Composite acid gel composition as well as preparation method and application thereof

Abstract

The invention belongs to the technical field of hair care products, and particularly relates to a composite acid gel composition as well as a preparation method and application thereof. The composite acid gel composition disclosed by the invention is prepared from the following components in parts by mass: 1.5 to 2.5 parts of capryloyl salicylic acid, 3.5 to 5 parts of glycolic acid, 0.8 to 1 part of arbutin, 0.05 to 0.1 part of piroctone olamine salt, 8 to 12 parts of a lotus-bacillus subtilis fermentation product, 5 to 6 parts of an emulsifying agent and 70 to 80 parts of water, the arbutin is prepared from alpha-arbutin and beta-arbutin. After capryloyl salicylic acid, glycolic acid, arbutin and a lotus-bacillus subtilis fermentation product are compounded, the composition can go deep into hair follicle sebaceous gland, dredge blocked pores and improve scalp folliculitis; the traditional Chinese medicine composition can effectively treat hair follicle deep blockage, accelerate old and waste cutin shedding, not only can solve the root problem of hair follicle deep blockage, but also can realize surface cutin renewal, and a product prepared from the traditional Chinese medicine composition is green, safe, mild and non-irritant, and can efficiently relieve scalp inflammation and inhibit dandruff.

Description

Technical Field

[0001] This invention belongs to the technical field of hair care products, specifically relating to a composite acid gel composition, its preparation method, and its application. Background Technology

[0002] With increasing life pressure, scalp inflammation is not only highly prevalent but also showing a serious trend of affecting younger people. It is strongly associated with common problems such as hair loss and dandruff. In addition, with the upgrading of consumer demand and stricter policy supervision, scalp care products that relieve scalp inflammation have become a research hotspot in this field.

[0003] There are existing reports on acidic washing and care products in the current technology. For example, Chinese Patent CN 112294708 A describes a weakly acidic shampoo and conditioner active agent, which mixes the following components in parts by weight: 20-30 parts of Polygonum multiflorum, 20-30 parts of Artemisia annua, 8-10 parts of Artemisia argyi, 10-20 parts of maple leaves, 8-10 parts of Angelica sinensis, 8-10 parts of Piper longum, 8-10 parts of dried tangerine peel, 6-8 parts of Smilax china, 6-8 parts of dandelion, 6-8 parts of pine needles, 6-8 parts of cypress branches, 6-8 parts of tea seed cake, 6-8 parts of lemongrass, 6-8 parts of ginger, 6-8 parts of black sesame, 6-8 parts of black beans, 6-8 parts of raw papaya, 6-8 parts of star anise, 6-8 parts of cloves, 6-8 parts of hand-washing fruit, and 10-20 parts of compound bacteria. The resulting composition not only promotes the full separation and extraction of active ingredients but also enhances or produces new effects, repairing hair quality. Another example is Chinese Patent CN 117257665. A method for preparing an oil-removing and dandruff-reducing shampoo includes an anti-dandruff agent and an oil-removing agent. The anti-dandruff agent is prepared by mixing an anionic composite gel and a dihydromyricetin derivative. The oil-removing agent includes a composite extract, anionic surfactant, and salicylic acid. The anionic composite gel is prepared by reacting a composite gel with 3-chloro-2-hydroxypropyltrimethylammonium chloride. The composite gel includes flaxseed gum and konjac gum. The dihydromyricetin derivative is prepared by introducing a triazole sulfonate group onto dihydromyricetin. However, the above methods or raw materials are numerous, and different raw materials have different stimulating targets, which may disrupt the balance of the composition and hinder the product from exerting a positive effect. Summary of the Invention

[0004] The purpose of this invention is to provide a composite acid gel composition, its preparation method, and its application. This composition is green, safe, mild, and non-irritating, and can effectively relieve scalp inflammation and inhibit dandruff.

[0005] This invention provides a composite acid gel composition, which, by weight parts, comprises the following components: 1.5-2.5 parts of capryloyl salicylic acid, 3.5-5 parts of glycolic acid, 0.8-1 parts of arbutin, 0.05-0.1 parts of piroctone olamine salt, 8-12 parts of lotus-Bacillus subtilis fermentation product, 5-6 parts of emulsifier, and 70-80 parts of water; The arbutin includes α-arbutin and β-arbutin.

