Combined product of polypeptide freeze-dried tablet and no-addition secondary-throwing solvent and preparation method thereof

文档序号:753624 发布日期:2021-04-06 浏览:11次 中文

阅读说明:本技术 多肽冻干片和无添加次抛型溶媒的组合产品及其制备方法 (Combined product of polypeptide freeze-dried tablet and no-addition secondary-throwing solvent and preparation method thereof ) 是由 丁文锋 于 2020-12-30 设计创作,主要内容包括:本发明公开一种组合产品,包括多肽冻干片和无添加次抛型溶媒。所述多肽冻干片由以下质量百分浓度的原料组成:生物活性美容多肽0.0001%-5%、赋形剂5%-15%、透明质酸钠0.1%-0.3%、水解胶原1%-3%,余量为水;所述无添加次抛型溶媒由以下质量百分浓度的组份制作而成:甜菜碱1.0%-4.0%、泛醇0.1%-1.0%、尿囊素0.1%-0.5%、透明质酸钠0.01%-0.1%、甘油1.0%-3.0%,余量为水。本发明所述的组合产品的制备方法,包括多肽冻干片的制备方法和无添加次抛型溶媒的制备方法。本发明所述的组合产品使用方便,一次一抛,安全高效,可以避免防腐剂对皮肤的伤害,高效解决祛皱抗衰、祛痘修复、美白祛斑、舒缓抗敏、祛除眼袋、生发固发等一系列的皮肤问题。(The invention discloses a combined product, which comprises a polypeptide freeze-dried tablet and an additive-free secondary-throwing solvent. The polypeptide freeze-dried tablet is prepared from the following raw materials in percentage by mass: 0.0001-5% of bioactive cosmetic polypeptide, 5-15% of excipient, 0.1-0.3% of sodium hyaluronate, 1-3% of hydrolyzed collagen and the balance of water; the non-additive secondary casting solvent is prepared from the following components in percentage by mass: 1.0 to 4.0 percent of betaine, 0.1 to 1.0 percent of panthenol, 0.1 to 0.5 percent of allantoin, 0.01 to 0.1 percent of sodium hyaluronate, 1.0 to 3.0 percent of glycerol and the balance of water. The preparation method of the combination product comprises a preparation method of a polypeptide freeze-dried tablet and a preparation method of an additive-free secondary-throwing solvent. The combination product of the invention has convenient use, one-time disposal, safety and high efficiency, can avoid the damage of the preservative to the skin, and efficiently solves a series of skin problems of wrinkle removal, anti-aging, acne removal, repair, whitening, freckle removal, soothing, anti-allergy, eye pouch removal, hair growth, hair strengthening and the like.)

1. A combined product comprises a polypeptide freeze-dried tablet and an additive-free secondary-throwing solvent, and is characterized in that the polypeptide freeze-dried tablet is composed of the following raw materials in percentage by mass: 0.0001-5% of bioactive cosmetic polypeptide, 5-15% of excipient, 0.1-0.3% of sodium hyaluronate, 1-3% of hydrolyzed collagen and the balance of water; the non-additive secondary casting solvent is prepared from the following components in percentage by mass: 1.0 to 4.0 percent of betaine, 0.1 to 1.0 percent of panthenol, 0.1 to 0.5 percent of allantoin, 0.01 to 0.1 percent of sodium hyaluronate, 1.0 to 3.0 percent of glycerol and the balance of water.

2. The combination product according to claim 1, wherein the bioactive cosmetic polypeptide is selected from the group consisting of a polypeptide with wrinkle-removing and anti-aging effects, a polypeptide with acne-removing and repairing effects, a polypeptide with whitening and freckle-removing effects, a polypeptide with soothing and anti-allergy effects, a polypeptide with pouch-removing effects, and a polypeptide with hair-growing and hair-fixing effects.

3. A combination product according to claim 2, wherein the polypeptide having wrinkle-removing and anti-ageing effects comprises tripeptide-1, acetyl hexapeptide-8, acetyl octapeptide-3, dipeptide diaminobutyryl benzylamide diacetate, β -alanyl hydroxyproline diaminobutyryl benzylamide, palmitoyl pentapeptide-4, palmitoyl tetrapeptide-7, carnosine, tripeptide-1 copper, palmitoyl tripeptide-1, palmitoyl tripeptide-5, palmitoyl oligopeptide, hexapeptide-9, hexapeptide-11, or a combination thereof.

