Coagulation-process two-color freeze-dried powder and preparation method thereof

Abstract

The invention relates to the technical field of cosmetics, in particular to coagulation-process two-color freeze-dried powder and a preparation method thereof. The solidification-method double-color freeze-dried powder comprises a lower solidification layer freeze-dried powder body and an upper non-solidification layer freeze-dried powder body; the lower solidification layer freeze-dried powder body comprises an excipient A and a functional substance A, and the excipient A comprises an excipient A1 and an excipient A2; and the upper non-solidification layer freeze-dried powder body comprises an excipient B and a functional substance B. The preparation method of the double-color freeze-dried powder comprises the following steps: preparing a lower solidification layer freeze-dried powder body; preparing an upper non-solidification layer freeze-dried powder body; the freeze-dried powder of the lower solidification layer and the freeze-dried powder of the upper non-solidification layer are used for preparing the two-color freeze-dried powder prepared through The double-color freeze-dried powder can be divided into an upper layer and a lower layer which are obvious in boundary, different raw materials can be added to each layer, and it is guaranteed that colors are evenly distributed; the two-color freeze-dried powder is produced by using a solidification method, so that the production process is simplified, the production cost is reduced, and the stability and the quality of the product are improved.

Description

Technical Field

[0001] The invention relates to the technical field of cosmetics, and in particular to a coagulation-based two-color freeze-dried powder and a preparation method thereof. Background Art

[0002] Freeze-dried powder is a product form widely used in the fields of cosmetics and medicine. The traditional freeze-dried powder production process can usually only produce products of a single color, which limits the diversity and innovation of the product. With the continuous changes in market demand, consumers' demand for cosmetics with unique appearance and functions is increasing. In the prior art, the production of two-color freeze-dried powder may have the following problems: it is difficult to mix different raw materials, resulting in uneven color distribution; the production process is complicated and the cost is high; the stability and quality of the product are difficult to guarantee. Summary of the invention

[0003] In order to overcome the shortcomings and deficiencies in the prior art, the purpose of the present invention is to provide a coagulation method two-color freeze-dried powder and a preparation method thereof, wherein the two-color freeze-dried powder can be divided into an upper and lower layer with a clear boundary, and different raw materials can be added to each layer respectively to ensure uniform color distribution and good stability; the present invention produces two-color freeze-dried powder by using a coagulation method, which helps to simplify the production process, reduce production costs, and improve product stability and quality.

[0004] The objective of the present invention is achieved through the following technical scheme: a coagulation method two-color freeze-dried powder, comprising a lower coagulation layer freeze-dried powder and an upper non-coagulation layer freeze-dried powder; the lower coagulation layer freeze-dried powder comprises excipient A and efficacy substance A, and the excipient A comprises excipient A1 and excipient A2; the upper non-coagulation layer freeze-dried powder comprises excipient B and efficacy substance B.

[0005] The dual-color freeze-dried powder of the present invention can be divided into two layers with obvious boundaries, forming different freeze-dried powder systems, and different raw materials can be added to each layer to ensure uniform color distribution and good stability; by adding different functional substances to two different systems, the activity of the functional substances can be more stably maintained, the stability can be improved, and the shelf life of the product can be extended. By adding different functional substances to two different systems, the activity of the functional substances can be more stably maintained, the stability can be improved, and the shelf life of the product can be extended; when a solvent is used for re-dissolution to form a system, it is not only convenient to use, but also can synergize and enhance the efficacy of the product.

[0006] Furthermore, the excipient A1 includes the following raw materials in weight percentage: 3-6% mannitol, 0.3-2% trehalose, 0.01-0.1% gellan gum, 0.05-0.15% soluble collagen and 91-95% water; the excipient A2 includes the following raw materials in weight percentage: 0.05-0.5% magnesium sulfate; the sum of the weight percentages of the excipient A1, excipient A2 and the functional substance A is 100%.

[0007] Furthermore, the excipient B comprises the following raw materials in weight percentage: 2-10% mannitol, 0-3% trehalose and 91-95% water; the sum of the weight percentages of the excipient B and the functional substance B is 100%.

[0008] Furthermore, the functional substance A and the functional substance B are at least one of blue copper peptide, astaxanthin, vitamin B12, rutin, gardenia fruit extract, cocoa extract, oligopeptide-1, ergothioneine and acetyl hexapeptide-8.

[0009] The efficacy substance A and efficacy substance B in the present invention can be efficacy substances with various different efficacy and different colors, such as blue copper peptide, astaxanthin, vitamin B12, rutin, gardenia fruit extract, cocoa extract and other colored efficacy substances, and can also be white efficacy substances such as oligopeptide-1, acetyl hexapeptide-8, ergothioneine and the like.

