CN114159341B - Freeze-dried eye patch and preparation method thereof - Google Patents

Abstract

The invention discloses a freeze-dried eye patch and a preparation method thereof. The freeze-dried eye mask stock solution consists of, by weight, 100 parts of sodium hyaluronate 1-2 parts, pullulan polysaccharide 0.1-1 part, recombinant humanized collagen 0.01-1 part, acetyl tetrapeptide-5.01-0.1 part, microalgae prebiotics 0.1-1 part, horse chestnut extract 0.1-1 part, ginger root nano carbonic acid extract 1-5 parts and the balance of pure water. The frozen dry eye patch is prepared by freeze-drying the stock solution, and under the synergistic effect of the recombinant humanized collagen, the acetyl tetrapeptide-5 and the horse chestnut extract, the eye skin elasticity is enhanced, the eye skin problems such as dark circles, eye bags, canthus veins and the like are effectively solved, and other components in the frozen dry eye patch are matched, so that the frozen dry eye patch has a good moisturizing effect.

Description

Freeze-dried eye patch and preparation method thereof

Technical Field

The invention belongs to the technical field of cosmetics, and relates to a freeze-dried eye patch and a preparation method thereof.

Background

The crowds with dark circles, eye bags, fish tail lines and fat particles are gradually increased due to external factors such as ultraviolet irradiation, long-time computer radiation, age increase, working pressure, bad living habit and the like. People with the eye skin problems often present a mental appearance of unrefined harvest and fatigue, and are more aged. The skin care product is used for caring eye skin, and the eye skin state with compactness, fineness and elasticity can be achieved through the beautifying and repairing effects of the skin care product.

The freeze-dried skin care product is prepared by freezing sterile solution into solid state, and performing vacuum pumping to sublimate and dry water, and has the following advantages: (1) The influence on the quality of heat-sensitive products is avoided, the heat-sensitive products are dried at low temperature, and the stability of the materials in a dry state is ensured; (2) The protein is not denatured, and the microorganism is not lost in biological activity; (3) can best maintain the original properties of the substance; (4) The loss of volatile components and nutrient components and aromatic components denatured by heat in the substance is small; (5) The volume and the shape of the dried product are basically unchanged, the rehydration is good, 95 to 99.5 percent of water in the substance can be removed, and the storage life of the product is long; (6) The liquid process is easy to operate, the aseptic treatment is simplified, the freeze-drying process can lead the wet materials to be subjected to aseptic filtration to a final container after being prepared, and the pollution of particles and bacteria is reduced; (7) The porous and crisp structure is formed, and the stability of the product in a dry state is promoted.

Disclosure of Invention

The invention provides a frozen dry eye patch capable of effectively solving the problem of eye skin and a preparation method thereof.

The technical scheme of the invention is as follows:

the freeze-dried eye mask stock solution consists of the following components in parts by weight as 100 parts: 1-2 parts of sodium hyaluronate, 0.1-1 part of pullulan polysaccharide, 0.01-1 part of recombinant humanized collagen, 0.01-0.1 part of acetyl tetrapeptide-5, 0.1-1 part of microalgae prebiotics, 0.1-1 part of horse chestnut extract, 1-5 parts of ginger root nano carbonic acid extract and the balance of pure water, wherein the recombinant humanized collagen is produced by fermenting Pichia pastoris with the preservation number of CGMCC No. 5021.

Preferably, in the freeze-dried eye mask stock solution, 0.05-0.8 part of recombinant humanized collagen is used, and more preferably 0.1-0.5 part of recombinant humanized collagen is used.

In the specific embodiment of the invention, the freeze-dried eye mask stock solution consists of the following components in parts by weight as 100 parts: 1 part of sodium hyaluronate, 0.1 part of pullulan, 0.1 part of recombinant humanized collagen, 0.1 part of acetyl tetrapeptide-5, 0.1 part of microalgae prebiotics, 0.1 part of horse chestnut extract, 1 part of ginger root nano carbonic acid extract and the balance of pure water.

The recombinant humanized collagen adopted by the invention has stronger functions of resisting oxidization and scavenging free radicals, can obviously reduce pathological damage of aging skin, improve collagen fiber tissue distribution, increase the quantity of skin elastic fibers and improve the shape of elastic fibers.

