Preparation method of beautiful millettia root polysaccharide and application of beautiful millettia root polysaccharide in skin care cream

Abstract

The invention discloses a preparation method of beautiful millettia root polysaccharide and application of the beautiful millettia root polysaccharide in skin care cream. The preparation method comprises the following steps: (1) firstly, drying beautiful millettia roots in the sun, crushing and sieving to obtain beautiful millettia root powder; (2) extracting the beautiful millettia root powder obtained in the step (1) by adopting a hot water extraction method; (3) performing rotary evaporation concentration, ethanol precipitation, macroporous resin AB-8 decoloration, Sevag reagent deproteinization, 3500Da dialysis and vacuum freeze drying on the beautiful millettia root water extract obtained in the step (2) to obtain beautiful millettia root polysaccharide MSCP; (4) performing sulfation modification on the water-soluble beautiful millettia root polysaccharide MSCP obtained in the step (3) to obtain sulfated beautiful millettia root polysaccharide SMSCP; and (5) compounding the sulfated beautiful millettia root polysaccharide SMSCP obtained in the step (4) with an emulsifier, a humectant, a preservative and deionized water, and preparing the skin-care cream according to the steps of oil phase and water phase preparation, emulsification and homogenization. The dispersibility of the modified polysaccharide in a water phase and an oil phase is greatly improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of polysaccharide modification and cosmetics, and in particular to a preparation method of Bauhinia championii polysaccharide and application thereof in skin care cream. BACKGROUND

[0002] Bauhinia championii, as a traditional medicine and food homologous plant, is widely distributed in southern China. Bauhinia championii water-soluble polysaccharide is one of the main active ingredients, which has good biological activity, including antioxidant, anti-inflammatory, immune regulation and other activities.

[0003] In terms of antioxidant stress, it can effectively remove excess free radicals in the body and slow down the process of cell aging. In the field of immune regulation, it can activate multiple links of the body's immune system and enhance the body's ability to resist external pathogen invasion. However, the molecular structure of Bauhinia championii polysaccharide in the natural state presents a high hydrophilicity, which greatly limits its application in many fields such as cosmetics and food that require high stability of oil-water phase. Therefore, it is necessary to modify the hydrophobicity of Bauhinia championii polysaccharide.

[0004] Polysaccharide sulfation modification is an important research direction of polysaccharide functionalization modification. This modification strategy can not only effectively improve the amphiphilic characteristics of polysaccharide molecules, but also significantly enhance their biological activity. However, the widely used sulfation modification system such as sulfur trioxide-pyridine method can realize the grafting of sulfate groups on polysaccharide molecules, but this system has process defects such as high sensitivity of reagents to water and harsh reaction conditions. Based on this, a new sulfation modification strategy with high efficiency and functional synergy effect is established. SUMMARY

[0005] The purpose of the present application is to provide a preparation method of Bauhinia championii polysaccharide, which modifies its molecular groups, changes Bauhinia championii polysaccharide from a hydrophilic molecule to an amphiphilic molecule with both hydrophilic and hydrophobic characteristics, thereby improving its emulsifying capacity and stabilizing oil-water phase to prepare oil-in-water emulsion.

[0006] Another purpose of the present application is to provide a skin care cream containing modified Bauhinia championii polysaccharide emulsion, which utilizes the emulsifying and stabilizing performance of modified Bauhinia championii polysaccharide to enhance the encapsulation of oily active substances with skin care efficacy, while synergistically exerting the anti-inflammatory, antioxidant and other advantages of Bauhinia championii polysaccharide. In addition, sulfation modification can further enhance the anti-inflammatory activity of polysaccharide, which is beneficial to skin soothing and repair.

[0007] To achieve the above purpose, the technical scheme adopted by the present application is as follows:

[0008] A preparation method of Bauhinia championii polysaccharide, the specific steps are as follows:

[0009] (1) Extraction of polysaccharides from Millettia pachynema Benth: The roots of Millettia pachynema Benth are cleaned, dried, and then crushed to an appropriate size and passed through a 60-100 mesh sieve. Water-soluble polysaccharides are extracted by water extraction and alcohol precipitation. Then, the polysaccharides are decolorized by AB-8 macroporous resin, deproteinated by the Sevag method, dialyzed at 3500 Da, and vacuum freeze-dried to obtain the polysaccharides from Millettia pachynema Benth. The purity of the reaction system is ensured to prevent moisture from interfering with the sulfation reaction.