[0010] Furthermore, the weight ratio of the freeze-dried powder in the lower coagulated layer to the freeze-dried powder in the upper non-coagulated layer is 5-8:2-5.

[0011] The present invention also provides a method for preparing a two-color freeze-dried powder by a solidification method, comprising the following steps: (1) Preparation of freeze-dried powder for the lower solidified layer: Heat and stir excipient A1 to dissolve, then cool it down, add excipient A2, stir until dissolved evenly, then add active ingredient A, stir until dissolved evenly, and keep warm after discharging; (2) Preparing the upper non-solidified layer of freeze-dried powder: heat and stir the excipient B to dissolve, then cool it down, then add the active ingredient B, stir and dissolve evenly, then cool it down, and discharge it for later use; (3) Using the lower coagulated layer freeze-dried powder and the upper non-coagulated layer freeze-dried powder to prepare the coagulation method two-color freeze-dried powder: the lower coagulated layer freeze-dried powder is first injected into the packaging bottle according to the ratio of the lower coagulated layer freeze-dried powder to the upper non-coagulated layer freeze-dried powder, and then the temperature is lowered to make the lower coagulated layer freeze-dried powder completely coagulate; then the upper non-coagulated layer freeze-dried powder is injected into the packaging bottle in which the lower coagulated layer freeze-dried powder has been coagulated according to the ratio of the lower coagulated layer freeze-dried powder to the upper non-coagulated layer freeze-dried powder, so that the upper non-coagulated layer freeze-dried powder remains in the upper layer, and then freeze-drying is carried out. After freeze-drying, the coagulation method two-color freeze-dried powder is obtained.

[0012] The present invention prepares a coagulation method two-color freeze-dried powder by adopting the above preparation method, wherein the lower layer of the freeze-dried powder is a lower coagulation layer freeze-dried powder, and the upper layer is an upper non-coagulation layer freeze-dried powder, and it looks like two layers of freeze-dried powder with different colors. The preparation method has a simple process and a high yield rate. Compared with other methods for producing two-color freeze-dried powder in the prior art, the freeze-dried powder prepared by the present invention has a more obvious boundary between the two layers of powder, a novel and beautiful appearance, and good appeal.

[0013] Furthermore, in step (1), excipient A1 is heated at 70-90°C and stirred to dissolve; after dissolution, the temperature is lowered to 30-50°C, excipient A2 is added, and stirred until dissolved evenly, a small amount of sample is taken and cooled to 20-40°C to observe whether coagulation occurs, and ensure that the freeze-dried powder in the lower coagulation layer can coagulate after cooling; after confirmation, the active ingredient A is added and stirred to dissolve evenly; after discharging, the temperature is maintained at 30-50°C and kept warm for later use.

[0014] Furthermore, in step (2), excipient B is heated at 70-90°C and stirred to dissolve; after dissolution, the temperature is lowered to 30-50°C, and active ingredient B is added and stirred to dissolve evenly; the temperature is lowered to 20-25°C and the material is discharged for use.

[0015] Furthermore, in step (3), the lower coagulated layer freeze-dried powder is first injected into the packaging bottle in a weight ratio of 0.5-0.8:0.2-0.5 between the lower coagulated layer freeze-dried powder and the upper non-coagulated layer freeze-dried powder, and then cooled to 20-40°C to completely solidify the lower coagulated layer freeze-dried powder; and then the upper non-coagulated layer freeze-dried powder is injected into the packaging bottle in which the lower coagulated layer freeze-dried powder has already solidified in a weight ratio of 0.5-0.8:0.2-0.5 between the lower coagulated layer freeze-dried powder and the upper non-coagulated layer freeze-dried powder, so that the upper non-coagulated layer freeze-dried powder can be kept in the upper layer, so that the two layers can be kept separated, and then freeze-dried. After freeze-drying, the solid method double-color freeze-dried powder is obtained.

[0016] Furthermore, in step (3), the freeze-drying process includes the following steps: (S1) Start the pre-freezing program, set the freezing temperature to -50 to -30°C, and the freezing time to 2 to 5 hours; (S2) After the pre-freezing process is completed, the primary drying stage is entered, the vacuum degree is set to 10-50 Pa, the plate layer temperature is -20--10 ° C, and maintained for 3-5 hours; then the plate layer temperature is set to -5-5 ° C, and maintained for 3-5 hours; then the plate layer temperature is set to 5-15 ° C, and maintained for 4-8 hours; (S3) After the primary drying stage is completed, the secondary drying stage is entered, the plate temperature is set to 35-45°C, the vacuum degree is 3-10 Pa, and the freeze-drying process is terminated after maintaining for 5-10 hours.

