CN113288841A - Facial mask liquid and preparation method thereof - Google Patents

Facial mask liquid and preparation method thereof Download PDF

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CN113288841A
CN113288841A CN202110741853.0A CN202110741853A CN113288841A CN 113288841 A CN113288841 A CN 113288841A CN 202110741853 A CN202110741853 A CN 202110741853A CN 113288841 A CN113288841 A CN 113288841A
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glabridin
liposome
water
cell
mask liquid
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CN113288841B (en
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卢永杰
程路诗
张炽坚
张兵
江桦
关焕敏
艾勇
何廷刚
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Hua An Tang Biotech Group Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
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    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/49Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/4973Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52Stabilizers
    • A61K2800/524Preservatives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/56Compounds, absorbed onto or entrapped into a solid carrier, e.g. encapsulated perfumes, inclusion compounds, sustained release forms

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Abstract

The invention relates to the technical field of cosmetics, in particular to a mask liquid and a preparation method thereof. The invention discloses a mask liquid, which uses sakura cell glabridin liposome, and transfers glabridin into epidermis deeper by utilizing the characteristic of fusion of liposome and cell membrane, so that the whitening effect is more obvious. In addition, the use of the cherry blossom cell water enables the glabridin liposome to have natural antiseptic and antioxidant effects, thereby being beneficial to prolonging the preservation time of the facial mask liquid liposome.

Description

Facial mask liquid and preparation method thereof
Technical Field
The invention relates to the technical field of cosmetics, in particular to a mask liquid and a preparation method thereof.
Background
Glabridin, also known as licoflavone or glabridin, is a flavonoid substance in Glycyrrhiza glabra with whitening and anti-aging effects, and achieves the whitening effect by removing free radicals and melanin in the muscle bottom. However, glabridin in a natural state after extraction is oil-soluble white powder, and in the application of O/W cosmetics, glabridin is generally emulsified after being dissolved in an oil phase, and is uniformly dispersed in a water phase by an emulsifier, or is solubilized in the water phase by a solubilizer, and the use method is complicated. Even so, glabridin can only stay in the stratum corneum, and melanocytes which generate melanin exist in a deeper basal layer and a deeper spinous cell layer of the epidermis, and the ordinary emulsified glabridin dissolved in the oil phase cannot directly reach the melanocytes, so that the whitening effect is greatly reduced.
Disclosure of Invention
In view of this, the invention provides a mask liquid and a preparation method thereof, and the mask liquid uses sakura cell glabridin liposome, so that the whitening effect of the mask liquid is more obvious.
The specific technical scheme is as follows:
the invention provides a mask liquid which comprises the following components in percentage by mass:
0 to 1.5 percent of thickening agent;
3-30% of polyol;
0.01-0.15% of chelating agent;
0.1 to 1.5 percent of preservative;
cherry blossom cell water glabridin liposome 0.1-10%;
the balance being water.
Preferably, the amount of the surfactant is, in mass percent,
0.001 to 0.6 percent of thickening agent;
5-25% of polyol;
0.01-0.1% of chelating agent;
0.2 to 1.0 percent of preservative;
cherry cell water glabridin liposome 0.5-5%.
In the present invention, the thickener is an acrylic acid (ester) thickener or a cellulose thickener. Wherein, the acrylic acid (ester) thickening agent needs to be added with a neutralizing agent to achieve the thickening effect, and the acrylic acid (ester) thickening agent is polyacrylic acid; the cellulose thickener is one or more selected from xanthan gum, sodium alginate and hydroxypropyl cellulose.
The polyol is easily soluble in water and has a certain moisturizing effect. One or more than two of polyhydric alcohol glycerol, propylene glycol, butanediol, isoprene glycol and hexanediol.
The neutralizing agent can make the acrylic acid (ester) type thickening agent reach the alkaline substance of thickening effect. The neutralizing agent is selected from triethanolamine, arginine, sodium hydroxide or potassium hydroxide.
The neutralizing agent is 0.05-0.2% by mass, more preferably 0.1-1% by mass, and still more preferably 0.1-0.5% by mass.
The chelating agent is disodium EDTA.
The preservative is a chemical preservative or a plant preservative. The preservative is one or more than two of phenoxyethanol, ethylhexyl glycerol, caprylyl glycol and colloidal silver.
