Oil control liposome and preparation method and application thereof

Abstract

The invention relates to an oil-control liposome as well as a preparation method and application thereof. The oil-control liposome comprises a liposome carrier and an oil-control composition loaded in the liposome carrier, the oil control composition comprises a yeast / zinc fermentation product, a lotus corniculatus seed extract, a lactobacillus fermentation lysate and VII type collagen. According to the skin oil control composition, four specific active components including the saccharomycetes / zinc fermentation product, the lotus corniculatus seed extract, the lactobacillus fermentation lysate and the VII type collagen are creatively combined, and the four specific active components are mutually matched and have a synergistic effect, so that an excellent skin oil control effect is comprehensively obtained in a multi-channel and multi-dimensional manner; in addition, potential mutual promotion and synergistic interaction effects are achieved on the oil control effect. Furthermore, the oil-control composition promotes permeation of effective components and acts on effective parts through a liposome wrapping technology, grease generation and secretion are controlled in a multi-channel mode, and the effective oil control effect is achieved.

Description

Technical Field

[0001] The invention belongs to the technical field of cosmetics, and relates to an oil-controlling liposome, a preparation method and application thereof, and in particular to an oil-controlling liposome, a preparation method thereof and application thereof in the preparation of cosmetics. Background Art

[0002] Skin oil can keep the skin soft and smooth and prevent excessive loss of moisture in the skin's stratum corneum. However, when the sebaceous glands are affected by endocrine factors, external stimuli and other factors, abnormal sebaceous gland secretion often occurs. Excessive oil leads to the formation of closed comedones, enlarged pores, decreased skin gloss, damaged skin barrier, increased inflammatory response and other skin problems.

[0003] With the development of society and the advancement of science and technology, people's demand for cosmetics is also increasing. Among them, oil-control and moisturizing products are favored by consumers because they can effectively regulate skin oil secretion and keep the skin fresh and comfortable.

[0004] Existing oil-control and moisturizing products mainly achieve their effects by adding chemically synthesized ingredients, such as dimethicone, zinc oxide, alcohol, etc. Although these ingredients can quickly absorb excess oil, long-term use may cause irritation to the skin and cannot fundamentally solve the problem of excessive oil secretion; such as salicylic acid, PCA-zinc, azelaic acid, etc., these ingredients mainly achieve oil control by absorbing excess sebum, unclogging pores or inhibiting lipid secretion, but most of these ingredients stay on the surface, the oil control effect is not obvious, and they will also cause great irritation to the skin. In addition, there are some products that maintain skin moisture by adding moisturizers, but these moisturizers are often ineffective and cannot meet the needs of consumers.

[0005] Therefore, it is very meaningful to develop an oil control product that can fundamentally solve the problem of excessive oil secretion and is gentle and safe to the skin. Summary of the invention

[0006] In view of the deficiencies in the prior art, the object of the present invention is to provide an oil-controlling liposome and a preparation method and application thereof, and in particular to provide an oil-controlling liposome and a preparation method thereof and application thereof in the preparation of cosmetics.

[0007] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0008] In a first aspect, the present invention provides an oil-controlling liposome, comprising a liposome carrier and an oil-controlling composition loaded in the liposome carrier; the oil-controlling composition comprises a yeast / zinc fermentation product, a Lotus japonicus seed extract, a lactobacillus fermentation lysate and type VII collagen.

[0009] The present invention creatively combines four specific active components, namely, yeast / zinc fermentation product, lotus seed extract, lactobacillus fermentation lysate and type VII collagen. The yeast / zinc fermentation product mainly inhibits 5α-reductase, thereby reducing the stimulation of sebaceous glands to secrete oil; the lotus seed extract can reduce the lipid synthesis and fusion of sebaceous gland cells, instantly reduce sebum secretion, and regulate the activity of sebaceous glands in a long-term manner; the lactic acid and sodium lactate rich in the lactobacillus fermentation lysate can effectively regulate the pH value of the skin and promote the formation of a good ecosystem by the flora on the skin; type VII collagen connects the basal layer with the underlying tissue by interacting with other types of collagen and part of the extracellular matrix. As an important skin nutrient, collagen peptide plays an important role in the skin care of oily skin.

[0010] The four specific active ingredients cooperate with each other and work synergistically to achieve excellent skin oil control effects in multiple ways and dimensions, and have the potential to promote each other and synergize the oil control effect. Furthermore, the above oil control composition is encapsulated by liposome technology to promote the penetration of active ingredients and act on effective parts, and control oil production and secretion in multiple ways to achieve effective oil control effects.

[0011] Preferably, the oil control composition comprises, by mass, 50-70 parts of yeast / zinc fermentation product, 5-20 parts of Lotus japonicus seed extract, 20-35 parts of lactobacillus fermentation lysate and 0.01-1 part of type VII collagen.

[0012] When the four active components in the oil-control composition are used together in the above-mentioned specific mass ratio, the synergistic promoting effect on the oil-control efficacy is more significant.

