CN117598920A - Hair loss preventing and hair growing composition and preparation method and application thereof - Google Patents
Hair loss preventing and hair growing composition and preparation method and application thereof Download PDFInfo
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- CN117598920A CN117598920A CN202311566736.0A CN202311566736A CN117598920A CN 117598920 A CN117598920 A CN 117598920A CN 202311566736 A CN202311566736 A CN 202311566736A CN 117598920 A CN117598920 A CN 117598920A
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
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Abstract
The invention relates to the technical field of skin care products, and further relates to an anti-hair loss hair-growing composition, a preparation method and application thereof. The raw materials comprise, by mass: pyrimidine derivative 0.1-2.5 wt%, adenosine 0.2-1.5 wt%, conditioner 0.01-6 wt% and solvent for the rest. The composition of the invention activates hair follicles endogenously and stimulates hair follicle regeneration through the synergistic effect of the components; exogenous toughen scalp barriers to resist oxidative stress; the technical effects of improving the hair growth speed and improving the hair color and scalp state in a multi-dimensional manner are achieved.
Description
Technical Field
The invention relates to the technical field of skin care products, in particular to the field of IPC A61K8, and further relates to an anti-hair loss hair growth composition, a preparation method and application thereof.
Background
Alopecia not only affects the image of a person, but also causes great psychological stress to a patient. At present, the age of the mainstream alopecia crowd shows a trend of younger due to the acceleration of the social life rhythm and the irregular life style of the work and rest.
Hair grows from the follicle, which absorbs nutrients from the body through the follicle, supporting hair growth. The growth of hair follicles exhibits periodicity, including a cell growth phase, a cell withdrawal phase, and a cell rest phase. Therefore, hair loss is closely related to hair follicles, and when certain factors such as irregular life habits, mental stress and the like have negative effects on hair follicles, the hair follicle cells have shortened growth period, cell withdrawal period and cell resting period, hair follicles shrink and degenerate, and further the hair follicle growth cycle is changed, so that hair is desulfurized in advance or hair growth is slow or even hair cannot grow normally.
Research reports that more than 90% of alopecia in clinical medicine is androgenetic alopecia/seborrheic alopecia, and the alopecia occurs for men and women, and is characterized in that: the hair follicle growth cycle is changed, the growth period is shortened, the resting period is prolonged, and finally the hair follicle micromation is caused; the symptoms are as follows: excessive secretion of grease, and irritation to scalp causes scalp erythema, dandruff, itching, odor, folliculitis, etc.; the generation mechanism comprises: (1) Androgen testosterone is converted into Dihydrotestosterone (DHT) with stronger activity under the action of 5 alpha reductase, androgen and A Receptor (AR) thereof are combined to form a DHT-AR complex, the DHT-AR complex is transferred into a cell nucleus, a specific gene is activated to generate specific protein, proliferation or differentiation of hair follicle cells is regulated, so that the growing period of hair is shortened, the hair enters a retrograde period prematurely, and the hair follicle is converted into a miniature hair follicle; (2) Follicular inflammatory cells cause connective tissue remodeling, which in turn causes progressive fibrosis around the hair follicle, damaging the hair follicle stem cells, and deregulating the hair follicle growth cycle; (3) The oxidative stress reaction releases 1L-1 alpha stored in the cells to accelerate and aggravate alopecia, and simultaneously excessive oxygen free radicals can damage the mitochondrial function of each cell in the hair follicle, so that the cells age and die, and further the hair follicle is damaged, thereby causing alopecia; (4) 1L-1 alpha, 1L-1 beta and other interleukins have inhibitory effects on hair follicle growth.
At present, the common medicament for treating alopecia on the market is 5% minoxidil, but researches show that side effects such as contact dermatitis, acceleration of heartbeat, headache and the like are easy to occur in the using process. Besides, natural plant extract components are adopted for hair loss prevention and hair growth, for example, chinese patent CN202111356865 discloses a hair loss prevention composition, a hair loss prevention washing and protecting product and a preparation method thereof, wherein the hair loss prevention composition comprises the following raw materials: fructus Phyllanthi extract, folium Camelliae sinensis extract, western herba Stachydis Japonicae extract, european larch extract and fructus Mali Pumilae extract. The data of this protocol may indicate that VEGF growth factor can be promoted; however, no data is shown to be effective in the hair growth situation.
Disclosure of Invention
The invention provides an anti-hair loss and hair growth composition, which comprises the following raw materials in percentage by mass: pyrimidine derivative 0.1-2.5 wt%, adenosine 0.1-1.5 wt%, conditioner 0.01-6 wt% and solvent for the rest.
Preferably, the mass ratio of the pyrimidine derivative to the adenosine is (0.1-2): (0.5-1).
Preferably, the mass ratio of the pyrimidine derivative to the adenosine is (0.1-1.5): (0.5-1).
Preferably, the pyrimidine derivative is selected from one or two of diaminopyrimidine oxide and pyrrolidinyl diaminopyrimidine oxide.
