CN110840793A - Fibroin mask liquid and preparation method thereof - Google Patents

Abstract

The invention belongs to the technical field of cosmetics, and provides fibroin mask liquid and a preparation method thereof. The fibroin mask liquid comprises the following components in parts by weight: 30-50 parts of silk protein hydrolysate, 5-13 parts of pomegranate peel extract, 3-8 parts of herba violae extract, 1-5 parts of pyrrosia lingua extract, 1-5 parts of mahonia stem extract, 0.5-2 parts of olive oil, 0.5-1.5 parts of diisostearyl malate, 0.1-0.5 part of decyl olivate, 0.1-0.6 part of triethanolamine, 0.1-0.5 part of 1,2 hexanediol, 0.5-2 parts of butanediol and 25-40 parts of water. The preparation method of the fibroin hydrolysate comprises the following steps: boiling silk in sodium carbonate aqueous solution for degumming, and then pressurizing and hydrolyzing the degummed silk in sodium hydroxide solution to obtain silk protein hydrolysate. By adopting the technical scheme, the problem that the facial mask liquid containing fibroin in the prior art is easy to breed microorganisms and is decayed is solved.

Description

Fibroin mask liquid and preparation method thereof

Technical Field

The invention belongs to the technical field of cosmetics, and relates to fibroin mask liquid and a preparation method thereof.

Background

With the increasing living standard of people, cosmetics become indispensable living goods for people, and the requirements of people on cosmetics tend to be natural, low-carbon, environment-friendly, nutritional, low-irritation or non-irritation and the like. Based on this, research on the use of natural fibroin and its derivatives is also receiving increasing attention, particularly in cosmetics. The fibroin, also known as silk fibroin, is natural polymer fibrin extracted from silk, accounts for 70-80% of the silk, contains eighteen amino acids required by human bodies, provides nutrient components required by skin whitening, has small molecular weight, can permeate skin, promotes cell metabolism, repairs damaged skin, and can form a protective film on the surface of skin and hair, and the protective film has flexibility and elasticity, and can achieve the effect of protecting hair and skin when being used for shampoo and skin care products. The fibroin needs to be hydrolyzed to obtain fibroin hydrolysate for human body to absorb. However, the fibroin hydrolysate contains various amino acids which are extremely suitable for the growth of microorganisms, so that the existing facial mask liquid containing fibroin is easy to breed microorganisms and decay in storage, and the facial mask is unstable in storage.

Disclosure of Invention

The invention provides a fibroin mask solution and a preparation method thereof, and solves the problem that the fibroin-containing mask solution in the prior art is easy to breed microorganisms and is putrefactive.

The technical scheme of the invention is realized as follows:

the fibroin mask liquid comprises the following components in parts by weight:

30-50 parts of silk protein hydrolysate, 5-13 parts of pomegranate peel extract, 3-8 parts of herba violae extract, 1-5 parts of pyrrosia lingua extract, 1-5 parts of mahonia stem extract, 0.5-2 parts of olive oil, 0.5-1.5 parts of diisostearyl malate, 0.1-0.5 part of decyl olivate, 0.1-0.6 part of triethanolamine, 0.1-0.5 part of 1,2 hexanediol, 0.5-2 parts of butanediol and 25-40 parts of water.

As a further technical scheme, the paint comprises the following components in parts by weight:

40 parts of fibroin hydrolysate, 9 parts of pomegranate peel extract, 5 parts of herba violae extract, 2 parts of pyrrosia lingua extract, 3 parts of mahonia stem extract, 1.2 parts of green fruit oil, 1 part of diisostearyl malate, 0.3 part of decyl olivate, 0.3 part of triethanolamine, 0.2 part of 1,2 hexanediol, 1.2 parts of butanediol and 32 parts of water.

As a further technical scheme, the preparation method of the fibroin hydrolysate comprises the following steps: boiling silk in sodium carbonate aqueous solution for degumming, and then pressurizing and hydrolyzing the degummed silk in sodium hydroxide solution to obtain silk protein hydrolysate.

According to a further technical scheme, the mass concentration of the sodium carbonate aqueous solution is 0.5%, the mass concentration of the sodium hydroxide solution is 1.25-1.6%, the pressure hydrolysis temperature is 130 ℃, and the hydrolysis time is 2-3 hours.

As a further technical scheme, the preparation method of the sweet herba violae extract comprises the following steps: decocting herba Violae powder with water, filtering, heating the filtrate, concentrating, eluting with ethanol, concentrating, and drying to obtain herba Violae extract.

As a further technical scheme, the preparation method of the pyrrosia lingua extract comprises the following steps: heating folium Pyrrosiae powder with ethanol under reflux, filtering, rotary evaporating the filtrate to remove ethanol, decocting with water, filtering, eluting the filtrate with ethyl acetate, concentrating, and drying to obtain folium Pyrrosiae extract.

As a further technical scheme, the preparation method of the mahonia stem extract comprises the following steps: decocting caulis Mahoniae powder with water, filtering, heating the filtrate, concentrating, eluting with ethanol, concentrating, and drying to obtain caulis Mahoniae extract.

As a further technical scheme, the preparation method of the pomegranate bark extract comprises the following steps: heating and refluxing pericarpium Granati powder obtained by pulverizing pericarpium Granati with ethanol, filtering, rotary evaporating the filtrate to remove ethanol, eluting with petroleum ether, eluting with ethyl acetate, concentrating, and drying to obtain pericarpium Granati extract.

