 1-3 parts of 1,2-hexanediol, and 0.1-1 part of allantoin; In step (3), in phase C, 1-4 parts of liposomes, 0.1-0.5 parts of xinxianketone, and 0.008-0.012 parts of gardenia essence; The sum of all components of phase A, phase B and phase C is 100 parts.
[0011] Furthermore, in step (3), the liposome is prepared by the following steps: S1, dissolving soybean lecithin, phytosterol, octadecylamine and squalene in anhydrous ethanol to obtain an organic phase; S2, mix glycerol and distilled water to obtain an aqueous phase; S3. The organic phase and the aqueous phase are mixed, and the mixture is subjected to rotary evaporation to remove the anhydrous ethanol in the suspension, and then the mixture is homogenized in a microfluidizer to obtain squalene liposomes.
[0012] Furthermore, in step (1) and step (2), heating is performed to 85°C.
[0013] Furthermore, in step (4), the first shear emulsification time is 1 min; the mixture is cooled to 40° C.; and the second shear emulsification time is 0.5 min.
[0014] Further, in step S1, the phytosterol includes at least one of cholesterol, stigmasterol or β-sitosterol; In step S1, the dosage ratios of soybean lecithin, phytosterols, octadecylamine, squalene, and anhydrous ethanol are 500-600 mg, 35-45 mg, 5-15 mg, 0.8-1.5 mL, and 50-100 mL, respectively.
[0015] Further, in step S2, the volume ratio of glycerol to distilled water is 1-5 mL:150 mL; In step S3, the mass ratio of the organic phase to the aqueous phase is 1:2. Furthermore, the method further comprises step S4, specifically comprising: dropping the squalene liposome obtained in S3 into an equal volume of sodium hyaluronate solution, stirring, and standing to obtain squalene liposomes coated with sodium hyaluronate; Preferably, in step S4, the mass concentration of the sodium hyaluronate solution is 0.5-1.5%wt.
[0016] Furthermore, the method further comprises step S5, specifically comprising: dropping the sodium hyaluronate-coated squalene liposomes obtained in S4 into an equal volume of chitosan solution, stirring, and standing to obtain sodium hyaluronate- and chitosan-loaded squalene liposomes; Preferably, in step S5, the mass concentration of the chitosan solution is 1-2%wt.
[0017] The present invention also provides a highly moisturizing facial cream prepared by any of the above-mentioned preparation methods.
[0018] The present invention has the following advantages: The preparation method of the highly moisturizing facial cream proposed by the present invention uses plant sterols to construct liposomes loaded with squalene, soybean lecithin, etc., so that the plant sterols are embedded between the phospholipid bilayers to stabilize the liposome architecture, while adjusting the lipid composition and vesicle size. In addition, sodium hyaluronate and chitosan coated liposomes help mask the bad smell of squalene, effectively increase the stability and biological activity of the liposomes, and improve their bioavailability. The constructed sustained-release loaded squalene nano delivery system is compounded with the facial cream, so that it forms an effective coating and stays on the surface of the skin, which helps to exert the long-lasting and highly moisturizing effect of the facial cream. BRIEF DESCRIPTION OF THE DRAWINGS
[0019] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.
[0020] Figure 1 XRD images of the cream and monomer prepared in Examples 1 to 3 of the present invention; Figure 2 Transmission electron microscope images and physical images of the facial creams prepared in Examples 1 to 3 of the present invention; Figure 3 This is a physical picture of the facial cream prepared in Examples 1 to 3 of the present invention placed at room temperature (25° C.) for 30 days; Figure 4 The actual pictures are of the facial creams prepared in Examples 1 to 3 and Comparative Examples 1 to 3 of the present invention; Figure 5 The stability analysis results of the creams prepared in Examples 1 to 3 of the present invention and Comparative Examples 1 to 3; Figure 6 The moisturizing analysis results of the facial creams prepared in Examples 1 to 3 of the present invention and Comparative Examples 1 to 3 are shown. DETAILED DESCRIPTION The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. In the absence of conflict, the embodiments of the present invention and the features in the embodiments can be combined with each other.