The invention also provides a preparation method of the facial mask liquid, which comprises the following steps:
step 1: mixing phospholipid, cholesterol, glabridin and cherry blossom cell water to form a suspension, and adjusting and shearing the suspension in a heating and heat preservation state to obtain a cherry blossom cell water glabridin liposome;
step 2: mixing thickener, polyalcohol, water, chelating agent, neutralizer, antiseptic and sakura cell glabridin liposome to obtain facial mask liquid.
In the step 1 of the invention, phospholipid, insoluble drug and water are mixed to obtain suspension, and the suspension is dispersed by high-speed shearing at a proper temperature, so that the phospholipid and the insoluble drug are crushed to form a micron scale. Under the micron scale, after long-time shearing, the insoluble drug particles and the phospholipid particles interact to emulsify, and then self-assemble to form the micron-scale liposome.
In the step 1 of the invention, no toxic or harmful organic solvent is used in the process of preparing the fat-soluble drug liposome, the production process is safe and environment-friendly, and the product safety is high; the preparation equipment and the process are simple, and the method is suitable for large-scale production and improves the production efficiency.
Cherry blossom (academic name: Cerasus sp.): is a general term of several plants in the genus of cerasus of the family Rosaceae, and is named as "Tokyo cherry blossom" in the newly revised name of "Chinese plant record", also called as "Japanese cherry blossom". The oriental cherry has extremely high ornamental value and also has the effects of medicine, skin care and the like. In the aspect of skin care, the cherry blossom has good effects of shrinking pores and balancing grease, contains rich natural vitamin A, B, E, and the cherry leaf flavone also has the effects of maintaining beauty, keeping young, strengthening mucous membrane and promoting sugar metabolism, and can be used for keeping young skin. Cherry blossom has the effects of tendering skin and brightening skin, is one of important raw materials of skin care products, is usually extracted and refined, experts extract the cherry blossom into cherry blossom tender oil by using a three-high fresh extraction technology, and the cherry blossom extract contains a component called cherry blossom enzyme which is commonly used for removing acnes. The cherry blossom cell water obtained by low-temperature vacuum distillation extraction contains trace volatile components, and the cherry blossom cell water is used as a solvent for preparing the liposome in the step 1, so that the obtained liposome has the effects of natural preservation and antioxidation, and the liposome is preserved without adding any preservative.
In addition, the glabridin liposome is used, a bilayer similar to a skin cell membrane structure is formed by soybean lecithin, the glabridin is wrapped in the bilayer, and the glabridin is transferred to a deeper part of the epidermis by utilizing the characteristic that the liposome can be fused with the cell membrane, so that the more effective whitening effect is achieved. The liposome is coated to be water-soluble, and can be directly added in O/W type or aqueous cosmetic preparation, and the transparency can be maintained after the addition.
In step 1 of the present invention, the phospholipid includes one or more of soybean lecithin, egg yolk lecithin, hydrogenated lecithin, dilauroyl phosphatidylcholine, dimyristoyl phosphorylcholine, dipalmitoyl phosphorylcholine, distearoyl phosphatidylcholine, dioleoyl phosphatidylcholine, dilauroyl phosphatidylethanolamine, dimyristoyl phosphatidylethanolamine, dipalmitoyl phosphatidylethanolamine, distearoyl phosphatidylethanolamine and dioleoyl phosphatidylethanolamine.
Before mixing, the method also comprises the following steps: adding a surfactant. The addition of a surfactant can facilitate the solubilization of the fat-soluble drug.
The surfactant is ionic surfactant and/or nonionic surfactant, wherein the cationic surfactant comprises quaternary ammonium salt, the anionic surfactant comprises higher fatty acid salt or sulfate salt, and the nonionic surfactant comprises one or more than two of tween, span, PEG fatty acid ester and polyglycerol-10-hard fatty acid ester.
Before mixing, the method also comprises the following steps: the polyol is added. The addition of the polyol can further facilitate the dissolution of a portion of the fat-soluble drug. Glabridin has low solubility in polyhydric alcohol.
The polyhydric alcohol comprises one or more of glycerol, propylene glycol, butylene glycol, pentylene glycol, and isoprene glycol.
In the step 1, according to the mass percentage,
2-15% of phospholipid;
0.01-5% of glabridin;
0-5% of cholesterol;
the balance is cherry blossom cell water.
Preferably, the amount of the surfactant is, in mass percent,
2-10% of phospholipid;
0.01-4% of glabridin;
0-4% of cholesterol;
the balance is cherry blossom cell water.
