Preparation method of fermented mud microspheres with multi-dimensional and efficient skin cleansing activity, and its products and applications

Abstract

The present invention provides a preparation method of fermented mud microspheres with multi-dimensional and efficient skin cleansing activity, as well as products and applications thereof. The fermented mud prepared by the method of the present invention is ground and fermented, thereby improving the particle uniformity and fineness of the mineral mud, improving the skin feel, and greatly increasing the specific surface area. The natural active ingredients and biosurfactants produced by fermentation at different stages can be integrated, and more acidic components can be produced through two fermentation treatments, which can better soften the stratum corneum and provide favorable conditions for removing blackheads. At the same time, the acidic components can dissolve impurities in the mineral mud, further increasing the specific surface area of ​​the product. Through the coordinated cooperation of the above steps, the fermented mud microspheres finally prepared have the effects of efficient oil control, deep cleaning, and blackhead removal.

Description

Technical Field

[0001] The invention belongs to the technical field of daily cosmetics, and specifically relates to a preparation method of fermented mud microspheres with multi-dimensional and efficient skin-cleansing activity, and a product and application thereof. Background Art

[0002] Mineral mud is often added to modern skin care products, mainly playing multiple roles such as gelling agent, anti-sticking powder, lubricant, colorant, antibacterial agent, etc. Commonly used mineral mud has a porous or layered structure. The early application of mineral mud in skin care products focused on physical properties such as increasing viscosity, preventing precipitation, and improving product gloss. With the diversified development of skin care products, higher requirements are put forward for mineral mud, that is, by adding mineral mud, skin care products can have the effects of efficient oil control, deep cleansing, etc.

[0003] CN113476370A discloses a skin care composition, which relates to the field of cosmetic technology. The skin care composition of the present invention comprises mineral mud, bamboo charcoal powder, silicon powder and plant extract; the plant extract comprises at least two of chamomile extract, fig extract and lotus extract. The three ingredients of mineral mud, bamboo charcoal powder and silicon powder all have good grease absorption effects, and after compounding, they can synergistically enhance the oil control effect of the product and play a role in regulating skin feel; the addition of plant extracts can further improve the oil control effect and storage stability of the skin care composition.

[0004] CN109998972A discloses a foam-rich cleansing mud, which includes the following components by weight percentage: 15-40% mineral mud; 1-15% alcohol moisturizer; 4-10% zwitterionic surfactant; 3-10% amino acid surfactant; 0.001-1% chelating agent; water is added to 100%; wherein the weight ratio of zwitterionic surfactant to amino acid surfactant is 2:1-1:3. The cleansing mud product of the invention uses a non-soap-based formula and can have good bubble performance and cleansing performance in the case of containing a large amount of mineral mud, which expands the application of mineral mud in cleansing products.

[0005] Although mineral mud has been frequently used as a physical cleansing and oil-control material in the prior art, it is far from meeting the needs of modern consumers with a variety of oily skin types, let alone the need for deep cleansing of oily skin and the removal of blackheads caused by staying up late or excessive exposure to computer and mobile phone screens. Therefore, how to solve the above problems through green and safe technology is a major difficulty in the manufacture of skin care raw materials. Summary of the invention

[0006] In view of the shortcomings of the prior art, the purpose of the present invention is to provide a preparation method of fermented mud microspheres with multi-dimensional and efficient skin cleansing activity, as well as its products and applications. The preparation method provided by the present invention prepares fermented mud containing rich natural active ingredients by simulating the way of microbial degradation of plants in nature, so as to solve the problem that mineral mud is not fully effective in skin care products.

[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 a method for preparing fermented mud microspheres having multi-dimensional and efficient skin cleansing activity, characterized in that the preparation method comprises:

[0009] (1) Grinding the mineral mud and then mixing it with the culture medium and pure water to obtain a mixed material;

[0010] (2) sterilizing the mixed material and then inoculating Bifidobacterium for primary fermentation;

[0011] (3) After the first fermentation is completed, vegetable oil is added to the fermentation liquid, and then yeast is added for secondary fermentation;

[0012] (4) After the secondary fermentation, lysozyme is added to perform lysozyme treatment, and then the fermented mud powder is dried to obtain fermented mud powder, and the fermented mud powder is granulated to obtain fermented mud microspheres.

[0013] The fermented mud prepared by the process of the present invention is ground and fermented, which improves the particle uniformity and fineness of the mineral mud, improves the skin feel, and greatly increases the specific surface area. The natural active ingredients and biosurfactants produced by fermentation at different stages can be integrated, and more acidic components can be produced through two fermentation treatments, which can better soften the stratum corneum and provide favorable conditions for removing blackheads. At the same time, the acidic components can dissolve impurities in the mineral mud and further increase the specific surface area of ​​the product. Through the coordinated cooperation of the above steps, the fermented mud microspheres finally prepared have the effects of efficient oil control, deep cleaning, and blackhead removal.