[0017] The beneficial effects of the present invention are as follows: the present invention uses a specific formula and a specific process, in combination with freeze-drying technology, to prepare a new type of two-color freeze-dried powder, wherein the lower layer of the freeze-dried powder is a lower solidified layer freeze-dried powder, and the upper layer is an upper non-solidified layer freeze-dried powder, which is viewed as two layers of freeze-dried powder with different colors. The present invention uses a solidification method to produce a two-color freeze-dried powder, which simplifies the production process and helps to improve the yield rate. Compared with other methods for producing two-color freeze-dried powder, the freeze-dried powder prepared by the present invention has a more obvious boundary between the two layers of powder, a novel and beautiful appearance, and good appeal; different functional substances are added to two different systems respectively, which can more stably maintain the activity of the functional substances, improve stability, and extend the shelf life of the product; when a solvent is used for re-dissolution to form a system, it is not only convenient to use, but also can synergize and enhance the efficacy of the product. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 This is a product picture of the two-color freeze-dried powder obtained by the solidification method in Example 1 of the present invention.

[0019] Figure 2 This is a product picture of the two-color freeze-dried powder obtained by the solidification method in Example 2 of the present invention.

[0020] Figure 3 This is a product picture of the two-color freeze-dried powder obtained by the solidification method in Example 3 of the present invention. DETAILED DESCRIPTION

[0021] In order to facilitate the understanding of those skilled in the art, the present invention is further described below in conjunction with embodiments and drawings. The contents mentioned in the implementation modes are not intended to limit the present invention.

[0022] In some embodiments of the present invention, a coagulation method two-color freeze-dried powder includes a lower coagulation layer freeze-dried powder and an upper non-coagulation layer freeze-dried powder; the lower coagulation layer freeze-dried powder includes excipient A and efficacy substance A, and the excipient A includes excipient A1 and excipient A2; the upper non-coagulation layer freeze-dried powder includes excipient B and efficacy substance B.

[0023] In some embodiments of the present invention, the excipient A1 includes the following raw materials in weight percentage: 3-6% mannitol, 0.3-2% trehalose, 0.01-0.1% gellan gum, 0.05-0.15% soluble collagen and 91-95% water; the excipient A2 includes the following raw materials in weight percentage: 0.05-0.5% magnesium sulfate; the weight percentage content of the functional substance A is 0.1-0.5%; the sum of the weight percentages of the excipient A1, excipient A2 and functional substance A is 100%.

[0024] In some embodiments of the present invention, the excipient A1 includes the following raw materials in weight percentage: 3-6% mannitol, 1-2% trehalose, 0.025-0.035% gellan gum, 0.05-0.15% soluble collagen and 91-95% water; the excipient A2 includes the following raw materials in weight percentage: 0.1-0.3% magnesium sulfate; the weight percentage content of the functional substance A is 0.2-0.3%; the sum of the weight percentages of the excipient A1, excipient A2 and functional substance A is 100%.

[0025] In some embodiments of the present invention, the excipient B comprises the following raw materials in weight percentage: 2-10% mannitol, 0-3% trehalose and 91-95% water; the weight percentage content of the functional substance B is 0.05-0.5%; the sum of the weight percentages of the excipient B and the functional substance B is 100%.

[0026] In some embodiments of the present invention, the excipient B comprises the following raw materials in weight percentage: 3-5% mannitol, 0-2% trehalose and 91-95% water; the weight percentage content of the functional substance B is 0.1-0.2%; the sum of the weight percentages of the excipient B and the functional substance B is 100%.

[0027] In some embodiments of the present invention, the efficacy substance A and the efficacy substance B are at least one of blue copper peptide, astaxanthin, vitamin B12, rutin, gardenia fruit extract, cocoa extract, oligopeptide-1, ergothioneine and acetyl hexapeptide-8.

[0028] In some embodiments of the present invention, the functional substance A is at least one of blue copper peptide, gardenia fruit extract and cocoa extract; and the functional substance B is at least one of astaxanthin, oligopeptide-1 and ergothioneine.

[0029] In some embodiments of the present invention, the weight ratio of the freeze-dried powder in the lower coagulated layer to the freeze-dried powder in the upper non-coagulated layer is 5-8:2-5.