[0013] The mass fraction of the yeast / zinc fermentation product can be selected as 50 parts, 53 parts, 55 parts, 58 parts, 60 parts, 62 parts, 65 parts, 67 parts, 68 parts, 70 parts, etc.; the mass fraction of the Lotus japonicus seed extract can be selected as 5 parts, 8 parts, 10 parts, 12 parts, 14 parts, 16 parts, 18 parts, 20 parts, etc.; the mass fraction of the lactobacillus fermentation lysate can be selected as 20 parts, 22 parts, 25 parts, 26 parts, 28 parts, 30 parts, 32 parts, 35 parts, etc.; the mass fraction of the type VII collagen can be selected as 0.01 parts, 0.05 parts, 0.08 parts, 0.1 parts, 0.2 parts, 0.3 parts, 0.4 parts, 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, 1 parts, etc.; other specific point values ​​within the above numerical ranges can be selected, and they will not be repeated here one by one.

[0014] Preferably, the raw materials for preparing the liposome carrier include lecithin, hydrogenated lecithin, cholesterol, a surfactant and chitosan or its salt.

[0015] Preferably, the mass ratio of the lecithin, hydrogenated lecithin, cholesterol and surfactant is (2-6):(0.1-2):(0.1-1):(0.5-2).

[0016] The product involved in the present invention uses the raw materials with the above-mentioned specific mass ratio as the raw materials for preparing the liposome carrier, so that the system loaded with the above-mentioned oil control composition has strong stability and can maintain excellent oil control effect for a long time.

[0017] The specific point values ​​in (2-6) can be 2, 3, 4, 5, 6, etc.; the specific point values ​​in (0.1-2) can be 0.1, 0.2, 0.4, 0.6, 0.8, 1.0, 1.2, 1.4, 1.6, 1.8, 2.0, etc.; the specific point values ​​in (0.1-1) can be 0.1, 0.2, 0.3, 0.5, 0.7, 0.9, 1.0, etc.; the specific point values ​​in (0.5-2) can be 0.5, 0.6, 0.7, 0.9, 1.0, 1.2, 1.4, 1.6, 1.8, 2.0, etc. Other specific point values ​​within the above numerical ranges can be selected, and they will not be repeated here.

[0018] Preferably, the surfactant includes any one of Tween-80, caprylic / capric triglyceride, glyceryl oleate, glyceryl stearate, steareth-21 or steareth-2, or a combination of at least two thereof.

[0019] Preferably, the mass ratio of the sum of the mass of lecithin, hydrogenated lecithin, cholesterol, and surfactant in the raw materials for preparing the liposome carrier to the mass ratio of the oil control composition is 1:(0.1-0.6), for example, 1:0.1, 1:0.2, 1:0.3, 1:0.4, 1:0.5, 1:0.6, etc. Other specific point values ​​within this numerical range can be selected, and they will not be repeated here one by one.

[0020] In a second aspect, the present invention provides a method for preparing the oil-controlling liposome according to the first aspect, the preparation method comprising the following steps:

[0021] (1) dissolving lecithin, hydrogenated lecithin, cholesterol and a surfactant, raw materials for preparing the liposome carrier, in an organic solvent, and removing the organic solvent by rotary evaporation to form a lipid film;

[0022] (2) preparing an aqueous solution of the oil control composition;

[0023] (3) mixing the lipid film with an aqueous solution of the oil control composition for hydration treatment to cause the film to fall off, and then performing ultrasonic treatment;

[0024] (4) Mixing the ultrasonically treated solution with an aqueous solution of chitosan or a salt thereof, and homogenizing under high pressure to obtain the oil-controlling liposome.

[0025] There is no particular order in which steps (1) and (2) are performed.

[0026] The oil-controlling liposome product of the present invention is prepared by a thin film hydration method combined with ultrasonic treatment and modification of chitosan or its salt, so that the stability of the product system is very excellent, and thus the excellent oil-controlling effect can be maintained for a long time.

[0027] Preferably, the organic solvent includes any one of anhydrous ethanol, ether, chloroform, or methanol, or a combination of at least two thereof.

[0028] Preferably, the mass concentration of the aqueous solution of the oil control composition is 0.7-1.5%, for example 0.7%, 0.8%, 0.9%, 1.0%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, etc.

[0029] Preferably, the pH value of the aqueous solution of the oil control composition is 6.5-7.5, for example, pH=6.5, pH=6.7, pH=6.8, pH=6.9, pH=7.0, pH=7.2, pH=7.5, etc.

[0030] Preferably, the hydration treatment is carried out at 40-60°C (e.g., 40°C, 45°C, 48°C, 50°C, 55°C, 60°C, etc.) under vacuum conditions for 5-30 min (e.g., 5 min, 10 min, 12 min, 15 min, 18 min, 20 min, 25 min, 30 min, etc.).