[0021] The thermodynamic instability of liposomes makes them susceptible to coagulation and rupture under environmental conditions. Therefore, it is crucial to improve the stability of liposome delivery systems. The inventors of this application have found that adding an appropriate amount of sterols is an effective way to improve the stability of liposome architecture. Liposome vesicles with cell membrane-like structures formed by self-assembly of amphiphilic substances such as phospholipids can simultaneously load hydrophilic and hydrophobic compounds.
[0022] On the one hand, an embodiment of the present invention provides a method for preparing a highly moisturizing facial cream, comprising the following steps: (1) Weigh squalane, beeswax, vitamin E, avocado oil, hydrogenated lecithin, isopropyl palmitate, stearyl alcohol, and dimethicone, mix, and heat to obtain phase A; (2) Weigh glycerin, carbomer 940, sodium hyaluronate, xanthan gum, 1,2-hexanediol, and allantoin, add deionized water, mix, and heat to obtain phase B; (3) Take liposomes, cinnamaldehyde, and gardenia essence to obtain phase C; (4) After mixing phase A and phase B, perform the first shear emulsification, cool, mix with phase C, perform the second shear emulsification, and stir to obtain a highly moisturizing facial cream.
[0023] A method for preparing a highly moisturizing facial cream proposed in an embodiment of the present invention utilizes plant sterols to construct liposomes loaded with squalene, soybean lecithin, etc., and combines electrostatic deposition technology to prepare sodium hyaluronate and chitosan coated liposomes, and the liposomes are compounded with squalane and incorporated into the facial cream. The small molecule polysaccharide coated nanoliposome vesicles can effectively regulate their stability, improve the poor solubility and low bioavailability of plant sterols and squalene, and further enhance the high value utilization of squalene and the long-lasting moisturizing effect of facial cream products. In one embodiment of the present invention, in the phase A of step (1), 0-4 parts of squalane, 2-4 parts of beeswax, 2-4 parts of vitamin E, 0.1-1 parts of avocado oil, 0.1-1 parts of hydrogenated lecithin, 0.1-1 parts of isopropyl palmitate, 1-2 parts of octadecyl alcohol, and 2-4 parts of dimethicone; In step (2), in phase B, 5-10 parts of glycerin, 0.1-1 part of Carbopol 940, 0.1-1 part of sodium hyaluronate, 0.08-0.12 part of xanthan gum, 1-3 parts of 1,2-hexanediol, and 0.1-1 part of allantoin; In step (3), in phase C, 1-4 parts of liposomes, 0.1-0.5 parts of xinxianketone, and 0.008-0.012 parts of gardenia essence; The sum of all components of phase A, phase B and phase C is 100 parts.
[0024] It should be noted that the components in phase A include weighed squalane, beeswax, vitamin E, avocado oil, hydrogenated lecithin, isopropyl palmitate, octadecyl alcohol, and dimethicone; the components in phase B include glycerin, carbomer 940, sodium hyaluronate, xanthan gum, 1,2-hexanediol, allantoin, and deionized water; the components in phase C include liposomes, cinnamone, and gardenia essence. The total number of components in phase A, phase B, and phase C is 100 parts.
[0025] In a preferred embodiment of the present invention, in step (1) phase A, 0-4 parts of squalane, 3 parts of beeswax, 3 parts of vitamin E, 0.5 parts of avocado oil, 0.5 parts of hydrogenated lecithin, 0.5 parts of isopropyl palmitate, 1.5 parts of octadecyl alcohol, and 3 parts of dimethicone; In step (2), phase B includes 6 parts of glycerin, 0.5 parts of Carbopol 940, 0.2 parts of sodium hyaluronate, 0.1 parts of xanthan gum, 2 parts of 1,2-hexanediol and 0.5 parts of allantoin; In step (3), phase C, 1-4 parts of liposomes, 0.2 parts of xinxianketone, and 0.01 parts of gardenia essence; The sum of all components of phase A, phase B and phase C is 100 parts.
[0026] In one embodiment of the present invention, in step (1) and step (2), heating is performed to 85°C.