A preparation method of fibroin mask liquid comprises the following steps:

s1, weighing the components according to the formula of the fibroin mask liquid for later use;

s2, mixing the pomegranate bark extract, the Chinese violet extract, the pyrrosia lingua extract and the mahonia stem extract, adding the mixture into the fibroin hydrolysate, and uniformly mixing to obtain a first mixed solution;

s3, mixing 1, 2-hexanediol, butanediol and olive oil, heating to 86-88 ℃, and uniformly mixing to obtain a second mixed solution;

s4, adding the first mixed solution into water at 86-88 ℃, uniformly mixing, adding the second mixed solution, diisostearyl malate and decyl olivate, and uniformly stirring to obtain a primary mixed material;

s5, cooling the primary mixed material to 45 ℃, adding triethanolamine, and uniformly stirring to obtain the silk protein mask liquid.

The working principle and the beneficial effects of the invention are as follows:

1. according to the invention, the fibroin hydrolysate is used as a raw material, and components such as fibroin hydrolysate, pomegranate bark extract, herba violae extract, pyrrosia lingua extract, mahonia stem extract, olive oil, diisostearyl malate, decyl olivate, triethanolamine, 1,2 hexanediol and butanediol are added, and the components are compatible with one another and have a synergistic effect, so that the prepared fibroin mask liquid has a good moisturizing effect, fine wrinkles can be reduced, the skin tightness is improved, the skin is fresh and cool after use, the use effect is good, the use requirements of consumers are met, and meanwhile, the fibroin mask is safe and reliable, and the problem that the fibroin mask liquid in the prior art is easy to breed microorganisms and is corrupt is effectively solved.

2. According to the facial mask liquid, the fibroin hydrolysate has high polypeptide content and good moisturizing effect, meanwhile, the fibroin can promote metabolism of skin cells, repair damaged skin, fade fine wrinkles of the skin and improve skin compactness, and the pomegranate bark extract is compatible with the fibroin hydrolysate, so that the fine wrinkle fading effect of the facial mask liquid is further improved.

3. According to the invention, the pomegranate bark extract, the herba violae extract, the pyrrosia lingua extract and the mahonia stem extract are added into the fibroin mask solution, and are mutually compatible, so that the growth of microorganisms such as bacteria, mold, saccharomycetes and the like in the mask solution can be inhibited, the storage stability of the mask solution is improved, the prepared fibroin mask solution is safe and reliable, and the problem that the fibroin mask solution in the prior art is easy to breed microorganisms and is putrefactive is effectively solved. In addition, the pomegranate bark extract, the Chinese violet extract, the pyrrosia lingua extract and the leatherleaf mahonia extract are all plant extracts, have good affinity with skin, high safety and no toxic or side effect, and avoid potential safety hazards caused by using preservatives.

4. According to the invention, the olive oil is added into the fibroin facial mask liquid, so that moisture in the facial mask liquid is easily absorbed by skin, the moisture content of the skin is improved, meanwhile, the olive oil can lock moisture in the skin and slow down the loss of the moisture, the skin is kept in a moist state, and the moisturizing effect of the facial mask liquid is improved.

5. In the invention, isostearyl malate and decyl olivate are added into the fibroin mask liquid, so that on one hand, the pomegranate peel extract, the Chinese violet extract, the pyrrosia lingua extract, the mahonia stem extract and the fibroin hydrolysate are dispersed in water more uniformly, and the stability of the mask liquid is improved; on the other hand, the mask liquid has good adhesiveness to the skin, so that moisture and nutritional ingredients in the mask liquid are absorbed by the skin better and more quickly, and the moisturizing effect of the mask liquid is improved.

6. According to the invention, the fibroin hydrolysate is obtained by adopting a pressurized hydrolysis mode, so that the fibroin hydrolysis is more thorough, the polypeptide content in the fibroin hydrolysate is high, and meanwhile, the mass concentration of a sodium hydroxide solution used for pressurized hydrolysis is 1.25-1.6%.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

The fibroin mask liquid comprises the following components in parts by weight:

30 parts of silk protein hydrolysate, 5 parts of pomegranate peel extract, 3 parts of Chinese violet extract, 1 part of pyrrosia lingua extract, 1 part of mahonia stem extract, 0.5 part of green fruit oil, 0.5 part of diisostearyl malate, 0.1 part of decyl olivate, 0.1 part of triethanolamine, 0.1 part of 1, 2-hexanediol, 0.5 part of butanediol and 25 parts of water;

the preparation method comprises the following steps:

s1, heating and boiling a sodium carbonate aqueous solution with the mass concentration of 0.5%, adding silk when the temperature rises to 90 ℃, boiling for 30min, taking out the silk after boiling, adding the silk into another boiled sodium carbonate aqueous solution with the mass concentration of 0.5%, boiling for 30min, taking out the silk after boiling, washing with deionized water for 3 times, drying at 60 ℃ to obtain degummed silk, adding the degummed silk and a sodium hydroxide solution with the mass concentration of 1.42% into a reaction kettle, pressurizing and heating to 130 ℃, carrying out hydrolysis reaction for 3h, cooling and depressurizing, opening the kettle, extracting hydrolysate by using a suction filtration device, adding concentrated hydrochloric acid to adjust the pH to be neutral, and obtaining a silk protein hydrolysate; then weighing the components according to the formula for later use;

s2, mixing the pomegranate bark extract, the Chinese violet extract, the pyrrosia lingua extract and the mahonia stem extract, adding the mixture into the fibroin hydrolysate, and uniformly mixing to obtain a first mixed solution;

s3, mixing 1, 2-hexanediol, butanediol and olive oil, heating to 86-88 ℃, and uniformly mixing to obtain a second mixed solution;

s4, adding the first mixed solution into water at 86-88 ℃, uniformly mixing, adding the second mixed solution, diisostearyl malate and decyl olivate, and uniformly stirring to obtain a primary mixed material;

s5, cooling the primary mixed material to 45 ℃, adding triethanolamine, and uniformly stirring to obtain the silk protein mask liquid.

