CN117679328A

CN117679328A - Liquid crystal mud film with repairing effect and preparation method thereof

Info

Publication number: CN117679328A
Application number: CN202311719037.5A
Authority: CN
Inventors: 宁辉; 郭海姣; 王晓娜; 韩婷婷; 杨素珍; 陈鑫; 李晓杰; 徐佩佩; 王晓霞
Original assignee: Shandong Furida Biological Co ltd
Current assignee: Shandong Furida Biological Co ltd
Priority date: 2023-12-14
Filing date: 2023-12-14
Publication date: 2024-03-12

Abstract

The invention discloses a liquid crystal mud film with repairing effect and a preparation method thereof, wherein the liquid crystal mud film comprises an oil phase and a water phase, and the oil phase comprises DZ091 bionic liquid crystal, octenyl succinic acid starch calcium and grease; the water phase comprises humectant, thickener, powder, antiseptic and water. The invention is proved by a large number of experimental tests: the DZ091 bionic liquid crystal and octenyl succinic acid starch calcium are compounded to enhance the structural stability of the liquid crystal, and the traditional mud film has better skin feel, milder and good repairing effect through a liquid crystal emulsification technology, is especially suitable for sensitive muscle groups, and also solves the problems of quick drying, tight after washing and single effect of the traditional mud film.

Description

Liquid crystal mud film with repairing effect and preparation method thereof

Technical Field

The invention relates to the technical field of cosmetics, in particular to a liquid crystal mud film with repairing effect and a preparation method thereof.

Background

Along with the influence of environmental factors such as air pollution, ultraviolet rays, changing seasons and the like, factors such as irregular work and rest, improper skin care and the like, sensitive muscle groups are increased year by year, and the awareness of consumers on sensitive muscle care is gradually enhanced, so that the continuous expansion of the whole sensitive muscle market is promoted. In recent years, consumers of sensitive muscle groups gradually advance from basic skin care requirements to higher-order efficacy, and the consumers show a refined and personalized trend.

The mud-like cleansing facial mask can enhance the regeneration capacity of the horny layer by removing aged horny layer and adsorb skin secretion so as to achieve the cleansing purpose. In terms of use feeling, the traditional mud film is not suitable for sensitive skin because a large amount of grease and moisture on skin are absorbed in the drying process, the skin is strongly tensed after being cleaned, and skin sensitivity is more easily caused. In terms of efficacy, the traditional mud film mainly takes cleaning as a main part, has single efficacy, and is no longer suitable for the current age of efficacy skin care, so that the moderate mud film with repairing efficacy is also a appeal of sensitive muscle groups.

The liquid crystal emulsification technology is used as a front preparation technology, and has obvious advantages in the field of cosmetics. The liquid crystal is an intermediate phase between liquid and solid, and because of the unique double-layer structure, a large amount of bound water can be contained in the liquid crystal phase, so that the water retention capacity of the stratum corneum is improved, and therefore, the liquid crystal emulsion or cream with high moisture retention property is deeply favored by sensitive muscle groups. The emulsion liquid crystal system in the cosmetic field generally belongs to lyotropic liquid crystal, is influenced by factors such as temperature, liquid crystal emulsifier type and content, preparation mode and the like, and has unstable liquid crystal structure, so that the application of the liquid crystal emulsion technology is limited.

At present, the research of combining a liquid crystal emulsification technology with a mud film dosage form is less, and no product application exists in the market, so that the development of a liquid crystal mud film with repairing efficacy, sensitive muscle application and stable liquid crystal structure is necessary, and the problems of poor skin feel, single dosage form, single efficacy and the like of the mud film product can be greatly solved.