Preferably, the pyrimidine derivative comprises a diaminopyrimidine oxide, a pyrrolidinyl diaminopyrimidine oxide.
Preferably, the mass ratio of the diaminopyrimidine oxide to the pyrrolidinyl diaminopyrimidine oxide is (0.5 to 1.5): (0.1-1).
Preferably, the mass ratio of the diaminopyrimidine oxide to the pyrrolidinyl diaminopyrimidine oxide is (0.5-1): (0.5-1).
Preferably, the mass ratio of the diaminopyrimidine oxide to the pyrrolidinyl diaminopyrimidine oxide is 1:0.5.
the applicant found during the research that when pyrimidine derivatives only exist diaminopyrimidine oxide in the system of the present application, the prepared composition has a certain effect of stimulating hair growth, but is far from minoxidil, and the melanin index of the skin can be improved only after 12 days of using the composition. Whereas the melanin index of the skin is markedly increased after 10 days of use of the composition when the pyrrolidinyl diaminopyrimidine oxide is introduced, at the same time the applicant has unexpectedly found that when both the diaminopyrimidine oxide and the pyrrolidinyl diaminopyrimidine oxide are present in the present application, the addition amount of the pyrimidine derivative in the present application significantly affects the hair growth of the composition, only when the mass ratio of the pyrimidine derivative to adenosine is (0.1 to 2): (0.5-1), especially when the mass ratio of pyrimidine derivative to adenosine is (0.1-1.5): (0.5-1), the hair is significantly increased after 14 days of use of the composition, and when the mass percentage of pyrimidine derivative is more than 2%, the hair is not significantly increased even if the amount of conditioner is increased, and the applicant believes that the poor water-solubility raw materials in the system of the present application include not only diaminopyrimidine oxide and pyrrolidinyl diaminopyrimidine oxide, but also adenosine, which stimulates hair growth by promoting FGF-7 factor secretion and the growth rate of hair to achieve an anti-hair-loss hair-growing effect, but has limited solubility in water and is hardly soluble in ethanol, and when the mass ratio of pyrimidine derivative to adenosine is (0.1-1.5): (0.5-1), the pyrimidine derivative can promote the dissolution of adenosine to a certain extent, thereby fully playing the role of the composition in stimulating hair growth; and when the mass ratio of the pyrimidine derivative to the adenosine is not (0.1-1.5): in the range of (0.5 to 1), the solubility of both the pyrimidine derivative and adenosine is limited to a certain extent, thereby reducing the effect.
Preferably, the conditioning agent is selected from one or more of biota orientalis (PLATYCLADUS ORIENTALIS) leaf extract, amino acid, nicotinamide, panthenol, vitamin E derivatives, ceramide, peptides.
Preferably, the conditioning agent comprises biota orientalis extract, amino acids, nicotinamide, panthenol and vitamin E.
Preferably, the mass ratio of the biota orientalis leaf extract, the amino acid, the nicotinamide, the panthenol and the vitamin E is (0.1-2): (0.02-0.3): (0.02-1): (0.05-1.5): (0.01-1).
Preferably, the mass ratio of the biota orientalis leaf extract, the amino acid, the nicotinamide, the panthenol and the vitamin E is (0.1-1): (0.02-0.2): (0.1-0.2): (0.1-0.5): (0.05-0.2).
Preferably, the biota orientalis extract: the mass ratio of the amino acid to the nicotinamide to the panthenol to the vitamin E is 0.4:0.025:0.2:0.11:0.1.
in order to enhance the effect of the composition on stimulating hair growth, the applicant has found that when the conditioner comprises cacumen Platycladi extract, amino acid, nicotinamide, panthenol and vitamin E, the conditioner can work together with diaminopyrimidine oxide and pyrrolidinyldiaminopyrimidine oxide to enhance the anti-hair loss and hair growth effects of the composition, and the applicant has found that the mass ratio of cacumen Platycladi extract, amino acid, nicotinamide, panthenol and vitamin E has a great influence on the hair growth effects of the composition, and the mass ratio of cacumen Platycladi extract, amino acid, nicotinamide, panthenol and vitamin E is (0.1-1): (0.02-0.2): (0.1-0.2): (0.1-0.5): (0.05-0.2), after the composition is used for 14 days, the hair is obviously increased, and the melanin index is obviously increased; meanwhile, the applicant also found that when the mass ratio of the biota orientalis extract, the amino acid, the nicotinamide, the panthenol and the vitamin E is 0.4:0.025:0.2:0.11: at 0.1, the effect of the composition on hair follicle length was approximately 5% minoxidil after 14 days of application.
Preferably, the amino acid is at least one selected from arginine, lysine and cysteine.
Preferably, the amino acid is arginine.