The horse chestnut extract adopted by the invention has the effects of removing red blood streak, removing edema, removing pouch and black eye, and the like.

The ginger root nano carbonic acid extract adopted by the invention has the effects of promoting blood flow, improving dark circles and the like.

The acetyl tetrapeptide-5 adopted by the invention has the effects of removing pouch, black eye and the like.

The active ingredients in the freeze-dried eye patch provided by the invention are safe, mild and free of irritation.

The invention also provides a preparation method of the frozen dry eye patch, which comprises the following steps:

(1) According to the proportion of each component in the freeze-dried eye mask stock solution, sodium hyaluronate and pullulan are dissolved in pure water, heated to 60+/-2 ℃, homogenized, stirred until the mixture is clear and transparent, cooled to 40+/-2 ℃, added with recombinant humanized collagen, acetyl tetrapeptide-5, microalgae prebiotics, horse chestnut extract and ginger root nano carbonic acid extract, and stirred until the mixture is clear and transparent;

(2) Sterilizing and filtering the solution obtained in the step (1) by using a 0.22 mu m filter element;

(3) Filling the filtered solution into an eye patch mould for freeze drying to obtain the frozen dry eye patch, wherein the freeze drying conditions are as follows: freezing at-50 ℃ for 1-2 hours, then heating to-10 ℃, controlling the vacuum at 10-30 Pa, drying for 10-20 hours, then heating to 30 ℃ again, controlling the vacuum at 10-20 Pa, and drying for 4-8 hours.

Further, the invention provides the freeze-dried eye patch prepared by the preparation method.

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

(1) In the freeze-dried eye patch, three components of the recombinant humanized collagen, the acetyl tetrapeptide-5 and the horse chestnut extract can generate a synergistic effect, so that the skin elasticity is obviously improved, the eye skin problems such as dark circles, eye bags, eye wrinkles and the like are effectively solved, and meanwhile, the freeze-dried eye patch is matched with other components in the freeze-dried eye patch, has a good moisturizing effect, and can improve the skin moisture of eyes.

(2) Compared with the common eye patch, the eye patch provided by the invention has the advantages that the freeze-drying process greatly ensures the stability of active ingredients of the recombinant humanized collagen, the acetyl tetrapeptide-5 and the horse chestnut extract, is not beneficial to microbial growth under the anhydrous condition, and prolongs the shelf life of the eye patch.

Detailed Description

The technical scheme of the invention is clearly and completely described below. It will be apparent that the described embodiments are only some, not all, of the embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.

In the invention, all raw materials can be purchased from the market, wherein the recombinant humanized collagen is purchased from Jiangsu Jiangshan Zhuangyuan biotechnology Co., and the horse chestnut extract is purchased from Shanghai Jia Ye practical Co., ltd; the ginger root nano carbonic acid extract is purchased from Shanghai Hongjiu corporation.

Example 1

The freeze-dried eye mask stock solution consists of the following components in parts by weight as 100 parts:

1 part of sodium hyaluronate, 0.1 part of pullulan, 0.1 part of recombinant humanized collagen, 0.1 part of acetyl tetrapeptide-5, 0.1 part of microalgae prebiotic, 0.1 part of horse chestnut extract, 1 part of ginger root nano carbonic acid extract and the balance of pure water.

The frozen dry eye patch is prepared by the following steps:

(1) According to the formula proportion, sodium hyaluronate and pullulan are dissolved in pure water, heated to 60 ℃, homogenized, stirred, clarified and transparent, cooled to 40 ℃, added with recombinant humanized collagen, acetyl tetrapeptide-5, microalgae prebiotics, horse chestnut extract and ginger root nano carbonic acid extract, and stirred until the mixture is clarified and transparent.

(2) And (3) filling the solution obtained in the step (1) into a filter pressing bag, and sterilizing and filtering by using a 0.22 mu m filter element.

(3) Filling the solution filtered in the step (2) into a crescent mold, putting the mold filled with the solution into a freeze dryer, freezing for 1-2 hours at-50 ℃, then heating to-10 ℃, controlling the vacuum at 10-30 Pa, drying for 10-20 hours, then heating to 30 ℃ again, controlling the vacuum at 10-20 Pa, drying for 4-8 hours, and discharging.

Comparative example 1

The composition of the frozen dry eye patch stock solution and the preparation process were the same as in example 1, except that no recombinant humanized collagen, acetyl tetrapeptide-5, and horse chestnut extract were added in an amount of 0.3 parts.