Disclosure of Invention

Aiming at the problems, the invention provides a liquid crystal mud film with repairing effect and a preparation method thereof, and the invention is proved by a large number of experimental tests: the structure stability of the liquid crystal is enhanced by compounding DZ091 bionic liquid crystal and octenyl succinic acid starch calcium, and the mud film prepared by the liquid crystal emulsification technology has better skin feel, milder skin care effect and good repairing effect compared with the traditional mud film, is especially suitable for sensitive muscle groups, and also solves the problems of quick drying, tight after washing and single effect of the traditional mud film.

In order to achieve the technical purpose, the technical scheme provided by the invention is as follows: the liquid crystal mud film with the repairing effect comprises an oil phase and a water phase, and is characterized in that the oil phase comprises the following components: DZ091 bionic liquid crystal, octenyl succinic acid starch calcium and grease; the aqueous phase comprises the following components: humectant, thickener, powder, antiseptic and water.

Furthermore, the water phase can also comprise other auxiliary materials such as skin feel conditioning agents and the like.

Wherein the DZ091 bionic liquid crystal plays a role of an emulsifier, and is purchased from Shanghai plant and sodium biotechnology Co., ltd, and the commercial name is DZ091 bionic liquid crystal, and the raw materials comprise cetylstearyl alcohol more than 50%, phytosterol 10% -20% and glycerol isostearate10 to 20 percent of the components and 1 to 5 percent of hydrogenated lecithin. Calcium starch octenyl succinate available from food ingredients Inc. under the trade name FARMAl ^TM AF1100。

Further, the liquid crystal mud film comprises the following components in percentage by mass: 2.0 to 5.0 percent of DZ091 bionic liquid crystal, 0.5 to 2.0 percent of octenyl succinic acid starch calcium, 2 to 20 percent of grease, 2 to 15 percent of humectant, 0.2 to 1.2 percent of thickener, 5 to 15 percent of powder, 0.4 to 2 percent of preservative, 0 to 18 percent of other auxiliary materials and the balance of water.

Further preferably, the liquid crystal mud film comprises the following components in percentage by mass: 2.5 to 3.5 percent of DZ091 bionic liquid crystal, 1.0 to 1.5 percent of octenyl succinic acid starch calcium, 5 to 15 percent of grease, 6 to 10 percent of humectant, 0.3 to 1.0 percent of thickener, 10 to 15 percent of powder, 0.4 to 1 percent of preservative, 0 to 9 percent of other auxiliary materials and the balance of water.

Further, the humectant comprises, but is not limited to, one or more humectants of glycerin, dipropylene glycol, butylene glycol, propylene glycol, methyl propylene glycol, 1, 2-hexanediol, and the thickener comprises, but is not limited to, sodium polyacrylate grafted starch, carbomer, xanthan gum, hydroxyethyl cellulose, polyacrylate crosslinked polymer-6, ammonium acryloyldimethyl taurate/VP copolymer, hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer, sepipplus 400 (available from saicing), simull EG (available from saicing), a combination of any one or more of magnesium aluminum silicate; the powder comprises, but is not limited to, any one or a combination of a plurality of powder of kaolin, bentonite, kieselguhr, titanium dioxide and carbon powder; the preservative is any one or more of hydroxyacetophenone, octanoyl hydroxamic acid and phenoxyethanol.

Further, the grease functions as an emollient, including, but not limited to, any one or a combination of two or more of cetostearyl alcohol, isononyl isononanoate, squalane, caprylic/capric triglyceride, beeswax, mineral oil, berkulare seed oil, white pool seed oil, polydimethylsiloxane, cyclopentadimethicone, isododecane, jojoba seed oil, tri (ethylhexanoic) glyceride, behenyl alcohol, shea butter, pentaerythritol tetraisostearate, dioctyl carbonate, tocopheryl acetate.

