Ectoine-containing composition and preparation method thereof

Abstract

The invention provides a composition containing Ectoine and a preparation method thereof, and belongs to the technical field of compositions of Ectoine. The preparation method comprises the steps of plant carrier preparation, plant carrier pretreatment, primary compounding, secondary compounding and mixing. The secondary compounding step comprises the following steps: putting a primary compound into deionized water, and uniformly stirring to prepare a primary compound liquid; putting the modified sodium hyaluronate into deionized water, and uniformly stirring to obtain a modified sodium hyaluronate solution; mixing the primary compound solution with a modified sodium hyaluronate solution, then adding gamma-aminobutyric acid, uniformly mixing, carrying out heat-preservation reaction in a water bath at 40-44 DEG C for 5.8-6.2 hours, and after the heat-preservation reaction is finished, drying to obtain a secondary compound; the composition prepared by the invention has relatively good moisturizing performance on skin, and is stable in slow release performance and lasting in action time.

Description

Technical Field

[0001] The invention belongs to the technical field of ectoine compositions, and particularly relates to an ectoine-containing composition and a preparation method thereof. Background Art

[0002] Ectoine, whose chemical name is 2-methyl-1,4,5,6-tetrahydropyrimidine-4-carboxylic acid, also known as tetrahydromethylpyrimidinecarboxylic acid, is a natural protective ingredient produced by microorganisms under extreme environments. It is an amino acid derivative and a cyclic amino acid. Ectoine is mainly derived from highly halophilic bacteria. The presence of Ectoine enables highly halophilic bacteria to survive in extreme environments such as high salt, high temperature, and strong ultraviolet rays.

[0003] Ecdoin can protect cells from damage caused by extreme environmental conditions, such as high temperature, dryness, strong ultraviolet radiation, etc. It can promote the repair and regeneration process of cells, increase skin elasticity, and reduce wrinkles and skin roughness. Ecdoin has a strong water-locking ability. It can form a tight water-locking film on the skin surface by virtue of its ability to complex water molecules, retaining skin moisture and keeping the skin hydrated. Ecdoin can also calm and soothe irritated and damaged skin, significantly increase the skin's regeneration process, improve skin tolerance, and protect the skin from the hazards of visible light and blue light radiation. Therefore, as a highly effective skin care ingredient, Ecdoin is widely used in skin care cosmetics such as toner, sunscreen, cream, facial mask, repair fluid and lotion, and is favored by many consumers.

[0004] Directly using ectoine in skin care cosmetics can effectively enhance the moisturizing, skin care and repairing properties, but its action time is short and the sustainability is poor. The ectoine-containing composition with sustained release properties prepared by the prior art is difficult to control the rate of water release. Under the action of external force, the system will suddenly break the emulsion and release water, and the encapsulated water will be released all at once on the skin surface, causing it to appear thick and greasy and uneven on the skin, which greatly affects the feeling of use.

[0005] CN116440018A discloses a water-slow-release composition containing ectoine and a preparation method thereof, which is composed of the following raw materials in parts by weight: butylene glycol, cyclopentasiloxane, glycerol, polydimethylsiloxane, composite emulsifier, sodium chloride, p-hydroxyacetophenone, ectoine, saccharide isomers, magnesium sulfate, 1,2-hexanediol / glycol, β-glucan, niacinamide, squalane, sodium hyaluronate, xanthan gum and composite essential oil; The moisture sustained-release composition containing ectoine prepared by the method is refreshing and moisturizing, and improves the applicability of the product based on the pleasant feeling of use by consumers. When applied to an arm with a moisture content of 30, the moisture content reaches a maximum value of about 60 at the 30th minute, and the moisture content is about 50 at the 360th minute. However, after 360 minutes, the moisture content will drop rapidly, and the action time of the composition is still relatively short. Summary of the invention

[0006] In order to solve the technical problems existing in the prior art, the present invention provides a composition containing ectoine and a preparation method thereof, which has good moisturizing and hydrating properties for the skin, stable sustained-release properties and a lasting action time.

