Recombinant Collagen Ionic Liquid Composition, Preparation Method and Application Thereof
Through the lysine citric acid ionic liquid and a composition of glycerol and recombinant collagen, the problem of difficult delivery of recombinant collagen through the skin is solved, efficient hair follicle repair and hair growth is achieved, and skin irritation and allergic reactions are reduced, and it has good application prospects.
Patent Information
- Application Number
- CN202411794366.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-09
- Publication Date
- 2025-08-01
- Estimated Expiration
- 2044-12-09
AI Technical Summary
Existing recombinant collagen is difficult to pass through the in vivo biological barrier, has low percutaneous delivery efficiency and may cause skin irritation and allergic reactions, and cannot effectively promote hair growth.
Using a composition composed of lysine citric acid ionic liquid, glycerin and recombinant collagen, the active ingredient is delivered directly to the skin surface to improve the transdermal efficiency of collagen and reduce skin irritability.
It realizes efficient collagen percutaneous delivery, promotes hair follicle repair and hair growth, reduces the user's allergic and irritating reactions, and has a short preparation cycle and low cost.
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Figure CN119235679B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of cosmetics, and particularly to a recombinant collagen ionic liquid composition, a preparation method thereof, and an application thereof. Background Art
[0002] Hair loss is the phenomenon of hair falling out from the scalp. Physiological hair loss is the normal hair loss caused by the body's metabolism; pathological hair loss refers to the abnormal or excessive hair loss caused by various factors such as genetics, hormonal changes, medical conditions, and nutritional deficiencies, resulting in sparse hair or even baldness. Alopecia not only affects personal self-image but also may have a profound impact on psychological and social aspects. Drug treatment is a common way to improve and treat hair loss due to its advantages such as convenience, easy use, and maintenance of effects. Among them, drugs such as minoxidil and finasteride have been proven to be effective in improving hair loss, but there are problems such as a long usage period, causing adverse reactions (such as rashes, headaches, hirsutism, lower limb edema, elevated blood pressure), and usage limitations (such as finasteride is not applicable to women). Therefore, it is necessary to develop functional ingredients with high safety and few side effects for promoting hair growth to make up for the deficiencies of existing methods.
[0003] Research shows that hair loss is mainly caused by the aging of hair follicle stem cells. Collagen type XVII has high biocompatibility and good efficacy, and is a key molecule to prevent the aging of hair follicle stem cells (Science, 2016, 351, 6273.), which can maintain the stem cell characteristics of hair follicles and promote hair regeneration. Among them, recombinant collagen can be produced on a large scale with high purity and effectively avoid the risk of pathogens, and has broad application prospects in the fields of cosmetics and biomedicine. However, recombinant collagen has a large relative molecular mass and a complex structure, and it is difficult to penetrate multiple biological barriers in the body and is easily metabolized and decomposed by gastric acid, enzymes, and the enterohepatic circulation. When used for promoting hair growth, more attention should be paid to the effective delivery of collagen type XVII to the target skin area to maximize the effect. Microneedles are a common method to improve the transdermal delivery efficiency of macromolecular active ingredients such as proteins and polypeptides, but they have a greater destructive effect on the skin, may cause local tissue damage and pain, and there is also a risk of cross-infection and allergic reactions. Ionic liquids have the advantages of strong dissolving ability and good transdermal absorption promotion. After being combined with active ingredients, they can be directly applied to the skin surface to deliver active ingredients, so as to increase the targeting and reduce adverse reactions, providing a new idea for the efficient delivery of collagen and promoting hair growth. However, the current ionic liquid formulations may have strong irritation and sensitization, and have poor skin applicability. Therefore, there is an urgent need for a system with a high transdermal drug delivery rate and low skin irritation to reduce the allergic reactions and discomfort of users while ensuring the efficient transdermal delivery of collagen.
[0004] Based on this, it is of great significance to provide a method for preparing a recombinant collagen ionic liquid composition with good protein solubility, high transdermal efficiency, low skin irritation, short preparation cycle, simple process, and continuous production. Summary of the Invention
[0005] The first object of the present invention is to provide a recombinant collagen ionic liquid composition to solve the above technical problems.
[0006] The second object of the present invention is to provide a method for preparing the recombinant collagen ionic liquid composition.