More preferably, the amount of the surfactant is, in mass percent,
2-8% of phospholipid;
0.1-3% of glabridin;
0-3% of cholesterol;
the balance is cherry blossom cell water.
In the invention, the weight percentage of the surfactant is 0.1-20%, preferably 0.1-15%, and more preferably 0.1-8%; 5 to 60% of a polyol, preferably 5 to 45%, more preferably 5 to 30%.
In step 1 of the invention, the heating temperature of the suspension liquid needs to be higher than the phase transition temperature of the phospholipid. The heating temperature is 50-100 ℃, and preferably 50-70 ℃; then, maintaining the heating temperature for shearing, wherein a shearing disperser is adopted for shearing; the shearing rate is 8000-20000 rpm (rotor diameter is 13mm), the shearing time is more than 30min, preferably more than 60min at the shearing rate of 8000-15000 rpm (rotor diameter is 13mm), more preferably 60-90 min. The liposome obtained after shearing is micron-sized.
The nano-scale liposome has better dispersibility and stability and better skin permeability. Therefore, the method further comprises, after the high-speed shearing in step 1 of the present invention: homogenizing under high pressure. The high-pressure homogenization can crush and thin the micron-sized liposome to obtain the nano-sized liposome. The high-pressure homogenization specifically comprises the following steps: each cycle was carried out at a pressure of 400bar, 600bar, 800bar, 1000bar for 2 or more times.
When the thickener is an acrylic acid (ester) thickener, the step 2 of the invention is specifically as follows: mixing and uniformly dispersing a thickening agent and polyhydric alcohol, adding water and a chelating agent, stirring and heating to 75-80 ℃, stopping heating after complete dissolution, then adding the mixture of a neutralizing agent and water into the above material body, stirring uniformly, adding the sakura cell glabridin liposome, keeping stirring, adding a preservative, and stirring uniformly to obtain a mask liquid;
when the thickener is a cellulose-type thickener, the step 2 of the invention specifically comprises the following steps: mixing thickener and polyalcohol, dispersing, adding water and chelating agent, stirring, heating to 75-80 deg.C, dissolving completely, stopping heating, adding sakura cell glabridin liposome, stirring, adding antiseptic, and stirring to obtain facial mask solution;
if the preservative is caprylyl glycol, the preservative can be added simultaneously with the thickener and the polyol.
According to the technical scheme, the invention has the following advantages:
the invention provides a mask liquid, which uses sakura cell glabridin liposome, and transfers glabridin into epidermis deeper by utilizing the characteristic of fusion of liposome and cell membrane, so that the whitening effect is more obvious. In addition, the use of the cherry blossom cell water enables the glabridin liposome to have natural antiseptic and antioxidant effects, thereby being beneficial to prolonging the preservation time of the facial mask liquid liposome.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
FIG. 1 is an optical microscope photograph (3 μm on scale) of liposomes in an emulsion prepared in step 1 of example 2 of the present invention;
FIG. 2 is an optical microscope photograph (3 μm on scale) of liposomes in the emulsion obtained in step 1 of example 3 of the present invention;
FIG. 3 is an optical microscope photograph (3 μm on scale) of liposomes in the emulsion obtained in step 1 of example 4 of the present invention;
FIG. 4 is an optical microscope photograph (3 μm on scale) of liposomes in the emulsion obtained in step 1 of example 5 of the present invention;
FIG. 5 is an optical microscope photograph (3 μm on scale) of liposomes in the emulsion obtained in step 1 of example 6 of the present invention;
FIG. 6 is an optical microscope photograph (3 μm on scale) of liposomes in an emulsion prepared in step 1 of example 7 of the present invention;
FIG. 7 is an optical microscope photograph (3 μm on scale) of liposomes in an emulsion prepared in step 1 of example 9 of the present invention;
FIG. 8 is a transmission electron micrograph (100 nm on a scale) of glabridin liposome prepared in step 2 of example 9 of the present invention;
FIG. 9 is a graph showing the results of B16 experiments in which Glabradin is Glabridin, GL is Glabridin liposome, and GL-S is Glabridin liposome-formulated oriental cherry plant water, in test example 3 of the present invention;
FIG. 10 is a histogram of melanin content in B16 cells according to Experimental example 3, wherein Glabradin is Glabridin, GL is Glabridin liposome, and GL-S is Glabridin liposome-compounded oriental cherry plant water.
