An oil control, volumizing and smoothing hair composition, method of making and use thereof

Abstract

The present application belongs to the technical field of daily cosmetics, and particularly relates to a composition for controlling oil, fluffing and smoothing hair, and a preparation method and application thereof. The present application uses black willow bark and dendrobium stem as fermentation raw materials to prepare a fermentation medium, inoculates Brazil mold into the fermentation medium containing the black willow bark and the dendrobium stem to perform fermentation, and obtains active substances rich in the effects of controlling oil, fluffing and smoothing hair. The preparation method of the composition for controlling oil, fluffing and smoothing hair avoids fermentation of each plant alone, simplifies the preparation process, reduces the production cost, and does not use any organic solvent in the preparation process. The prepared composition is safe to human body, harmless to the environment, and beneficial to environmental protection.

Description

Technical Field

[0001] This invention belongs to the field of daily cosmetics technology, specifically relating to a composition for controlling oil, volumizing and smoothing hair, its preparation method and application. Background Technology

[0002] With the fast pace of modern life, unhealthy dietary habits such as consuming greasy and spicy foods, and unhealthy lifestyles such as staying up late, easily stimulate the secretion of sebum from the scalp's sebaceous glands. Therefore, oily scalp and hair have become a problem for many people. Oily scalp problems can easily lead to an imbalance in the scalp's microbial environment, causing dandruff, seborrheic dermatitis, and in severe cases, even hair loss.

[0003] Currently, most oil-controlling hair care products on the market are simply hair products with added oil-controlling ingredients to give them this function. These ingredients typically include surfactants and plant extracts. However, most existing plant extracts that claim to control oil are obtained through water extraction, alcohol extraction, or ultrasonic extraction. This process often fails to effectively extract many active ingredients from the plants, making it difficult for the resulting plant extracts to fundamentally tighten scalp pores and reduce sebum secretion. Consequently, the corresponding hair products are unlikely to achieve an effective oil-controlling effect.

[0004] Patent publication number CN11445233A discloses an oil-controlling and dandruff-reducing shampoo, comprising water, hair conditioning agents, surfactants, chelating agents, emulsifiers, preservatives, pH adjusters, dandruff-reducing agents, fragrances, sodium chloride, skin conditioning agents, and moisturizers. This formula can gently cleanse the scalp and hair, reducing itching and hair loss; however, it does not reduce sebum secretion from the sebaceous glands, thus only treating the symptoms, not the root cause. Furthermore, using this shampoo leaves hair dry and rough.

[0005] Patent publication number CN110368345A discloses an oil-controlling and anti-hair loss shampoo, further revealing its formula as follows: 3-5 parts geraniol, 3-6 parts phytosterol, 0.3-0.6 parts linolenic acid, 1-3 parts baijiu (Chinese white liquor), 2-4 parts palmitate, 1-3 parts mogroside V, 2-5 parts polyquaternium-392, 12-16 parts herbal extracts for oil control and anti-hair loss, 1-2 parts white vinegar, 0.3-0.6 parts sesame oil, and 70-80 parts deionized water. The herbal extracts for oil control and anti-hair loss are extracted using an ethanol heating reflux method, which fails to effectively extract the active ingredients from the herbs. While the resulting shampoo has good oil-controlling effects, it cannot fundamentally tighten scalp pores or reduce sebum secretion.

[0006] In summary, existing technologies generally suffer from problems such as poor oil control, difficulty in fundamentally reducing sebum secretion, and dry, rough hair after use. Summary of the Invention

[0007] To overcome the aforementioned technical problems, the present invention aims to provide a composition for controlling oil, increasing volume, and smoothing hair, its preparation method, and its application. The preparation process of the oil-controlling, volume, and smoothing hair composition provided by the present invention involves the co-fermentation of black willow bark and Dendrobium nobile, enabling the resulting composition to fundamentally reduce sebum secretion from the sebaceous glands, resulting in excellent scalp oil control, increased hair volume, and smoother hair.

[0008] To achieve the above objectives, the technical solution of the present invention is as follows:

[0009] A method for preparing a composition for oil control, volumizing and smoothing hair, specifically comprising: using black willow bark powder, Dendrobium nobile stem powder, carbon source, nitrogen source, trace elements and water as a fermentation medium, and fermenting the fermentation medium by inoculating Aspergillus brasiliensis seed liquid to obtain a composition for oil control, volumizing and smoothing hair.

[0010] Furthermore, a method for preparing a composition that controls oil, adds volume, and smooths hair includes the following steps:

[0011] S1. Mix black willow bark powder, Dendrobium nobile stem powder with carbon source, nitrogen source, trace elements and water evenly, sterilize and cool down to obtain fermentation culture medium;

[0012] S2. Inoculate the Aspergillus brasiliensis seed liquid into the fermentation medium prepared in step S1, introduce sterile air, and carry out fermentation to obtain plant fermentation broth.

[0013] S3. The plant fermentation broth obtained in step S2 is subjected to inactivation treatment and filtration treatment to obtain the final product.

[0014] Furthermore, in step S1 of the preparation method of the oil-controlling, fluffy, and smooth hair composition, the preparation method of black willow bark powder is as follows: dry black willow bark is ground into powder, passed through a 50-120 mesh sieve, and the lower layer of powder is taken out to obtain the black willow bark powder; the preparation method of Dendrobium nobile powder is as follows: dry Dendrobium nobile stems are ground into powder, passed through a 50-120 mesh sieve, and the lower layer of powder is taken out to obtain the Dendrobium nobile stem powder;

[0015] Furthermore, in step S2 of the method for preparing the oil-controlling, volumizing, and smoothing hair composition, the method for preparing the *Aspergillus brasiliensis* seed solution is as follows: *Aspergillus brasiliensis* colonies are picked up with an inoculation loop and cultured in a liquid culture medium to obtain a concentration of 1×10⁻⁶. 7 -1×10 9 The seed culture of Aspergillus brasiliensis was prepared at a concentration of cfu / ml; the culture conditions were: temperature 25-35℃, rotation speed 100-300 rpm, and culture time 72-120 h.