[0030] In some embodiments of the present invention, a method for preparing a two-color freeze-dried powder by a solidification method comprises the following steps: (1) Preparation of freeze-dried powder for the lower solidified layer: Heat and stir excipient A1 to dissolve, then cool it down, add excipient A2, stir until dissolved evenly, then add active ingredient A, stir until dissolved evenly, and keep warm after discharging; (2) Preparing the upper non-solidified layer of freeze-dried powder: heat and stir the excipient B to dissolve, then cool it down, then add the active ingredient B, stir and dissolve evenly, then cool it down, and discharge it for later use; (3) Using the lower coagulated layer freeze-dried powder and the upper non-coagulated layer freeze-dried powder to prepare the coagulation method two-color freeze-dried powder: the lower coagulated layer freeze-dried powder is first injected into the packaging bottle according to the ratio of the lower coagulated layer freeze-dried powder to the upper non-coagulated layer freeze-dried powder, and then allowed to cool down to make it completely coagulated; then the upper non-coagulated layer freeze-dried powder is injected into the packaging bottle in which the lower coagulated layer freeze-dried powder has been coagulated according to the ratio of the lower coagulated layer freeze-dried powder to the upper non-coagulated layer freeze-dried powder, so that the upper non-coagulated layer freeze-dried powder remains in the upper layer, and then freeze-dried. After freeze-drying, the coagulation method two-color freeze-dried powder is obtained.

[0031] In some embodiments of the present invention, in step (1), excipient A1 is heated at 70-90°C and stirred to dissolve; after dissolution, the temperature is lowered to 40-45°C, excipient A2 is added, and stirred until dissolved evenly, a small amount of sample is taken and cooled to 20-40°C to observe whether coagulation occurs, and ensure that the freeze-dried powder in the lower coagulation layer can coagulate after cooling; after confirmation, the active ingredient A is added and stirred to dissolve evenly; after discharging, the temperature is maintained at 30-50°C and kept warm for use.

[0032] In some embodiments of the present invention, in step (1), excipient A1 is heated at 70-90°C and stirred to dissolve; after dissolution, the temperature is lowered to 40-45°C, excipient A2 is added, and stirred until dissolved evenly, a small amount of sample is taken and cooled to 20-25°C to observe whether coagulation occurs, and ensure that the freeze-dried powder in the lower coagulation layer can coagulate after cooling; after confirmation, the active ingredient A is continued to be added and stirred to dissolve evenly; after discharging, the temperature is maintained at 40-50°C and kept warm for later use.

[0033] In some embodiments of the present invention, in step (2), excipient B is heated at 70-90°C and stirred to dissolve; after dissolution, the temperature is lowered to 30-50°C, and the active ingredient B is added and stirred to dissolve evenly; the temperature is lowered to 20-25°C and the material is discharged for use.

[0034] In some embodiments of the present invention, in step (2), excipient B is heated at 70-90°C and stirred to dissolve; after dissolution, the temperature is lowered to 40-45°C, and the active ingredient B is added and stirred to dissolve evenly; the temperature is lowered to 20-25°C and the material is discharged for use.

[0035] In some embodiments of the present invention, in step (3), the lower coagulated layer freeze-dried powder is first injected into a packaging bottle in a weight ratio of 0.5-0.8:0.2-0.5 between the lower coagulated layer freeze-dried powder and the upper non-coagulated layer freeze-dried powder, and then cooled to 20-40°C, preferably below 25°C, to completely solidify it; then the upper non-coagulated layer freeze-dried powder is injected into the packaging bottle in which the lower coagulated layer freeze-dried powder has solidified in a weight ratio of 0.5-0.8:0.2-0.5 between the lower coagulated layer freeze-dried powder and the upper non-coagulated layer freeze-dried powder, so that the upper non-coagulated layer freeze-dried powder can be kept in the upper layer, so that the two layers can be kept separated, and then freeze-dried. After freeze-drying, a solid method two-color freeze-dried powder is obtained.

[0036] In some embodiments of the present invention, in step (3), the freeze-drying process comprises the following steps: (S1) Start the pre-freezing program, set the freezing temperature to -50 to -30°C, and the freezing time to 2 to 5 hours; (S2) After the pre-freezing process is completed, the primary drying stage is entered, the vacuum degree is set to 10-50 Pa, the plate layer temperature is -20--10 ° C, and maintained for 3-5 hours; then the plate layer temperature is set to -5-5 ° C, and maintained for 3-5 hours; then the plate layer temperature is set to 5-15 ° C, and maintained for 4-8 hours; (S3) After the primary drying stage is completed, the secondary drying stage is entered, the plate temperature is set to 35-45°C, the vacuum degree is 3-10 Pa, and the freeze-drying process is terminated after maintaining for 5-10 hours.

[0037] Example 1 In this embodiment, a coagulation method two-color freeze-dried powder includes a lower coagulation layer freeze-dried powder and an upper non-coagulation layer freeze-dried powder; the lower coagulation layer freeze-dried powder includes excipient A and active substance A, and the excipient A includes excipient A1 and excipient A2; the upper non-coagulation layer freeze-dried powder includes excipient B and active substance B.

