Dengcobicine composition as well as preparation method and application thereof

Abstract

The invention belongs to the technical field of hair care, and particularly relates to a hair-containing cobillian composition as well as a preparation method and application of the hair-containing cobillian composition. The composition is prepared from the following components in parts by weight: 0.7 to 1.7 parts of pyrrolidinyl diaminopyrimidine oxide, 1.25 to 2.25 parts of radix angelicae sinensis extract, 0.7 to 1.7 parts of copper tripeptide-1, 0.008 to 0.02 part of hexapeptide-3, 35 to 55 parts of glycerol and 11 to 18 parts of a stabilizer, the stabilizer is prepared from maltodextrin and distearyl phthalic diamide. Pyrrolidinyl diaminopyrimidine oxide is matched with active substances of the angelica sinensis extract, tripeptide-1 copper and hexapeptide-3 to be combined, the effects of hair growth, hair loss prevention, oil control and the like of the composition can be synergistically improved from multiple dimensions, the active substances are matched with specific stabilizer components, it can be effectively ensured that a formed hair containing composition system is uniform, and the hair containing effect is good. The long-term stability of the composition is maintained, and meanwhile, the percutaneous absorption effect of the percutaneous absorption composition is enhanced.

Description

Technical Field

[0001] The invention belongs to the technical field of hair care, and in particular relates to a hair growth and hair loss composition, a preparation method and an application thereof. Background Art

[0002] Over 250 million people in China suffer from hair loss, a significant population that severely impacts their mental health and quality of life. Hair loss can be broadly categorized as senile, pathological, neurotic, and seborrheic (also known as androgenic) alopecia. Seborrheic alopecia is a common type of hair loss, and is becoming more common among younger people. Seborrheic alopecia is associated with androgen levels in the body. Because androgen-binding receptors are present in specialized male cells within hair follicles, androgen levels can influence the degeneration and atrophy of hair follicles. Generally, around age 20, progressive, slow hair loss occurs on the forehead, temples, and top of the head. Initially, itching is common, and hair falls out in large quantities when scratching or combing. The hair that falls out has short roots and no hair bulbs. The symptoms progress slowly, varying in severity and severity. After several years, the hair on the crown and temples becomes sparse, and the scalp becomes shiny. The head may become oily, greasy, or flaky, with fine, soft, and yellow 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 they are limited to drug use, which is not conducive to the daily treatment and maintenance of seborrheic alopecia. Cocamidopropyl betaine (chemical name: pyrrolidino diaminopyrimidine oxide) is a class of compounds synthesized by chemical modification based on the chemical structure of minoxidil. Its anti-hair loss and hair growth effects are comparable to minoxidil, but it is milder than minoxidil. It has been approved for use in anti-hair loss shampoo and hair care products in China, Japan, Europe and the United States, and is widely used in anti-hair loss shampoo, essence and other hair care products, and is used as a daily shampoo and hair care product. During the use of anti-hair loss products, the delivery of anti-hair loss active ingredients to the hair follicles is the key to their efficacy. Due to the low solubility of cocamidopropyl betaine in water, its poor formula compatibility and skin permeability lead to reduced transdermal absorption effect, reducing the effect of the corresponding product in promoting hair growth. Summary of the Invention

[0004] The purpose of the present invention is to overcome the deficiencies of the above-mentioned prior art and provide a hair-growing kobelu composition and its preparation method and application, so as to effectively improve the problem of transdermal absorption of kobelu and its related hair-growing ingredients and promote the thickness and growth of hair.

[0005] To achieve the above objectives, the technical solutions adopted by the present invention include:

[0006] In a first aspect, the present invention provides a hair-promoting composition comprising the following components in parts by weight: 0.7-1.7 parts of pyrrolidinodiaminopyrimidine oxide, 1.25-2.25 parts of angelica 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 a stabilizer; the stabilizer comprises maltodextrin and distearyl phthalamide.

[0007] In the hair styling composition of the present invention:

[0008] Pyrrolidinodiaminopyrimidine oxide (PDPO) acts as a potassium channel opener, effectively promoting the proliferation of hair papilla cells and stimulating hair follicle regeneration. It also nourishes hair follicles by dilating blood vessels, increasing nutrients and oxygen to the hair roots. It also accelerates new hair growth by optimizing the hair follicle growth cycle. Pyrrolidinodiaminopyrimidine oxide can also reduce serum levels of 5α-reductase, androgen receptors, and dihydrotestosterone, demonstrating effective prevention and treatment of common hair loss types such as androgenic alopecia.