[0014] Preferably, the mineral mud in step (1) comprises kaolin and / or Amazonian white mud.

[0015] Preferably, the grinding in step (1) is performed to a particle size of ≤50 μm, for example, 5 μm, 10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 35 μm, 40 μm or 45 μm.

[0016] In the present invention, the mineral mud is ground to a particle size of less than 50 microns, which can effectively increase the specific surface area of ​​the mineral mud and enhance the adsorption capacity of impurities such as oil, dirt, blackheads, etc. on the skin surface and inside the pores.

[0017] Preferably, the culture medium comprises Antarctica spathula powder, Norway spruce leaf powder, Icelandic lichen powder and water.

[0018] Preferably, the particle sizes of the Antarctic thorn algae powder, the Norway spruce leaf powder and the Icelandic lichen powder are all 5000-10000 mesh, for example, 6000 mesh, 7000 mesh, 8000 mesh or 9000 mesh.

[0019] The culture medium of the present invention is a plant culture medium. Through the combination of Antarctic stalk algae powder, Norway spruce leaf powder and Icelandic lichen powder, a large amount of natural active ingredients such as total glycosides, polysaccharides and flavonoids can be released during the fermentation process. It has a good effect of inhibiting 5α-reductase and plays a role in treating both the symptoms and the root causes of endogenous oil control.

[0020] Preferably, the culture medium further comprises any one or a combination of at least two of a carbon source, a nitrogen source or an inorganic salt.

[0021] Preferably, the nitrogen source includes yeast extract; the carbon source includes glucose; and the inorganic salt includes any one or a combination of at least two of potassium dihydrogen phosphate, magnesium sulfate or sodium chloride.

[0022] Preferably, the culture medium comprises, by mass, 1-3 parts of Antarctic stalk algae powder (for example, 1.2 parts, 1.5 parts, 1.8 parts, 2 parts, 2.2 parts, 2.5 parts or 2.8 parts, etc.), 1-3 parts of Norway spruce leaf powder (for example, 1.2 parts, 1.5 parts, 1.8 parts, 2 parts, 2.2 parts, 2.5 parts or 2.8 parts, etc.), 1-3 parts of Iceland lichen powder (for example, 1.2 parts, 1.5 parts, 1.8 parts, 2 parts, 2.2 parts, 2.5 parts or 2.8 parts, etc.), and 0.5-1 parts of a carbon source (for example, 0.5 parts). , 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts or 1 parts, etc.), nitrogen source 0.5-1 parts (for example, it can be 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts or 1 parts, etc.), inorganic salt 0.01-0.2 parts (for example, it can be 0.03 parts, 0.05 parts, 0.07 parts, 0.1 parts, 0.13 parts, 0.15 parts, 0.17 parts or 0.19 parts, etc.) and water 85-99 parts (for example, it can be 86 parts, 87 parts, 88 parts, 89 parts, 90 parts, 91 parts, 93 parts, 95 parts, 97 parts or 98 parts, etc.).

[0023] Preferably, measured by mass percentage, the mixed material in step (1) comprises 10-15% of mineral mud (for example, 10.5%, 11%, 12%, 12.5%, 13%, 13.5%, 14% or 14.5%, etc.), 3-5% of culture medium (for example, 3.2%, 3.5%, 3.8%, 4%, 4.2%, 4.5% or 4.8%, etc.) and 80%-90% of water (for example, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88% or 89%, etc.).

[0024] Preferably, the sterilization temperature in step (2) is 115-125°C (for example, 116°C, 118°C, 120°C, 122°C or 124°C, etc.), and the sterilization time is 15-20 min (for example, 16 min, 17 min, 18 min or 19 min, etc.).

[0025] Preferably, the bifidobacterium comprises Bifidobacterium adolescentis and / or Bifidobacterium breve.

[0026] The fermentation bacteria used in the primary fermentation of the present invention are selected from bifidobacteria, which can enable the plant culture medium to release a large amount of natural active ingredients such as total glycosides, polysaccharides, flavonoids, etc. during the fermentation process, thereby making the final product have a good 5α-reductase inhibition effect.

[0027] Preferably, the inoculation amount of the bifidobacterium in step (2) is 1-10% (v / v), for example, it can be 2% (v / v), 3% (v / v), 4% (v / v), 5% (v / v), 6% (v / v), 7% (v / v), 8% (v / v) or 9% (v / v), etc.

