An oil control fluffy composition, its preparation method and application

Abstract

The present application belongs to the technical field of cosmetics, and specifically relates to an oil-control and fluffy composition, a preparation method and application thereof. The composition contains, in parts by mass, 4-8 parts of polyquaternary ammonium salt 11, 2-5 parts of octanoyl glycine, 2-8 parts of rhamnolipid and 1-3 parts of an oil-control composition; wherein the oil-control composition is compounded by North American pine cone extract, buckthorn fruit extract and radix codonopsis fermentation extract at a mass ratio of (5-7):1:(2.2-3.6). The present application realizes excellent oil control, bacteriostasis and antioxidant effects by scientific proportioning of specific components and synergistic effect among the components, and can significantly improve hair fluffiness and durability.

Description

Technical Field

[0001] This invention belongs to the technical field of cosmetics, specifically relating to an oil-controlling and fluffy composition, its preparation method, and its application. Background Technology

[0002] With the fast pace of life, changes in dietary structure, and environmental factors, problems such as excessive scalp oil production and scalp microecological imbalance are becoming increasingly common. Excessive scalp oil production is mainly related to overactive sebaceous glands. 5α-reductase can convert testosterone into dihydrotestosterone (DHT), a key substance that stimulates excessive sebum secretion. DHT also damages hair follicles, causing hair to lose support and become flat. Furthermore, the proliferation of harmful bacteria on the scalp surface and increased oxidative stress can also trigger scalp itching and inflammation, further affecting scalp and hair health.

[0003] Currently, most oil-controlling and volumizing hair care products on the market achieve short-term oil control by adding a single oil-controlling ingredient or surfactant. However, these products suffer from drawbacks such as poor oil control longevity, dry scalp, and damage to the scalp barrier. Some products add large amounts of chemical styling agents to achieve a volumizing effect, which can lead to dry, frizzy hair and increased scalp burden with long-term use. Furthermore, the extraction processes of natural active ingredients in existing products are not optimized enough, resulting in low utilization rates of active ingredients. Moreover, the lack of synergistic design when multiple ingredients are combined makes it difficult to simultaneously achieve multiple benefits such as oil control, antibacterial properties, antioxidant effects, and volumizing.

[0004] Therefore, developing a hair care composition based on natural active ingredients, achieving synergistic effects through scientific compounding, possessing excellent oil control and long-lasting properties, antibacterial and antioxidant capabilities, and hair volume enhancement, while being gentle and non-irritating, has become an urgent need in the current hair care product industry. Summary of the Invention

[0005] In view of the shortcomings of the prior art, the purpose of this invention is to provide an oil-controlling and fluffing composition that has excellent oil-controlling, antibacterial, and antioxidant effects as well as a long-lasting fluffy effect, and is gentle and non-irritating with high utilization rate of active ingredients.

[0006] To achieve the above objectives, the present invention discloses the following technical solutions: In a first aspect, the present invention provides an oil-controlling and fluffy composition, wherein, by mass parts, the composition contains the following components: 4-8 parts of polyquaternium salt 11, 2-5 parts of capryloyl glycine, 2-8 parts of rhamnolipid and 1-3 parts of oil-controlling composition; The oil-controlling composition is composed of North American pine cone extract, vitex fruit extract and codonopsis fermented extract in a mass ratio of (5-7):1:(2.2-3.6).

[0007] Preferably, the preparation method of the North American pine cone extract includes the following steps: Step 1.1: Place the dried North American pine cones in a high-speed grinder and grind them. Pass them through a 40-mesh sieve to obtain pine cone powder. Step 1.2: Place pine cone powder in a supercritical CO2 extraction vessel and adjust the extraction parameters: extraction pressure is 25-35 MPa, extraction temperature is 40-50℃, CO2 flow rate is 20-30 L / h per kg of material, and the entrainer is a composite entrainer made of medium-chain triglycerides, camellia seed oil and anhydrous ethanol in a volume ratio of 1:2:5. The pumping rate of the composite entrainer is 20v / v% of the total CO2 fluid flow rate. Dynamic extraction is performed for 2-3 hours. After extraction, the mixture is introduced into a separator through a pressure reducing valve for depressurization separation. The separation pressure is 6-8 MPa and the separation temperature is 50-60℃ to obtain the crude extract. Step 1.3: Transfer the crude extract to a vacuum evaporator and completely remove ethanol under conditions of 50-60℃ and a vacuum degree of ≤-0.09MPa to obtain the active ingredient-rich oil of North American pine cones, which is the North American pine cone extract.

