Siberian elm root extract as well as extraction method and application thereof

A two-stage enzymatic process enhances the extraction of polyphenols and polysaccharides from spring elm root bark, addressing low content issues and improving skin elasticity and reducing UV-induced pigmentation in skincare products.

CN120305178APending Publication Date: 2025-07-15MAKEUP (GUANGZHOU) BIOCHEMICAL TECH CO LTD

Patent Information

Application Number
CN202510523387.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-04-24
Publication Date
2025-07-15

AI Technical Summary

Technical Problem

In the prior art, the active ingredients of the spring elm root extract are unclear, have low content, and have a single function and use, making it difficult to effectively utilize its multiple effects in skin topical agents.

Method used

Ultrasonic assisted phased enzymatic decomposition method was adopted, and the spring elm roots were enzymatically dissolved using complex enzyme preparation I and complex enzyme preparation II, decomposing the cell walls and releasing polyphenols and polysaccharide active ingredients. Combined with ultrasonic assisted, cell penetration was enhanced, and high content of spring elm root extract was extracted.

Benefits of technology

It improves the total phenols and total sugar content in spring elm root extract, enhances its antioxidant and firming skin effects, especially in cosmetics, which show significant anti-aging and reducing ultraviolet ray-induced spots.

✦ Generated by Eureka AI based on patent content.

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Abstract

According to the elm root extract and the extraction method and application thereof, ultrasonic-assisted staged enzymolysis is adopted, elm roots are decomposed through the special activity of various enzymes, cells are broken, and the material transfer barrier between cell walls and cells is reduced, so that the purpose of extracting effective active ingredients of polyphenol and polysaccharide in the elm roots to the maximum extent is achieved. According to the invention, the effective active ingredients in the elm root extract are increased in a targeted manner, and it is proved that the elm root extract has an anti-inflammatory effect and also has an anti-skin aging cosmetic application, especially a tightening effect, and has a good application prospect in cosmetic compositions. The composition can be applied to personal care products with anti-aging and firming effects.
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Description

Technical Field

[0001] The present invention relates to an extract of Ulmus davidiana var. japonica roots, an extraction method thereof, and an application, and particularly relates to an extract of Ulmus davidiana var. japonica roots, an extraction method of the extract of Ulmus davidiana var. japonica roots, and an application in cosmetics, belonging to the field of cosmetics. Background Art

[0002] Ulmus davidiana var. japonica (Rehd.) Nakai, also known as mountain elm, is a plant of the genus Ulmus in the family Ulmaceae. It is often used as a greening tree and has very rich resources. Its root bark and stem bark are often used in traditional Chinese medicine and are also called elm white bark. In folk, it is used to treat liver damage diseases such as jaundice and hepatitis. According to the "Shennong Ben Cao Jing" records: "It is mainly used for the treatment of unobstructed urination and defecation, and can promote water passage and remove pathogenic factors." In traditional medicine, it has the effects of promoting diuresis, relieving stranguria, and detumescence, and is mostly used for treating constipation or skin ulcers, inflammation and other medical uses.

[0003] The currently known extraction methods of Ulmus davidiana var. japonica root bark are mostly simple reflux extractions such as water extraction or ethanol organic solvents, and there are also extraction methods such as ultrasonic-assisted extraction, microwave-assisted extraction, supercritical fluid extraction, and subcritical water extraction, but they are not widely used.

[0004] It is reported that in a patent (CN109602658A), a skin care composition containing an extract of Ulmus davidiana var. japonica roots uses a composite enzyme of 0.05% pectinase and 0.2% cellulase to enzymatically hydrolyze for 0.5 - 3 hours, and synergistically uses a microwave extraction process to extract the active substances of Ulmus davidiana var. japonica roots, and it is confirmed that the composition containing the extract of Ulmus davidiana var. japonica roots has the effects of moisturizing the skin and enhancing the elasticity and gloss of the skin, but does not clarify the main active ingredients and their contents in the extract of Ulmus davidiana var. japonica roots under this method. Similarly, Zhou et al. used a composite enzyme of cellulase, pectinase, and β-glucosidase to synergistically extract the root bark of Ulmus davidiana var. japonica. Under the optimal extraction conditions obtained according to the response surface method, the total phenolic content in the extract of Ulmus davidiana var. japonica roots was 16.04 mg GAE / g DW, and the total sugar content was 123.75 mg GE / g DW, and the content of active substances was low.