[0007] In view of the above technical problems, the present invention adopts the following technical solutions: A method for preparing a composition containing ectoine, comprising the steps of preparing a plant carrier, pretreating the plant carrier, primary compounding, secondary compounding and mixing, specifically as follows: 1. Preparation of plant vector The thyme leaves are placed in 8-12 times the mass of deionized water for washing, and then vacuum dried after washing, the drying temperature is controlled to be 60-64°C, the vacuum degree is 0.03-0.05MPa, the drying time is 2.8-3.2h, and after drying, the thyme leaves are crushed to a particle size of 48-52μm to obtain thyme leaf powder; the thyme leaf powder is placed in 6-9 times the mass of ethanol solution and stirred, the stirring temperature is 45-50°C, the stirring time is 1.8-2.2h, and after stirring, an ultrasonic extraction is performed, the extraction time is 32-37min, the ultrasonic power is 275-285W, and the ultrasonic The frequency is 32-37kHz. After the ultrasonic treatment, the temperature is raised to 58-62°C at a rate of 0.3-0.6°C / min, and the mixture is stirred for 38-42min before secondary ultrasonic extraction. The extraction time is 24-26min, the ultrasonic power is 295-305W, and the ultrasonic frequency is 27-32kHz. After the ultrasonic extraction, a mixed solution is obtained. The mixed solution is filtered to obtain a filter residue, and the filter residue is vacuum dried at 64-66°C for 5.8-6.2h at a vacuum degree of 0.02-0.04MPa. After the vacuum drying, the mixture is crushed to a particle size of 8-12μm to obtain a plant carrier. The volume concentration of the ethanol solution is 68-72%.

[0008] 2. Plant carrier pretreatment The plant carrier is placed in an ethanol solution, polyethylene glycol 200 is added, the temperature is raised to 53-57° C., and the mixture is stirred at 250-260 rpm for 28-32 minutes. After the stirring is completed, chitosan solution and sodium cocoyl glycinate are added, and the stirring is continued for 37-42 minutes. After the stirring is completed, the mixture is dried to obtain a pretreated plant carrier. The mass ratio of the plant carrier, ethanol solution, polyethylene glycol 200, chitosan solution and sodium cocoyl glycinate is 6.3-6.7:78-82:0.6-0.8:10.6-11.0:0.8-1.2; The mass concentration of the ethanol solution is 24-26%; The chitosan solution is a mixture of chitosan and acetic acid solution, the mass ratio of the chitosan to the acetic acid solution is 2.4-2.6:32-37, and the mass concentration of the acetic acid solution is 18-22wt%.

[0009] 3. One-time compound Add octyldodecanol and disodium lauroamphodiacetate to deionized water, stir evenly to obtain a mixed solution one; place ectoine in deionized water for ultrasonic dispersion, the ultrasonic time is 18-22 minutes, the ultrasonic power is 107-112W, and the ultrasonic frequency is 24-26kHz. After the ultrasonic treatment, add the mixed solution one and stir evenly to obtain an ectoine mixed solution; add the pretreated plant carrier to the ectoine mixed solution, heat it to 38-42°C at a rate of 0.4-0.6°C / min, stir it at 472-485rpm for 1.4-1.6h, add glutathione, stir evenly, filter, wash and dry to obtain a primary complex; The mass ratio of the deionized water, octyldodecanol and disodium lauroamphodiacetate is 98-103:1.4-1.6:1.0-1.3; The mass ratio of ectoine, deionized water and mixed solution 1 is 7.8-8.2:68.0-72.0:34.3-35.0; The mass ratio of the ectoine mixed solution, the pretreated plant carrier and glutathione is 68.0-72.0:5.8-6.2:1.0-1.2.

[0010] 4. Secondary compound The primary complex is placed in deionized water and stirred evenly to obtain a primary complex liquid; the modified sodium hyaluronate is placed in deionized water and stirred evenly to obtain a modified sodium hyaluronate solution; the primary complex liquid is mixed with the modified sodium hyaluronate solution, and then γ-aminobutyric acid is added and mixed evenly, and the mixture is kept warm in a water bath at 40-44° C. for 5.8-6.2 hours. After the warming reaction is completed, the mixture is freeze-dried at -42 to -38° C. for 18.0-22.0 hours, and then naturally recovered to room temperature to obtain a secondary complex; In the primary composite liquid, the mass ratio of the primary composite to deionized water is 4.8-5.2:58-62; In the modified sodium hyaluronate solution, the mass ratio of modified sodium hyaluronate to deionized water is 4.7-5.3:40-45; The mass ratio of the primary composite solution, the modified sodium hyaluronate solution, and the γ-aminobutyric acid is 18.2-18.7:27.2-27.7:2.0-2.3; The preparation method of the modified sodium hyaluronate is as follows: 9.8-10.2 g of sodium hyaluronate is added to 85-90 g of deionized water, and after stirring evenly, 3.0-3.4 g of sodium periodate is added, and the reaction is carried out under light-proof conditions at a reaction temperature of 20-24° C. for a reaction time of 2.8-3.2 h. After the reaction is completed, the modified sodium hyaluronate is obtained by filtering, washing, and drying. In the preparation method of the modified sodium hyaluronate, the mass ratio of the sodium hyaluronate, deionized water, and sodium periodate is 9.8-10.2:85-90:3.0-3.4.