[0009] Traditional Chinese Medicine believes that "hair is the residue of blood," and hair growth is closely related to blood saturation. Angelica extract has the benefits of nourishing blood and qi, activating blood circulation, and promoting blood circulation, providing adequate nutrients to hair follicles, thereby promoting hair growth. Angelica extract also has anti-inflammatory and antioxidant properties, which can reduce scalp inflammation, alleviate symptoms such as itching, redness, and swelling, reduce oxidative stress damage to hair follicle cells, protect their normal function, and improve scalp health.

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

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

[0012] In the present invention, pyrrolidino diaminopyrimidine oxide is used as the main active substance for promoting hair growth, and angelica extract, tripeptide-1 copper and hexapeptide-3 are compounded as auxiliary active substances. It can open the scalp potassium channel opener and promote the proliferation of hair papilla cells while achieving the effects of relieving scalp inflammation, slowing down 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, the present invention utilizes water-insoluble distearylphthalamide and water-soluble maltodextrin as stabilizers, achieving multiple stabilizing effects. This significantly enhances the stability of the hair-styling composition, ensuring it resists stratification, precipitation, or degradation under diverse environments. Furthermore, glycerin not only serves as a solvent for pyrrolidinodiaminopyrimidine oxide, angelica extract, and distearylphthalamide but also serves as a moisturizing component, enhancing the moisturizing efficacy of the hair-styling composition and improving its overall effectiveness.

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

[0015] Preferably, the hair growth composition comprises the following components in parts by weight: 1.25 parts of pyrrolidino diamino pyrimidine oxide, 1.25 parts of pyrrolidino diamino pyrimidine oxide, 1.75 parts of angelica extract, 1.25 parts of tripeptide-1 copper, 0.013 parts of hexapeptide-3, 45.813 parts of glycerol and 15 parts of stabilizer.

[0016] Experimental research found that when pyrrolidinopyrimidine oxide is combined with the three auxiliary active ingredients of angelica extract, tripeptide-1 copper, and hexapeptide-3 in the above-mentioned optimal dosage ratio, the components cooperate with each other and can exert an ideal synergistic effect to improve the skin permeability of the composition, significantly enhance its hair growth, oil control and barrier repair effects, and achieve excellent hair solidification, anti-hair loss and other effects.

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

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

[0019] Preferably, the preparation method of the angelica extract includes any one of the following three methods:

[0020] Method 1:

[0021] Mixing angelica root powder and water, heating and filtering to obtain a filtrate, and concentrating and drying the filtrate to obtain an angelica extract;

[0022] Method 2:

[0023] The angelica root powder and glacial acetic acid are mixed, ultrasonically treated and washed to obtain a mixture, a composite extractant is added to the mixture, ultrasonically treated twice, and then filtered, the filtrate is collected, and the filtrate is concentrated and dried to obtain the angelica extract;

[0024] Method 3:

[0025] S1. Mixing angelica rhizome powder and water, heating and filtering to obtain a filter residue and a primary filtrate;

[0026] S2, concentrating and drying the primary filtrate in step S1, and obtaining a powder as the primary extract;

[0027] S3, adding glacial acetic acid to the filter residue in step S1, ultrasonically treating and washing to obtain a mixture;

[0028] S4, adding a composite extractant to the mixture, performing a second ultrasonic treatment and filtering to obtain a secondary filtrate;

[0029] S5, performing secondary concentration and secondary drying on the secondary filtrate of step S4, and obtaining a powder as the secondary extract;

[0030] S6. Mixing the primary extract and the secondary extract to obtain the angelica extract.

[0031] More preferably, the preparation method of the angelica extract comprises the following steps:

[0032] S1. Mixing angelica rhizome powder and water, heating and filtering to obtain a filter residue and a primary filtrate;

[0033] S2, concentrating and drying the primary filtrate in step S1, and obtaining a powder as the primary extract;

[0034] S3, adding glacial acetic acid to the filter residue in step S1, ultrasonically treating and washing to obtain a mixture;

[0035] S4, adding a composite extractant to the mixture, performing a second ultrasonic treatment and filtering to obtain a secondary filtrate;

[0036] S5, performing secondary concentration and secondary drying on the secondary filtrate of step S4, and obtaining a powder as the secondary extract;

[0037] S6. Mixing 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 rhizome powder to water is 1:(2-5);

[0040] (II) In step S1, the heating treatment temperature is 60-85° C. and the heating treatment time is 4-7 hours;