[0005] In summary, the existing technologies for extracting Ulmus davidiana var. japonica roots based on enzymatic methods have deficiencies such as unclear active components of the extract, low content, and relatively single efficacy and uses. Since different extraction methods have a great impact on the types and yields of active ingredients in the final product, as well as the efficacy of the final product, therefore, how to screen out a method that is more conducive to extracting active ingredients that can be used in skin external agents from the root bark of Ulmus davidiana var. japonica is still a technical problem faced by researchers in this field.

[0006] Based on this, there is an urgent need to provide an extraction method for extracting active substances from the root bark of Ulmus davidiana var. japonica that can be used in the field of skin topical agents, and the extract has high contents of phenolic and polysaccharide active ingredients, has multiple effects of improving skin elasticity and firmness while reducing age spots caused by ultraviolet rays, and makes full use of the resources of Ulmus davidiana var. japonica root bark. Summary of the Invention

[0007] In order to solve the deficiencies of the above technologies, the present invention provides an extract of Ulmus davidiana var. japonica root bark, an extraction method thereof, and an application.

[0008] In order to solve the above technical problems, the technical solution adopted by the present invention is: an extraction method for an extract of Ulmus davidiana var. japonica root bark, and the extraction method is as follows:

[0009] Ultrasonic-assisted staged enzymatic hydrolysis is adopted to decompose the root bark of Ulmus davidiana var. japonica through the special activities of various enzymes to maximize the extraction of effective active ingredients in the root bark of Ulmus davidiana var. japonica;

[0010] The effective active ingredients include polyphenols and polysaccharides, and the various enzymes include complex enzyme preparation I and complex enzyme preparation II.

[0011] Preferably, the extraction method includes the following steps:

[0012] S1. Take the dried root bark of Ulmus davidiana var. japonica, cut and crush it to 40-60 mesh, and then add a citrate buffer solution with pH 5.0 containing ethanol for ultrasonic pretreatment to obtain a crude extract of Ulmus davidiana var. japonica root bark;

[0013] S2. Then add complex enzyme preparation I at 45°C - 55°C, enzymatically hydrolyze for 3 - 5 h, inactivate at 80°C in a water bath for 10 minutes, and then centrifuge to collect the supernatant to obtain the first enzymatic hydrolysis solution. Retain the residue, and the centrifugation conditions are: 4000 rpm, 15 minutes;

[0014] S3. The residue after centrifugation is redissolved in a phosphate buffer solution with pH 6.5, and complex enzyme preparation II is added at 30°C - 50°C for enzymatic hydrolysis for 1 - 3 h to obtain a secondary enzymatic hydrolysis solution;

[0015] S4. Mix the first enzymatic hydrolysis solution and the second enzymatic hydrolysis solution, add 5 times the amount of absolute ethanol to make the alcohol content greater than 70%, reflux and extract at 50°C - 60°C for 2 h, extract three times, filter, combine the three extraction solutions, recover ethanol from the extraction solution, and obtain an extract of Ulmus davidiana var. japonica root bark.

[0016] Preferably, in step S1, the mass ratio of the root bark of Ulmus davidiana var. japonica to the citrate buffer solution is 1:10 - 20;

[0017] The mass concentration of the citrate buffer solution is 0.1 M, which is mixed by ethanol and citrate buffer solution in a ratio of 1:1, and the final concentration of ethanol ≤ 15%;

[0018] In step S1, the ultrasonic conditions are: ultrasonic pretreatment at 40°C and 200 W for 10 - 20 minutes.

[0019] Preferably, in step S2, the composition components and mass ratio of the complex enzyme preparation Ⅰ are: ferulic acid esterase, cellulase, pectinase, and xylanase with a ratio of 1:4:2:1; the addition amount of complex enzyme Ⅰ is 1 - 5% of the mass of the root of Ulmus davidiana var. japonica.

[0020] Preferably, in step S3, the mass ratio of the root bark of Ulmus davidiana var. japonica to the phosphate buffer solution is 1:5 - 15, and the mass concentration of the phosphate buffer solution is 0.1 M.