[0011] 5. Mix Add the secondary complex and Tween 20 to deionized water, stir evenly, then add sorbitol, camellia oil, gum arabic, and niacinamide, stir evenly, and then perform homogenization, the homogenization time is 4.8-5.2 min, the homogenization pressure is 2.6-3.0 MPa, the homogenization times are 3 times, and after the homogenization is completed, a composition containing ectoine is obtained; The mass ratio of the deionized water, the secondary complex, Tween 20, sorbitol, camellia oil, gum arabic and nicotinamide is 90-94:8.5-9.0:2.4-2.6:0.8-1.2:0.40-0.44:0.73-0.77:0.54-0.56.

[0012] A composition containing ectoine is prepared by the above-mentioned preparation method.

[0013] Compared with the prior art, the present invention has achieved the following beneficial effects: 1. The present invention adopts a specific method to prepare a composition containing ectoine, which uses powder of leaves of Lamiaceae plants as a carrier to load ectoine. Specifically, the powder is first dispersed, and then amino groups are introduced through ingredients such as chitosan, so that the surface of the plant carrier contains amino groups, and then it is compounded with ectoine. Specifically, ectoine is dispersed to obtain a mixed liquid, and the ectoine is rich in hydroxyl groups and the like, and then the pretreated plant carrier and glutathione are added, so that the hydroxyl group of ectoine can be combined with the pretreated plant carrier and the amino group of glutathione through intermolecular forces, the firmness is good and the loading is complete, thereby improving the stability of the loading. Qualitative and sufficient, glutathione can also enhance the skin barrier function, which can improve the skin's resistance for a long time. In the secondary compounding step, the modified aldehyde-modified sodium hyaluronate is introduced, which can cross-link with the amino groups on the surface of the primary compound, thereby improving the stability of the secondary compound. In addition, γ-aminobutyric acid has good skin regeneration and repair functions, which can be firmly combined with the primary compound and has a good long-term effect, thereby achieving a firm combination of ectoine, plant carrier and modified sodium hyaluronate. It is mixed with other ingredients to improve the moisturizing performance of the composition and ensure the sustained release performance, so that the composition has long-lasting moisturizing and hydrating performance and excellent sustained release performance; 2. The composition containing ectoine prepared by the present invention is used on the inner side of the arm with a moisture content of 27.1%, the application area is 5.0 cm×5.0 cm, the application amount is 1.8 g, the moisture content after 20 minutes of application is 65.7-67.8%, the moisture content after 3.0 hours of application is 62.5-64.6%, the moisture content after 6.0 hours of application is 59.1-61.5%, and the moisture content after 10.0 hours of application is 55.3-57.7%. DETAILED DESCRIPTION

[0014] In order to more clearly understand the technical features, purposes and effects of the present invention, specific embodiments of the present invention are now described.

[0015] Example 1 1. Preparation of plant vector The thyme leaf powder was placed in 10 times the mass of deionized water for washing, and then vacuum dried after washing, the drying temperature was controlled to be 62°C, the vacuum degree was 0.04MPa, the drying time was 3.0h, and the powder was crushed to a particle size of 50μm to obtain thyme leaf powder; the thyme leaf powder was placed in 8 times the mass of ethanol solution for stirring, the stirring temperature was 47°C, the stirring time was 2.0h, and an ultrasonic extraction was performed after the stirring, the extraction time was 35min, the ultrasonic power was 280W, and the ultrasonic frequency was 35kHz. After the ultrasonic extraction, the temperature was raised to 60°C at a rate of 0.5°C / min, and after stirring for 40min, a second ultrasonic extraction was performed, the extraction time was 25min, the ultrasonic power was 300W, and the ultrasonic frequency was 30kHz. After the ultrasonic extraction, a mixed solution was obtained; the mixed solution was filtered to obtain a filter residue, and the filter residue was vacuum dried at 65°C for 6.0h and the vacuum degree was 0.03MPa. After the vacuum drying, the powder was crushed to a particle size of 10μm to obtain a plant carrier; The volume concentration of the ethanol solution is 70%.