Example 2

The fibroin mask liquid comprises the following components in parts by weight:

50 parts of fibroin hydrolysate, 13 parts of pomegranate peel extract, 8 parts of Chinese violet extract, 5 parts of pyrrosia lingua extract, 5 parts of Chinese mahonia extract, 2 parts of green fruit oil, 1.5 parts of diisostearyl malate, 0.5 part of decyl olivate, 0.6 part of triethanolamine, 0.5 part of 1, 2-hexanediol, 2 parts of butanediol and 40 parts of water;

the preparation method is the same as that of example 1.

Example 3

The fibroin mask liquid comprises the following components in parts by weight:

35 parts of silk protein hydrolysate, 8 parts of pomegranate peel extract, 4 parts of Chinese violet extract, 5 parts of pyrrosia lingua extract, 5 parts of Chinese mahonia extract, 1 part of green fruit oil, 0.9 part of diisostearyl malate, 0.2 part of decyl olivate, 0.2 part of triethanolamine, 0.2 part of 1,2 hexanediol, 1 part of butanediol and 30 parts of water;

the preparation method is the same as that of example 1.

Example 4

The fibroin mask liquid comprises the following components in parts by weight:

45 parts of silk protein hydrolysate, 10 parts of pomegranate peel extract, 6 parts of Chinese violet extract, 4 parts of pyrrosia lingua extract, 4 parts of Chinese mahonia extract, 1.5 parts of green fruit oil, 1.2 parts of diisostearyl malate, 0.4 part of decyl olivate, 0.4 part of triethanolamine, 0.4 part of 1,2 hexanediol, 1.5 parts of butanediol and 35 parts of water;

the preparation method is the same as that of example 1.

Example 5

The fibroin mask liquid comprises the following components in parts by weight:

40 parts of fibroin hydrolysate, 9 parts of pomegranate peel extract, 5 parts of Chinese violet extract, 2 parts of pyrrosia lingua extract, 3 parts of Chinese mahonia extract, 1.2 parts of green fruit oil, 1 part of diisostearyl malate, 0.3 part of decyl olivate, 0.3 part of triethanolamine, 0.2 part of 1,2 hexanediol, 1.2 parts of butanediol and 32 parts of water;

the preparation method is the same as that of example 1.

Example 6

The fibroin mask liquid comprises the following components in parts by weight:

40 parts of fibroin hydrolysate, 9 parts of pomegranate peel extract, 5 parts of Chinese violet extract, 2 parts of pyrrosia lingua extract, 3 parts of Chinese mahonia extract, 1.2 parts of green fruit oil, 1 part of diisostearyl malate, 0.3 part of decyl olivate, 0.3 part of triethanolamine, 0.2 part of 1,2 hexanediol, 1.2 parts of butanediol and 32 parts of water;

the preparation method comprises the following steps:

s1, heating and boiling a sodium carbonate aqueous solution with the mass concentration of 0.5%, adding silk when the temperature rises to 90 ℃, boiling for 30min, taking out the silk after boiling, adding the silk into another boiled sodium carbonate aqueous solution with the mass concentration of 0.5%, boiling for 30min, taking out the silk after boiling, washing with deionized water for 3 times, drying at 50 ℃ to obtain degummed silk, adding the degummed silk and a sodium hydroxide solution with the mass concentration of 1.25% into a reaction kettle, pressurizing and heating to 130 ℃, carrying out hydrolysis reaction for 2h, cooling and depressurizing, opening the kettle, extracting hydrolysate by using a suction filtration device, adding concentrated hydrochloric acid to adjust the pH to be neutral, and obtaining a silk protein hydrolysate; then weighing the components according to the formula for later use;

s2, mixing the pomegranate bark extract, the Chinese violet extract, the pyrrosia lingua extract and the mahonia stem extract, adding the mixture into the fibroin hydrolysate, and uniformly mixing to obtain a first mixed solution;

s3, mixing 1, 2-hexanediol, butanediol and olive oil, heating to 86-88 ℃, and uniformly mixing to obtain a second mixed solution;

s4, adding the first mixed solution into water at 86-88 ℃, uniformly mixing, adding the second mixed solution, diisostearyl malate and decyl olivate, and uniformly stirring to obtain a primary mixed material;

s5, cooling the primary mixed material to 45 ℃, adding triethanolamine, and uniformly stirring to obtain the silk protein mask liquid.

