Preparation method of high-efficiency stable mulberry root extract containing oxyresveratrol and application thereof in relieving skin itching
Oxidized resveratrol was extracted from mulberry roots using an ultrasound-assisted eutectic solvent method, which solved the problems of difficult extraction and poor stability of oxidized resveratrol, achieving efficient extraction and improved stability. It is suitable for cosmetics, has a long-lasting inhibitory effect on itch receptors, and is suitable for sensitive skin.
Patent Information
- Application Number
- CN202510356978.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-25
- Publication Date
- 2025-11-25
- Estimated Expiration
- 2045-03-25
AI Technical Summary
Oxidized resveratrol faces challenges in practical applications, including difficult extraction, poor stability, poor water solubility, and low transdermal efficiency. Traditional methods suffer from low efficiency, high cost, and unpleasant skin feel, limiting its application in cosmetics and pharmaceutical preparations.
An ultrasound-assisted eutectic solvent method was employed, using a green solvent system composed of betaine and 1,3-propanediol/ethyl lactate, combined with mild ultrasonic conditions, to extract oxidized resveratrol from mulberry roots. The strong hydrogen bonding of the eutectic solvent enhanced solubility and stability, while the ultrasonic cavitation effect promoted cell wall rupture, improving the extraction rate and avoiding high-temperature oxidation.
This method achieves efficient extraction of oxidized resveratrol, enhancing its application in cosmetics. It also provides long-lasting inhibition of the itch receptor MRGPX1, making it suitable for sensitive skin. It is highly effective and biocompatible, overcoming the environmental pollution and technical bottlenecks of traditional methods.
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Figure CN120168348B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of cosmetics, in particular to a preparation method of a mulberry root extract containing oxyresveratrol with high efficiency and stability and application thereof in relieving skin itching. BACKGROUND
[0002] Oxyresveratrol is a natural derivative of resveratrol, which can be extracted from the bark and roots of mulberry, has multiple biological activities, and is a natural polyphenol compound with strong antioxidant, anti-inflammatory and tyrosinase enzyme activity. It can exhibit wide application potential in the fields of medicine, cosmetics and food through mechanisms such as free radical scavenging, regulation of inflammatory signaling pathways and blockage of melanin production.
[0003] However, oxyresveratrol faces multiple challenges in practical application. First, the natural extraction of the component is difficult, mainly relying on limited sources such as Moraceae plants, and the traditional extraction process is low in efficiency and high in cost. Second, its chemical properties are extremely unstable, and it is easily affected by light, heat, oxygen and acid-base environment, leading to degradation and loss of activity. In addition, the problems of poor water solubility (almost insoluble in water) and low transdermal efficiency also seriously limit the application effect of the component in cosmetics and pharmaceutical preparations. The conventional solution such as spray drying embedding technology can partially improve the stability, but it has defects such as low encapsulation rate, insufficient loading rate and complex process, and the polysaccharide wall material easily leads to poor skin feel.
[0004] In summary, it is urgent to develop a preparation method of oxyresveratrol with high extraction rate and high stability to meet the high market demand for oxyresveratrol. SUMMARY
[0005] The present application aims to overcome the deficiencies of the prior art and provide a preparation method of a mulberry root extract containing oxyresveratrol with high efficiency and stability and application thereof in relieving skin itching. In the present application, an ultrasonic-assisted low eutectic solvent method is used, a green solvent system composed of betaine and 1,3-propanediol / ethyl lactate is used as the basis, and mild ultrasonic conditions are combined to realize the efficient extraction of oxyresveratrol from mulberry roots. The technology enhances the solubility and stability of the target component through the strong hydrogen bonding of the low eutectic solvent, and the ultrasonic cavitation effect promotes cell wall rupture, which improves the extraction rate and avoids the risk of high temperature oxidation. The obtained extract not only can long-term inhibit the itch receptor MRGPX1, but also is suitable for sensitive skin due to the removal of irritating ingredients, and has high efficiency and biocompatibility, breaking through the environmental pollution and technical bottlenecks of traditional methods.