[0010] (2) Preparation of polysaccharide solution from Millettia pachynema Benth: The dried polysaccharides from Millettia pachynema Benth are slowly added to anhydrous DMSO, and a polysaccharide solution with a mass-volume ratio of 20%-30% is prepared under stirring at a speed of 180-220 r / min for 30-40 min to ensure that the polysaccharides are fully dissolved to form a uniform solution.

[0011] (3) Sulfation modification

[0012] Under the protection of a nitrogen atmosphere, sulfur trioxide and sulfur trioxide-trimethylamine complex are slowly added in the order of polysaccharide: SO3: SO3-TMA = 1:2-3:1-2 (molar ratio). The addition rate of sulfur trioxide is controlled at 0.5-0.7 mL per minute, and the addition rate of sulfur trioxide-trimethylamine complex is controlled at 0.3-0.5 mL per minute to avoid excessive reaction and side reactions. A temperature control device is used to stabilize the reaction temperature at 40-50°C, and the reaction is continuously stirred at a speed of 200-280 r / min for 12-16 h to promote the reaction of the polysaccharides with the two sulfation reagents, gradually introduce sulfonic acid groups to achieve sulfation, and optimize the amphiphilicity.

[0013] After the above reaction is completed, dodecyl mercaptan is slowly added to the reaction system, and the addition amount is controlled according to the mass ratio of polysaccharide to dodecyl mercaptan of 10:1-2. The addition process is carried out under continuous stirring, and the addition rate is controlled at 0.2-0.4 mL per minute to ensure that the dodecyl mercaptan is uniformly dispersed and fully interacts with the sulfated polysaccharides, and the lipophilicity of the dodecyl mercaptan is used to further strengthen the amphiphilicity.

[0014] (4) Reaction termination and post-treatment

[0015] After the reaction is completed, the reaction solution is quickly poured into a large amount of ice water to rapidly cool and terminate the reaction, preventing excessive reaction and degradation of the polysaccharides. A 5%-10% sodium bicarbonate solution is used to adjust the pH of the reaction solution to 7-8 to neutralize excess acidic substances. Then, dialysis, freeze-drying, and other conventional methods are used for separation and purification to obtain sulfated modified polysaccharides from Millettia pachynema Benth with optimized performance, which can be used for subsequent product development such as skin cream.

[0016] The application also protects the use of the polysaccharides from Millettia pachynema Benth prepared by the above method in skin cream.

[0017] A method for preparing a skin cream containing sulfated modified Bauhinia Purpurea polysaccharide emulsion, the specific steps are as follows:

[0018] (1) The formula of the skin cream

[0019] The modified Bauhinia Purpurea polysaccharide prepared by the aforementioned method: 5% to 10% (mass percentage, the same below). As the core active ingredient, the modified Bauhinia Purpurea polysaccharide not only has good amphiphilicity, which helps to stabilize the cream system, but also can interact with skin cells in multiple ways due to its unique chemical structure, such as enhancing skin moisture retention and regulating skin inflammatory response.

[0020] Plant oils: 10% to 20%, choose high-quality plant oils such as olive oil and avocado oil. These plant oils are rich in unsaturated fatty acids and vitamins, which can nourish the skin and form a natural protective film on the skin surface, preventing water loss and providing nutrients to the skin to promote skin metabolism.

[0021] Emulsifier: 3% to 6%, using cetyl stearyl alcohol and polysorbate-60. The oil phase and water phase can be uniformly mixed to form a stable cream system, ensuring that each component is evenly distributed in the cream, improving the stability and effectiveness of the product.

[0022] Moisturizing agent: 8% to 15%, including glycerol and sodium hyaluronate. Moisturizing agents can absorb and lock in moisture, working synergistically with modified Bauhinia Purpurea polysaccharide to further enhance skin moisture retention, keeping the skin hydrated for a long time. For example, sodium hyaluronate can absorb thousands of times its own weight of water, forming a moist film on the skin surface.

[0023] Preservative: 0.5% to 1%, such as phenoxyethanol and methylparaben. Preservatives can inhibit the growth and reproduction of microorganisms, prolong the shelf life of the product, and ensure the safety of the skin cream during storage and use.