4. The combination product according to claim 2, wherein the polypeptide having an acne-removing repairing effect comprises myristoyl hexapeptide-5, myristoyl hexapeptide-23, tetrapeptide-1, antibacterial pentadecapeptide (VKRWKKWRWKWKKWV), hexapeptide-9, palmitoyl pentapeptide-4, or a combination thereof.

5. The combination product of claim 2, wherein the polypeptide having whitening and spot-removing effects comprises nonapeptide-1, tetrapeptide-27, decapeptide-12, hexapeptide-2, carnosine, glutathione, or a combination thereof.

6. A combination product according to claim 2, wherein the polypeptide having soothing anti-allergy effects comprises palmitoyl tripeptide-8, acetyl tetrapeptide-15, acetyl tetrapeptide-40, acetyl dipeptide-1 cetyl ester, acetyl hexapeptide-49, or a combination thereof.

7. The combination product of claim 2, wherein the polypeptide having pouch-removing action comprises acetyl tetrapeptide-5, palmitoyl tetrapeptide-7, dipeptide-2, palmitoyl tripeptide-1, palmitoyl pentapeptide-4, or a combination thereof.

8. The combination product of claim 2, wherein the polypeptide having hair growth promoting and hair strengthening effects comprises tripeptide-1 copper, acetyl tetrapeptide-3, biotin tripeptide-1, myristoyl pentapeptide-17, myristoyl hexapeptide-16, or a combination thereof.

9. The combination product according to claim 1, wherein the excipient is selected from mannitol, trehalose, lactose, pullulan, dextran, or a combination thereof.

10. The method for preparing a combination product according to claim 1, wherein the method comprises a method for preparing a lyophilized polypeptide tablet and a method for preparing a non-additive secondary-disposable vehicle.

11. The method for preparing a combination product according to claim 10, wherein the method for preparing a lyophilized polypeptide tablet comprises the following steps:

(1) weighing raw materials according to mass percent, putting 0.0001-5% of bioactive cosmetic polypeptide, 5-15% of excipient, 0.1-0.3% of sodium hyaluronate, 1-3% of hydrolyzed collagen and the balance of water in a mixing container, stirring for 10-15 min at the rotating speed of 500-800 rpm, mixing and dissolving, and filtering by using a 0.22 mu m filter membrane to obtain a filtered solution;

(2) filling the filtered solution into a groove of an aluminum foil blister sheet in a GMP standard environment, wherein the filling amount is 0.3-1.5 mL, so as to obtain a filled solution;

(3) pre-starting a vacuum freeze dryer, reducing the temperature of a freeze-drying plate layer to-45 ℃ to-40 ℃, and preserving the temperature for 2-3 h;

(4) putting the filled solution into a vacuum freeze dryer, vacuumizing, maintaining the vacuum degree at 30Pa, heating to-5 ℃, preserving heat for 10-15 h, then heating to 10 ℃, and preserving heat for 1-3 h;

(5) and maintaining the vacuum degree at 30Pa, continuously heating to 30 ℃, preserving the heat for 1-3 h, heating to 38 ℃, preserving the heat for 8-12h, and completing freeze drying to obtain the polypeptide freeze-dried tablet.

12. The method of preparing a combination product according to claim 10, wherein the method of preparing the non-additively disposable vehicle comprises the steps of:

(1) weighing raw materials according to the mass percent, adding 1.0-3.0% of glycerol, 0.01-0.1% of sodium hyaluronate, 0.1-0.5% of allantoin and the balance of water into a mixing container, heating to 80-85 ℃, and uniformly stirring;

(2) cooling to 40-45 ℃, adding 0.1-1.0% of panthenol and 1.0-4.0% of betaine, stirring for 5-10 min, and filtering with a 0.22 mu m filter membrane to obtain a filtered solution;

(3) and (3) forming the plastic ampoule by adopting a blowing and filling technology, filling the filtered solution into the plastic ampoule with the filling amount of 1.0-1.5 mL, and sealing the filled plastic ampoule to obtain the non-additive secondary-throwing solvent.

Technical Field

The invention belongs to the technical field of beauty polypeptide, and particularly relates to a combined product of a polypeptide freeze-dried tablet and an additive-free secondary-throwing solvent and a preparation method thereof.