[0016] Furthermore, in step S2 of the preparation method of the oil-controlling, volumizing, and smoothing hair composition, the liquid culture medium is potato composite culture medium. The preparation method is as follows: take 3g of potassium dihydrogen phosphate, 1.5g of magnesium sulfate heptahydrate, 8mg of vitamin B1, 20g of glucose, and 20% potato juice to a total volume of 1000mL, sterilize at 120℃ for 20min, and store for later use; wherein the 20% potato juice is prepared by: taking 200g of peeled potatoes, cutting them into small pieces, adding 1000mL of water and boiling for 20min, filtering out the potato pieces, and adding the filtrate to 1000mL to obtain the final product.

[0017] Furthermore, in step S1 of the preparation method of the oil-controlling, fluffy and smooth hair composition, the total amount of black willow bark powder and Dendrobium nobile stem powder added is 0.5-2.0% of the mass of the fermentation culture medium, and the mass ratio of black willow bark powder to Dendrobium nobile stem powder is 5-9:1.

[0018] Furthermore, in step S1 of the method for preparing the oil-controlling, fluffy, and smooth hair composition, the carbon source is at least one of dextrin, fructose, sucrose, and glucose, and the amount of carbon source added is 0.8-2% of the mass of the fermentation medium; the nitrogen source is at least one of soybean peptone, yeast extract, and cottonseed meal, and the amount of nitrogen source added is 0.4-1.8% of the mass of the fermentation medium.

[0019] Furthermore, in step S1 of the preparation method of the oil-controlling, volumizing and smoothing hair composition, the trace element is B vitamins, and the amount of the trace element added is 0.05-0.3% of the mass of the fermentation culture medium; the water is added to 100% of the mass of the fermentation culture medium.

[0020] Furthermore, in step S1 of the method for preparing the oil-controlling, volumizing, and smoothing hair composition, the sterilization temperature is 121°C, the sterilization pressure is 0.1 MPa, and the sterilization time is 30 min.

[0021] Furthermore, in step S2 of the method for preparing the oil-controlling, volumizing, and smoothing hair composition, the inoculation amount of Aspergillus brasiliensis seed liquid is 1-3% of the mass of the fermentation medium; the fermentation temperature is 25-35℃, the rotation speed is 100-250rpm, and the fermentation time is 56-96h.

[0022] The inoculum size of *Aspergillus brasiliensis* seed culture has a significant impact on the fermentation process. Specifically, when the inoculum size is less than 1%, the insufficient amount of *Aspergillus brasiliensis* in the fermentation medium results in a low number of *Aspergillus brasiliensis*, leading to inefficient utilization of nutrients and reduced production of oil-controlling, fluffy, and hair-smoothing active substances in the plant fermentation broth. Conversely, when the inoculum size exceeds 3%, the excessive number of *Aspergillus brasiliensis* introduced into the fermentation medium causes them to proliferate rapidly. This can lead to the bacteria consuming the produced oil-controlling, fluffy, and hair-smoothing active substances, resulting in a lower overall production of these active substances.

[0023] Fermentation temperature and time have a significant impact on the fermentation process. Specifically, the fermentation temperature of this invention should be controlled between 25-35℃. When the fermentation temperature is below 25℃ or above 35℃, *Aspergillus brasiliensis* grows slowly, and the nutrients in the fermentation medium cannot be effectively utilized, easily leading to a lower concentration of active substances in the final product. The fermentation time should be controlled between 56-96 hours. When the fermentation time is less than 56 hours, *Aspergillus brasiliensis* is still in its growth phase, the concentration of *Aspergillus brasiliensis* in the fermentation broth is low, and many nutrients in the fermentation medium are not utilized or transformed, resulting in a lower concentration of oil-controlling, fluffy, and smooth hair active substances in the final product. When the fermentation time is greater than 96 hours, *Aspergillus brasiliensis* proliferates rapidly, and the bacteria enter the apoptosis phase, easily leading to cell autolysis. The prepared oil-controlling, fluffy, and smooth hair active substances will be further consumed, resulting in a lower concentration of active substances in the final product.

[0024] Furthermore, in step S3 of the method for preparing the oil-controlling, volumizing, and smoothing hair composition, the inactivation treatment temperature is 85-115℃ and the inactivation treatment time is 15-30min; the filtration treatment uses a diatomaceous earth filter or a microfiltration membrane.

[0025] The present invention also provides an oil-controlling, volumizing, and smoothing hair composition prepared by the above-described method for preparing the oil-controlling, volumizing, and smoothing hair composition, which is used in the preparation of hair products.

[0026] This invention uses black willow bark powder, Dendrobium nobile stem powder, carbon source, nitrogen source, trace elements, and water as a fermentation medium. The fermentation medium is inoculated with Aspergillus brasiliensis seed liquid to obtain a composition that controls oil, promotes volume, and smooths hair. During fermentation, Aspergillus brasiliensis utilizes the black willow bark powder, Dendrobium nobile stem powder, carbon source, and nitrogen source in the fermentation medium for growth and reproduction. This process releases active substances from the black willow bark powder and Dendrobium nobile stem powder into the fermentation liquid. The final product contains active substances that control scalp oil, promote volume, and smooth hair. Furthermore, the inventors discovered during their research that only fermentation using Aspergillus brasiliensis seed liquid yields the optimal effects of controlling scalp oil, promoting volume, and smoothing hair.

[0027] Compared with conventional methods such as water extraction and ultrasonic extraction, fermentation uses microbial metabolism to transform active ingredients into smaller molecules that are more easily absorbed, resulting in a final product containing more active substances.

[0028] The oil-controlling, volumizing, and smoothing hair composition provided by this invention can be prepared into any formulation conventionally prepared in the field of hair care products, and can be formulated into, for example, solutions, suspensions, emulsions, pastes, gels, creams, water, powders, soaps, surfactant-containing detergents, oils, powder creams, sprays, etc., but this invention is not limited thereto. More specifically, the compositions of this invention can be prepared into the following formulations: hair conditioner, hair nourishing cream, hair massage cream, hair essence, shampoo cream, shampoo foam, shampooing lotion, hair moisturizing cream, shampoo, conditioner, etc.