[0016] 2. Plant carrier pretreatment 6.5 g of the plant carrier was placed in 80 g of 25 wt% ethanol solution, 0.7 g of polyethylene glycol 200 was added, the temperature was raised to 55° C., and the mixture was stirred at 255 rpm for 30 min. After the stirring was completed, 10.8 g of chitosan solution and 1.0 g of sodium cocoyl glycinate were added, and the stirring was continued for 40 min. After the stirring was completed, the mixture was dried to obtain a pretreated plant carrier; The chitosan solution is a mixture of chitosan and acetic acid solution, the mass ratio of the chitosan to the acetic acid solution is 2.5:35, and the mass concentration of the acetic acid solution is 20wt%.

[0017] 3. One-time compound Add 1.5g of octyldodecanol and 1.2g of disodium lauroamphoacetate to 100g of deionized water, stir evenly to obtain a mixed solution one; place 8.0g of ectoine in 70.0g of deionized water for ultrasonic dispersion, the ultrasonic time is 20min, the ultrasonic power is 110W, and the ultrasonic frequency is 25kHz. After the ultrasonic treatment, add 34.6g of mixed solution one and stir evenly to obtain an ectoine mixed solution; add 6.0g of pretreated plant carrier to 70.0g of the ectoine mixed solution, heat to 40°C at a rate of 0.5°C / min, stir at 480rpm for 1.5h, add 1.1g of glutathione, stir evenly, filter, wash and dry to obtain a primary complex.

[0018] 4. Secondary compound 5.0 g of the primary complex was placed in 60 g of deionized water and stirred to obtain a primary complex liquid; 5.0 g of modified sodium hyaluronate was placed in 42 g of deionized water and stirred to obtain a modified sodium hyaluronate solution; 18.4 g of the primary complex liquid was mixed with 27.5 g of the modified sodium hyaluronate solution, and then 2.1 g of γ-aminobutyric acid was added and mixed to obtain a secondary complex; the mixture was kept warm in a water bath at 42° C. for 6.0 h, and after the reaction was completed, the mixture was freeze-dried at -40° C. for 20.0 h and then naturally recovered to room temperature to obtain a secondary complex; The preparation method of the modified sodium hyaluronate is as follows: 10.0 g of sodium hyaluronate is added to 87 g of deionized water, and after stirring evenly, 3.2 g of sodium periodate is added, and the reaction is carried out in a light-proof condition at a reaction temperature of 22° C. for a reaction time of 3.0 h. After the reaction is completed, the modified sodium hyaluronate is obtained by filtering, washing, and drying.

[0019] 5. Mix Add 8.7 g of the secondary complex and 2.5 g of Tween 20 to 92 g of deionized water, stir evenly, then add 1.0 g of sorbitol, 0.42 g of camellia oil, 0.75 g of gum arabic, and 0.55 g of niacinamide, stir evenly, and then homogenize. The homogenization time is 5.0 min, the homogenization pressure is 2.8 MPa, and the homogenization times are 3 times. After the homogenization is completed, a composition containing ectoine is obtained.

[0020] Example 2 1. Preparation of plant vector The thyme leaf powder was placed in 8 times the mass of deionized water for washing, and then vacuum dried after washing, the drying temperature was controlled to be 60°C, the vacuum degree was 0.03MPa, the drying time was 2.8h, and the powder was crushed to a particle size of 48μm after drying to obtain thyme leaf powder; the thyme leaf powder was placed in 6 times the mass of ethanol solution for stirring, the stirring temperature was 45°C, the stirring time was 1.8h, and an ultrasonic extraction was performed after the stirring, the extraction time was 32min, the ultrasonic power was 275W, and the ultrasonic frequency was 32kHz. After the ultrasonic extraction, the temperature was raised to 58°C at a rate of 0.3°C / min, and after stirring for 38min, a second ultrasonic extraction was performed, the extraction time was 24min, the ultrasonic power was 295W, and the ultrasonic frequency was 27kHz. After the ultrasonic extraction, a mixed solution was obtained; the mixed solution was filtered to obtain a filter residue, and the filter residue was vacuum dried at 64°C for 5.8h and the vacuum degree was 0.02MPa. After the vacuum drying, the powder was crushed to a particle size of 8μm to obtain a plant carrier; The volume concentration of the ethanol solution is 68%.