Example 7

The fibroin mask liquid comprises the following components in parts by weight:

40 parts of fibroin hydrolysate, 9 parts of pomegranate peel extract, 5 parts of Chinese violet extract, 2 parts of pyrrosia lingua extract, 3 parts of Chinese mahonia extract, 1.2 parts of green fruit oil, 1 part of diisostearyl malate, 0.3 part of decyl olivate, 0.3 part of triethanolamine, 0.2 part of 1,2 hexanediol, 1.2 parts of butanediol and 32 parts of water;

the preparation method comprises the following steps:

s1, heating and boiling a sodium carbonate aqueous solution with the mass concentration of 0.5%, adding silk when the temperature rises to 90 ℃, boiling for 30min, taking out the silk after boiling, adding the silk into another boiled sodium carbonate aqueous solution with the mass concentration of 0.5%, boiling for 30min, taking out the silk after boiling, washing with deionized water for 2 times, drying at 60 ℃ to obtain degummed silk, adding the degummed silk and a sodium hydroxide solution with the mass concentration of 1.6% into a reaction kettle, pressurizing and heating to 130 ℃, carrying out hydrolysis reaction for 3h, cooling and depressurizing, opening the kettle, extracting hydrolysate by using a suction filtration device, adding concentrated hydrochloric acid to adjust the pH to be neutral, and obtaining a silk protein hydrolysate; then weighing the components according to the formula for later use;

s2, mixing the pomegranate bark extract, the Chinese violet extract, the pyrrosia lingua extract and the mahonia stem extract, adding the mixture into the fibroin hydrolysate, and uniformly mixing to obtain a first mixed solution;

s3, mixing 1, 2-hexanediol, butanediol and olive oil, heating to 86-88 ℃, and uniformly mixing to obtain a second mixed solution;

s4, adding the first mixed solution into water at 86-88 ℃, uniformly mixing, adding the second mixed solution, diisostearyl malate and decyl olivate, and uniformly stirring to obtain a primary mixed material;

s5, cooling the primary mixed material to 45 ℃, adding triethanolamine, and uniformly stirring to obtain the silk protein mask liquid.

Comparative example 1

The fibroin mask liquid comprises the following components in parts by weight:

40 parts of fibroin hydrolysate, 9 parts of pomegranate peel extract, 5 parts of Chinese violet extract, 2 parts of pyrrosia lingua extract, 3 parts of Chinese mahonia extract, 1.2 parts of green fruit oil, 1 part of diisostearyl malate, 0.3 part of decyl olivate, 0.3 part of triethanolamine, 0.2 part of 1,2 hexanediol, 1.2 parts of butanediol and 32 parts of water;

the preparation method comprises the following steps of S1: heating and boiling a sodium carbonate aqueous solution with the mass concentration of 0.5%, adding silk when the temperature rises to 90 ℃, boiling for 30min, taking out the silk after boiling, adding the silk into another boiled sodium carbonate aqueous solution with the mass concentration of 0.5%, boiling for 30min, taking out the silk after boiling, washing with deionized water for 2 times, drying at 60 ℃ to obtain degummed silk, adding the degummed silk and a sodium hydroxide solution with the mass concentration of 1.6% into a reaction kettle, heating to 100 ℃ for hydrolysis reaction for 3h, cooling, opening the kettle, extracting a hydrolysate by using a suction filtration device, adding concentrated hydrochloric acid to adjust the pH to be neutral, and obtaining a fibroin hydrolysate; then weighing the components according to the formula for later use; the rest of the procedure was the same as in example 1.

Comparative example 2

The fibroin mask liquid comprises the following components in parts by weight:

40 parts of fibroin hydrolysate, 9 parts of pomegranate peel extract, 5 parts of Chinese violet extract, 2 parts of pyrrosia lingua extract, 3 parts of Chinese mahonia extract, 1.2 parts of green fruit oil, 1 part of diisostearyl malate, 0.3 part of decyl olivate, 0.3 part of triethanolamine, 0.2 part of 1,2 hexanediol, 1.2 parts of butanediol and 32 parts of water;

the preparation method comprises the following steps of S1: heating and boiling a sodium carbonate aqueous solution with the mass concentration of 0.5%, adding silk when the temperature rises to 90 ℃, boiling for 30min, taking out the silk after boiling, adding the silk into another boiled sodium carbonate aqueous solution with the mass concentration of 0.5%, boiling for 30min, taking out the silk after boiling, washing with deionized water for 2 times, drying at 60 ℃ to obtain degummed silk, adding the degummed silk and a sodium hydroxide solution with the mass concentration of 1.6% into a reaction kettle, heating to 100 ℃, carrying out hydrolysis reaction for 5h, cooling, opening the kettle, extracting a hydrolysate by using a suction filtration device, adding concentrated hydrochloric acid to adjust the pH value to be neutral, and obtaining a fibroin hydrolysate; then weighing the components according to the formula for later use; the rest of the procedure was the same as in example 1.

Comparative example 3

The fibroin mask liquid comprises the following components in parts by weight:

40 parts of fibroin hydrolysate, 9 parts of pomegranate peel extract, 5 parts of Chinese violet extract, 2 parts of pyrrosia lingua extract, 3 parts of Chinese mahonia extract, 1.2 parts of green fruit oil, 1 part of diisostearyl malate, 0.3 part of decyl olivate, 0.3 part of triethanolamine, 0.2 part of 1,2 hexanediol, 1.2 parts of butanediol and 32 parts of water;

the preparation method comprises the following steps of S1: heating and boiling a sodium carbonate aqueous solution with the mass concentration of 0.5%, adding silk when the temperature rises to 90 ℃, boiling for 30min, taking out the silk after boiling, adding the silk into another boiled sodium carbonate aqueous solution with the mass concentration of 0.5%, boiling for 30min, taking out the silk after boiling, washing with deionized water for 2 times, drying at 60 ℃ to obtain degummed silk, adding the degummed silk and a sodium hydroxide solution with the mass concentration of 1.6% into a reaction kettle, pressurizing and heating to 110 ℃ for hydrolysis reaction for 3h, cooling and depressurizing, opening the kettle, extracting a hydrolysate by using a suction filtration device, adding concentrated hydrochloric acid to adjust the pH to be neutral, and obtaining a fibroin hydrolysate; then weighing the components according to the formula for later use; the rest of the procedure was the same as in example 1.