[0021] Preferably, in step S3, the composition components and mass ratio of the complex enzyme preparation Ⅱ are: β-glucosidase and esterase with a ratio of 2:1, and the addition amount of complex enzyme Ⅱ is 0.5 - 1.5% of the mass of the residue.

[0022] A root extract of Ulmus davidiana var. japonica is obtained by using the above-mentioned extraction method of the root extract of Ulmus davidiana var. japonica;

[0023] The content of the main characteristic components in the obtained root extract of Ulmus davidiana var. japonica is:

[0024] The total phenolic content is 20.5 - 46.8 mg GAE / g DW, and the total sugar content is 189.0 - 215.6 mg GE / g DW.

[0025] An application of a root extract of Ulmus davidiana var. japonica can be used as an antioxidant active ingredient and / or a skin-tightening active ingredient in personal care products.

[0026] Preferably, the personal care products include one or more of lotion, cream, essence, and mask.

[0027] Preferably, the types of composition components in the personal care products also include solvents, humectants, thickeners, preservatives, emulsifiers, surfactants, auxiliaries, fragrances, whitening agents, and anti-aging agents.

[0028] The present invention discloses a root extract of Ulmus davidiana var. japonica, its extraction method, and application. By using ultrasonic-assisted staged enzymatic hydrolysis, the root of Ulmus davidiana var. japonica is decomposed by the special activities of various enzymes, the cells are ruptured, and the mass transfer barriers of cell walls and intercellular substances are reduced, so as to achieve the purpose of maximizing the extraction of polyphenols and polysaccharides in the root of Ulmus davidiana var. japonica. The effective active components in the root extract of Ulmus davidiana var. japonica are specifically improved, and it is confirmed that in addition to the anti-inflammatory effect, the root extract of Ulmus davidiana var. japonica also has the effect of anti-skin aging, especially the skin-tightening effect, and has good application prospects in cosmetic compositions. Description of the Drawings

[0029] Figure 1 It is a bar chart of the relative expression level of zebrafish type Ⅰ collagen gene of the present invention.

[0030] Figure 2 This is the bar graph of the relative expression level of the zebrafish elastin gene of the present invention.

[0031] Figure 3 This is the result graph of the ultraviolet stain characteristics count in the human efficacy test of the present invention.

[0032] Figure 4 This is the result graph of the brown stain characteristics count in the human efficacy test of the present invention.

[0033] Figure 5 This is the usage result graph of a certain volunteer in the human efficacy test of the present invention. Detailed implementation manners

[0034] The present invention will be further described in detail below in conjunction with the accompanying drawings and specific implementation manners.

[0035] To solve the defects in the prior art such as the low utilization rate of the roots of Ulmus davidiana var. japonica, numerous plant extraction processes, and the difficulty in screening a method for extracting active ingredients that can be used in the cosmetic field from the roots of Ulmus davidiana var. japonica, the present invention provides an extract of the roots of Ulmus davidiana var. japonica, its extraction method, and application. The highly active extract of the roots of Ulmus davidiana var. japonica obtained by the extraction method for simultaneously extracting a high content of phenolic compounds and polysaccharide compounds has a good effect of improving skin elasticity and firmness and reducing stains caused by ultraviolet rays, and can be widely applied in the cosmetic field.

[0036] It is known that the extract of the roots of Ulmus davidiana var. japonica is a traditional Chinese medicine, and its existing effects include anti-inflammatory, antibacterial, antioxidant, anti-tumor, anti-septicemia, etc. The extract of the roots of Ulmus davidiana var. japonica obtained by the present invention has stronger biological activity for specific active ingredient compositions such as phenolic compounds and polysaccharide compounds. In addition to the above uses, the extract of the roots of Ulmus davidiana var. japonica obtained by the present invention further has a firming effect on the skin. In particular, it can improve the problems caused by skin photoaging, can effectively promote the gene expression of collagen (col1ala, colla1b, and colla2) and elastin (Elna), inhibit the inflammatory factor TNF-α, maintain skin elasticity and reduce wrinkles while reducing skin inflammatory reactions caused by ultraviolet stimulation and ultraviolet stains caused by ultraviolet rays.