[0021] 2. Plant carrier pretreatment 6.3 g of the plant carrier was placed in 78 g of 24 wt% ethanol solution, 0.6 g of polyethylene glycol 200 was added, the temperature was raised to 53° C., and the mixture was stirred at 250 rpm for 28 min. After the stirring was completed, 10.6 g of chitosan solution and 0.8 g of sodium cocoyl glycinate were added, and the stirring was continued for 37 min. After the stirring was completed, the mixture was dried to obtain a pretreated plant carrier; The chitosan solution is a mixture of chitosan and acetic acid solution, the mass ratio of the chitosan to the acetic acid solution is 2.5:32, and the mass concentration of the acetic acid solution is 18wt%.

[0022] 3. One-time compound Add 1.4g of octyldodecanol and 1.0g of disodium lauroamphoacetate to 98g of deionized water, stir evenly to obtain a mixed solution one; place 7.8g of ectoine in 68.0g of deionized water for ultrasonic dispersion, the ultrasonic time is 18min, the ultrasonic power is 107W, and the ultrasonic frequency is 24kHz. After the ultrasonic treatment, add 34.3g of mixed solution one and stir evenly to obtain an ectoine mixed solution; add 5.8g of pretreated plant carrier to 68.0g of the ectoine mixed solution, heat to 38°C at a rate of 0.4°C / min, stir at 472rpm for 1.4h, add 1.0g of glutathione, stir evenly, filter, wash and dry to obtain a primary complex.

[0023] 4. Secondary compound 4.8 g of the primary complex was placed in 58 g of deionized water and stirred evenly to obtain a primary complex liquid; 4.7 g of modified sodium hyaluronate was placed in 40 g of deionized water and stirred evenly to obtain a modified sodium hyaluronate solution; 18.2 g of the primary complex liquid was mixed with 27.2 g of the modified sodium hyaluronate solution, and then 2.0 g of γ-aminobutyric acid was added and mixed evenly, and the mixture was kept warm in a 40°C water bath for 5.8 hours. After the warming reaction was completed, the mixture was freeze-dried at -42°C for 18.0 hours, and then naturally recovered to room temperature to obtain a secondary complex; The preparation method of the modified sodium hyaluronate is as follows: 9.8 g of sodium hyaluronate is added to 85 g of deionized water, and after stirring evenly, 3.0 g of sodium periodate is added, and the reaction is carried out in a light-proof condition at a reaction temperature of 20° C. for a reaction time of 2.8 h. After the reaction is completed, the modified sodium hyaluronate is obtained by filtering, washing, and drying.

[0024] 5. Mix Add 8.5g of the secondary complex and 2.4g of Tween 20 to 90g of deionized water, stir evenly, then add 0.8g of sorbitol, 0.40g of camellia oil, 0.73g of gum arabic, and 0.54g of niacinamide, stir evenly, and then homogenize. The homogenization time is 4.8min, the homogenization pressure is 2.6MPa, and the homogenization times are 3 times. After the homogenization is completed, a composition containing ectoine is obtained.

[0025] Example 3 1. Preparation of plant vector The thyme leaf powder was placed in 12 times the mass of deionized water for washing, and then vacuum dried after washing, the drying temperature was controlled to be 64°C, the vacuum degree was 0.05MPa, the drying time was 3.2h, and the powder was crushed to a particle size of 52μm after drying to obtain thyme leaf powder; the thyme leaf powder was placed in 9 times the mass of ethanol solution for stirring, the stirring temperature was 50°C, the stirring time was 2.2h, and an ultrasonic extraction was performed after the stirring, the extraction time was 37min, the ultrasonic power was 285W, and the ultrasonic frequency was 37kHz. After the ultrasonic extraction, the temperature was raised to 62°C at a rate of 0.6°C / min, and the ultrasonic extraction was performed twice after stirring for 42min, the extraction time was 26min, the ultrasonic power was 305W, and the ultrasonic frequency was 32kHz. After the ultrasonic extraction, a mixed solution was obtained; the mixed solution was filtered to obtain a filter residue, and the filter residue was vacuum dried at 66°C for 6.2h and the vacuum degree was 0.04MPa. After the vacuum drying, the powder was crushed to a particle size of 12μm to obtain a plant carrier; The volume concentration of the ethanol solution is 72%.