[0038] Furthermore, the excipient A1 includes the following raw materials in weight percentage: 4% mannitol, 2% trehalose, 0.025% gellan gum, 0.1% soluble collagen, and 93.575% water; the excipient A2 includes the following raw materials in weight percentage: 0.1% magnesium sulfate; the sum of the weight percentages of the excipient A1, excipient A2, and efficacy substance A is 100%. The efficacy substance A is a gardenia fruit extract, and its weight percentage in the freeze-dried powder of the lower solidified layer is 0.2%.

[0039] Furthermore, the excipient B includes the following raw materials in weight percentage: 3% mannitol, 2% trehalose, and 94.9% water; the sum of the weight percentages of the excipient B and the efficacy substance B is 100%. The efficacy substance B is oligopeptide-1, and its weight percentage in the upper non-solidified layer of freeze-dried powder is 0.1%.

[0040] Furthermore, the weight ratio of the freeze-dried powder in the lower coagulated layer to the freeze-dried powder in the upper non-coagulated layer is 3:2.

[0041] This embodiment also provides a method for preparing a two-color freeze-dried powder by a solidification method, comprising the following steps: (1) Preparation of freeze-dried powder for the lower solidification layer: Heat excipient A1 at 80°C and stir to dissolve; after dissolution, cool it down to 40°C, add excipient A2, stir until dissolved evenly, take a small amount of sample and cool it down to 20°C to observe whether solidification occurs, and ensure that the freeze-dried powder for the lower solidification layer can solidify after cooling; after confirmation, continue to add active ingredient A and stir to dissolve evenly; after discharging, keep it at 40°C and keep it warm for later use; (2) Preparing the upper non-solidified layer of freeze-dried powder: heat and stir the excipient B to dissolve, then cool it down, then add the active ingredient B, stir and dissolve evenly, then cool it down, and discharge it for later use; (3) Using the lower coagulated layer freeze-dried powder and the upper non-coagulated layer freeze-dried powder to prepare the coagulation method two-color freeze-dried powder: the lower coagulated layer freeze-dried powder is first injected into the packaging bottle at a weight ratio of 3:2 between the lower coagulated layer freeze-dried powder and the upper non-coagulated layer freeze-dried powder, and then cooled to 20°C to make it completely coagulated; then the upper non-coagulated layer freeze-dried powder is injected into the packaging bottle where the lower coagulated layer freeze-dried powder has been coagulated at a weight ratio of 3:2 between the lower coagulated layer freeze-dried powder and the upper non-coagulated layer freeze-dried powder, so that the upper non-coagulated layer freeze-dried powder can be kept in the upper layer, so that the two layers can be kept separated, and then freeze-dried. After freeze-drying, the solid method two-color freeze-dried powder is obtained.

[0042] Furthermore, in step (3), the freeze-drying process includes the following steps: (S1) Start the pre-freezing program, set the freezing temperature to -40°C and the freezing time to 3h; (S2) After the pre-freezing process is completed, the primary drying stage is entered, the vacuum degree is set to 25pa, the plate layer temperature is 5-10℃, and maintained for 5h; then the plate layer temperature is set to 5℃, maintained for 5h, and then the plate layer temperature is set to 10℃, maintained for 6h; (S3) After the first drying stage, the second drying stage is entered, the plate temperature is set to 40°C, the vacuum degree is set to 5 Pa, and the freeze-drying process is terminated after maintaining for 8 hours.

[0043] Example 2 In this embodiment, a coagulation method two-color freeze-dried powder includes a lower coagulation layer freeze-dried powder and an upper non-coagulation layer freeze-dried powder; the lower coagulation layer freeze-dried powder includes excipient A and active substance A, and the excipient A includes excipient A1 and excipient A2; the upper non-coagulation layer freeze-dried powder includes excipient B and active substance B.

[0044] Furthermore, the excipient A1 includes the following raw materials in weight percentage: 4% mannitol, 2% trehalose, 0.03% gellan gum, 0.1% soluble collagen, and 93.47% water; the excipient A2 includes the following raw materials in weight percentage: 0.2% magnesium sulfate; the sum of the weight percentages of the excipient A1, excipient A2, and efficacy substance A is 100%. The efficacy substance A is a cocoa extract, and its weight percentage in the freeze-dried powder of the lower solidified layer is 0.2%.

[0045] Further, the excipient B comprises the following raw materials in weight percentage: 4% mannitol, 1% trehalose, and 94.9% water; the sum of the weight percentages of the excipient B and the efficacy substance B is 100%. The efficacy substance B is ergothioneine, and the weight percentage in the upper non-solidified layer of freeze-dried powder is 0.1%.