[0027] In one embodiment of the present invention, in step (4), the first shear emulsification time is 1 min; the temperature is cooled to 40° C.; and the second shear emulsification time is 0.5 min. In a preferred embodiment of the present invention, in step (3), the liposome is prepared by the following steps: S1, dissolving soybean lecithin, phytosterol, octadecylamine and squalene in anhydrous ethanol to obtain an organic phase; S2, mix glycerol and distilled water to obtain an aqueous phase; S3. The organic phase and the aqueous phase are mixed, and the mixture is subjected to rotary evaporation to remove the anhydrous ethanol in the suspension, and then the mixture is homogenized in a microfluidizer to obtain squalene liposomes.
[0028] In one embodiment of the present invention, in step S1, the phytosterol includes at least one of cholesterol, stigmasterol or β-sitosterol. In the embodiment of the present invention, β-sitosterol shows a good effect in stabilizing the liposome framework, and β-sitosterol is preferred.
[0029] In one embodiment of the present invention, in step S1, the dosage ratio of soybean lecithin, phytosterol, octadecylamine, squalene, and anhydrous ethanol is 500-600 mg, 35-45 mg, 5-15 mg, 0.8-1.5 mL, and 50-100 mL. Preferably, in step S1, the dosage ratio of soybean lecithin, phytosterol, octadecylamine, squalene, and anhydrous ethanol is 562.5 mg, 39.375 mg, 9.375 mg, 1.2 mL, and 75 mL.
[0030] In the embodiment of the present invention, the main constituent of soybean lecithin is phospholipids, which are similar to the constituents of biological membranes, play a barrier protection and moisturizing role on the skin, and can improve skin nutrition. Squalene is mainly derived from the liver of deep-sea fish. Phytosterols are mainly derived from by-products in the processing and preparation of vegetable oils. Both squalene and phytosterols are compounds that are poorly soluble in water and have low bioavailability. Liposome vesicles with a cell membrane-like structure formed by self-assembly of amphiphilic substances such as phospholipids can simultaneously load hydrophilic and hydrophobic compounds, thereby improving the stability of the liposome delivery system.
[0031] In one embodiment of the present invention, in step S2, the volume ratio of glycerol to distilled water is 1-5 mL: 150 mL. Preferably, in step S2, the volume ratio of glycerol to distilled water is 3.75 mL: 150 mL.
[0032] In one embodiment of the present invention, in step S3, the mass ratio of the organic phase to the aqueous phase is 1:2.
[0033] In one embodiment of the present invention, in step S3, the rotary evaporation conditions are 55° C. and 100 Mpa.
[0034] In one embodiment of the present invention, in step S3, the homogenization pressure is 12000 Psi and the number of homogenization times is 3 times.
[0035] In one embodiment of the present invention, in steps S1 , S2 , and S3 , mixing is performed by stirring.
[0036] In one embodiment of the present invention, step S4 is further included, specifically, dropping the squalene liposomes obtained in S3 into an equal volume of sodium hyaluronate solution, stirring, and standing to obtain sodium hyaluronate-coated squalene liposomes (HA NPs).
[0037] In the embodiments of the present invention, sodium hyaluronate is an anionic mucopolysaccharide widely present in the extracellular matrix of connective tissues of animals and humans. Its high viscoelasticity, plasticity, permeability and good biocompatibility can be widely used in biomaterials, and can play a unique role as a moisturizing factor in cosmetics. In the embodiments of the present invention, sodium hyaluronate helps to mask the bad smell of squalene, thereby increasing the stability and biological activity of liposomes and improving their bioavailability.
[0038] In one embodiment of the present invention, in step S4, the mass concentration of the sodium hyaluronate solution is 0.5-1.5%wt.
[0039] Preferably, in step S4, the mass concentration of the sodium hyaluronate solution is 0.9%wt.
[0040] In one embodiment of the present invention, step S5 is also included, specifically: dripping the squalene liposomes coated with sodium hyaluronate obtained in S4 into an equal volume of chitosan solution, stirring, and standing to obtain squalene liposomes (CS HA NP) loaded with sodium hyaluronate and chitosan. Chitosan is a copolymer obtained by deacetylation of chitin, and its structure is mainly composed of two units, N-acetyl-D-glucosamine and D-glucosamine. Chitosan can be used as a thickener, rheology modifier and emulsion stabilizer, and its strong hydration ability, good film-forming property and strong antibacterial ability make it useful for beauty masks and wound healing materials. In the embodiment of the present invention, the chitosan coating can further mask the bad smell of squalene, effectively increase the stability and biological activity of the liposomes, and improve its bioavailability. In one embodiment of the present invention, in step S5, the mass concentration of the chitosan solution is 1-2%wt. Preferably, in step S5, the mass concentration of the chitosan solution is 1.5%wt.