[0026] 2. Plant carrier pretreatment 6.7 g of the plant carrier was placed in 82 g of 26 wt% ethanol solution, 0.8 g of polyethylene glycol 200 was added, the temperature was raised to 57°C, and the mixture was stirred at 260 rpm for 32 min. After the stirring was completed, 11.0 g of chitosan solution and 1.2 g of sodium cocoyl glycinate were added and the stirring was continued for 42 min. After the stirring was completed, the mixture was dried to obtain a pretreated plant carrier; The chitosan solution is a mixture of chitosan and acetic acid solution, the mass ratio of the chitosan to the acetic acid solution is 2.5:37, and the mass concentration of the acetic acid solution is 22wt%.

[0027] 3. One-time compound Add 1.6g of octyldodecanol and 1.3g of disodium lauroamphoacetate to 103g of deionized water, stir evenly to obtain a mixed solution one; place 8.2g of ectoine in 72.0g of deionized water for ultrasonic dispersion, the ultrasonic time is 22min, the ultrasonic power is 112W, and the ultrasonic frequency is 26kHz. After the ultrasonic treatment, add 35.0g of mixed solution one and stir evenly to obtain an ectoine mixed solution; add 6.2g of pretreated plant carrier to 72.0g of the ectoine mixed solution, heat to 42°C at a rate of 0.6°C / min, stir at 485rpm for 1.6h, add 1.2g of glutathione, stir evenly, filter, wash and dry to obtain a primary complex.

[0028] 4. Secondary compound 5.2 g of the primary complex was placed in 62 g of deionized water and stirred evenly to obtain a primary complex liquid; 5.3 g of modified sodium hyaluronate was placed in 45 g of deionized water and stirred evenly to obtain a modified sodium hyaluronate solution; 18.7 g of the primary complex liquid was mixed with 27.7 g of the modified sodium hyaluronate solution, and then 2.3 g of γ-aminobutyric acid was added and mixed evenly, and the mixture was kept warm in a water bath at 44° C. for 6.2 h. After the warming reaction was completed, the mixture was freeze-dried at -38° C. for 22.0 h, and then naturally recovered to room temperature to obtain a secondary complex; The preparation method of the modified sodium hyaluronate is as follows: 10.2 g of sodium hyaluronate is added to 90 g of deionized water, and after stirring evenly, 3.4 g of sodium periodate is added, and the reaction is carried out in a light-proof condition at a reaction temperature of 24° C. for a reaction time of 3.2 h. After the reaction is completed, the modified sodium hyaluronate is obtained by filtering, washing, and drying.

[0029] 5. Mix 9.0 g of the secondary complex and 2.6 g of Tween 20 were added to 94 g of deionized water, and after stirring, 1.2 g of sorbitol, 0.44 g of camellia oil, 0.77 g of gum arabic, and 0.56 g of niacinamide were added. After stirring, homogenization was performed. The homogenization time was 5.2 min, the homogenization pressure was 3.0 MPa, and the homogenization times were 3 times. After the homogenization treatment was completed, a composition containing ectoine was obtained.

[0030] Comparative Example 1 Based on Example 1, the changes are as follows: Omit the plant carrier pretreatment step; The first compounding step is to place 8.0g of ectoine in 70.0g of deionized water for ultrasonic dispersion, the ultrasonic time is 20min, the ultrasonic power is 110W, and the ultrasonic frequency is 25kHz. After the ultrasonic treatment, an ectoine mixed solution is obtained; 6.0g of plant carrier is added to the 70.0g ectoine mixed solution, the temperature is increased to 40°C at a rate of 0.5°C / min, and stirred at 480rpm for 1.5h. After the stirring is completed, the mixture is filtered, washed, and dried to obtain a first compound; The rest of the operations are the same.

[0031] Comparative Example 2 Based on Example 1, the changes are as follows: The secondary compounding step is omitted; in the compounding step, the secondary compound is replaced by the primary compound in equal amounts; The rest of the operations are the same.