[0029] Compared with existing technologies, the composition for oil control, volumizing and smoothing hair, its preparation method and application provided by the present invention have the following technical advantages:

[0030] (1) The composition prepared by the present invention using the seed liquid fermentation method of Aspergillus brasiliensis is rich in active substances from black willow bark and Dendrobium nobile stem, and has excellent effects on scalp oil control, hair fluffing and hair smoothing.

[0031] (2) In this invention, black willow bark and Dendrobium nobile stem are fermented together, which avoids fermenting each plant separately, greatly simplifies the preparation process, shortens the preparation cycle, and reduces production costs. At the same time, research has shown that the active substance composition obtained by fermenting black willow bark and Dendrobium nobile stem together is more effective than the combination of fermented single plants.

[0032] (3) The composition for oil control, fluffing and smoothing hair provided by the present invention does not use any organic solvents in the preparation process. The resulting composition is safe for human body and harmless to the environment, which is beneficial to environmental protection. Detailed Implementation

[0033] The present invention is further described below through specific embodiments, but the present invention is not limited to the following embodiments. Those skilled in the art can make various modifications based on the basic idea of ​​the present invention, but as long as they do not depart from the basic idea of ​​the present invention, they are all within the scope of the present invention.

[0034] The Aspergillus brasiliensis used in this specific embodiment is Aspergillus brasiliensis (BNCC341632), and the Saccharomyces cerevisiae used in this invention is Saccharomyces cerevisiae (BNCC336054). Both strains were purchased from Beijing Beina Chuanglian Biotechnology Research Institute. It should be noted that commercially available Aspergillus brasiliensis can be used to prepare the composition of this invention with oil-controlling, hair-volumizing, and smoothing effects, and is not limited to the Aspergillus brasiliensis (BNCC341632) mentioned above.

[0035] The microfiltration membrane used in this specific embodiment is a polypropylene microfiltration membrane column, and the pore diameter of the polypropylene microfiltration membrane column is 2.5 μm.

[0036] Example 1

[0037] An oil-controlling, volumizing, and smoothing hair composition is prepared by the following steps:

[0038] (1) Grind the dried black willow bark and Dendrobium nobile stem into powder, pass them through an 80-mesh sieve, and take the bottom layer of powder to obtain black willow bark powder and Dendrobium nobile stem powder.

[0039] (2) Use an inoculation loop to pick up Aspergillus brasiliensis colonies and place them into potato composite medium. Incubate at 28°C and 120 rpm for 96 h to obtain a bacterial concentration of 1×10⁻⁶. 8 Aspergillus brasiliensis seed culture (cfu / ml);

[0040] (3) Mix the black willow bark powder and Dendrobium nobile stem powder obtained in step (1) with carbon source, nitrogen source, trace elements and water evenly, sterilize at 121℃ and 0.1MPa for 30 minutes and then cool down to obtain fermentation culture medium.

[0041] (4) Inoculate the Aspergillus brasiliensis seed liquid obtained in step (2) into the fermentation medium obtained in step (3). The inoculation amount of Aspergillus brasiliensis seed liquid is 2% of the mass of the fermentation medium. Sterile air is introduced and fermented at 28°C and 150 rpm for 72 hours to obtain plant fermentation liquid.

[0042] (5) The plant fermentation liquid obtained in step (4) is kept at 90°C for 20 minutes to inactivate it, and then filtered using a diatomaceous earth filter to obtain a composition that controls oil, makes hair fluffy and smooth.

[0043] The liquid culture medium in step (2) is potato composite culture medium. The preparation method is as follows: take 3g of potassium dihydrogen phosphate, 1.5g of magnesium sulfate heptahydrate, 8mg of vitamin B1, 20g of glucose, and 20% potato juice to a total volume of 1000mL. Sterilize at 120℃ for 20min and store for later use. The 20% potato juice is prepared as follows: take 200g of peeled potatoes, cut them into small pieces, add 1000mL of water and boil for 20min. Filter out the potato pieces and add the filtrate to 1000mL.

[0044] In step (3), the total amount of black willow bark powder and Dendrobium nobile stem powder added is 1.0% of the fermentation medium mass, and the mass ratio of black willow bark powder to Dendrobium nobile stem powder is 7:1. The carbon source is dextrin, added at 1.2% of the fermentation medium mass. The nitrogen source is soybean peptone, added at 0.8% of the fermentation medium mass. The trace element is vitamin B1, added at 0.1% of the fermentation medium mass. Water is added to 100% of the fermentation medium mass.

[0045] The preparation methods of the oil-controlling, fluffy and smooth hair compositions provided in Examples 2-9 and Comparative Examples 1-10 are the same as those in Example 1, except that the fermentation raw materials and their amounts, carbon source, nitrogen source and their amounts, trace element types, strain types and fermentation temperature are changed. The parameters that were changed in Examples 2-11 and Comparative Examples 1-10 are shown in Table 1.