Background

The freeze-dried cosmetic tablet (Cosmetics freeze-dried tablets) refers to a cosmetic which is prepared by carrying out vacuum freeze-drying process on liquid skin care products, forming at one time, and preparing into loose-structure tablets (blocks or spheres or powder) according to different moulds, and can be quickly dissolved in a medium to care human skin. The freeze-dried tablet is dehydrated and dried powder, can be stored for a long time without adding a preservative, is milder and more friendly to the skin, is a real green skin care product, and can greatly reduce the probability of allergy particularly to sensitive skin.

The polypeptide is a compound formed by connecting amino acids together through peptide bonds, and has multiple effects of removing wrinkles, resisting aging, resisting bacteria, removing acnes, whitening, removing freckles, relieving, resisting allergy, removing pouches, growing hair, consolidating hair and the like. Since the polypeptide can remarkably improve various skin problems, the polypeptide is widely applied to skin care products. In order to isolate the influence of oxygen and moisture on the polypeptide and ensure the activity and stability of the polypeptide to the maximum extent, the polypeptide needs to be lyophilized and stored hermetically, so that the polypeptide lyophilized tablet which is safe, efficient and convenient to use is prepared.

The freeze-dried tablet is generally packaged by a blister material, and compared with a penicillin bottle, the packaging mode is convenient to carry and safe and convenient to use. When in use, the upper aluminum foil layer is uncovered, the freeze-dried piece is taken out and placed in the palm, and the solvent is added for dissolution.

The polypeptide freeze-dried tablet is sterile, no preservative is needed to be added, but in order to prevent microbial contamination introduced into a solvent and influence the use safety of the product, the preservative is generally added into the solvent to prevent the microbial growth, and the commonly used preservative combination is phenoxyethanol and methyl hydroxybenzoate, germa BP and methyl hydroxybenzoate, polydimethylene biguanide and the like, however, sensitive symptoms such as erythema, desquamation, pimple and pruritus can be caused on the skin by using the skin care product containing the substances for a long time, but the growth of the microorganisms cannot be inhibited by adding no or little preservative, so the product quality is influenced.

Therefore, there is a need to provide a combination of a lyophilized polypeptide tablet and a non-additive, sterile, sub-disposable vehicle.

Disclosure of Invention

In view of the defects of the prior art, one of the purposes of the present invention is to provide a combination product of a polypeptide lyophilized tablet and no secondary-disposable solvent. The polypeptide freeze-dried tablet adopts a vacuum freeze-drying technology, and the polypeptide solution is formed in the groove of the aluminum foil bubble cap tablet at one time to prepare the tablet with a loose structure. The polypeptide freeze-dried tablet is sterile, has no preservative, can ensure the activity and stability of the polypeptide to the maximum extent, and is safe, efficient and convenient to use. The non-additive secondary-disposable solvent adopts a blowing and filling technology, namely a bottle blowing (Blow) -filling (Fill) -sealing (Seal), which is called BFS technology for short, the molding of the plastic ampoule and the filling of the solvent liquid are completed at one time under the aseptic condition, and the filled plastic ampoule is sealed to obtain the non-additive secondary-disposable solvent. The solvent is not required to be added with preservative, the ampoule bottle is packaged independently, one freeze-dried tablet is matched with one non-additive disposable solvent for use, and the disposable ampoule bottle is disposable, so that the harm to skin caused by the addition of the preservative can be avoided, and the influence on the use safety of the product caused by the microbial pollution introduced into the solvent can be prevented.

The invention also aims to provide a preparation method of the combination product of the polypeptide freeze-dried tablet and no secondary throwing type solvent.

In order to achieve the purpose, the invention adopts the following technical scheme:

a combined product comprises a polypeptide freeze-dried tablet and an additive-free secondary-throwing solvent, wherein the polypeptide freeze-dried tablet comprises the following raw materials in percentage by mass: 0.0001-5% of bioactive cosmetic polypeptide, 5-15% of excipient, 0.1-0.3% of sodium hyaluronate, 1-3% of hydrolyzed collagen and the balance of water; the non-additive secondary casting solvent is prepared from the following components in percentage by mass: 1.0 to 4.0 percent of betaine, 0.1 to 1.0 percent of panthenol, 0.1 to 0.5 percent of allantoin, 0.01 to 0.1 percent of sodium hyaluronate, 1.0 to 3.0 percent of glycerol and the balance of water.