[0028] Preferably, the temperature of the primary fermentation in step (2) is 30-40°C (for example, 31°C, 33°C, 35°C, 37°C or 39°C, etc.), the pH is 6.5-7.5 (for example, 6.6, 6.8, 7, 7.2 or 7.4, etc.), and the time is 15-20h (for example, 16h, 17h, 18h or 19h, etc.).

[0029] Preferably, the vegetable oil in step (3) includes oleifera seed oil.

[0030] Preferably, the amount of vegetable oil added in step (3) is 1-5% of the total mass of the fermentation liquid, for example, it can be 1.5%, 2%, 2.5%, 3%, 3.5%, 4% or 4.5%.

[0031] The present invention creatively combines the fermentation of kuasa oleifera seed oil with mineral mud. The oil is fermented by yeast to be converted into sophora bioside. Sophora bioside has the characteristics of low toxicity, biodegradability, environmental friendliness, good thermal stability, wide acid-base tolerance range, high salt tolerance, etc.; secondly, sophora bioside is a biosurfactant with good fat-dissolving and degreasing functions. After the stratum corneum of the skin is softened, sophora bioside will penetrate into the pores to dissolve the oil and blackheads, and then be adsorbed and taken away by kaolin or Amazonian white mud, so that the final product can achieve the effects of internal and external oil control, cleaning, and blackhead removal.

[0032] Preferably, the inoculation amount of the yeast in step (3) is 1-5% (v / v), for example, it can be 1.5% (v / v), 2% (v / v), 2.5% (v / v), 3% (v / v), 3.5% (v / v), 4% (v / v) or 4.5% (v / v), etc.

[0033] Preferably, the temperature of the secondary fermentation in step (3) is 25-30°C (for example, it can be 26°C, 27°C, 28°C, 29°C or 30°C, etc.), the pH is 4.0-6.5 (for example, it can be 4.1, 4.3, 4.5, 4.7, 5, 5.2, 5.5, 5.8, 6, 6.2 or 6.4, etc.), and the time is 20-30h (for example, it can be 21h, 23h, 25h, 27h or 29h, etc.).

[0034] Preferably, the amount of lysozyme added in step (4) is 0.1-1% of the total mass of the fermentation broth after the secondary fermentation, for example, it can be 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8% or 0.9%, etc.

[0035] Preferably, the drying method in step (4) is fluidized bed spray drying.

[0036] Preferably, the inlet temperature of the spray drying is 180-200°C (for example, it may be 182°C, 185°C, 188°C, 190°C, 192°C, 195°C or 198°C, etc.), the outlet temperature is 75-85°C (for example, it may be 76°C, 78°C, 80°C, 82°C or 84°C, etc.), and the pressure is 0.2-0.5 MPa (for example, it may be 0.25 MPa, 0.3 MPa, 0.35 MPa, 0.4 MPa or 0.45 MPa, etc.).

[0037] Any specific point value within the above numerical range can be selected, and will not be described in detail here.

[0038] In a second aspect, the present invention provides a fermented mud microsphere, which is prepared by the method described in the first aspect.

[0039] In a third aspect, the present invention provides a use of the fermented mud microspheres as described in the second aspect in the preparation of cosmetics.

[0040] Compared with the prior art, the present invention has the following beneficial effects:

[0041] The fermented mud prepared by the method of the present invention is ground and fermented, which improves the particle uniformity and fineness of the mineral mud, improves the skin feel, and greatly increases the specific surface area. It can integrate the natural active ingredients and biosurfactants produced by fermentation at different stages, and through two fermentation treatments, it can produce more acidic components, which can better soften the stratum corneum and provide favorable conditions for removing blackheads. At the same time, the acidic components can dissolve impurities in the mineral mud and further increase the specific surface area of ​​the product. Through the coordinated cooperation of the above steps, the fermented mud microspheres finally obtained have the effects of efficient oil control, deep cleaning, and blackhead removal. DETAILED DESCRIPTION

[0042] 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.

[0043] Some material information involved in the following examples and comparative examples is shown in Table 1:

[0044] Table 1

[0045]

[0046] The preparation methods of Antarctic stalk algae powder, Norway spruce leaf powder and Iceland lichen powder are all to grind the raw materials directly into 5000-10000 meshes by ultrafine grinding machine;

[0047] The rest of the raw materials can be used as long as they are purchased from regular dealers.