[0041] (III) In step S2, the concentration method includes concentration under reduced pressure, and the temperature of the concentration under reduced pressure is 60-85° C.;

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

[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° C., the power of the ultrasonic treatment is 300-500 W, and the time of the ultrasonic treatment is 30-60 min;

[0045] (VII) In step S4, the mass ratio of the mixture to the composite extractant is 1:(3-8); the composite extractant comprises 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° C., the power of the secondary ultrasonic treatment is 300-500 W, and the time of the secondary ultrasonic treatment is 1-3 hours;

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

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

[0049] Preferably, in step S4, the composite extractant comprises 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] The present invention uses water extraction and composite organic solvent extraction to effectively extract the rhizomes of Angelica sinensis, and then mixes the substances extracted by the two methods to form the Angelica sinensis extract of the present invention. The water extraction method can extract polysaccharides (such as heteropolysaccharides composed of monosaccharides such as D-glucose, D-xylose, and D-galactose), organic acids, amino acids, and some coumarin-type active substances from the rhizomes of Angelica sinensis. The composite organic solvent extraction method can effectively extract volatile active substances such as polyphenols, flavonoids, and saponins from the rhizomes of Angelica sinensis. The two different extraction methods are used to extract the rhizomes of Angelica sinensis in succession, making full use of the filter residue of the rhizomes of Angelica sinensis after water extraction. The Angelica sinensis extract finally obtained is not only rich in active components soluble in water, but also rich in active components soluble in organic solvents. When the hair growth composition is subsequently prepared, the Angelica sinensis extract is also more conducive to the transdermal absorption of the comparable formula, exerting a synergistic effect, and better achieving the comparable hair growth effect.

[0052] During the water extraction process, the angelica rhizome powder is fully swollen in the step of heating treatment. After the water extraction is completed to obtain the filter residue, the angelica rhizome powder is pretreated with glacial acetic acid before being extracted with a composite extractant. The purpose of the pretreatment is to destroy the fully swollen angelica cell walls with the glacial acetic acid, thereby increasing the permeability of the cells. This is more conducive to the dissolution of active substances such as polyphenols, flavonoids, and saponins when an organic solvent is subsequently used for extraction.

[0053] The present invention prepares the angelica extract into a powdered form for the following purposes: (1) to fully remove the organic solvent remaining in the composite organic solvent extraction process, reduce the irritation of the angelica extract, and make the Shengfa Kebilu composition safer; (2) to be more conducive to maintaining the stability of the angelica extract; and (3) to increase the proportion of the active components of the angelica extract in the subsequent composition, which is more conducive to the angelica extract to play a synergistic and synergistic role.

[0054] In a second aspect, the present invention provides a method for preparing the hair styling composition, comprising the following steps:

[0055] (1) mixing pyrrolidinodiaminopyrimidine oxide, angelica extract, distearyl phthalamide and a solvent to obtain phase A;

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

[0057] (3) Mixing the phase A and the phase B and homogenizing them to obtain the hair-raising composition.

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

[0059] Preferably, the high-speed shear dispersion treatment is carried out at a rotation speed of 8000-12000 rpm and a time of 20-40 min.

[0060] Preferably, the high-pressure homogenization treatment is carried out under a pressure of 50-120 MPa and the number of cycles is 3-6 times.

[0061] In the present invention, the prepared phase A and phase B are fully mixed by homogenization, so that the hair styling composition forms a uniform system, further improving the stability of the composition.

[0062] In a third aspect, the present invention provides use of the hair stimulating composition in preparing hair products.

[0063] Preferably, the mass percentage of the hair volumizing composition in the hair product is 1-20%.

[0064] The hair product of the present invention is any preparation conventionally prepared in the field of hair products, and can be formulated into, for example, solutions, suspensions, emulsions, pastes, gels, creams, water, powders, soaps, detergents containing surfactants, oils, powder creams, 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 essential oil, shampoo, shampoo soap, shampoo powder, hair mask, conditioner, hair spray, hair gel and hair lotion.

[0066] Compared with the prior art, the present invention has the following beneficial effects:

[0067] (1) In order to solve the problems of low water solubility of clopidogrel and poor compatibility in hair products, the present invention provides a clopidogrel composition for hair growth. In the present invention, active ingredients such as pyrrolidinodiaminopyrimidine oxide (clopidogrel), angelica extract, tripeptide-1 copper, and hexapeptide-3 are combined, and stabilizers and solvent components are compounded. The resulting hair growth composition system is uniform, and clopidogrel is evenly dispersed in a water-soluble solvent, which is beneficial to enhancing the transdermal absorption effect of clopidogrel and improving the compatibility of clopidogrel with other hair raw materials.