[0031] Preferably, the ultrasonic treatment is carried out at 20-35°C (e.g., 20°C, 22°C, 25°C, 28°C, 30°C, 35°C, etc.) for 20-40 min (e.g., 20 min, 25 min, 28 min, 30 min, 32 min, 35 min, 38 min, 40 min, etc.).

[0032] Preferably, after the ultrasonic treatment, the solution is further stirred for 30-150 min, for example, 30 min, 50 min, 60 min, 80 min, 90 min, 100 min, 120 min, 130 min, 150 min, etc.

[0033] Other specific point values ​​within the aforementioned numerical ranges can be selected and will not be described in detail here.

[0034] Preferably, the chitosan or its salt includes carboxymethyl deacetylated chitosan, chitosan hydrochloride, chitosan quaternary ammonium salt and the like.

[0035] Preferably, the concentration of chitosan or its salt in the aqueous solution of chitosan or its salt is 0.1-0.5%, such as 0.1%, 0.2%, 0.3%, 0.4%, 0.5% and the like.

[0036] Preferably, the pH value of the aqueous solution of chitin or its salt is 6.5-7.5, for example, pH=6.5, pH=6.7, pH=6.8, pH=6.9, pH=7.0, pH=7.2, pH=7.5, etc.

[0037] Preferably, the mass ratio of the solution after ultrasonic treatment in step (3) to the aqueous solution of chitin or its salt is (2-8):1, for example 2:1, 3:1, 4:1, 5:1, 6:1, 7:1, 8:1, etc.

[0038] Preferably, the high-pressure homogenization is carried out at 400-700 bar (e.g., 400 bar, 450 bar, 500 bar, 530 bar, 550 bar, 580 bar, 600 bar, etc.) for 3-30 min (e.g., 3 min, 10 min, 15 min, 20 min, 25 min, 30 min, etc.).

[0039] In a third aspect, the present invention provides use of the oil-controlling liposome according to the first aspect in preparing cosmetics.

[0040] The oil-controlling liposome product of the present invention has high adaptability and can be used directly or as a raw material for preparing cosmetics with various dosage forms and various functions.

[0041] Preferably, the cosmetics include lotions, emulsions, essences, face creams, facial masks, make-up removers, sunscreen products, and make-up products.

[0042] Compared with the prior art, the present invention has the following beneficial effects:

[0043] The present invention creatively combines four specific active components, namely, yeast / zinc fermentation product, Lotus japonicus seed extract, lactobacillus fermentation lysate and type VII collagen. The four specific active components cooperate with each other and work synergistically to achieve excellent skin oil control effects in multiple channels and dimensions, and have the potential to promote each other and synergize the oil control effect. Furthermore, the above oil control composition is encapsulated by liposome technology to promote the penetration of active ingredients and act on effective parts, and control oil production and secretion in multiple channels to achieve an effective oil control effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0044] Figure 1 is a transmission electron microscope (TEM) morphological observation picture of the freshly prepared liposome sample of Example 1;

[0045] Figure 2 The morphological observations of the liposome sample of Example 1 after storage at 25° C. for 30 days were observed by transmission electron microscopy (TEM). DETAILED DESCRIPTION

[0046] In order to further explain the technical means and effects adopted by the present invention, the technical solution of the present invention is further described below in conjunction with the preferred embodiments of the present invention, but the present invention is not limited to the scope of the embodiments.

[0047] The weight percentages of the components involved in the following embodiments or comparative examples are all calculated based on the actual content of the effective ingredients contained in the commercially available raw materials. The commercially available raw materials may also selectively contain any one or a combination of at least two of solvents, fillers, diluents, stabilizers, pH regulators, antibacterial agents, antioxidants or impurities within the permitted range.

[0048] The sources of raw materials involved in the following examples or comparative examples are as follows:

[0049] The yeast / zinc fermentation product was purchased from Zefang (Guangzhou) Biological Co., Ltd.;

[0050] Lotus japonicus seed extract was obtained from Guangzhou Jiaye Biotechnology Co., Ltd.

[0051] Lactobacillus fermentation lysate was purchased from Zefang (Guangzhou) Biological Co., Ltd.;

[0052] Type VII collagen was purchased from Shanxi Jinbo Biopharmaceutical Co., Ltd.;

[0053] Phosphatidylcholine was purchased from Shanghai MacLean Biochemical Technology Co., Ltd.;

[0054] Hydrogenated lecithin was purchased from Guangzhou Chengzhi Trading Co., Ltd.

[0055] Carboxymethyl chitosan was purchased from Guangzhou Hean Chemical Co., Ltd.