In the prior art, the diaminopyrimidine oxide and the pyrrolidinyl diaminopyrimidine oxide have poor water solubility and skin permeability, and most solvents are ethanol, so that the diaminopyrimidine oxide and the pyrrolidinyl diaminopyrimidine oxide are prepared into tincture for use, but the application range of the diaminopyrimidine oxide is limited due to the large irritation of ethanol. In order to increase the solubility of the diaminopyrimidine oxide and the pyrrolidinyl diaminopyrimidine oxide while reducing its irritation; preferably, the solvent is a mixture of an alcohol compound and water.
Preferably, the alcohol compound accounts for 30-40% by mass.
Preferably, the alcohol compound is selected from one or more of ethanol, propylene glycol, butanediol and methyl propylene glycol.
Preferably, the alcohol compound is selected from the group consisting of ethanol and methyl propylene glycol.
Preferably, the mass ratio of the ethanol to the methyl propylene glycol is (2.5-3.5): 1.
preferably, the anti-hair loss and hair growth composition comprises the following raw materials in percentage by mass: 1 to 2 percent of pyrimidine derivative, 0.5 to 1.5 percent of adenosine, 0.5 to 5 percent of conditioner and the balance of solvent.
The second aspect of the invention provides a preparation method of the hair-loss preventing and hair-growing composition, which comprises the following steps:
s1, weighing all raw materials according to mass percentage;
s2, mixing and stirring pyrimidine derivatives and alcohol compounds for 1-3 min to obtain a solution 1;
s3, adding water into the solution 1, and stirring to obtain a uniform and transparent solution to obtain a solution 2;
s4, adding amino acid into the solution 2, and uniformly stirring to obtain a solution 3;
s5, uniformly mixing vitamin E, adding the mixture into the solution 3, and uniformly stirring to obtain a solution 4;
s6, adding the biota orientalis extract, adenosine, nicotinamide and panthenol into the solution 4, and uniformly stirring to obtain the compound.
In a third aspect the present invention provides the use of an anti-hair loss hair growth composition for the preparation of personal care and scalp care products.
Preferably, the anti-hair loss hair growth composition is used for preparing essence.
Preferably, the preparation method of the essence comprises the following steps: adding sodium benzotriazole-based butylphenol sulfonate, a pH regulator, a chelating agent, a thickening agent, a solubilizer and pigment into the hair-growing composition, and uniformly mixing to obtain the hair-growing composition.
Preferably, the pH adjuster is citric acid.
Preferably, the chelating agent comprises EDTA-2Na and Spectrastat TM PHL (INCI: 1, 2-hexanediol, octanoyl hydroxamic acid, and 1, 3-propanediol); the mass ratio is 0.05:0.5.
preferably, the thickener comprises sodium polyacryl dimethyl taurate and xanthan gum; the mass ratio is 0.3:0.05.
preferably, the solubilizing agent is SOLUBILISANT LRI (INCI: PEG-40 hydrogenated castor oil, PPG-26 butanol polyether 26).
Preferably, the pigments include CI 19140 and CI 15985; the mass ratio is 0.01:0.005.
the applicant finds that the independent anti-hair-loss hair-growing composition has obvious color change at a high temperature of 50 ℃ in the experimental process, and when the composition is used for preparing essence, the obtained essence can exist stably at the high temperature of 50 ℃ and has excellent stability.
The beneficial effects are that:
1. the mass ratio of pyrimidine derivative to adenosine is (0.1-2): (0.5-1), especially when the mass ratio of pyrimidine derivative to adenosine is (0.1-1.5): (0.5-1), the hair is significantly increased after 14 days of application of the composition.
2. When the conditioner comprises the biota orientalis extract, amino acid, nicotinamide, panthenol and vitamin E, the conditioner can co-act with diaminopyrimidine oxide and pyrrolidinyl diaminopyrimidine oxide to improve the anti-hair loss and hair growth effects of the composition.
3. When the mass ratio of the biota orientalis leaf extract to the amino acid to the nicotinamide to the panthenol and the vitamin E is 0.4:0.025:0.2:0.11: at 0.1, the effect of the composition on hair follicle length was approximately 5% minoxidil after 14 days of application.
4. When the alcohol compound is selected from the combination of ethanol and methyl propylene glycol, the solubility of the diaminopyrimidine oxide and the pyrrolidinyl diaminopyrimidine oxide can be improved and the irritation can be reduced.
5. The composition is compounded by pyrimidine derivatives (diaminopyrimidine oxide and pyrrolidinyl diaminopyrimidine oxide), adenosine and conditioning agents (cacumen biotae extract, amino acid, nicotinamide, panthenol and vitamin E), and on one hand, the activity of 5 alpha-protoenzyme can be inhibited, so that testosterone conversion DHT (androgenic dihydrotestosterone) can be reduced; on the other hand, the hair follicle can be activated, the hair follicle regeneration is stimulated, the hair growth cycle is prolonged, and the growth of new hair is accelerated; in addition, the hair follicle can expand blood vessels of the scalp, improve blood microcirculation around hair follicles and increase nutrient substances supplied to hair follicle cells; improving the resistance of scalp to exogenous environmental stimulus and strengthening scalp barrier; the oxidation stress reaction is resisted, and the hair follicle blockage caused by scalp oxidation is avoided; thereby achieving the multi-dimensional anti-drop effect.