[0006] To achieve the above-mentioned purposes, the technical scheme adopted by the present application is as follows:
[0007] In a first aspect, the present application provides a preparation method of a mulberry root extract containing oxidized trans-resveratrol, comprising the following steps:
[0008] After the dried and crushed root of mulberry is added into an aqueous solution of a deep eutectic solvent for ultrasonic extraction, the product is collected after centrifugation, and the supernatant is obtained, thereby obtaining the mulberry root extract containing oxidized trans-resveratrol.
[0009] The aqueous solution of the deep eutectic solvent is composed of a hydrogen bond acceptor, a hydrogen bond donor and water; the hydrogen bond acceptor includes at least one of betaine, choline chloride, glycine and L-proline; the hydrogen bond donor includes at least one of 1,3-propanediol, 1,2-propanediol, ethylene glycol, butanediol, 1,3-butanediol, 1,4-butanediol, oxalic acid, malic acid and ethyl lactate; preferably, the hydrogen bond acceptor is betaine, and the hydrogen bond donor is 1,3-propanediol and ethyl lactate.
[0010] The molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 1:(2-5); preferably, the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 1:(3-4).
[0011] The total mass concentration of the hydrogen bond acceptor and the hydrogen bond donor in the deep eutectic solvent is 70-95%; preferably, the total mass concentration of the hydrogen bond acceptor and the hydrogen bond donor in the deep eutectic solvent is 85-90%.
[0012] The temperature of the ultrasonic extraction is 40-60℃; or / and, the power of the ultrasonic extraction is 150-250W, and the time of the ultrasonic extraction is 20-50min; preferably, the temperature, power and time of the ultrasonic extraction are 50℃, 200W and 30min, respectively.
[0013] The solid-liquid ratio of the ultrasonic extraction is 1g:(10-30)mL; preferably, the solid-liquid ratio of the ultrasonic extraction is 1g:(15-20)mL.
[0014] In a second aspect, the present application provides a mulberry root extract containing oxidized trans-resveratrol prepared by the preparation method of the mulberry root extract containing oxidized trans-resveratrol according to the first aspect.
[0015] In a third aspect, the present application provides an application of the mulberry root extract containing oxidized trans-resveratrol according to the second aspect in the preparation of a cosmetic.
[0016] As a preferred embodiment of the third aspect, the cosmetic includes one or more of cosmetic water, emulsion, cream, mask, serum and spray.
[0017] In a fourth aspect, the present application provides an emulsion, which comprises the following components in mass percentage: thickening agent 0.05-0.3%, humectant 0.5-1%, pH regulator 0.01-0.3%, emulsifier 0.5-5%, preservative 0.5-3%, the mulberry root extract containing oxidized white resveratrol 1-10%, and water in balance.
[0018] As a preferred embodiment of the fourth aspect, the emulsifier comprises at least one of caprylic / capric triglyceride, C14-22 alcohol, C12-20 alkyl glucoside, cetyl stearyl glucoside, isononyl isononanoate, dimethicone, PEG-40 hydrogenated castor oil, stearyl alcohol, sucrose stearate, hydroxystearic acid, polymethylsilsesquioxane, pentaerythrityl distearate, sucrose stearate, dimethicone; and / or, the preservative comprises at least one of p-hydroxyacetophenone, polyhydric alcohol; and / or, the thickening agent comprises at least one of polyacrylate crosspolymer-6, carbomer, carrageenan, gellan gum, xanthan gum, microcrystalline cellulose, cellulose gum, ethyl cellulose, tara gum, guar gum, acryloyldimethyltaurine ammonium / VP copolymer; and / or, the humectant comprises at least one of glycerin, D-panthenol, vitamin B5, 1,3-butanediol, 1,2-hexanediol, 1,3-propanediol, sodium hyaluronate, tremella polysaccharide, trehalose, betaine, allantoin, low molecular weight sodium hyaluronate; and / or, the pH regulator comprises at least one of arginine, disodium ethylenediaminetetraacetate, tromethamine, disodium EDTA.