[0046] Table 1

[0047] Group Fermentation raw materials and their dosage Carbon source, nitrogen source and their addition amount Trace element types strain type and inoculum amount Fermentation temperature and fermentation time Parameters changed compared to Example 1 Example 1 Black willow bark: Dendrobium nobile stem = 7:1 Dextrin 1.2%, Soy peptone 0.8% Vitamin B1 Aspergillus brasiliensis 2% 28℃、 72h —— Example 2 Black willow bark: Dendrobium nobile stem = 5:1 Dextrin 1.2%, Soy peptone 0.8% Vitamin B1 Aspergillus brasiliensis 2% 28℃ 72h The ratio of fermentation raw materials was changed to 5:1. Example 3 Black willow bark: Dendrobium nobile stem = 9:1 Dextrin 1.2%, Soy peptone 0.8% Vitamin B1 Aspergillus brasiliensis 2% 28℃ 72h The ratio of fermentation raw materials was changed to 9:1. Example 4 Black willow bark: Dendrobium nobile stem = 7:1 Fructose 1.2%, Soy peptone 0.8% Vitamin B1 Aspergillus brasiliensis 2% 28℃ 72h Carbon source changed to fructose Example 5 Black willow bark: Dendrobium nobile stem = 7:1 Dextrin 1.2%, tryptone 0.8% Vitamin B1 Aspergillus brasiliensis 2% 28℃ 72h The nitrogen source is changed to tryptone. Example 6 Black willow bark: Dendrobium nobile stem = 7:1 Dextrin 1.2%, Yeast extract 0.8% Vitamin B1 Aspergillus brasiliensis 2% 28℃ 72h Nitrogen source changed to yeast extract Example 7 Black willow bark: Dendrobium nobile stem = 7:1 Dextrin 1.2%, Soy peptone 0.8% Vitamin B5 Aspergillus brasiliensis 2% 28℃ 72h The type of trace element has been changed to vitamin B5. Example 8 Black willow bark: Dendrobium nobile stem = 7:1 Dextrin 1.2%, Soy peptone 0.8% Vitamin B1 Aspergillus brasiliensis 2% 25℃ 72h The fermentation temperature was changed to 25℃ Example 9 Black willow bark: Dendrobium nobile stem = 7:1 Dextrin 1.2%, Soy peptone 0.8% Vitamin B1 Aspergillus brasiliensis 2% 35℃ 72h The fermentation temperature was changed to 35℃ Comparative Example 1 1% black willow bark Dextrin 1.2%, Soy peptone 0.8% Vitamin B1 Aspergillus brasiliensis 2% 28℃ 72h All fermentation raw materials are made from black willow bark. Comparative Example 2 Dendrobium nobile stem 1% Dextrin 1.2%, Soy peptone 0.8% Vitamin B1 Aspergillus brasiliensis 2% 28℃ 72h The fermentation raw materials are all made from Dendrobium nobile stems. Comparative Example 3 Black willow bark: Dendrobium nobile leaves = 7:1 Dextrin 1.2%, Soy peptone 0.8% Vitamin B1 Aspergillus brasiliensis 2% 28℃ 72h The fermentation raw material was changed to Dendrobium nobile leaves instead of Dendrobium nobile stems. Comparative Example 4 Black willow leaves: Dendrobium nobile stems = 7:1 Dextrin 1.2%, Soy peptone 0.8% Vitamin B1 Aspergillus brasiliensis 2% 28℃ 72h The fermentation raw material was changed to black willow leaves instead of black willow bark. Comparative Example 5 Black willow bark : Dendrobium officinale stem = 7 : 1 Dextrin 1.2%, Soy peptone 0.8% Vitamin B1 Aspergillus brasiliensis 2% 28℃ 72h The fermentation raw material was changed from Dendrobium officinale stems to Dendrobium nobile stems. Comparative Example 6 Black willow bark: Dendrobium nobile stem = 7:1 Dextrin 1.2%, Soy peptone 0.8% Vitamin B1 2% of brewer's yeast 28℃ 72h Change the strain type to brewer's yeast Comparative Example 7 Black willow bark: Dendrobium nobile stem = 7:1 Dextrin 1.2%, Soy peptone 0.8% none Aspergillus brasiliensis 2% 28℃ 72h No trace elements added Comparative Example 8 Black willow bark: Dendrobium nobile stem = 7:1 Dextrin 1.2%, Soy peptone 0.8% Vitamin A Aspergillus brasiliensis 2% 28℃ 72h Replace trace elements with vitamin A Comparative Example 9 Black willow bark: Dendrobium nobile stem = 7:1 Dextrin 1.2%, Soy peptone 0.8% Vitamin B1 Aspergillus brasiliensis 2% 15℃ 72h Fermentation temperature lowered Comparative Example 10 Black willow bark: Dendrobium nobile stem = 7:1 Dextrin 1.2%, Soy peptone 0.8% Vitamin B1 Aspergillus brasiliensis 2% 45℃ 72h Fermentation temperature rise Comparative Example 11 Black willow bark: Dendrobium nobile stem = 7:1 Dextrin 1.2%, Soy peptone 0.8% Vitamin B1 Aspergillus brasiliensis 0.5% 28℃ 72h The inoculum size of Aspergillus brasiliensis seed culture was reduced. Comparative Example 12 Black willow bark: Dendrobium nobile stem = 7:1 Dextrin 1.2%, Soy peptone 0.8% Vitamin B1 Aspergillus brasiliensis 5% 28℃ 72h Increased inoculum size of Aspergillus brasiliensis seed culture Comparative Example 13 Black willow bark: Dendrobium nobile stem = 7:1 Dextrin 1.2% Soy peptone 0.8% 28 Vitamin B1 Aspergillus brasiliensis 2% 28℃ 40h Shortened fermentation time Comparative Example 14 Black willow bark: Dendrobium nobile stem = 7:1 Dextrin 1.2%, Soy peptone 0.8% Vitamin B1 Aspergillus brasiliensis 2% 28℃ 105h Extended fermentation time

[0048] Example 10

[0049] An oil-controlling, volumizing, and smoothing hair composition is prepared by the following steps:

[0050] (1) Grind the dried black willow bark into powder, pass it through a 50-mesh sieve, and take the bottom layer of powder to obtain black willow bark powder; grind the dried Dendrobium nobile stem into powder, pass it through a 120-mesh sieve, and take the bottom layer of powder to obtain Dendrobium nobile stem powder.

[0051] (2) Use an inoculation loop to pick up Aspergillus brasiliensis colonies and transfer them to potato broth. Incubate at 29°C and 250 rpm for 120 h to obtain a bacterial concentration of 1×10⁻⁶. 9 Aspergillus brasiliensis seed culture (cfu / ml);

[0052] (3) Mix the black willow bark powder and Dendrobium nobile stem powder obtained in step (1) with carbon source, nitrogen source, trace elements and water evenly, sterilize at 121℃ and 0.1MPa for 30 minutes and then cool down to obtain fermentation culture medium.

