A hair-removing composition and method of making and using same

Abstract

The present application belongs to the technical field of hair care, and particularly relates to a hair growth promoting composition and a preparation method and application thereof. The composition comprises the following components in parts by weight: pyrrolidinyl diaminopyrimidine oxide 0.7-1.7 parts, angelica extract 1.25-2.25 parts, tripeptide-1 copper 0.7-1.7 parts, hexapeptide-3 0.008-0.02 parts, glycerol 35-55 parts, and a stabilizer 11-18 parts; the stabilizer comprises maltodextrin and distearyl phthalic acid amide. The pyrrolidinyl diaminopyrimidine oxide is combined with the angelica extract, tripeptide-1 copper and hexapeptide-3 active substances, which can synergistically improve the hair growth and hair loss prevention, oil control and other effects of the composition from multiple dimensions, and the combination of the active substances and the specific stabilizer component can effectively ensure the uniformity of the formed hair growth composition system, maintain the long-term stability of the composition, and enhance the transdermal absorption effect of the composition.

Description

Technical Field

[0001] This invention belongs to the field of hair care technology, and in particular relates to a hair care composition, its preparation method and application. Background Technology

[0002] More than 250 million people in China suffer from hair loss, a massive population issue that seriously impacts their mental health and quality of life. Hair loss can be broadly categorized into age-related hair loss, pathological hair loss, neurogenic hair loss, and seborrheic alopecia (or androgenetic alopecia). Seborrheic alopecia is a common type and is showing a trend towards affecting younger people. It is related to the level of androgens in the body. Because androgen-binding receptors exist in special androgen cells of hair follicles, androgen levels also affect the degeneration and atrophy of hair follicles. It typically begins around age 20 with progressive, slow hair loss in the frontal, temporal, and vertex areas. Initially, itchy scalp is common, with significant hair loss when scratching or combing. The shed hairs have short roots and the hair bulb disappears. The hair loss process is slow and can be phased, with varying degrees of severity. After several years, it can lead to thinning hair on the crown or temples, a shiny scalp, oily scalp with dandruff, and fine, soft, yellowish hair.

[0003] In clinical practice, drugs such as finasteride, dutasteride, and minoxidil are commonly used to treat seborrheic alopecia. The use of these drugs can easily lead to problems such as dry scalp, blood pressure fluctuations, and palpitations, and their use is limited to medication, making them unsuitable for daily treatment and maintenance of seborrheic alopecia. Copyrrolidine (chemical name: pyrrolidine diaminopyrimidine oxide) is a compound synthesized by chemical modification based on the chemical structure of minoxidil. Its anti-hair loss and hair growth efficacy is comparable to minoxidil, but it is milder. It is approved for use in anti-hair loss shampoos and conditioners in China, Japan, and Europe and the United States, and is widely used in anti-hair loss shampoos, serums, and other hair care products as daily hair care products. In the use of anti-hair loss products, the follicular delivery of the anti-hair loss active ingredients is crucial to their efficacy. Due to the low water solubility of copyrrolidine, its compatibility with formulations and its poor skin penetration lead to reduced transdermal absorption, thus reducing the hair growth-promoting effect of the corresponding products. Summary of the Invention

[0004] The purpose of this invention is to overcome the shortcomings of the prior art and provide a hair growth composition, its preparation method and application, so as to effectively improve the transdermal absorption of hair growth components such as hair growth components and promote hair density and lushness.

[0005] To achieve the above objectives, the technical solution adopted by the present invention includes:

[0006] In a first aspect, the present invention provides a Shengfa Cocopyroxene composition comprising the following components in parts by weight: 0.7-1.7 parts of pyrrolidine diaminopyrimidine oxide, 1.25-2.25 parts of Angelica sinensis extract, 0.7-1.7 parts of tripeptide-1 copper, 0.008-0.02 parts of hexapeptide-3, 35-55 parts of glycerol, and 11-18 parts of stabilizer; wherein the stabilizer comprises maltodextrin and distearate phthalamide.

[0007] In the Shengfa composition described in this invention:

[0008] Pyrrolidinyl diaminopyrimidine oxide (Kopiro), as a potassium channel opener, can effectively promote the proliferation of dermal papilla cells, stimulate hair follicle regeneration, and nourish hair follicles by dilating blood vessels to increase nutrients and oxygen to the hair roots. It can also accelerate new hair growth by optimizing the hair follicle growth cycle. Simultaneously, pyrrolidinyl diaminopyrimidine oxide can reduce serum levels of 5α-reductase, androgen receptors, and dihydrotestosterone, showing good preventative and therapeutic effects on common types of hair loss such as androgenetic alopecia.

[0009] Traditional Chinese medicine believes that "hair is the surplus of blood," meaning that hair growth is closely related to blood sufficiency. Angelica extract has the effects of nourishing blood and qi, and promoting blood circulation, providing sufficient nutrition to hair follicles and thus promoting hair growth. At the same time, Angelica extract has anti-inflammatory and antioxidant effects, which can reduce scalp inflammation, relieve symptoms such as scalp itching and redness, reduce oxidative stress damage to hair follicle cells, protect the normal function of hair follicle cells, and improve scalp health.

[0010] Tripeptide-1 copper (GHK-Cu) is a copper-rich tripeptide molecule with the sequence GHK, widely found in human blood, saliva, and urine. GHK-Cu, with its unique affinity for copper ions, promotes wound healing, activates skin regeneration, and stimulates hair follicle activity.