Drawings
FIG. 1 is a graph showing the effect of experimental groups on the appearance of whole hair on the back of androgenic alopecia model mice;
in the figure: a is a control group; b is a testosterone group; c is group 1; d is group 2; e is example 3; f is group 4; g is example 5; k is minoxidil group.
FIG. 2 is an appearance of topical hair on the back of androgenic alopecia mice from the experimental group;
in the figure: a is a control group; b is a testosterone group; c is group 1; d is group 2; e is example 3; f is group 4; g is example 5; k is minoxidil group.
FIG. 3 is a graph showing the effect of experimental groups on the back melanin index of androgenic alopecia mice;
in the figure: a is a control group; b is a testosterone group; c is group 1; d is group 2; e is example 3; f is group 4; g is example 5; k is minoxidil group.
FIG. 4 is a graph of HE staining of skin tissue of mice in the experimental group;
in the figure: a is a control group; b is a testosterone group; c is group 2; d is minoxidil group.
FIG. 5 is a statistical plot of hair follicle length in experimental mice;
in the figure: a is a control group; b is a testosterone group; c is group 2; d is minoxidil group.
FIG. 6 is a graph showing the stability of the hair loss preventing and hair growth composition of example 2 for 1 month;
in the figure: a is-18 ℃; b is a cycle (-18-50 ℃); c is 45 ℃; d is 50 ℃.
Fig. 7 is a graph of stability of the concentrate for 1 month;
in the figure: a is-18 ℃; b is a cycle (-18-50 ℃); c is 45 ℃; d is 50 ℃.
Detailed Description
Example 1
Example 1 provides an anti-hair loss and hair growth composition, which comprises the following raw materials in percentage by mass: pyrimidine derivative 1.5%, adenosine 0.5%, conditioner 1.245% and the balance of solvent.
The pyrimidine derivative is a diaminopyrimidine oxide.
The conditioner comprises cacumen Platycladi extract, amino acid, nicotinamide, panthenol and vitamin E.
The mass ratio of the biota orientalis leaf extract to the amino acid to the nicotinamide to the panthenol to the vitamin E is 0.1:0.025:1:0.11:0.01; the biota orientalis extract is purchased from Shanghai Jia Kai biological Co., ltd., trade name: hairdian AP.
The amino acid is arginine.
The solvent is a mixture of an alcohol compound and water.
The alcohol compound accounts for 40 percent by mass
The alcohol compound is selected from the group consisting of ethanol and methyl propylene glycol.
The mass ratio of the ethanol to the methyl propylene glycol is 3:1.
a preparation method of the hair-loss preventing and hair-growing composition comprises the following steps:
s1, weighing all raw materials according to mass percentage;
s2, mixing and stirring pyrimidine derivatives and alcohol compounds for 2min to obtain a solution 1;
s3, adding water into the solution 1, and stirring to obtain a uniform and transparent solution to obtain a solution 2;
s4, adding amino acid into the solution 2, and uniformly stirring to obtain a solution 3;
s5, uniformly mixing vitamin E, adding the mixture into the solution 3, and uniformly stirring to obtain a solution 4;
s6, adding the biota orientalis extract, adenosine, nicotinamide and panthenol into the solution 4, and uniformly stirring to obtain the compound.
Example 2
Example 2 provides an anti-hair loss and hair growth composition, which comprises the following raw materials in percentage by mass: pyrimidine derivative 1.5%, adenosine 0.5%, conditioner 0.835% and the balance of solvent.
The pyrimidine derivative is a combination of a diaminopyrimidine oxide and a pyrrolidinyldiaminopyrimidine oxide.
The mass ratio of the diaminopyrimidine oxide to the pyrrolidinyl diaminopyrimidine oxide is 1:0.5.
the conditioner comprises cacumen Platycladi extract, amino acid, nicotinamide, panthenol and vitamin E.
The mass ratio of the biota orientalis leaf extract to the amino acid to the nicotinamide to the panthenol to the vitamin E is 0.4:0.025:0.2:0.11:0.1; the biota orientalis extract is purchased from Shanghai Jia Kai biological Co., ltd., trade name: hairdian AP.
The amino acid is arginine.
The solvent is a mixture of an alcohol compound and water.
The alcohol compound accounts for 40 percent by mass
The alcohol compound is selected from the group consisting of ethanol and methyl propylene glycol.
The mass ratio of the ethanol to the methyl propylene glycol is 3:1.
a preparation method of the hair-loss preventing and hair-growing composition comprises the following steps:
s1, weighing all raw materials according to mass percentage;
s2, mixing and stirring pyrimidine derivatives and alcohol compounds for 2min to obtain a solution 1;
s3, adding water into the solution 1, and stirring to obtain a uniform and transparent solution to obtain a solution 2;
s4, adding amino acid into the solution 2, and uniformly stirring to obtain a solution 3;
s5, uniformly mixing vitamin E, adding the mixture into the solution 3, and uniformly stirring to obtain a solution 4;
s6, adding the biota orientalis extract, adenosine, nicotinamide and panthenol into the solution 4, and uniformly stirring to obtain the compound.