[0046] Furthermore, the weight ratio of the freeze-dried powder in the lower coagulated layer to the freeze-dried powder in the upper non-coagulated layer is 3:2.

[0047] This embodiment also provides a method for preparing a two-color freeze-dried powder by a solidification method, comprising the following steps: (1) Preparation of freeze-dried powder for the lower solidification layer: Heat excipient A1 at 80°C and stir to dissolve; after dissolution, cool it down to 40°C, add excipient A2, stir until dissolved evenly, take a small amount of sample and cool it down to 22°C to observe whether solidification occurs to ensure that the freeze-dried powder for the lower solidification layer can solidify after cooling; after confirmation, continue to add active ingredient A and stir to dissolve evenly; after discharging, keep it at 40°C and keep it warm for later use; (2) Preparing the upper non-solidified layer of freeze-dried powder: heat and stir the excipient B to dissolve, then cool it down, then add the active ingredient B, stir and dissolve evenly, then cool it down, and discharge it for later use; (3) Using the lower coagulated layer freeze-dried powder and the upper non-coagulated layer freeze-dried powder to prepare the coagulation method two-color freeze-dried powder: the lower coagulated layer freeze-dried powder is first injected into the packaging bottle at a weight ratio of 3:2 between the lower coagulated layer freeze-dried powder and the upper non-coagulated layer freeze-dried powder, and then cooled to 22°C to make it completely coagulated; then the upper non-coagulated layer freeze-dried powder is injected into the packaging bottle where the lower coagulated layer freeze-dried powder has been coagulated at a weight ratio of 3:2 between the lower coagulated layer freeze-dried powder and the upper non-coagulated layer freeze-dried powder, so that the upper non-coagulated layer freeze-dried powder can be kept in the upper layer, so that the two layers can be kept separated, and then freeze-dried. After freeze-drying, the solid method two-color freeze-dried powder is obtained.

[0048] Furthermore, in step (3), the freeze-drying process includes the following steps: (S1) Start the pre-freezing program, set the freezing temperature to -40°C and the freezing time to 3h; (S2) After the pre-freezing process is completed, the primary drying stage is entered, the vacuum degree is set to 25pa, the plate layer temperature is 5-10℃, and maintained for 5h; then the plate layer temperature is set to 5℃, maintained for 5h, and then the plate layer temperature is set to 10℃, maintained for 6h; (S3) After the first drying stage, the second drying stage is entered, the plate temperature is set to 40°C, the vacuum degree is set to 5 Pa, and the freeze-drying process is terminated after maintaining for 8 hours.

[0049] Example 3 In this embodiment, a coagulation method two-color freeze-dried powder includes a lower coagulation layer freeze-dried powder and an upper non-coagulation layer freeze-dried powder; the lower coagulation layer freeze-dried powder includes excipient A and active substance A, and the excipient A includes excipient A1 and excipient A2; the upper non-coagulation layer freeze-dried powder includes excipient B and active substance B.

[0050] Furthermore, the excipient A1 includes the following raw materials in weight percentage: 4% mannitol, 2% trehalose, 0.035% gellan gum, 0.1% soluble collagen, and 93.265% water; the excipient A2 includes the following raw materials in weight percentage: 0.3% magnesium sulfate; the sum of the weight percentages of the excipient A1, excipient A2, and efficacy substance A is 100%. The efficacy substance A is blue copper peptide, and its weight percentage in the freeze-dried powder of the lower solidified layer is 0.3%.

[0051] Furthermore, the excipient B comprises the following raw materials in weight percentage: 5% mannitol, 94.8% water; the sum of the weight percentages of the excipient B and the functional substance B is 100%. The functional substance B is astaxanthin, and the weight percentage in the upper non-solidified layer of freeze-dried powder is 0.2%.

[0052] Furthermore, the weight ratio of the freeze-dried powder in the lower coagulated layer to the freeze-dried powder in the upper non-coagulated layer is 3:2.