Comparative example 4

The fibroin mask liquid comprises the following components in parts by weight:

40 parts of fibroin hydrolysate, 9 parts of pomegranate peel extract, 5 parts of Chinese violet extract, 2 parts of pyrrosia lingua extract, 3 parts of Chinese mahonia extract, 1.2 parts of green fruit oil, 1 part of diisostearyl malate, 0.3 part of decyl olivate, 0.3 part of triethanolamine, 0.2 part of 1,2 hexanediol, 1.2 parts of butanediol and 32 parts of water;

the preparation method comprises the following steps of S1: heating and boiling a sodium carbonate aqueous solution with the mass concentration of 0.5%, adding silk when the temperature rises to 90 ℃, boiling for 30min, taking out the silk after boiling, adding the silk into another boiled sodium carbonate aqueous solution with the mass concentration of 0.5%, boiling for 30min, taking out the silk after boiling, washing with deionized water for 2 times, drying at 60 ℃ to obtain degummed silk, adding the degummed silk and a sodium hydroxide solution with the mass concentration of 1.6% into a reaction kettle, pressurizing and heating to 120 ℃ for hydrolysis reaction for 3h, cooling and depressurizing, opening the kettle, extracting a hydrolysate by using a suction filtration device, adding concentrated hydrochloric acid to adjust the pH to be neutral, and obtaining a fibroin hydrolysate; then weighing the components according to the formula for later use; the rest of the procedure was the same as in example 1.

Comparative example 5

The fibroin mask liquid comprises the following components in parts by weight:

40 parts of fibroin hydrolysate, 9 parts of pomegranate peel extract, 5 parts of Chinese violet extract, 2 parts of pyrrosia lingua extract, 3 parts of Chinese mahonia extract, 1.2 parts of green fruit oil, 1 part of diisostearyl malate, 0.3 part of decyl olivate, 0.3 part of triethanolamine, 0.2 part of 1,2 hexanediol, 1.2 parts of butanediol and 32 parts of water;

the preparation method comprises the following steps of S1: heating and boiling a sodium carbonate aqueous solution with the mass concentration of 0.5%, adding silk when the temperature rises to 90 ℃, boiling for 30min, taking out the silk after boiling, adding the silk into another boiled sodium carbonate aqueous solution with the mass concentration of 0.5%, boiling for 30min, taking out the silk after boiling, washing with deionized water for 2 times, drying at 60 ℃ to obtain degummed silk, adding the degummed silk and a sodium hydroxide solution with the mass concentration of 1.6% into a reaction kettle, pressurizing and heating to 130 ℃ for hydrolysis reaction for 4h, cooling and depressurizing, opening the kettle, extracting a hydrolysate by using a suction filtration device, adding concentrated hydrochloric acid to adjust the pH to be neutral, and obtaining a fibroin hydrolysate; then weighing the components according to the formula for later use; the rest of the procedure was the same as in example 1.

Comparative example 6

The fibroin mask liquid comprises the following components in parts by weight:

40 parts of fibroin hydrolysate, 9 parts of pomegranate peel extract, 5 parts of Chinese violet extract, 2 parts of pyrrosia lingua extract, 3 parts of Chinese mahonia extract, 1.2 parts of green fruit oil, 1 part of diisostearyl malate, 0.3 part of decyl olivate, 0.3 part of triethanolamine, 0.2 part of 1,2 hexanediol, 1.2 parts of butanediol and 32 parts of water;

the preparation method comprises the following steps of S1: heating and boiling a sodium carbonate aqueous solution with the mass concentration of 0.5%, adding silk when the temperature rises to 90 ℃, boiling for 30min, taking out the silk after boiling, adding the silk into another boiled sodium carbonate aqueous solution with the mass concentration of 0.5%, boiling for 30min, taking out the silk after boiling, washing with deionized water for 2 times, drying at 60 ℃ to obtain degummed silk, adding the degummed silk and a sodium hydroxide solution with the mass concentration of 0.8% into a reaction kettle, pressurizing and heating to 130 ℃ for hydrolysis reaction for 4h, cooling and depressurizing, opening the kettle, extracting a hydrolysate by using a suction filtration device, adding concentrated hydrochloric acid to adjust the pH to be neutral, and obtaining a fibroin hydrolysate; then weighing the components according to the formula for later use; the rest of the procedure was the same as in example 1.

The conditions of the fibroin hydrolysates of examples 1-7 and comparative examples 1-6 are shown in the following table:

TABLE 1 conditions of fibroin hydrolysates of examples 1 to 7 and comparative examples 1 to 6

The hydrolysis conditions of examples 2 to 5 were the same as those of example 1, and the conditions of the obtained fibroin hydrolysate were the same as those of example 1, and thus, they were omitted.

As can be seen from the data in Table 1, the hydrolysis time is saved under the condition of pressurized hydrolysis, the fibroin is completely hydrolyzed under the hydrolysis condition that the reaction is carried out for 2-3 hours at 130 ℃ and the mass concentration of the sodium hydroxide solution is 1.25% -1.6%, and the hydrolysate is golden yellow and clear.