Example 3
Example 3 provides an anti-hair loss and hair growth composition, which comprises the following raw materials in percentage by mass: pyrimidine derivative 0.6%, adenosine 0.5%, conditioner 3.325%, and solvent balance.
The pyrimidine derivative is a combination of a diaminopyrimidine oxide and a pyrrolidinyldiaminopyrimidine oxide.
The mass ratio of the diaminopyrimidine oxide to the pyrrolidinyl diaminopyrimidine oxide is 0.5:0.1.
the conditioner comprises cacumen Platycladi extract, amino acid, nicotinamide, panthenol and vitamin E.
The mass ratio of the biota orientalis leaf extract to the amino acid to the nicotinamide to the panthenol to the vitamin E is 2:0.025:0.2:1:0.1; the biota orientalis extract is purchased from Shanghai Jia Kai biological Co., ltd., trade name: hairdian AP.
The amino acid is arginine.
The solvent is a mixture of an alcohol compound and water.
The alcohol compound accounts for 40 percent by mass
The alcohol compound is selected from the group consisting of ethanol and methyl propylene glycol.
The mass ratio of the ethanol to the methyl propylene glycol is 3:1.
a preparation method of the hair-loss preventing and hair-growing composition comprises the following steps:
s1, weighing all raw materials according to mass percentage;
s2, mixing and stirring pyrimidine derivatives and alcohol compounds for 2min to obtain a solution 1;
s3, adding water into the solution 1, and stirring to obtain a uniform and transparent solution to obtain a solution 2;
s4, adding amino acid into the solution 2, and uniformly stirring to obtain a solution 3;
s5, uniformly mixing vitamin E, adding the mixture into the solution 3, and uniformly stirring to obtain a solution 4;
s6, adding the biota orientalis extract, adenosine, nicotinamide and panthenol into the solution 4, and uniformly stirring to obtain the compound.
Example 4
Example 4 provides an anti-hair loss and hair growth composition, which comprises the following raw materials in percentage by mass: pyrimidine derivative 0.9%, adenosine 0.5%, conditioner 1.75%, and solvent balance.
The pyrimidine derivative is a combination of a diaminopyrimidine oxide and a pyrrolidinyldiaminopyrimidine oxide.
The mass ratio of the diaminopyrimidine oxide to the pyrrolidinyl diaminopyrimidine oxide is 0.8:0.1.
the conditioner comprises cacumen Platycladi extract, amino acid, nicotinamide and vitamin E.
The mass ratio of the biota orientalis leaf extract to the amino acid to the nicotinamide to the vitamin E is 1:0.2:0.05:0.5; the biota orientalis extract is purchased from Shanghai Jia Kai biological Co., ltd., trade name: hairdian AP.
The amino acid is arginine.
The solvent is a mixture of an alcohol compound and water.
The alcohol compound accounts for 40 percent by mass
The alcohol compound is selected from the group consisting of ethanol and methyl propylene glycol.
The mass ratio of the ethanol to the methyl propylene glycol is 3:1.
a preparation method of the hair-loss preventing and hair-growing composition comprises the following steps:
s1, weighing all raw materials according to mass percentage;
s2, mixing and stirring pyrimidine derivatives and alcohol compounds for 2min to obtain a solution 1;
s3, adding water into the solution 1, and stirring to obtain a uniform and transparent solution to obtain a solution 2;
s4, adding amino acid into the solution 2, and uniformly stirring to obtain a solution 3;
s5, uniformly mixing vitamin E, adding the mixture into the solution 3, and uniformly stirring to obtain a solution 4;
s6, adding the biota orientalis extract, adenosine, nicotinamide and panthenol into the solution 4, and uniformly stirring to obtain the compound.
Example 5
Example 5 provides an anti-hair loss and hair growth composition, which comprises the following raw materials in percentage by mass: pyrimidine derivative 1.5%, adenosine 1%, conditioner 1.45%, and solvent balance.
The pyrimidine derivative is a combination of a diaminopyrimidine oxide and a pyrrolidinyldiaminopyrimidine oxide.
The mass ratio of the diaminopyrimidine oxide to the pyrrolidinyl diaminopyrimidine oxide is 0.5:1.
the conditioner comprises cacumen Platycladi extract, amino acid, nicotinamide, panthenol and vitamin E.
The mass ratio of the biota orientalis extract to the amino acid to the nicotinamide to the panthenol to the vitamin E is 0.6:0.2:0.05:0.5:0.1; the biota orientalis extract is purchased from Shanghai Jia Kai biological Co., ltd., trade name: hairdian AP.
The amino acid is arginine.
The solvent is a mixture of an alcohol compound and water.