[0024] Deionized water: the rest, as a solvent, provides a uniform dispersion medium for each component, making the cream have appropriate texture and flowability.

[0025] (2) The preparation method of the skin cream

[0026] Oil phase preparation: Mix the plant oils and emulsifiers, heat to 70-80°C, and mix thoroughly at a stirring speed of 180-220 rpm / min to form a stable oil phase system.

[0027] Water phase preparation: Dissolve the modified Bauhinia Purpurea polysaccharide, moisturizing agent, and preservative in deionized water, also heat to 70-80°C, and stir at a speed of 200-250 r / min to ensure complete dissolution of each component and form a uniform water phase.

[0028] Emulsification homogenization: under the condition of continuous stirring, the water phase is slowly added into the oil phase, and the adding speed is controlled at 2-3 mL per minute. Then, the emulsification homogenization equipment is used to emulsify and homogenize the oil phase and the water phase at a speed of 2500-3000 rpm / min for 5-10 min, so as to fully emulsify the oil phase and the water phase and form a skin cream with fine and uniform texture. Finally, the cream is cooled to room temperature and packaged for storage.

[0029] Compared with the prior art, the present application has the following advantages and beneficial effects:

[0030] (1) The present application adopts the sulfur trioxide-dimethyl sulfoxide (SO3-DMSO) method, and introduces sulfur trioxide-trimethylamine and dodecyl mercaptan for synergistic modification, realizing the optimization of amphiphilicity. The dispersion of the modified polysaccharide in the water phase and the oil phase is greatly improved, which can be uniformly distributed in the skin cream system, ensuring the stability and uniformity of the product quality.

[0031] (2) The modified polysaccharide from Millettia pachycarpa has obvious synergistic effect. In the skin cream, the modified polysaccharide from Millettia pachycarpa synergizes with other ingredients to significantly improve the comprehensive performance of the product. In terms of anti-inflammatory, it can effectively reduce the inflammatory reaction of the skin and improve the problems of skin sensitivity and redness; in terms of promoting skin metabolism, it synergizes with plant oils to enhance the luster and elasticity of the skin.

[0032] (3) High safety: the raw materials and modification methods used in the present application are relatively mild, which do not introduce harmful impurities while ensuring the activity of polysaccharide. Through safety test, the skin cream has no irritation and no allergic reaction, which meets the safety standards of cosmetics and is suitable for people of all skin types.

[0033] (4) The process of the present application is simple and easy to industrialize: compared with the traditional polysaccharide modification method, the modification process of the present application is relatively simple, the reaction conditions are easy to control, the raw materials are widely available, and the cost is controllable, which has good industrial application prospect and can provide strong support for large-scale production of high-performance skin care products. DETAILED DESCRIPTION

[0034] The technical solutions in the embodiments of the present application will be described below in conjunction with the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the present application.

[0035] A preparation method of polysaccharide from Millettia pachycarpa, the specific steps are as follows:

[0036] (1) Extraction of polysaccharides from Millettia pachynema Benth: The roots of Millettia pachynema Benth are cleaned, dried, and then crushed to an appropriate size and passed through a 60-100 mesh sieve. Water-soluble polysaccharides are extracted by water extraction and alcohol precipitation. Then, the polysaccharides are decolorized by AB-8 macroporous resin, deproteinated by the Sevag method, dialyzed at 3500 Da, and vacuum freeze-dried to obtain the polysaccharides from Millettia pachynema Benth. The purity of the reaction system is ensured to prevent moisture from interfering with the sulfation reaction.

[0037] (2) Preparation of polysaccharide solution from Millettia pachynema Benth: The dried polysaccharides from Millettia pachynema Benth are slowly added to anhydrous DMSO, and a polysaccharide solution with a mass-volume ratio of 20%-30% is prepared under stirring at a speed of 180-220 r / min for 30-40 min to ensure that the polysaccharides are fully dissolved to form a uniform solution.

[0038] (3) Sulfation modification

[0039] Under the protection of a nitrogen atmosphere, sulfur trioxide and sulfur trioxide-trimethylamine complex are slowly added in the order of polysaccharide: SO3: SO3-TMA = 1:2-3:1-2 (molar ratio). The addition rate of sulfur trioxide is controlled at 0.5-0.7 mL per minute, and the addition rate of sulfur trioxide-trimethylamine complex is controlled at 0.3-0.5 mL per minute to avoid excessive reaction and side reactions. A temperature control device is used to stabilize the reaction temperature at 40-50°C, and the reaction is continuously stirred at a speed of 200-280 r / min for 12-16 h to promote the reaction of the polysaccharides with the two sulfation reagents, gradually introduce sulfonic acid groups to achieve sulfation, and optimize the amphiphilicity.

