CN114557937A

CN114557937A - Freeze-dried powder and preparation method thereof

Info

Publication number: CN114557937A
Application number: CN202210402358.1A
Authority: CN
Inventors: 姜宁
Original assignee: Guangzhou Xinman Cosmetics Co ltd
Current assignee: Guangzhou Xinman Cosmetics Co ltd
Priority date: 2022-04-18
Filing date: 2022-04-18
Publication date: 2022-05-31

Abstract

The invention discloses freeze-dried powder and a preparation method thereof, wherein the freeze-dried powder comprises mannitol, sodium alginate, cell complex biological peptide, nicotinamide, a fructus cnidii extract, a glycyrrhiza glabra extract, a lotus leaf extract and deionized water. According to the freeze-dried powder disclosed by the invention, mannitol and sodium alginate are added as a protective agent and a shaping agent, so that on one hand, the damage of an active ingredient during freeze-drying is reduced, the biological activity of the active ingredient is furthest kept, on the other hand, the dosage of mannitol is reduced, and the freeze-dried powder has more excellent moisturizing performance.

Description

Freeze-dried powder and preparation method thereof

Technical Field

The invention belongs to the technical field of cosmetics, and particularly relates to freeze-dried powder as well as a preparation method and application thereof.

Background

The freeze-dried powder is prepared by freezing the water in the liquid medicine in advance by adopting a vacuum freeze-drying method of a freeze dryer, and then sublimating the frozen water in the liquid medicine in a vacuum sterile environment, thereby obtaining freeze drying. In short, the water in the liquid medicine is pumped out under low temperature environment, and the original medicine effect is kept. As a technique for efficiently maintaining the effectiveness of active ingredients, the lyophilization process has been increasingly used in the cosmetic industry.

CN106619150A discloses a gamma PGA modified natural sunscreen moisturizing liposome freeze-dried powder, which comprises the following components in percentage by mass: 2-5% of rutin and pineapple leaf extract, 15-35% of phospholipid, 5-10% of cholesterol, 2-8% of positive charge control agent, 803-12% of Tween, 0.5-2% of VE, 0.5-2% of VC, 1-14% of beta glucan, 1-3% of gamma polyglutamic acid, 20-60% of freeze-drying protective agent and less than or equal to 5% of water, wherein the sum of the mass of the components is 100%. The freeze-dried liposome powder can be directly added into cosmetics after hydration, is sun-proof and moisture-retaining, and has the advantages of low irritation, good transdermal absorption effect and high release rate of active ingredients.

CN113181343A discloses a preparation method of a repairable ceramide moisturizing freeze-dried powder, wherein the prepared freeze-dried powder comprises 1-10 parts of ceramide, 10-30 parts of mannitol, 5-10 parts of L-arginine, 11-2 parts of oligopeptide-11, 31-2 parts of oligopeptide-2, 51-2 parts of oligopeptide-51, 2-5 parts of centella asiatica, 1-4 parts of polygonum cuspidatum root, 2-4 parts of scutellaria baicalensis, 1-3 parts of tea leaves and 5-10 parts of aloe.

At present, mannitol sugar is mostly adopted as a protective agent or excipient in cosmetic freeze-dried powder sold on the market, and too high concentration of mannitol can cause cells to be rapidly dehydrated, so that the moisturizing function of the product is greatly reduced.

Disclosure of Invention

In order to solve the technical problems, the invention provides freeze-dried powder and a preparation method thereof.

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

a lyophilized powder comprises mannitol, sodium alginate, cell complex biological peptide, nicotinamide, fructus Cnidii extract, Glycyrrhrizae radix extract, folium Nelumbinis extract and deionized water.

Preferably, the freeze-dried powder comprises the following components in percentage by mass: 1-3% of mannitol, 3-6% of sodium alginate, 4-7% of cell composite biological peptide, 20-25% of nicotinamide, 0.3-0.5% of fructus cnidii extract, 2-5% of glycyrrhiza glabra extract, 0.1-0.3% of lotus leaf extract and the balance of deionized water.

Further preferably, the moisturizing freeze-dried powder comprises the following components in percentage by mass: 1.3-2.7% of mannitol, 3.2-5.5% of sodium alginate, 5-6% of cell composite biological peptide, 21-24% of nicotinamide, 0.35-0.45% of fructus cnidii extract, 2.5-4.5% of glycyrrhiza glabra extract, 0.12-0.28% of lotus leaf extract and the balance of deionized water.

Most preferably, the freeze-dried powder comprises the following components in percentage by mass: 2% of mannitol, 4% of sodium alginate, 5.5% of cell composite biological peptide, 22% of nicotinamide, 0.4% of fructus cnidii extract, 3% of glycyrrhiza glabra extract, 0.2% of lotus leaf extract and the balance of deionized water.