[0011] Hexapeptide-3 is a small peptide with a sequence similar to the 6-amino acid fragment in the type III unit of fibronectin. It can promote the expression of laminin-5 and β1 integrin, collagen adhesion, and strengthen the adhesion between cells and the intercellular matrix (ECM), thereby promoting skin repair and enhancing the barrier function of the scalp.

[0012] In this invention, pyrrolidine diaminopyrimidine oxide is used as the main active substance to promote hair growth. It is combined with Angelica sinensis extract, tripeptide-1 copper and hexapeptide-3 as auxiliary active substances. It can open the potassium channels of the scalp and promote the proliferation of hair papilla cells, while relieving scalp inflammation, reducing scalp damage, strengthening the scalp barrier and stimulating hair follicle activity. While promoting hair growth, it maintains the health of the scalp. The final composition shows a good effect of promoting hair growth and preventing hair loss.

[0013] Furthermore, this invention uses water-insoluble distearate phthalamide and water-soluble maltodextrin as stabilizers, achieving multiple stabilizing effects and significantly improving the stability of the Shengfa picroximation composition system, ensuring that it does not experience stratification, precipitation, or degradation under different environments. In addition, glycerin can not only serve as a solvent for pyrrolyl diaminopyrimidine oxide, Angelica sinensis extract, and distearate phthalamide, but also as a moisturizing component, enhancing the moisturizing effect of the Shengfa composition and improving its overall performance.

[0014] Preferably, the hair-growth composition comprises the following components in parts by weight: 0.9-1.55 parts of pyrrolidine diaminopyrimidine oxide, 1.6-1.9 parts of Angelica sinensis extract, 1-1.5 parts of tripeptide-1 copper, 0.01-0.015 parts of hexapeptide-3, 35-55 parts of glycerin, and 11-18 parts of stabilizer.

[0015] Preferably, the hair-generating composition comprises the following components in parts by weight: 1.25 parts of pyrrolidine diaminopyrimidine oxide, 1.25 parts of pyrrolidine diaminopyrimidine oxide, 1.75 parts of Angelica sinensis extract, 1.25 parts of tripeptide-1 copper, 0.013 parts of hexapeptide-3, 45.813 parts of glycerin, and 15 parts of stabilizer.

[0016] Experimental studies have revealed that when pyrrolidine diaminopyrimidine oxide is combined with Angelica sinensis extract, tripeptide-1 copper, and hexapeptide-3 in the above-mentioned optimal dosage ratio, the components work together to exert an ideal synergistic effect, thereby improving the skin permeability of the composition, significantly enhancing its hair growth, oil control, and barrier repair effects, and achieving excellent hair strengthening and anti-hair loss effects.

[0017] Preferably, the mass ratio of maltodextrin to distearate phthalamide is (8.5-13):(2.5-5).

[0018] More preferably, the mass ratio of maltodextrin to distearate phthalamide is 11.25:3.75.

[0019] Preferably, the method for preparing the Angelica sinensis extract includes any one of the following three methods:

[0020] Method 1:

[0021] Angelica root powder and water are mixed, heated and filtered to obtain filtrate. The filtrate is then concentrated and dried to obtain Angelica extract.

[0022] Method 2:

[0023] Angelica root and rhizome powder was mixed with glacial acetic acid, and after ultrasonic treatment and washing, a mixture was obtained. A compound extractant was added to the mixture, and after a second ultrasonic treatment, the mixture was filtered. The filtrate was collected, concentrated and dried to obtain Angelica extract.

[0024] Method 3:

[0025] S1. Mix Angelica root powder with water, heat the mixture, and then filter it to obtain filter residue and primary filtrate.

[0026] S2. The filtrate obtained in step S1 is concentrated and dried to obtain a primary extract;

[0027] S3. Add glacial acetic acid to the filter residue described in step S1, and obtain a mixture after ultrasonic treatment and washing.

[0028] S4. Add the composite extractant to the mixture, perform a second ultrasonic treatment, and then filter to obtain a second filtrate.

[0029] S5. The secondary filtrate obtained in step S4 is concentrated and dried a second time to obtain a secondary extract.

[0030] S6. Mix the primary extract and the secondary extract to obtain the Angelica extract.

[0031] More preferably, the method for preparing the Angelica sinensis extract includes the following steps:

[0032] S1. Mix Angelica root powder with water, heat the mixture, and then filter it to obtain filter residue and primary filtrate.

[0033] S2. The filtrate obtained in step S1 is concentrated and dried to obtain a primary extract;

[0034] S3. Add glacial acetic acid to the filter residue described in step S1, and obtain a mixture after ultrasonic treatment and washing.

[0035] S4. Add the composite extractant to the mixture, perform a second ultrasonic treatment, and then filter to obtain a second filtrate.

[0036] S5. The secondary filtrate obtained in step S4 is concentrated and dried a second time to obtain a secondary extract.

[0037] S6. Mix the primary extract and the secondary extract to obtain the Angelica extract.