[0056] Example 1

[0057] The present embodiment provides an oil-control liposome, whose components include a liposome carrier and an oil-control composition loaded in the liposome carrier, wherein the mass ratio of the liposome carrier to the oil-control composition is 1:0.3; wherein the oil-control composition is composed, by mass, of 60 parts of yeast / zinc fermentation product, 12 parts of Lotus japonicus seed extract, 28 parts of lactobacillus fermentation lysate, and 0.1 parts of type VII collagen; wherein the mass ratio of lecithin, hydrogenated lecithin, cholesterol, and Tween-80 in the raw materials for preparing the liposome carrier is 4:1:0.5:1, and carboxymethyl deacetylated chitosan is configured into an aqueous solution with a pH of 7 and a concentration of 0.2wt% for standby use.

[0058] The preparation method is as follows:

[0059] (1) dissolving lecithin, hydrogenated lecithin, cholesterol and Tween-80 in anhydrous ethanol, and removing the anhydrous ethanol by rotary evaporation using a rotary evaporator to form a lipid film;

[0060] (2) dissolving the raw materials of the oil control composition in water, adjusting the pH to 7, and preparing an aqueous solution with a concentration of 1.16 wt %;

[0061] (3) mixing the lipid film obtained in step (1) with the aqueous solution of the oil control composition obtained in step (2), performing a hydration treatment at 50° C. under vacuum conditions for 20 min to allow the film to fall off, and then performing an ultrasonic treatment at 30° C. for 30 min; and then continuing to stir in a magnetic stirrer for 2 h;

[0062] (4) The treated solution obtained in step (3) was mixed with an aqueous solution of carboxymethyl chitosan at a mass ratio of 5:1, and homogenized at 550 bar for 15 minutes to obtain the oil-controlling liposome.

[0063] Example 2

[0064] The present embodiment provides an oil-control liposome, whose components include a liposome carrier and an oil-control composition loaded in the liposome carrier, wherein the mass ratio of the liposome carrier to the oil-control composition is 1:0.2; wherein the oil-control composition is composed, by mass, of 50 parts of a yeast / zinc fermentation product, 20 parts of a Lotus japonicus seed extract, 20 parts of a lactobacillus fermentation lysate, and 0.5 parts of type VII collagen; wherein the mass ratio of lecithin, hydrogenated lecithin, cholesterol, and Tween-80 in the raw materials for preparing the liposome carrier is 3:2:0.4:1.5, and carboxymethyl deacetylated chitosan is prepared into an aqueous solution with a pH of 7.4 and a concentration of 0.4wt% for standby use.

[0065] The preparation method is as follows:

[0066] (1) dissolving lecithin, hydrogenated lecithin, cholesterol and Tween-80 in anhydrous ethanol, and removing the anhydrous ethanol by rotary evaporation using a rotary evaporator to form a lipid film;

[0067] (2) dissolving the raw materials of the oil control composition in water, adjusting the pH to 7.4, and preparing an aqueous solution with a concentration of 1.5 wt %;

[0068] (3) mixing the lipid film obtained in step (1) with the aqueous solution of the oil control composition obtained in step (2), performing a hydration treatment at 60° C. under vacuum conditions for 15 min to allow the film to fall off, and then performing an ultrasonic treatment at 35° C. for 20 min; and then continuing to stir in a magnetic stirrer for 1 h;

[0069] (4) The treated solution obtained in step (3) was mixed with an aqueous solution of carboxymethyl chitosan at a mass ratio of 3:1, and homogenized at 500 bar high pressure for 15 minutes to obtain the oil-controlling liposome.

[0070] Example 3

[0071] The present embodiment provides an oil-control liposome, whose components include a liposome carrier and an oil-control composition loaded in the liposome carrier, wherein the mass ratio of the liposome carrier to the oil-control composition is 1:0.4; wherein the oil-control composition is composed, by mass, of 70 parts of yeast / zinc fermentation product, 8 parts of Lotus japonicus seed extract, 35 parts of lactobacillus fermentation lysate, and 0.05 parts of type VII collagen; wherein the mass ratio of lecithin, hydrogenated lecithin, cholesterol, and Tween-80 in the raw materials for preparing the liposome carrier is 4:0.5:1:1.5, and carboxymethyl deacetylated chitosan is configured into an aqueous solution with a pH of 7.2 and a concentration of 0.1wt% for standby use.

[0072] The preparation method is as follows:

[0073] (1) dissolving lecithin, hydrogenated lecithin, cholesterol and Tween-80 in anhydrous ethanol, and removing the anhydrous ethanol by rotary evaporation using a rotary evaporator to form a lipid film;

[0074] (2) Dissolving the raw materials of the oil control composition in water and adjusting the pH to 6.8 to prepare an aqueous solution with a concentration of 1.22%;

[0075] (3) mixing the lipid film obtained in step (1) with the aqueous solution of the oil control composition obtained in step (2), performing a hydration treatment at 40° C. under vacuum conditions for 30 min to allow the film to fall off, and then performing an ultrasonic treatment at 25° C. for 40 min; and then continuing to stir in a magnetic stirrer for 2 h;

[0076] (4) The treated solution obtained in step (3) was mixed with an aqueous solution of carboxymethyl deacetylated chitosan at a mass ratio of 7:1, and homogenized at 600 bar high pressure for 15 minutes to obtain the oil-controlling liposome.