Comparative example 2

The ingredients and preparation process of the frozen dry eye patch stock solution were the same as in example 1, except that acetyl tetrapeptide-5, horse chestnut extract was not added, and the addition amount of the recombinant humanized collagen was 0.3 part.

Comparative example 3

The composition and preparation process of the frozen dry eye patch stock solution were the same as in example 1, except that recombinant humanized collagen and horse chestnut extract were not added, and the addition amount of acetyl tetrapeptide-5 was 0.3 part.

Test examples

1. Subject enrollment criteria

(1) The ages are 30-60 years, the canthus has fine lines or wrinkles, bags and black eyes, and the degree level of the wrinkles of the subjects is set according to the wrinkle grading map according to the requirements of clinical test schemes.

(2) Exclusion criteria

Subjects have participated in additional clinical studies for nearly three months;

antihistamines used for the last week or immunosuppressants used for the last month;

anti-inflammatory drugs are used at the tested part in the last two months;

insulin dependent diabetes mellitus patients;

a patient suffering from a respiratory disease undergoing treatment;

women in lactation or striae gravidarum;

allergic constitution, allergic dermatitis, etc., and has skin diseases or disease history;

a population undergoing dermatological treatment, or a subject taking hydroxy acids, whitening, anti-aging drugs for one month;

the test area has large-area marks, scratches, white spots, pigmented nevi, keloids and other frontal skin characterizations affecting the test;

in addition, the test person in charge determines that the test person in charge is not suitable for the population as the test subject.

(3) Limiting matters

During the test, the treatment of the influence test on the tested part is forbidden, other skin care products and other products influencing the test are forbidden to be used in the test, and daily necessities such as bath foam, perfumed soap, shampoo and the like are consistent with those used before the test starts, so that replacement is forbidden.

2. The testing method comprises the following steps: 96 healthy subjects are selected, randomly divided into 4 groups, and 24 subjects in each group are respectively frozen dry eye patches prepared in example 1 and comparative examples 1-3, and the using method is as follows: the test subjects use the sample after face cleaning in the morning and evening, wet the place of the dark under-eye ring and the eye pouch with water, then put the freeze-dried eye patch under the eyes, take out the eye patch cloth and apply the patch immediately, press lightly until the freeze-dried eye patch is absorbed completely. Long-term sun exposure, outdoor exercises, travel, etc. cannot be performed during the entire test period, cosmetics or medicines having similar efficacy to the sample must not be used during the entire test period, and the subject must not change the daily care habits during the test period.

3. Test method and results

The following test results all used the average value of each test time point of each group of subjects.

(1) Canthus test

Recording data was taken from the corner of the eye using an Antera 3D, and wrinkles at this location were automatically analyzed, and the results are shown in Table 1.

TABLE 1 results of eye corner wrinkle volume detection

Table 2 results of measuring the protrusion volume of the pouch

As is apparent from tables 1 and 2, although the contents of the active ingredients in comparative examples 1 to 3 are the same as those in example 1, the addition of only the recombinant humanized collagen, acetyl tetrapeptide-5 or horse chestnut extract can improve the canthus wrinkles and the eye bags, but the effect thereof is poor, while example 1 containing the recombinant humanized collagen, acetyl tetrapeptide-5 and horse chestnut extract has significantly better improvement effect on the canthus wrinkles and the eye bags than comparative examples 1 to 3, indicating that the recombinant humanized collagen, acetyl tetrapeptide-5 and horse chestnut extract have a synergistic effect and can more effectively improve the canthus wrinkles and the eye bags.

(2) Moisture efficacy test

The test environment is temperature: 21.0 ℃ +/-1.0 ℃; humidity: 50% + -10% of the room, the test person was sitting still for 30min, the test area was tested for stratum corneum water content using MoistureMeterSC, and the test area was tested for water loss using VapoMeter, and the results are shown in Table 3.

TABLE 3 skin moisture content (%)

Test sample	Basic value	2h after using the product	4 hours after using the product	After the product is used for 8 hours
					Example 1	30.11	35.05	35.48	39.99
Comparative example 1	30.04	35.07	35.45	40.03
					Comparative example 2	30.07	35.01	35.252	39.97
Comparative example 3	29.95	34.86	35.61	39.82

TABLE 4 percutaneous skin moisture loss test results

As is clear from tables 3 and 4, the frozen dry eye patch of example 1 has a better moisturizing effect than comparative examples 1 to 3, can significantly increase the skin water content, and has a good moisturizing effect by keeping the skin water in a long-lasting state.