Comparative example 7

The fibroin mask liquid comprises the following components in parts by weight:

40 parts of fibroin hydrolysate, 5 parts of herba violae extract, 2 parts of pyrrosia lingua extract, 3 parts of mahonia stem extract, 1.2 parts of green fruit oil, 1 part of diisostearyl malate, 0.3 part of decyl olivate, 0.3 part of triethanolamine, 0.2 part of 1,2 hexanediol, 1.2 parts of butanediol and 32 parts of water;

the preparation method is the same as that of example 1 except that the pomegranate rind extract is not added in step S2.

Comparative example 8

The fibroin mask liquid comprises the following components in parts by weight:

40 parts of fibroin hydrolysate, 9 parts of pomegranate peel extract, 2 parts of pyrrosia lingua extract, 3 parts of mahonia stem extract, 1.2 parts of olive oil, 1 part of diisostearyl malate, 0.3 part of decyl olivate, 0.3 part of triethanolamine, 0.2 part of 1,2 hexanediol, 1.2 parts of butanediol and 32 parts of water;

the preparation method is the same as example 1 except that the extract of herba corydalis Bungeanae is not added in step S2.

Comparative example 9

The fibroin mask liquid comprises the following components in parts by weight:

40 parts of fibroin hydrolysate, 9 parts of pomegranate peel extract, 5 parts of Chinese violet extract, 3 parts of Chinese mahonia extract, 1.2 parts of green fruit oil, 1 part of diisostearyl malate, 0.3 part of decyl olivate, 0.3 part of triethanolamine, 0.2 part of 1,2 hexanediol, 1.2 parts of butanediol and 32 parts of water;

the preparation method is the same as example 1 except that the pyrrosia lingua extract is not added in step S2.

Comparative example 10

The fibroin mask liquid comprises the following components in parts by weight:

40 parts of fibroin hydrolysate, 9 parts of pomegranate peel extract, 5 parts of herba violae extract, 2 parts of pyrrosia lingua extract, 1.2 parts of olive oil, 1 part of diisostearyl malate, 0.3 part of decyl olivate, 0.3 part of triethanolamine, 0.2 part of 1,2 hexanediol, 1.2 parts of butanediol and 32 parts of water;

the preparation method is the same as example 1 except that the mahonia stem extract is not added in step S2.

Comparative example 11

The fibroin mask liquid comprises the following components in parts by weight:

40 parts of fibroin hydrolysate, 9 parts of pomegranate peel extract, 5 parts of herba violae extract, 2 parts of pyrrosia lingua extract, 3 parts of mahonia stem extract, 1 part of diisostearyl malate, 0.3 part of decyl olivate, 0.3 part of triethanolamine, 0.2 part of 1,2 hexanediol, 1.2 parts of butanediol and 32 parts of water;

the preparation method is the same as example 1 except that the olive oil is not added in step S3.

Comparative example 12

The fibroin mask liquid comprises the following components in parts by weight:

40 parts of fibroin hydrolysate, 9 parts of pomegranate peel extract, 5 parts of herba violae extract, 2 parts of pyrrosia lingua extract, 3 parts of mahonia stem extract, 1.2 parts of green fruit oil, 0.3 part of triethanolamine, 0.2 part of 1,2 hexanediol, 1.2 parts of butanediol and 32 parts of water;

the preparation method is the same as that of example 1 except that diisostearyl malate and decyl olivate are not added in step S4.

In examples 1 to 7 and comparative examples 1 to 12,

the preparation method of the herba corydalis Bungeanae extract comprises the following steps: decocting herba Violae powder with water, filtering, heating the filtrate, concentrating, eluting with ethanol, concentrating, and drying to obtain herba Violae extract;

the preparation method of the pyrrosia lingua extract comprises the following steps: heating folium Pyrrosiae powder with ethanol under reflux, filtering, rotary evaporating the filtrate to remove ethanol, decocting with water, filtering, eluting the filtrate with ethyl acetate, concentrating, and drying to obtain folium Pyrrosiae extract;

the preparation method of the mahonia stem extract comprises the following steps: decocting caulis Mahoniae powder with water, filtering, heating the filtrate, concentrating, eluting with ethanol, concentrating, and drying to obtain caulis Mahoniae extract;

the preparation method of the pomegranate bark extract comprises the following steps: heating and refluxing pericarpium Granati powder obtained by pulverizing pericarpium Granati with ethanol, filtering, rotary evaporating the filtrate to remove ethanol, eluting with petroleum ether, eluting with ethyl acetate, concentrating, and drying to obtain pericarpium Granati extract.

The following performance tests were performed on the facial mask solutions prepared in examples 1 to 7 and comparative examples 7 to 12:

1. and (3) microbial detection: the total number of bacteria, total number of molds/yeasts, heat-resistant coliform group, staphylococcus aureus, pseudomonas aeruginosa and the like in the samples and the samples stored for 30 days were detected according to the method specified in technical specification for cosmetic safety (2015 edition), and the detection results are shown in the following table:

TABLE 2 microbiological examination results of the facial mask solutions prepared in examples 1 to 7 and comparative examples 7 to 12

Note: in the above table, - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -.