[0006] Preferably, the mass ratio of α-arbutin to β-arbutin in the arbutin is 1:0.1-0.5.

[0007] Preferably, the composite acid gel composition comprises the following components in parts by weight: 2 parts capryloyl salicylic acid, 4 parts glycolic acid, 1 part arbutin, 0.08 parts piroctone olamine salt, 10 parts lotus-Bacillus subtilis fermentation product, 5 parts emulsifier and 70 parts water. In the arbutin, the mass ratio of α-arbutin to β-arbutin is 1:0.2.

[0008] Preferably, the method for preparing the lotus-Bacillus subtilis fermentation product includes: Lotus flower samples, fructose, Bacillus subtilis and water were mixed and aerobic fermented to obtain fermentation broth; The fermentation broth was subjected to enzymatic hydrolysis, enzyme inactivation, solid-liquid separation, and concentration and drying with a compound enzyme to obtain the lotus-Bacillus subtilis fermentation product. The complex enzyme includes: flavor protease and cellulase.

[0009] Preferably, the lotus sample includes any one of the following (1)-(3): (1) White lotus flowers and / or leaves; (2) Yellow lotus flowers and / or leaves; (3) The flowers and / or leaves of the red lotus.

[0010] Preferably, the mass ratio of the lotus sample, fructose, Bacillus subtilis, and water is 10:0.02-0.05:0.3-0.6:80-90; The effective viable count of Bacillus subtilis is ≥1×10⁻⁶. 8 cfu / g; The aerobic fermentation time is 36-48 hours, and the temperature is 38-40℃.

[0011] Preferably, the mass ratio of the fermentation broth to the compound enzyme is 100:1-3; In the complex enzyme, the mass ratio of flavor protease to cellulase is 0.06-1:1; The enzymatic hydrolysis is performed at a temperature of 45-50℃ for 6-12 hours.

[0012] This invention provides a method for preparing the composite acid gel composition described above, comprising the following steps: Capryloyl salicylic acid, glycolic acid, arbutin, piroctone ketone ethanolamine salt, emulsifier, water, and lotus-Bacillus subtilis fermentation product were mixed evenly to obtain a composite acid gel composition.

[0013] This invention provides the application of the composite acid gel composition described above in the preparation of personal care products.

[0014] The present invention provides a shampoo comprising: the composite acid gel composition described in the above technical solution.

[0015] Beneficial effects: This invention provides a composite acid gel composition, which, by weight parts, comprises the following components: 1.5-2.5 parts of capryloyl salicylic acid, 3.5-5 parts of glycolic acid, 0.8-1 parts of arbutin, 0.05-0.1 parts of piroctone olamine salt, 8-12 parts of lotus-Bacillus subtilis fermentation product, 5-6 parts of emulsifier, and 70-80 parts of water; wherein the arbutin comprises α-arbutin and β-arbutin.

[0016] Compared with the prior art, the advantages of the present invention include: The composite acid gel composition provided by this invention contains capryloyl salicylic acid, glycolic acid, and arbutin. The three compounds can penetrate deep into the hair follicle sebaceous glands, unclog pores, and improve scalp folliculitis. At the same time, the composition does not easily penetrate into the dermis, has low irritation, and can accelerate the shedding of dead skin cells after acting on the stratum corneum. It can not only solve the root cause of deep hair follicle blockage, but also achieve surface keratin renewal, with good results.

[0017] In addition, the composite acid gel composition of the present invention also contains lotus-Bacillus subtilis fermentation products, in which the effective active ingredients have high bioavailability and can synergistically exert antioxidant and immunomodulatory effects with capryloyl salicylic acid, glycolic acid and arbutin. Moreover, the products prepared in this way are green, safe, mild and non-irritating. Detailed Implementation

[0018] Unless otherwise specified, all reagents and equipment used in this invention are conventionally purchased.

[0019] The lotus sample of the present invention preferably includes: lotus flowers and / or leaves; when the lotus sample is composed of lotus flowers and leaves, there are no special requirements for the amount of flowers and leaves used, as long as the total amount meets the sample requirements.