[0019] Compared with the prior art, the present application has the following beneficial effects:
[0020] 1) The present application uses an ultrasonic-assisted deep eutectic solvent method, and takes a green solvent system composed of betaine and 1,3-propanediol / ethyl lactate as the basis, and combines with mild ultrasonic conditions, to realize efficient extraction of oxidized white resveratrol from mulberry roots. The technology enhances the solubility and stability of the target component through the strong hydrogen bond effect of the deep eutectic solvent, and at the same time, the ultrasonic cavitation effect promotes the rupture of the cell wall, so that the extraction rate is improved and the risk of high temperature oxidation is avoided.
[0021] 2) The present inventors, based on the specific part of mulberry roots, have carried out a large amount of screening and optimization on the types and ratios of hydrogen bond acceptors and hydrogen bond donors in the deep eutectic solvent, and finally determined the deep eutectic solvent composed of betaine, 1,3-propanediol / ethyl lactate and water. The experiments show that when the molar ratio of hydrogen bond acceptor and hydrogen bond donor in the solvent is 1:(2-5), the content and stability of oxidized white resveratrol in the mulberry root extract are both high.
[0022] 3) The present application further verifies through experiments that the obtained mulberry root extract not only can long-acting inhibit the itch receptor MRGPX1, but also is suitable for sensitive skin due to the removal of stimulating components, has high efficiency and biocompatibility, breaks through the environmental pollution and technical bottlenecks of traditional methods, and has a broad market application prospect. BRIEF DESCRIPTION OF DRAWINGS
[0023] Figure 1 The mechanism diagram for blocking the itch signal transmission by combining the itch receptor MRGPRX1 through the oxidation of white resveratrol. DETAILED DESCRIPTION
[0024] In order to better illustrate the purpose, technical scheme and advantages of the present application, the present application will be further described below in combination with specific examples.
[0025] Other materials, reagents, etc. used in the examples can be obtained from commercial channels if not specifically stated.
[0026] Example 1 Preparation method of mulberry root extract containing oxidation of white resveratrol
[0027] (1) Preparation of a eutectic solvent:
[0028] Mix betaine, 1,3-propanediol and ethyl lactate in a molar ratio of 1:3:1 to obtain a mixed solution, uniformly mix 90 g of the mixed solution with 10 g of deionized water to obtain a eutectic solvent; the molar ratio of hydrogen bond acceptor and hydrogen bond donor of the eutectic solvent is 1:4, and the total mass concentration is 90%.
[0029] (2) Preparation of mulberry root extract:
[0030] Collect the roots of mulberry trees, clean them, and then dry them in a constant temperature oven at 50°C until the weight is constant. Grind and crush, then pass through an 80-mesh sieve. After filtration, 1 g is added to the eutectic solvent prepared in step (1), and the solid-liquid ratio is 1 g:20 mL. Use ultrasonic extraction method, ultrasonic temperature 50°C, power 200W, extraction time 30min, collect the product and centrifuge, take the supernatant to obtain the mulberry root extract containing oxidation of white resveratrol, and name the extract as Example 1.
[0031] Example 2 Preparation method of mulberry root extract containing oxidation of white resveratrol
[0032] (1) Preparation of a eutectic solvent:
[0033] Mix betaine, 1,3-propanediol and ethyl lactate in a molar ratio of 1:2.5:0.5 to obtain a mixed solution, uniformly mix 85 g of the mixed solution with 15 g of deionized water to obtain a eutectic solvent; the molar ratio of hydrogen bond acceptor and hydrogen bond donor of the eutectic solvent is 1:3, and the total mass concentration is 85%.
[0034] (2) Preparation of mulberry root extract:
[0035] The root of mulberry was collected, washed and dried in a constant temperature oven at 50°C until constant weight. After grinding and sieving through an 80-mesh sieve, 1 g of the sample was added to the deep eutectic solvent prepared in step (1) with a solid-liquid ratio of 1 g: 15 mL. The product was collected by centrifugation, and the supernatant was obtained to give the mulberry root extract containing oxyresveratrol, which was named as Example 2.