TABLE 3 microbiological examination results of the facial mask solutions prepared in examples 1 to 7 and comparative examples 7 to 12 after 30 days of storage

As can be seen from the data in table 3, the total number of bacteria in the facial mask solutions of examples 1 to 7 and comparative examples 7 to 12 is less than 10/mL, the total number of mold/yeast is less than 10/mL, and heat-resistant coliform groups, staphylococcus aureus and pseudomonas aeruginosa are not detected, and meanwhile, the total number of bacteria, mold/yeast, heat-resistant coliform groups, staphylococcus aureus and pseudomonas aeruginosa in the facial mask solutions of examples 1 to 7 are not changed after being stored for 30 days, and the results of microbial examination show that the facial mask solutions meet the requirements of technical specifications for cosmetic safety (2015 edition), which indicates that the facial mask solutions prepared by the method are safe and reliable, and effectively solve the problem that the facial mask solutions containing fibroin in the prior art are prone to microbial growth and spoilage.

Compared with the facial mask liquids of examples 1 to 7, the total number of bacteria and the total number of mold/yeast of the facial mask liquids of comparative examples 7 to 10 are increased in the sample after being stored for 30 days, which indicates that the facial mask liquids of comparative examples 7 to 10 are easy to breed microorganisms in the storage process and are unstable in storage. The formula of the facial mask liquid of the comparative example 7 is not added with a pomegranate bark extract, the formula of the facial mask liquid of the comparative example 8 is not added with a herba violae extract, the formula of the facial mask liquid of the comparative example 9 is not added with a pyrrosia lingua extract, the formula of the facial mask liquid of the comparative example 10 is not added with a mahonia extract, and the compatibility of the pomegranate bark extract, the herba violae extract, the pyrrosia lingua extract and the mahonia extract is proved, so that the growth of microorganisms such as bacteria, mold, saccharomycetes and the like in the facial mask liquid can be inhibited, the storage stability of the facial mask liquid is improved, and the prepared silk protein facial mask liquid is safe.

2. Moisture retention: the moisture content of the skin stratum corneum is measured according to a capacitance method specified in QB/T4256-2011 'guidelines for evaluating moisturizing effects of cosmetics'. During testing, 30 female volunteers are selected, the average age is 30 years old, the positions of the subjects are the inner sides of the forearms of the two hands of the subjects, a use area and a blank control area are divided before use, the fibroin masks prepared in examples 1-7 and comparative examples 7-12 are respectively used in the use area, the blank control group is not treated, the moisture content of the stratum corneum of the skin is respectively tested on the use area and the blank control area by using a skin moisture tester before use and after 4 hours of use, and the test results are shown in table 4:

TABLE 4 results of moisture retention test of facial mask solutions of examples 1 to 7 and comparative examples 7 to 12

As can be seen from Table 4, after the fibroin facial mask solutions of examples 1-7 are used for 4 hours, the moisture value of the stratum corneum of the skin is remarkably improved, and the moisture increase value is as high as 13.7%, which shows that the fibroin facial mask solutions of examples 1-7 have good moisturizing and moisturizing effects and meet the use requirements of consumers.

Compared with the facial mask solutions of examples 1-7, the moisture value of the stratum corneum of the skin after 4 hours of using the facial mask solution of comparative example 11 is less increased, because the olive oil is not added in the raw material of the facial mask solution of comparative example 11, and diisostearyl malate and decyl oleate are not added in the raw material of the facial mask solution of comparative example 12, which indicates that the water replenishing and moisturizing effects of the facial mask solution are remarkably improved due to the addition of the olive oil, the diisostearyl malate and the decyl oleate. The olive oil is added into the facial mask liquid, so that moisture in the facial mask liquid is easily absorbed by skin, the moisture content of the skin is improved, meanwhile, the olive oil can lock moisture in the skin and slow down the loss of the moisture, the skin is kept in a moist state, and the moisturizing effect of the facial mask liquid is improved. The addition of the isostearyl malate and the decyl olivate can ensure that the pomegranate rind extract, the herba violae extract, the pyrrosia lingua extract, the mahonia stem extract and the fibroin hydrolysate are dispersed in water more uniformly, thereby improving the stability of the facial mask liquid; on the other hand, the mask liquid has good adhesiveness to the skin, so that moisture and nutritional ingredients in the mask liquid are absorbed by the skin better and more quickly, and the moisturizing effect of the mask liquid is improved.

3. And (3) testing the use effect:

the test population of 260 people, the age of 25-40 years old, is divided into 13 groups, each group of 20 people, the skin condition of the test population meets the inclusion standard of the test subjects, 1-7 groups of test subjects respectively use the facial mask liquid prepared in examples 1-7, and 8-13 groups of test subjects respectively use the facial mask liquid prepared in comparative examples 7-12. The using method comprises the following steps: applying the facial mask liquid once every two days at night, and after continuously using for one month, scoring the facial mask liquid used by a subject according to the skin condition of the subject. The scoring interval is 0-10 points, and then the results and the summarized data are collected, as shown in table 5:

TABLE 5 effects of use of facial mask solutions of examples 1 to 7 and comparative examples 7 to 12

Group of	Degree of freshness	Moisture retention	Sense of tightness	Thin lines of desalination
					Example 1	9.19	9.56	9.32	9.03
Example 2	9.27	9.43	9.52	9.17
					Example 3	9.22	9.52	9.34	9.06
Example 4	9.35	9.59	9.27	9.23
					Example 5	9.21	9.63	9.42	9.15
Example 6	9.36	9.57	9.55	9.21
					Example 7	9.38	9.66	9.53	9.26
Comparative example 7	8.31	9.16	9.07	8.23
					Comparative example 8	8.26	9.32	9.14	8.67
Comparative example 9	8.08	9.24	9.09	8.42
					Comparative example 10	8.35	9.07	9.16	8.51
Comparative example 11	8.16	7.25	7.43	8.17
					Comparative example 12	6.59	7.82	6.75	8.56