[0048] Example 1

[0049] This embodiment provides a method for preparing fermented mud microspheres with multi-dimensional and efficient skin cleansing activity, the steps of the method are:

[0050] (1) Grind dried Amazon white mud (water content below 5%) to a particle size of 35±5 μm, then mix with culture medium and pure water (Amazon white mud accounts for 12%, culture medium accounts for 4%, and the balance is pure water) and put into a fermentation tank, wherein the culture medium comprises 2 parts of Antarctic stalk algae powder, 2 parts of Norway spruce leaf powder, 2 parts of Iceland lichen powder, 0.5 parts of yeast extract powder, 0.5 parts of glucose, 0.02 parts of potassium dihydrogen phosphate, 0.02 parts of magnesium sulfate, 0.02 parts of sodium chloride and 94 parts of water;

[0051] (2) The material in the fermentation tank was sterilized at 120°C for 18 min, and then the Bifidobacterium adolescentis bacterial solution was inoculated at a 5% (v / v) inoculation rate, and fermented at 35°C and pH 7 for 18 h;

[0052] (3) After the first fermentation, add olea europaea seed oil (3% of the total fermentation liquid) to the fermentation liquid, then inoculate the yeast liquid at a rate of 3% (v / v), and carry out the second fermentation at 28°C and pH 5.5 for 25 h;

[0053] (4) After the secondary fermentation, add lysozyme (the amount added is 0.5% of the total amount of the fermentation liquid) for lysozyme treatment;

[0054] (5) The lysed material is subjected to fluidized bed spray drying to obtain fermented mud powder. The inlet temperature of the fluidized bed is set to 190° C., the outlet temperature is set to 80° C., and the pressure is set to 0.3 MPa. The fermented mud powder is granulated to obtain fermented mud microspheres.

[0055] Example 2

[0056] This embodiment provides a method for preparing fermented mud microspheres with multi-dimensional and efficient skin cleansing activity, the steps of the method are:

[0057] (1) Grind dry kaolin (water content less than 5%) to a particle size of 30±5 μm, then mix with culture medium and pure water (10% kaolin, 5% culture medium, and the balance pure water) and put into a fermentation tank, wherein the culture medium comprises 3 parts of Antarctic stalk algae powder, 1.5 parts of Norway spruce leaf powder, 2.5 parts of Iceland lichen powder, 0.5 parts of yeast extract powder, 0.5 parts of glucose, 0.02 parts of potassium dihydrogen phosphate, 0.02 parts of magnesium sulfate, 0.02 parts of sodium chloride and 93 parts of water;

[0058] (2) The material in the fermentation tank was sterilized at 115°C for 20 min, and then the Bifidobacterium breve bacterial solution was inoculated at an inoculum rate of 8% (v / v), and a primary fermentation was carried out at 40°C and pH 6.5 for 15 h;

[0059] (3) After the first fermentation, add olea europaea seed oil (2% of the total fermentation liquid) to the fermentation liquid, then inoculate the yeast liquid at a rate of 5% (v / v), and carry out the second fermentation at 30°C and pH 4.5 for 30 h;

[0060] (4) After the secondary fermentation, lysozyme (the amount added is 0.4% of the total amount of the fermentation liquid) is added for lysozyme treatment;

[0061] (5) The lysed material is subjected to fluidized bed spray drying to obtain fermented mud powder. The inlet temperature of the fluidized bed is set to 200° C., the outlet temperature is set to 75° C., and the pressure is set to 0.4 MPa. The fermented mud powder is granulated to obtain fermented mud microspheres.

[0062] Example 3

[0063] This embodiment provides a method for preparing fermented mud microspheres with multi-dimensional and efficient skin cleansing activity, the steps of the method are:

[0064] (1) Grind dried Amazon white mud (water content below 5%) to a particle size of 45±5 μm, then mix with culture medium and pure water (Amazon white mud accounts for 15%, culture medium accounts for 3%, and the balance is pure water) and put into a fermentation tank, wherein the culture medium comprises 1.5 parts of Antarctic stalk algae powder, 3 parts of Norway spruce leaf powder, 1.5 parts of Iceland lichen powder, 0.5 parts of yeast extract powder, 0.5 parts of glucose, 0.02 parts of potassium dihydrogen phosphate, 0.02 parts of magnesium sulfate, 0.02 parts of sodium chloride and 94 parts of water;

[0065] (2) The material in the fermentation tank was sterilized at 125°C for 15 min, and then the Bifidobacterium breve bacterial solution was inoculated at a 10% (v / v) inoculation rate, and a fermentation was carried out at 30°C and pH 7.5 for 20 h;

[0066] (3) After the first fermentation, olea europaea seed oil (4% of the total fermentation liquid) was added to the fermentation liquid, and then the yeast liquid was inoculated at a rate of 2% (v / v), and the second fermentation was carried out at 25°C and pH 6.5 for 20 h;

[0067] (4) After the secondary fermentation, lysozyme (the amount added is 0.8% of the total amount of the fermentation liquid) is added for lysozyme treatment;

[0068] (5) The lysed material is subjected to fluidized bed spray drying to obtain fermented mud powder. The inlet temperature of the fluidized bed is set to 180° C., the outlet temperature is set to 85° C., and the pressure is set to 0.5 MPa. The fermented mud powder is granulated to obtain fermented mud microspheres.