[0037] First, the extraction method of the present invention uses the root bark part of the roots of Ulmus davidiana var. japonica, and includes the following steps:

[0038] S1. Take the dried root bark of Ulmus davidiana var. japonica, cut and crush it to 40-60 mesh, and then add a citrate buffer solution with ethanol and pH 5.0 for ultrasonic pretreatment to obtain a crude extract of the roots of Ulmus davidiana var. japonica.

[0039] Among them, the root bark of Ulmus davidiana var. japonica is the root bark of a plant of the genus Ulmus (Ulmus) in the family Ulmaceae, preferably the root bark of Ulmus davidiana var. japonica from Huadian City, Jilin City;

[0040] Inner bark of Ulmus davidiana var. japonica: The mass ratio of the material to the citrate buffer solution (0.1M) is 1:10 - 20. Ethanol and citrate buffer are mixed at a ratio of 1:1 (the final concentration of ethanol ≤ 15%). Ultrasonic conditions: Pretreat with ultrasound at 40°C and 200W for 10 - 20 minutes.

[0041] S2. Then add complex enzyme preparation Ⅰ at 45°C - 55°C, enzymatically hydrolyze for 3 - 5h, inactivate in a water bath at 80°C for 10 minutes, and then centrifuge (4000rpm, 15 minutes) to collect the supernatant to obtain the first enzymatic hydrolysate, and retain the residue;

[0042] The components and mass ratio of complex enzyme preparation Ⅰ are: feruloyl esterase, cellulase, pectinase, and xylanase at a ratio of 1:4:2:1.

[0043] The addition amount of complex enzyme Ⅰ is 1 - 5% of the mass of the inner bark of Ulmus davidiana var. japonica.

[0044] S3. The centrifuged residue is redissolved in phosphate buffer at pH 6.5. Add complex enzyme preparation Ⅱ at 30°C - 50°C and enzymatically hydrolyze for 1 - 3h to obtain the secondary enzymatic hydrolysate;

[0045] Inner bark of Ulmus davidiana var. japonica: The mass ratio of the material to the phosphate buffer solution (0.1M) is 1:5 - 15.

[0046] The components and mass ratio of complex enzyme preparation Ⅱ are: β - glucosidase and esterase at a ratio of 2:1. The addition amount of complex enzyme Ⅱ is 0.5 - 1.5% of the mass of the residue.

[0047] S4. Mix the first enzymatic hydrolysate and the second enzymatic hydrolysate, add 5 times the amount of absolute ethanol to make the alcohol content greater than 70%, reflux and extract at 50°C - 60°C for 2h, extract three times, filter, combine the three extraction solutions, recover ethanol from the extraction solution to obtain the extract of the inner bark of Ulmus davidiana var. japonica.

[0048] For the above extraction method, the core lies in adopting ultrasonic - assisted staged targeted enzymatic hydrolysis. Ultrasonic assistance enhances the breaking of cell walls, promotes enzyme penetration, and improves the enzymatic hydrolysis efficiency. In the first stage, feruloyl esterase, cellulase, pectinase, and xylanase cooperate to destroy the cell wall, decompose components such as cellulose, hemicellulose, and pectin in the inner bark of Ulmus davidiana var. japonica, reduce the mass transfer barrier of cell walls and inter - cellular substances, and release intracellular phenols and soluble sugars. In the second stage, for the bound phenols such as bakuchiol in the form of glycosides or esters that are difficult to extract, β - glucosidase and esterase are used to release free phenol substances. Through staged enzymatic hydrolysis of cell wall destruction and phenol release, combined with ultrasonic - assisted penetration, the yields of phenols and polysaccharides are specifically improved.

[0049] Furthermore, the extract of the root bark of Ulmus davidiana var. japonica extracted by the method of the present invention was analyzed, and the analysis showed that its main characteristic components included: the total phenolic content was 20.5 - 46.8 mg GAE / g DW, and the total sugar content was 189.0 - 215.6 mg GE / g DW.

[0050] The extract of the root bark of Ulmus davidiana var. japonica extracted by the method of the present invention is a yellow to brownish-yellow solution.