The invention also provides a preparation method of the liquid crystal mud film, which is characterized by comprising the following steps of:

s1, preparation of an aqueous phase:

adding the thickener into water, stirring and dispersing until no particles exist, adding the powder raw material, stirring and dispersing until no particles exist, adding the humectant, and heating to 80-85 ℃;

s2, oil phase preparation:

heating the grease to 80-85 ℃ for melting, and then adding DZ091 bionic liquid crystal and octenyl succinic acid starch calcium for melting and dispersing;

s3, homogenizing:

mixing the water phase and the oil phase, homogenizing, adding other auxiliary materials such as preservative and the like when the temperature is reduced to 40-50 ℃, and stirring and mixing uniformly to prepare the liquid crystal mud film.

Further, the homogenizing speed of the step S3 is 3000 rpm-8000 rpm, and the homogenizing time is 4-6 min.

The beneficial technical effects of the invention are as follows:

1. according to the liquid crystal mud film prepared by the invention, DZ091 bionic liquid crystal is compounded with octenyl succinic acid starch calcium, so that the stability of the mud film and the liquid crystal structure is improved.

2. The mud film prepared by the liquid crystal emulsification technology is more friendly to sensitive muscles and better in skin feel; the DZ091 bionic liquid crystal is compounded with the octenyl succinic acid starch calcium, so that the trans-epidermal water loss TEWL value can be obviously reduced when both D14 and D28 are used, and the repairing effect is good;

3. the liquid crystal mud film prepared by the liquid crystal emulsification technology solves the problems of quick drying and tight washing of the traditional mud film.

Drawings

Fig. 1: a sample polarized light morphological map of example 1;

fig. 2: a sample polarized light morphological map of example 2;

fig. 3: morphology of the sample of example 2 under polarized light after 1 month of cold and hot cycling;

fig. 4: a sample polarized light morphological map of example 3;

fig. 5: a sample polarized light morphological map of example 4;

fig. 6: morphology of the sample of comparative example 1 under polarized light;

fig. 7: morphology of the sample of comparative example 2 under polarized light;

fig. 8: morphology of the sample of comparative example 2 under polarized light after 1 month of cold and hot cycling.

Detailed Description

The invention is further illustrated by the examples and figures which follow, without thereby restricting the invention to the scope of the examples described. Based on the embodiments of the present invention, any changes to the present invention without making any creative changes to the present invention fall within the protection scope of the present invention. Meanwhile, in the examples of the present invention, all the preparation materials are commercially available products well known to those skilled in the art unless otherwise specified.

Table 1 formulations of liquid crystal mud films of examples 1 to 4 and comparative examples 1 to 4

The above mentioned GRANPOWDER USQ is purchased from Grant Industries, inc., INCI name: polydimethyl silsesquioxane (60%), HDI/trimethylol hexyl lactone cross-linked polymer (40%); SSE-20 is sold under the trade name Glucoarate ^TM SSE-20emulsifier was purchased from Libo, INCI name: PEG-20 methyl glucose sesquistearate (99.975%), tocopherol (vitamin E) (0.025%); SS trade name is glucose (TM) SS EMULSIFIER,41G FBR DR, available from road run, INCI name: methyl glucose sesquistearate.

The preparation methods of the mud film samples of examples 1 to 4 and comparative examples 1 to 4 include the following steps:

s1, preparation of an aqueous phase:

adding a thickening agent (xanthan gum, aluminum magnesium silicate and SEPIPLUS 400) into water, stirring and dispersing until no particles exist, adding powder raw materials, stirring and dispersing until no particles exist, adding a humectant (dipropylene glycol and glycerol), and heating to 80-85 ℃;

s2, oil phase preparation:

heating oil to 80-85 ℃ for melting, and then adding DZ091 bionic liquid crystal and octenyl succinic acid starch calcium (raw materials used in the comparative example are shown in table 1) for melting and dispersing;

s3, homogenizing:

mixing and homogenizing the water phase and the oil phase, cooling to 45 ℃ for 5min at a homogenizing speed of 5000rpm, adding the preservative, and uniformly stirring and mixing to obtain the liquid crystal mud film.