[0040] After the above reaction is completed, dodecyl mercaptan is slowly added to the reaction system, and the addition amount is controlled according to the mass ratio of polysaccharide to dodecyl mercaptan of 10:1-2. The addition process is carried out under continuous stirring, and the addition rate is controlled at 0.2-0.4 mL per minute to ensure that the dodecyl mercaptan is uniformly dispersed and fully interacts with the sulfated polysaccharides, thereby further strengthening the amphiphilicity by the lipophilicity of dodecyl mercaptan.

[0041] (4) Reaction termination and post-treatment

[0042] After the reaction is completed, the reaction solution is quickly poured into a large amount of ice water to rapidly cool and terminate the reaction, preventing excessive reaction and degradation of the polysaccharides. A 5%-10% sodium bicarbonate solution is used to adjust the pH of the reaction solution to 7-8 to neutralize excess acidic substances. Then, dialysis, freeze-drying, and other conventional methods are used for separation and purification to obtain sulfated modified polysaccharides from Millettia pachynema Benth with optimized performance, which can be used for subsequent product development such as skin cream.

[0043] The application also protects the use of the polysaccharides from Millettia pachynema Benth prepared by the above method in skin cream.

[0044] A method for preparing a skin cream containing sulfated modified Bauhinia Purpurea polysaccharide emulsion, the specific steps are as follows:

[0045] (2) Skin cream formula

[0046] The modified Bauhinia Purpurea polysaccharide prepared by the aforementioned method: 5% to 10% (mass percentage, the same below). As the core active ingredient, the modified Bauhinia Purpurea polysaccharide not only has good amphiphilicity, which helps to stabilize the cream system, but also can interact with skin cells in multiple ways due to its unique chemical structure, such as enhancing skin moisture retention and regulating skin inflammatory response.

[0047] Plant oil: 10% to 20%, choose high-quality plant oils such as olive oil and avocado oil. These plant oils are rich in unsaturated fatty acids and vitamins, which can nourish the skin and form a natural protective film on the skin surface, preventing water loss and providing nutrients to the skin to promote skin metabolism.

[0048] Emulsifier: 3% to 6%, using cetyl stearyl alcohol and polysorbate-60. The oil phase and water phase can be uniformly mixed to form a stable cream system, ensuring that each component is evenly distributed in the cream, improving the stability and effectiveness of the product.

[0049] Moisturizer: 8% to 15%, including glycerol and sodium hyaluronate. Moisturizers can absorb and lock in moisture, working synergistically with modified Bauhinia Purpurea polysaccharide to further enhance skin moisture retention, keeping the skin hydrated for a long time. For example, sodium hyaluronate can absorb thousands of times its own weight of water, forming a moist film on the skin surface.

[0050] Preservative: 0.5% to 1%, such as phenoxyethanol and methylparaben. Preservatives can inhibit the growth and reproduction of microorganisms, prolong the shelf life of the product, and ensure the safety of the skin cream during storage and use.

[0051] Deionized water: the rest, as a solvent, provides a uniform dispersion medium for each component, making the cream have appropriate texture and flowability.

[0052] (2) Skin cream preparation method

[0053] Oil phase preparation: Mix the plant oil and emulsifier, heat to 70-80°C, and mix thoroughly at a stirring speed of 180-220 rpm / min to form a stable oil phase system.

[0054] Water phase preparation: Dissolve the modified Bauhinia Purpurea polysaccharide, moisturizer, and preservative in deionized water, also heat to 70-80°C, and stir at a speed of 200-250 r / min to ensure complete dissolution of each component and form a uniform water phase.

[0055] Emulsification homogenization: under the condition of continuous stirring, the water phase is slowly added into the oil phase, and the adding speed is controlled at 2-3 mL per minute. Subsequently, the emulsification homogenization equipment is used to emulsify and homogenize for 5-10 minutes at a speed of 2500-3000 rpm / min, so that the oil phase and the water phase are fully emulsified to form a skin cream with fine and uniform texture. Finally, the cream is cooled to room temperature and packaged for storage.