[0053] (4) Inoculate the Aspergillus brasiliensis seed liquid obtained in step (2) into the fermentation medium obtained in step (3). The inoculation amount of Aspergillus brasiliensis seed liquid is 1% of the mass of the fermentation medium. Sterile air is introduced and fermented at 30°C and 250 rpm for 96 hours to obtain plant fermentation liquid.

[0054] (5) The plant fermentation liquid obtained in step (4) is kept at 115°C for 15 minutes to inactivate it, and then filtered using a diatomaceous earth filter to obtain an oil-controlling, fluffy and smooth hair composition.

[0055] The liquid culture medium in step (2) is potato composite culture medium. The preparation method is as follows: take 3g of potassium dihydrogen phosphate, 1.5g of magnesium sulfate heptahydrate, 8mg of vitamin B1, 20g of glucose, and 20% potato juice to a total volume of 1000mL. Sterilize at 120℃ for 20min and store for later use. The 20% potato juice is prepared as follows: take 200g of peeled potatoes, cut them into small pieces, add 1000mL of water and boil for 20min. Filter out the potato pieces and add the filtrate to 1000mL.

[0056] In step (3), the total amount of black willow bark powder and Dendrobium nobile stem powder added is 0.5% of the fermentation medium mass, and the mass ratio of black willow bark powder to Dendrobium nobile stem powder is 7:1. The carbon source is dextrin, added at 0.8% of the fermentation medium mass. The nitrogen source is cottonseed powder, added at 1.8% of the fermentation medium mass. The trace element is vitamin B1, added at 0.2% of the fermentation medium mass. Water is added to 100% of the fermentation medium mass.

[0057] Example 11

[0058] An oil-controlling, volumizing, and smoothing hair composition is prepared by the following steps:

[0059] (1) Grind the dried black willow bark into powder, pass it through a 120-mesh sieve, and take the bottom layer of powder to obtain black willow bark powder; grind the dried Dendrobium nobile stem into powder, pass it through a 50-mesh sieve, and take the bottom layer of powder to obtain Dendrobium nobile stem powder.

[0060] (2) Use an inoculation loop to pick up Aspergillus brasiliensis colonies and place them into potato broth. Incubate at 32°C and 200 rpm for 72 h to obtain a bacterial concentration of 1×10⁻⁶. 7 Aspergillus brasiliensis seed culture (cfu / ml);

[0061] (3) Mix the black willow bark powder and Dendrobium nobile stem powder obtained in step (1) with carbon source, nitrogen source, trace elements and water evenly, sterilize at 121℃ and 0.1MPa for 30 minutes and then cool down to obtain fermentation culture medium.

[0062] (4) Inoculate the Aspergillus brasiliensis seed liquid obtained in step (2) into the fermentation medium obtained in step (3). The inoculation amount of Aspergillus brasiliensis seed liquid is 3% of the mass of the fermentation medium. Sterile air is introduced and fermented at 32°C and 120 rpm for 56 hours to obtain plant fermentation liquid.

[0063] (5) The plant fermentation liquid obtained in step (4) is kept at 85°C for 30 minutes to inactivate it. Then the inactivated mixed fermentation liquid is filtered through a 2.5μm polypropylene microfiltration membrane column to obtain an oil-controlling, fluffy and smooth hair composition.

[0064] The liquid culture medium in step (2) is potato composite culture medium. The preparation method is as follows: take 3g of potassium dihydrogen phosphate, 1.5g of magnesium sulfate heptahydrate, 8mg of vitamin B1, 20g of glucose, and 20% potato juice to a total volume of 1000mL. Sterilize at 120℃ for 20min and store for later use. The 20% potato juice is prepared as follows: take 200g of peeled potatoes, cut them into small pieces, add 1000mL of water and boil for 20min. Filter out the potato pieces and add the filtrate to 1000mL.

[0065] In step (3), the total amount of black willow bark powder and Dendrobium nobile stem powder added is 2% of the fermentation medium mass, and the mass ratio of black willow bark powder to Dendrobium nobile stem powder is 7:1. The carbon source is glucose, added at 2.0% of the fermentation medium mass. The nitrogen source is soybean peptone, added at 0.4% of the fermentation medium mass. The trace element is vitamin B1, added at 0.2% of the fermentation medium mass. Water is added to 100% of the fermentation medium mass.

[0066] Application example: A shampoo for controlling oil, volumizing and smoothing hair, and its preparation method.

[0067] The compositions obtained in Examples 1-11 and Comparative Examples 1-14 were prepared into shampoos, and the shampoo formulations are shown in Table 2:

[0068] Table 2. Shampoo formulas for oil control, volumizing, and smoothing hair.

[0069]

[0070] The preparation method of the oil-controlling, volumizing, and smoothing shampoo is as follows: Add all materials of phase A to the main pot, stir thoroughly until uniformly transparent, then add all materials of phase B, stir thoroughly until uniformly transparent, heat to 65°C, then add all materials of phase C sequentially, stirring thoroughly until completely dissolved and uniform, then heat to 80°C and maintain this temperature for 12 minutes to defoam. At 80°C, add all materials of phase D, stir until completely dissolved and uniform, and maintain this temperature for 12 minutes to defoam. Cool to 45°C, then add all materials of phase E sequentially, stirring thoroughly to obtain the shampoo.

[0071] Experimental Example 1: Scalp Sebum Secretion Test

[0072] Test samples: Shampoos prepared using the compositions obtained in Examples 1-11 and Comparative Examples 1-14 as active substances, and control shampoos (the preparation method of the shampoos is the same as that in the application examples).