[0077] Example 4

[0078] This example provides an oil-controlling liposome, the components of which differ from those of Example 1 only in that the raw materials for preparing the liposome carrier are different: lecithin is missing, and its reduced amount is distributed to the mass of hydrogenated lecithin, while other components and contents remain unchanged. The preparation process thereof refers to Example 1.

[0079] Example 5

[0080] This example provides an oil-controlling liposome, the components of which differ from those of Example 1 only in that the raw materials used to prepare the liposome carrier are different: hydrogenated lecithin is missing, and its reduced amount is distributed to the mass of lecithin, while other components and contents remain unchanged. The preparation process thereof refers to Example 1.

[0081] Example 6

[0082] This embodiment provides an oil-controlling liposome, the components of which differ from those of the embodiment 1 only in the mass ratio of the raw materials for preparing the liposome carrier: the mass ratio of lecithin, hydrogenated lecithin, cholesterol, and Tween-80 in the raw materials for preparing the liposome carrier is 2:3:1.5:1, and the other components and contents remain unchanged. The preparation process thereof refers to the embodiment 1.

[0083] Example 7

[0084] This embodiment provides an oil-controlling liposome, the components of which are the same as those of Example 1. The difference between the preparation process and that of Example 1 is that no ultrasonic treatment is performed in step (3), and the mixture is directly stirred in a magnetic stirrer after the hydration treatment. Other conditions remain unchanged.

[0085] Example 8

[0086] This embodiment provides an oil-controlling liposome, the components of which are the same as those of embodiment 1. The difference between the preparation process and that of embodiment 1 is that no stirring treatment is performed after the ultrasonic treatment in step (3). Other conditions remain unchanged.

[0087] Example 9

[0088] This embodiment provides an oil-controlling liposome, the components of which differ from those of the embodiment 1 only in that the raw materials for preparing the liposome carrier do not contain carboxymethyl deacetylated chitosan, the preparation process does not carry out step (4), and the solution obtained after the treatment in step (3) is the final product.

[0089] Comparative Example 1

[0090] This comparative example provides an oil-controlling liposome, the components of which differ from those of Example 1 only in the formula of the oil-controlling composition: the yeast / zinc fermentation product is missing, and the reduced amount thereof is proportionally distributed to the mass of Lotus japonicus seed extract, lactobacillus fermentation lysate and type VII collagen, while the other components and contents remain unchanged. The preparation process thereof refers to Example 1.

[0091] Comparative Example 2

[0092] This comparative example provides an oil-controlling liposome, the components of which differ from those of Example 1 only in the formula of the oil-controlling composition: the extract of Lotus japonicus seeds is missing, and the reduced amount thereof is proportionally distributed to the mass of the yeast / zinc fermentation product, the lactobacillus fermentation lysate, and the type VII collagen, while the other components and contents remain unchanged. The preparation process thereof refers to Example 1.

[0093] Comparative Example 3

[0094] This comparative example provides an oil-controlling liposome, the components of which differ from those of Example 1 only in the formula of the oil-controlling composition: the lactobacillus fermentation lysate is missing, and the reduced amount thereof is proportionally distributed to the mass of the yeast / zinc fermentation product, the Lotus japonicus seed extract, and the type VII collagen, while the other components and contents remain unchanged. The preparation process thereof refers to Example 1.

[0095] Comparative Example 4

[0096] This comparative example provides an oil-controlling liposome, the components of which differ from those of Example 1 only in the formula of the oil-controlling composition: type VII collagen is missing, and its reduced amount is proportionally distributed to the mass of the yeast / zinc fermentation product, the Lotus japonicus seed extract, and the lactobacillus fermentation lysate, while the other components and contents remain unchanged. The preparation process thereof refers to Example 1.

[0097] Comparative Example 5

[0098] This comparative example provides an oil control composition, which is composed of 60 parts of yeast / zinc fermentation product, 12 parts of Lotus japonicus seed extract, 28 parts of lactobacillus fermentation lysate and 0.1 parts of type VII collagen by weight. The components are mixed to form an oil control composition aqueous solution with a concentration of 1.16wt%.

[0099] Comparative Example 6

[0100] This comparative example provides a blank liposome, which is different from Example 1 in that all the oil control compositions are replaced with an equal amount of deionized water.

[0101] Test Example 1

[0102] Evaluation of the appearance stability of oil-controlling liposomes:

[0103] The freshly prepared liposome samples of Examples 1-9 and Comparative Examples 1-4 were observed from the appearance and morphology. The samples had no precipitation, no flocculation and stratification, were evenly dispersed and had good fluidity, and obvious opalescence was observed under light. Then, each group of liposomes was stored for 28 days under the conditions of 25°C, sunlight, cold (-20°C), heat (48°C), cold and heat (-20°C / 7 days, 48°C / 7 days cycle), and then each group of liposomes was observed. The results are shown in Table 1.