[0041] On the other hand, the embodiments of the present invention also provide a highly moisturizing facial cream prepared by any of the above-mentioned preparation methods.
[0042] Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.
[0043] Example 1 A method for preparing a highly moisturizing facial cream comprises the following steps: (1) Weigh 4 g of squalane, 3 g of beeswax, 3 g of vitamin E, 0.5 g of avocado oil, 0.5 g of hydrogenated lecithin, 0.5 g of isopropyl palmitate, 1.5 g of octadecyl alcohol and 3 g of dimethicone, mix, and heat to 85°C to obtain phase A; (2) Weigh 6 g of glycerol, 0.5 g of Carbopol 940, 0.2 g of sodium hyaluronate, 0.1 g of xanthan gum, 2 g of 1,2-hexanediol and 0.5 g of allantoin, add deionized water, mix, and heat to 85°C to obtain phase B; (3) Take 4 g of liposomes, 0.2 g of xinxian ketone, and 0.01 g of gardenia essence, and mix them to obtain phase C; (4) Mix phase A and phase B and emulsify them by shearing for 1 min, cool to 40°C, add phase C, emulsify them by shearing again for 0.5 min, and stir evenly to obtain a highly moisturizing facial cream loaded with squalene liposomes; Among them, the sum of all the components of phase A, phase B, and phase C is 100 g; Wherein, in step (3), the method for preparing liposomes comprises the following steps: 1) Organic phase: Soy lecithin (562.5 mg), β-sitosterol (39.375 mg), octadecylamine (9.375 mg) and squalene (1.2 mL) were dissolved in anhydrous ethanol (75 mL) and stirred to obtain an organic phase; 2) Aqueous phase: Dissolve glycerol (3.75 mL) in distilled water (150 mL) and stir to obtain an aqueous phase; 3) The organic phase was slowly injected into the aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase was 1:2; the mixture was stirred for 1 h, anhydrous ethanol in the suspension was removed by rotary evaporation at 55°C and 100 MPa, and the mixture was homogenized three times in a microfluidizer at a homogenization pressure of 12000 Psi to obtain squalene liposomes (SQ NPs).
[0044] Example 2 A method for preparing a highly moisturizing facial cream comprises the following steps: (1) Weigh 4 g of squalane, 3 g of beeswax, 3 g of vitamin E, 0.5 g of avocado oil, 0.5 g of hydrogenated lecithin, 0.5 g of isopropyl palmitate, 1.5 g of octadecyl alcohol and 3 g of dimethicone, mix, and heat to 85°C to obtain phase A; (2) Weigh 6 g of glycerol, 0.5 g of Carbopol 940, 0.2 g of sodium hyaluronate, 0.1 g of xanthan gum, 2 g of 1,2-hexanediol and 0.5 g of allantoin, add deionized water, mix, and heat to 85°C to obtain phase B; (3) Take 4 g of liposomes, 0.2 g of xinxian ketone, and 0.01 g of gardenia essence, mix them to obtain phase C; (4) Mix phase A and phase B and emulsify them by shearing for 1 min, cool to 40°C, and add phase C; emulsify them by shearing again for 0.5 min, and stir evenly to obtain a highly moisturizing facial cream loaded with squalene and coated with sodium hyaluronate liposomes; Among them, the sum of all the components of phase A, phase B, and phase C is 100 g; Wherein, in step (3), the method for preparing liposomes comprises the following steps: S1, organic phase: dissolve soybean lecithin (562.5 mg), β-sitosterol (39.375 mg), squalene (1.2 mL) and octadecylamine (9.375 mg) in anhydrous ethanol (75 mL) and stir to obtain an organic phase; S2, aqueous phase: Take glycerol (3.75 mL) in distilled water (150 mL), stir and dissolve to obtain aqueous phase; S3, slowly injecting the organic phase into the aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 1:2; stirring for 1 h, removing the anhydrous ethanol in the suspension by rotary evaporation at 55°C and 100 MPa, and homogenizing in a microfluidizer for 3 times at a homogenization pressure of 12000 Psi to obtain squalene liposomes (SQ NP); S4. Drop the above squalene liposome (SQ NP) suspension into an equal volume of sodium hyaluronate solution (0.9%wt), stir, and let stand to obtain sodium hyaluronate-coated squalene liposome (HA NP).