[0056] Example 1: Preparation and sulfation modification of Millettia pachynema polysaccharide

[0057] 1. Preparation of Millettia pachynema polysaccharide

[0058] (1) Raw material pretreatment: The dried Millettia pachynema is crushed and sieved to prepare Millettia pachynema powder. The sieve is 60 mesh.

[0059] (2) Hot water extraction: The Millettia pachynema powder is mixed with deionized water at a mass-volume ratio of 1:20, continuously stirred at 100°C for 2 hours to ensure that the polysaccharide is fully dissolved. Filter the filtrate. Repeat 3 times.

[0060] (3) Concentration: Use a rotary evaporation instrument to concentrate the Millettia pachynema water extract at 60°C. The concentration volume is 1 / 10 of the original volume, thereby reducing the subsequent ethanol consumption.

[0061] (4) Alcohol precipitation: Add anhydrous ethanol to the filtrate slowly, control the final ethanol concentration at 70%, and stand at 4°C for 18 hours to precipitate the polysaccharide. Use a high-speed refrigerated centrifuge to collect the precipitate at a speed of 8000 r / min.

[0062] (5) Polysaccharide redissolution: Add 10 times the volume of water to the polysaccharide precipitate, and heat and stir at 60°C for 60 minutes to obtain a polysaccharide solution.

[0063] (6) Decolorization: Use AB-8 macroporous resin to decolorize the polysaccharide solution. Mix the macroporous resin AB-8 with the concentrated solution at a volume ratio of 1:1, stir at 55°C for 3 hours for decolorization. After decolorization is completed, remove the resin by filtration.

[0064] (7) Protein removal by Sevag method: Add 1 / 4 volume of Sevag reagent to the decolorized polysaccharide solution, where the Sevag reagent is prepared by mixing chloroform and n-butanol at a volume ratio of 5:1. Then shake well at room temperature for 30 minutes, and then centrifuge at 8000 rpm for 3 minutes, and keep the uppermost layer of the polysaccharide solution. Repeat the protein removal operation 3 times.

[0065] (8) Removal of organic reagents by rotary evaporation: After the polysaccharide solution is completed, concentrate it to 1 / 5 of the original volume at 60°C to remove chloroform and n-butanol.

[0066] (9) Dialysis: 3500 Da dialysis to remove small molecular impurities and pigments.

[0067] (10) Freeze-drying: The solution of B. mori polysaccharide was pre-frozen at -80°C for 6 h, and then vacuum freeze-dried for 36 h. The freeze-dried product was B. mori polysaccharide.

[0068] 2. Sulfated modification of B. mori polysaccharide

[0069] (1) 10 g of B. mori polysaccharide was dissolved in 50 mL of anhydrous DMSO to prepare a 20% (mass / volume) polysaccharide solution.

[0070] (2) Under nitrogen protection, sulfur trioxide and sulfur trioxide-trimethylamine complex were slowly added in the ratio of polysaccharide: SO3: SO3-TMA = 1:2 (molar ratio). When adding sulfur trioxide, the rate was controlled at 0.5 mL per minute; when adding sulfur trioxide-trimethylamine complex, the rate was 0.3 mL per minute to avoid excessive reaction and side reactions.

[0071] (3) The reaction temperature was stabilized at 40°C using a temperature control device, and the reaction was continuously stirred at 200 r / min for 12 h to promote the reaction of polysaccharide with the two sulfating reagents, gradually introducing sulfonic acid groups to achieve sulfation and optimize the amphiphilicity.

[0072] (4) Slowly add dodecyl mercaptan to the reaction system, with the dropwise addition amount being in the ratio of 5:1 of polysaccharide to dodecyl mercaptan. The dropwise addition process was carried out under continuous stirring, with the rate being controlled at 0.2 mL per minute to ensure uniform dispersion of dodecyl mercaptan and its full interaction with the sulfated polysaccharide molecules, further strengthening the amphiphilicity by its lipophilicity.

[0073] (5) Adjust the pH of the reaction solution to 7 using 5% sodium bicarbonate solution to neutralize excess acidic substances.

[0074] (6) Ultrafiltration: The neutralized solution was first subjected to ultrafiltration using an ultrafiltration membrane with a molecular weight cutoff of 10000 Da to remove large molecular impurities, and the permeate was collected.