[0020] To further illustrate the present invention, the solutions provided by the present invention will be described in detail below with reference to the embodiments, but they should not be construed as limiting the scope of protection of the present invention.

[0021] Example 1 The steps for preparing a composite acid gel composition are as follows: (1) Preparation of lotus-Bacillus subtilis fermentation products White lotus flowers (specifically, Ice Heart Lotus flowers) Nelumbo nucifera The petals of 'Bingxin' were cleaned, dried, and crushed to obtain a lotus flower sample; Lotus flower samples, fructose, and Bacillus subtilis ( Bacillus subtilis The effective viable bacteria count is 1×10⁻⁶. 8 CFU / g) and water were mixed evenly at a mass ratio of 10:0.02:0.3:90 and fermented aerobically at 40℃ for 48 hours to obtain fermentation broth; The fermentation broth and the compound enzyme (in which the mass ratio of flavor protease to cellulase is 0.06:1) were mixed at a mass ratio of 100:1 and enzymatically hydrolyzed at 45℃ for 12 hours. The hydrolysate was then subjected to enzyme inactivation and solid-liquid separation to obtain the supernatant. The supernatant was then concentrated and dried (until the mass of the substance no longer changed) to obtain the lotus-Bacillus subtilis fermentation product.

[0022] (2) Preparation of composite acid gel composition The composite acid gel composition comprises, by weight parts, the following components: 2 parts capryloyl salicylic acid, 4 parts glycolic acid, 1 part arbutin, 0.08 parts piroctone olamine salt, 10 parts lotus-Bacillus subtilis fermentation product, 5 parts alkyl glycoside, and 70 parts water. In the arbutin, the mass ratio of α-arbutin to β-arbutin is 1:0.2.

[0023] At 60°C, capryloyl salicylic acid, glycolic acid, arbutin, piroctone olamine salt, alkyl glycoside and water are mixed evenly. After the mixture is cooled to 35-38°C, lotus-Bacillus subtilis fermentation product is added and mixed evenly to obtain a composite acid gel composition.

[0024] Example 2 The only difference from Example 1 is that the white lotus flowers in Example 1 are replaced with yellow lotus flowers; The yellow lotus is the Ice Beauty Lotus ( Nelumbo 'Bing Jiao').

[0025] Example 3 The only difference from Example 1 is that the white lotus flowers in Example 1 are replaced with red lotus flowers; The red lotus is a red peony ( Nelumbo nucifera 'Hong Mudan').

[0026] Example 4 The steps for preparing a composite acid gel composition are as follows: (1) Preparation of lotus-Bacillus subtilis fermentation products The white lotus flowers (specifically, the Ice Heart Lotus) Nelumbo nucifera The petals of 'Bingxin' were cleaned, dried, and crushed to obtain a lotus flower sample; Lotus flower samples, fructose, and Bacillus subtilis (effective viable count of 1×10⁻⁶) were added. 8 CFU / g) and water were mixed evenly at a mass ratio of 10:0.05:0.6:80 and fermented aerobically at 40℃ for 48 hours to obtain fermentation broth; The fermentation broth and the compound enzyme (in which the mass ratio of flavor protease to cellulase is 1:1) were mixed at a mass ratio of 100:3 and enzymatically hydrolyzed at 45℃ for 12 hours. The hydrolysate was then subjected to enzyme inactivation, solid-liquid separation, and concentration and drying (until the mass of the substance no longer changed) to obtain the lotus-Bacillus subtilis fermentation product.

[0027] (2) Preparation of composite acid gel composition The composite acid gel composition comprises, by weight parts, the following components: 2 parts capryloyl salicylic acid, 4 parts glycolic acid, 1 part arbutin, 0.08 parts piroctone olamine salt, 10 parts lotus-Bacillus subtilis fermentation product, 5 parts alkyl glycoside, and 70 parts water. In the arbutin, the mass ratio of α-arbutin to β-arbutin is 1:0.5.

[0028] At 60°C, capryloyl salicylic acid, glycolic acid, arbutin, piroctone olamine salt, alkyl glycoside and water are mixed evenly. After the mixture is cooled to 35-38°C, lotus-Bacillus subtilis fermentation product is added and mixed evenly to obtain a composite acid gel composition.