Detailed Description
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it should be apparent that the embodiments described below are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
This example is the preparation of cherry blossom cell water
Weighing fresh petal of oriental cherry 50kg, cutting into size of 4-5 mm with a cutter, placing into drying equipment at low temperature of 150L, setting vacuum degree at-90 kPa, extracting temperature at about 40 deg.C, stirring speed at 30rmp, and extracting time at 6 h. Condensing and collecting cherry cell water, and filtering with 0.22 μm filter membrane to obtain cherry cell water.
Example 2
The preparation formula of the sakura cell water glabridin liposome is shown in table 1, and the preparation method comprises the following specific steps:
(1) adding phospholipid (PC 95%), glabridin and cholesterol into cherry blossom cell water, heating in water bath at 50 deg.C, and high-speed shearing with experiment type IKA high-speed shearing disperser at 10000rpm for 30min to obtain uniform emulsion.
(2) And (2) homogenizing the uniform emulsion obtained in the step (1) under high pressure, and circulating for 2 times under 400/600/800/1000bar pressure respectively to obtain the uniform sakura cell water glabridin liposome.
As can be seen in FIG. 1, after high shear in step 1, a multi-lamellar globular structure resembling liposomes is observed in the emulsion in step 1.
Examples 3 to 5
The preparation formula of the sakura cell water glabridin liposome is shown in table 1, and the preparation method comprises the following specific steps:
(1) adding phospholipid (PC 95%), glabridin and cholesterol into cherry blossom cell water, heating in water bath at 60 deg.C, and high-speed shearing with experiment type IKA high-speed shearing disperser at 10000rpm for 60min to obtain uniform emulsion.
(2) And (2) homogenizing the uniform emulsion obtained in the step (1) under high pressure, and circulating for 2 times under 400/600/800/1000bar pressure respectively to obtain the uniform sakura cell water glabridin liposome.
As can be seen from FIGS. 2 to 4, after the high-speed shearing in step 1, a multi-layer spherical structure similar to liposome can be observed in the emulsion in step 1.
Example 6
The preparation formula of the sakura cell water glabridin liposome is shown in table 1, and the preparation method comprises the following specific steps:
(1) adding phospholipid (PC 95%), polyglycerol-10-stearate, glabridin and cholesterol into cherry blossom cell water, heating in water bath at 50 deg.C, and high-speed shearing at 10000rpm for 30min with an experimental IKA high-speed shearing disperser to obtain uniform emulsion.
(2) And (2) homogenizing the uniform emulsion obtained in the step (1) under high pressure, and circulating for 2 times under 400/600/800/1000bar pressure respectively to obtain the uniform sakura cell water glabridin liposome.
As can be seen in FIG. 5, after high shear in step 1, a multi-lamellar globular structure resembling liposomes is observed in the emulsion in step 1.
Examples 7 to 8
The preparation formula of the sakura cell water glabridin liposome is shown in table 1, and the preparation method comprises the following specific steps:
(1) adding phospholipid (PC 95%), polyglycerol-10-stearate, glabridin and cholesterol into a mixture of oriental cherry cell water and butanediol, heating in a water bath at 50 deg.C, and high-speed shearing with an experimental IKA high-speed shearing disperser at 10000rpm for 30min to obtain uniform emulsion.
(2) And (2) homogenizing the uniform emulsion obtained in the step (1) under high pressure, and circulating for 2 times under 400/600/800/1000bar pressure respectively to obtain the uniform sakura cell water glabridin liposome.
As can be seen in FIG. 6, in example 7, after high shear in step 1, a multi-lamellar globular structure resembling liposomes is observed in the emulsion in step 1.
Example 9
The preparation formula of the sakura cell water glabridin liposome is shown in table 1, and the preparation method comprises the following specific steps:
(1) adding phospholipid (PC 95%), polyglycerol-10-stearate, glabridin and cholesterol into cherry blossom cell water, heating in water bath at 60 deg.C, and high-speed shearing at 10000rpm for 60min with an experimental IKA high-speed shearing disperser to obtain uniform emulsion.
(2) And (2) homogenizing the uniform emulsion obtained in the step (1) under high pressure, and circulating for 2 times under 400/600/800/1000bar pressure respectively to obtain the uniform sakura cell water glabridin liposome.
As can be seen in FIG. 7, after high shear in step 1, a multi-lamellar globular structure resembling liposomes is observed in the step 1 emulsion.