[0007] The third object of the present invention is to provide the use of the recombinant collagen ionic liquid composition in promoting hair follicle repair and hair growth.
[0008] In order to achieve the above objectives, the following technical solutions are adopted:
[0009] In a first aspect, the present invention provides a recombinant collagen ionic liquid composition, comprising, by mass, 19.8-79.99 parts of lysine citrate ionic liquid, 20-80 parts of glycerol, and 0.01-0.2 parts of recombinant collagen;
[0010] The lysine citrate ionic liquid is mainly composed of lysine and citric acid, and the molar ratio of lysine to citric acid is 4-1:2-1.
[0011] As a further technical solution, the invention comprises, by weight, 29.85-49.95 parts of lysine citrate ionic liquid, 50-70 parts of glycerol and 0.05-0.15 parts of recombinant collagen.
[0012] As a further technical solution, the preparation method of the lysine citrate ionic liquid comprises: mixing lysine, citric acid and water for reaction, and removing water after the reaction to prepare the lysine citrate ionic liquid.
[0013] As a further technical solution, the reaction temperature is 25-100°C;
[0014] The reaction time is 12-24 hours.
[0015] As a further technical solution, the method of removing moisture includes reduced pressure distillation.
[0016] As a further technical solution, the recombinant collagen includes type XVII recombinant collagen.
[0017] As a further technical solution, the mixture further comprises 0-30 parts of water by mass.
[0018] Second aspect, the present invention provides a preparation method of the above recombinant collagen ionic liquid composition, comprising: mixing the components in the formula amounts and preparing the recombinant collagen ionic liquid composition.
[0019] As a further technical solution, the components other than recombinant collagen are first mixed and then recombinant collagen is added for mixing.
[0020] Third aspect, the present invention provides the application of the above recombinant collagen ionic liquid composition in promoting hair follicle repair and hair growth.
[0021] Compared with the prior art, the present invention has the following beneficial effects:
[0022] The recombinant collagen ionic liquid composition provided by the present invention is mainly composed of lysine citrate ionic liquid, glycerol and recombinant collagen in specific ratios. Among them, the lysine citrate ionic liquid is a product of natural components, with good biocompatibility and safety, and has the advantages of good skin permeability, no irritation, convenient administration, etc. This composition can effectively reduce the allergic and irritating reactions of users; it contains active ingredients for promoting hair growth, is easy to use, can be directly applied topically to the scalp area, has strong targeting and high hair growth efficiency.
[0023] The preparation method of the recombinant collagen ionic liquid composition provided by the present invention has a short preparation period, simple process, can be continuously produced, and has low cost. Description of the Drawings
[0024] In order to more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the following will briefly introduce the drawings required for use in the description of the specific embodiments or the prior art. Obviously, the drawings in the following description are some embodiments of the present invention. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative efforts.
[0025] Figure 1 1H NMR spectrum of lysine citrate ionic liquid;
[0026] Figure 2 1H NMR spectrum of arginine octanoate ionic liquid;
[0027] Figure 3 1H NMR spectrum of proline citrate ionic liquid;
[0028] Figure 4 Lysine citrate ionic liquid;
[0029] Figure 5 Recombinant collagen ionic liquid composition;
[0030] Figure 6Results of the mouse hair growth experiment
[0031] Figure 7 Control of the subject in Test Example 3 before and after using the recombinant collagen ionic liquid composition
[0032] Figure 8 Control of the subject in Test Example 4 before and after using the recombinant collagen ionic liquid composition Detailed implementation mode
[0033] The following will describe the implementation schemes of the present invention in detail in combination with the implementation modes and examples. However, those skilled in the art will understand that the following implementation modes and examples are only used to illustrate the present invention and should not be regarded as limiting the scope of the present invention. Based on the examples in the present invention, all other examples obtained by those of ordinary skill in the art without creative work belong to the scope protected by the present invention. Those not specifying specific conditions are carried out according to conventional conditions or conditions recommended by the manufacturer. Those reagents or instruments not indicating the manufacturer can be obtained as conventional products through commercial purchase.