[0069] Example 4

[0070] This embodiment provides a method for preparing fermented mud microspheres with multi-dimensional and efficient skin cleansing activity. The steps of the method are different from those of Example 1 only in that the Amazon white mud is ground to a particle size of 65±5 μm, and the amount of kaolin added is kept unchanged. The remaining steps and process parameters are consistent with those of Example 1.

[0071] Example 5

[0072] This embodiment provides a method for preparing fermented mud microspheres with multi-dimensional and efficient skin cleansing activity. The steps of the method are different from those of Example 1 only in that the culture medium does not include Antarctic stalk algae powder, and the reduced amount thereof is distributed to the Norway spruce leaf powder and the Icelandic lichen powder in proportion. The remaining steps and process parameters are consistent with those of Example 1.

[0073] Example 6

[0074] The present embodiment provides a method for preparing fermented mud microspheres with multi-dimensional and efficient skin cleansing activity. The steps of the method differ from those of Example 1 only in that the culture medium does not include Norway spruce leaf powder, and the reduced amount thereof is distributed to Antarctic spathula powder and Icelandic lichen powder in proportion. The remaining steps and process parameters are consistent with those of Example 1.

[0075] Example 7

[0076] This embodiment provides a method for preparing fermented mud microspheres with multi-dimensional and efficient skin cleansing activity. The steps of the method are different from those of Example 1 only in that the culture medium does not include Icelandic lichen powder, and the reduced amount is distributed to Antarctic stalk algae powder and Norway spruce leaf powder in proportion. The remaining steps and process parameters are consistent with those of Example 1.

[0077] Example 8

[0078] This embodiment provides a method for preparing fermented mud microspheres with multi-dimensional and efficient skin cleansing activity. The steps of the method are different from those of Example 1 only in that the vegetable oil is palm oil and the amount of vegetable oil added is kept unchanged. The remaining steps and process parameters are consistent with those of Example 1.

[0079] Comparative Example 1

[0080] This comparative example provides a method for preparing fermented mud microspheres with multi-dimensional and efficient skin cleansing activity, the method comprising:

[0081] (1) Grinding dried Amazonian white mud (water content less than 5%) to a particle size of 35 ± 5 μm, then mixing with culture medium and pure water (Amazonian white mud accounts for 12%, culture medium accounts for 4%, and the remainder is pure water) and then putting into a fermentation tank, wherein the composition of the culture medium is 2 parts of Antarctic stalk algae powder, 2 parts of Norway spruce leaf powder, 2 parts of Icelandic lichen powder and 94 parts of water;

[0082] (2) sterilizing the material in the fermentation tank at 120°C for 18 min, then inoculating Bifidobacterium adolescentis at a 5% (v / v) inoculum, and fermenting at 35°C and pH 7 for 18 h;

[0083] (3) After fermentation, add lysozyme (the amount added is 0.5% of the total amount of the fermentation liquid) for lysozyme treatment;

[0084] (4) The lysed material is subjected to fluidized bed spray drying to obtain fermented mud powder. The inlet temperature of the fluidized bed is set to 190° C., the outlet temperature is set to 80° C., and the pressure is set to 0.3 MPa. The fermented mud powder is granulated to obtain fermented mud microspheres.

[0085] Comparative Example 2

[0086] This comparative example provides a method for preparing fermented mud microspheres with multi-dimensional and efficient skin cleansing activity, and the steps of the method are as follows:

[0087] (1) Grinding dried Amazon white mud (water content less than 5%) to a particle size of 35 ± 5 μm, then mixing with oleifera seed oil and purified water (Amazon white mud accounts for 12%, oleifera seed oil accounts for 3%, and the remainder is purified water) and putting into a fermentation tank;

[0088] (2) The material in the fermentation tank was sterilized at 120°C for 18 min, and then the yeast solution was inoculated at a 3% (v / v) inoculation rate, and fermented at 28°C and pH 5.5 for 25 h;

[0089] (3) After fermentation, add lysozyme (the amount added is 0.5% of the total amount of the fermentation liquid) for lysozyme treatment;

[0090] (4) The lysed material is subjected to fluidized bed spray drying to obtain fermented mud powder. The inlet temperature of the fluidized bed is set to 190° C., the outlet temperature is set to 80° C., and the pressure is set to 0.3 MPa. The fermented mud powder is granulated to obtain fermented mud microspheres.