[0075] (7) Dialysis: The permeate was placed in a dialysis bag with a molecular weight cutoff of 3500 Da and dialyzed in deionized water for 3 days, with the dialysis solution being changed daily to remove unreacted reagents and small molecular impurities.

[0076] (8) Vacuum freeze-drying: The dialyzed solution was concentrated under reduced pressure, and the sulfated polysaccharide SMSCP was obtained by vacuum freeze-drying.

[0077] Example 2: Preparation of a skin cream containing sulfated B. mori polysaccharide emulsion

[0078] 1. Preparation of raw materials for skin cream

[0079] (1) Sulfated polysaccharide from the roots of Asparagus officinalis L. : prepared by the modification method of Example 1, 7 g (7% by mass) was accurately weighed. Ensure that the polysaccharide remains dry during storage to avoid moisture affecting its performance.

[0080] (2) Vegetable oil: 15 g of high-quality olive oil was selected, which is rich in monounsaturated fatty acids such as oleic acid, which can effectively moisturize the skin and enhance the skin barrier function; at the same time, 3 g of avocado oil was prepared, which is rich in nutrients such as vitamin E, potassium, and magnesium, further enhancing the skin nourishing effect.

[0081] (3) Emulsifier: 4 g of cetylstearyl alcohol and 1 g of polysorbate-60 were weighed, which synergistically work together, cetylstearyl alcohol can provide good emulsion stability, and polysorbate-60 can help enhance the fusion effect of the oil phase and the water phase, ensuring that the emulsion texture is fine and uniform.

[0082] (4) Humectant: 10 g of glycerol was measured, which has strong hygroscopicity and can absorb moisture from the air and retain it on the skin surface; then 3 g of sodium hyaluronate was added, the total amount of the two is 13 g, which synergistically enhances the skin's ability to retain moisture.

[0083] (5) Preservative: 0.7 g of phenoxyethanol was accurately weighed, which effectively inhibits microbial growth, prolongs the shelf life of the cream, and ensures the safety of the product during the use period.

[0084] (6) Deionized water: according to the total amount of the above ingredients, make up the rest to 100 g, as a solvent medium for uniform dispersion of each ingredient, to ensure that the cream has appropriate texture and good flowability.

[0085] 2. Preparation process of skin care cream

[0086] (1) Oil phase preparation

[0087] The prepared 15 g of olive oil and 3 g of avocado oil were poured into a clean stainless steel container, 4 g of cetylstearyl alcohol and 1 g of polysorbate-60 were added. The container was placed in a constant temperature water bath, slowly heated to 75°C, and stirred at a speed of 200 r / min at the same time, so that the ingredients were fully mixed and uniform, forming a stable oil phase system, ensuring the uniformity of the oil phase, and preparing for the subsequent emulsification.

[0088] (2) Water phase preparation

[0089] In another suitable container, 7 g of sulfated polysaccharide from the roots of Asparagus officinalis L., 10 g of glycerol, 3 g of sodium hyaluronate, and 0.7 g of phenoxyethanol were added, and the calculated deionized water (about 72.3 g) was slowly poured. Similarly, the container was placed in a constant temperature water bath, heated to 75°C, and stirred at a speed of 170 r / min until all the solid ingredients were completely dissolved, forming a uniform water phase, ensuring that the functional ingredients in the water phase are uniformly dispersed.

[0090] (3) Emulsification homogenization

[0091] Under the condition of continuous stirring (the stirring speed is kept at 200 r / min), the water phase is slowly added to the oil phase using a constant flow pump, and the dropping speed is controlled at 2.5 mL per minute to ensure that the emulsification process is smooth. After the water phase is added, the mixture is immediately transferred to a high-speed emulsification homogenizer, and homogenized at a speed of 2800 r / min for 8 minutes to fully emulsify the oil phase and the water phase, forming a skin cream emulsion with fine and uniform texture.

[0092] (4) Cooling and packaging

[0093] The emulsified and homogenized cream emulsion is quickly transferred to a cooling device and slowly cooled to room temperature, and appropriate stirring can be performed during the process to prevent local overheating or overcooling, which may cause uneven cream. After the cream is cooled to room temperature, sterile packaging materials are used for packaging to ensure that the product is not contaminated during storage and use, and maintains good quality.