[0045] Example 3 A method for preparing a highly moisturizing facial cream comprises the following steps: (1) Weigh 4 g of squalane, 3 g of beeswax, 3 g of vitamin E, 0.5 g of avocado oil, 0.5 g of hydrogenated lecithin, 0.5 g of isopropyl palmitate, 1.5 g of octadecyl alcohol and 3 g of dimethicone, mix, and heat to 85°C to obtain phase A; (2) Weigh 6 g of glycerol, 0.5 g of Carbopol 940, 0.2 g of sodium hyaluronate, 0.1 g of xanthan gum, 2 g of 1,2-hexanediol and 0.5 g of allantoin, add deionized water, mix, and heat to 85°C to obtain phase B; (3) Take 4 g of liposomes, 0.2 g of xinxian ketone, and 0.01 g of gardenia essence, mix them to obtain phase C; (4) Mix phase A and phase B, shear emulsify for 1 min, cool to 40°C, add phase C, shear emulsify again for 0.5 min, and stir evenly to obtain a highly moisturizing facial cream loaded with squalene and coated with sodium hyaluronate and chitosan liposomes; Among them, the sum of all the components of phase A, phase B, and phase C is 100 g; Wherein, in step (3), the method for preparing liposomes comprises the following steps: S1, organic phase: dissolve soybean lecithin (562.5 mg), β-sitosterol (39.375 mg), squalene (1.2 mL) and octadecylamine (9.375 mg) in anhydrous ethanol (75 mL) and stir to obtain an organic phase; S2, aqueous phase: Take glycerol (3.75 mL) in distilled water (150 mL), stir and dissolve to obtain aqueous phase; S3, slowly injecting the organic phase into the aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 1:2; stirring for 1 h, removing the anhydrous ethanol in the suspension by rotary evaporation at 55°C and 100 MPa, and homogenizing in a microfluidizer for 3 times at a homogenization pressure of 12000 Psi to obtain squalene liposomes (SQ NP); S4, dropping the above squalene liposome (SQ NP) suspension into an equal volume of sodium hyaluronate solution (0.9%wt), stirring, and standing to obtain sodium hyaluronate-coated squalene liposome (HA NP); S5. Drop the above HA NP into an equal volume of chitosan solution (1.5%wt), stir, and let stand to obtain sodium hyaluronate and chitosan coated squalene liposomes (CS HA NP). Comparative Example 1 Same as Example 1, except that in step (3), liposomes not loaded with squalene are added to the facial cream. Comparative Example 2 Same as Example 1, except that in step (3), the liposomes in the cream are replaced by an equal amount of pure water.
[0046] Comparative Example 3 The same as Example 1, except that in step (3), the liposomes in the cream are replaced by an equal amount of pure water, and an equal amount of soy lecithin (562.5 mg) and squalene (1.2 mL) are added to phase A.
[0047] Test Example 1 Liposome crystal form test In order to explore the crystal changes and molecular interactions of β-sitosterol, squalene (SQ), sodium hyaluronate (HA), chitosan (CS) and soybean lecithin (SP) before and after liposome formation, X-ray diffraction analysis was performed on monomers and liposome freeze-dried powder.