[0034] In the first aspect, the present invention provides a recombinant collagen ionic liquid composition mainly composed of lysine citrate ionic liquid, glycerol and recombinant collagen. By mass, the mass fraction of lysine citrate ionic liquid can be, for example, but not limited to, 19.8 parts, 40 parts, 60 parts or 79.99 parts;
[0035] For the recombinant collagen ionic liquid composition, glycerol is preferably used as a solubilizer to improve the dissolution rate of collagen, optimize the color of the composition and reduce the viscosity of the composition. The mass fraction of glycerol can be, for example, but not limited to, 20 parts, 40 parts, 60 parts or 80 parts;
[0036] The mass fraction of recombinant collagen can be, for example, but not limited to, 0.01 part, 0.05 part, 0.1 part, 0.15 part or 0.2 part;
[0037] The lysine citrate ionic liquid is mainly composed of lysine and citric acid, and the molar ratio of lysine to citric acid can be, for example, but not limited to, 4:1, 3:2, 2:3 or 1:2.
[0038] The recombinant collagen ionic liquid composition provided by the present invention can effectively reduce the allergic and irritating reactions of users, promote the scalp absorption of recombinant collagen, and has a good effect of promoting hair follicle growth and hair growth. In some optional implementation modes, by mass, it includes 29.85 - 49.95 parts of lysine citrate ionic liquid, 50 - 70 parts of glycerol and 0.05 - 0.15 parts of recombinant collagen.
[0039] In some alternative embodiments, the method for preparing the lysine citrate ionic liquid comprises: mixing lysine, citric acid and water for reaction, and removing the water after the reaction is completed to obtain the lysine citrate ionic liquid.
[0040] The method for preparing the lysine citrate ionic liquid is simple, convenient and low in cost.
[0041] In some alternative embodiments, the temperature of the reaction can be, for example, but not limited to, 25°C, 50°C, 75°C or 100°C;
[0042] The reaction time can be, for example, but not limited to, 12 h, 18 h or 24 h.
[0043] In some alternative embodiments, the method for removing the water includes but is not limited to vacuum distillation, or other methods for removing water well-known to those skilled in the art.
[0044] In some alternative embodiments, the recombinant collagen includes type XVII recombinant collagen.
[0045] In some alternative embodiments, by mass parts, it further includes 0 - 30 parts of water, which can be, for example, but not limited to, 0 part, 5 parts, 10 parts, 20 parts, 25 parts or 30 parts.
[0046] In a second aspect, the present invention provides a method for preparing the above-mentioned recombinant collagen ionic liquid composition, comprising: mixing the respective components in a formulated amount and then preparing the recombinant collagen ionic liquid composition.
[0047] This preparation method has a short cycle, a simple process, can be continuously produced, and is low in cost.
[0048] To ensure the uniformity of raw material mixing and the solubility and stability of collagen in the composition, in some alternative embodiments, the components other than the recombinant collagen are first mixed and then the recombinant collagen is added for mixing.
[0049] In a third aspect, the present invention provides the application of the above-mentioned recombinant collagen ionic liquid composition in promoting hair follicle repair and hair growth.
[0050] The recombinant collagen ionic liquid composition provided by the present invention can effectively reduce the allergic and irritating reactions of users, promote the scalp absorption of recombinant collagen, and has a good effect of promoting hair follicle growth and hair growth.
[0051] The present invention will be further illustrated below by specific examples and comparative examples. However, it should be understood that these examples are only for more detailed illustration and should not be construed as limiting the present invention in any form.
[0052] Example 1
[0053] This example provides an amino acid ionic liquid, the appearance of which is as Figure 4 shown, and it is mainly prepared through the following steps:
[0054] Under a nitrogen atmosphere, 0.4 mol of lysine is added to a round-bottom flask, and then 50 mL of deionized water is added and stirred well to mix evenly at a rotation speed of 800 rpm;
[0055] 0.1 mol of citric acid is dissolved in 50 mL of deionized water, and then it is dropped into the reaction vessel and mixed evenly. At 80 °C, magnetic stirring reaction is carried out for 12 hours;
[0056] After the reaction is completed, most of the water is removed by rotary evaporation at 70 °C, and then it is dried in a vacuum oven at 60 °C for 48 hours to remove the residual water, obtaining lysine citrate ionic liquid (4:1).