[0008] Preferably, the preparation method of the Codonopsis pilosula fermented extract includes the following steps: Step 2.1: Crush and sieve the dried Codonopsis pilosula to obtain Codonopsis pilosula powder. Mix the Codonopsis pilosula powder with deionized water at a mass-volume ratio of 1:(10-15)g / mL. Stir at 80-90℃ and 100-150r / min for 12-16h to obtain fermentation substrate liquid. Sterilize with high-pressure steam at 121℃ for 15min and cool for later use. Step 2.2: The viable count is 1×10⁻⁶. 8 The concentration of *Schizosaccharomyces cerevisiae* broth at CFU / mL and the viable count was 1×10⁻⁶. 8 A compound yeast solution was obtained by mixing CFU / mL Bereida spp. culture at a volume ratio of 5:3. Step 2.3: Inoculate the compound yeast culture into the fermentation substrate at an inoculation rate of 6-8 v / v%, and ferment at 25-28℃ and 150-200 r / min for 48-60 h. During the fermentation process, the aeration rate is maintained at 1.1-1.3 vvm to obtain the fermentation broth. Step 2.4: Centrifuge the fermentation broth at 5000-8000 r / min to collect the fermentation supernatant. Filter the fermentation supernatant through a 0.22 μm polyethersulfone microporous membrane to remove bacteria. Concentrate the filtrate under reduced pressure to 1 / 3 of its original volume to obtain the Codonopsis pilosula fermentation extract.

[0009] Secondly, the present invention provides the application of the oil-controlling and volumizing composition described in the first aspect in the preparation of hair care products having oil-controlling, antibacterial and / or volumizing effects.

[0010] Preferably, the hair care product is shampoo, hair cream, hair spray, scalp serum, scalp spray, hair mask, or conditioner.

[0011] Thirdly, the present invention provides an oil-controlling and volumizing shampoo, wherein the shampoo contains the composition described in the first aspect.

[0012] Preferably, the shampoo also contains cosmetic-acceptable excipients and solvents.

[0013] More preferably, the excipient is at least one selected from humectants, thickeners, daily fragrances, pH adjusters, chelating agents, surfactants, colorants, and stabilizers; The solvent is deionized water.

[0014] Fourthly, the present invention provides a method for preparing the shampoo described in the third aspect, the method comprising the following steps: The shampoo is obtained by mixing, stirring, homogenizing, dispersing, filtering, and bottling the composition, excipients, and solvent.

[0015] In this invention: As a cationic polymer, polyquaternium 11 has good film-forming and adsorption properties, which can firmly adhere to the hair surface to form a breathable protective film, reducing the damage of the external environment to the hair. At the same time, it can neutralize the negative charge on the hair surface, reduce the electrostatic attraction between hair strands, reduce tangling and adhesion, significantly improve the fluffiness and smoothness of the hair, and has a certain moisturizing property, which can improve the problem of dry and frizzy hair, and enhance the elasticity and support of the hair.

[0016] Capryloyl glycine has both antibacterial and moisturizing effects. It has a significant inhibitory effect on harmful bacteria such as Propionibacterium acnes and Malassezia on the scalp surface, and can regulate the scalp microecological balance, reducing scalp itching and inflammation caused by bacterial growth. At the same time, it can penetrate deep into the stratum corneum of the scalp to replenish and lock in moisture, maintain the water-oil balance of the scalp, relieve the dryness and tightness of the scalp, and is gentle and non-irritating, and has a protective effect on the scalp barrier.

[0017] Rhamnollipids are biosurfactants with excellent emulsifying, dispersing, and cleaning abilities. They can gently remove excess oil and dirt from the scalp without damaging the scalp's sebum film. Their unique molecular structure can reduce the surface tension of hair strands, promote the penetration and absorption of other active ingredients, and also have certain antibacterial and antioxidant activities. They can help regulate the scalp's microecology, reduce oxidative stress damage to the scalp, and enhance the oil control and hair care effects of products.

[0018] The North American pine cone extract is prepared using supercritical CO2 extraction technology combined with a specific composite entrainer. It is enriched with a variety of active ingredients such as terpenes and flavonoids, and has significant 5α-reductase inhibitory activity. It can reduce DHT production at the source and inhibit excessive sebum secretion from the sebaceous glands. At the same time, it has strong antioxidant capacity, which can remove free radicals from the scalp, reduce oxidative damage, protect hair follicle health, and provide a good environment for hair growth.

[0019] Vitex trifolia fruit extract contains active ingredients such as volatile oils, flavonoids, and alkaloids, which have antibacterial, anti-inflammatory, and antioxidant effects. It can inhibit the growth of harmful bacteria on the scalp, reduce scalp inflammation, and relieve scalp itching. At the same time, it can promote scalp blood circulation, provide nutrition to hair follicles, enhance hair toughness, and help improve hair volume and support.