[0104] Table 1

[0105] Group 25℃ illumination -20℃ 48℃ Hot and cold cycle Example 1 No change No change No change No change No change Example 2 No change No change No change No change No change Example 3 No change No change No change No change No change Example 4 No change Lighter color No change No change No change Example 5 No change Lighter color No change Darkening Darkening Example 6 No change Lighter color No change Darkening Slightly darker color Example 7 No change No change No change Slightly darker color No change Example 8 No change No change No change Slightly darker color No change Example 9 No change Lighter color No change Slightly darker color Slightly darker color Comparative Example 1 No change Slightly lighter color No change No change No change Comparative Example 2 No change Slightly lighter color No change No change No change Comparative Example 3 No change No change No change Slightly darker color No change Comparative Example 4 No change No change No change No change No change

[0106] From the results in Table 1, it can be seen that the oil-controlling liposome products of the present invention exhibit excellent stability under light, heat, cold and other conditions, especially the products of Examples 1-3 have better stability, and the raw material formula and preparation process conditions of the liposome carrier affect the stability of the product.

[0107] Test Example 2

[0108] Evaluation of the encapsulation efficiency and stability of oil-controlling liposomes:

[0109] The ultrafiltration centrifugation method is used to detect the encapsulation rate of oil-controlling liposomes. The oil-controlling liposomes are placed in an ultrafiltration tube equipped with an ultrafiltration membrane and centrifuged at 8000r / min for 30 minutes. The free drug can pass through the ultrafiltration membrane under the action of centrifugal force, while the liposomes are retained, thereby achieving the separation of the two. This method is mostly used to determine the encapsulation rate of water-soluble drug liposomes. This test example uses protein concentration to calculate the encapsulation rate and uses biuret to detect the concentration of free protein. The details are as follows:

[0110] (1) Preparation of Biuret Reagent: Weigh 1.50 g of copper sulfate (CuSO 4 ·5H 2 O) and 6.0 g potassium sodium tartrate (KNaC 4 H 4 O 6 ·4H 2 O), dissolve in 500 ml of water, add 300 ml of 10% NaOH solution under stirring, dilute with water to 1 liter, and store in a plastic bottle.

[0111] (2) Determination of standard curve: Divide 12 test tubes into two groups, add 0, 0.2, 0.4, 0.6, 0.8, 1.0 mL of 10 mg / mL crystallized bovine serum albumin (BSA) standard solution, add water to 1 mL, and then add 4 mL of biuret reagent. After shaking thoroughly, place at 25°C for 30 minutes, and measure the absorbance at 540 nm. Use the first test tube without the standard solution as the blank control solution. Take the average value of the two groups of measurements, and draw a standard curve with the protein content as the horizontal axis and the absorbance value as the vertical axis.

[0112] (3) Sample determination: The protein concentration of the samples of Examples 1-9 and Comparative Examples 1-3 after being placed at 25° C. for 0 days, 7 days, 14 days, and 28 days was determined by the same method as above, and the encapsulation efficiency (%) was calculated based on the standard curve. The results are shown in Table 2.

[0113] Table 2

[0114]

[0115]

[0116] From the results in Table 2, it can be seen that the oil-controlling liposome product of the present invention has little change in the protein encapsulation rate after being placed at room temperature for 28 days, especially the encapsulation rate of the products of Examples 1-3 has basically no change, the product shows excellent stability, and the raw material formula and preparation process conditions of the liposome carrier affect the stability of the product.

[0117] Test Example 3

[0118] Human skin patch test:

[0119] Using the closed patch test method, 0.025 mL of the samples obtained in Examples 1-9 and Comparative Examples 1-6 were taken and placed in a patch tester (and the group with an equal volume of water added but no sample added was used as a blank control group), and applied to the selected position on the back of the subjects (a total of 30 people, 3 males, 27 females, aged 19-55 years old, meeting the subject selection criteria) with a low-sensitivity tape. After pasting, press lightly with fingers to make it evenly attached to the skin for 24 hours. The subjects kept the patch site dry within 24 hours, avoiding intense exercise, scratching the patch site, long-term sunlight exposure, etc. After 24 hours, the tester was removed and marked. After 30 minutes, the indentation disappeared and the skin reaction was observed under sufficient light according to the standards in Table 3.

[0120] Table 3

[0121]

[0122]

[0123] The results showed that in the human skin closed patch test, all subjects had negative reactions for the samples obtained from Examples 1-9 and Comparative Examples 1-6, i.e., there was no adverse skin reaction among 30 subjects, indicating that the products involved in the present invention have no adverse reactions to the human body and are highly safe.