[0094] Emulsification performance test:

[0095] The sulfated polysaccharide SMSCP prepared in Example 1 is mixed with vegetable oil at a mass ratio of 1:5, and ultrasonic emulsification treatment is performed to obtain an emulsion. The power of ultrasonic emulsification is 300 W, and the time is 5 minutes. The stability of the prepared emulsion is tested:

[0096] The centrifugal stability of the prepared emulsion is tested, and the volume ratio of the upper cream layer is measured after centrifugation at 3000 r / min for 30 minutes.

[0097] The storage stability of the prepared emulsion is also tested: it is placed at 25℃ for 30 days, and the layering condition is observed and the particle size change is measured.

[0098] Emulsification performance test results:

[0099] The average particle size of the emulsion of the sulfated polysaccharide SMSCP is 260 nm; the stability: after storage at 25℃ for 30 days, the volume ratio of the cream layer is 4%.

[0100] The test results show that the average particle size of the emulsion of the sulfated polysaccharide SMSCP is small, the emulsification performance is good, and the stability is high.

[0101] The present application has the following beneficial effects:

[0102] (1) The present application adopts the sulfur trioxide-dimethyl sulfoxide (SO3-DMSO) method, and introduces sulfur trioxide-trimethylamine and dodecyl mercaptan for synergistic modification, realizing the optimization of amphiphilicity. The dispersibility of the modified polysaccharide in the water phase and the oil phase is greatly improved, and it can be uniformly distributed in the skin cream system, ensuring the stability and uniformity of the product quality.

[0103] (2) Modified Aescin has obvious synergistic effect. In skin care cream, modified Aescin has synergistic effect with other ingredients, which significantly improves the comprehensive performance of the product. In terms of anti-inflammatory, it can effectively reduce skin inflammatory reaction and improve skin sensitivity, redness and other problems. In terms of promoting skin metabolism, it can enhance the luster and elasticity of the skin in cooperation with plant oils.

[0104] (3) High safety: The raw materials and modification methods used in the application are relatively mild, which can ensure the activity of polysaccharide without introducing harmful impurities. Through safety test, the skin care cream has no irritation and no allergic reaction, which meets the safety standards of cosmetics and is suitable for people with various skin types.

[0105] (4) The process of the application is simple and easy to industrialize: Compared with the traditional polysaccharide modification method, the modification process of the application is relatively simple, the reaction conditions are easy to control, the raw materials are widely available, the cost is controllable, and it has good industrial application prospect, which can provide strong support for large-scale production of high-performance skin care products.

[0106] It should be further noted that the terms "comprising", "including", or any other variant thereof are intended to cover non-exclusive inclusion, so that processes, methods, articles or devices including a series of elements not only include those elements, but also include other elements not explicitly listed, or inherent to such processes, methods, articles or devices. Without more limitations, the element defined by the statement "including a" does not exclude the presence of additional identical elements in the process, method, article or device including the element.

Claims

1. A method for preparing *Smilax glabra* polysaccharide, characterized in that, The preparation method includes the following steps: (1) Niu Dali is first dried, crushed and sieved to obtain Niu Dali powder; (2) The powder obtained in step (1) is extracted by hot water extraction. (3) The water extract of *Smilax glabra* obtained in step (2) was concentrated by rotary evaporation, precipitated with ethanol, decolorized with macroporous resin AB-8, deproteinized with Sevag reagent, dialyzed at 3500 Da and freeze-dried under vacuum to obtain *Smilax glabra* polysaccharide MSCP. (4) The water-soluble polysaccharide MSCP obtained in step (3) is modified by sulfation to obtain sulfated polysaccharide SMSCP. (5) The sulfated SMSCP obtained in step (4) is compounded with emulsifier, moisturizer, preservative and deionized water, and the cream is prepared by oil phase, water phase preparation and emulsification homogenization steps to obtain the skin care cream.

2. The method for preparing *Achyranthes bidentata* polysaccharide according to claim 1, characterized in that, In step (1) of crushing and sieving, the particle size of the Niu Dali powder is measured.

3. The method for preparing *Achyranthes bidentata* polysaccharide according to claim 1, characterized in that, In step (2) hot water extraction, the powder of *Smilax glabra* is mixed with deionized water at a mass-volume ratio of 1:20 to 1:25 and stirred at high speed at 80 to 100°C for 2 to 3 hours to ensure that the polysaccharides are fully dissolved. The mixture is then filtered and the filtrate is collected. This process is repeated 3 times.