[0048] First, monomers of β-sitosterol, squalene (SQ), sodium hyaluronate (HA), chitosan (CS) and soybean lecithin (SP), as well as the liposome samples obtained in Examples 1 to 3, were freeze-dried, and XRD patterns were recorded using an X-ray diffractometer. Cu-Kα was used as the radiation source, the voltage was 40 kV, the current was 15 mA, and for the incident beam, the divergence slit was set to 1° and the receiving slit was set to 0.1 mm. The scanning rate was 4° / min, and the scanning range was 5~40°. The results are shown in Figure 1 . like Figure 1As shown, the β-sitosterol powder showed a sharp diffraction peak, indicating a highly crystalline morphology, but the XRD pattern after participating in the formation of liposomes was relatively rounded, indicating that the β-sitosterol loaded in the liposomes was in an amorphous form and had intermolecular interactions with phospholipids. Test Example 2 Liposome microstructure In order to understand the microscopic morphology of squalene liposomes, transmission electron microscopy was used to observe the vesicles of liposomes. The liposomes were diluted to 1000 times with deionized water, 10 uL of the diluted sample (Example 1-3) was dropped on the copper mesh, left to stand for 10 min, excess sample was absorbed, 10 uL of uranyl acetate dye solution was added to the original copper mesh, left to stand for 1 min, excess dye solution was absorbed, dried and observed under the microscope. The results are shown in Figure 2 .
[0049] like Figure 2 As shown in the figure, the squalene liposomes coated with sodium hyaluronate and chitosan are uniform, stable and translucent. The liposome vesicles have a round structure and are dispersed in the nanoemulsion system without aggregation and fusion.
[0050] like Figure 3 As shown, after being placed at room temperature (25°C) for 30 days, the liposomes coated with small molecule polysaccharides (HA NP, CS HANP) showed no obvious precipitation and aggregation by naked eye observation, and their state was better than that of the uncoated liposomes (SQ NP).
[0051] Test Example 3 Cream stability test aHeat resistance and stability Take an appropriate amount of squalene cream sample in a transparent sealed bottle, keep it at 60℃ for 24 hours, and observe whether the cream has stratification and demulsification after returning to room temperature. Figure 4 and Figure 5 .
[0052] like Figure 4 As shown, the facial cream prepared by the present invention has a fine cream body and a light yellow appearance. After application, it is refreshing and non-greasy, and is easy to spread and has good ductility.
[0053] b Freeze-thaw stability Take an appropriate amount of squalene cream sample in a transparent sealed bottle and place it in a -20℃ refrigerator for 24 hours. Take out the sample, wait for it to return to room temperature and place it in a -20℃ refrigerator again for 24 hours. Repeat this three times and take out the sample. After returning to room temperature, observe whether the cream has stratification and demulsification. The results are shown in Figure 5 .
[0054] c Centrifugal stability Take an appropriate amount of squalene cream sample in a 10 mL EP tube, centrifuge the tube containing the sample at 3000 r / min for 20 min, and observe whether the cream has stratification and demulsification after the end. Figure 5 .
[0055] like Figure 5 As shown in the figure, after centrifugation at 3000 r / min for 20 min, the cream still did not show stratification and demulsification. After the cream was placed in a -20℃ refrigerator for 24 h and repeatedly frozen and thawed three times, and kept at 60℃ for 24 h, no stratification of the emulsion was observed, indicating that the cream has good centrifugal, cold-resistant and heat-resistant stability.
[0056] Test Example 4 Face cream moisturizing rate test Weigh an appropriate amount of squalene cream sample and apply it evenly on a 7.5×5.0 cm 2 On the glass plate, the mass of the tape and the plate is recorded as M0, and the mass of the tape and the plate after applying the cream is recorded as M1. Place it in a constant temperature box with a humidity RH = 60% and a temperature of 27°C, and weigh it every 2, 4, 6, 8, 10, 12, and 24 hours. The mass at this time is recorded as M2, and the moisturizing rate of each sample is calculated according to the following formula:
[0057] The changes of moisturizing rate of liposome cream at different time Figure 6 As shown in the figure, the moisturizing rate of the creams showed a downward trend over time, and the moisturizing rates of the creams in Example Groups 1 to 3 were all higher than those in the Comparative Example Group. After 4 hours, the moisturizing rates of the creams in Comparative Example Groups 1 to 3 dropped sharply, while the moisturizing rates of Examples 1 to 3 were maintained at more than 70%, which showed that the liposome cream modified with small molecule polysaccharides had good long-term moisturizing ability.
[0058] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.