[0124] Test Example 4

[0125] Human body oil control efficacy test:

[0126] (1) Preparation before the test: 75 suitable subjects (22 males and 53 females, aged 19-45 years) were screened. The test site was the sides of the nose. The test area was cleaned with an alkaline facial cleanser the night before the test and the test area could not be exposed to water until the next day. Before the formal test, the subjects used an alkaline facial cleanser to clean their faces and started the test 30 minutes after cleaning. During the test, the subjects could not drink water or beverages, their noses were exposed, they were in the test state and remained relaxed, could not move around at will, reduced emotional fluctuations, avoided scratching the test site, and avoided contact with drugs, similar cosmetics, and alcohol lamps that could affect the results. The subjects obeyed the staff's arrangements.

[0127] (2) Determination:

[0128] The above 75 subjects were divided into 15 groups, each with 5 subjects. The efficacy evaluators used latex cots to measure the samples obtained in Examples 1-9 and Comparative Examples 1-6 (the samples in each group were diluted with deionized water to a dosing concentration of 5%) at (2.0±0.1) mg / cm 2 Apply the dosage evenly on the specified area of ​​the subject's nose, use a syringe for quantitative sampling, and the application method is shown in Table 4.

[0129] After using the sample for 2 hours and 6 hours, the efficacy evaluator used oil-absorbing paper to wipe the oil on both sides of the nose of the subject, paying attention to keeping the left and right areas wiped and the wiping force consistent, and recorded the weight of the oil wiped off the oil-absorbing paper (excluding the mass of the oil-absorbing paper) by analytical balance, and analyzed the results. Among them, the reduction rate of nose oil mass at the nth hour = [Tn (uncoated sample) - Tn (coated sample)] / Tn (uncoated sample) × 100%. The results are shown in Table 5.

[0130] Table 4

[0131] Serial number Group Nose application position Record the quality of grease wiped by oil-absorbing paper at the nth hour 1 Uncoated samples Left nose Tn(uncoated sample) 2 Coating samples Right nose Tn(coating sample)

[0132] Table 5

[0133]

[0134]

[0135] As can be seen from the data results in Table 5, the oil-control liposome product involved in the present invention can significantly inhibit the oil secretion of the nose wing of the human body, that is, it has an excellent oil-control effect. By comparing the results of Example 1 and Comparative Examples 1-4, it can be seen that the four components of yeast / zinc fermentation product, Lotus japonicus seed extract, lactobacillus fermentation lysate and type VII collagen synergize in the oil-control effect. By comparing the results of Example 1 and Comparative Example 5, it can be seen that by loading the oil-control composition on the liposome, its oil-control effect is improved. By comparing the results of Example 1 and Examples 4-9, it can be seen that the preparation raw materials of the liposome carrier and the preparation process of the product also affect its oil-control effect to a certain extent.

[0136] Test Example 5

[0137] Evaluation of particle size stability of oil-controlling liposomes:

[0138] The freshly prepared liposome sample of Example 1 was stored at 25°C for 30 days and then freeze-dried to obtain freeze-dried powder, which was dissolved in deionized water to form a 0.2% aqueous solution and ultrasonically treated for 20 minutes before testing. The fresh sample and the sample stored for 30 days were placed in the sample cell of a DLS instrument (dynamic light scattering analyzer) for particle size (nm) detection, and the results are shown in Table 6.

[0139] Table 6

[0140] sample Particle size on day 0 / nm Particle size on day 30 / nm Example 1 137.9 127.3

[0141] From the results in Table 6, it can be seen that the particle size of the oil-controlling liposome product of the present invention changes little after being placed at 25° C. for 30 days, showing excellent stability.

[0142] The transmission electron microscopy (TEM) morphology of the fresh sample and the sample after 30 days of storage are shown in Figure 2. Figure 1 and Figure 2 As shown, the oil-controlling liposome product of the present invention is spherical under a transmission electron microscope, and is evenly distributed with clear boundaries and a particle size of about 130 nm, which is consistent with the DLS particle size detection result. According to the results of transmission electron microscopy, the oil-controlling liposomes have no obvious changes in morphology after 30 days of storage, showing a stability characteristic that is superior to that of conventional liposomes.

[0143] Test Example 6

[0144] Evaluation of the oil-control effect of oil-control liposomes on sebaceous gland cells:

[0145] The evaluation was conducted based on immortalized human sebaceous gland cells SZ95. An in vitro oil secretion model was established by stimulating hormone substances. After drug administration, the oil control effect of the sample on sebaceous gland cells was evaluated by evaluating the trend of lipid droplet synthesis. Specific detection method:

[0146] (1) Cell inoculation: Dilute the cells to the inoculation density with cell culture medium and inoculate them into a 96-well plate with 200 μL added to each well. 2 Culture in an incubator for 24 h ± 2 h.

[0147] (2) Dosing treatment: After the cells in the 96-well plate reach an appropriate degree of confluence, the dosing operation is performed according to the experimental groups in Table 7. The culture medium in the 96-well plate is discarded, and the culture medium containing the test substance is added to the test wells; normal cell culture medium is added to the blank control wells, with the amount of liquid added to each well being 200 μL. After the dosing is completed, the 96-well plate is placed in a CO 2 Culture in an incubator for 24 h ± 2 h.