[0051] Example 1:

[0052] The dried root bark of Ulmus davidiana var. japonica from Huadian City, Jilin City was sheared and crushed to 50 mesh, and a citrate buffer solution (0.1 M) with 15% ethanol at pH 5.0 (ethanol and citrate buffer were mixed at a ratio of 1:1) was added. Ultrasonic pretreatment was carried out at 40 °C and 200 W for 15 minutes to obtain a crude extract of the root bark of Ulmus davidiana var. japonica. The mass ratio of the root bark of Ulmus davidiana var. japonica to the citrate buffer solution was 1:15. Then, a compound enzyme preparation I (the mass ratio of ferulic acid esterase, cellulase, pectinase, and xylanase was 1:4:2:1) accounting for 3% of the mass of the root bark of Ulmus davidiana var. japonica was added at 50 °C. After enzymatic hydrolysis for 4 h, it was inactivated in a water bath at 80 °C for 10 minutes and then centrifuged (4000 rpm, 15 minutes) to collect the supernatant to obtain the first enzymatic hydrolysate, and the residue was retained; the centrifuged residue was redissolved in a phosphate buffer solution at pH 6.5 (the mass ratio of the root bark of Ulmus davidiana var. japonica to the phosphate buffer solution (0.1 M) was 1:10). A compound enzyme preparation II (the mass ratio of β-glucosidase and esterase was 2:1) accounting for 1% of the mass of the residue was added at 40 °C, and enzymatic hydrolysis was carried out for 2 h to obtain a secondary enzymatic hydrolysate. The first enzymatic hydrolysate and the secondary enzymatic hydrolysate were mixed, and 5 times the amount of absolute ethanol was added to make the ethanol content greater than 70%. Reflux extraction was carried out at 55 °C for 2 h, and extraction was carried out three times. The three extraction solutions were filtered and combined, and the ethanol in the extraction solution was recovered to obtain the extract of the root bark of Ulmus davidiana var. japonica.

[0053] Example 2:

[0054] The dry root bark of Ulmus davidiana var. japonica from Huadian City, Jilin City was cut and crushed to 40 mesh, and added to a citrate buffer solution (0.1M) with pH 5.0 containing 15% ethanol (ethanol and citrate buffer solution were mixed at a ratio of 1:1). It was pretreated by ultrasonic wave at 40°C and 200W for 10 minutes to obtain a crude extract of Ulmus davidiana var. japonica root. The material-liquid mass ratio of Ulmus davidiana var. japonica root bark to citrate buffer solution was 1:10. Then, at 45°C, 1% of the mass of Ulmus davidiana var. japonica root of complex enzyme preparation I (the mass ratio of ferulic acid esterase, cellulase, pectinase, and xylanase was 1:4:2:1) was added, and after enzymatic hydrolysis for 3h, it was inactivated by a water bath at 80°C for 10 minutes and then centrifuged (4000rpm, 15 minutes) to collect the supernatant to obtain the first enzymatic hydrolysis solution, and the residue was retained; the residue after centrifugation was redissolved in a phosphate buffer solution with pH 6.5 (the material-liquid mass ratio of Ulmus davidiana var. japonica root bark to phosphate buffer solution (0.1M) was 1:5). At 30°C, 0.5% of the mass of the residue of complex enzyme preparation II (the mass ratio of β-glucosidase and esterase was 2:1) was added and enzymatically hydrolyzed for 1h to obtain the secondary enzymatic hydrolysis solution. The first enzymatic hydrolysis solution and the secondary enzymatic hydrolysis solution were mixed, and 5 times the amount of absolute ethanol was added to make the alcohol content greater than 70%. It was refluxed and extracted at 55°C for 2h, extracted three times, filtered, and the three extraction solutions were combined. The extraction solution was recycled ethanol to obtain the extract of Ulmus davidiana var. japonica root.

[0055] Example 3:

[0056] The dry root bark of Ulmus davidiana var. japonica from Huadian City, Jilin City was cut and crushed to 60 mesh, and added to a citrate buffer solution (0.1M) with pH 5.0 containing 15% ethanol (ethanol and citrate buffer solution were mixed at a ratio of 1:1). It was pretreated by ultrasonic wave at 40°C and 200W for 20 minutes to obtain a crude extract of Ulmus davidiana var. japonica root. The material-liquid mass ratio of Ulmus davidiana var. japonica root bark to citrate buffer solution was 1:20. Then, at 55°C, 5% of the mass of Ulmus davidiana var. japonica root of complex enzyme preparation I (the mass ratio of ferulic acid esterase, cellulase, pectinase, and xylanase was 1:4:2:1) was added, and after enzymatic hydrolysis for 5h, it was inactivated by a water bath at 80°C for 10 minutes and then centrifuged (4000rpm, 15 minutes) to collect the supernatant to obtain the first enzymatic hydrolysis solution, and the residue was retained; the residue after centrifugation was redissolved in a phosphate buffer solution with pH 6.5 (the material-liquid mass ratio of Ulmus davidiana var. japonica root bark to phosphate buffer solution (0.1M) was 1:15). At 30°C, 1.5% of the mass of the residue of complex enzyme preparation II (the mass ratio of β-glucosidase and esterase was 2:1) was added and enzymatically hydrolyzed for 3h to obtain the secondary enzymatic hydrolysis solution. The first enzymatic hydrolysis solution and the secondary enzymatic hydrolysis solution were mixed, and 5 times the amount of absolute ethanol was added to make the alcohol content greater than 70%. It was refluxed and extracted at 55°C for 2h, extracted three times, filtered, and the three extraction solutions were combined. The extraction solution was recycled ethanol to obtain the extract of Ulmus davidiana var. japonica root.

[0057] Comparative Example 1: Except for no ultrasonic pretreatment, other operations were the same as in Example 1.

[0058] Comparative Example 2: Except for no secondary enzymatic hydrolysis, other operations were the same as in Example 1.

[0059] Comparative Example 3: Spring elm root extract extracted with ordinary ethanol: Take the dried spring elm root bark, cut and crush it, and add 5 times the amount of anhydrous ethanol to make the alcohol content greater than 70%. Reflux and extract at 55°C for 2 hours, extract three times, filter, and combine the three extraction solutions.

[0060] Comparison of the differences in the content of main active ingredients and antioxidant activities among the spring elm root extracts obtained in Examples 1-3 and Comparative Examples 1-3.

[0061] 1. Determination of total phenols

[0062] Refer to the Folin-Ciocalteu method

[0063] 2. Determination of total sugars

[0064] Refer to the phenol-sulfuric acid method

[0065] 3. Determination of DPPH free radical scavenging ability

[0066] Refer to "Cosmetics - Free Radical (DPPH) Scavenging Test Method"

[0067] 3. FRAP ferric ion reducing ability determination

[0068] Determine the total antioxidant capacity by referring to the FRAP method

[0069] The results of the active substance content and antioxidant capacity of Examples 1-3 and Comparative Examples 1-3 are shown in Table 1:

[0070] Table 1 Comparison of active substance content and antioxidant capacity of examples and comparative examples

[0071]

[0072] It can be seen from this that the molecules of the spring elm root extract extracted based on the present invention are different in quality and quantity from the molecules described in the prior art. The extract of the present invention is different from the conventional spring elm root extract in that its total phenol and total sugar contents are significantly increased. It has been demonstrated in the examples of the present invention that the spring elm root extract obtained by this method has stronger antioxidant efficacy than the spring elm root extract obtained by the conventional method.

[0073] For the spring elm root extract extracted by the present invention, the effective active ingredients are specifically increased, and it has been confirmed that in addition to the anti-inflammatory effect, the spring elm root extract also has the effect of anti-skin aging, especially the firming effect, and has good prospects for application in cosmetic products.

[0074] The extract of Ulmus propinqua Koidz. root can be applied to personal care products with anti-aging and firming effects. Preferably, the extract of Ulmus propinqua Koidz. root serves as an antioxidant active ingredient and / or a skin firming active ingredient in the personal care products.

[0075] The personal care products include one or more of lotion, cream, essence, and facial mask. Further, the types of components in the personal care products also include solvent, humectant, thickener, preservative, emulsifier, surfactant, auxiliary, fragrance, whitening agent, and anti-aging agent.

[0076] The following combines specific examples to further verify the extract of Ulmus propinqua Koidz. root of the present invention and its specific application effects in cosmetic products.