Test example 1: stability test

The samples of examples 1 to 4 and comparative examples 1 to 4 were placed at room temperature, -18 ℃,4 ℃,45 ℃ and the cold and hot cycle (-18 ℃,4 ℃,45 ℃ and once every 3 days) respectively, and the stability of the products was judged by judging whether the phenomena of oil outlet, water outlet, thickening of the materials and the like occur, and if the phenomena of instability of the oil outlet, water outlet, thickening of the materials and the like do not occur, the products pass through the stability, and do not pass through the reasons of the indication, and the specific results are shown in the following table 2.

TABLE 2 stability test results

From Table 2, in examples 1 to 4, the DZ091 bionic liquid crystal and the octenyl succinic acid starch calcium are compounded in different proportions, and the stability result is good; in comparative example 1, only DZ091 bionic liquid crystal is adopted, and the phenomenon of thickening of a material body occurs at low temperature; comparative example 2DZ091 bionic liquid crystal is compounded with USQ, and the phenomenon of thickening of a material body occurs at low temperature; comparative example 3, wherein SS, SSE-20emulsifier and octenyl succinic acid starch calcium are compounded, the prepared mud film with a non-liquid crystal structure has the phenomenon of thickening materials at low temperature and circulation; comparative example 4 mud film was prepared using only starch calcium octenyl succinate, and the phenomenon of unstable output of recycled water and oil occurred at normal temperature, low temperature, high temperature. Therefore, the liquid crystal mud film prepared by compounding the DZ091 bionic liquid crystal and the octenyl succinic acid starch calcium can improve the stability of the mud film.

Test example 2: liquid crystal structural stability experiment

The prepared samples of examples 1 to 4 and comparative examples 1 to 2 were photographed under a polarizing microscope to obtain microscopic morphology patterns, and comparative example 3 was a non-liquid crystal mud film, and no liquid crystal structure was observed under a polarizing microscope, no photographing was performed, and comparative example 4 was not passed in stability and no photographing was performed. The polarized light morphological diagrams of examples 1 to 4 and comparative examples 1 to 2 are shown in detail in fig. 1,2, and 4 to 7.

The samples of examples 1 to 4 and comparative examples 1 to 2, which were placed at room temperature, -18 ℃,4 ℃, and 45 ℃ in test example 1, were periodically photographed for a liquid crystal structure, and changes in the liquid crystal structure were recorded, and the results are shown in table 3, and the figures of the polarized light patterns after 1 month of the cold and hot cycles of example 2 and comparative example 2 are shown in fig. 3 and 8.

TABLE 3 results of liquid crystal structure stability experiments

As is clear from fig. 1 to 8 and table 3, the liquid crystal structures of examples 1 to 4 are significantly more than those of comparative examples 1 to 2, and the stability of the liquid crystal structures is good, and the liquid crystal structures of comparative examples 1 to 2 are less, and the high temperature and cycle stability are poor. The liquid crystals of examples 2 and 3 had a small structure, a uniform size, a better morphology, the liquid crystals of examples 1 and 4 had a larger structure, a larger difference in size, and a slightly inferior stability. The liquid crystal mud film prepared by compounding the bionic liquid crystal and the octenyl succinic acid starch calcium can improve the number of liquid crystal structures and the stability of the liquid crystal structures, but the compounding proportion of the bionic liquid crystal and the octenyl succinic acid starch calcium also can influence the shape and the stability of the liquid crystal.

Test example 3: skin feel test experiment

Questionnaires (28 persons are drawn in this questionnaire, the ages are 23-50 years old, and men and women are not limited).

28 subjects were enrolled in the experiment, and examples 1 to 4 and comparative examples 1 to 3, which passed the stability at room temperature, were used as test samples, and the sample of comparative example 4 could not be tested due to water and oil at room temperature. The same sample is used for 4 volunteers to try out, the product is respectively tried on the face, 4 g of sample is accurately weighed each time, the sample is uniformly smeared on the face, and the face is cleaned by clean water after 30 minutes. Four indexes of the dry crack speed, the moistening degree, the smearing feeling and the no discomfort are used as evaluation standards, and the examples 1 to 4 and the comparative examples 1 to 3 are scored: a score of 1-5 points, a higher score indicates that the sample is favored by volunteers, and the better the performance. The detailed results are shown in Table 4.