The bioactive beautifying polypeptide is selected from polypeptide with wrinkle removing and anti-aging effects, polypeptide with acne removing and repairing effects, polypeptide with whitening and freckle removing effects, polypeptide with soothing and anti-allergy effects, polypeptide with eye pouch removing effects and polypeptide with hair growing and hair strengthening effects.

The polypeptide with wrinkle-removing and anti-aging effects comprises tripeptide-1, acetyl hexapeptide-8, acetyl octapeptide-3, dipeptide diaminobutyrylbenzylamide diacetate, beta-alanyl hydroxyproline diaminobutyrylbenzylamide, palmitoyl pentapeptide-4, palmitoyl tetrapeptide-7, carnosine, tripeptide-1 copper, palmitoyl tripeptide-1, palmitoyl tripeptide-5, palmitoyl oligopeptide, hexapeptide-9, hexapeptide-11, or a combination thereof.

The polypeptide with the acne-removing and repairing effects comprises myristoyl hexapeptide-5, myristoyl hexapeptide-23, tetrapeptide-1, antibacterial pentadecapeptide (VKRWKKWRWKWKKWV), hexapeptide-9, palmitoyl pentapeptide-4, or a combination thereof.

The polypeptide with whitening and freckle removing effects comprises nonapeptide-1, tetrapeptide-27, decapeptide-12, hexapeptide-2, carnosine, glutathione or a combination thereof.

The polypeptide with soothing and anti-allergy effects comprises palmitoyl tripeptide-8, acetyl tetrapeptide-15, acetyl tetrapeptide-40, acetyl dipeptide-1 cetyl esters, acetyl hexapeptide-49, or a combination thereof.

The polypeptide with the function of removing under-eye puffiness comprises acetyl tetrapeptide-5, palmitoyl tetrapeptide-7, dipeptide-2, palmitoyl tripeptide-1, palmitoyl pentapeptide-4, or the combination thereof.

The polypeptide with hair growth promoting and hair strengthening effects comprises tripeptide-1 copper, acetyl tetrapeptide-3, biotin tripeptide-1, myristoyl pentapeptide-17, myristoyl hexapeptide-16, or their combination.

The excipient of the invention is selected from mannitol, trehalose, lactose, pullulan, dextran or the combination thereof.

The preparation method of the combination product comprises a preparation method of a polypeptide freeze-dried tablet and a preparation method of an additive-free secondary-throwing solvent.

The preparation method of the polypeptide freeze-dried tablet comprises the following steps:

(1) weighing raw materials according to mass percent, putting 0.0001-5% of bioactive cosmetic polypeptide, 5-15% of excipient, 0.1-0.3% of sodium hyaluronate, 1-3% of hydrolyzed collagen and the balance of water in a mixing container, stirring for 10-15 min at the rotating speed of 500-800 rpm, mixing and dissolving, and filtering by using a 0.22 mu m filter membrane to obtain a filtered solution;

(2) filling the filtered solution into a groove of an aluminum foil blister sheet in a GMP standard environment, wherein the filling amount is 0.3-1.5 mL, so as to obtain a filled solution;

(3) pre-starting a vacuum freeze dryer, reducing the temperature of a freeze-drying plate layer to-45 ℃ to-40 ℃, and preserving the temperature for 2-3 h;

(4) putting the filled solution into a vacuum freeze dryer, vacuumizing, maintaining the vacuum degree at 30Pa, heating to-5 ℃, preserving heat for 10-15 h, then heating to 10 ℃, and preserving heat for 1-3 h;

(5) and maintaining the vacuum degree at 30Pa, continuously heating to 30 ℃, preserving the heat for 1-3 h, heating to 38 ℃, preserving the heat for 8-12h, and completing freeze drying to obtain the polypeptide freeze-dried tablet.

The preparation method of the non-additive secondary-polishing solvent comprises the following steps:

(1) weighing raw materials according to the mass percent, adding 1.0-3.0% of glycerol, 0.01-0.1% of sodium hyaluronate, 0.1-0.5% of allantoin and the balance of water into a mixing container, heating to 80-85 ℃, and uniformly stirring;

(2) cooling to 40-45 ℃, adding 0.1-1.0% of panthenol and 1.0-4.0% of betaine, stirring for 5-10 min, and filtering with a 0.22 mu m filter membrane to obtain a filtered solution;

(3) and (3) forming the plastic ampoule by adopting a blowing and filling technology, filling the filtered solution into the plastic ampoule with the filling amount of 1.0-1.5 mL, and sealing the filled plastic ampoule to obtain the non-additive secondary-throwing solvent.