[0068] (2) The Shengfa Kebilu composition of the present invention is compounded with water-soluble and water-insoluble active ingredients, so that pyrrolidino diaminopyrimidine oxide (kebilu), angelica extract, tripeptide-1 copper, and hexapeptide-3 can play a synergistic role, which can well promote the expression of alkaline phosphatase in dermal papilla cells, inhibit the secretion of oil in sebaceous gland cells, and promote the migration of keratinocytes. Alkaline phosphatase is one of the molecular markers of hair follicle dermal papilla cells, and its expression level can reflect the activity and functional state of dermal papilla cells; the increase in alkaline phosphatase expression can activate the Wnt / β-catenin signaling pathway, which plays a key role in the formation of hair follicles and the growth of hair. Activating this pathway can promote the proliferation and differentiation of hair follicle dermal papilla cells, thereby promoting hair growth. The oil production of sebaceous gland cells is inhibited, which means that the composition has an oil control effect, can reduce the secretion of scalp oil, and alleviate the problem of seborrheic alopecia. The enhanced migration of keratinocytes indicates that the Shengfa Kobilu composition has the effect of repairing the scalp barrier, accelerating the repair and reconstruction of the skin barrier, promoting the normal growth of hair follicle cells in the scalp, and promoting hair growth and hair growth. In summary, the Kobilu composition of the present invention has multiple benefits, promoting hair growth in multiple dimensions while also strengthening and preventing hair loss, thereby maintaining a lush and full head of hair.

[0069] (3) The present invention uses water-soluble maltodextrin and water-insoluble distearylphthalamide as solvents for the system, thereby achieving multiple stabilizing effects, maintaining the stability of the system, and improving the usability of the comparably formulated composition in the formulation. DETAILED DESCRIPTION

[0070] To better illustrate the purpose, technical solutions and advantages of the present invention, the present invention will be further described below in conjunction with specific embodiments. Those skilled in the art should understand that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.

[0071] Unless otherwise specified, all raw materials involved in the following examples and comparative examples are commercially available general 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] The present embodiment 1-5 provides a hair-raising composition, the specific formula of which is shown in Table 1 (total weight parts is 100 parts). The preparation method of the composition comprises the following steps:

[0075] (1) mixing pyrrolidinodiaminopyrimidine oxide, angelica extract, distearyl phthalamide and glycerin to obtain phase A;

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

[0077] (3) Phase A and phase B are mixed, and the mixture is homogenized at 80 MPa for 4 cycles to obtain the hair-raising and comparable composition.

[0078] The preparation process of the angelica extract includes:

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

[0080] S2, the primary filtrate was concentrated under reduced pressure and spray-dried at 70°C (inlet air temperature was 100°C; outlet air temperature was 60°C), and the obtained powder was the primary extract;

[0081] S3, adding 1.5 times by weight of glacial acetic acid to the filter residue of step S1, ultrasonically treating the filter residue at 30° C. and 400 W for 40 min, and rinsing the filter residue with deionized water three times to remove the glacial acetic acid to obtain a mixture;

[0082] S4. Add 5 times the mass of a composite extractant of ethanol, glycerol, and petroleum ether to the mixture (the volume ratio of ethanol, glycerol, and petroleum ether is 6:3:1), perform a second ultrasonic treatment (at 45° C., at 400 W for 2 h), and then filter to obtain a secondary 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), and the obtained powder is the secondary extract;

[0084] S6. Mixing the primary extract and the secondary extract to obtain an angelica extract.

[0085] Table 1 Formula of the hair-raising and comparable composition described in Examples 1-5 (parts by weight)

[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 sinensis extract is different.

[0089] The preparation process of the angelica extract described in this embodiment comprises the following steps:

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

[0091] S2, the primary filtrate was concentrated under reduced pressure and spray-dried at 60°C (inlet air temperature was 110°C; outlet air temperature was 70°C), and the obtained powder was the primary extract;

[0092] S3, adding 2 times the mass of glacial acetic acid to the filter residue of step S1, ultrasonically treating the filter residue at 20° C. and 300 W for 60 min, and rinsing the filter residue with deionized water 5 times to remove the glacial acetic acid to obtain a mixture;

[0093] S4, adding 3 times by mass of a composite extractant of ethanol, glycerol, and petroleum ether (the volume ratio of ethanol, glycerol, and petroleum ether is 4.5:4:1.5) to the mixture, performing a second ultrasonic treatment (at 40° C., at 300 W for 3 h), and then filtering to obtain a secondary 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), and the obtained powder is the secondary extract;

[0095] S6. Mixing the primary extract and the secondary extract to obtain an 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 sinensis extract is different.