[0036] Preparation method of mulberry root extract containing oxyresveratrol
[0037] (1) Preparation of deep eutectic solvent:
[0038] Betaine, 1,3-propanediol and ethyl lactate were mixed in a molar ratio of 1:4:1 to obtain a mixed solution. Then 95 g of the mixed solution was uniformly mixed with 5 g of deionized water to obtain a deep eutectic solvent. The molar ratio of hydrogen bond acceptor and hydrogen bond donor of the deep eutectic solvent was 1:5, and the total mass concentration was 95%.
[0039] (2) Preparation of mulberry root extract:
[0040] The root of mulberry was collected, washed and dried in a constant temperature oven at 50°C until constant weight. After grinding and sieving through an 80-mesh sieve, 1 g of the sample was added to the deep eutectic solvent prepared in step (1) with a solid-liquid ratio of 1 g: 15 mL. The product was collected by centrifugation, and the supernatant was obtained to give the mulberry root extract containing oxyresveratrol, which was named as Example 2.
[0041] Preparation method of mulberry root extract containing oxyresveratrol
[0042] (1) Preparation of deep eutectic solvent:
[0043] Betaine, 1,3-propanediol and ethyl lactate were mixed in a molar ratio of 1:4:1 to obtain a mixed solution. Then 95 g of the mixed solution was uniformly mixed with 5 g of deionized water to obtain a deep eutectic solvent. The molar ratio of hydrogen bond acceptor and hydrogen bond donor of the deep eutectic solvent was 1:5, and the total mass concentration was 95%.
[0044] (2) Preparation of mulberry root extract:
[0045] The root of mulberry was collected, washed and dried in a constant temperature oven at 50°C until constant weight. After grinding and sieving through an 80-mesh sieve, 1 g of the sample was added to the deep eutectic solvent prepared in step (1) to obtain a solid-liquid ratio of 1 g: 10 mL. The product was collected by centrifugation, and the supernatant was obtained to obtain the mulberry root extract containing oxyresveratrol, which was named as Example 4.
[0046] Comparative Example 1
[0047] Compared with the preparation method of Example 1, only the selection of the hydrogen bond acceptor was different, i.e., choline chloride was used instead of betaine, and the remaining steps were exactly the same as Example 1.
[0048] Comparative Example 2
[0049] Compared with the preparation method of Example 1, only the selection of the hydrogen bond donor was different, i.e., no 1,3-propanediol was added, and an equivalent amount of ethyl lactate was used to make up the missing amount, and the remaining steps were exactly the same as Example 1.
[0050] Comparative Example 3
[0051] Compared with the preparation method of Example 1, only the selection of the hydrogen bond donor was different, i.e., no ethyl lactate was added, and an equivalent amount of 1,3-propanediol was used to make up the missing amount, and the remaining steps were exactly the same as Example 1.
[0052] Comparative Example 4
[0053] Compared with the preparation method of Example 1, only the selection of the hydrogen bond donor was different, i.e., butanediol was used instead of 1,3-propanediol and ethyl lactate, and the remaining steps were exactly the same as Example 1.
[0054] Comparative Example 5
[0055] Compared with the preparation method of Example 1, only the molar ratio of the hydrogen bond acceptor and the hydrogen bond donor was different, i.e., betaine, 1,3-propanediol, and ethyl lactate were mixed in a molar ratio of 1:0.75:0.25 (i.e., the molar ratio of the hydrogen bond acceptor and the hydrogen bond donor was 1:1), and the remaining steps were exactly the same as Example 1.
[0056] Comparative Example 6
[0057] Compared with the preparation method of Example 1, only the molar ratio of the hydrogen bond acceptor and the hydrogen bond donor was different, i.e., betaine, 1,3-propanediol, and ethyl lactate were mixed in a molar ratio of 1:4.5:1.5 (i.e., the molar ratio of the hydrogen bond acceptor and the hydrogen bond donor was 1:6), and the remaining steps were exactly the same as Example 1.