[0091] Comparative Example 3

[0092] This comparative example provides a method for preparing fermented mud microspheres with multi-dimensional and efficient skin cleansing activity, and the steps of the method are as follows:

[0093] (1) Grinding dried Amazonian white mud (water content less than 5%) to a particle size of 35 ± 5 μm, then mixing with culture medium and pure water (Amazonian white mud accounts for 12%, culture medium accounts for 4%, and the remainder is pure water) and then putting into a fermentation tank, wherein the composition of the culture medium is 2 parts of Antarctic stalk algae powder, 2 parts of Norway spruce leaf powder, 2 parts of Icelandic lichen powder and 94 parts of water;

[0094] (2) The material in the fermentation tank was sterilized at 120°C for 18 min, and then the Bifidobacterium adolescentis bacterial solution was inoculated at a 5% (v / v) inoculation rate, and fermented at 35°C and pH 7 for 18 h;

[0095] (3) After the first fermentation, yeast culture liquid was inoculated into the fermentation liquid at a rate of 3% (v / v), and the second fermentation was carried out at 28°C and pH 5.5 for 25 h;

[0096] (4) After the secondary fermentation, add lysozyme (the amount added is 0.5% of the total amount of the fermentation liquid) for lysozyme treatment;

[0097] (5) The lysed material is subjected to fluidized bed spray drying to obtain fermented mud powder. The inlet temperature of the fluidized bed is set to 190° C., the outlet temperature is set to 80° C., and the pressure is set to 0.3 MPa. The fermented mud powder is granulated to obtain fermented mud microspheres.

[0098] Comparative Example 4

[0099] This embodiment provides a method for preparing fermented mud microspheres with multi-dimensional and efficient skin cleansing activity. The steps of the method are different from those of Example 1 only in that the strain used in the first fermentation is yeast and the inoculation amount is kept unchanged. The remaining steps and process parameters are consistent with those of Example 1.

[0100] Comparative Example 5

[0101] This embodiment provides a method for preparing fermented mud microspheres with multi-dimensional and efficient skin cleansing activity. The steps of the method are different from those of Example 1 only in that the strain used in the secondary fermentation is Bifidobacterium adolescentis, and the inoculation amount is kept unchanged. The remaining steps and process parameters are consistent with those of Example 1.

[0102] Test Example 1

[0103] The samples prepared in Examples 1-8 and Comparative Examples 1-5 were tested for BET specific surface area, oil absorption value and 5α-reductase inhibition rate.

[0104] The BET specific surface area determination method is carried out in accordance with GB / T 19587-2004 The method for determining the specific surface area of ​​solid substances by the BET principle of gas adsorption is carried out.

[0105] Oil absorption value determination method: accurately weigh 100.00g of the material to be tested (powdered material before granulation), add linseed oil drop by drop into 100g of the material to be tested, and stir with a spatula. When linseed oil is first added, the material is in a loose state. As the amount of linseed oil added increases, the material and linseed oil are fully mixed, and then all the materials are bonded together to reach a non-loose state. If linseed oil is continued to be added, the material system will become thinner. At this time, the amount of linseed oil used is the oil absorption value of the filler to be tested.

[0106] 5α-reductase inhibition rate test method:

[0107] (1) Sample treatment: Weigh 60 mg of sample from each group and dilute to 10 ml with PBS to prepare a sample solution with a concentration of 6 mg / ml. Centrifuge and take the supernatant for detection as the sample solution.

[0108] (2) Test process:

[0109] Sample tube A: Take 1 mL of sample solution into a test tube, add 1 mL of 5α-reductase solution, 1 mL of NADPH solution, and 1 mL of testosterone solution, and mix well;

[0110] B Sample background tube: Take 1 mL of sample solution in a test tube, add 1 mL of 5α-reductase solution, 1 mL of NADPH solution, and 1 mL of PBS solution, and mix well;

[0111] C solvent tube: add 1 mL 5α-reductase solution, 1 mL NADPH solution, and 2 mL testosterone solution, and mix well;

[0112] D solvent background tube: add 1mL 5α-reductase solution, 1mL NADPH solution, and 2mL PBS solution, and mix well; react each reaction solution at 37℃ for 20 minutes, remove an appropriate amount of sample solution, and measure the absorbance at 340nm.

[0113] The calculation formula is: Inhibition rate (%) = [1-(OD A -OD B ) / ( OD C -OD D )] ×100

[0114] The test results are shown in Table 2.

[0115] Table 2

[0116]

[0117] It can be seen from the data in Table 2 that the fermented mud microspheres prepared in the embodiment of the present invention have a larger specific surface area, a higher oil absorption value, and a higher 5α-reductase inhibition rate, indicating that the product prepared in the present invention has excellent oil control, deep cleansing, blackhead removal and other effects.