[0057] Example 2
[0058] This example provides an amino acid ionic liquid, which is mainly prepared through the following steps:
[0059] Under a nitrogen atmosphere, 0.3 mol of lysine is added to a round-bottom flask, and then 50 mL of deionized water is added and stirred well to mix evenly at a rotation speed of 800 rpm;
[0060] 0.1 mol of citric acid is dissolved in 50 mL of deionized water, and then it is gradually dropped into the reaction vessel and mixed evenly. At 80 °C, magnetic stirring reaction is carried out for 12 hours;
[0061] After the reaction is completed, most of the water is removed by rotary evaporation at 70 °C, and then it is dried in a vacuum oven at 60 °C for 48 hours to remove the residual water, obtaining lysine citrate ionic liquid (3:1).
[0062] Example 3
[0063] This example provides an amino acid ionic liquid, which is mainly prepared through the following steps:
[0064] Under a nitrogen atmosphere, 0.2 mol of lysine is added to a round-bottom flask, and then 50 mL of deionized water is added and stirred well to mix evenly at a rotation speed of 800 rpm;
[0065] 0.1 mol of citric acid is dissolved in 50 mL of deionized water, and then it is gradually dropped into the reaction vessel and mixed evenly. At 80 °C, magnetic stirring reaction is carried out for 12 hours;
[0066] After the reaction was completed, most of the water was removed by rotary evaporation at 70 °C, and the residual water was removed by drying in a vacuum oven at 60 °C for 48 hours to obtain lysine citrate ionic liquid (2:1).
[0067] Example 4
[0068] This example provides an amino acid ionic liquid, which is mainly prepared by the following steps:
[0069] Under a nitrogen atmosphere, 0.1 mol of lysine was added to a round-bottom flask, and then 50 mL of deionized water was added and stirred well to mix evenly at a rotation speed of 800 rpm;
[0070] 0.1 mol of citric acid was dissolved in 50 mL of deionized water, and then added dropwise to the reaction vessel and mixed evenly. At 80 °C, magnetic stirring reaction was carried out for 12 hours;
[0071] After the reaction was completed, most of the water was removed by rotary evaporation at 70 °C, and the residual water was removed by drying in a vacuum oven at 60 °C for 48 hours to obtain lysine citrate ionic liquid (1:1).
[0072] Example 5
[0073] This example provides an amino acid ionic liquid, which is mainly prepared by the following steps:
[0074] Under a nitrogen atmosphere, 0.1 mol of lysine was added to a round-bottom flask, and then 50 mL of deionized water was added and stirred well to mix evenly at a rotation speed of 800 rpm;
[0075] 0.15 mol of citric acid was dissolved in 50 mL of deionized water, and then added dropwise to the reaction vessel and mixed evenly. At 25 °C, magnetic stirring reaction was carried out for 24 hours;
[0076] After the reaction was completed, most of the water was removed by rotary evaporation at 70 °C, and the residual water was removed by drying in a vacuum oven at 60 °C for 48 hours to obtain lysine citrate ionic liquid (1:1.5).
[0077] Example 6
[0078] This example provides an amino acid ionic liquid, which is mainly prepared by the following steps:
[0079] Under a nitrogen atmosphere, 0.1 mol of lysine was added to a round-bottom flask, and then 50 mL of deionized water was added and stirred well to mix evenly at a rotation speed of 800 rpm;
[0080] 0.2 mol of citric acid was dissolved in 50 mL of deionized water, and then added dropwise to the reaction vessel and mixed evenly. At 100 °C, magnetic stirring reaction was carried out for 18 hours;
[0081] After the reaction was completed, most of the water was removed by rotary evaporation at 70°C, and then the residual water was removed by drying in a vacuum oven at 60°C for 48 hours to obtain lysine citrate ionic liquid (1:2).