[0073] Experimental Methods: 520 volunteers with oily scalps were selected (20 volunteers used one shampoo). A two-week shampooing period was set before the test to avoid the influence of the original product depositing on the hair and scalp. During the shampooing period, volunteers used an unconditioned baby shampoo as a shampooing agent every 2 or 3 days. After the two-week shampooing period, volunteers used the test sample themselves, taking the sample according to their hair volume and length, once every 2 days. The oil content of the volunteers' scalps was tested before use and after 4 weeks of use. The oil content of the scalp before and after use was recorded, and the change rate of scalp oil content before and after use was calculated to determine the oil-controlling effect of the shampoo.

[0074] The instrument used for the test was a skin oil test probe (Sebumeter SM815).

[0075] Change rate of scalp oil content = (scalp oil content after use - scalp oil content before use) / scalp oil content before use × 100%.

[0076] Experimental results: The experimental results are shown in Table 1.

[0077] Table 1 Results of scalp sebum secretion test

[0078] Group Change in scalp oiliness after 4 weeks of use / % Comparison Example 8.4 Example 1 -25.2 Example 2 -24.6 Example 3 -23.5 Example 4 -22.4 Example 5 -23.8 Example 6 -22.1 Example 7 -22.3 Example 8 -21.8 Example 9 -20.9 Example 10 -20.5 Example 11 -24.8 Comparative Example 1 -15.3 Comparative Example 2 -3.2 Comparative Example 3 -14.2 Comparative Example 4 -4.0 Comparative Example 5 -16.6 Comparative Example 6 -3.1 Comparative Example 7 -8.2 Comparative Example 8 -5.8 Comparative Example 9 -16.0 Comparative Example 10 -14.2 Comparative Example 11 -16.1 Comparative Example 12 -18.8 Comparative Example 13 -15.5 Comparative Example 14 -14.9

[0079] As shown in Table 1, the shampoos corresponding to the examples and comparative examples all have scalp oil control effects, with the products from the examples exhibiting better oil control than those from the comparative examples. The shampoo prepared in Example 1 shows the best scalp oil control effect and is therefore the preferred embodiment of this invention. The scalp oil control effect of Example 1 is superior to that of Examples 8 and 9 and Comparative Examples 9 and 10, indicating that the fermentation temperature also affects the fermentation effect, ultimately influencing the scalp oil control effect of the composition. In this invention, the fermentation temperature should be limited to 25-35℃; exceeding this temperature range results in a poorer scalp oil control effect. The scalp oil control effect of Example 1 is superior to that of Examples 2-6, indicating that the mass ratio of black willow bark to Dendrobium nobile stems, as well as the types of carbon and nitrogen sources, affect the fermentation process.

[0080] The scalp oil control effect of Example 1 is better than that of Comparative Examples 1-5, indicating that there is a synergistic effect between black willow bark and Dendrobium nobile stem in the composition of the present invention. The two are fermented together by Aspergillus brasiliensis, and the final composition has a good scalp oil control effect. The scalp oil control effect of the composition prepared by fermentation of a single plant, or by replacing black willow bark with black willow leaves, Dendrobium nobile stem with Dendrobium nobile leaves, or Dendrobium officinale stem, is poor.

[0081] The scalp oil control effect of Example 1 is better than that of Comparative Example 6, indicating that the fermentation strain has an important influence on the fermentation process of the present invention. When brewer's yeast is used for fermentation, the scalp oil control effect of the resulting composition is poor.

[0082] The scalp oil control effect of Example 1 is better than that of Example 7 and Comparative Example 8, indicating that the addition and type of trace elements affect the fermentation process and ultimately the scalp oil control effect of the composition. In this invention, the addition of B vitamins as a fermentation medium results in a composition with better scalp oil control, while the composition without B vitamins has a poorer effect. Adding vitamin A as a trace element further worsens the fermentation effect.

[0083] The scalp oil control effect of Example 1 is better than that of Comparative Examples 9 and 10, indicating that the fermentation temperature also affects the fermentation effect and ultimately affects the scalp oil control effect of the composition. In this invention, the fermentation temperature should be limited to 25-35℃. If the temperature exceeds this range, the scalp oil control effect of the resulting composition will be poor.

[0084] The scalp oil control effect of Example 1 is better than that of Comparative Examples 11 and 12, indicating that the inoculation amount of Aspergillus brasiliensis seed liquid affects the fermentation process. If the inoculation amount is too small, the nutrients in the fermentation medium cannot be effectively utilized, and the amount of oil-controlling, fluffy, and smooth hair active substances in the plant fermentation liquid is small. If the inoculation amount is too large, Aspergillus brasiliensis will multiply too much in the fermentation medium too early, which will easily cause the produced oil-controlling, fluffy, and smooth hair active substances to be consumed by the bacteria themselves, resulting in less active substances produced, thus affecting the scalp oil control effect of the prepared composition.

[0085] The scalp oil control effect of Example 1 is better than that of Comparative Examples 13 and 14. This indicates that when the fermentation time is less than 56 hours, Aspergillus brasiliensis is still in its growth phase, the concentration of Aspergillus brasiliensis in the fermentation broth is low, and many nutrients in the fermentation medium are not utilized or transformed. As a result, the final product contains fewer active substances for oil control, volume, and smooth hair. When the fermentation time is greater than 96 hours, Aspergillus brasiliensis multiplies rapidly, and the bacteria enter the apoptosis phase, making them prone to cell autolysis. The prepared active substances for oil control, volume, and smooth hair will be further consumed, resulting in fewer active substances in the final product, thus affecting the scalp oil control effect of the prepared composition.

[0086] Experimental Example 2: Hair Bundle Fluffiness and Hair Combing Performance Test

[0087] Test samples: Shampoos prepared using the compositions obtained in Examples 1-11 and Comparative Examples 1-14 as active substances, and control group shampoos (the preparation method of the shampoos is referred to the application examples).