[0058] Comparative Example 7
[0059] Compared with the preparation method of Example 1, only the solid-liquid ratio, ultrasonic temperature, power and extraction time in the preparation method of mulberry root extract are different, the solid-liquid ratio in the comparative example is 1 g:5 mL, the ultrasonic temperature is 30℃, the power is 100 W, and the extraction time is 10 min, and the remaining steps are exactly the same as Example 1.
[0060] Comparative Example 8
[0061] Compared with the preparation method of Example 1, only the solid-liquid ratio, ultrasonic temperature, power and extraction time in the preparation method of mulberry root extract are different, the solid-liquid ratio in the comparative example is 1 g:40 mL, the ultrasonic temperature is 70℃, the power is 300 W, and the extraction time is 60 min, and the remaining steps are exactly the same as Example 1.
[0062] Comparative Example 9
[0063] The root of the mulberry tree was collected, washed and dried to constant weight in a constant temperature oven at 50℃, ground and sieved through an 80 mesh sieve, and 1 g of the filtrate was added to a 75% ethanol aqueous solution, with a solid-liquid ratio of 1 g:20 mL. The ultrasonic extraction method was used, with an ultrasonic temperature of 50℃, a power of 200 W, and an extraction time of 30 min. The product was collected by centrifugation, and the supernatant was obtained.
[0064] Comparative Example 10
[0065] Compared with the preparation method of Example 1, only the extraction site is different, i.e. the branches of the mulberry tree are used instead of the root, and the remaining steps are exactly the same as Example 1.
[0066] Effect experiment
[0067] 1) High performance liquid chromatography method for detecting the content and stability of oxidized resveratrol in examples and comparative examples
[0068] Oxidized resveratrol content detection: 1 mL of the prepared mulberry root extract was accurately measured and diluted in 9 mL of methanol, filtered through a 0.22 μm filter, and the content of oxidized resveratrol in the extract was determined by high performance liquid chromatography. The standard solution was prepared by using the oxidized resveratrol standard (purchased from Yuan Ye Bio, item number B21467) with gradient concentration, and the standard curve was drawn, and the content of oxidized resveratrol in the sample M0 was calculated according to the standard curve formula. The chromatographic column used was a C18 column (100 mm x 2.1 mm, 3 μM), the mobile phase was 60% methanol, the flow rate was 0.5 mL / min, and the sample volume was 10 μL.
[0069] Stability test: 5 mL of mulberry root extract prepared in the examples and comparative examples were respectively taken into 10 mL transparent sealed PE bottles, and placed at temperatures of 4 ℃, 25 ℃ and 50 ℃, respectively, under 15W light illumination, then the mass M1 of oxidized white resveratrol was detected on the 7th day, and the detection method was consistent with M0, and then the retention rate of oxidized white resveratrol was calculated, and the retention rate of oxidized white resveratrol = M1 / M0 x 100%.