[0118] It can be seen from Example 4 that the particle size of the mineral mud directly affects the specific surface area of ​​the product, which in turn affects its oil absorption effect and 5α-reductase inhibition rate;

[0119] It can be seen from Examples 5-7 that the Antarctic stalk algae powder, the Norway spruce leaf powder, and the Icelandic lichen powder in the plant culture medium have a synergistic effect, and the combination of the three can make the 5α-reductase inhibition rate of the product higher;

[0120] As can be seen from Example 8, the type of vegetable oil also affects the oil absorption and oil control effects of the product;

[0121] It can be seen from Comparative Examples 1-2 that when the mineral mud is fermented only once, the oil absorption value and 5α-reductase inhibition rate of the product are significantly lower;

[0122] It can be seen from Comparative Example 3 that when no vegetable oil is added in the secondary fermentation, the oil absorption value and 5α-reductase inhibition rate of the product will also be affected.

[0123] It can be seen from Comparative Examples 4-5 that only when the strains used in the primary fermentation or the secondary fermentation are the strains selected by the present invention, the oil control effect of the obtained product can be better.

[0124] Test Example 2

[0125] Test objects: fermented mud microspheres prepared in Examples 1-8 and Comparative Examples 1-5.

[0126] Test method:

[0127] 1. Total glycosides test

[0128] (1) Preparation of reference solution: Accurately weigh an appropriate amount of Centella asiatica total glycosides reference substance and dissolve it in ethanol to prepare a 1 mg / mL solution.

[0129] (2) Preparation of standard curve: Accurately measure 0, 0.5, 1.0, 1.5, 2.0, and 2.5 mL of the reference solution respectively into a 100 mL volumetric flask, place in an 80°C water bath to evaporate the solvent, take out, add 2 mL of sulfuric acid, shake well, place in an 80°C water bath to heat for 30 min, take out, place in an ice bath and add about 80 mL of ethanol, take out, dilute to the scale with ethanol, shake well, and measure the absorbance at a wavelength of 276 nm using the first tube as the blank by spectrophotometry. Draw a standard curve with concentration as the horizontal axis and absorbance as the vertical axis. The result requires R2 ≥ 0.999.

[0130] (3) Preparation of test solution:

[0131] Weigh a certain amount of fermented mud microspheres, extract with anhydrous ethanol by ultrasonic for 10 minutes, filter, and dilute the filtrate to a 100mL volumetric flask to obtain the test solution. Accurately measure 1mL of the test solution, follow the standard curve preparation procedure, and measure the absorbance at a wavelength of 276nm.

[0132] 2. Total Sugar Test

[0133] (1) Preparation of reference solution: Accurately weigh 10 mg of anhydrous glucose dried to constant weight at 120°C and place it in a 100 mL volumetric flask. Add pure water to the mark and shake well to prepare a 0.1 mg / mL reference solution.

[0134] (2) Preparation of standard curve: Prepare glucose standard solutions with concentrations of 0.02, 0.04, 0.06, 0.08, and 0.10 mg / mL. Accurately pipette 1 mL of the standard solution into a test tube, add 1 mL of 5% phenol solution, then add 5 mL of concentrated sulfuric acid, shake well, place in a boiling water bath for 15 minutes, cool to room temperature, and measure its absorbance at a wavelength of 485 nm. Draw a standard curve with concentration as the horizontal axis and absorbance as the vertical axis. The result requires R 2 ≥0.999.

[0135] (3) Preparation of test solution

[0136] Weigh a certain amount of fermented mud microspheres, extract with pure water ultrasonically for 10 minutes, filter, dilute the filtrate to a 100mL volumetric flask to obtain the test solution, take 1mL of the test solution, add 1mL of 5% phenol solution (phenol must be prepared before use), then add 5mL of concentrated sulfuric acid to the test tube, boil in water for 15 minutes, and cool to room temperature. Measure its absorbance value at a wavelength of 485nm on a UV spectrophotometer.

[0137] 3. Total flavonoids test

[0138] (1) Preparation of reference solution: Accurately weigh 20 mg of rutin reference substance that has been dried to constant weight at 120°C and place it in a 100 mL volumetric flask. Add 70% ethanol to dissolve and dilute to the mark. Shake well to prepare a 0.2 mg / mL reference solution.

[0139] (2) Preparation of standard curve: Accurately pipette 0.5, 1.0, 2.0, 4.0, mL of rutin reference solution into a 25 mL volumetric flask, add 70% ethanol to 10 mL, then add 0.7 mL of 5% sodium nitrite solution, shake well, let stand for 6 min, then add 0.7 mL of 10% aluminum nitrate solution, shake well, let stand for 6 min, then add 5.5 mL of 4.3% sodium hydroxide solution, dilute to scale with 70% ethanol, shake well, let stand for 15 min, use 70% ethanol as reference solution, and measure absorbance at a wavelength of 510 nm. Draw a standard curve with absorbance value (A) as the ordinate and rutin reference concentration (C) as the abscissa. The result requires R 2 ≥0.999.