The alcohol compound accounts for 40 percent by mass
The alcohol compound is selected from the group consisting of ethanol and methyl propylene glycol.
The mass ratio of the ethanol to the methyl propylene glycol is 3:1.
a preparation method of the hair-loss preventing and hair-growing composition comprises the following steps:
s1, weighing all raw materials according to mass percentage;
s2, mixing and stirring pyrimidine derivative alcohol compounds for 2min to obtain a solution 1;
s3, adding water into the solution 1, and stirring to obtain a uniform and transparent solution to obtain a solution 2;
s4, adding amino acid into the solution 2, and uniformly stirring to obtain a solution 3;
s5, uniformly mixing vitamin E, adding the mixture into the solution 3, and uniformly stirring to obtain a solution 4;
s6, adding the biota orientalis extract, adenosine, nicotinamide and panthenol into the solution 4, and uniformly stirring to obtain the compound.
Performance test:
efficacy test (one):
control group: no drug treatment;
testosterone group: testosterone propionate injection, a mouse male pattern of baldness (the pattern is the same as the other groups except for normal controls);
minoxidil group: 5% minoxidil;
group of examples: the compositions prepared in examples 1 to 5.
1. Materials and methods
1. Material
1.1 laboratory animals
Male C57BL/6 mice, 6-7 weeks old, body weight (20+2) g, supplied by Beijing Vietnam Lihua laboratory animal technology Co., ltd, animal license number SCXK 2016-0006. It is fed in a 12h light/12 h dark environment to eat and drink water freely.
1.2 major instrumentation and reagents
4% paraformaldehyde (sonebao, china); isoflurane (ravode, china); paraffin microtomes (Thermo company, usa); small animal anesthesia machine (ravode corporation, china); inverted microscope (Olympus corporation, japan).
2. Method of
2.1 animal model building and Experimental grouping
Control, testosterone, example 1, example 2, example 3, example 4, example 5 and minoxidil. The day before the molding starts, the hair in the center of the back of the experimental animal is removed by a skin preparation knife, the skin preparation area of each mouse is about 2cm x3cm, the skin preparation area is dehaired by using dehairing paste, and the hair remained after the skin preparation is removed. After 24h of dehairing, testosterone solution (1 mg/mL) was applied to the other groups except the control group, which mice were given a dissolution control. Example 1, example 2, example 3, example 4, bid and minoxidil groups each apply the corresponding examples once a day, 0.1 mL/day, for 14 consecutive days.
2.2 Hair growth Condition
On days 3, 7, 10, 12 and 14 of administration, hair growth at the hair removal site was observed for each group of mice, and the whole back hair was photographed by a digital camera, and the effects of the group of example 1, the group of example 2, the group of example 3, the group of example 4 and the group of example 5 on hair growth of mice were observed.
2.3 skin glasses to observe changes in topical hair on the back
Changes in local hair growth on the backs of the mice in each group were examined by dermatoscopy on days 3, 7, 10, 12 and 14 of dosing, respectively.
2.4 color tester detects changes in skin color on the back
The change in melanin on the backs of the mice of each group was detected by a color tester on days 3, 7, 10, 12 and 14 of dosing, respectively.
2.5HE staining to observe follicular changes
At the end of the experiment, mice were anesthetized, back skin was taken, tissue was fixed with 4% paraformaldehyde, after trimming, dehydrating, and transparentizing, tissue was embedded, cut into 4 μm thick sections, further dewaxed, stained, dehydrated, transparentized and sealed, and hair follicle changes were observed under a 20-fold optical microscope.
2.6 statistical analysis
All data were statistically processed using SPSS17.0 software, and comparisons among groups were analyzed using one-way ANOVA, and data were averaged ± standard deviationRepresentation, P<0.05 is a statistical difference, P>A difference of 0.05 could not be considered.
2. Experimental results
1. Influence on the overall hair appearance of the back of androgenic alopecia mice
To observe the effect of each experimental group on the back hair growth of androgenic alopecia mice, the whole back skin of the mice was photographed on days 3, 7, 10, 12 and 14 of the medication, respectively. The results are shown in FIG. 1.
As can be seen from fig. 1, each group of back skin was pink with no hair growth on days 3 and 7.
On day 10, the control and minoxidil group back skin appeared visibly gray, the testosterone group back skin pink, the example 2 group, the example 4 group and the bid back portion were gray.
On day 12, the control and minoxidil groups changed from grey to black, the testosterone groups were grey elsewhere, and the other groups appeared grey to varying degrees, with example 2 groups being comparable to example 5 groups, appearing visibly grey, followed by example 4, example 3 and example 1 groups.
On day 14, the back of the minoxidil group of the control group was black, the testosterone group was gray, the black level of the example 2 group was obvious and comparable to that of the example 5 group, and the black levels of the groups were compared: example 2 group > example 5 group > example 4 group > example 3 group > example 1 group.