[0053] This embodiment also provides a method for preparing a two-color freeze-dried powder by a solidification method, comprising the following steps: (1) Preparation of freeze-dried powder for the lower solidification layer: Heat excipient A1 at 80°C and stir to dissolve; after dissolution, cool down to 40°C, add excipient A2, stir until dissolved evenly, take a small amount of sample and cool it to 24°C to observe whether solidification occurs to ensure that the freeze-dried powder for the lower solidification layer can solidify after cooling; after confirmation, continue to add active ingredient A and stir to dissolve evenly; after discharging, keep at 40°C and keep warm for later use; (2) Preparing the upper non-solidified layer of freeze-dried powder: heat and stir the excipient B to dissolve, then cool it down, then add the active ingredient B, stir and dissolve evenly, then cool it down, and discharge it for later use; (3) Using the lower coagulated layer freeze-dried powder and the upper non-coagulated layer freeze-dried powder to prepare the coagulation method two-color freeze-dried powder: the lower coagulated layer freeze-dried powder is first injected into the packaging bottle at a weight ratio of 3:2 between the lower coagulated layer freeze-dried powder and the upper non-coagulated layer freeze-dried powder, and then cooled to 24°C to make it completely coagulated; then the upper non-coagulated layer freeze-dried powder is injected into the packaging bottle where the lower coagulated layer freeze-dried powder has been coagulated at a weight ratio of 3:2 between the lower coagulated layer freeze-dried powder and the upper non-coagulated layer freeze-dried powder, so that the upper non-coagulated layer freeze-dried powder can be kept in the upper layer, so that the two layers can be kept separated, and then freeze-dried. After freeze-drying, the solid method two-color freeze-dried powder is obtained.

[0054] Furthermore, in step (3), the freeze-drying process includes the following steps: (S1) Start the pre-freezing program, set the freezing temperature to -40°C and the freezing time to 3h; (S2) After the pre-freezing process is completed, the primary drying stage is entered, the vacuum degree is set to 25pa, the plate layer temperature is 5-10℃, and maintained for 5h; then the plate layer temperature is set to 5℃, maintained for 5h, and then the plate layer temperature is set to 10℃, maintained for 6h; (S3) After the first drying stage, the second drying stage is entered, the plate temperature is set to 40°C, the vacuum degree is set to 5 Pa, and the freeze-drying process is terminated after maintaining for 8 hours.

[0055] The compositions of the raw materials in the upper non-coagulated layer freeze-dried powder and the lower coagulated layer freeze-dried powder prepared in Examples 1-3 are shown in Table 1 below:

[0056] The coagulation method two-color freeze-dried powder prepared in Example 1-3 was tested for performance, and the test results are as follows: Test Example 1: Accelerated stability test Accelerated testing is a method based on applying load to the system. The inherent danger of any accelerated test is that the cosmetics are subjected to conditions far exceeding those actually experienced. The results of accelerated tests should be compared and confirmed with objective results under normal storage conditions. Several common accelerated stability test conditions for cosmetics: Heat resistance test: The product is tested for stability at a temperature higher than the actual storage conditions.

[0057] Cold resistance test: The product is tested for stability at a temperature lower than the actual storage conditions.

[0058] Lighting test: The product is tested for stability by irradiating with sunlight and simulating an environment with actual environmental changes.

[0059] The two-color freeze-dried powder cosmetic samples were placed at 25°C, 5°C, -15°C, 45°C, and simulated natural light conditions for observation and testing at intervals of 1 week, 1 month, 2 months, and 3 months. The test results are shown in Table 2 below:

[0060] It can be seen from the above table that under different conditions, the two-color freeze-dried powder of Examples 1-3 showed good stability after 3 months of accelerated testing.

[0061] Test Example 2: Solubility Test The solubility test was conducted by using purified water to perform a dissolution test, comparing the solubility of the coagulation method two-color freeze-dried powders of different embodiments, and the solubility of the finished products after being placed for different periods of time. The test results are shown in Table 3 below:

[0062] From the above table, it can be seen that the solubility of the two-color freeze-dried powder is related to the different functional substances added. Different functional substances will affect the solubility of the product, but the impact is not significant. As the storage time increases, the solubility of the two-color freeze-dried powder decreases slightly, and the decrease is small.

[0063] The above embodiments are preferred implementation schemes of the present invention. In addition, the present invention may also be implemented in other ways. Any obvious replacement without departing from the concept of the present invention is within the protection scope of the present invention.

Claims

1. A coagulation method two-color freeze-dried powder, characterized in that: It comprises a lower coagulated layer of freeze-dried powder and an upper non-coagulated layer of freeze-dried powder; the lower coagulated layer of freeze-dried powder comprises excipient A and efficacy substance A, and the excipient A comprises excipient A1 and excipient A2; the upper non-coagulated layer of freeze-dried powder comprises excipient B and efficacy substance B.

2. The solidification method two-color freeze-dried powder according to claim 1, characterized in that: The excipient A1 comprises the following raw materials in weight percentage: 3-6% mannitol, 0.3-2% trehalose, 0.01-0.1% gellan gum, 0.05-0.15% soluble collagen and 91-95% water; the excipient A2 comprises the following raw materials in weight percentage: 0.05-0.5% magnesium sulfate; the sum of the weight percentages of the excipient A1, excipient A2 and the functional substance A is 100%.