[0032] Performance Testing Test method: 50 volunteers were selected, including 25 males and 25 females, aged between 20 and 45 years old, and were equally divided into 5 groups, each with 10 volunteers. The male-female ratio and the average age in each group were the same, and they were recorded as A1-A5; then the compositions prepared in Examples 1-3 and Comparative Examples 1-2 were evenly applied to the inner sides of both arms of the volunteers in groups A1-A5, with an application area of ​​5.0 cm×5.0 cm and an application amount of 1.8 g. In an environment with a temperature of 26°C and a relative humidity of 45%, the skin moisture content of different groups at different times was tested, and the test results were expressed as average values; before the start of the test, the skin moisture content of the area on the inner side of the arm of each group of volunteers in groups A1-A5 where the composition was applied was 27.1%; Among them, the corresponding relationship between volunteers and compositions is as follows:

[0033] The test results of skin moisture content (%) of the area on the inner arm where the composition was applied at different times are as follows:

[0034] The present invention adopts a specific method to prepare a composition containing ectoine, that is, powder of leaves of Lamiaceae plants is used as a carrier to load ectoine, specifically, the powder is first dispersed, and then amino groups are introduced through components such as chitosan, so that the surface of the plant carrier contains amino groups, and then it is compounded with ectoine, specifically, ectoine is dispersed to obtain a mixed liquid, and the ectoine is enriched with groups such as hydroxyl groups, and then the pretreated plant carrier and glutathione are added, so that the hydroxyl groups of ectoine can be combined with the pretreated plant carrier and the amino groups of glutathione through intermolecular forces, the firmness is good and the loading is complete, and the stability of the loading is improved. The glutathione can also enhance the skin barrier function, which can improve the skin's resistance for a long time. In the secondary compounding step, the modified aldehyded sodium hyaluronate is introduced, which can cross-link with the amino groups on the surface of the primary complex, thereby improving the stability of the secondary complex. In addition, γ-aminobutyric acid has good skin regeneration and repair functions, which can be firmly combined with the primary complex and has a good long-term effect, thereby achieving a firm combination of ectoine, plant carrier and modified sodium hyaluronate. It is mixed with other ingredients to improve the moisturizing performance of the composition and ensure the sustained-release performance, so that the composition has long-lasting moisturizing and hydrating properties and excellent sustained-release properties.

[0035] Comparative Example 1 directly uses a plant carrier to load ectoine, wherein the plant carrier has poor agglomeration property, and the loading of ectoine in the first compounding step is uneven, which results in uneven compounding of the first compound with modified sodium hyaluronate in the second compounding step, resulting in poor sustained release performance of the product, affecting the long-term moisturizing and hydrating performance; Comparative Example 2 omits the second compounding step, and although the plant carrier loads ectoine, its loading is unstable, affecting the long-term effectiveness of the composition.

[0036] Unless otherwise specified, all ratios and percentages described in the present invention are by mass ratios and percentages are by mass percentages.

[0037] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention is described in detail with reference to the aforementioned embodiments, those skilled in the art can still modify the technical solutions described in the aforementioned embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for preparing a composition containing ectoine, characterized in that: The method comprises the steps of preparing a plant carrier, pretreating the plant carrier, first compounding, second compounding and mixing; The plant carrier pretreatment step comprises placing the plant carrier in an ethanol solution, adding polyethylene glycol 200, stirring at 53-57° C. and 250-260 rpm for 28-32 minutes, adding chitosan solution and sodium cocoyl glycinate and stirring for 37-42 minutes to prepare a pretreated plant carrier; The first compounding step comprises: adding octyldodecanol and disodium lauroamphodiacetate to deionized water, stirring evenly to obtain a mixed solution; placing ectoine in deionized water for ultrasonic dispersion, adding the mixed solution to obtain an ectoine mixed solution; adding the pretreated plant carrier to the ectoine mixed solution, stirring at 38-42° C. and 472-485 rpm for 1.4-1.6 hours, and adding glutathione to obtain a first compound; The secondary compounding step is to place the primary compound in deionized water to obtain a primary compound liquid; mix the primary compound liquid with a modified sodium hyaluronate solution, then add γ-aminobutyric acid and mix evenly, and react in a water bath at 40-44° C. for 5.8-6.2 hours to obtain a secondary compound.