[0038] Preferably, it includes at least one of the following (I)-(X):

[0039] (I) In step S1, the mass ratio of the Angelica sinensis root powder to water is 1:(2-5);

[0040] (II) In step S1, the temperature of the heat treatment is 60-85℃ and the heat treatment time is 4-7h;

[0041] (III) In step S2, the concentration method includes vacuum concentration, and the vacuum concentration temperature is 60-85℃;

[0042] (Ⅳ) In step S2, the drying method includes spray drying, and the conditions for spray drying are: inlet air temperature of 90-110℃ and outlet air temperature of 50-70℃;

[0043] (V) In step S3, the mass ratio of the filter residue to glacial acetic acid is 1:(0.8-2);

[0044] (VI) In step S3, the temperature of the ultrasonic treatment is 20-35℃, the power of the ultrasonic treatment is 300-500W, and the time of the ultrasonic treatment is 30-60min;

[0045] (VII) In step S4, the mass ratio of the mixture to the composite extractant is 1:(3-8); the composite extractant includes at least two of ethanol, glycerol, butanediol and petroleum ether;

[0046] (VIII) In step S4, the temperature of the secondary ultrasonic treatment is 40-50℃, the power of the secondary ultrasonic treatment is 300-500W, and the time of the secondary ultrasonic treatment is 1-3h.

[0047] (IX) In step S5, the secondary concentration method includes vacuum concentration, and the vacuum concentration temperature is 40-60℃;

[0048] (X) In step S5, the secondary drying method includes spray drying, and the conditions for spray drying are: inlet air temperature of 70-90℃ and outlet air temperature of 40-50℃.

[0049] Preferably, in step S4, the composite extractant includes ethanol, glycerol, and petroleum ether.

[0050] More preferably, in step S4, the volume ratio of ethanol, glycerol and petroleum ether is (4.5-8):(2-4):(0.8-1.5).

[0051] This invention employs both water extraction and compound organic solvent extraction to effectively extract Angelica sinensis rhizomes. The substances obtained from these two extraction methods are then mixed to form the Angelica sinensis extract of this invention. Water extraction can extract polysaccharides (such as heteropolysaccharides composed of monosaccharides like D-glucose, D-xylose, and D-galactose), organic acids, amino acids, and some coumarin-like active substances from the Angelica sinensis rhizomes. Compound organic solvent extraction can effectively extract volatile active substances such as polyphenols, flavonoids, and saponins from the Angelica sinensis rhizomes. The sequential extraction of Angelica sinensis rhizomes using two different methods fully utilizes the residue after water extraction. The resulting Angelica sinensis extract is rich in both water-soluble and organic solvent-soluble active components. In subsequent preparation of the dermal absorption composition, the Angelica sinensis extract is more conducive to transdermal absorption of the product, exerting a synergistic effect and better achieving the desired dermal absorption.

[0052] In the water extraction process of this invention, the heating treatment step has already fully swollen the Angelica sinensis root and rhizome powder. After the water extraction is completed and the filter residue is obtained, this invention pre-treats the powder with glacial acetic acid before using the compound extractant. The purpose is to use glacial acetic acid to break down the fully swollen Angelica sinensis cell walls, increase cell permeability, and facilitate the dissolution of active substances such as polyphenols, flavonoids, and saponins during subsequent extraction with organic solvents.

[0053] The present invention prepares Angelica extract into powder form for the following purposes: (1) to fully remove the organic solvent remaining in the compound organic solvent extraction process, reduce the irritation of Angelica extract, and make the Shengfa Kebi Luo composition safer; (2) to better maintain the stability of Angelica extract; (3) to increase the proportion of Angelica extract in the active components in the subsequent composition, which is more conducive to the synergistic effect of Angelica extract.

[0054] Secondly, the present invention provides a method for preparing the aforementioned hair-growth composition, comprising the following steps:

[0055] (1) Pyrrolidinyl diaminopyrimidine oxide, Angelica sinensis extract, distearate phthalamide and solvent were mixed to obtain phase A;

[0056] (2) Mix tripeptide-1 copper, hexapeptide-3, maltodextrin and water to obtain phase B;

[0057] (3) Mix the A phase and the B phase and homogenize them to obtain the Shengfa Kobi Luo composition.

[0058] Preferably, the homogenization process includes high-speed shear dispersion or high-pressure homogenization.

[0059] Preferably, the conditions for the high-speed shear dispersion treatment are a rotation speed of 8000-12000 rpm and a time of 20-40 min.

[0060] Preferably, the high-pressure homogenization treatment is performed at 50-120 MPa for 3-6 cycles.

[0061] The present invention uses homogenization to fully mix the A phase and B phase prepared above, thereby forming a homogeneous system of the composition and further improving the stability of the composition.

[0062] Thirdly, the present invention provides the application of the aforementioned hair-enhancing composition in the preparation of hair care products.

[0063] Preferably, the hair-strengthening composition accounts for 1-20% by mass in the hair product.

[0064] The hair care product described in this invention can be 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, creams, and sprays.

[0065] Preferably, the hair product includes at least one of scalp care essence, scalp care water, scalp nourishing cream, scalp massage cream, hair essence, hair oil, shampoo, shampoo bar, shampoo powder, hair mask, conditioner, hair spray, hair gel, and hair lotion.

[0066] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0067] (1) To address the problems of low water solubility and poor compatibility of apicor in hair products, this invention provides a apicor composition for hair care. In this invention, active components such as pyrrolidine diaminopyrimidine oxide (apicor), angelica extract, tripeptide-1 copper, and hexapeptide-3 are combined and compounded with stabilizers and solvent components. The resulting hair care composition system is homogeneous, and apicor is uniformly dispersed in a water-soluble solvent, which is beneficial to enhancing the transdermal absorption effect of apicor and improving the compatibility of apicor with other hair care raw materials.