[0020] The fermented extract of Codonopsis pilosula is prepared by a combined fermentation of Schizosaccharomyces cerevisiae and Saccharomyces bereaves, which transforms the polysaccharides, saponins and other components in Codonopsis pilosula into small molecule active substances that are more easily absorbed by the scalp. It has good moisturizing and repairing effects, can repair the damaged scalp barrier and maintain the water-oil balance of the scalp; at the same time, it can regulate scalp metabolism, enhance scalp resistance, and work synergistically with other ingredients to improve the overall oil control and volume effect.

[0021] The beneficial effects of this invention are: 1. This invention achieves a synergistic enhancement of oil control, antibacterial, antioxidant, and fluffing effects by compounding polyquaternium 11, capryloyl glycine, rhamnolipids, and a specific ratio of oil-controlling composition (North American pine cone extract, Vitex trifolia fruit extract, and Codonopsis pilosula fermented extract). Among them, the three extracts of the oil-controlling composition show a significant synergistic effect in inhibiting 5α-reductase activity and scavenging free radicals. Its oil control and antioxidant effects are far superior to those of a single extract, solving the problem of single efficacy and poor synergy of existing products.

[0022] 2. The shampoo provided by the present invention regulates sebum secretion from the source by inhibiting 5α-reductase activity through an oil-control composition. Combined with the mild cleansing effect of rhamnolipid and the antibacterial effect of capryloylglycine, it achieves long-lasting oil control while maintaining the scalp microecological balance. Combined with the film-forming and antistatic effects of polyquaternium 11, it can significantly improve the fluffiness and support of hair. Detailed Implementation

[0023] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to specific embodiments. However, the following embodiments are merely preferred embodiments of this invention and not all of them. For clarity, not all features of the actual embodiments are described.

[0024] Based on the embodiments described in the implementation plan, other embodiments obtained by those skilled in the art without creative effort are all within the protection scope of this invention.

[0025] I. Raw Materials North American pine cones: The dried fruit of the North American pine (Pinus strobus L.) of the Pinaceae family, commercially available; Codonopsis pilosula: The dried root of Codonopsis pilosula, belonging to the genus Codonopsis in the family Campanulaceae, is commercially available. Chestnut wine fissillar: accession number GDMCC 2.64, purchased from Guangdong Provincial Microbial Culture Collection Center; Bereidae: accession number GDMCC 2.66, purchased from Guangdong Provincial Center for Microbial Culture Collection; Vitex trifolia fruit extract: Vitex trifolia fruit extract, purchased from Langlin Bioresources Co., Ltd.; Medium-chain triglycerides: purchased from Wuhan Qiaofeng Chemical Technology Co., Ltd.; All raw materials used in the other embodiments are commercially available.

[0026] II. North American pine cone extract The preparation method of the North American pine cone extract is as follows: Step 1: Place the dried North American pine cones in a high-speed grinder and grind them. Pass them through a 40-mesh sieve to obtain pine cone powder. Step 2: Place 1 kg of pine cone powder into a supercritical CO2 extraction vessel and adjust the extraction parameters as follows: extraction pressure is 28 MPa, extraction temperature is 46℃, CO2 flow rate is 22 L / h, and the entrainer is a composite entrainer made of medium-chain triglycerides, camellia seed oil and anhydrous ethanol in a volume ratio of 1:2:5. The pumping rate of the composite entrainer is 20 v / v% of the total CO2 fluid flow rate. Dynamic extraction is performed for 3 h. After extraction, the mixture is introduced into a separator through a pressure reducing valve for pressure reduction separation. The separation pressure is 6 MPa and the separation temperature is 50℃ to obtain the crude extract. Step 3: Transfer the crude extract to a vacuum evaporator and completely remove ethanol under conditions of 50°C and a vacuum degree of ≤-0.09MPa to obtain the active ingredient-rich oil of North American pine cones, which is the North American pine cone extract.

[0027] III. Codonopsis pilosula fermented extract The preparation method of the Codonopsis pilosula fermentation extract is as follows: Step 1: Crush and sieve the dried Codonopsis pilosula to obtain Codonopsis pilosula powder. Mix the Codonopsis pilosula powder with deionized water at a mass-volume ratio of 1:15 g / mL. Stir at 80-90℃ and 100-150 r / min for 12-16 h to obtain fermentation substrate liquid. Sterilize at 121℃ with high pressure steam for 15 min and cool for later use. Step 2: The viable count is 1×10⁻⁶ 8 The concentration of *Schizosaccharomyces cerevisiae* broth at CFU / mL and the viable count was 1×10⁻⁶. 8 A compound yeast solution was obtained by mixing CFU / mL Bereida spp. culture at a volume ratio of 5:3. Step 3: Inoculate the compound yeast culture into the fermentation substrate at an inoculation rate of 6-8 v / v%, and ferment at 28℃ and 150-200 r / min for 60 h. During the fermentation process, the aeration rate is maintained at 1.1-1.3 vvm to obtain the fermentation broth. Step 4: Centrifuge the fermentation broth at 5000 r / min to collect the fermentation supernatant. Filter the fermentation supernatant through a 0.22 μm polyethersulfone microporous membrane to remove bacteria. Concentrate the filtrate under reduced pressure to 1 / 3 of its original volume to obtain the Codonopsis pilosula fermentation extract.