The invention also provides a preparation method of the freeze-dried powder, which comprises the following steps:

(1) uniformly mixing mannitol, sodium alginate, cell complex biological peptide, nicotinamide, fructus cnidii extract, glycyrrhiza glabra extract, lotus leaf extract and deionized water according to the formula ratio, and filtering to obtain sterile filtrate;

(2) and (2) freeze-drying the sterile filtrate obtained in the step (1), and crushing to obtain the freeze-dried powder.

Preferably, the conditions of the freeze-drying in the step (2) are: and (4) carrying out freeze drying after quick freezing by using liquid nitrogen.

The invention also provides application of the multi-dry powder in preparation of cosmetics.

Preferably, the cosmetic is at least one of essence, facial mask, cream and gel.

Preferably, the solvent of the freeze-dried powder is: water or aqueous hyaluronic acid solution.

Further preferably, the freeze-dried powder and the solvent are 30 mg: 2.5 ml.

The invention also provides a cosmetic, which comprises the freeze-dried powder or the freeze-dried powder prepared by the preparation method.

The beneficial effects of the invention are as follows:

(1) according to the freeze-dried powder disclosed by the invention, mannitol and sodium alginate are added as a protective agent and a shaping agent, so that on one hand, the damage of an active ingredient during freeze-drying is reduced, the biological activity of the active ingredient is furthest maintained, on the other hand, the dosage of mannitol is reduced, and the freeze-dried powder has more excellent moisturizing performance.

(2) The freeze-dried powder disclosed by the invention has the effects of moisturizing and repairing (repairing skin barriers), and meanwhile, the freeze-dried powder is good in safety, free of stimulation to skin and suitable for long-term use.

Detailed Description

The embodiments of the present invention are described below in conjunction with specific embodiments, and before the embodiments of the present invention are further described, it is to be understood that the scope of the present invention is not limited to the specific embodiments described below; it is also to be understood that the terminology used in the examples is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present invention.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.

The sources of the raw materials used in the present invention are not limited, and the raw materials used in the present invention are all those commonly available in the art unless otherwise specified. The cell composite biological peptide is provided by Guangzhou Elegag Biotechnology Limited, and comprises the components of glycerol, propylene glycol, collagen, hyaluronic acid, oligopeptide 1, oligopeptide 2 and oligopeptide 5; niacinamide is available from imperial corporation (the netherlands); the extract of Glycyrrhiza GLABRA (Glycyrrhiza GLABRA) root is provided by Onli, Shanghai; fructus cnidii extract, product specification: 10% of osthole; lotus leaf extract, product specification, flavone 30%.

Freeze-dried powder (Lance skin repair freeze-dried powder)

The compositions and amounts of the lyophilized powders in the examples and comparative examples are shown in table 1.

TABLE 1 composition and amount of lyophilized powder

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

Second, evaluation of moisturizing efficacy

1. Measuring instrument

A skin moisture tester Comeometer CM825 and a skin moisture loss tester Tewameter TM 300.

2. Detection site

(1) Skin stratum corneum moisture content-cheek;

(2) skin transdermal water loss-cheek.

3. Detecting an environment

The environmental temperature of the test is 20.5-21.4 ℃, and the relative humidity is 48.9-53.9% RH.

4. Detection method

Reference T/ZHCA 003-. Selecting Chinese healthy female subjects with dry facial skin, water shortage and poor facial skin barrier function, wherein the TEWL basic value of a test area is more than or equal to 12, and the age range is 18-60 years. The test product was used before (D0) and 28 days (D28) to measure the stratum corneum water content and the percutaneous water loss of the skin of the subjects, respectively, by the front and back control method.

(1) Specific detection method

The subject cleans the face with the face cleaning product, wipes the skin dry with dry facial tissue, sits still for 20min in a laboratory at a temperature of 21 + -1 deg.C and a humidity of 50 + -10% RH; the laboratory technician operates the Tewameter, Corneometer instrument to determine the relevant index of the subject's test site.

(2) Criteria for inclusion and exclusion of test population

Inclusion criteria were:

1.1 healthy women, aged 18-60 years;

1.2 dry facial skin, lack of moisture;

1.3 the barrier function of facial skin is poor, and the TEWL basic value of a test area is more than or equal to 12;

1.4 can be well matched with testers, and the regularity of life can be kept during the research period;

1.5 can read and understand all contents of the informed consent and voluntarily sign the informed consent;

1.6 during the test period, consent was not given to the use of any cosmetics, drugs and nutraceuticals that have an impact on the outcome;

1.7 other corresponding inclusion criteria.

Exclusion criteria:

any person with any of the following conditions must be excluded from this study:

2.1 facial skin diseases may affect the judgment of the test result;

2.2 those with high allergic constitution;

2.3 pregnant, lactating or female intended to become pregnant during the test;

2.4 patients with severe center of gravity, liver and kidney function damage and severe immunologic hypofunction;

2.5 those with mental disorders, severe endocrine disorders, and oral contraceptives;

the drug clinical testers or other testers are involved in the treatment within 2.630 days, or the drug which has an influence on the test result in systematic use within about 1 week;

those with cosmetic products that were orally and topically administered within 2.72 weeks that may have an effect on the outcome of the test;

2.8 the test person can not be matched;

2.9 investigators considered inappropriate for attending to the present investigator;

2.10 other corresponding exclusion criteria.