[0029] Comparative Example 1 The only difference from Example 1 is that the white lotus in Example 1 is replaced with white water lilies; The white water lily is the European white water lily. Nymphaea alba ).

[0030] Comparative Example 2 The only difference from Example 1 is that step (1) is as follows: (1) Preparation of lotus-Bacillus subtilis fermentation products The white lotus flowers (specifically, the Ice Heart Lotus) Nelumbo nucifera The petals of 'Bingxin' were cleaned, dried, and crushed to obtain a lotus flower sample; Lotus flower samples, fructose, and Bacillus subtilis (effective viable count of 1×10⁻⁶) were added. 8 CFU / g) and water were mixed evenly at a mass ratio of 10:0.02:0.3:90 and fermented aerobically at 40℃ for 48 hours to obtain fermentation broth; The fermentation broth was subjected to solid-liquid separation to obtain a supernatant, which was then concentrated and dried (until the mass of the substance no longer changed) to obtain the lotus-Bacillus subtilis fermentation product.

[0031] Comparative Example 3 The only difference from Example 1 is that it uses Lactobacillus plantarum ( Lactobacillus plantarum Replace Bacillus subtilis in Example 1.

[0032] Comparative Example 4 The only difference from Example 1 is that step (2) is as follows: (2) Preparation of composite acid gel composition The composite acid gel composition comprises, by weight parts, the following components: 2 parts capryloyl salicylic acid, 4 parts glycolic acid, 1 part arbutin, 0.08 parts piroctone olamine salt, 10 parts lotus-Bacillus subtilis fermentation product, 5 parts alkyl glycoside, and 70 parts water. The arbutin in question is α-arbutin.

[0033] At 60°C, capryloyl salicylic acid, glycolic acid, arbutin, piroctone olamine salt, alkyl glycoside and water are mixed evenly. After the mixture is cooled to 35-38°C, lotus-Bacillus subtilis fermentation product is added and mixed evenly to obtain a composite acid gel composition.

[0034] Comparative Example 5 The only difference from Example 1 is that step (2) is as follows: (2) Preparation of composite acid gel composition The composite acid gel composition comprises the following components by weight: 2 parts capryloyl salicylic acid, 4 parts glycolic acid, 1 part arbutin, 0.08 parts piroctone olamine salt, 20 parts lotus-Bacillus subtilis fermentation product, 5 parts alkyl glycoside, and 70 parts water. In the arbutin, the mass ratio of α-arbutin to β-arbutin is 1:0.2.

[0035] At 60°C, capryloyl salicylic acid, glycolic acid, arbutin, piroctone olamine salt, alkyl glycoside and water are mixed evenly. After the mixture is cooled to 35-38°C, lotus-Bacillus subtilis fermentation product is added and mixed evenly to obtain a composite acid gel composition.

[0036] Validation Example 1: Stimulus Validation The composite acid gel compositions prepared in Examples 1-4 and Comparative Examples 1-5 were dissolved in sterile water to obtain analytes with a final concentration of 0.1 g / mL. Nine Japanese white rabbits were used as validation subjects (one rabbit for each test solution). The acute eye irritation test method of the "Cosmetic Hygiene Standard" was adopted. 0.1 mL of the test solution was instilled into the conjunctival sac of one eye of the rabbit once, with the other eye not in contact with the eye as a self-control. The eye was closed for 1 second, and the test solution was instilled for 30 seconds. The eyes were then rinsed with distilled water. At 1 h, 24 h and 48 h after instillation of the test solution, the eye membranes were observed with a handheld slit lamp for any abnormalities (such as redness, swelling, itching, etc., indicated that the test solution was irritating). The irritation of different test solutions was evaluated. The results are shown in Table 1.

[0037] Table 1 Irritation properties of different test solutions

[0038] Based on the results in Table 1, it can be seen that the composite acid gel compositions prepared by the methods in Examples 1-4 have no irritation to rabbit eyes. Although the composite acid gel compositions prepared in Comparative Examples 3 and 4 showed abnormalities such as conjunctival hyperemia and edema in the test animals within 1 hour after being instilled, these abnormalities disappeared spontaneously after 24 hours, and no toxic effects were observed, indicating only mild irritation.