[0070] The results are shown in Table 1:
[0071] Table 1: Oxidized white resveratrol content and stability test results
[0072]
[0073] According to the results in Table 1, it can be seen that: 1) comparing the results of the examples with those of Comparative Examples 1-4 and 9, it can be seen that the preparation method of the present application is obviously better than the alcohol extraction method, and the composition of the deep eutectic solvent has a great influence on the extraction efficiency and stability of oxidized white resveratrol, and the deep eutectic solvent composed of betaine, 1,3-propanediol and ethyl lactate makes the mulberry root extract prepared have higher content and stability of oxidized white resveratrol, which produces unexpected technical effects; 2) comparing the results of the examples with those of Comparative Examples 5-6, it can be known that the molar ratio of hydrogen bond acceptor and hydrogen bond donor also has an influence on the extraction efficiency and stability of oxidized white resveratrol, and the experiments of the present application prove that the molar ratio of hydrogen bond acceptor and hydrogen bond donor in the range of 1:2-5 has better experimental effects; 3) comparing the results of the examples with those of Comparative Examples 7-8, it can be known that the solid-liquid ratio in the preparation process, as well as the temperature, power and extraction time of ultrasonic, all have certain influence on the extraction efficiency and stability of oxidized white resveratrol; 4) comparing the results of the examples with those of Comparative Example 10 shows that: mulberry root and mulberry branch are both common sources of oxidized white resveratrol in the art, and the present inventors previously based on this specific part of mulberry root, screened and optimized the types and ratios of hydrogen bond acceptor and hydrogen bond donor in the deep eutectic solvent, and finally determined the deep eutectic solvent composed of betaine and 1,3-propanediol / ethyl lactate and water, and the content and stability of oxidized white resveratrol in the mulberry branch extract prepared by using the solvent in the present application are both greatly different from those in the mulberry root extract, which shows that even for different parts of the same plant, the deep eutectic solvent is not universal due to the different compositions of different parts, and the experiments of the present application prove that the deep eutectic solvent composed of betaine and 1,3-propanediol / ethyl lactate and water is only suitable for high-efficiency extraction of oxidized white resveratrol from mulberry root.
[0074] Application example
[0075] An emulsion is provided, the components (mass percentage) of which are shown in Table 2; wherein the mulberry root extract containing oxidized white resveratrol used in application examples 1-4 is the mulberry root extract containing oxidized white resveratrol prepared in examples 1-4, the mulberry root extract containing oxidized white resveratrol used in application examples 5-6 is the mulberry root extract containing oxidized white resveratrol prepared in example 1; the mulberry root extract containing oxidized white resveratrol used in comparative application examples 1-9 is the mulberry root extract containing oxidized white resveratrol prepared in comparative examples 1-9; in addition, a blank application example is set, and the only difference between the blank application example and application example 1 is that the mulberry root extract containing oxidized white resveratrol is not added.
[0076] Table 2 Component composition of emulsion (mass percentage)
[0077]
[0078] The present application example provides a preparation method of an emulsion, which comprises the following steps:
[0079] (1) Mix the humectant, thickening agent and part of the pH adjuster (EDTA-disodium) with water, stir and heat to 85°C, then homogenize at a speed of 1300 rpm for 4 min, and keep warm after homogenization for standby, to obtain a pre-prepared A phase;
[0080] (2) Mix the emulsifier, heat to 75°C, then homogenize at a speed of 1300 rpm for 4 min, and keep warm after homogenization for standby, to obtain a pre-prepared B phase;
[0081] (3) Mix the preservative, heat to melt at 60°C, to obtain a pre-prepared C phase;
[0082] (4) Warm the pre-prepared A phase to 80°C, add the pre-prepared B phase at a speed of 300 rpm, stir and mix, then cool to 60°C, add the pre-prepared C phase at a speed of 300 rpm, stir and mix, then cool to below 45°C, add the mulberry root extract containing oxidized white resveratrol, continue to stir for 8 min, finally add the remaining pH adjuster (arginine) to adjust the pH to 5.5-7.0, stop stirring, discharge, to obtain the emulsion.
[0083] 2. Effects of application examples 1-6 and comparative application examples 1-9 on mouse itching model
[0084] Experimental animals: 128 SPF grade ICR mice, 5-6 weeks old, weighing 20-25 g, half male and half female, provided by Guangdong Experimental Animal Center, and randomly divided into 16 groups, 8 mice in each group.
[0085] Experimental method: After 1 week of adaptive feeding, the back hair of all mice was cut off with scissors, and then washed clean with depilatory cream,
[0086] The exposed skin area was about 2 cm x 2 cm. After 24 h, 0.2 g of the emulsion prepared in Application Example 1-6, Comparative Application Example 1-9 and Blank Application Example was applied to the exposed skin surface of the mice, once a day, for 7 consecutive days. 30 min after the last application, 0.01 mL / g of a solution of itch peptide BAM8-22 was injected subcutaneously at the center of the depilated area on the back of all the mice (0.01% BAM8-22 solution was prepared in advance with normal saline), and the number of scratches within 10 min was observed and recorded immediately (one scratch was counted when the mouse scratched continuously until a short pause occurred).