[0028] IV. Oil-controlling composition 1. Composition 1-3 According to the raw material mass ratio in Table 1, compounding was performed to obtain composition 1-3; Table 1. Mass ratio of raw materials for compositions 1-3 North American pine cone extract 5 6 7 Vitex fruit extract 1 1 1 Codonopsis pilosula fermented extract 2.2 3 3.6 2. Composition 4-6 According to the raw material mass ratio in Table 2, compounding was performed to obtain composition 4-6; Table 2. Mass ratio of raw materials for composition 4-6 North American pine cone extract / 6 6 Vitex fruit extract 1 / 1 Codonopsis pilosula fermented extract 3 3 / Note: " / " in the table indicates no addition.

[0029] 3. Composition 7-9 Composition 7: Based on composition 2, the difference from composition 2 is that the North American pine cone extract is replaced with North American pine cone extract①, thus obtaining composition 7; The preparation method of the North American pine cone extract ① is the same as that of the North American pine cone extract, except that the medium-chain triglycerides in the composite entrainer in step 2 are replaced with soybean oil, while the rest remain unchanged, to obtain the North American pine cone extract ①.

[0030] Composition 8: Based on composition 2, the difference from composition 2 is that the North American pine cone extract is replaced with North American pine cone extract ②, thus obtaining composition 8; The preparation method of the North American pine cone extract ② is the same as that of the North American pine cone extract, except that the camellia seed oil in the composite entrainer in step 2 is replaced with soybean oil, while the rest remains unchanged, to obtain the North American pine cone extract ②.

[0031] Composition 9: Based on composition 2, the difference from composition 2 is that the North American pine cone extract is replaced with North American pine cone extract ③, thus obtaining composition 9; The preparation method of the North American pine cone extract ③ is the same as that of the North American pine cone extract, except that the volume ratio of medium-chain triglycerides, camellia seed oil and anhydrous ethanol in the composite entrainer in step 2 is adjusted to 2:1:5, while the rest remain unchanged, to obtain the North American pine cone extract ③.

[0032] See Table 3 for details.

[0033] Table 3. Mass ratio of raw materials for composition 7-9 North American pine cone extract① 6 / / North American pine cone extract ② / 6 / North American pine cone extract ③ / / 6 Vitex fruit extract 1 1 1 Codonopsis pilosula fermented extract 3 3 3 Note: " / " in the table indicates no addition.

[0034] 4. Composition 10-13 Composition 10: Based on composition 2, the difference from composition 2 is that the fermented extract of Codonopsis pilosula is replaced with fermented extract of Codonopsis pilosula ①, thus obtaining composition 10; The preparation method of the Codonopsis pilosula fermented extract ① is the same as that of the Codonopsis pilosula fermented extract, except that the compound yeast liquid in step 2 is changed to a separate chestnut wine fissilla yeast liquid, while the rest remains unchanged, thus obtaining the Codonopsis pilosula fermented extract ①.

[0035] Composition 11: Based on composition 2, the difference from composition 2 is that the fermented extract of Codonopsis pilosula is replaced with fermented extract of Codonopsis pilosula ②, thus obtaining composition 11; The preparation method of the Codonopsis pilosula fermented extract ② is the same as that of the Codonopsis pilosula fermented extract, except that the compound yeast liquid in step 2 is changed to a single Bereida spp. yeast liquid, while the rest remains unchanged, to obtain the Codonopsis pilosula fermented extract ②.

[0036] Composition 12: Based on composition 2, the difference from composition 2 is that the fermented extract of Codonopsis pilosula is replaced with fermented extract of Codonopsis pilosula ③, thus obtaining composition 12; The preparation method of the Codonopsis pilosula fermented extract ③ is the same as that of the preparation method of Codonopsis pilosula fermented extract, except that the Saccharomyces cerevisiae in the compound yeast liquid in step 2 is replaced with Saccharomyces cerevisiae (GDMCC 2.182, purchased from Guangdong Provincial Microbial Culture Collection Center), and the rest remains unchanged, thus obtaining Codonopsis pilosula fermented extract ③.