[0077] 1. Effects of the extract of Ulmus propinqua Koidz. root prepared according to Example 1 on the synthesis genes of collagen and elastin:

[0078] Referring to T / ZHCA 015-2022 "Method for Evaluating the Firming Effect of Cosmetics - Relative Expression Level of Elastin Gene in Zebrafish Larvae", the relative expression levels of collagen genes (col1a1a, col1a1b, and col1a2) and elastin gene (Elna) were measured. The results are as Figure 1 and Figure 2 shown.

[0079] Figure 1 is the bar chart of the relative expression level of type I collagen gene in zebrafish *p < 0.05, Figure 2 is the bar chart of the relative expression level of elastin gene in zebrafish *p < 0.05. From the bar chart results, it can be seen that the extract of Ulmus propinqua Koidz. root obtained in the present invention can promote the synthesis of type I collagen and elastin by increasing the expression levels of collagen and elastin-related genes, further proving its certain anti-wrinkle and firming effects.

[0080] 2. Select the extract of Ulmus propinqua Koidz. root prepared in Example 1 to prepare a lotion containing 2% extract of Ulmus propinqua Koidz. root for a human efficacy test. The formula is as follows:

[0081]

[0082] Process steps: Phase A pre-mixes butylene glycol, xanthan gum, and HA. Accurately weigh Phase A, heat it in a water bath at 80°C, homogenize it rapidly for 5 min until uniform, keep it warm for 20 min and then start cooling; when it cools to 60°C, accurately weigh Phase B, add Phase B to Phase A, homogenize for 1 - 3 min, stir for 15 - 30 min until well-mixed; discharge at 40°C and let it stand for 24 h.

[0083] Twenty-eight healthy Chinese subjects aged 18 to 55 years (4 males and 24 females) were selected to continuously use the test sample for 28 days under normal conditions. No adverse events occurred during the test period, and no adverse reactions were observed in all subjects. The results showed that the test product had good safety.

[0084] The skin elasticity R2 value and F4 value were measured using a Cutometer skin elasticity tester (probe aperture: 2 mm) (Courage&Khazaka, Germany). The results are shown in Tables 2 and 3.

[0085] Test requirements: Take the average value after testing three times.

[0086] Detection site: Below the cheekbones of the face.

[0087] Parameter explanation: The F value is the area value within the envelope curve formed during the application and elimination of negative pressure in all test cycles, that is, the F4 value of the Cutometer skin elasticity tester. The smaller the value, the tighter the skin.

[0088] The R value is the ratio of the skin's rebound displacement after the first elimination of negative pressure to the maximum tensile displacement of the skin during the first application of negative pressure, that is, the R2 value of the Cutometer skin elasticity tester. The closer the value is to 1, the better the skin elasticity.

[0089] Table 2: Comparison of skin elasticity F4 before and after use

[0090]

[0091] Table 3: Comparison of skin elasticity R2 before and after use

[0092]

[0093] The instrument results showed that after 14 days of continuous use of the test product, the skin elasticity R2 value increased significantly by 8.70% (P < 0.001); after 28 days of use, the skin elasticity R2 value increased significantly by 9.36% (P = 0.006), and the F4 value decreased significantly by 30.92% (P < 0.001). That is, after 28 days of using the lotion containing 2% Ulmus davidiana var. japonica root extract, the skin elasticity and firmness were significantly improved.

[0094] Moreover, the VISIA shooting results showed that after 28 days of use, the ultraviolet spot feature count decreased by 14.62% (as Figure 3 shown), and the brown spot feature count decreased by 13.29% (as Figure 4 shown).

[0095] Among them, the usage results of a certain volunteer are as Figure 5As shown, its freckles are -41.93%, ultraviolet freckles are -14.43%, and brown spots are -28.95%.

[0096] In summary, the cosmetics containing the spring elm root extract obtained by the method of the present invention have the effects of significantly improving skin elasticity and firmness, and reducing ultraviolet freckles and brown spots.

[0097] The above embodiments are not limitations of the present invention, and the present invention is not limited to the above examples. Changes, modifications, additions, or substitutions made by those skilled in the art within the scope of the technical solution of the present invention also fall within the protection scope of the present invention.

Claims

1. A method for extracting an extract of Ulmus propinqua Koidz. roots, characterized in that: The extraction method is as follows: Ultrasound-assisted staged enzymatic hydrolysis is adopted to decompose the root bark of Ulmus propinqua Koidz. through the special activities of various enzymes, so as to extract the effective active ingredients in the root bark of Ulmus propinqua Koidz. to the maximum extent; The effective active ingredients include polyphenols and polysaccharides, and the various enzymes include complex enzyme preparation I and complex enzyme preparation II.