[0068] (2) The Shengfa Kopilot composition of the present invention combines water-soluble and water-insoluble active components, allowing pyrrolidone diaminopyrimidine oxide (Kopilot), Angelica sinensis extract, tripeptide-1 copper, and hexapeptide-3 to exert a synergistic effect, which can effectively promote the expression of alkaline phosphatase in dermal papilla cells, inhibit sebum secretion from sebaceous gland cells, and promote the migration of keratinocytes. Alkaline phosphatase is one of the molecular markers of dermal papilla cells in hair follicles, and its expression level can reflect the activity and functional state of dermal papilla cells. Increased alkaline phosphatase expression can activate the Wnt / β-catenin signaling pathway, which plays a key role in hair follicle formation and hair growth. Activation of this pathway can promote the proliferation and differentiation of dermal papilla cells in hair follicles, thereby promoting hair growth. The inhibition of sebum secretion from sebaceous gland cells means that the composition has an oil-controlling effect, which can reduce scalp sebum secretion and alleviate the problem of seborrheic alopecia. The promoted migration of keratinocytes indicates that the Shengfa Kobilol composition has a scalp barrier repairing effect, accelerates the repair and reconstruction of the skin barrier, is conducive to the normal growth of hair follicle cells in the scalp, and promotes hair growth and hair strengthening. In summary, the Kobilol composition of the present invention has multiple effects, which can promote hair growth from multiple dimensions, while also playing a role in strengthening hair and preventing hair loss, thereby effectively maintaining a thick and lush hair condition.

[0069] (3) The present invention uses both water-soluble maltodextrin and water-insoluble distearate phthalamide as solvents as stabilizers for the system, which can achieve a variety of stabilizing effects, maintain the stability of the system, and improve the usability of comparable compositions in the formulation. Detailed Implementation

[0070] To better illustrate the objectives, technical solutions, and advantages of this invention, the invention will be further described below with reference to specific embodiments. Those skilled in the art should understand that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

[0071] Unless otherwise specified, all raw materials used in the following examples and comparative examples are commercially available and commonly used raw materials.

[0072] The DE value of the maltodextrin described in the following examples and comparative examples is 15%-20%.

[0073] Examples 1-5

[0074] Examples 1-5 provide a Shengfa Kobiro composition, the specific formulation of which is shown in Table 1 (total weight parts: 100 parts). The preparation method of the composition includes the following steps:

[0075] (1) Pyrrolidinyl diaminopyrimidine oxide, Angelica sinensis extract, distearate phthalamide and glycerin were mixed to obtain phase A;

[0076] (2) Mix tripeptide-1 copper, hexapeptide-3, maltodextrin and water to obtain phase B;

[0077] (3) Mix phase A and phase B, and homogenize them under high pressure of 80 MPa for 4 cycles to obtain the Shengfa Kobi Luo composition.

[0078] The preparation process of Angelica sinensis extract includes:

[0079] S1. Mix Angelica root and rhizome powder with 3 times the mass of water, heat at 70°C for 5 hours, and then filter to obtain filter residue and primary filtrate.

[0080] S2. The filtrate from the first application is concentrated under reduced pressure and spray-dried at 70°C (inlet air temperature 100°C; outlet air temperature 60°C) to obtain the powder, which is the primary extract.

[0081] S3. Add 1.5 times the mass of glacial acetic acid to the filter residue from step S1, and sonicate it at 30°C and 400W for 40 minutes. After sonication, rinse it three times with deionized water to remove the glacial acetic acid and obtain a mixture.

[0082] S4. Add 5 times the mass of a composite extractant of ethanol, glycerol and petroleum ether (volume ratio of ethanol, glycerol and petroleum ether is 6:3:1) to the mixture, perform a second ultrasonic treatment (conditions are 45℃, ultrasonic treatment time is 400W, time is 2h), and then filter to obtain a second filtrate.

[0083] S5. The secondary filtrate is concentrated under reduced pressure and spray-dried at 50°C (inlet air temperature is 80°C; outlet air temperature is 45°C) to obtain the powder as the secondary extract.

[0084] S6. Mix the primary extract and the secondary extract to obtain Angelica extract.

[0085] Table 1. Formulation table (parts by weight) of the Shengfa Kobi Luo compositions described in Examples 1-5.

[0086]

[0087] Example 6

[0088] This embodiment provides a Shengfa Kebiluo composition, which differs from Example 1 only in that the preparation process of the Angelica extract is different.

[0089] The preparation process of Angelica sinensis extract described in this embodiment includes the following steps:

[0090] S1. Mix Angelica root and rhizome powder with 2 times the mass of water, heat at 85°C for 4 hours, and then filter to obtain filter residue and primary filtrate.

[0091] S2. The filtrate from the first application is concentrated under reduced pressure and spray-dried at 60°C (inlet air temperature 110°C; outlet air temperature 70°C) to obtain the powder, which is the primary extract.

[0092] S3. Add 2 times the mass of glacial acetic acid to the filter residue from step S1, and sonicate at 20°C and 300W for 60 minutes. After sonication, rinse with deionized water 5 times to remove the glacial acetic acid and obtain a mixture.