As can be seen from fig. 8, glabridin was successfully encapsulated in liposomes.
Example 10
The preparation formula of the sakura cell water glabridin liposome is shown in table 1, and the preparation method comprises the following specific steps:
(1) adding phospholipid (PC 95%), polyglycerol-10-stearate, glabridin and cholesterol into a mixture of oriental cherry cell water and butanediol, heating in water bath at 50 deg.C, and high-speed shearing with an experimental IKA high-speed shearing disperser at 8000rpm for 30min to obtain uniform emulsion.
(2) And (2) homogenizing the uniform emulsion obtained in the step (1) under high pressure, and circulating for 2 times under 400/600/800/1000bar pressure respectively to obtain transparent and uniform sakura cell glabridin water liposome.
Example 11
The preparation formula of the sakura cell water glabridin liposome is shown in table 1, and the preparation method comprises the following specific steps:
(1) adding phospholipid (PC 95%), polyglycerol-10-stearate, glabridin and cholesterol into a mixture of oriental cherry cell water and butanediol, heating in water bath at 60 deg.C, and high-speed shearing with an experimental IKA high-speed shearing disperser at 10000rpm for 30min to obtain uniform emulsion.
(2) And (2) homogenizing the uniform emulsion obtained in the step (1) under high pressure, and circulating for 2 times under 400/600/800/1000bar pressure respectively to obtain transparent and uniform sakura cell glabridin water liposome.
Example 12
The preparation formula of the sakura cell water glabridin liposome is shown in table 1, and the preparation method comprises the following specific steps:
(1) adding phospholipid (PC 95%), polyglycerol-10-stearate, glabridin and cholesterol into a mixture of oriental cherry cell water and butanediol, heating in a water bath at 50 deg.C, and high-speed shearing with an experimental IKA high-speed shearing disperser at 10000rpm for 60min to obtain uniform emulsion.
(2) And (2) homogenizing the uniform emulsion obtained in the step (1) under high pressure, and circulating for 2 times under 400/600/800/1000bar pressure respectively to obtain transparent and uniform sakura cell glabridin water liposome.
Example 13
The preparation formula of the sakura cell water glabridin liposome is shown in table 1, and the preparation method comprises the following specific steps:
(1) adding phospholipid (PC 95%), polyglycerol-10-stearate, glabridin and cholesterol into a mixture of oriental cherry cell water and butanediol, heating in a water bath at 50 deg.C, and high-speed shearing with an experimental IKA high-speed shearing disperser at 10000rpm for 90min to obtain uniform emulsion.
(2) And (2) homogenizing the uniform emulsion obtained in the step (1) under high pressure, and circulating for 2 times under 400/600/800/1000bar pressure respectively to obtain transparent and uniform sakura cell glabridin water liposome.
Comparative example 1
The preparation formula of glabridin liposome in this example is shown in table 1, and the specific preparation steps are as follows:
(1) adding phospholipid (PC 95%), glabridin and cholesterol into water, heating in water bath at 60 deg.C, and high-speed shearing with experiment type IKA high-speed shearing disperser at 10000rpm for 60min to obtain uniform emulsion.
(2) And (2) homogenizing the uniform emulsion obtained in the step (1) under high pressure, and circulating for 2 times under 400/600/800/1000bar pressure respectively to obtain uniform glabridin liposome.
Comparative examples 2 to 3
The comparative example is the preparation of sakura cell water glabridin liposome, the formula is shown in table 1, and the preparation steps are as follows:
(1) dissolving phospholipid (PC 95%), polyglycerol-10-stearate, glabridin and cholesterol in 200g methanol-chloroform (mass ratio of 62:38) to obtain clear and transparent solution, and performing rotary evaporation to remove organic solvent to obtain the film.
(2) And (2) placing the film obtained in the step (1) in a water bath at 60 ℃, and adding a mixed solution of oriental cherry cell water and butanediol in a prescription amount while stirring to obtain a crude emulsion. Homogenizing the crude emulsion under high pressure, and circulating for 2 times under 400/600/800/1000bar pressure to obtain sakura cell glabridin liposome.
Comparative example 4
The comparative example is the preparation of sakura cell water glabridin liposome, the formula is shown in table 1, and the preparation steps are as follows:
(1) adding phospholipid (PC 95%), polyglycerol-10-stearate, glabridin and cholesterol into a mixture of water and butanediol, heating in water bath at 30 deg.C, and high-speed shearing with an experimental IKA high-speed shearing disperser at 10000rpm for 30min to obtain uniform emulsion.