[0148] Table 7

[0149]

[0150] (3) Staining: Discard the old solution in the 96-well plate, wash the plate twice with phosphate buffer solution, add 100 μL of fixative to each well to fix the cells; discard the fixative, add oil red solution to stain at 37°C for 30 min; then discard the oil red solution, add an appropriate amount of ultrapure water to wash for 5 min; repeat 3 times.

[0151] (4) Photographing and observation: Take photos under a microscope and record the staining results, and use image analysis software to calculate the staining area percentage "% Area". The results are shown in Table 8.

[0152] Table 8

[0153] Group %Area Example 1 15.2 Model control group 24.4 Blank control group 5.8

[0154] From the data results in Table 8, it can be seen that the amount of lipid droplet synthesis in the oil control composition liposomes of the present invention at a concentration of 0.125 mg / mL is significantly reduced compared with the model control group, that is, the oil control composition of the present invention has an excellent ability to inhibit lipid droplet synthesis.

[0155] The applicant declares that the present invention illustrates the technical solution of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned embodiments, that is, it does not mean that the present invention must rely on the above-mentioned embodiments to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of various raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0156] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.

[0157] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

Claims

1. An oil-controlling liposome, characterized in that: The oil-controlling liposome comprises a liposome carrier and an oil-controlling composition loaded in the liposome carrier; the oil-controlling composition comprises a yeast / zinc fermentation product, a Lotus japonicus seed extract, a lactobacillus fermentation lysate and type VII collagen.

2. The oil-controlling liposome according to claim 1, characterized in that: The oil control composition comprises, by weight, 50-70 parts of yeast / zinc fermentation product, 5-20 parts of Lotus japonicus seed extract, 20-35 parts of lactobacillus fermentation lysate and 0.01-1 part of type VII collagen.

3. The oil-controlling liposome according to claim 1 or 2, characterized in that: The raw materials for preparing the liposome carrier include lecithin, hydrogenated lecithin, cholesterol, a surfactant and chitosan or its salt; Preferably, the mass ratio of the lecithin, hydrogenated lecithin, cholesterol and surfactant is (2-6):(0.1-2):(0.1-1):(0.5-2); Preferably, the surfactant includes any one of Tween-80, caprylic / capric triglyceride, glyceryl oleate, glyceryl stearate, steareth-21 or steareth-2, or a combination of at least two thereof.

4. The oil-controlling liposome according to any one of claims 1 to 3, characterized in that: The mass ratio of the sum of the masses of lecithin, hydrogenated lecithin, cholesterol and surfactant in the raw materials for preparing the liposome carrier to the mass ratio of the oil control composition is 1:(0.1-0.6).

5. The method for preparing the oil-controlling liposome according to any one of claims 1 to 4, characterized in that: The preparation method comprises the following steps: (1) dissolving lecithin, hydrogenated lecithin, cholesterol and a surfactant, raw materials for preparing the liposome carrier, in an organic solvent, and removing the organic solvent by rotary evaporation to form a lipid film; (2) preparing an aqueous solution of the oil control composition; (3) mixing the lipid film with an aqueous solution of the oil control composition for hydration treatment to cause the film to fall off, and then performing ultrasonic treatment; (4) Mixing the ultrasonically treated solution with an aqueous solution of chitin or its salt, and homogenizing under high pressure to obtain the oil-controlling liposome.

6. The method for preparing the oil-controlling liposome according to claim 5, characterized in that: The organic solvent includes any one of anhydrous ethanol, ether, chloroform, or methanol, or a combination of at least two thereof; Preferably, the mass concentration of the aqueous solution of the oil control composition is 0.7-1.5%; Preferably, the pH value of the aqueous solution of the oil control composition is 6.5-7.

5.

7. The method for preparing the oil-controlling liposome according to claim 5 or 6, characterized in that: The hydration treatment is carried out at 40-60° C. under vacuum conditions for 5-30 min; Preferably, the ultrasonic treatment is performed at 20-35° C. for 20-40 min; Preferably, the solution is further stirred for 30-150 min after the ultrasonic treatment.

8. The method for preparing the oil-controlling liposome according to any one of claims 5 to 7, characterized in that: The concentration of chitin or its salt in the aqueous solution of chitin or its salt is 0.1-0.5%; Preferably, the pH value of the aqueous solution of chitin or its salt is 6.5-7.

5.

9. The method for preparing the oil-controlling liposome according to any one of claims 5 to 8, characterized in that: The mass ratio of the solution after ultrasonic treatment in step (3) to the aqueous solution of chitosan or its salt is (2-8):1; Preferably, the high-pressure homogenization is performed at 400-700 bar for 3-30 min.

10. Use of the oil-controlling liposome according to any one of claims 1 to 4 in the preparation of cosmetics; Preferably, the cosmetics include lotions, emulsions, essences, face creams, facial masks, make-up removers, sunscreen products, and make-up products.

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