TABLE 4 skin feel test results

As can be seen from Table 4, the overall satisfaction degree of example 2 > example 3 > example 1 > example 4 > comparative example 2 > comparative example 1 > comparative example 3, and the overall satisfaction degree of example 2 and example 3 were not greatly different from each other by comparison of comparative examples 1 to 4 and comparative examples 1 to 3. Examples 1 to 4 the skin feel of the liquid crystal mud film prepared by compounding the DZ091 bionic liquid crystal and the octenyl succinic starch calcium was more excellent than that of the liquid crystal mud film prepared by comparative example 1 using the DZ091 bionic liquid crystal alone, that of comparative example 2 prepared by DZ091 bionic liquid crystal and USQ, and that of comparative example 3 non-liquid crystal mud film.

Test example 4: irritation evaluation test

30 subjects are recruited in the experiment, the ages of men and women are not limited, the ages of men and women are 23-50 years, examples 1-4 and comparative examples 1-3 with the stability passing at room temperature are used as test objects, blank is negative control, and the test method is that the selection area is not more than 50mm ² A suitable plaque tester with a depth of about 1mm is provided, and about 0.020 to 0.025g of a test object is added into the plaque tester by a closed type patch test method. The external hypoallergenic tape was applied to the back of the subjects, and each tester tested eight samples, blank, examples 1-4, comparative examples 1-3, 24After the removal of the test substance for an hour, the skin reaction was observed at 0.5, 24 and 48 hours after the removal, and the results were recorded according to the skin reaction classification standard (Table 5) in cosmetic safety technical Specification 2015, and the detailed results are shown in Table 6.

TABLE 5 skin reaction grading criteria

TABLE 6 test results of stimulation evaluation

As can be seen from Table 6, the samples of examples 1 to 4 did not exhibit adverse reaction, and were mild and non-irritating; adverse reactions of different degrees appear in all of comparative examples 1 to 3, wherein the adverse reaction of the non-liquid crystal mud film comparative example 3 is the most serious. The liquid crystal mud film prepared from DZ091 bionic liquid crystal and octenyl succinic acid starch calcium is milder, and the irritation of the mud film is reduced.

Test example 5: human body repair efficacy evaluation experiment

30 lactic acid stinging test positive subjects were recruited, and human body repair efficacy was evaluated for example 2 and comparative example 3, with ages 18 to 50, without limitation. Example 2 was applied to the left face of the subject, comparative example 3 was applied to the right face of the subject, and the samples were each applied about 2g per week for 4 weeks, and the trans-epidermal water loss TEWL value (tewatter TM 300) was evaluated. The test period was before use (D0), after use for 2 weeks (D14), after use for 4 weeks (D28). Under the test condition, the higher the TEWL value is, the more the transepidermal water loss amount representing the unit time and the unit cross-sectional area is; the lower the TEWL value, the less transepidermal water loss per unit time, per unit cross-sectional area, and the detailed results are shown in table 7.

TABLE 7 TEWL value and statistical result of facial transepidermal Water loss

Note that: (1) the normal test P value is more than 0.05, which shows that the data obeys normal distribution, paired t test is adopted, and if the data does not obey normal distribution, non-parameter test is adopted; (2) the significance P value is less than 0.05, which shows that compared with the significance P value before use, the significance P value is different from the significance P value, and the significance P value is expressed by 'x'; p value < 0.01, indicated by "; p value < 0.001, indicated by "×". The significance P value is more than or equal to 0.05, which shows that compared with the significance P value before use, no significance difference exists, and the significance P value is represented by "-".