Compared with the prior art, the invention has the advantages that:

the combination product is convenient to use, is disposable, safe and efficient, and the freeze-dried tablet can ensure the activity and stability of the polypeptide to the maximum extent, so that a series of skin problems of wrinkle removal, anti-aging, acne removal, repair, whitening, freckle removal, soothing, anti-allergy, pouch removal, hair growth, hair strengthening and the like can be efficiently solved; compared with the non-additive non-secondary-polishing sterile aqueous solvent, the non-additive secondary-polishing sterile aqueous solvent can prevent the solvent from breeding microorganisms in the continuous use process after being started, so that the use safety of the product is influenced; compared with a solvent added with the preservative, the preservative can avoid the damage of the preservative to the skin.

Detailed Description

For a better understanding of the present invention, the following detailed description of the invention is given in conjunction with examples, however, it should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention.

Example 1 preparation of a combination of a wrinkle-removing anti-aging polypeptide lyophilized tablet and no added secondary-disposable vehicle

1.1 preparation of polypeptide lyophilized tablet for removing wrinkles and resisting aging

(1) Weighing raw materials according to the mass percentage, putting 0.01% acetyl hexapeptide-8, 0.01% palmitoyl pentapeptide-4, 5% trehalose, 10% mannitol, 0.2% sodium hyaluronate, 1% hydrolyzed collagen and the balance of water into a mixing container, stirring for 12min at the rotating speed of 600rpm, mixing and dissolving, and filtering by using a 0.22 mu m filter membrane to obtain a filtered solution;

(2) filling the filtered solution into a groove of an aluminum foil blister sheet in a GMP standard environment, wherein the filling amount is 1.0mL, so as to obtain a filled solution;

(3) starting a vacuum freeze dryer in advance, reducing the temperature of a freeze-drying plate layer to-45 ℃, and preserving the heat for 2.5 hours;

(4) putting the filled solution into a vacuum freeze dryer, vacuumizing, maintaining the vacuum degree at 30Pa, heating to-5 ℃, keeping the temperature for 13h, heating to 10 ℃, and keeping the temperature for 2 h;

(5) and maintaining the vacuum degree at 30Pa, continuously heating to 30 ℃, keeping the temperature for 2h, heating to 38 ℃, keeping the temperature for 10h, and completing freeze drying to obtain the polypeptide freeze-dried tablet.

1.2 preparation of additive-free Secondary polishing-type solvent

(1) Weighing the raw materials according to the mass percent, adding 2.0 percent of glycerin, 0.05 percent of sodium hyaluronate, 0.3 percent of allantoin and the balance of water into a mixing container, heating to 80-85 ℃, and uniformly stirring;

(2) cooling to 40-45 ℃, adding 0.5% of panthenol and 2.5% of betaine, stirring for 10min, and filtering by using a 0.22-micron filtering membrane to obtain a filtered solution;

(3) and (3) forming the plastic ampoule by adopting a blowing and filling technology, filling the filtered solution into the plastic ampoule with the filling amount of 1.0mL, and sealing the filled plastic ampoule to obtain the non-additive secondary-throwing solvent.

Example 2 preparation of a combination product of an anti-acne repair polypeptide lyophilized tablet and no added secondary-disposable solvent

2.1 preparation of acne-removing repairing polypeptide lyophilized tablet

(1) Weighing raw materials according to the mass percentage, putting 0.01% of myristoyl hexapeptide-23, 0.01% of hexapeptide-9, 5% of trehalose, 10% of mannitol, 0.2% of sodium hyaluronate, 1% of hydrolyzed collagen and the balance of water in a mixing container, stirring for 12min at the rotating speed of 600rpm, mixing and dissolving, and filtering by using a 0.22 mu m filter membrane to obtain a filtered solution;

(2) filling the filtered solution into a groove of an aluminum foil blister sheet in a GMP standard environment, wherein the filling amount is 1.0mL, so as to obtain a filled solution;

(3) starting a vacuum freeze dryer in advance, reducing the temperature of a freeze-drying plate layer to-45 ℃, and preserving the heat for 2.5 hours;

(4) putting the filled solution into a vacuum freeze dryer, vacuumizing, maintaining the vacuum degree at 30Pa, heating to-5 ℃, keeping the temperature for 13h, heating to 10 ℃, and keeping the temperature for 2 h;

(5) and maintaining the vacuum degree at 30Pa, continuously heating to 30 ℃, keeping the temperature for 2h, heating to 38 ℃, keeping the temperature for 10h, and completing freeze drying to obtain the polypeptide freeze-dried tablet.