[0087] Itch peptide BAM8-22 is an agonist of itch receptor MRGPRX1, which triggers itch signal transmission by binding to and activating the itch receptor, resulting in the production of an itching sensation. The inventors found in practice that oxymorcofol can competitively bind to the active pocket of itch receptor MRGPRX1 (see the attached Figure 1 , thereby inhibiting the itch signal induced by itch peptide BAM8-22, achieving the effect of reducing the itching sensation.
[0088] The results are shown in Table 3:
[0089] Table 3
[0090]
[0091]
[0092] The results in Table 3 show that the average number of scratches of Application Example 1-6 is lower than that of Comparative Application Example 1-9, indicating that the average number of scratches of mice is positively correlated with the content of oxymorcofol in mulberry root extract, also verifying that oxymorcofol can inhibit the itch signal induced by itch peptide BAM8-22, achieving the effect of reducing the itching sensation.
[0093] 3. Human skin patch test
[0094] Thirty volunteers, 15 males and 15 females, aged 20-50 years, were recruited, and a closed patch test method was used. Equal amounts (0.020 mL-0.025 mL) of test samples (emulsions prepared in Application Example 1-6, Comparative Application Example 1-9 and Blank Application Example) were placed in a specific patch tester, which was attached to the arm of the volunteer with a low-sensitization adhesive tape, and was pressed lightly to ensure uniform attachment to the skin, and was left for 24 h. The blank control group was distilled water, and the blank application example was an emulsion without mulberry root extract. After 24 h, the patch tester was removed, and the skin reaction was observed at 0.5 h, 24 h and 48 h, and the results were recorded. The skin adverse reaction grades are shown in Table 4 below.
[0095] Table 4
[0096]
[0097] After the human patch test, the emulsions provided by application examples 1-6 and comparative application examples 1-9 of the present application were all negative reactions, which were safe and non-irritating to human skin.
[0098] 4. Human efficacy test of the composition for relieving skin itching
[0099] Experimental method: According to the "Cosmetic Safety Technology Standard" (2015) test, 96 Asian adult testers aged 18-60 years who felt that their skin was easy to itch and sensitive were randomly divided into 16 groups, 6 people in each group. Volunteers applied the sample to the whole face once a day in the morning and evening (the sample was the emulsion prepared by application examples 1-6, comparative application examples 1-9, and blank application examples), and visited to collect data on day 0 and day 28. After the volunteers visited, they washed their faces with facial cleanser, sat in an air-conditioned room with a temperature of 21±1℃ and a humidity of 50±10% for 30 minutes, and filled out the subjective sensory questionnaire to evaluate the current facial itching level with a score of 0-9. The higher the score, the higher the itching level, and 0 represents no feeling and 9 represents unbearable.
[0100] The results are shown in Table 5.
[0101] Table 5
[0102] Average pruritus score at day 0 Average pruritus score at day 28 Example 1 7.2 7.2 Example 2 7.2 0.8 Example 3 7.3 1.2 Example 4 7.0 1.3 Example 5 7.3 1.7 Example 6 7.2 1.5 Comparative Example 1 7.0 1.0 Comparative Example 2 7.3 5.8 Comparative Example 3 7.2 6.3 Comparative Example 4 7.3 6.2 Comparative Example 5 7.0 6.7 Comparative Example 6 7.0 5.5 Comparative Example 7 7.2 5.8 Comparative Example 8 7.3 5.2 Comparative Example 9 7.3 5.2 7.2 6.8
[0103] The results in Table 3 show that the average itching score of application examples 1-6 is lower than that of comparative application examples 1-9, indicating that the emulsion containing mulberry root extract containing oxidized white resveratrol prepared by the preparation method of the present application has better effect of relieving skin itching.