[0098] The preparation process of the angelica extract described in this embodiment comprises the following steps:

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

[0100] S2, the primary filtrate is concentrated under reduced pressure and spray-dried at 85°C (inlet air temperature is 90°C; outlet air temperature is 60°C), and the obtained powder is the primary extract;

[0101] S3, adding 0.8 times by weight of glacial acetic acid to the filter residue of step S1, ultrasonically treating the filter residue at 35° C. and 500 W for 30 min, and rinsing the filter residue with deionized water twice after the ultrasonic treatment to remove the glacial acetic acid, thereby obtaining a mixture;

[0102] S4. Add 8 times by weight 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 (at 50° C., 500 W for 1 h), and then filter to obtain a secondary filtrate;

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

[0104] S6. Mixing the primary extract and the secondary extract to obtain an 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 sinensis extract is different.

[0107] The preparation process of the angelica extract described in this embodiment comprises the following steps:

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

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

[0112] The preparation process of the angelica extract described in this embodiment comprises the following steps:

[0113] S1. Mixing angelica root powder and 1.5 times the mass of glacial acetic acid, ultrasonically treating the mixture at 30°C and 400W for 40 min, and rinsing with deionized water three times to remove the glacial acetic acid to obtain a mixture;

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

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

[0116] Comparative Examples 1-10

[0117] Comparative Examples 1-10 provide a hair-raising composition, the specific formula of which is shown in Table 2 (total weight parts is 100 parts). The preparation method of the composition is the same as that of Example 1, the only difference being the formula.

[0118] Table 2 Formula of the hair-raising and comparable composition described in Comparative Examples 1-10 (parts by weight)

[0119]

[0120]

[0121] Comparative Example 11

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

[0123] Comparative Example 12

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

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

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

[0127] S2, the primary filtrate was concentrated under reduced pressure and spray-dried at 70°C (inlet air temperature was 100°C; outlet air temperature was 60°C), and the obtained powder was the primary extract;

[0128] S3, adding 1.5 times by weight of glacial acetic acid to the filter residue of step S1, ultrasonically treating the filter residue at 30° C. and 400 W for 40 min, and rinsing the filter residue with deionized water three times to remove the glacial acetic acid to obtain a mixture;

[0129] S4. Add 5 times the mass of a composite extractant of ethanol, glycerol, and petroleum ether to the mixture (the volume ratio of ethanol, glycerol, and petroleum ether is 6:3:1), perform a second ultrasonic treatment (at 45° C., at 400 W for 2 h), and then filter to obtain a secondary 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), and the obtained powder is the secondary extract;

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

[0132] Comparative Example 13

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

[0134] Comparative Example 14

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

[0136] Comparative Example 15

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

[0138] Comparative Example 16

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

[0140] Comparative Example 17

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

[0142] Effect Examples

[0143] 1. Stability test:

[0144] Test sample: the hair-storing and hair-comparing compositions described in Examples 1-9 and Comparative Examples 1-17;

[0145] Testing Procedure: 10 mL of each of the hair growth compositions of Examples 1-9 and Comparative Examples 1-17 were placed in colorless, transparent PE sample bottles. These samples were placed at 4°C, 25°C, and 45°C, and the delamination of the samples was observed at month 0 and month 1. The results are shown in Table 3.

[0146] Table 3

[0147]

[0148]

[0149]

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

[0151] When comparative examples 9-10 used maltodextrin and distearyl phthalamide as stabilizers respectively, the stability of the prepared Shengfa Kebi Luo composition system was poor. After being placed at different temperatures for one month, different degrees of stratification occurred. Comparative example 12 replaced the angelica extract with a Panax notoginseng root extract with similar efficacy. Although the extraction process of the Panax notoginseng root extract and the angelica extract was the same, the species of the plants were different, and the active substances of the plant extracts finally obtained were different. The synergistic effects of the components in the system were also different, resulting in the stability of the final composition being still low. Similarly, when comparative example 14 replaced hexapeptide-3 with acetyl hexapeptide-8, comparative example 15 replaced the aqueous phase stabilizer with hydrolyzed corn starch, comparative example 16 replaced the oil phase stabilizer with dimethyl silicone oil, and comparative example 17 replaced the oil phase solvent with 1,2-butanediol, the changes in the types of polypeptides, stabilizers, and solvents would affect the compatibility between the components, ultimately leading to changes in the stability of the system and the occurrence of different degrees of stratification.