2.2 preparation of additive-free Secondary polishing-type solvent

(1) Weighing the raw materials according to the mass percent, adding 2.0 percent of glycerin, 0.05 percent of sodium hyaluronate, 0.3 percent of allantoin and the balance of water into a mixing container, heating to 80-85 ℃, and uniformly stirring;

(2) cooling to 40-45 ℃, adding 0.5% of panthenol and 2.5% of betaine, stirring for 10min, and filtering by using a 0.22-micron filtering membrane to obtain a filtered solution;

(3) and (3) forming the plastic ampoule by adopting a blowing and filling technology, filling the filtered solution into the plastic ampoule with the filling amount of 1.0mL, and sealing the filled plastic ampoule to obtain the non-additive secondary-throwing solvent.

Example 3 preparation of a combination product of a whitening and spot-removing polypeptide lyophilized tablet and no secondary-disposable vehicle

3.1 preparation of whitening and freckle-removing polypeptide freeze-dried tablet

(1) Weighing raw materials according to the mass percent, putting 0.01 percent of tetrapeptide-27, 0.01 percent of hexapeptide-2, 5 percent of trehalose, 10 percent of mannitol, 0.2 percent of sodium hyaluronate, 1 percent of hydrolyzed collagen and the balance of water into a mixing container, stirring for 12min at the rotating speed of 600rpm, mixing and dissolving, and filtering by using a 0.22 mu m filter membrane to obtain a filtered solution;

(2) filling the filtered solution into a groove of an aluminum foil blister sheet in a GMP standard environment, wherein the filling amount is 1.0mL, so as to obtain a filled solution;

(3) starting a vacuum freeze dryer in advance, reducing the temperature of a freeze-drying plate layer to-45 ℃, and preserving the heat for 2.5 hours;

(4) putting the filled solution into a vacuum freeze dryer, vacuumizing, maintaining the vacuum degree at 30Pa, heating to-5 ℃, keeping the temperature for 13h, heating to 10 ℃, and keeping the temperature for 2 h;

(5) and maintaining the vacuum degree at 30Pa, continuously heating to 30 ℃, keeping the temperature for 2h, heating to 38 ℃, keeping the temperature for 10h, and completing freeze drying to obtain the polypeptide freeze-dried tablet.

3.2 preparation of additive-free Secondary polishing-type solvent

(1) Weighing the raw materials according to the mass percent, adding 2.0 percent of glycerin, 0.05 percent of sodium hyaluronate, 0.3 percent of allantoin and the balance of water into a mixing container, heating to 80-85 ℃, and uniformly stirring;

(2) cooling to 40-45 ℃, adding 0.5% of panthenol and 2.5% of betaine, stirring for 10min, and filtering by using a 0.22-micron filtering membrane to obtain a filtered solution;

(3) and (3) forming the plastic ampoule by adopting a blowing and filling technology, filling the filtered solution into the plastic ampoule with the filling amount of 1.0mL, and sealing the filled plastic ampoule to obtain the non-additive secondary-throwing solvent.

Example 4 preparation of a combination of a soothing anti-allergy polypeptide lyophilized tablet and no added secondary-disposable vehicle

4.1 preparation of soothing anti-allergy polypeptide lyophilized tablet

(1) Weighing raw materials according to mass percent, putting 0.01 percent of palmitoyl tripeptide-8, 0.01 percent of acetyl dipeptide-1 cetyl ester, 5 percent of trehalose, 10 percent of mannitol, 0.2 percent of sodium hyaluronate, 1 percent of hydrolyzed collagen and the balance of water into a mixing container, stirring for 12min at the rotating speed of 600rpm, mixing and dissolving, and filtering by using a 0.22 mu m filter membrane to obtain a filtered solution;