[0104] Finally, it should be noted that the above examples are only used to illustrate the technical solutions of the present application and do not limit the scope of protection of the present application. Although the present application has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present application can be modified or replaced by equivalents without departing from the essence and scope of the technical solutions of the present application.
Claims
1. A method for preparing a mulberry root extract containing oxidized resveratrol, characterized in that, Includes the following steps: The roots and stems of mulberry trees were dried, crushed, and then added to an aqueous solution of a eutectic solvent for ultrasonic extraction. After extraction, the product was collected, the supernatant was centrifuged, and the mulberry root extract containing oxidized resveratrol was obtained. The aqueous solution of the eutectic solvent consists of a hydrogen bond acceptor, a hydrogen bond donor, and water. The hydrogen bond acceptor is betaine, and the hydrogen bond donors are 1,3-propanediol and ethyl lactate, with a molar ratio of 1:2 to 5 for the hydrogen bond acceptor and the hydrogen bond donor.
2. The preparation method according to claim 1, characterized in that, The molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 1:3~4.
3. The preparation method according to claim 1 or 2, characterized in that, The total mass concentration of hydrogen bond acceptors and hydrogen bond donors in the eutectic solvent is 70-95%.
4. The preparation method according to claim 3, characterized in that, The total mass concentration of hydrogen bond acceptors and hydrogen bond donors in the eutectic solvent is 85-90%.
5. The preparation method according to claim 1 or 2, characterized in that, The ultrasonic extraction temperature is 40~60℃, the ultrasonic extraction power is 150~250W, and the ultrasonic extraction time is 20~50 min; the material-to-liquid ratio of the ultrasonic extraction is 1g:(10~30)mL.
6. The preparation method according to claim 5, characterized in that, The ultrasonic extraction temperature is 50℃, the ultrasonic extraction power is 200W, and the ultrasonic extraction time is 30min; the material-to-liquid ratio of the ultrasonic extraction is 1g:(15~20)mL.
7. The mulberry root extract containing oxidized resveratrol prepared by the preparation method according to any one of claims 1-6.
8. The application of the mulberry root extract containing oxidized resveratrol as described in claim 7 in the preparation of cosmetics, wherein the cosmetics include one or more of the following: toner, lotion, cream, mask, serum, and spray.
9. An emulsion, characterized in that, The emulsion comprises the following components by weight percentage: 0.05-0.3% thickener, 0.5-1% humectant, 0.01-0.3% pH adjuster, 0.5-5% emulsifier, 0.5-3% preservative, 1-10% mulberry root extract containing oxidized resveratrol as described in claim 7, and water as the balance.
10. The emulsion as described in claim 9, characterized in that, The emulsifier includes at least one of the following: caprylic / capric triglyceride, C14-22 alcohol, C12-20 alkyl glucoside, cetearyl glucoside, isononyl isononanoate, polydimethylsiloxane, PEG-40 hydrogenated castor oil, stearyl alcohol, sucrose stearate, hydroxystearic acid, polymethyl silsesquioxane, pentaerythritol distearate, and sucrose stearate; The preservative includes at least one of p-hydroxyacetophenone and polyols; The thickener includes at least one of the following: polyacrylate crosspolymer-6, carbomer, carrageenan, gellan gum, xanthan gum, microcrystalline cellulose, cellulose gum, ethyl cellulose, argan gum, guar gum, and ammonium acryloyldimethyl taurate / VP copolymer. The moisturizer includes at least one of glycerin, D-panthenol, vitamin B5, 1,3-butanediol, 1,2-hexanediol, 1,3-propanediol, sodium hyaluronate, tremella polysaccharide, trehalose, betaine, and allantoin. The pH adjuster includes at least one of arginine, disodium ethylenediaminetetraacetate, and tromethamine.
11. The emulsion as described in claim 9, characterized in that, The moisturizer is low molecular weight sodium hyaluronate.
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