[0093] S4. Add 3 times the mass of a composite extractant of ethanol, glycerol and petroleum ether (volume ratio of ethanol, glycerol and petroleum ether is 4.5:4:1.5) to the mixture, perform a second ultrasonic treatment (conditions are 40℃, ultrasonic treatment time is 300W, time is 3h), and then filter to obtain the second filtrate.

[0094] S5. The secondary filtrate is concentrated under reduced pressure and spray-dried at 40°C (inlet air temperature is 90°C; outlet air temperature is 50°C) to obtain the powder as the secondary extract.

[0095] S6. Mix the primary extract and the secondary extract to obtain Angelica extract.

[0096] Example 7

[0097] This embodiment provides a Shengfa Kebiluo composition, which differs from Example 1 only in that the preparation process of the Angelica extract is different.

[0098] The preparation process of Angelica sinensis extract described in this embodiment includes the following steps:

[0099] S1. Mix Angelica root and rhizome powder with 5 times the mass of water, heat at 60°C for 7 hours, and then filter to obtain filter residue and primary filtrate.

[0100] S2. The filtrate from the first application is concentrated under reduced pressure and spray-dried at 85°C (inlet air temperature 90°C; outlet air temperature 60°C) to obtain the powder, which is the primary extract.

[0101] S3. Add 0.8 times the mass of glacial acetic acid to the filter residue from step S1, and sonicate at 35°C and 500W for 30 minutes. After sonication, rinse twice with deionized water to remove the glacial acetic acid and obtain a mixture.

[0102] S4. Add 8 times the mass of a composite extractant of glycerol and petroleum ether (the volume ratio of glycerol to petroleum ether is 2:0.8) to the mixture, perform a second ultrasonic treatment (conditions are 50℃, ultrasonic treatment time is 500W, and time is 1h), and then filter to obtain the second filtrate.

[0103] S5. The secondary filtrate is concentrated under reduced pressure and spray-dried at 60°C (inlet air temperature 70°C; outlet air temperature 40°C) to obtain the powder as the secondary extract.

[0104] S6. Mix the primary extract and the secondary extract to obtain Angelica extract.

[0105] Example 8

[0106] This embodiment provides a Shengfa Kebiluo composition, which differs from Example 1 only in that the preparation process of the Angelica extract is different.

[0107] The preparation process of Angelica sinensis extract described in this embodiment includes the following steps:

[0108] S1. Mix Angelica root and rhizome powder with 3 times the mass of water, heat at 70°C for 5 hours, and then filter to obtain filter residue and primary filtrate.

[0109] S2. The filtrate is concentrated under reduced pressure and spray-dried at 70°C (inlet air temperature is 100°C; outlet air temperature is 60°C) to obtain the powder, which is Angelica sinensis extract.

[0110] Example 9

[0111] This embodiment provides a Shengfa Kebiluo composition, which differs from Example 1 only in that the preparation process of the Angelica extract is different.

[0112] The preparation process of Angelica sinensis extract described in this embodiment includes the following steps:

[0113] S1. Mix Angelica root and rhizome powder with 1.5 times the mass of glacial acetic acid, and sonicate at 30℃ and 400W for 40 minutes. After sonication, rinse with deionized water 3 times to remove glacial acetic acid and obtain the mixture.

[0114] S2. Add 5 times the mass of a composite extractant of ethanol, glycerol and petroleum ether (volume ratio of ethanol, glycerol and petroleum ether is 6:3:1) to the mixture, perform a second ultrasonic treatment (conditions are 45℃, ultrasonic treatment time is 400W, time is 2h), and then filter to obtain a second filtrate.

[0115] S3. The secondary filtrate is concentrated under reduced pressure and spray-dried at 50°C (inlet air temperature is 80°C; outlet air temperature is 45°C) to obtain the powder, which is Angelica sinensis extract.

[0116] Comparative Examples 1-10

[0117] Comparative Examples 1-10 provide a composition for producing a high-quality product, the specific formulation of which is shown in Table 2 (total parts by weight: 100 parts). The preparation method of the composition is the same as that of Example 1, the only difference being the formulation.

[0118] Table 2. Formulation table (parts by weight) of the Shengfa Comparable Compositions described in Comparative Examples 1-10

[0119]

[0120]

[0121] Comparative Example 11

[0122] This comparative example provides a Shengfa Kobi composition, which differs from Example 1 only in that an equal amount of diaminopyrimidine oxide is used to replace pyrrolidinyl diaminopyrimidine oxide, while the other components and amounts remain unchanged.

[0123] Comparative Example 12

[0124] This comparative example provides a Shengfa Kebi Luo composition, which differs from Example 1 only in that an equal amount of Panax notoginseng root extract is used to replace Angelica sinensis extract, while the other components and amounts remain unchanged.

[0125] The preparation process of the Panax notoginseng extract includes the following steps:

[0126] S1. Mix the Panax notoginseng root powder with 3 times the mass of water, heat at 70°C for 5 hours, and then filter to obtain filter residue and primary filtrate.

[0127] S2. The filtrate from the first application is concentrated under reduced pressure and spray-dried at 70°C (inlet air temperature 100°C; outlet air temperature 60°C) to obtain the powder, which is the primary extract.

[0128] S3. Add 1.5 times the mass of glacial acetic acid to the filter residue from step S1, and sonicate it at 30°C and 400W for 40 minutes. After sonication, rinse it three times with deionized water to remove the glacial acetic acid and obtain a mixture.