(2) filling the filtered solution into a groove of an aluminum foil blister sheet in a GMP standard environment, wherein the filling amount is 1.0mL, so as to obtain a filled solution;

(3) starting a vacuum freeze dryer in advance, reducing the temperature of a freeze-drying plate layer to-45 ℃, and preserving the heat for 2.5 hours;

(4) putting the filled solution into a vacuum freeze dryer, vacuumizing, maintaining the vacuum degree at 30Pa, heating to-5 ℃, keeping the temperature for 13h, heating to 10 ℃, and keeping the temperature for 2 h;

(5) and maintaining the vacuum degree at 30Pa, continuously heating to 30 ℃, keeping the temperature for 2h, heating to 38 ℃, keeping the temperature for 10h, and completing freeze drying to obtain the polypeptide freeze-dried tablet.

4.2 preparation of additive-free Secondary polishing-type solvent

(1) Weighing the raw materials according to the mass percent, adding 2.0 percent of glycerin, 0.05 percent of sodium hyaluronate, 0.3 percent of allantoin and the balance of water into a mixing container, heating to 80-85 ℃, and uniformly stirring;

(2) cooling to 40-45 ℃, adding 0.5% of panthenol and 2.5% of betaine, stirring for 10min, and filtering by using a 0.22-micron filtering membrane to obtain a filtered solution;

(3) and (3) forming the plastic ampoule by adopting a blowing and filling technology, filling the filtered solution into the plastic ampoule with the filling amount of 1.0mL, and sealing the filled plastic ampoule to obtain the non-additive secondary-throwing solvent.

Example 5 preparation of a combination of a pouch-removing polypeptide lyophilized tablet and no added secondary-disposable vehicle

5.1 preparation of polypeptide lyophilized tablet for removing pouch

(1) Weighing raw materials according to the mass percentage, putting 0.01% of acetyl tetrapeptide-5, 0.01% of dipeptide-2, 5% of trehalose, 10% of mannitol, 0.2% of sodium hyaluronate, 1% of hydrolyzed collagen and the balance of water into a mixing container, stirring for 12min at the rotating speed of 600rpm, mixing and dissolving, and filtering by using a 0.22 mu m filter membrane to obtain a filtered solution;

(2) filling the filtered solution into a groove of an aluminum foil blister sheet in a GMP standard environment, wherein the filling amount is 1.0mL, so as to obtain a filled solution;

(3) starting a vacuum freeze dryer in advance, reducing the temperature of a freeze-drying plate layer to-45 ℃, and preserving the heat for 2.5 hours;

(4) putting the filled solution into a vacuum freeze dryer, vacuumizing, maintaining the vacuum degree at 30Pa, heating to-5 ℃, keeping the temperature for 13h, heating to 10 ℃, and keeping the temperature for 2 h;

(5) and maintaining the vacuum degree at 30Pa, continuously heating to 30 ℃, keeping the temperature for 2h, heating to 38 ℃, keeping the temperature for 10h, and completing freeze drying to obtain the polypeptide freeze-dried tablet.

5.2 preparation of additive-free Secondary polishing-type solvent

(1) Weighing the raw materials according to the mass percent, adding 2.0 percent of glycerin, 0.05 percent of sodium hyaluronate, 0.3 percent of allantoin and the balance of water into a mixing container, heating to 80-85 ℃, and uniformly stirring;

(2) cooling to 40-45 ℃, adding 0.5% of panthenol and 2.5% of betaine, stirring for 10min, and filtering by using a 0.22-micron filtering membrane to obtain a filtered solution;

(3) and (3) forming the plastic ampoule by adopting a blowing and filling technology, filling the filtered solution into the plastic ampoule with the filling amount of 1.0mL, and sealing the filled plastic ampoule to obtain the non-additive secondary-throwing solvent.