3. The solidification method two-color freeze-dried powder according to claim 1, characterized in that: The excipient B comprises the following raw materials in weight percentage: 2-10% mannitol, 0-3% trehalose and 91-95% water; the sum of the weight percentages of the excipient B and the functional substance B is 100%.

4. The coagulation method two-color freeze-dried powder according to claim 1, characterized in that: The efficacy substance A and the efficacy substance B are at least one of blue copper peptide, astaxanthin, vitamin B12, rutin, gardenia fruit extract, cocoa extract, oligopeptide-1, ergothioneine and acetyl hexapeptide-8.

5. The solidification method two-color freeze-dried powder according to claim 1, characterized in that: The weight ratio of the freeze-dried powder in the lower coagulated layer to the freeze-dried powder in the upper non-coagulated layer is 5-8:2-5.

6. A method for preparing a two-color freeze-dried powder by solidification method according to any one of claims 1 to 5, characterized in that: The steps include: (1) Preparation of freeze-dried powder for the lower solidified layer: Heat and stir excipient A1 to dissolve, then cool it down, add excipient A2, stir until dissolved evenly, then add active ingredient A, stir until dissolved evenly, and keep warm after discharging; (2) Preparing the upper non-solidified layer of freeze-dried powder: heat and stir the excipient B to dissolve it, then cool it down, then add the active ingredient B, stir and dissolve it evenly, then cool it down, and discharge it for later use; (3) Using the lower coagulated layer freeze-dried powder and the upper non-coagulated layer freeze-dried powder to prepare the coagulation method two-color freeze-dried powder: the lower coagulated layer freeze-dried powder is first injected into the packaging bottle according to the ratio of the lower coagulated layer freeze-dried powder to the upper non-coagulated layer freeze-dried powder, and then the temperature is lowered to make the lower coagulated layer freeze-dried powder completely coagulate; then the upper non-coagulated layer freeze-dried powder is injected into the packaging bottle in which the lower coagulated layer freeze-dried powder has been coagulated according to the ratio of the lower coagulated layer freeze-dried powder to the upper non-coagulated layer freeze-dried powder, so that the upper non-coagulated layer freeze-dried powder remains in the upper layer, and then freeze-drying is carried out. After freeze-drying, the coagulation method two-color freeze-dried powder is obtained.

7. The method for preparing a two-color freeze-dried powder by solidification method according to claim 6, characterized in that: In step (1), excipient A1 is heated at 70-90°C and stirred to dissolve; after dissolution, the temperature is lowered to 30-50°C, excipient A2 is added, and stirred until dissolved evenly, a small amount of sample is taken and cooled to 20-40°C to observe whether coagulation occurs, and ensure that the lower coagulation layer of freeze-dried powder can coagulate after cooling; after confirmation, the active ingredient A is added and stirred to dissolve evenly; after discharging, the temperature is maintained at 30-50°C and kept warm for later use.

8. The method for preparing a two-color freeze-dried powder by solidification method according to claim 6, characterized in that: In step (2), excipient B is heated at 70-90°C and stirred to dissolve; after dissolution, the temperature is lowered to 30-50°C, and active ingredient B is added and stirred to dissolve evenly; the temperature is lowered to 20-25°C and the material is discharged for use.

9. The method for preparing a two-color freeze-dried powder by solidification method according to claim 6, characterized in that: In step (3), the lower coagulated layer freeze-dried powder is first injected into the packaging bottle in a weight ratio of 0.5-0.8:0.2-0.5, and then cooled to 20-40°C to completely solidify the lower coagulated layer freeze-dried powder; then the upper non-coagulated layer freeze-dried powder is injected into the packaging bottle in which the lower coagulated layer freeze-dried powder has already solidified in a weight ratio of 0.5-0.8:0.2-0.5, so that the upper non-coagulated layer freeze-dried powder remains in the upper layer and the two layers are kept separated, and then freeze-dried to obtain the solid method double-color freeze-dried powder.

10. The method for preparing a two-color freeze-dried powder by solidification method according to claim 6, characterized in that: In step (3), the freeze-drying process includes the following steps: (S1) Start the pre-freezing program, set the freezing temperature to -50 to -30°C, and the freezing time to 2 to 5 hours; (S2) After the pre-freezing process is completed, the primary drying stage is entered, the vacuum degree is set to 10-50 Pa, the plate layer temperature is -20--10 ° C, and maintained for 3-5 hours; then the plate layer temperature is set to -5-5 ° C, and maintained for 3-5 hours; then the plate layer temperature is set to 5-15 ° C, and maintained for 4-8 hours; (S3) After the primary drying stage is completed, the secondary drying stage is entered, the plate temperature is set to 35-45°C, the vacuum degree is 3-10 Pa, and the freeze-drying process is terminated after maintaining for 5-10 hours.

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