[0039] The fur on both sides of the spine of each Japanese plover (9 rabbits in total, 1 rabbit used for each test solution) was trimmed, with a trimmed area of ​​approximately 6 cm² on each side. 2 Observe each animal for any abnormalities within 24 hours. If no abnormalities are observed, apply 0.5 mL of each test substance directly to the shaved skin side, cover with clean gauze, and secure with non-irritating adhesive tape. The other side of the back of the same Japanese rabbit serves as a negative control. After 24 hours, remove the gauze and wash away any remaining test substances with warm water. Observe the skin reaction at the application site at 1 hour, 24 hours, and 48 hours after removing the test substances.

[0040] The results showed that, regardless of whether the test substances were used in the examples or comparative examples, no edema or erythema occurred after application to the skin of Japanese rabbits. This indicates that the test substances exhibited no acute skin irritation and were highly safe.

[0041] Verification Example 2: Anti-inflammatory efficacy verification The composite acid gel compositions prepared in Examples 1-4 and Comparative Examples 1-5 were dissolved in sterile water to obtain analytes with a final concentration of 0.1 g / mL. RAW264.7 macrophages were used as the research subject to establish a cellular inflammation model by stimulating cells with lipopolysaccharide (LPS), a bacterial endotoxin. T1, Ttotal, and T0 were set up: macrophages were seeded and cultured for 24 hours, then the test substances were added, followed by the addition of 1 μg / mL LPS (T1) 2 hours later. The group receiving only LPS (Ttotal) and the group receiving only diluent (T0) were stimulated for 24 hours. The supernatant was collected, and the pro-inflammatory inflammatory factor TNF was analyzed using an ELISA kit. The α release level was determined, and the average TNF-α inhibition rate of each treatment was calculated according to the following formula. Three replicates were set up for each analyte. The results are shown in Table 2.

[0042] The TNF-α inhibition rate (%) is calculated as [(Ttotal - T1) / (Ttotal - T0)] × 100%.

[0043] Table 2 TNF levels in different treatments inhibition rate of α

[0044] As shown in Table 2, the composite acid gel compositions prepared in Examples 1-4 have high TNF content. α-inhibition rate, while in the comparative example, after changing the raw materials or the preparation method, TNF... The inhibition rate of α was only 18.63%-26.91%.

[0045] Validation Example 3: Dandruff Suppression Validation The composite acid gel compositions prepared in Examples 1-4, Comparative Examples 1, and Comparative Examples 3-5 were dissolved in sterile water to obtain analytes with a final concentration of 0.1 g / mL. Several male and female volunteers were selected (inclusion criteria are shown in Table 3).

[0046] Table 3 Volunteer Selection Criteria

[0047] The volunteers were divided into groups of 10, with 5 men and 5 women in each group, and divided into 8 groups (Group 1 to Group 8); each person in each group parted their hair in half from the middle. Group 1: The test sample prepared in Example 1 was used to wash the left half of the hair of the participants for 5 minutes; Group 2: The test sample prepared in Example 2 was used to wash the left half of the hair of the participants for 5 minutes; Group 3: The test sample prepared in Example 3 was used to wash the left half of the hair of the participants for 5 minutes; Group 4: The test sample prepared in Example 4 was used to wash the left half of the hair of the group members for 5 minutes; Group 5: The test sample prepared in Comparative Example 1 was used to wash the left half of the hair of the participants for 5 minutes; Group 6: The test sample prepared in Comparative Example 3 was used to wash the left half of the hair of the participants for 5 minutes; Group 7: The test sample prepared in Comparative Example 4 was used to wash the left half of the hair of the participants for 5 minutes; Group 8: The test sample prepared in Comparative Example 5 was used to wash the left half of the hair of the participants for 5 minutes; The right side of each group's hair was washed with clean water for 5 minutes (referred to as the control group). After each 5-minute treatment, the hair was washed three times with warm water for 1 minute each time, and then air-dried. The number of dandruffs (unit: dandruff) of each subject was observed and counted at 24h, 48h, and 72h after the hair was dried. The average number of dandruffs for 10 people in groups 1 to 8 was counted, and the average number of dandruffs for 80 people in the control group was counted. The results are shown in Table 4 (only integer values ​​are retained in Table 4).