(2) And (2) homogenizing the uniform emulsion obtained in the step (1) under high pressure, and circulating for 2 times under 400/600/800/1000bar pressure to obtain transparent and uniform glabridin liposome.
TABLE 1 example and comparative example formulations
Figure BDA0003141656210000101
Test example 1
The glabridin liposomes prepared in example 9 and comparative example 1 were dispersed using PBS as a dispersant, and the average particle diameter was measured using a Zeta sizer; separating the encapsulated and free glabridin by an ultrafiltration centrifugal tube, detecting the glabridin content by HPLC and calculating the encapsulation rate. Test results are shown in table 2.
As can be seen from the results in table 2, in the example, in step 1, glabridin was emulsified and dissolved in water to obtain liposomes, and the particle size of the liposomes in the emulsion was about 5 to 20 μm. The sakura cell aqueous glabridin liposome prepared in most examples has basically no difference in appearance, average particle size and glabridin content from the liposome prepared by the film method of comparative examples 2-3. Example 9 compared with the cherry blossom cell water glabridin liposome prepared in comparative example 1, there was no substantial difference in appearance, average particle size, and glabridin content, which indicates that the effect of preparing liposome using cherry blossom cell water instead of pure water in the example was substantially uniform, and the liposome was able to replace pure water as solvent. The glabridin liposome prepared by the liposome preparation method of comparative example 4 is in a yellow turbid state in appearance, and insoluble particles exist; the sample has larger particle size, the encapsulation efficiency of the glabridin medicament is obviously reduced, which shows that when the temperature is insufficient, the phospholipid phase cannot be fully converted into the liquid crystal phase, and fat-soluble medicaments such as glabridin and the like are difficult to fully react with phospholipid molecules, so that the particle size is increased, the encapsulation efficiency is reduced, and the quality of a liposome preparation is reduced.
Table 2 characterization of glabridin liposomes for examples and comparative examples
Figure BDA0003141656210000111
Figure BDA0003141656210000121
Test example 2
The glabridin liposomes prepared in the examples and the comparison were subjected to preservative challenge test.
Inoculating certain amount of bacteria and fungi, and detecting the change of microbial quantity according to the detection method of the preservative efficacy test of the microorganisms in United states Pharmacopeia USP32<51> at intervals of 0 day, 7 days, 14 days, 21 days and 28 days, wherein the test results are shown in Table 3.
The microbial detection was carried out according to the national standard GB7918.2-87 "cosmetic microbial Standard test method", and the test results are shown in Table 4.
As can be seen from tables 3 and 4, the sakura cell glabridin liposome prepared in the examples can inhibit the growth of microorganisms and has a certain preservative effect.
Table 3 preservative challenge test results for glabridin liposomes of examples 2, 6, 8, 9, 10
Figure BDA0003141656210000122
Figure BDA0003141656210000131
TABLE 4
Figure BDA0003141656210000132
Test example 3
The sakura cell aqueous glabridin liposome prepared in example 9 and comparative 1 was subjected to MTT toxicity test and melanin content test on mouse melanoma cells B16.
1. B16 cells were plated in 96-well plates at 5X 10 cells per well3Density inoculation of cells and incubation at 37 deg.C5% CO in the breeding box2Treating glabridin liposome and pure glabridin with different concentrations for 24 hr. Then, 20. mu.L of MTT solution (5mg/mL) was added to each well, and the cells were maintained at 37 ℃ for 3 h. The supernatant was carefully aspirated and its absorbance at 570nm was measured by a microplate reader (Bio-Rad, USA) to calculate the cell inhibition rate.
Fig. 9 is a graph showing the results of the B16 cell inhibition ratio test provided in this test example. The higher the cytostatic rate, the higher the cell death rate. Generally, the inhibition rate is below 20%, and no toxicity is considered. As shown in FIG. 9, the inhibition rate of pure glabridin is much higher than that of liposome, and the safety of liposome is better than that of pure glabridin.