[0088] Test Method: A. Hair Bundle Preparation: Prepare 260 hair bundles to be tested (cylindrical hair bundles, specifications: net weight of hair: 8g, length 25cm, 10 hair bundles per test sample). Soak the hair bundles in a 75wt% alcohol solution for 30 minutes, clean them thoroughly, and then soak them in a 3wt% sodium fatty alcohol polyoxyethylene ether sulfate (AES) aqueous solution for 30 minutes. Rinse with tap water while smoothing the hair, wash thoroughly, and hang to air dry at room temperature before use.

[0089] B. Sample Preparation: Gently and evenly apply 1.5 mL of test sample to the upper, middle, and lower sections of the hair strand, rubbing each section 5 times on both sides. Then rinse with tap water while smoothing the hair, rinse thoroughly, and hang the hair strand to air dry at room temperature. Prepare 3 hair strands to be tested following steps A and B, and conduct hair strand fluffiness and combability tests respectively.

[0090] C. Hair Bundle Fluffiness Test: Before using the sample, the unused hair bundles were naturally dried and clipped to the test clips for a dry hair fluffiness test. Each hair bundle was tested 10 times, and the average result was taken. After using the sample, the hair bundles were hung to dry overnight at room temperature, then clipped to the test clips for a dry hair fluffiness test. Each hair bundle was tested 10 times, and the average result was taken. The rate of change in hair bundle fluffiness before and after using the test sample was calculated to evaluate the hair fluffiness effect of the test sample.

[0091] Change rate of hair volume (%) = (hair volume after use - hair volume before use) / hair volume before use × 100%.

[0092] Test instrument: MTT175 hair tester (TressVolumeAccessory accessory).

[0093] D. Wet Hair Combing Performance Test: Before using the sample, comb the unused hair strand to be tested after it has been air-dried, then wet it once and comb it three times in each direction. Then, clip it onto the test clip and perform the wet hair combing performance test. Repeat the test five times, and take the average value. After using the sample, hang the hair strand to air dry at room temperature overnight. Comb the hair strand to be tested, then wet it once and comb it three times in each direction. Then, clip it onto the test clip and perform the wet hair combing performance test. Repeat the test five times, and take the average value. Calculate the rate of change in the wet hair combing performance before and after using the test sample to evaluate the effect of the test sample on hair smoothness.

[0094] The less effort required to comb hair, the easier the hair strands are to comb, meaning the smoother the hair is.

[0095] Change rate of wet hair combing effort (%) = A (wet hair combing effort after use - wet hair combing effort before use) / wet hair combing effort before use × 100%.

[0096] E. Dry hair combing ability test:

[0097] Before using the sample, the unused hair strand was combed smooth, once in each direction, and then clipped to the test clip for a dry hair combing ability test. This test was repeated 5 times, and the average result was taken. After using the sample, the hair strand was hung to dry overnight at room temperature. The hair strand was then combed smooth, once in each direction, and then clipped to the test clip for a dry hair combing ability test. This test was repeated 5 times, and the average result was taken. The rate of change in the dry hair combing ability before and after using the test sample was calculated to evaluate the effect of the test sample on hair smoothness.

[0098] Change rate of dry hair combing effort (%) = (dry hair combing effort after use - dry hair combing effort before use) / dry hair combing effort before use × 100%.

[0099] Experimental results: The experimental results are shown in Table 3.

[0100] Table 3. Test results of hair bundle fluffiness and hair combing performance

[0101] Group Hair volume change rate / % Change rate of wet hair combing performance / % Change rate of dry hair combing performance / % Comparison Example -0.8 -2.6 -0.5 Example 1 32.7 -48.3 -38.6 Example 2 30.4 -45.3 -35.9 Example 3 31.5 -46.8 -37.2 Example 4 29.6 -42.6 -35.5 Example 5 31.0 -44.3 -36.8 Example 6 28.5 -43.8 -34.8 Example 7 27.9 -41.7 -32.6 Example 8 28.1 -38.2 -33.0 Example 9 26.6 -40.5 -34.2 Example 10 26.2 -38.5 -32.3 Example 11 31.6 -46.1 -37.1 Comparative Example 1 14.7 -16.3 -13.4 Comparative Example 2 2.8 -6.5 -2.8 Comparative Example 3 17.2 -17.8 -15.3 Comparative Example 4 4.6 -12.0 -4.2 Comparative Example 5 17.5 -19.2 -15.0 Comparative Example 6 4.4 -3.7 -5.2 Comparative Example 7 18.3 -15.8 -13.8 Comparative Example 8 16.9 -14.2 -12.6 Comparative Example 9 20.7 -27.5 -26.5 Comparative Example 10 16.5 -25.3 -24.2 Comparative Example 11 20.6 -26.8 -23.5 Comparative Example 12 22.4 -30.5 -26.2 Comparative Example 13 23.5 -24.6 -22.5 Comparative Example 14 21.2 -32.1 -26.8

[0102] As shown in Table 2, the shampoos provided in the embodiments and comparative examples of the present invention can all fluff up hair and make it smooth, and the products of the embodiments are more effective than those of the comparative examples. Among them, the shampoo prepared in Example 1 has the best scalp oil control effect and is the preferred embodiment of the present invention.

[0103] The hair volume and combing performance of Example 1 are superior to those of Comparative Examples 1-5, indicating that in the composition of the present invention, the composition obtained by co-fermentation of black willow bark and Dendrobium nobile stem significantly improves the smoothness and volume of hair compared to the composition obtained by fermenting either black willow bark or Dendrobium nobile stem alone. At the same time, the active substances obtained by fermentation of black willow leaves, Dendrobium nobile leaves, and Dendrobium officinale stems do not improve the smoothness and volume of hair as much as those obtained by fermentation of black willow bark and Dendrobium nobile stems alone. That is, black willow leaves, Dendrobium nobile leaves, and Dendrobium officinale stems cannot achieve the technical effect of co-fermentation of black willow bark and Dendrobium nobile stems of the present invention.

[0104] The hair volume and combing performance of Example 1 are better than those of Comparative Example 6, indicating that the fermentation strain has an important influence on the fermentation process of the present invention. When brewer's yeast is used for fermentation, the composition obtained has a poorer effect on improving the volume and smoothness of the hair.