[0048] Table 4. Average dandruff count in different treatments

[0049] As shown in Table 4, the composite acid gel compositions prepared in Examples 1-4 effectively inhibit dandruff, with the composite acid gel composition prepared in Example 1 exhibiting the best anti-dandruff effect. While the composite acid gel composition in the comparative example showed good initial anti-dandruff effect, its effectiveness diminished over time.

[0050] In summary, the present invention, by compounding capryloyl salicylic acid, glycolic acid, α-arbutin, β-arbutin, piroctone olamine salt, lotus-Bacillus subtilis fermentation product, emulsifier, and water, produces a composition that can penetrate deep into the hair follicle sebaceous glands, unclog pores, and improve scalp folliculitis; it also accelerates the shedding of dead skin cells, not only solving the root cause of deep hair follicle blockage but also achieving surface keratin renewal. Furthermore, the product prepared in this way is green, safe, gentle, and non-irritating, effectively relieving scalp inflammation and inhibiting dandruff.

[0051] Although the above embodiments have provided a detailed description of the present invention, they are only some embodiments of the present invention, and not all embodiments. People can obtain other embodiments based on these embodiments without creative effort, and these embodiments all fall within the protection scope of the present invention.

Claims

1. A complex acid gel composition, characterized by, The complex acid gel composition comprises, in mass parts, the following ingredients: capryloyl salicylic acid 1.5-2.5 parts, glycolic acid 3.5-5 parts, arbutin 0.8-1 part, piroctone olamine 0.05-0.1 part, ferment of H. helianthus and B. subtilis 8-12 parts, emulsifier 5-6 parts, and water 70-80 parts. The arbutin comprises: α-arbutin and β-arbutin.

2. The complex acid gel composition according to claim 1, characterized by In the arbutin, the mass ratio of α-arbutin to β-arbutin is 1:0.1-0.

5.

3. The complex acid gel composition according to claim 1 or 2, characterized by, The complex acid gel composition comprises, in mass parts, the following ingredients: capryloyl salicylic acid 2 parts, glycolic acid 4 parts, arbutin 1 part, piroctone olamine 0.08 part, ferment of H. helianthus and B. subtilis 10 parts, emulsifier 5 parts, and water 70 parts. In the arbutin, the mass ratio of α-arbutin to β-arbutin is 1:0.

2.

4. The complex acid gel composition according to claim 1 or 2, characterized by, The preparation method of the ferment of H. helianthus and B. subtilis comprises: mixing a H. helianthus sample, fructose, B. subtilis, and water to perform aerobic fermentation to obtain a fermentation liquor; performing enzymolysis on the fermentation liquor with a complex enzyme, inactivating the enzyme, performing solid-liquid separation, and concentrating and drying to obtain the ferment of H. helianthus and B. subtilis; The complex enzyme comprises: flavor protease and cellulase.

5. The complex acid gel composition according to claim 4, wherein The H. helianthus sample comprises any one of the following (1)-(3): (1) flower and / or leaf of white H. helianthus; (2) flower and / or leaf of yellow H. helianthus; (3) flower and / or leaf of red H. helianthus.

6. The complex acid gel composition according to claim 4, wherein The mass ratio of the H. helianthus sample, fructose, B. subtilis, and water is 10:0.02-0.05:0.3-0.6:80-90. The effective viable cell number of the Bacillus subtilis is ≥1×10 8 cfu / g; The aerobic fermentation is performed for 36-48 h at a temperature of 38-40℃.

7. The complex acid gel composition according to claim 4, wherein The mass ratio of the fermentation liquor to the complex enzyme is 100:1-3. In the complex enzyme, the mass ratio of flavor protease to cellulase is 0.06-1:

1. The enzymolysis is performed at a temperature of 45-50℃ for 6-12 h.

8. A process for the preparation of the complex acid gel composition according to any one of claims 1 to 7, characterized in that, The following steps are included: mixing capryloyl salicylic acid, glycolic acid, arbutin, piroctone olamine, emulsifier, water, and the ferment of H. helianthus and B. subtilis uniformly to obtain a complex acid gel composition.

9. Use of the complex acid gel composition of any one of claims 1-7 in the preparation of a washing and caring product.

10. A shampoo, characterized by, The shampoo comprises: the complex acid gel composition of any one of claims 1-7.

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