4. The method for preparing *Achyranthes bidentata* polysaccharide according to claim 1, characterized in that, In step (3) concentration, the concentrate is 1 / 10 to 1 / 5 of the volume of the water extract; In step (3) ethanol precipitation, the volume ratio of the ethanol solution to the polysaccharide concentrate after protein removal is 4:1; the alcohol is 95% ethanol. In step (3) decolorization with macroporous resin AB-8, the volume ratio of macroporous resin AB-8 to polysaccharide solution is 1:

1. In step (3) deproteinization, the Sevag reagent is chloroform to n-butanol in a volume ratio of 4:1, the shaking time is 30-40 min, and the deproteinization is performed 3-5 times. In step (3) dialysis, a 3500Da dialysis bag is used to remove small molecule impurities; In step (3), the freeze-drying time is 36 to 48 hours.

5. The method for preparing *Achyranthes bidentata* polysaccharide according to claim 1, characterized in that, In step (4), the sulfur trioxide-dimethyl sulfoxide (SO3-DMSO) method is used, and sulfur trioxide derivatives and long-chain sulfides are introduced for synergistic modification. The specific steps include: In step (4) sulfation modification, during the solution preparation process, 10-15g of *Euphorbia lathyris* polysaccharide is dissolved in 50mL of anhydrous DMSO to prepare a polysaccharide solution with a mass-volume ratio of 20%-30%. In step (4) sulfation modification, during the reaction process, under nitrogen protection, SO3-DMSO complex is slowly added at a ratio of polysaccharide:SO3 = 1:3 to 1:5 (molar ratio), the reaction temperature is maintained at 40 to 50°C, and the reaction is continuously stirred at a speed of 220 to 280 r / min for 12 to 16 h. In step (4) sulfation modification, under continuous stirring, sulfur trioxide-trimethylamine is slowly added at a rate of 0.3-0.5 mL per minute, according to a molar ratio of polysaccharide to sulfur trioxide-trimethylamine complex of 1:1-2. During the addition process, the reaction temperature is maintained at 40-50℃, and the reaction is continued with stirring for 3-5 hours. In step (4) sulfation modification, long-chain sulfide dodecyl mercaptan is slowly added dropwise to the reaction system. The amount added is based on a mass ratio of polysaccharide to long-chain sulfide of 10:1 to 2. The dropping rate is controlled at 0.2 to 0.4 mL per minute. The mixture is stirred continuously at 40 to 50 °C for 1 to 2 hours to allow it to fully interact with the sulfated polysaccharide molecules and enhance the amphiphilicity of the modified polysaccharide by utilizing its lipophilicity. In step (4) sulfation modification, after the reaction is completed, the reaction solution is poured into ice water and the pH is adjusted to 7-8 with sodium bicarbonate solution; In step (4) post-sulfation modification, the neutralized solution is first ultrafiltered with an ultrafiltration membrane with a molecular weight cutoff of 10000 Da to remove macromolecular impurities and collect the permeate. In step (4) of the post-sulfation modification process, the permeate is placed into a dialysis bag with a molecular weight cutoff of 3500 Da and dialyzed in deionized water for 3 to 5 days. The dialysis solution is changed daily to remove unreacted reagents and small molecule impurities.

6. The application of *Smilax glabra* polysaccharide prepared by the method described in any one of claims 1-5 in skin care creams.

7. A skin care cream, characterized in that, The skin cream comprises the following components by weight percentage: The polysaccharide prepared by the method of any one of claims 1-5 is 5% to 10% of *Smilax glabra* polysaccharide. Vegetable oil: 10%–20%; Emulsifier: 3%–6%; Moisturizer: 8%–15%; Preservatives: 0.5%–1%; Deionized water: Balance.

8. A skin care cream according to claim 7, characterized in that, The vegetable oil is selected from olive oil or avocado oil.

9. A skin care cream according to claim 7, characterized in that, The emulsifier is selected from cetearyl alcohol or polysorbate-60.

10. A skin care cream according to claim 7, characterized in that, The moisturizer is glycerin or sodium hyaluronate; the preservative is phenoxyethanol or methylparaben.