[0152] 2. Promote hair growth test:

[0153] Test Principle: The human hair cycle consists of the anagen, catagen, and telogen phases. The induction and maintenance of the anagen phase of hair follicles determines the time of hair regeneration and the length of the hair shaft. Therefore, factors that promote the entry of hair follicles into the anagen phase and maintain their proliferation state are key to promoting luxuriant hair growth. Studies have confirmed that alkaline phosphatase (ALP) is a molecular marker for dermal papilla cells (DPCs) of hair follicles. It can enhance the activity of DPCs by participating in cell signaling in dermal papilla cells of hair follicles, thereby promoting the growth and development of hair follicles. This test determines the effectiveness of the test sample in promoting hair growth by measuring the relative expression of the ALP gene in dermal papilla cells.

[0154] Test samples: the Shengfa Kebiluo compositions of Examples 1-9 and Comparative Examples 1-17 were prepared into solutions with a mass concentration of 1% using H-DMEM culture medium containing 10% FBS (hereinafter referred to as culture medium) as a solvent.

[0155] Test steps: DPCs cells in the logarithmic phase were seeded in 6-well culture plates (2×10 51 mL of culture medium was added to the blank control group and 1 mL of test sample was added to the sample group, and the cells were cultured for another 24 h. After the culture was completed, total RNA from DPCs cells in each well was extracted and reverse transcribed for fluorescence quantitative PCR. Real-time fluorescence quantitative results were obtained using 2 －△△CT The test results are shown in Table 4.

[0156] 3. Oil control effect test:

[0157] In this test, human sebaceous gland cells SZ95 were selected to construct an in vitro acne model. The sebum secretion process of human skin was simulated by the oil secretion of SZ95 cells. The oil content of sebaceous gland cells was qualitatively and quantitatively detected by fluorescence quantitative method, so as to evaluate whether the test substance has the effect of controlling oil.

[0158] Test sample: The Shengfa Kebiluo composition of Examples 1-9 and Comparative Examples 1-17 was prepared into a solution with a mass concentration of 1% using H-DMEM containing 10% FBS and 10 μM testosterone culture medium as solvent.

[0159] Test steps: SZ95 cells in the logarithmic phase were seeded in 24-well culture plates (2×10 4 Cells / well) were added, culture medium was added, and the culture medium (10% FBS H-DMEM) was discarded after culturing at 5% CO2 and 37°C for 24 hours; then 0.5 mL of H-DMEM culture medium containing 10% FBS was added to the blank control group, 0.5 mL of 10 μM testosterone culture medium was added to the model control group, 0.5 mL of the test sample solution (containing 1% test sample and 10 μM testosterone) was added to the sample group, and the model control group and the test sample group were cultured for 24 hours, and the blank control group was cultured under the same conditions for 24 hours; after the modeling was completed, the culture medium was discarded, the cells were washed with PBS solution, and then stained with 3 mM Nile Red (Source Leaf Bio), incubated at 37°C in the dark for 10 minutes, washed with PBS, and the Nile Red fluorescence intensity was detected using a multifunctional microplate reader with an excitation wavelength of 485 nm / emission wavelength of 565 nm. The fluorescence grayscale value was converted by Image J 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-layer structure, which includes the basal layer, spinous layer, granular cell layer, clear layer, and the outermost non-living keratinocytes from the inside to the outside. Keratinocytes continuously divide, proliferate, differentiate and denucleate, and in this process gradually migrate to the outermost layer of the skin to form a skin barrier. The function of the skin barrier depends on the integrity of the brick wall structure of the stratum corneum. The repair function of the skin barrier mainly depends on the migration, proliferation and differentiation of keratinocytes. After the skin is damaged, keratinocytes will migrate to the damaged area to promote wound healing and reconstruction of the skin barrier. Therefore, the cell scratch test can be used to evaluate the effect of the test sample on the migration and repair ability of keratinocytes, thereby reflecting its effect on the skin barrier repair function.

[0162] Test sample: the Shengfa Kebiluo composition of Example 1-9 and Comparative Example 1-17 was prepared into a solution with a mass concentration of 3% using DMEM culture medium containing 1 wt% fetal bovine serum as a solvent.