[0037] Composition 13: Based on composition 2, the difference from composition 2 is that the fermented extract of Codonopsis pilosula is replaced with fermented extract of Codonopsis pilosula ④, thus obtaining composition 13; The preparation method of the Codonopsis pilosula fermented extract ④ is the same as that of the Codonopsis pilosula fermented extract, except that the volume ratio of Schizosaccharomyces cerevisiae liquid and Saccharomyces bereaves liquid in the compound yeast liquid in step 2 is adjusted to 3:5, while the rest remains unchanged, thus obtaining the Codonopsis pilosula fermented extract ④.

[0038] V. Performance Testing 1. Oil control test 1.1 Test Principle Based on the fact that 5α-reductase can convert testosterone (T) into dihydrotestosterone (DHT), and DHT is a key factor leading to excessive scalp oil and hair follicle atrophy, the oil-controlling efficacy of the composition was evaluated by detecting its inhibitory effect on 5α-reductase activity.

[0039] 1.2 Test Materials and Instruments: Reagents: Female SD rat liver (for preparation of crude 5α-reductase extract), testosterone (T), reduced nicotinamide adenine dinucleotide phosphate (NADPH), phosphate buffer (0.1 mol / L, pH 5.5), methanol (pre-cooled), finasteride (positive control), and compositions 1-13 (test samples). All reagents were of analytical grade.

[0040] Instruments: High-speed centrifuge, carbon dioxide incubator, full-wavelength microplate reader, constant temperature water bath, sterile operating table.

[0041] Test sample preparation: Dissolve compositions 1-13 in anhydrous ethanol to prepare 0.1 wt% test solutions; prepare the positive control finasteride with anhydrous ethanol to a concentration of 80 μg / mL; and prepare the blank control group with anhydrous ethanol.

[0042] 1.3 Test Procedure: Preparation of crude 5α-reductase extract: Under sterile conditions, livers of female SD rats were taken, connective tissue was removed, and the livers were sliced. Five volumes of tissue extraction enzyme buffer were added, and the supernatant was collected after repeated differential centrifugation. This was the crude 5α-reductase extract, which was stored at -80°C with 10% glycerol for later use. The protein content was determined by the Coomassie brilliant blue method.

[0043] Enzyme reaction system construction: Add reagents to centrifuge tubes in the following order, with a total volume of 1 mL: 300 μL phosphate buffer, 500 μL crude 5α-reductase extract (1.5 mg / mL), 50 μL testosterone solution (1 mmol / L), 50 μL test solution (or positive control solution, blank control solution), and 100 μL NADPH solution (1 mmol / L).

[0044] Incubation and termination of reaction: Place the centrifuge tube in a 37°C water bath for 60 min, and add 1 mL of pre-cooled methanol to terminate the reaction.

[0045] Absorbance measurement: Centrifuge at 4000 r / min for 10 min, collect the supernatant, and measure the absorbance values ​​of the blank control group, positive control group, and each test group at 242 nm. Record the absorbance (CA0, CA2) at 0 min and 60 min respectively. 60 ), calculate ΔCT=CA 60 -CA0.

[0046] Inhibition rate calculation: The inhibition rate of each composition against 5α-reductase was calculated using the following formula: .

[0047] Results evaluation: The higher the inhibition rate, the stronger the inhibitory effect of the composition on 5α-reductase and the better the oil control effect.

[0048] 1.4 Test Results The results of 5α-reductase inhibition rate are shown in Table 4; Table 4 Results of 5α-reductase inhibition rate in each group Positive control 62.41 Composition 1 51.23 Composition 2 54.78 Composition 3 53.19 Composition 4 34.51 Composition 5 36.14 Composition 6 32.63 Composition 7 39.22 Composition 8 38.47 Composition 9 40.05 Composition 10 35.37 Composition 11 36.24 Composition 12 34.53 Composition 13 38.92 1.5 Results Analysis As shown in Table 4, the 5α-reductase inhibition rate of the positive control (finasteride) was 62.41%. The inhibition rates of compositions 1-3 (compound extracts of North American pine cones, Vitex trifolia fruit extract, and Codonopsis pilosula fermented extract in a specific ratio) were 51.23%, 54.78%, and 53.19%, respectively, all significantly higher than those of compositions 4-6 (binary compound system lacking any one extract). Among them, composition 2 had the highest inhibition rate, indicating that when the three extracts were compounded in a mass ratio of (5-7):1:(2.2-3.6), they had a significant synergistic effect in inhibiting 5α-reductase activity. The absence of any one component would lead to a significant decrease in the oil-controlling effect.