5. Calculation method

The change rate is calculated by the following formula relative to the change rate before use:

the product was used for 28 days Δ (difference) D28-D0.

In the formula, D0-skin parameter base value before the product was applied to the test area.

D28-skin parameter values for 28 days of product use in a test area.

N-number of subjects.

6. The result of the detection

The application method of the test product Lance skin repair freeze-dried powder (30mg freeze-dried powder +2.5ml solvent) comprises the following steps: after cleaning the skin in the morning and evening and before moisturizing the skin, mixing and dissolving the freeze-dried powder and a solvent, and patting a proper amount of the mixture on the cleaned skin until the mixture is absorbed, wherein the Lanace skin repair freeze-dried powder provided by the comparative example 4 has poor appearance and poor rehydration, does not meet the quality standard of enterprise products, and finally does not participate in detection.

(1) Moisture content of stratum corneum

Table 2 shows the results of measurement of the moisture content of the stratum corneum (N. 33)

The higher the measurement value is, the higher the moisture content of the skin stratum corneum is, the more moist the skin is, and the test result in table 2 shows that the moisture content of the skin stratum corneum of the use area of the product of the subject is remarkably increased (79.94-89.47%) compared with the basic value in 28 days of using the product, so that the freeze-dried powder disclosed by the invention has a better moisturizing function.

(2) Skin percutaneous water loss

Table 3 shows the results of the skin moisture loss test

Lower measurements indicate less skin transepidermal water loss and better skin barrier function. The test results in table 3 show that the skin percutaneous water loss of the product using area of the subject is remarkably reduced (8.02-9.87%) compared with the basic value in 28 days of using the product, so that the freeze-dried powder disclosed by the invention has a better skin barrier repair function.

Third, evaluation of safety

The safety of the sample to the human skin is observed through a human trial test, when a subject visits, any adverse event which occurs in the period of using the sample by the subject is carefully inquired, checked and recorded, the adverse event comprises the expression, the occurrence time, the treatment measures and the return, and the relationship between the adverse event and the used sample is judged.

Skin reaction: no reaction, 0 is graded;

skin reaction: weak erythema, grade 1;

skin reaction: erythema, infiltration, papules, graded as 2;

skin reaction: erythema, edema, papules, blisters graded as 3;

skin reaction: erythema, edema, bulla, graded as 4.

After test feedback, the freeze-dried powder is continuously used for 28 days without any adverse reaction on skin, which shows that the freeze-dried powder has good safety and no stimulation.

The present invention has been further described with reference to specific embodiments, which are only exemplary and do not limit the scope of the present invention. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.

Claims

1. A lyophilized powder is characterized by comprising mannitol, sodium alginate, cell complex biological peptide, nicotinamide, fructus cnidii extract, glycyrrhiza glabra extract, lotus leaf extract and deionized water.

2. The freeze-dried powder according to claim 1, which comprises the following components in percentage by mass: 1-3% of mannitol, 3-6% of sodium alginate, 4-7% of cell composite biological peptide, 20-25% of nicotinamide, 0.3-0.5% of fructus cnidii extract, 2-5% of glycyrrhiza glabra extract, 0.1-0.3% of lotus leaf extract and the balance of deionized water.

3. The freeze-dried powder according to claim 2, which is characterized by comprising the following components in percentage by mass: 1.5-2.7% of mannitol, 0.8-1.0% of sodium alginate, 5-6% of cell composite biological peptide, 21-25% of nicotinamide, 0.35-0.45% of fructus cnidii extract, 2.5-4.5% of glycyrrhiza glabra extract, 0.12-0.28% of lotus leaf extract and the balance of deionized water.

4. The freeze-dried powder according to claim 3, which comprises the following components in percentage by mass: 2.4% of mannitol, 0.9% of sodium alginate, 5.5% of cell composite biological peptide, 24% of nicotinamide, 0.4% of fructus cnidii extract, 3% of glycyrrhiza glabra extract, 0.2% of lotus leaf extract and the balance of deionized water.

5. A method of preparing a lyophilized powder of any one of claims 1-4, comprising the steps of:

(2) and (2) freeze-drying the sterile filtrate obtained in the step (1), and crushing to obtain the polypeptide freeze-dried powder.

6. The method according to claim 5, wherein the conditions of the freeze-drying in step (2) are: and (4) carrying out freeze drying after quick freezing by using liquid nitrogen.

7. Use of a lyophilized powder according to any of claims 1-4 in the preparation of a cosmetic product.

8. The use of claim 7, wherein the cosmetic is at least one of a serum, a mask, a cream, and a gel.

9. The use of claim 8, wherein the vehicle of the lyophilized powder is: water or aqueous hyaluronic acid solution.

10. A cosmetic comprising the lyophilized powder of any one of claims 1-4 or the wet lyophilized powder prepared by the preparation method of any one of claims 5-6.