2. A method for preparing a composition containing ectoine according to claim 1, characterized in that, The steps of preparing the plant carrier are as follows: placing the thyme leaf in 8-12 times the mass of deionized water for washing, performing vacuum drying after washing, controlling the drying temperature to be 60-64° C., the vacuum degree to be 0.03-0.05 MPa, and the drying time to be 2.8-3.2 h, and crushing the thyme leaf powder to a particle size of 48-52 μm after drying to obtain the thyme leaf powder; placing the thyme leaf powder in 6-9 times the mass of ethanol solution for stirring, the stirring temperature to be 45-50° C., the stirring time to be 1.8-2.2 h, and performing an ultrasonic extraction after stirring, the extraction time to be 32-37 min, and the ultrasonic power to be 275-2 85W, the ultrasonic frequency is 32-37kHz, after the ultrasonic treatment, the temperature is raised to 58-62°C at a rate of 0.3-0.6°C / min, stirred for 38-42min, and then a secondary ultrasonic extraction is performed, the extraction time is 24-26min, the ultrasonic power is 295-305W, the ultrasonic frequency is 27-32kHz, after the ultrasonic extraction, a mixed solution is obtained; the mixed solution is filtered to obtain a filter residue, the filter residue is vacuum dried at 64-66°C, the drying time is 5.8-6.2h, the vacuum degree is 0.02-0.04MPa, after the vacuum drying is completed, it is crushed to a particle size of 8-12μm to obtain a plant carrier; The volume concentration of the ethanol solution is 68-72%.

3. A method for preparing a composition containing ectoine according to claim 1, characterized in that, In the plant carrier pretreatment step, the mass ratio of the plant carrier, the ethanol solution, the polyethylene glycol 200, the chitosan solution and the sodium cocoyl glycinate is 6.3-6.7:78-82:0.6-0.8:10.6-11.0:0.8-1.2; The mass concentration of the ethanol solution is 24-26%; The chitosan solution is a mixture of chitosan and acetic acid solution, the mass ratio of the chitosan to the acetic acid solution is 2.4-2.6:32-37, and the mass concentration of the acetic acid solution is 18-22wt%.

4. A method for preparing a composition containing ectoine according to claim 1, characterized in that, In the first compounding step, the ultrasonic dispersion has an ultrasonic time of 18-22 min, an ultrasonic power of 107-112 W, and an ultrasonic frequency of 24-26 kHz.

5. A method for preparing a composition containing ectoine according to claim 1, characterized in that, In the first compounding step, the mass ratio of the deionized water, octyldodecanol and disodium lauroamphodiacetate is 98-103:1.4-1.6:1.0-1.3; The mass ratio of ectoine, deionized water and mixed solution 1 is 7.8-8.2:68.0-72.0:34.3-35.0; The mass ratio of the ectoine mixed solution, the pretreated plant carrier and glutathione is 68.0-72.0:5.8-6.2:1.0-1.

2.

6. A method for preparing a composition containing ectoine according to claim 1, characterized in that, In the secondary compounding step, in the primary compounding liquid, the mass ratio of the primary compound to deionized water is 4.8-5.2:58-62; In the modified sodium hyaluronate solution, the mass ratio of modified sodium hyaluronate to deionized water is 4.7-5.3:40-45; The mass ratio of the primary composite liquid, the modified sodium hyaluronate solution and the gamma-aminobutyric acid is 18.2-18.7:27.2-27.7:2.0-2.

3.

7. A method for preparing a composition containing ectoine according to claim 1, characterized in that, The preparation method of the modified sodium hyaluronate is as follows: 9.8-10.2g of sodium hyaluronate is added to 85-90g of deionized water, and after stirring evenly, 3.0-3.4g of sodium periodate is added, and the reaction is carried out in a light-proof condition at a reaction temperature of 20-24°C and a reaction time of 2.8-3.2h. After the reaction is completed, the modified sodium hyaluronate is obtained by filtering, washing and drying.

8. A method for preparing a composition containing ectoine according to claim 7, characterized in that, In the preparation method of the modified sodium hyaluronate, the mass ratio of the sodium hyaluronate, deionized water, and sodium periodate is 9.8-10.2:85-90:3.0-3.

4.

9. A method for preparing a composition containing ectoine according to claim 1, characterized in that, The mixing step comprises adding the secondary complex and Tween 20 to deionized water, stirring evenly, adding sorbitol, camellia oil, gum arabic, and niacinamide, stirring evenly, and performing homogenization, wherein the homogenization time is 4.8-5.2 minutes, the homogenization pressure is 2.6-3.0 MPa, the homogenization times are 3 times, and after the homogenization is completed, a composition containing ectoine is obtained; The mass ratio of the deionized water, the secondary complex, Tween 20, sorbitol, camellia oil, gum arabic and nicotinamide is 90-94:8.5-9.0:2.4-2.6:0.8-1.2:0.40-0.44:0.73-0.77:0.54-0.56.

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