[0049] The North American pine cone extracts prepared by compositions 7-9 using different composite entrainers all showed lower inhibition rates than composition 2, indicating that the composite entrainer composed of medium-chain triglycerides, camellia seed oil, and anhydrous ethanol in a volume ratio of 1:2:5 can extract the active ingredients in North American pine cones more efficiently. Replacing the entrainer components or adjusting the ratio will reduce the oil-controlling activity of the extract.

[0050] The Codonopsis pilosula fermented extracts prepared by different yeasts in compositions 10-13 showed lower inhibition rates (35.37%, 36.24%, 34.53%, and 38.92%) than those in composition 2. This indicates that the compound yeast liquid, which is a mixture of Schizosaccharomyces cerevisiae and Saccharomyces bereaves in a volume ratio of 5:3, can more fully convert the active ingredients in Codonopsis pilosula. Fermentation with a single yeast or changing the type and ratio of yeast will affect the synergistic oil-controlling effect of the extract.

[0051] 2. Antioxidant test 2.1 Test Principle DPPH free radicals have a characteristic absorption peak at 517 nm. When the antioxidant components in the composition bind to DPPH free radicals, the intensity of the absorption peak decreases. The scavenging rate is calculated by the change in absorbance to evaluate the antioxidant capacity.

[0052] 2.2 Test Materials and Instruments Reagents: DPPH (1,1-diphenyl-2-trinitrophenylhydrazine), anhydrous ethanol, vitamin C (Vc, positive control), and composition 1-13 (test samples). All reagents were of analytical grade.

[0053] Instruments: Full-wavelength microplate reader, pipettes, volumetric flasks, and light-proof centrifuge tubes.

[0054] Test sample preparation: Dissolve compositions 1-13 in anhydrous ethanol to prepare 0.5 wt% test solutions; prepare a 0.5 wt% solution of positive control vitamin C in anhydrous ethanol; and prepare anhydrous ethanol as the blank control group.

[0055] 2.3 Test Procedure: Preparation of DPPH solution: Prepare a 0.1 mmol / L DPPH solution with anhydrous ethanol and store it in the dark and refrigerated for later use.

[0056] Reaction system construction: Take 1.0 mL of test solution (or positive control solution, blank control solution) and place it in a light-protected centrifuge tube. Add 1.0 mL of DPPH solution, shake well, and let stand at room temperature in the dark for 30 min.

[0057] Reference system setup: Take another 1.0 mL of test solution (or positive control solution, blank control solution), add 1.0 mL of anhydrous ethanol, shake well, and let stand at room temperature in the dark for 30 min to serve as the reference system.

[0058] Absorbance measurement: Using anhydrous ethanol as a blank control, the absorbance values ​​of each reaction system (A2) and the reference system (A1) were measured at 517 nm; at the same time, the absorbance (A0) of the mixture of 1.0 mL anhydrous ethanol and 1.0 mL DPPH solution was measured.

[0059] Scavenging rate calculation: The scavenging rate of each composition against DPPH free radicals is calculated using the following formula: .

[0060] Results evaluation: The higher the clearance rate, the stronger the antioxidant activity of the composition, which can effectively reduce oxidative stress damage to the scalp and help improve scalp health.

[0061] 2.4 Test Results The DPPH free radical scavenging results are shown in Table 5; Table 5 DPPH free radical scavenging rate of each group Positive control group 97.72 Composition 1 78.25 Composition 2 80.44 Composition 3 77.03 Composition 4 67.35 Composition 5 70.49 Composition 6 62.48 Composition 7 73.94 Composition 8 75.31 Composition 9 76.89 Composition 10 75.33 Composition 11 74.25 Composition 12 79.17 Composition 13 77.62 2.5 Results Analysis As shown in Table 5, the DPPH free radical scavenging rate of the positive control (vitamin C) was 97.72%. The scavenging rates of compositions 1-3 of the present invention were 78.25%, 80.44%, and 77.03%, respectively, all higher than those of compositions 4-6. This further demonstrates that the three extracts, when combined, have a synergistic antioxidant effect, can more efficiently scavenge free radicals, and reduce oxidative stress damage to the scalp. Among them, composition 2 had the highest DPPH free radical scavenging rate, consistent with the oil control test results, indicating that the composition at this ratio can achieve the best synergistic effect in both oil control and antioxidant properties, and can comprehensively protect scalp health.