[0140] (3) Preparation of test solution: Same as total glycoside test. Accurately measure 1 mL of the test solution and follow the steps in the preparation of standard curve to measure the absorbance at 276 nm.

[0141] 4. Sophorolipid Content

[0142] The HPLC method was used to test the sophorolipid content of the samples; the high performance liquid chromatography method was determined in accordance with General Rules 0512 of Part IV of the 2020 edition of the Chinese Pharmacopoeia.

[0143] 5. Mercury, cadmium, arsenic and lead content

[0144] The mercury, cadmium, arsenic and lead contents in the samples were tested by atomic absorption spectrometry (only Examples 1-3 were tested), and the atomic absorption method was used in accordance with General Rules 0406 of Part IV of the 2020 Edition of the Chinese Pharmacopoeia.

[0145] The test results are shown in Tables 3 and 4.

[0146] Table 3

[0147]

[0148] Table 4

[0149]

[0150] It can be seen from the data in Tables 3 and 4 that the fermented mud microspheres prepared in Examples 1-3 of the present invention have a total glycoside content of active ingredients ≥0.2%, a total sugar content ≥0.5%, a total flavonoid content ≥0.2, and a sophorolipid content ≥0.2, indicating that the product prepared by the present invention has excellent oil control, deep cleaning, blackhead removal and other effects, and the contents of mercury, cadmium, arsenic and lead are all below the provisions of the "Technical Specification for Safety of Cosmetics", so the safety of the product is also higher.

[0151] The present invention uses the above-mentioned embodiments to illustrate the preparation method of fermented mud microspheres with multi-dimensional and efficient skin cleansing activity, its products and applications, 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, the equivalent replacement of the raw materials of the product of the present invention, the addition of auxiliary ingredients, the selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0152] 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.

[0153] 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. A method for preparing fermented mud microspheres with multi-dimensional and efficient skin cleansing activity, characterized in that: The preparation method comprises: (1) Grinding the mineral mud and then mixing it with the culture medium and pure water to obtain a mixed material; The grinding to a particle size of ≤50 μm; The culture medium comprises, by weight, 1-3 parts of Antarctic stalk algae powder, 1-3 parts of Norway spruce leaf powder, 1-3 parts of Iceland lichen powder, 0.5-1 parts of a carbon source, 0.5-1 parts of a nitrogen source, 0.01-0.2 parts of an inorganic salt, and 85-99 parts of water; (2) sterilizing the mixed material and then inoculating Bifidobacterium for primary fermentation; The bifidobacterium includes Bifidobacterium adolescentis and / or Bifidobacterium breve; (3) After the first fermentation is completed, vegetable oil is added to the fermentation liquid, and then yeast is added to perform a second fermentation; the vegetable oil includes olea oleifera seed oil, and the amount of the added vegetable oil is 1-5% of the total mass of the fermentation liquid; the vegetable oil is converted into sophoroside esters by yeast fermentation; (4) After the secondary fermentation, lysozyme is added for lysozyme treatment, and then the fermented mud powder is dried to obtain fermented mud powder, and the fermented mud powder is granulated to obtain fermented mud microspheres.

2. The preparation method according to claim 1, characterized in that The mineral mud in step (1) includes kaolin and / or Amazonian white mud.

3. The preparation method according to claim 1, characterized in that: Calculated by weight percentage, the mixed material in step (1) includes 10-15% mineral mud, 3-5% culture medium and 80%-90% water.

4. The preparation method according to claim 1, characterized in that: The amount of bifidobacterium introduced in step (2) is 1-10% (v / v); The temperature of the first fermentation in step (2) is 30-40°C, the pH is 6.5-7.5, and the fermentation time is 15-20h; The yeast in step (3) is added at a concentration of 1-5% (v / v); The temperature of the secondary fermentation in step (3) is 25-30°C, the pH is 4.0-6.5, and the time is 20-30 hours.

5. The preparation method according to claim 1, characterized in that: The amount of lysozyme added in step (4) is 0.1-1% of the total mass of the fermentation liquid after the secondary fermentation; The drying method in step (4) is fluidized bed spray drying; The inlet temperature of the spray drying is 180-200°C, the outlet temperature is 75-85°C, and the pressure is 0.2-0.5MPa.

6. A fermented mud microsphere, characterized in that: The fermented mud microspheres are prepared by the method according to any one of claims 1 to 5.

7. Use of the fermented mud microspheres as claimed in claim 6 in the preparation of cosmetics.

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