[0129] S4. Add 5 times the mass of a composite extractant of ethanol, glycerol and petroleum ether (volume ratio of ethanol, glycerol and petroleum ether is 6:3:1) to the mixture, perform a second ultrasonic treatment (conditions are 45℃, ultrasonic treatment time is 400W, time is 2h), and then filter to obtain a second filtrate.

[0130] S5. The secondary filtrate is concentrated under reduced pressure and spray-dried at 50°C (inlet air temperature is 80°C; outlet air temperature is 45°C) to obtain the powder as the secondary extract.

[0131] S6. Mix the primary extract and the secondary extract to obtain Panax notoginseng root extract.

[0132] Comparative Example 13

[0133] This comparative example provides a Shengfa Kobiro composition, which differs from Example 1 only in that an equal amount of palmitoyl tripeptide-5 is used to replace tripeptide-1 copper, while the other components and amounts remain unchanged.

[0134] Comparative Example 14

[0135] This comparative example provides a Shengfa Comparable composition, which differs from Example 1 only in that an equal amount of acetyl hexapeptide-8 is used to replace hexapeptide-3, while the other components and amounts remain unchanged.

[0136] Comparative Example 15

[0137] This comparative example provides a Shengfa Comparable Composition, which differs from Example 1 only in that an equal amount of hydrolyzed corn starch is used to replace maltodextrin, while the other components and their amounts remain unchanged.

[0138] Comparative Example 16

[0139] This comparative example provides a Shengfa Kobi composition, which differs from Example 1 only in that an equal amount of dimethyl silicone oil is used to replace distearate phthalamide, while the other components and amounts remain unchanged.

[0140] Comparative Example 17

[0141] This comparative example provides a composition that differs from Example 1 only in that an equal amount of 1,2-butanediol is used to replace glycerol, while the other components and their amounts remain unchanged.

[0142] Example of effect

[0143] 1. Stability test:

[0144] Test samples: Shengfa comparable compositions described in Examples 1-9 and Comparative Examples 1-17;

[0145] Test procedure: Take 10 mL of the saturation compositions of Examples 1-9 and Comparative Examples 1-17 respectively and place them in colorless transparent PE sample bottles. Place the above samples at 4℃, 25℃, and 45℃ respectively, and observe the layering of the samples at month 0 and month 1. The specific results are shown in Table 3.

[0146] Table 3

[0147]

[0148]

[0149]

[0150] Stability test results show that the Shengfa Kobi composition of the present invention has good stability. After being placed for one month under low temperature (4°C), room temperature (25°C) and high temperature (45°C) conditions, the composition does not show any stratification.

[0151] In Comparative Examples 9-10, when maltodextrin and distearate phthalamide were used individually as stabilizers, the resulting Shengfa Kobilo compositions exhibited poor stability, showing varying degrees of stratification after being placed at different temperatures for one month. In Comparative Example 12, Angelica sinensis extract was replaced with Panax notoginseng root extract, which has similar efficacy. Although the extraction processes for Panax notoginseng root extract and Angelica sinensis extract are the same, the different plant species result in different active substances in the final plant extracts, and the synergistic effects of the components in the system also differ, leading to a still low stability of the final composition. Similarly, in Comparative Example 14, hexapeptide-3 was replaced with acetyl hexapeptide-8; in Comparative Example 15, the aqueous phase stabilizer was replaced with hydrolyzed corn starch; in Comparative Example 16, the oil phase stabilizer was replaced with dimethyl silicone oil; and in Comparative Example 17, the oil phase solvent was replaced with 1,2-butanediol. The changes in the type of peptide, stabilizer, and solvent affected the compatibility between the components, ultimately leading to changes in the stability of the system and varying degrees of stratification.

[0152] 2. Hair growth promotion test:

[0153] Test Principle: The human hair cycle includes the anagen (growth) phase, catagen (transitional) phase, and telogen (resting) phase. The induction and maintenance of the anagen phase in hair follicles determine the hair regeneration time and hair shaft length. Therefore, factors that promote hair follicle entry into the anagen phase and maintain its proliferative state are key to promoting lush hair growth. Research has confirmed that alkaline phosphatase (ALP) is a molecular marker of dermal papillary cells (DPCs) in hair follicles. It can enhance the activity of DPCs by participating in cell signaling in DPCs, thereby promoting hair follicle growth and development. This test determines the effectiveness of the test sample in promoting hair growth by measuring the relative expression level of the ALP gene in dermal papillary cells.

[0154] Test samples: The Shengfa Kobi composition of Examples 1-9 and Comparative Examples 1-17 was prepared into a 1% mass concentration solution using H-DMEM culture medium (hereinafter referred to as culture medium) containing 10% FBS as a solvent.

[0155] Test procedure: DPCs cells in the logarithmic growth phase were seeded into 6-well culture plates (2 × 10⁻⁶ cells / well). 5Cells per well (1 mL) were added to culture medium and incubated at 37°C with 5% CO2 for 24 hours, after which the culture medium was discarded. Subsequently, 1 mL of culture medium was added to the blank control group, and 1 mL of test sample was added to the sample group, and incubation continued for another 24 hours. After culture, total RNA was extracted from each well of DPCs, and reverse transcription was performed for quantitative real-time PCR. Real-time quantitative PCR results were analyzed using 2... －△△CT The calculation was performed using the method described above. The test results are shown in Table 4.