2. B16 cells were plated at 2X 10 per well5Individual cells were seeded at a density in 12-well plates and then incubated at 37 ℃ and 5% CO2Incubate for 24 hours. After adding deionized water alone to the control group, and adding pure glabridin, liposomes of example 6 and liposomes of example 11 at different concentrations to the sample group, respectively, and adding 200nM α -MSH, respectively, for 48 hours, the cells were lysed in 1mL of 1M NaOH (containing 10% DMSO) for 30 minutes, incubated in a water bath at 80 ℃ for 1 hour, and then centrifuged at 3000rpm for 20 minutes. The relative amount of melanin in the cells was calculated by measuring the Optical Density (OD) of the supernatant at 475nm by an ELISA reader.
Melanin content (%) ═ ODs/OD 0X 100
OD0 is control ODs is sample group optical density
FIG. 10 is a histogram of melanin content of B16 cells provided in this test example. As shown in fig. 10, before the sample is added, the black content of the melanoma cells is about 100%, and after different samples with different concentrations are added, the melanin can be significantly reduced, wherein the liposome prepared by using the cherry blossom cell water has the most significant effect, which indicates that the liposome has a certain whitening synergistic effect.
Example 14
1. Mixing and uniformly dispersing 0.002% of polyacrylic acid, 2.0% of 1, 3-propylene glycol and 3.0% of glycerin, adding 90.70% of deionized water and 0.1% of EDTA disodium, keeping stirring and heating to 80 ℃, wherein the stirring speed cannot be too high so as to avoid generating bubbles;
2. after complete dissolution, heating was stopped. 0.2% triethanolamine and 3% deionized water were mixed and added to a body of material which was cooled to almost room temperature, and after stirring well, 4% of the sakura cell aqueous glabridin liposome prepared in example 6 (glabridin content 0.5%) was added and the stirring was maintained.
3. Finally, 0.6 percent of phenoxyethanol is added as a preservative and stirred evenly.
Example 15
1. Mixing 0.15% xanthan gum, 0.15% sodium alginate and 0.3% hydroxyethyl cellulose with 2.0% 1, 2-hexanediol, 3.0% 1, 3-propanediol, 5% glycerol, 3.0% butanediol, 1.0% octaethylene glycol and 12.0% isoprene glycol, uniformly dispersing, adding 72.99% deionized water and 0.01% disodium EDTA, stirring and heating to 80 ℃, wherein the stirring speed cannot be too high to avoid generating bubbles;
after complete dissolution, heating was stopped. Adding 4% of sakura cell water glabridin liposome (glabridin content 0.5%) obtained in example 6 into the mixture cooled to room temperature, and stirring to room temperature.
Example 16
1. Mixing 0.001% of polyacrylic acid, 0.15% of xanthan gum and 0.15% of sodium alginate with 0.5% of 1, 2-hexanediol, 2.0% of 1, 3-propanediol, 4% of glycerol, 2.0% of butanediol and 2.0% of isoprene glycol, uniformly dispersing, adding 85.45% of deionized water and 0.05% of disodium EDTA, keeping stirring and heating to 80 ℃, wherein the stirring speed cannot be too high so as to avoid generating bubbles;
2. after complete dissolution, heating was stopped. Dissolving 0.1% arginine in 3% deionized water, adding into a material body which is almost cooled to room temperature, stirring well, adding 4% of sakura cell aqueous glabridin liposome prepared in example 6 (glabridin content: 0.5%) and keeping stirring.
3. And finally, adding 0.2% of colloidal silver solution (with active matter content of 0.3%) as a preservative and uniformly stirring.
Example 17
1. Mixing and uniformly dispersing 0.001% of polyacrylic acid, 0.15% of xanthan gum and 0.15% of sodium alginate with 0.5% of 1, 2-hexanediol, 2.0% of 1, 3-propanediol, 4% of glycerol and 2.0% of isoprene glycol, adding 85.85% of deionized water and 0.05% of EDTA disodium, keeping stirring and heating to 80 ℃, wherein the stirring speed cannot be too high so as not to generate bubbles;
2. after complete dissolution, heating was stopped. Further, 0.02% high purity glabridin powder dispersed with 2.0% butanediol was added to the step 1 material body at about 45 ℃ and kept under stirring.
3. 0.1% arginine was dissolved in 3% deionized water and added to the body which was allowed to cool to room temperature.
4. And finally, adding 0.2% of colloidal silver solution (with active matter content of 0.3%) as a preservative and uniformly stirring.
Test example 4
Appearance test, pH test and viscosity test were performed on the facial mask solutions prepared in examples 1 to 4, and the results are shown in table 5. As can be seen from Table 5, the facial mask solutions prepared in examples 1-4 have the appearance and physical and chemical properties meeting the requirements of cosmetics.