As can be seen from the data in Table 5, compared with the facial mask solutions of comparative examples 7 to 12, the facial mask solutions of the examples 1 to 7 of the present invention were used by the subjects for 30 days, and the effects of the facial mask solutions were scored as high, and the freshness, moisture retention, firmness and fine grain reduction were scored as above 9, indicating that the facial mask solutions of the examples 1 to 7 of the present invention have not only good moisturizing and moisturizing effects, but also fine grain reduction and skin firmness enhancement, and the skin freshness after use is high, and the facial mask solutions are well-scored by the subjects, and the use effects are good, and the use requirements of consumers are satisfied.

Compared with the facial mask solutions of examples 1 to 7, the facial mask solutions of comparative examples 7 to 12 are relatively poor in freshness, the facial mask solution of comparative example 12 is the worst in freshness, the comparative examples 11 to 12 are poor in moisture retention and poor in skin tightening feeling after use, and the facial mask solutions of comparative example 7 and comparative example 11 are poor in fine line fading effect, so that the prepared facial mask solution has good effects of moisturizing, desalting fine lines, improving skin tightening feeling and being high in freshness only through mutual compatibility and synergistic effect of the components in the formula of the facial mask solution, and the effects cannot be achieved due to the fact that any one of the components is lacked.

The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. The fibroin mask liquid is characterized by comprising the following components in parts by weight:

30-50 parts of silk protein hydrolysate, 5-13 parts of pomegranate peel extract, 3-8 parts of herba violae extract, 1-5 parts of pyrrosia lingua extract, 1-5 parts of mahonia stem extract, 0.5-2 parts of olive oil, 0.5-1.5 parts of diisostearyl malate, 0.1-0.5 part of decyl olivate, 0.1-0.6 part of triethanolamine, 0.1-0.5 part of 1,2 hexanediol, 0.5-2 parts of butanediol and 25-40 parts of water.

2. The fibroin mask solution according to claim 1, which comprises the following components in parts by weight:

40 parts of fibroin hydrolysate, 9 parts of pomegranate peel extract, 5 parts of herba violae extract, 2 parts of pyrrosia lingua extract, 3 parts of mahonia stem extract, 1.2 parts of green fruit oil, 1 part of diisostearyl malate, 0.3 part of decyl olivate, 0.3 part of triethanolamine, 0.2 part of 1,2 hexanediol, 1.2 parts of butanediol and 32 parts of water.

3. The fibroin mask solution according to claim 1 or 2, wherein the fibroin hydrolysate is prepared by the following steps: boiling silk in sodium carbonate aqueous solution for degumming, and then pressurizing and hydrolyzing the degummed silk in sodium hydroxide solution to obtain silk protein hydrolysate.

4. The fibroin mask solution according to claim 3, wherein the mass concentration of the sodium carbonate aqueous solution is 0.5%, the mass concentration of the sodium hydroxide solution is 1.25-1.6%, the pressure hydrolysis temperature is 130 ℃, and the hydrolysis time is 2-3 h.

5. The fibroin mask solution according to claim 3, wherein the preparation method of the extract of herba corydalis Bungeanae comprises the following steps: decocting herba Violae powder with water, filtering, heating the filtrate, concentrating, eluting with ethanol, concentrating, and drying to obtain herba Violae extract.

6. The fibroin mask solution according to claim 3, wherein the preparation method of the pyrrosia lingua extract comprises the following steps: heating folium Pyrrosiae powder with ethanol under reflux, filtering, rotary evaporating the filtrate to remove ethanol, decocting with water, filtering, eluting the filtrate with ethyl acetate, concentrating, and drying to obtain folium Pyrrosiae extract.

7. The fibroin mask solution according to claim 3, wherein the preparation method of the mahonia stem extract comprises the following steps: decocting caulis Mahoniae powder with water, filtering, heating the filtrate, concentrating, eluting with ethanol, concentrating, and drying to obtain caulis Mahoniae extract.

8. The fibroin mask solution according to claim 3, wherein the pomegranate peel extract is prepared by the following method: heating and refluxing pericarpium Granati powder obtained by pulverizing pericarpium Granati with ethanol, filtering, rotary evaporating the filtrate to remove ethanol, eluting with petroleum ether, eluting with ethyl acetate, concentrating, and drying to obtain pericarpium Granati extract.

9. The preparation method of the fibroin mask solution is characterized by comprising the following steps:

s1, weighing the components for later use according to the formula of the fibroin mask solution as claimed in any one of claims 1-8;

s2, mixing the pomegranate bark extract, the Chinese violet extract, the pyrrosia lingua extract and the mahonia stem extract, adding the mixture into the fibroin hydrolysate, and uniformly mixing to obtain a first mixed solution;

s3, mixing 1, 2-hexanediol, butanediol and olive oil, heating to 86-88 ℃, and uniformly mixing to obtain a second mixed solution;

s4, adding the first mixed solution into water at 86-88 ℃, uniformly mixing, adding the second mixed solution, diisostearyl malate and decyl olivate, and uniformly stirring to obtain a primary mixed material;

s5, cooling the primary mixed material to 45 ℃, adding triethanolamine, and uniformly stirring to obtain the silk protein mask liquid.