Claims
1. A method for preparing a highly moisturizing facial cream, characterized in that: The steps include: (1) Weigh squalane, beeswax, vitamin E, avocado oil, hydrogenated lecithin, isopropyl palmitate, stearyl alcohol, and dimethicone, mix, and heat to obtain phase A; (2) Weigh glycerin, carbomer 940, sodium hyaluronate, xanthan gum, 1,2-hexanediol, and allantoin, add deionized water, mix, and heat to obtain phase B; (3) Weigh liposomes, fennel, and gardenia essence, mix them, and obtain phase C; (4) After mixing phase A and phase B, perform the first shear emulsification, cool, mix with phase C, perform the second shear emulsification, and stir to obtain a highly moisturizing facial cream.
2. The preparation method according to claim 1, characterized in that: Step (1) In phase A, 0-4 parts of squalane, 2-4 parts of beeswax, 2-4 parts of vitamin E, 0.1-1 parts of avocado oil, 0.1-1 parts of hydrogenated lecithin, 0.1-1 parts of isopropyl palmitate, 1-2 parts of octadecyl alcohol, and 2-4 parts of dimethicone; In step (2), in phase B, 5-10 parts of glycerin, 0.1-1 part of Carbopol 940, 0.1-1 part of sodium hyaluronate, 0.08-0.12 part of xanthan gum, 1-3 parts of 1,2-hexanediol, and 0.1-1 part of allantoin; In step (3), in phase C, 1-4 parts of liposomes, 0.1-0.5 parts of xinxianketone, and 0.008-0.012 parts of gardenia essence; The sum of all components of phase A, phase B and phase C is 100 parts.
3. The preparation method according to claim 1 or 2, characterized in that: In step (3), the liposome is prepared by the following steps: S1, dissolving soybean lecithin, phytosterol, octadecylamine and squalene in anhydrous ethanol and mixing to obtain an organic phase; S2, mix glycerol and distilled water to obtain an aqueous phase; S3. The organic phase and the aqueous phase are mixed, and the mixture is subjected to rotary evaporation to remove the anhydrous ethanol in the suspension, and then the mixture is homogenized in a microfluidizer to obtain squalene liposomes.
4. The preparation method according to claim 1, characterized in that: In step (1) and step (2), heating is performed to 85°C.
5. The preparation method according to claim 1, characterized in that: In step (4), the first shear emulsification time is 1 min; the mixture is cooled to 40° C.; and the second shear emulsification time is 0.5 min.
6. The preparation method according to claim 3, characterized in that: In step S1, the phytosterol includes at least one of cholesterol, stigmasterol or β-sitosterol; In step S1, the dosage ratios of soybean lecithin, phytosterols, octadecylamine, squalene, and anhydrous ethanol are 500-600 mg, 35-45 mg, 5-15 mg, 0.8-1.5 mL, and 50-100 mL, respectively.
7. The preparation method according to claim 3, characterized in that: In step S2, the volume ratio of glycerol to distilled water is 1-5 mL:150 mL; In step S3, the mass ratio of the organic phase to the aqueous phase is 1:
2.
8. The preparation method according to claim 3, characterized in that: The step S4 is further included, specifically comprising: dropping the squalene liposome obtained in S3 into an equal volume of sodium hyaluronate solution, stirring, and standing to obtain the squalene liposome coated with sodium hyaluronate; Preferably, in step S4, the mass concentration of the sodium hyaluronate solution is 0.5-1.5%wt.
9. The preparation method according to claim 8, characterized in that: The step S5 is further included, specifically comprising: dropping the sodium hyaluronate-coated squalene liposome obtained in S4 into an equal volume of chitosan solution, stirring, and standing to obtain the sodium hyaluronate- and chitosan-loaded squalene liposome; Preferably, in step S5, the mass concentration of the chitosan solution is 1-2%wt.
10. A highly moisturizing facial cream prepared by the preparation method according to any one of claims 1 to 9.
Citation Information
Patent Citations
Long-lasting moisturizing face cream and its preparation method
CN111973494B
An anti-aging and antioxidant liposome face cream and its preparation method
CN113262194B
Synergistic repair composition containing tea polyphenol and application thereof
CN118161433A