[0156] 3. Oil control effect test:

[0157] This test used human sebaceous gland cells SZ95 to construct an in vitro acne model. The sebum secretion of SZ95 cells was used to simulate the sebum secretion process of human skin. The sebum content of sebaceous gland cells was qualitatively and quantitatively detected by fluorescence quantitative method, so as to evaluate whether the test product has the effect of oil control.

[0158] Test samples: The Shengfa Kobilo compositions of Examples 1-9 and Comparative Examples 1-17 were prepared into a 1% (w / w) solution using H-DMEM containing 10% FBS and 10 μM testosterone culture medium as solvents.

[0159] Test procedure: SZ95 cells in the logarithmic growth phase were seeded into 24-well culture plates (2 × 10⁻⁶ cells / well). 4 Cells were cultured in H-DMEM (10% FBS in 10% FBS) at 5% CO2 and 37°C for 24 h, then the culture medium was discarded. Subsequently, the blank control group was added to 0.5 mL of H-DMEM containing 10% FBS, the model control group was added to 0.5 mL of 10 μM testosterone culture medium, and the sample group was added to 0.5 mL of test sample solution (containing 1% test sample and 10 μM testosterone). The model control group and test sample group were cultured for 24 h, while the blank control group was cultured under the same conditions for 24 h. After modeling, the culture medium was discarded, cells were washed with PBS, stained with 3 mM Nile red (from Yuanye Biotechnology), and incubated at 37°C in the dark for 10 min. After washing with PBS, the Nile red fluorescence intensity was detected using a multi-mode microplate reader at an excitation wavelength of 485 nm and an emission wavelength of 565 nm. The fluorescence grayscale values ​​were converted using ImageJ to evaluate the relative fluorescence intensity of the blank control group, model control group, and test sample group. The test results are shown in Table 4.

[0160] 4. Barrier Repair Effect Test

[0161] Test Principle: The stratum corneum is a continuous, multi-layered structure, comprising, from the inside out, the basal layer, spinous layer, granular cell layer, stratum lucidum, and the outermost layer of lifeless keratinocytes. Keratinocytes continuously divide, proliferate, differentiate, and denucleate, gradually migrating to the outermost layer of the skin to form the skin barrier. The function of the skin barrier depends on the integrity of the stratum corneum's brick-and-mortar structure. The repair function of the skin barrier mainly relies on the migration, proliferation, and differentiation of keratinocytes. After skin injury, keratinocytes migrate to the site of injury, promoting wound healing and skin barrier reconstruction. Therefore, the cell scratch test can assess the impact of a test sample on the migration and repair capabilities of keratinocytes, thus reflecting its role in the skin barrier repair function.

[0162] Test samples: The Shengfa Kobilo compositions of Examples 1-9 and Comparative Examples 1-17 were prepared into 3% solutions using DMEM medium containing 1 wt% fetal bovine serum as a solvent.

[0163] Test procedure: Keratinocytes in the logarithmic growth phase (i.e., cell suspension) were seeded into a culture insert (4×10⁶ cells / year). 5 The cell count was set up as follows: 24 cells / mL. A blank control group and a test sample group were also set up, with 2 culture inserts in each group, 2 wells per insert. 70 μL of cell suspension was seeded in each well, and the cells were cultured at 37°C with 5% CO2 for 24 h. When the cell coverage was above 95%, the scratched inserts were vertically removed from the 24-well plate using sterile forceps. Each well was washed once with 1 mL of PBS solution. 1 mL of 1 wt% fetal bovine serum in DMEM medium was added to the blank control group, and 1 mL of the prepared test sample solution was added to the test sample group.

[0164] The cells were observed under a microscope at 0h and 24h time points, and images of the scratched areas were taken. The scratch area of ​​each group was measured using ImageJ software, and the cell migration rate (%) was calculated.

[0165] Cell migration rate (%) = 1 - S 24 / S0.

[0166] In the formula: S 24 S0 represents the area of ​​the scratched area after 24 hours; S0 represents the area of ​​the scratched area after 0 hours.

[0167] The test results are shown in Table 4.

[0168] Table 4

[0169]

[0170]

[0171] Table 4 shows that the Shengfa Kobilo composition of the present invention can increase the expression level of alkaline phosphatase gene in dermal papilla cells, inhibit sebum secretion from sebaceous gland cells, and promote the migration of keratinocytes, indicating that the Shengfa Kobilo composition of the present invention has excellent effects in promoting hair growth, controlling oil, and repairing the hair barrier. In Examples 8-9, when the Angelica sinensis extract was extracted using only water or a compound solvent, the change in the preparation process led to a certain degree of change in the types and proportions of components in the composition, resulting in a certain degree of decrease in the growth, oil control, and barrier repair effects of the prepared Shengfa composition compared to Example 1.