(3) Elasticity test:

the test subjects were tested for elasticity at the canthus using elastometers and the results are shown in table 5.

TABLE 5 skin elasticity test results

As is clear from table 5, the skin elasticity of the test site was significantly improved after 28 days using the lyophilized eye patch prepared in example 1, as compared with comparative examples 1 to 3. The content of the active ingredient in comparative examples 1 to 3 was the same as that in example 1, but the effect was poor, indicating that the recombinant humanized collagen, acetyl tetrapeptide-5, horse chestnut extract had a synergistic effect, and further improved skin elasticity.

(4) Volunteer self-assessment

The test person of example 1 was subjected to a questionnaire and the results showed that volunteer self-evaluation was 100% effective on dark circles.

The experiments show that the synergistic effect among the recombinant humanized collagen, the acetyl tetrapeptide-5 and the horse chestnut extract enhances the effect of the freeze-dried eye patch in removing the eye bags, the dark circles and the wrinkles. When the weight part of the added recombinant humanized collagen is 0.1 part, good synergistic effect can be generated between the added recombinant humanized collagen and the acetyl tetrapeptide-5 and the horse chestnut extract. The recombinant humanized collagen in the frozen dry eye patch adopts 0.1 part, so that the production cost is minimized, and compared with the traditional eye skin care product, the prepared frozen dry eye patch can well protect the activity of active ingredients, promote the quick penetration of the active ingredients into the skin to be absorbed, exert the biological activity and effectively solve the problem of eye aging such as dark circles, eye bags, wrinkles and the like.

Claims (6)

1. The freeze-dried eye mask stock solution is characterized by comprising the following components in parts by weight as 100 parts: 1-2 parts of sodium hyaluronate, 0.1-1 part of pullulan polysaccharide, 0.01-1 part of recombinant humanized collagen, 50.01-0.1 part of acetyl tetrapeptide-0.1 part of microalgae prebiotics, 0.1-1 part of horse chestnut extract, 1-5 parts of ginger root nano carbonic acid extract and the balance of pure water, wherein the recombinant humanized collagen is produced by fermenting Pichia pastoris with the preservation number of CGMCC No. 5021.

2. The stock solution for freeze-dried eye patch according to claim 1, wherein the recombinant humanized collagen is 0.05 to 0.8 parts.

3. The stock solution for freeze-dried eye patch according to claim 1, wherein the recombinant humanized collagen is 0.1 to 0.5 parts.

4. The stock solution for freeze-dried eye patches according to claim 1, which is characterized by comprising the following components in parts by weight of 100 parts: 1 part of sodium hyaluronate, 0.1 part of pullulan, 0.1 part of recombinant humanized collagen, 0.1 part of acetyl tetrapeptide-5, 0.1 part of microalgae prebiotics, 0.1 part of horse chestnut extract, 1 part of ginger root nano carbonic acid extract and the balance of pure water.

5. The preparation method of the frozen dry eye patch is characterized by comprising the following steps of:

(1) According to the proportion of each component in the freeze-dried eye mask stock solution of any one of claims 1 to 4, sodium hyaluronate and pullulan are dissolved in pure water, heated to 60+/-2 ℃, homogenized, stirred to be clear and transparent, cooled to 40+/-2 ℃, added with recombinant humanized collagen, acetyl tetrapeptide-5, microalgae prebiotics, horse chestnut extract and ginger root nano carbonic acid extract, and stirred to be clear and transparent;

(2) Sterilizing and filtering the solution obtained in the step (1) by using a 0.22 mu m filter element;

(3) Filling the filtered solution into an eye patch mould for freeze drying to obtain the frozen dry eye patch, wherein the freeze drying conditions are as follows: freezing at-50 ℃ for 1-2 hours, then heating to-10 ℃, controlling the vacuum at 10-30 Pa, drying for 10-20 hours, then heating to 30 ℃ again, controlling the vacuum at 10-20 Pa, and drying for 4-8 hours.

6. A lyophilized eye patch prepared according to the method of claim 5.