From Table 7, it is clear that the liquid crystal mud film prepared from DZ091 bionic liquid crystal and octenyl succinic acid starch calcium in example 2 can significantly reduce the TEWL value by using both D14 and D28, and has significant repairing effect; the non-liquid crystal mud film of comparative example 3 has no remarkable reduction effect on TEWL when using D14 and D28, and has no repairing effect. Therefore, the liquid crystal mud film prepared from DZ091 bionic liquid crystal and octenyl succinic acid starch calcium has good repairing effect.

Claims

1. The liquid crystal mud film with the repairing effect comprises an oil phase and a water phase, and is characterized in that the oil phase comprises the following components: DZ091 bionic liquid crystal, octenyl succinic acid starch calcium and grease; the aqueous phase comprises the following components: humectant, thickener, powder, antiseptic and water.

2. The liquid crystal mud film of claim 1 wherein the aqueous phase further comprises other excipients.

3. The liquid crystal mud film according to claim 1 or 2, wherein the liquid crystal mud film comprises the following components in percentage by mass: 2.0 to 5.0 percent of DZ091 bionic liquid crystal, 0.5 to 2.0 percent of octenyl succinic acid starch calcium, 2 to 20 percent of grease, 2 to 15 percent of humectant, 0.2 to 1.2 percent of thickener, 5 to 15 percent of powder, 0.4 to 2 percent of preservative, 0 to 18 percent of other auxiliary materials and the balance of water.

4. A liquid crystal mud film according to claim 3, wherein the liquid crystal mud film comprises the following components in percentage by mass: 2.5 to 3.5 percent of DZ091 bionic liquid crystal, 1.0 to 1.5 percent of octenyl succinic acid starch calcium, 5 to 15 percent of grease, 6 to 10 percent of humectant, 0.3 to 1.0 percent of thickener, 10 to 15 percent of powder, 0.4 to 1 percent of preservative, 0 to 9 percent of other auxiliary materials and the balance of water.

5. The liquid crystal mud film of claim 1 wherein the humectant is one or more of glycerin, dipropylene glycol, butylene glycol, propylene glycol, methyl propylene glycol, 1, 2-hexanediol.

6. The liquid crystal mud film of claim 1 wherein the thickener is any one or more of sodium polyacrylate, sodium polyacrylate grafted starch, carbomer, xanthan gum, hydroxyethyl cellulose, polyacrylate crosslinked polymer-6, ammonium acryloyldimethyl taurate/VP copolymer, hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer, sepipplus 400, simullegeleg, magnesium aluminum silicate.

7. The liquid crystal mud film of claim 1, wherein the powder is any one or a combination of a plurality of kaolin, bentonite, kieselguhr, titanium dioxide and carbon powder; the preservative is any one or more of hydroxyacetophenone, octanoyl hydroxamic acid and phenoxyethanol.

8. The liquid crystal mud film according to claim 1, wherein the grease is any one or a combination of two or more of cetostearyl alcohol, isononyl isononanoate, squalane, caprylic/capric triglyceride, beeswax, mineral oil, berhard walnut seed oil, white pool seed oil, polydimethylsiloxane, cyclopentadimethicone, isododecane, jojoba seed oil, tri (ethylhexanoic) glyceride, behenyl alcohol, shea butter, pentaerythritol tetraisostearate, dioctyl carbonate, and tocopheryl acetate.

9. The method for preparing a liquid crystal mud film according to claim 3, which comprises the following steps:

s1, preparation of an aqueous phase:

s2, oil phase preparation:

s3, homogenizing:

mixing the water phase and the oil phase, homogenizing, adding the preservative and other auxiliary materials when the temperature is reduced to 40-50 ℃, and stirring and mixing uniformly to prepare the liquid crystal mud film.

10. The method for preparing a liquid crystal mud film according to claim 9 wherein the homogenizing speed of the step S3 is 3000rpm to 8000rpm, and the homogenizing time is 4 to 6min.