[0062] 6. Oil-controlling and volumizing shampoo The preparation method of the shampoo is as follows: Step 1: Add the prescribed amount of deionized water to the mixing tank. Add disodium EDTA, butanediol, and glycerol in sequence at a stirring speed of 300-400 r / min. Stir until completely dissolved. Slowly add carbomer and continue stirring until the carbomer is completely dispersed. Heat to 75-80℃ and keep warm while stirring for 10 min. Step 2: Adjust the temperature and speed to 55-60℃ and 250-300r / min, add rhamnolipid, capryloyl glycine, 1,2-hexanediol and p-hydroxyacetophenone in sequence, stir until completely dissolved, cool to 45-50℃, add oil-controlling composition 2, sodium hyaluronate and polyquaternium salt 11, stir for 20min, turn on the homogenizer, homogenize at 8000-10000r / min for 25min to improve the fineness and stability of the system; Step 3: Continue cooling to 38-40℃, add daily fragrance and coloring agent, stir at 300-500r / min until the system has uniform color and aroma, adjust the pH value of the system to 5.5-6.5 with pH adjuster, filter the liquid with 200 mesh nylon filter cloth, defoam, and then aseptically bottle and seal the package to obtain the oil-controlling and fluffy shampoo.

[0063] The amount of raw materials added in the above preparation method is detailed in Table 6.

[0064] Table 6 Shampoo Ingredients and Additive Amounts Polyquaternium 11 4 6 8 Capryloylglycine 2 3.5 5 rhamnolipid 2 5 8 Oil-control composition 2 1 2 3 glycerin 3 3 3 1,2-Hexanediol 1.2 1.2 1.2 Butylene glycol 2 2 2 Carbomer 0.3 0.3 0.3 Sodium hyaluronate 0.2 0.2 0.2 p-Hydroxyacetophenone 0.1 0.1 0.1 pH adjuster Appropriate amount Appropriate amount Appropriate amount Daily Fragrances Appropriate amount Appropriate amount Appropriate amount Colorant Appropriate amount Appropriate amount Appropriate amount Disodium EDTA 0.04 0.04 0.04 Deionized water Add to 100 Add to 100 Add to 100 VII. Efficacy Testing 1. Volunteer Recruitment Recruitment criteria: 20 male volunteers aged 23-40; scalp type of normal to oily, meeting the criteria of "obvious scalp oiliness and hair strands easily becoming flat and sticky 1-2 days after washing"; no history of scalp inflammation, allergies, or hair loss; no use of oil-control / volumizing hair care products within 1 month prior to the test, and agree to discontinue use of other functional hair care products during the test period.

[0065] 2. Test Samples and Grouping Test samples: The shampoo of Example 2 and a commercially available brand of oil-control shampoo (excluding polyquaternium 11 and rhamnolipid, as well as the ingredients in the oil-control composition).

[0066] Grouping method: Volunteers were randomly divided into two groups of 10 each, and used the shampoo in Example 2 and a commercially available brand of oil-control shampoo respectively.

[0067] 4. Testing methods and cycle Pretreatment: 24 hours before the test, all volunteers used a basic shampoo without silicone oil or oil-controlling ingredients to wash their hair, patted it dry with the same towel, and then let it air dry naturally. The hair was then placed in a constant temperature and humidity environment (temperature 25±2℃, humidity 50±5%) for 24 hours.

[0068] Frequency of use: Wash your hair every two days, following your usual shampooing routine (take the same amount of sample, lather it up, massage your scalp for 1-2 minutes, and rinse with 38±2℃ water until there is no residue), and continue to use for 4 weeks.

[0069] Data recording: After the test (4 weeks later), volunteers filled out an efficacy evaluation questionnaire, the scores of each group's evaluation dimensions were calculated, and the average value was taken.

[0070] 5. Evaluation Dimensions and Standards A 10-point scoring system is used, with specific dimensions as shown in Table 7: Table 7 Evaluation Criteria Scalp refreshment 10 points: Scalp feels dry and not oily from the time of washing until the next washing; 0 points: Scalp becomes oily and sticky shortly after washing, sticking to the scalp. Oily and sticky hair 10 points: Hair is not sticky and each strand is distinct from the next wash; 0 points: Hair is severely sticky and clump-like, lacking volume. Dry hair volume 10 points: After drying, the hair strands are full and voluminous, with clear support at the roots and strong layering; 0 points: After drying, the hair strands are flat and lie tightly against the scalp without any gaps. Fluffy and durable 10 points: Hair retains good volume after washing and before the next wash; 0 points: Hair becomes completely flat within one day after washing. Flushing smoothness 10 points: No dryness after rinsing, hair is smooth and easy to comb; 0 points: Hair is tangled, dry and difficult to rinse clean. Itching rate 10 points: No scalp itching or stinging during use; 0 points: Frequent itching after use, requiring scratching. 6. Scoring Results The results of the volunteers' subjective ratings are shown in Table 8; Table 8 Scoring Results Scalp refreshment 8.2 6.3 Oily and sticky hair 7.5 5.1 Dry hair volume 8.3 6.5 Fluffy and durable 7.6 5.8 Flushing smoothness 7.8 4.5 Itching rate 8.0 7.2 7. Results Analysis: As shown in Table 8, the experimental group using the shampoo of Example 2 scored higher than the group using a commercially available brand of oil-control shampoo in all evaluation dimensions. This indicates that the oil-control and volumizing shampoo of the present invention exhibits excellent comprehensive efficacy in actual use. It can not only achieve long-lasting oil control and volumizing, but also improve scalp health and enhance user comfort, showing significant advantages over similar products on the market.