TABLE 5
Figure BDA0003141656210000151
Test example 5
Stability test of the facial mask solutions obtained in examples 1 to 4
The stability test method comprises the following steps: the samples of examples 1 to 4 were stored at a high temperature in the dark of 40 ℃ for one month, at a room temperature in the dark of 25 ℃ for one month, at a low temperature in the dark of 4 ℃ for one month, and at a natural light for one month, and after returning to the room temperature, the appearance of the samples was observed and compared with the room temperature in the dark, and the results are shown in table 6.
As is clear from Table 6, the stability of the facial mask solutions obtained in examples 1 to 4 was good.
TABLE 6
Figure BDA0003141656210000161
Test example 6
Screening subjects 90 humans, wherein the blank control group: 30 persons, using a mask solution without glabridin (the mask solution differs from example 16 only in that glabridin is not added); experimental groups: 30 persons, using the facial mask solution prepared in example 16; control group: 30 persons, using the facial mask solution prepared in example 17. After cleaning face in the evening every day, a proper amount of the face cream is applied to the face (about 5g) and continuously used for 8 weeks. Skin color was measured on the facial skin of the subject 3 times after the start day, 4 weeks and 8 weeks (using a Colorimeter, germany), and the test results are shown in table 7.
The value of L obtained by color measurement represents the brightness of the skin, and the larger the value, the more the color is biased to white. b represents the degree of blue-yellow, the greater the number, the more yellow the skin. The ITA ° values are used for skin color grading, the larger the value, the brighter the skin.
As can be seen from table 7, the whitening effect of the facial mask solution prepared from the sakura cell water glabridin liposome of the experimental group was more significant than that of the facial mask solution prepared from the pure glabridin of the control group.
TABLE 7
Figure BDA0003141656210000171
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. The mask liquid is characterized by comprising the following components in percentage by mass:
0 to 1.5 percent of thickening agent;
3-30% of polyol;
0.01-0.15% of chelating agent;
0.1 to 1.5 percent of preservative;
cherry blossom cell water glabridin liposome 0.1-10%;
the balance being water.
2. The mask liquid according to claim 1, characterized in that, by mass percentage,
0.001 to 0.6 percent of thickening agent;
5-25% of polyol;
0.01-0.1% of chelating agent;
0.2 to 1.0 percent of preservative;
cherry cell water glabridin liposome 0.5-5%.
3. The mask liquid according to claim 1, wherein the thickener is a cellulose-type thickener or an acrylic acid (ester) -based thickener to which a neutralizing agent is added;
one or more than two of polyhydric alcohol glycerol, propylene glycol, butanediol, isoprene glycol and hexanediol;
the neutralizing agent is selected from triethanolamine, arginine, sodium hydroxide or potassium hydroxide;
the chelating agent is EDTA disodium;
the preservative is one or more than two of phenoxyethanol, ethylhexyl glycerol, caprylyl glycol and colloidal silver.
4. The preparation method of the facial mask liquid is characterized by comprising the following steps:
step 1: mixing phospholipid, cholesterol, glabridin and cherry blossom cell water to form a suspension, and adjusting and shearing the suspension in a heating and heat preservation state to obtain a cherry blossom cell water glabridin liposome;
step 2: mixing thickener, polyalcohol, water, chelating agent, neutralizer, antiseptic and sakura cell glabridin liposome to obtain facial mask liquid.
5. The method according to claim 4, wherein the shearing rate in step 1 is 8000rpm or more and the time is 30min or more.
6. The method according to claim 4, wherein the temperature for the heat-holding in step 1 is not lower than the phase transition temperature of the phospholipid.
7. The method of claim 4, wherein prior to obtaining the liposome emulsion, further comprising: homogenizing under high pressure;
the high-pressure homogenization specifically comprises the following steps: each cycle was carried out at a pressure of 400bar, 600bar, 800bar, 1000bar for 2 or more times.
8. The method of claim 4, wherein step 1, prior to said mixing, further comprises: adding a surfactant.
9. The method of claim 4, wherein step 1, prior to said mixing, further comprises: the polyol is added.
10. The method according to claim 4, wherein in the step 1, the reaction mixture is subjected to a reaction in a mass percentage,
2-15% of phospholipid;
0.01-5% of glabridin;
0-5% of cholesterol;
the balance is cherry blossom cell water.
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