[0172] In Comparative Examples 1-6, when any one or two of the following four active ingredients were missing: citric acid, Angelica sinensis extract, copper tripeptide-1, and hexapeptide-3, and the proportions of other active ingredients were increased to keep the total mass ratio of active ingredients constant, the hair growth effect, oil control effect, and barrier repair effect of the resulting hair-growth composition all decreased to varying degrees. In Comparative Examples 7-8, the dosage ratios of the above four active ingredients exceeded the limits of this invention, and the hair growth effect, oil control effect, and barrier repair effect of the composition also decreased to a certain extent compared with the examples. The above results indicate that the four active ingredients—citric acid, Angelica sinensis extract, copper tripeptide-1, and hexapeptide-3—used in this invention can only exert a better synergistic effect when combined within a specific dosage ratio range, thereby significantly enhancing the hair growth, oil control, and barrier repair effects of the composition. All four ingredients are indispensable. In Comparative Examples 11-14, when the active components in the compositions were replaced with those with similar functions, the overall hair growth and oil control effects of the resulting hair-growth compositions decreased to some extent. This indicates that the four active substances selected in this invention cannot be replaced conventionally; the four specific components must work together to maximize the hair growth and oil control effects of the composition. In Comparative Examples 9-10, when only maltodextrin or distearate phthalamide was used as a stabilizer, and in Comparative Examples 15-17, when maltodextrin, distearate phthalamide, and glycerin were replaced with other similar substances, the system became unstable. The active substances in the composition were prone to precipitation, which reduced the synergistic effect between the active ingredients, resulting in poorer hair growth, oil control, and barrier repair effects of the final composition.

[0173] Finally, it should be noted that the above embodiments are used to illustrate the technical solutions of the present invention and not to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A composition for producing hair growth, characterized in that, The Shengfa Kobi Luo composition comprises the following components in parts by weight: 0.7-1.7 parts of pyrrolidine diaminopyrimidine oxide, 1.25-2.25 parts of Angelica sinensis extract, 0.7-1.7 parts of tripeptide-1 copper, 0.008-0.02 parts of hexapeptide-3, 35-55 parts of glycerin, and 11-18 parts of stabilizer; The stabilizers include maltodextrin and distearate phthalamide; The preparation method of the Angelica sinensis extract includes the following steps: S1. Mix Angelica root powder with water, heat the mixture, and then filter it to obtain filter residue and primary filtrate. S2. The filtrate obtained in step S1 is concentrated and dried to obtain a primary extract; S3. Add glacial acetic acid to the filter residue described in step S1, and obtain a mixture after ultrasonic treatment and washing. S4. Add a composite extractant to the mixture, perform a second ultrasonic treatment, and then filter to obtain a secondary filtrate; the composite extractant is at least two of ethanol, glycerol, and petroleum ether. S5. The secondary filtrate obtained in step S4 is concentrated and dried a second time to obtain a secondary extract. S6. Mix the primary extract and the secondary extract to obtain the Angelica extract; Includes at least one of the following (I)-(X): (I) In step S1, the mass ratio of the Angelica sinensis root powder to water is 1:(2-5); (II) In step S1, the temperature of the heat treatment is 60-85℃ and the heat treatment time is 4-7h; (III) In step S2, the concentration method includes vacuum concentration, and the vacuum concentration temperature is 60-85℃; (IV) In step S2, the drying method includes spray drying, and the conditions for spray drying are: inlet air temperature of 90-110℃ and outlet air temperature of 50-70℃; (V) In step S3, the mass ratio of the filter residue to glacial acetic acid is 1:(0.8-2); (VI) In step S3, the temperature of the ultrasonic treatment is 20-35℃, the power of the ultrasonic treatment is 300-500W, and the time of the ultrasonic treatment is 30-60min; (VII) In step S4, the mass ratio of the mixture and the composite extractant is 1:(3-8). (VIII) In step S4, the temperature of the secondary ultrasonic treatment is 40-50℃, the power of the secondary ultrasonic treatment is 300-500W, and the time of the secondary ultrasonic treatment is 1-3h. (IX) In step S5, the secondary concentration method includes vacuum concentration, and the vacuum concentration temperature is 40-60℃; (X) In step S5, the secondary drying method includes spray drying, and the conditions for spray drying are: inlet air temperature of 70-90℃ and outlet air temperature of 40-50℃.

2. The Shengfa Comparable Composition as described in claim 1, characterized in that, The Shengfa Kobi Luo composition comprises the following components in parts by weight: 0.9-1.55 parts of pyrrolidine diaminopyrimidine oxide, 1.6-1.9 parts of Angelica sinensis extract, 1-1.5 parts of tripeptide-1 copper, 0.01-0.015 parts of hexapeptide-3, 35-55 parts of glycerin, and 11-18 parts of stabilizer.

3. The Shengfa Comparable Composition as described in claim 2, characterized in that, The Shengfa Kobiro composition comprises the following components in parts by weight: 1.25 parts of pyrrolidine diaminopyrimidine oxide, 1.75 parts of Angelica sinensis extract, 1.25 parts of tripeptide-1 copper, 0.013 parts of hexapeptide-3, 45.813 parts of glycerin, and 15 parts of stabilizer.

4. The Shengfa Comparable Composition as described in claim 1, characterized in that, The mass ratio of maltodextrin to distearate phthalamide is (8.5-13):(2.5-5).

5. The method for preparing the Shengfa Kobi Luo composition according to any one of claims 1-3, characterized in that, Includes the following steps: (1) Pyrrolidinyl diaminopyrimidine oxide, Angelica sinensis extract, distearate phthalamide and glycerin were mixed to obtain phase A; (2) Mix tripeptide-1 copper, hexapeptide-3, maltodextrin and water to obtain phase B; (3) Mix the A phase and the B phase and homogenize them to obtain the Shengfa Kobi Luo composition.

Images