[0163] Test steps: Keratinocytes in the logarithmic phase (i.e., cell suspension) were inoculated into culture inserts (4×10 5 Cells / mL) were collected for a blank control group and a test sample group. Each group consisted of two culture inserts with two wells each. 70 μL of cell suspension was inoculated into each well and cultured at 5% CO2 and 37°C for 24 h. When the cell confluence was above 95%, the scratched inserts in the 24-well plate were vertically removed using sterile tweezers. Each well was washed once with 1 mL of PBS solution. 1 mL of DMEM medium containing 1 wt% fetal bovine serum 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 0 h and 24 h, and the scratched area was photographed. The scratched 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] Where: S 24 is the scratch area at 24 h; S0 is the scratch area after 0 h.

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

[0168] Table 4

[0169]

[0170]

[0171] The results in Table 4 show that the hair-promoting kobelu composition of the present invention can increase the expression level of the alkaline phosphatase gene in dermal papilla cells, inhibit oil secretion in sebaceous gland cells, and promote the migration of keratinocytes, demonstrating that the hair-promoting kobelu composition of the present invention has excellent efficacy in promoting hair growth, controlling oiliness, and repairing hair barrier. Specifically, when the Angelica sinensis extracts described in Examples 8-9 were extracted using only water or a mixed solvent, the changes in the preparation process resulted in a certain degree of change in the types and proportions of the components in the composition, resulting in a certain degree of reduction in the growth, oiliness, and hair barrier repair effects of the prepared hair-promoting compositions compared to Example 1.

[0172] In comparative examples 1-6, any one or two of coccutaneous vine, angelica extract, tripeptide-1 copper and hexapeptide-3 are missing, and the proportion of other active substances is increased accordingly so that the total mass ratio of the active substances remains unchanged. The hair growth effect, oil control effect and barrier repair effect of the obtained hair growth composition are all reduced to varying degrees. In comparative examples 7-8, the dosage ratio of the above four active substances exceeds the specified range of the present invention. The hair growth effect, oil control effect and barrier repair effect of the composition are also reduced to a certain extent compared with the first embodiment. The above results show that the four active components of coccutaneous vine, angelica extract, tripeptide-1 copper, and hexapeptide-3 used in the present invention can only exert a better synergistic effect when compounded within a specific amount ratio range, thereby significantly enhancing the hair growth, oil control and barrier repair effects of the composition. None of the four components can be missing. In Comparative Examples 11-14, when the active ingredients in the compositions were replaced with functionally similar active ingredients, the overall hair growth and oil control effects of the resulting hair-promoting compositions also decreased to a certain extent. This demonstrates that the four active ingredients selected in the present invention cannot be conventionally replaced; only the interaction of the four specific ingredients maximizes the hair growth and oil control effects of the composition. Furthermore, when only maltodextrin or distearylphthalamide was used as a stabilizer in Comparative Examples 9-10, and when maltodextrin, distearylphthalamide, and glycerin were replaced with other similar substances in Comparative Examples 15-17, the systems became unstable, the active ingredients in the compositions easily precipitated, and the synergistic effect between the active ingredients was reduced, resulting in poor hair growth, oil control, and barrier repair effects of the final compositions.

[0173] Finally, it should be noted that the above embodiments are intended to illustrate the technical solutions of the present invention rather than 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 the technical solutions of the present invention may be modified or replaced by equivalents without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A hair growth and hair loss composition, characterized in that: The hair growth composition comprises the following components in parts by weight: 0.7-1.7 parts of pyrrolidinodiaminopyrimidine oxide, 1.25-2.25 parts of angelica 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 a stabilizer; The stabilizers include maltodextrin and distearylphthalamide.

2. The hair volumizing composition according to claim 1, wherein The hair growth composition comprises the following components in parts by weight: 0.9-1.55 parts of pyrrolidinodiaminopyrimidine oxide, 1.6-1.9 parts of angelica extract, 1-1.5 parts of tripeptide-1 copper, 0.01-0.015 parts of hexapeptide-3, 35-55 parts of glycerol and 11-18 parts of stabilizer.

3. The hair volumizing composition according to claim 2, wherein The hair growth composition comprises the following components in parts by weight: 1.25 parts of pyrrolidinodiaminopyrimidine oxide, 1.75 parts of angelica extract, 1.25 parts of tripeptide-1 copper, 0.013 parts of hexapeptide-3, 45.813 parts of glycerol and 15 parts of stabilizer.