[0105] The hair volume and combing performance of Example 1 were better than those of Comparative Examples 7-14, indicating that the addition and type of trace elements, fermentation temperature, inoculation amount of Aspergillus brasiliensis seed liquid and fermentation time affected the fermentation process, thereby affecting the volume and smoothness of the hair in the prepared shampoo.

[0106] Experiment Example 3: Evaluation of Usage Effect

[0107] Test samples: Shampoos prepared using the compositions obtained in Examples 1-11 and Comparative Examples 1-14 as active substances, and control shampoos;

[0108] Test method: 520 volunteers with oily scalps were selected (20 volunteers used one shampoo). A 2-week wash-out period was set before the test to avoid the influence of the original product depositing on the hair and scalp.

[0109] During the shampooing period, volunteers used unconditioned baby shampoo as a shampooing agent every 2 or 3 days. After the 2-week shampooing period, volunteers used the shampoo provided by this invention, adjusting the amount according to their hair volume and length, once every 2 days. The scalp oil content of volunteers was tested before and 4 weeks after use. Follow-up interviews were conducted before and 4 weeks after use, and volunteers were asked to complete questionnaires. The percentages of volunteers who showed significant effectiveness, effectiveness, and ineffectiveness were statistically analyzed.

[0110] Evaluation results: The evaluation results are shown in Table 3.

[0111] Table 3 Evaluation Results of Usage Effectiveness

[0112]

[0113] As shown in Table 3, the shampoo prepared from the oil-controlling, volumizing, and smoothing hair composition provided by this invention can significantly reduce scalp oil secretion and scalp itching, resulting in volumizing and smoothing hair. However, the shampoos prepared using the compositions obtained in Comparative Examples 1-14 show significantly reduced effectiveness in reducing scalp oil secretion, alleviating scalp itching, and achieving volumizing and smoothing hair.

[0114] The above embodiments are merely illustrative of the preparation method of the present invention and are not intended to limit the invention. Anyone skilled in the art should not modify the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by those skilled in the art without departing from the technical concept provided by the present invention are still covered by the claims of the present invention.

Claims

1. A method for preparing a composition that controls oil, adds volume, and smooths hair, characterized in that, Specifically: Using black willow bark powder, Dendrobium nobile stem powder, carbon source, nitrogen source, trace elements, and water as the fermentation medium, the bacteria were inoculated with Aspergillus brasiliensis (… Aspergillus brasiliensis The BNCC341632 seed liquid was fermented in the fermentation medium to obtain a composition of oil-controlling, fluffy and smooth hair; The method for preparing the oil-controlling, volumizing, and smoothing hair composition includes the following steps: S1. Mix the black willow bark powder, Dendrobium nobile stem powder, carbon source, nitrogen source, trace elements and water evenly, sterilize and cool down to obtain the fermentation culture medium; S2. Inoculate the Aspergillus brasiliensis seed liquid into the fermentation medium prepared in step S1, introduce sterile air, and carry out fermentation to obtain plant fermentation liquid. S3. The plant fermentation liquid obtained in step S2 is subjected to inactivation treatment and filtration treatment to obtain the composition of oil control, fluffy and smooth hair. The inactivation treatment in step S3 is carried out at a temperature of 85-115℃ for 15-30 minutes; the filtration treatment is carried out using a diatomaceous earth filter or a microfiltration membrane. The inoculum size of the Aspergillus brasiliensis seed culture is 1-3% of the mass of the fermentation medium. The concentration of the Aspergillus brasiliensis seed solution is 1×10⁻⁶. 7 -1×10 9 cfu / ml; The trace element is B vitamins, and the amount added is 0.05-0.3% of the mass of the fermentation culture medium.

2. The method for preparing the composition for oil control, volumizing, and smoothing hair according to claim 1, characterized in that, The total amount of black willow bark powder and dendrobium nobile stem powder added is 0.5-2.0% of the mass of the fermentation culture medium, and the mass ratio of black willow bark powder to dendrobium nobile stem powder is 5-9:

1.

3. The method for preparing the composition for oil control, volumizing, and smoothing hair according to claim 1, characterized in that, The fermentation temperature is 25-35℃, the rotation speed is 100-250rpm, and the fermentation time is 56-96h.

4. The method for preparing the composition for oil control, volumizing, and smoothing hair according to claim 1, characterized in that, The carbon source is at least one of dextrin, fructose, sucrose, and glucose; the amount of carbon source added is 0.8-2% of the mass of the fermentation medium; the nitrogen source is at least one of soybean peptone, yeast extract, and cottonseed meal; the amount of nitrogen source added is 0.4-1.8% of the mass of the fermentation medium.

5. The method for preparing the composition for oil control, volumizing, and smoothing hair according to claim 1, characterized in that, The water is added to 100% of the mass of the fermentation medium.

6. The method for preparing the composition for oil control, volumizing, and smoothing hair according to claim 1, characterized in that, The preparation steps of the Aspergillus brasiliensis seed liquid are as follows: Aspergillus brasiliensis colonies are picked up with an inoculation loop and cultured in liquid culture medium. The culture conditions are: temperature 25-35℃, rotation speed 100-300rpm, and culture time 72-120h.

7. The method for preparing the composition for oil control, volumizing, and smoothing hair according to claim 1, characterized in that, The preparation steps of the black willow bark powder are as follows: the dried black willow bark is ground into powder, passed through a 50-120 mesh sieve, and the lower layer of powder is taken out to obtain the black willow bark powder; the preparation steps of the Dendrobium nobile powder are as follows: the dried Dendrobium nobile stem is ground into powder, passed through a 50-120 mesh sieve, and the lower layer of powder is taken out to obtain the Dendrobium nobile stem powder.

8. The composition for controlling oil, volumizing and smoothing hair prepared by the method of preparing the composition for controlling oil, volumizing and smoothing hair according to any one of claims 1-7.

9. The use of the composition for controlling oil, increasing volume and smoothing hair according to claim 8 in the preparation of hair products.

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