Results: the group of examples 2, 5, 4 and 3 can promote hair growth, wherein the external application effects of the group of examples 2 and 5 are most obvious.
2. Effects on topical hair growth on the back of androgenic alopecia mice
The local hair growth on the back of each group of mice was examined by a dermatoscope and the results are shown in fig. 2.
As can be seen from fig. 2, the back skin of each group of mice did not grow hair on days 3 and 7.
On day 10, the control group began growing sparse hair, and no apparent hair was found in the other groups.
On day 12, the control group showed more fine hair, minoxidil group showed hair, testosterone group did not show hair, but example 2, example 5, example 4 began to grow sparse hair.
On day 14, the control and minoxidil groups showed a significant increase in hair, testosterone group showed sparse hair, example 2 had a significant increase in hair, example 5 had a significant increase in hair, and then example 4, example 3, and example 1.
Results: the example 2 and example 5 groups significantly promote hair regrowth, followed by the example 4 and example 3 groups.
3. Influence on the extent of blackness of the back of androgenic alopecia mice
The degree of black on the backs of the mice in each group was measured by a color tester, and the results are shown in fig. 3.
As can be seen from fig. 3, there was no significant change in the back skin melanin index (P > 0.05) for each group on days 3 and 7.
On day 10, the control and minoxidil groups had very significantly elevated melanin index (P < 0.001), the example 2 group, the example 3 group, the example 4 group, and the example 5 group had significantly elevated melanin index (P < 0.05) compared to the testosterone group.
On day 12, the melanin index was significantly increased (P < 0.001) in the example 2, example 5 and minoxidil groups, and significantly increased (P < 0.05) in the example 3 and example 4 groups, as compared to the testosterone group.
On day 14, the melanin index was significantly increased (P < 0.001) for the example 2 and example 5 groups, and significantly increased (P < 0.01) for the example 4 group, as compared to the testosterone group.
Results: the group of example 2, the group of example 4 and the group of example 5 can obviously increase the black degree of the back of the mice and promote the hair growth.
4. Example 2 group effect on hair follicle Length in androgen-hair loss mice
The change in the length of the hair follicle of the mice was observed by HE staining, and the results are shown in fig. 4 and 5.
As can be seen from fig. 4 and 5: the testosterone group had the shortest hair follicle length, the control group had the longest hair follicle length, and the example 2 group significantly promoted hair follicle length (fig. 4).
Both the example 2 and minoxidil groups significantly promoted changes in hair follicle length compared to testosterone groups, with statistical significance (fig. 5, p < 0.001).
Results: example 2 group significantly promoted hair follicle growth and hair regeneration.
(II) stability test of anti-hair loss hair growth composition and essence of example 2:
the essence comprises the following raw materials in percentage by mass: 1.5% of pyrimidine derivative, 0.5% of adenosine, 0.835% of conditioner, 0.1% of sodium benzotriazolyl butylphenol sulfonate, 0.01% of pH regulator, 0.55% of chelating agent, 0.35% of thickener, 0.1% of solubilizer, 0.015% of pigment and the balance of solvent.
The pyrimidine derivative is a combination of a diaminopyrimidine oxide and a pyrrolidinyldiaminopyrimidine oxide.
The mass ratio of the diaminopyrimidine oxide to the pyrrolidinyl diaminopyrimidine oxide is 1:0.5.
the conditioner comprises cacumen Platycladi extract, amino acid, nicotinamide, panthenol and vitamin E.
The mass ratio of the biota orientalis leaf extract to the amino acid to the nicotinamide to the panthenol to the vitamin E is 0.4:0.025:0.2:0.11:0.1; the biota orientalis extract is purchased from Shanghai Jia Kai biological Co., ltd., trade name: hairdian AP.
The amino acid is arginine.
The pH regulator is citric acid.
The chelating agent comprises EDTA-2Na and Spectrastat TM PHL (INCI: 1, 2-hexanediol, octanoyl hydroxamic acid, and 1, 3-propanediol); the mass ratio is 0.05:0.5.
the thickener comprises sodium polyacryl dimethyl taurate and xanthan gum; the mass ratio is 0.3:0.05.
the solubilizing agent is SOLUBILISANT LRI (INCI: PEG-40 hydrogenated castor oil, PPG-26 butanol polyether 26).
The pigments include CI 19140 and CI 15985; the mass ratio is 0.01:0.005.
the solvent is a mixture of an alcohol compound and water.
The alcohol compound accounts for 40 percent by mass
The alcohol compound is selected from the group consisting of ethanol and methyl propylene glycol.
The mass ratio of the ethanol to the methyl propylene glycol is 3:1.
the preparation method of the essence comprises the following steps: mixing the above materials.
Performance test:
(1) The anti-hair loss hair-growing composition and essence (the initial color is light yellow) are respectively circulated at-18 ℃ and (-18-50 ℃) and 45 ℃; stability profile for 1 month at 50 ℃ is shown in figures 6 and 7.