[0082] The amino acid ionic liquids prepared above were experimentally verified. The results showed that Examples 1-6 all successfully prepared ionic liquids, and the experimental results of Example 3 were as follows:
[0083] H NMR spectrum Figure 1 As shown, the lysine citrate ionic liquid 1 H NMR spectroscopy revealed signals corresponding to methylene groups at 1.95-1.43 ppm (m, -CH2), 3.029 (m, -CH2), and 3.756 (m, -CH2), and a signal corresponding to amino groups at 7.46 ppm (s, -NH2), representing L-lysine fragments. Signals corresponding to methylene groups at 2.757 (q, -CH2) and 2.662 (q, -CH2) were observed, indicating citric acid-related fragments. The chemical shift shift of 8.51 (s, -COOH) for the carboxyl group of citric acid confirmed the successful synthesis of [L-Lys][CA]. These results indicate the successful preparation of the [L-Lys][CA] ionic liquid.
[0084] Comparative Example 1
[0085] An arginine octanoate ionic liquid (NMR hydrogen spectrum as Figure 2 ), the difference from Example 2 is that lysine is replaced by arginine, and citric acid is replaced by caprylic acid.
[0086] Comparative Example 2
[0087] A proline citrate ionic liquid (NMR hydrogen spectrum as Figure 3 ), which differs from Example 2 in that lysine is replaced by proline.
[0088] Comparative Example 3
[0089] An amino acid ionic liquid, which differs from Example 2 in that citric acid is replaced by butyric acid.
[0090] Example 7
[0091] A recombinant collagen ionic liquid composition is mainly prepared by the following steps:
[0092] Water, glycerol and the amino acid ionic liquid prepared in Example 1 were uniformly mixed to obtain a mixed solution, and then type XVII recombinant collagen was dissolved in the mixed solution, and stirred at 30° C. for 10 hours to obtain a recombinant collagen ionic liquid composition.
[0093] Among them, the mass ratio of water, glycerol, amino acid ionic liquid and recombinant collagen type XVII is 10:70:20:0.1.
[0094] Example 8
[0095] A recombinant collagen ionic liquid composition is mainly prepared by the following steps:
[0096] Mix water, glycerol and the amino acid ionic liquid prepared in Example 2 evenly to obtain a mixed solution, and then dissolve recombinant collagen type XVII in the mixed solution, and stir at 30 °C for 10 hours to obtain a recombinant collagen ionic liquid composition.
[0097] Among them, the mass ratio of water, glycerol, amino acid ionic liquid and recombinant collagen type XVII is 5:60:35:0.1.
[0098] Example 9
[0099] A recombinant collagen ionic liquid composition is mainly prepared by the following steps:
[0100] Mix water, glycerol and the amino acid ionic liquid prepared in Example 3 evenly to obtain a mixed solution, and then dissolve recombinant collagen type XVII in the mixed solution, and stir at 30 °C for 10 hours to obtain a recombinant collagen ionic liquid composition.
[0101] Among them, the mass ratio of water, glycerol, amino acid ionic liquid and recombinant collagen type XVII is 30:50:19.8:0.2.
[0102] Example 10
[0103] A recombinant collagen ionic liquid composition is mainly prepared by the following steps:
[0104] Mix glycerol and the amino acid ionic liquid prepared in Example 2 evenly to obtain a mixed solution, and then dissolve recombinant collagen type XVII in the mixed solution, and stir at 30 °C for 10 hours to obtain a recombinant collagen ionic liquid composition.
[0105] Among them, the mass ratio of glycerol, amino acid ionic liquid and recombinant collagen type XVII is 20:79.99:0.01.
[0106] Example 11
[0107] A recombinant collagen ionic liquid composition is mainly prepared by the following steps:
[0108] Mix glycerol with the amino acid ionic liquid prepared in Example 3 to obtain a homogeneous mixed solution, and then dissolve type XVII recombinant collagen in the mixed solution. Stir at 30 °C for 10 hours to obtain a recombinant collagen ionic liquid composition.
[0109] Among them, the mass ratio of glycerol, amino acid ionic liquid and type XVII recombinant collagen is 80:19.9:0.1.
[0110] Comparative Example 4
[0111] The difference from Example 8 is that the amino acid ionic liquid of Comparative Example 1 is used.
[0112] Comparative Example 5
[0113] The difference from Example 8 is that the amino acid ionic liquid of Comparative Example 2 is used.
[0114] Comparative Example 6
[0115] The difference from Example 8 is that the amino acid ionic liquid of Comparative Example 3 is used.