Example 6 preparation of a combination of Hair growth and Hair solidification polypeptide lyophilized tablet and No additional Secondary-throw vehicle

6.1 preparation of polypeptide lyophilized tablet for promoting Hair growth and consolidating hair

(1) Weighing raw materials according to the mass percent, putting 0.01% of myristoyl pentapeptide-17, 0.01% of myristoyl hexapeptide-16, 5% of trehalose, 10% of mannitol, 0.2% of sodium hyaluronate, 1% of hydrolyzed collagen and the balance of water in a mixing container, stirring for 12min at the rotating speed of 600rpm, mixing and dissolving, and filtering by using a 0.22 mu m filter membrane to obtain a filtered solution;

(2) filling the filtered solution into a groove of an aluminum foil blister sheet in a GMP standard environment, wherein the filling amount is 1.0mL, so as to obtain a filled solution;

(3) starting a vacuum freeze dryer in advance, reducing the temperature of a freeze-drying plate layer to-45 ℃, and preserving the heat for 2.5 hours;

(4) putting the filled solution into a vacuum freeze dryer, vacuumizing, maintaining the vacuum degree at 30Pa, heating to-5 ℃, keeping the temperature for 13h, heating to 10 ℃, and keeping the temperature for 2 h;

(5) and maintaining the vacuum degree at 30Pa, continuously heating to 30 ℃, keeping the temperature for 2h, heating to 38 ℃, keeping the temperature for 10h, and completing freeze drying to obtain the polypeptide freeze-dried tablet.

6.2 preparation of additive-free Secondary polishing-type solvent

(1) Weighing the raw materials according to the mass percent, adding 2.0 percent of glycerin, 0.05 percent of sodium hyaluronate, 0.3 percent of allantoin and the balance of water into a mixing container, heating to 80-85 ℃, and uniformly stirring;

(2) cooling to 40-45 ℃, adding 0.5% of panthenol and 2.5% of betaine, stirring for 10min, and filtering by using a 0.22-micron filtering membrane to obtain a filtered solution;

(3) and (3) forming the plastic ampoule by adopting a blowing and filling technology, filling the filtered solution into the plastic ampoule with the filling amount of 1.0mL, and sealing the filled plastic ampoule to obtain the non-additive secondary-throwing solvent.

Example 7 anti-aging efficacy test

7.1 Subjects

60 healthy women, 30-50 years old, were randomized into 2 groups, with an average of 30 people per group.

7.2 test specimens

Example 1 placebo as blank control.

7.3 test Instrument

Cotomermameter MPA580 host, manufactured by Courage + Khazaka, Germany (CK, Germany), the probe used was a Revistometer RV600 elastofiber tissue test probe.

7.4 test procedures

Measuring blank R2, R5 and R7 values 30min after cleaning the face area,

wherein R2 ═ Ua/Uf, R5 ═ Ur/Ue, R7 ═ Ur/Uf,

ua: the recovery value of the skin from the removal of the negative pressure to the next successive test of the repressurization of the skin surface;

and (Uf): the maximum amount of stretching of the skin in the presence of negative pressure;

ur: after the negative pressure is removed for 0.1s, the recovery value and the viscoelasticity part value, or the plastic part value, of the skin are obtained;

ue: after constant negative pressure is applied to the skin, the stretching amount of the skin is 0.1s, and the stretching amount of the elastic part is positioned;

the test specimens were then applied evenly to the face twice a day, with the application being adhered to the face in the morning and evening, without the use of other cosmetics, for 4 weeks, and the skin R2, R5, R7 values of the test areas before and after administration were recorded and tested, respectively. The test of the same subject is performed by the same measuring person.

7.5 test results

The efficacy of the product in improving skin elasticity and resisting aging is evaluated by comparing the changes of R2, R5 and R7 values of the skin before and after administration, wherein the changes of R2, R5 and R7 values are shown in the following table 1:

TABLE 1 Change in the values of R2, R5, R7 in the skin before and after administration of each group

Note: the closer the R2, R5, R7 values are to 1, the better the skin elasticity.

As can be seen from the data in the table, the measured values of R2, R5 and R7 of the skin are significantly improved after 4 weeks using the combination product of example 1, and the change rates of R2, R5 and R7 before and after the test are greater, compared with those of the placebo group, indicating that the combination product of example 1 can significantly improve the elasticity of the skin and has excellent anti-aging effect.

The foregoing is a more detailed description of the present invention in connection with specific preferred embodiments thereof, and is not intended to limit the invention to the particular forms disclosed. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.

10页详细技术资料下载
上一篇:一种医用注射器针头装配设备
下一篇:一种自体脂肪源干细胞细胞因子提取液的眼霜制备方法

网友询问留言

已有0条留言

还没有人留言评论。精彩留言会获得点赞!

精彩留言,会给你点赞!

技术分类