Figure 6 shows that the anti-hair loss hair growth composition exhibits a slight discoloration after 1 month of standing at 45 ℃ and a significant discoloration after 1 month of standing at 50 ℃.
FIG. 7 shows that the color of the essence is substantially consistent after 1 month of standing at-18deg.C, circulating (-18-50deg.C), 45deg.C, and 50deg.C, without color change.
(2) The essence is taken out at the temperature of-18 ℃,5 ℃,25 ℃,45 ℃,50 ℃ and high and low temperature cycle (-18 ℃ -25 ℃ -45 ℃), the test period is 3 months, and the essence is taken out and evaluated according to the index of the following table when the test period is 1 week, 2 weeks, 1 month, 2 months and 3 months, and the appearance, smell, color, texture, smearing use feeling and use performance are all evaluated; the results are shown in Table 2.
The scoring criteria are shown in table 1:
TABLE 1
TABLE 2
Table 2 shows that the essence is taken out at the high and low temperature cycle (-18 ℃ to 25 ℃ to 45 ℃) in the test period of 6 days and 10 days, and the appearance, smell, color and texture of the essence are good, and the essence has no bad change compared with the sealing sample stored at normal temperature;
the test period of the essence under the illumination condition is 1 week, 2 weeks, and the essence is taken out when the period is 1 month, so that the appearance, smell, color and texture of the essence are good, and the essence has no bad change compared with the sealing sample stored at normal temperature;
the test period of the essence is 1 week, 2 weeks and 1 month at the temperature of 18 ℃ below zero, the appearance, smell, color and texture of the essence are taken out, and the essence has no bad change compared with the sealing sample stored at normal temperature;
the test period of the essence at 25 ℃ is 1 week, 2 weeks, 1 month, 2 months and 3 months, the appearance, smell, color and texture of the essence are taken out, and the essence has no bad change compared with a seal sample stored at normal temperature;
the test period of the essence at 45 ℃ is 1 week, 2 weeks, 1 month, 2 months and 3 months, the appearance, smell, color and texture of the essence are taken out, and the essence has no bad change compared with a seal sample stored at normal temperature;
the test period of the essence is 1 week, 2 weeks and 1 month at 50 ℃, and the appearance, smell, color and texture of the essence are taken out, so that the essence has no bad change compared with a seal sample stored at normal temperature;
the test cycle of the essence at 5 ℃ is 1 week, 2 weeks, 1 month, 2 months and 3 months, the appearance, smell, color and texture of the essence are taken out, and the essence has no bad change compared with the sealing sample stored at normal temperature.
Claims (10)
1. The hair loss preventing and growing composition is characterized by comprising the following raw materials in percentage by mass: pyrimidine derivative 0.1-2.5 wt%, adenosine 0.1-1.5 wt%, conditioner 0.01-6 wt% and solvent for the rest.
2. The hair-loss preventing and hair-growing composition according to claim 1, wherein the mass ratio of the pyrimidine derivative to the adenosine is (0.1 to 2): (0.5-1).
3. The hair-loss preventing and hair-growing composition according to claim 1 or 2, wherein the pyrimidine derivative is selected from one or a combination of two of diaminopyrimidine oxide and pyrrolidinyldiaminopyrimidine oxide.
4. The hair-loss preventing and hair-growing composition according to claim 3, wherein the mass ratio of the diaminopyrimidine oxide to the pyrrolidinyl diaminopyrimidine oxide is (0.5 to 1.5): (0.1-1).
5. The hair-loss preventing and hair-growing composition according to claim 4, wherein the conditioning agent is selected from one or more of biota orientalis extract, amino acid, nicotinamide, panthenol, vitamin E derivative, ceramide, peptides.
6. The hair-loss preventing and hair-growing composition according to claim 5, wherein the mass ratio of the biota orientalis leaf extract, the amino acid, the nicotinamide, the panthenol and the vitamin E is (0.1-2): (0.02-0.3): (0.02-1): (0.05-1.5): (0.01-1).
7. The hair-loss preventing and hair-growing composition according to claim 6, wherein the amino acid is at least one selected from arginine, lysine and cysteine.
8. The anti-hair growth composition of claim 7, wherein the solvent is a mixture of an alcohol compound and water.
9. A method of preparing an anti-hair growth composition according to claim 8, comprising the steps of:
s1, weighing all raw materials according to mass percentage;
s2, mixing and stirring pyrimidine derivatives and alcohol compounds for 1-3 min to obtain a solution 1;
s3, adding water into the solution 1, and stirring to obtain a uniform and transparent solution to obtain a solution 2;
s4, adding amino acid into the solution 2, and uniformly stirring to obtain a solution 3;
s5, uniformly mixing vitamin E, adding the mixture into the solution 3, and uniformly stirring to obtain a solution 4;
s6, adding the biota orientalis extract, adenosine, nicotinamide and panthenol into the solution 4, and uniformly stirring to obtain the compound.
10. Use of an anti-hair growth composition according to any one of claims 1 to 8 for the preparation of personal care and scalp care products.
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