[0116] Comparative Example 7
[0117] The difference from Example 8 is that a different amino acid ionic liquid is used. The preparation method of this amino acid ionic liquid is as follows:
[0118] Under a nitrogen atmosphere, add 0.1 mol of lysine to a round-bottom flask, and then add 50 mL of deionized water and stir well to mix evenly at a rotation speed of 800 rpm;
[0119] Dissolve 0.4 mol of citric acid in 50 mL of deionized water, and then dropwise add it to the reaction vessel and mix evenly. Stir magnetically at 100 °C for 18 hours;
[0120] After the reaction is completed, rotate and evaporate to remove most of the water at 70 °C, and then dry in a vacuum oven at 60 °C for 48 hours to remove the residual water to obtain lysine citrate ionic liquid (1:4).
[0121] Test Example 1
[0122] Evaluate the effect of the recombinant collagen ionic liquid composition prepared by the present invention on promoting hair growth in mice. Female C57BL / 6J mice (6 - 8 weeks old, 18 - 20 g) were selected. The hair on their backs was cut short with an electric clipper. An appropriate amount of depilatory cream was evenly applied to the haircut area to remove the remaining hair, then washed and dried with warm water. The application area was about 3 cm × 2 cm. The back skin of the mice was considered clean when it was smooth, without damage and residual hair. Then, the depilated area and the surrounding part were disinfected with 75% ethanol. Mice with pink skin and hair in the telogen phase were selected to establish a mouse hair loss model. The next day, the mice were randomly divided into groups of 3 each, namely a blank group (given normal saline), a collagen group (the concentration of recombinant collagen was the same as that in Example 8), groups of Examples 7 - 11, and groups of Comparative Examples 4 - 5. The appearances of the products of Example 8, Comparative Example 4, Comparative Example 5, and Comparative Example 6 are as Figure 5 shown. Each group was topically administered in the depilated area on the back of the mice once a day, with a dosage of 0.5 mL, covering the depilated area, and continuously applied for 14 days. Observe the hair changes in the mice from 1 to 21 days.
[0123] Seven days after administration, the backs of the mice in the blank group were still pink, and the hair follicles were in the telogen phase; the backs of the mice in the collagen group and the group of Example 10 (with the least content of recombinant collagen in the composition) showed a small amount of light gray, indicating that collagen could promote the entry of hair follicles from the telogen phase into the growth phase, and a small number of hair follicles grew; different degrees of hair follicle growth occurred in the groups of Examples 7, 8, 9, 11 and Comparative Examples 4 - 5. There was no significant difference between the groups of Examples 7, 8, 11 and Comparative Examples 4, 5. The light gray area on the back of the mice in the group of Example 9 was larger and more uniform, mainly because this composition contained a higher content of recombinant protein. As Figure 6As shown, 12 days after administration, the back skin of mice in the blank group, collagen group, and Example 10 group presented light gray to gray, and there were short hairs growing in some areas. Among them, the collagen group and Example 10 group were superior to the blank group; the mice in Example 7, 8, 9, 11 groups and Comparative Example 4, 5 groups showed better hair growth status, and the mice were dark gray to black. Among them, the hair growth in Example 9 group was the best. There was no significant difference in hair growth in Example 7, 8, 11 groups, but they were superior to Comparative Example 4, 5 groups; there was no significant difference in hair conditions in Comparative Example 4, 5 groups, but they were superior to the blank group and collagen group. 14 days after administration, the hairs of mice in the blank group and collagen group were short and did not fully recover to the level before hair removal. The hairs of some mice in Example 10 group recovered to the normal level. The mice in Example 7, 8, 9, 11 groups and Comparative Example 4, 5 groups all recovered to the normal level, and their hairs were black and gray. After stopping the administration and continuing to observe the mice, it was found that some mice in Comparative Example 5 group began to lose hair and the back hairs were sparse, while there was no hair loss in Example 7 - 11 groups and Comparative Example 4 group. The above results indicate that ionic liquids can promote hair growth in mice, but their composition affects the hair growth effect and persistence. The ionic liquid compositions (Example 7 - 11 groups) of the present invention have a better effect on promoting hair growth.