4. The hair volumizing composition according to any one of claims 1 to 3, characterized in that: The preparation method of the angelica extract includes any one of the following three methods: Method 1: Mixing angelica root powder and water, heating and filtering to obtain a filtrate, and concentrating and drying the filtrate to obtain an angelica extract; Method 2: The angelica root powder and glacial acetic acid are mixed, ultrasonically treated and washed to obtain a mixture, a composite extractant is added to the mixture, ultrasonically treated twice, and then filtered, the filtrate is collected, and the filtrate is concentrated and dried to obtain the angelica extract; Method 3: S1. Mixing angelica rhizome powder and water, heating and filtering to obtain a filter residue and a primary filtrate; S2, concentrating and drying the primary filtrate in step S1, and obtaining a powder as the primary extract; S3, adding glacial acetic acid to the filter residue in step S1, ultrasonically treating and washing to obtain a mixture; S4, adding a composite extractant to the mixture, performing a second ultrasonic treatment and filtering to obtain a secondary filtrate; S5, performing secondary concentration and secondary drying on the secondary filtrate of step S4, and obtaining a powder as the secondary extract; S6. Mixing the primary extract and the secondary extract to obtain the angelica extract.

5. The hair volumizing composition according to claim 4, wherein The preparation method of the angelica extract comprises the following steps: S1. Mixing angelica rhizome powder and water, heating and filtering to obtain a filter residue and a primary filtrate; S2, concentrating and drying the primary filtrate in step S1, and obtaining a powder as the primary extract; S3, adding glacial acetic acid to the filter residue in step S1, ultrasonically treating and washing to obtain a mixture; S4, adding a composite extractant to the mixture, performing a second ultrasonic treatment and filtering to obtain a secondary filtrate; S5, performing secondary concentration and secondary drying on the secondary filtrate of step S4, and obtaining a powder as the secondary extract; S6. Mixing the primary extract and the secondary extract to obtain the angelica extract.

6. The hair volumizing composition according to claim 5, wherein Including at least one of the following (I)-(X): (I) In step S1, the mass ratio of the angelica rhizome powder to water is 1:(2-5); (II) In step S1, the heating treatment temperature is 60-85° C. and the heating treatment time is 4-7 hours; (III) In step S2, the concentration method includes concentration under reduced pressure, and the temperature of the concentration under reduced pressure is 60-85° C.; (IV) In step S2, the drying method includes spray drying, and the conditions of the spray drying are: an inlet air temperature of 90-110°C and an outlet air temperature of 50-70°C; (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° C., the power of the ultrasonic treatment is 300-500 W, and the time of the ultrasonic treatment is 30-60 min; (VII) In step S4, the mass ratio of the mixture to the composite extractant is 1:(3-8); the composite extractant comprises at least two of ethanol, glycerol, butanediol, and petroleum ether; (VIII) In step S4, the temperature of the secondary ultrasonic treatment is 40-50° C., the power of the secondary ultrasonic treatment is 300-500 W, and the time of the secondary ultrasonic treatment is 1-3 hours; (IX) In step S5, the secondary concentration method includes vacuum concentration, and the vacuum concentration temperature is 40-60° C.; (X) In step S5, the secondary drying method includes spray drying, and the conditions of the spray drying are: inlet air temperature is 70-90°C; outlet air temperature is 40-50°C.

7. The hair volumizing composition according to claim 1, wherein The mass ratio of the maltodextrin to distearylphthalamide is (8.5-13):(2.5-5).

8. The method for preparing the hair volumizing composition according to any one of claims 1 to 7, wherein: The following steps are involved: (1) mixing pyrrolidinodiaminopyrimidine oxide, angelica extract, distearyl phthalamide and glycerin to obtain phase A; (2) mixing tripeptide-1 copper, hexapeptide-3, maltodextrin and water to obtain phase B; (3) Mixing the phase A and the phase B and homogenizing them to obtain the hair-raising composition.

9. Use of the hair stimulating composition according to any one of claims 1 to 7 in preparing hair products.

10. The use according to claim 8, characterized in that The mass percentage of the hair-nourishing composition in the hair product is 1-20%; The hair products include at least one of scalp care essence, scalp care water, scalp nourishing cream, scalp massage cream, hair essence, hair essential oil, shampoo, shampoo soap, shampoo powder, hair mask, hair conditioner, hair spray, hair gel and hair lotion.

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