[0071] Finally, it should be noted that the above descriptions are merely preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A composition for controlling oil and creating a fluffy texture, characterized in that, The composition contains the following components in parts by weight: 4-8 parts of polyquaternium salt 11, 2-5 parts of capryloyl glycine, 2-8 parts of rhamnolipid and 1-3 parts of oil-controlling composition; The oil-controlling composition is composed of North American pine cone extract, vitex fruit extract and codonopsis fermented extract in a mass ratio of (5-7):1:(2.2-3.6); The preparation method of the North American pine cone extract includes the following steps: Step 1.1: Place the dried North American pine cones in a high-speed grinder and grind them. Pass them through a 40-mesh sieve to obtain pine cone powder. Step 1.2: Place pine cone powder in a supercritical CO2 extraction vessel and adjust the extraction parameters: extraction pressure is 25-35 MPa, extraction temperature is 40-50℃, CO2 flow rate is 20-30 L / h per kg of material, and the entrainer is a composite entrainer made of medium-chain triglycerides, camellia seed oil and anhydrous ethanol in a volume ratio of 1:2:

5. The pumping rate of the composite entrainer is 20v / v% of the total CO2 fluid flow rate. Dynamic extraction is performed for 2-3 hours. After extraction, the mixture is introduced into a separator through a pressure reducing valve for depressurization separation. The separation pressure is 6-8 MPa and the separation temperature is 50-60℃ to obtain the crude extract. Step 1.3: Transfer the crude extract to a vacuum evaporator and completely remove ethanol under conditions of 50-60℃ and a vacuum degree of ≤-0.09MPa to obtain the active ingredient-rich oil of North American pine cones, which is the North American pine cone extract. The preparation method of the Codonopsis pilosula fermented extract includes the following steps: Step 2.1: Crush and sieve the dried Codonopsis pilosula to obtain Codonopsis pilosula powder. Mix the Codonopsis pilosula powder with deionized water at a mass-volume ratio of 1:(10-15)g / mL. Stir at 80-90℃ and 100-150r / min for 12-16h to obtain fermentation substrate liquid. Sterilize with high-pressure steam at 121℃ for 15min and cool for later use. Step 2.2: The viable count is 1×10⁻⁶. 8 The concentration of *Schizosaccharomyces cerevisiae* broth at CFU / mL and the viable count was 1×10⁻⁶. 8 A compound yeast solution was obtained by mixing CFU / mL Bereida spp. culture at a volume ratio of 5:

3. Step 2.3: Inoculate the compound yeast culture into the fermentation substrate at an inoculation rate of 6-8 v / v%, and ferment at 25-28℃ and 150-200 r / min for 48-60 h. During the fermentation process, the aeration rate is maintained at 1.1-1.3 vvm to obtain the fermentation broth. Step 2.4: Centrifuge the fermentation broth at 5000-8000 r / min to collect the fermentation supernatant. Filter the fermentation supernatant through a 0.22 μm polyethersulfone microporous membrane to remove bacteria. Concentrate the filtrate under reduced pressure to 1 / 3 of its original volume to obtain the Codonopsis pilosula fermentation extract.

2. The use of the oil-controlling and volumizing composition of claim 1 in the preparation of hair care products having oil-controlling and / or volumizing effects.

3. The application according to claim 2, characterized in that, The hair care products mentioned are shampoos, hair creams, hair sprays, scalp serums, scalp sprays, hair masks, or conditioners.

4. A shampoo for controlling oil and adding volume, characterized in that, The shampoo contains the composition of claim 1.

5. The shampoo according to claim 4, characterized in that, The shampoo also contains cosmetic-grade excipients and solvents.

6. The shampoo according to claim 5, characterized in that, The excipients are at least one of the following: humectant, thickener, daily fragrance, pH adjuster, chelating agent, surfactant, colorant, and stabilizer. The solvent is deionized water.

7. The method for preparing shampoo according to claim 6, characterized in that, The preparation method includes the following steps: The shampoo is obtained by mixing, stirring, homogenizing, dispersing, filtering, and bottling the composition, excipients, and solvent.