[0124] Test Example 2
[0125] The hair growth promoting effect of the recombinant collagen ionic liquid composition prepared by the present invention was evaluated. Eighty volunteers with hair loss problems, aged 25 - 55 years old, were selected and divided into 4 groups, with 20 people in each group. The compositions of Comparative Example 4 and Examples 8, 9, 11 were used respectively (the pH of Comparative Examples 5, 7 could not meet the requirements of skin care products (≥pH4.5) and could not be used for human experiments; the smell of Comparative Example 6 was strong, causing reactions such as nausea in the subjects, and the subjects were unwilling to accept the trial) for 14 days or more, applied once a day, evenly covering the test area, and left to stay for 15 - 30 min; the usage results and feelings were evaluated.
[0126] Table 1
[0127] 。
[0128] According to the test results in Table 1, it can be seen that Examples 8, 9, 11 of the recombinant collagen ionic liquid composition provided by the present invention have obvious hair growth promotion, and the effective rate is 80% or more. Compared with Comparative Example 4, Examples 8, 9, 11 are more excellent in terms of safety and usage feelings. The acceptance rate of the smell of the composition by the subjects is 100%, and no adverse reactions occurred during the use period.
[0129] Test Example 3
[0130] Male, 45 years old, used the recombinant collagen ionic liquid composition in Example 8 seven times a week, applied it to the scalp, and it was completely absorbed without pressing for 15 minutes. After continuous use for 14 days, short hair grew out and hair density increased ( Figure 7 ).
[0131] Test Example 4
[0132] Female, 50 years old, used the recombinant collagen ionic liquid composition in Example 8 seven times a week, applied it to the scalp, and it was completely absorbed without pressing for 15 minutes. After continuous use for 60 days, the hair loss phenomenon was significantly improved and the hair density was significantly increased ( Figure 8 ).
[0133] From the above results, it can be seen that the recombinant collagen ionic liquid composition provided by the present invention has good solubility, high transdermal efficiency, low irritation, short preparation cycle, simple process, and the ionic liquid composition that can be continuously produced and its preparation method are of great significance.
[0134] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements on some or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present invention.
Claims
1. A recombinant collagen ionic liquid composition, characterized in that, By mass parts, it includes 19.8 - 79.99 parts of lysine citrate ionic liquid, 20 - 80 parts of glycerol, and 0.01 - 0.2 parts of recombinant collagen; the lysine citrate ionic liquid is mainly composed of lysine and citric acid, and the molar ratio of lysine to citric acid is 4 - 1:2 - 1; the recombinant collagen includes type XVII recombinant collagen.
2. The recombinant collagen ionic liquid composition according to claim 1, characterized in that By mass parts, it includes 29.85 - 49.95 parts of lysine citrate ionic liquid, 50 - 70 parts of glycerol, and 0.05 - 0.15 parts of recombinant collagen.
3. The recombinant collagen ionic liquid composition according to claim 1, wherein The preparation method of the lysine citrate ionic liquid includes: mixing lysine, citric acid and water for reaction, and removing water after the reaction to prepare the lysine citrate ionic liquid.
4. The recombinant collagen ionic liquid composition according to claim 3, wherein The temperature of the reaction is 25 - 100 °C; the time of the reaction is 12 - 24 h.
5. The recombinant collagen ionic liquid composition according to claim 3, wherein The way of removing water includes vacuum distillation.
6. The recombinant collagen ionic liquid composition according to claim 1, wherein By mass parts, it further includes 0 - 30 parts of water.
7. A method for preparing the recombinant collagen ionic liquid composition according to any one of claims 1-6, characterized in that, It includes: After mixing the components in the formula amount, a recombinant collagen ionic liquid composition is prepared.
8. The preparation method according to claim 7, characterized in that, First, mix the components except recombinant collagen and then add recombinant collagen for mixing.
9. Use of the recombinant collagen ionic liquid composition according to any one of claims 1 - 6 in the preparation of cosmetics for promoting hair follicle repair and hair growth.
Citation Information
Patent Citations
Amino acid ionic liquid for foodstuffs and medical treatments
CN102190589A
High-transdermal supermolecular recombinant collagen and preparation method thereof
CN117959207A
Recombinant XVII type collagen for promoting hair growth as well as preparation method and application of recombinant XVII type collagen
CN118221802A