2. The extraction method of the slippery elm root extract according to claim 1, characterized in that: It includes the following steps: S1. Take the dried root bark of Ulmus propinqua Koidz., cut and crush it to 40-60 meshes, and then add it to a pH 5.0 citrate buffer solution containing ethanol for ultrasonic pretreatment to obtain a crude extract of Ulmus propinqua Koidz. S2. Then add complex enzyme preparation I at 45°C - 55°C, enzymatically hydrolyze for 3 - 5 h, inactivate it in a water bath at 80°C for 10 minutes, and then centrifuge to collect the supernatant to obtain the first enzymatic hydrolysate. The residue is retained. The centrifugation conditions are: 4000 rpm, 15 minutes; S3. The residue after centrifugation is redissolved in a pH 6.5 phosphate buffer solution, and complex enzyme preparation II is added at 30°C - 50°C for enzymatic hydrolysis for 1 - 3 h to obtain a secondary enzymatic hydrolysate; S4. Mix the first enzymatic hydrolysate and the second enzymatic hydrolysate, add 5 times the amount of absolute ethanol to make the alcohol content greater than 70%, reflux and extract at 50°C - 60°C for 2 h, extract three times, filter, combine the three extracts, recover ethanol from the extract, and obtain the extract of Ulmus propinqua Koidz.

3. The extraction method of the slippery elm root extract according to claim 2, characterized in that: In step S1, the material-liquid mass ratio of the root bark of Ulmus propinqua Koidz. to the citrate buffer solution is 1:10 - 20; The mass concentration of the citrate buffer solution is 0.1 M, which is mixed by ethanol and citrate buffer solution in a ratio of 1:1, and the final concentration of ethanol ≤ 15%; In step S1, the ultrasonic conditions are: ultrasonic pretreatment at 40°C and 200 W for 10 - 20 minutes.

4. The extraction method of the slippery elm root extract according to claim 2, characterized in that: In step S2, the composition components and mass ratio of the complex enzyme preparation I are: ferulic acid esterase, cellulase, pectinase, and xylanase in a ratio of 1:4:2:1; the addition amount of complex enzyme I is 1 - 5% of the mass of the root bark of Ulmus propinqua Koidz.

5. The extraction method of the slippery elm root extract according to claim 1, characterized in that: In step S3, the material-liquid mass ratio of the root bark of Ulmus propinqua Koidz. to the phosphate buffer solution is 1:5 - 15, and the mass concentration of the phosphate buffer solution is 0.1 M.

6. The extraction method of the extract of Ulmus propinqua Koidz. root according to claim 1, characterized in that: In step S3, the composition components and mass ratio of the complex enzyme preparation II are: β-glucosidase and esterase in a ratio of 2:1, and the addition amount of complex enzyme II is 0.5 - 1.5% of the mass of the residue.

7. A kind of Ulmus propinqua Koidz. root extract, characterized in that: It is obtained by using the extraction method of the extract of the root bark of Ulmus propinqua Koidz. described in any one of claims 1 - 6; The content of the main characteristic components in the extract of the root bark of Ulmus propinqua Koidz. obtained by extraction is: The total phenolic content is 20.5 - 46.8 mg GAE / g DW, and the total sugar content is 189.0 - 215.6 mg GE / g DW.

8. Use of the extract of Ulmus propinqua Koidz. root according to claim 7, characterized in that: The extract of the root bark of Ulmus propinqua Koidz. is used as an antioxidant active ingredient and / or a skin-tightening active ingredient in personal care products.

9. Use of the extract of Ulmus davidiana var. japonica roots according to claim 8, characterized in that: The personal care products include one or more of lotion, cream, essence, and mask.

10. The application of the extract of Ulmus davidiana var. japonica roots according to claim 9, characterized in that: The types of composition components in the personal care products also include solvent, humectant, thickener, preservative, emulsifier, surfactant, auxiliary, essence, whitening agent, and anti-aging agent.

Citation Information

Patent Citations

  • Skin-care composition containing an ulmus davidiana root extract

    CN109602658A

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