A firming anti-wrinkle cream containing extract of myrobalan

The preparation of an extract rich in tannic acid and gallic acid by hydrolyzing gallnut with glycosidase solves the problem of scarce tannic acid hydrolase resources, realizes the preparation of multifunctional ingredients in cosmetics, and enhances the firming and anti-wrinkle effect.

CN117323280BActive Publication Date: 2026-02-10WUFENG CHICHENG BIOTECH +1
View PDF 2 Cites 0 Cited by

Patent Information

Application Number
CN202311313949.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-10-11
Publication Date
2026-02-10
Estimated Expiration
2043-10-11

AI Technical Summary

Technical Problem

In the current technology, tannic acid hydrolase resources are scarce and costly, making it difficult to effectively prepare gallnut extract rich in various functional ingredients, resulting in poor effects of firming and anti-wrinkle cosmetics.

Method used

Gallnut was hydrolyzed using glycosidase to prepare a gallnut extract rich in tannic acid and gallic acid. This extract was then combined with other cosmetic ingredients to prepare a firming and anti-wrinkle face cream.

Benefits of technology

Gallnut extract is rich in various components that can effectively inhibit elastase, promote the synthesis of type I collagen, and reduce MMP-1 secretion, thus achieving better firming and anti-wrinkle effects at a lower cost.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure BDA0004488799540000021
    Figure BDA0004488799540000021
  • Figure BDA0004488799540000041
    Figure BDA0004488799540000041
  • Figure BDA0004488799540000061
    Figure BDA0004488799540000061
Patent Text Reader

Abstract

The application discloses a firming and anti-wrinkle cream containing a gallnut extract, and belongs to the field of cosmetics. The gallnut medicine is extracted, and glycosidase is used to hydrolyze tannic acid into gallic acid, so that the hydrolysis conversion efficiency can be controlled, the prepared gallnut extract can better inhibit elastase, promote type I collagen synthesis and reduce the secretion of MMP-1, and thus the prepared cosmetic has better firming and anti-wrinkle effects.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This invention belongs to the field of cosmetics, specifically relating to a firming and anti-wrinkle face cream containing gallnut extract. Background Technology

[0002] Gallnut extract is a common cosmetic ingredient. Gallnuts are rich in tannic acid (also known as tannin), which, according to studies, has various pharmacological effects such as antibacterial, anti-inflammatory, astringent, and hemostatic properties, making it a common pharmaceutical raw material. The structure of tannic acid is still unclear, but it is generally believed to be an ester formed by the combination of the five hydroxyl groups of glucose and galloyl group. Tannic acid is highly water-soluble, and a high concentration can be obtained by extracting and refining gallnuts.

[0003] Tannic acid can be hydrolyzed to remove glycosides, yielding gallic acid, a polyphenol compound. Studies have shown that most plant polyphenols possess strong antioxidant properties, scavenging free radicals and protecting cells from oxidative damage. Currently, to achieve the industrial production of gallic acid, the commonly used methods for tannic acid hydrolysis include acid-base methods, fermentation, and enzymatic methods. Among these, acid-base and fermentation methods are difficult to control and easily generate byproducts. In contrast, enzymatic methods offer milder reaction conditions and precise controllable enzyme cleavage sites, which helps reduce byproducts.

[0004] The most commonly used enzyme for the hydrolysis of tannic acid is tanninase, a hydrolytic enzyme produced by fungi (mainly Aspergillus niger) through extraspore induction. It can directionally cleave ester bonds, phenolic bonds, and glycosidic bonds in tannic acid molecules, generating gallic acid. Tanninase has a high enzymatic hydrolysis efficiency; literature shows that the hydrolysis conversion rate of tannic acid using tanninase can reach over 98%. However, with the increasing scarcity of fungal and tanninase resources, there is an urgent need to find other alternative tannic acid hydrolytic enzymes. Glycoside hydrolases are a class of enzymes that can hydrolyze the glycosidic bonds in various sugar-containing compounds (including monosaccharides, oligosaccharides, polysaccharides, saponins, and glycoproteins) via endo- or exo-cleavage. They are currently widely used in drug production and synthesis. For example, Zhang Liying et al., through research on the role of glycoside hydrolases in the biotransformation of traditional Chinese medicine components, derived a method for converting geniposide to geniposide using glycoside hydrolases (Zhang Liying 2012).

[0005] Unlike tanninases, glycoside hydrolases are present in almost all organisms, making them more widely available and less expensive. More importantly, glycoside hydrolases can only convert a portion of tannic acid into gallic acid, resulting in products rich in various chemical components that possess multiple functions, including antibacterial, anti-inflammatory, astringent, hemostatic, and antioxidant properties. Therefore, they hold promise for better performance in pharmaceuticals.

[0006] Based on this, the present invention provides a firming and anti-wrinkle face cream containing gallnut extract. This cosmetic uses glycosidase to hydrolyze the key ingredient gallnut, resulting in a product rich in various components. Experiments show that the prepared gallnut extract can more effectively inhibit elastase, promote type I collagen synthesis, and reduce MMP-1 secretion. Therefore, it can be used as the main ingredient in firming and anti-wrinkle cosmetics and exert its excellent effects. Summary of the Invention

[0007] The purpose of this invention is to provide a firming and anti-wrinkle face cream containing gallnut extract, which aims to improve the firming and anti-wrinkle effects of cosmetics.

[0008] The firming and anti-wrinkle face cream provided by this invention is made from the following raw materials in the indicated weight ratios:

[0009]

[0010] The active ingredient is gallnut extract; the auxiliary active ingredients are selected from one or more of caffeine, horse chestnut extract, hydroxypropyl tetrahydropyrantriol, glycosphingolipids, allantoin, anti-aging and skin-sculpting extract, tocopheryl acetate, and vitrazol; the anti-allergic agent is selected from one or more of betaine, dipotassium glycyrrhizate, and water-soluble total glycosides of Centella asiatica; the skin feel modifier is selected from one or more of behenol, triolein, tocopherol, cetyl ethylhexanoate, trimethylolpropionyl lactone crosspolymer, silica, and plant oils; and the pH adjuster is tetrahydroxypropyl ethylenediamine.

[0011] The preparation method of the gallnut extract includes the following steps:

[0012] (1) Take gallnut medicinal material, crush it, add water for warm soaking and extraction, filter the extract, centrifuge and concentrate and dry it, and wash it with ether to obtain crude gallnut extract.

[0013] (2) The crude extract was redissolved in water to prepare a solution with a solid content of 10-30%. Then, glycosidase was added to make the enzyme content 20-100 U / ml and the pH was adjusted to 4-6. Then, it was heated to 40-60℃ for hydrolysis. After 2-5 hours, it was heated to boiling to inactivate the enzyme. After centrifugation, it was concentrated and dried to obtain a gallnut extract rich in tannic acid and gallic acid.

[0014] In the above method for preparing gallnut extract, step (1) is to extract tannic acid. A crude tannic acid extract with high content can be obtained by defatting and decolorizing. The extraction temperature, water addition amount and time affect the purity and yield of the product and can be further optimized. Step (2) is to hydrolyze and convert tannic acid. The conversion efficiency can be controlled by using glycosidase to obtain gallnut extract containing both tannic acid and gallic acid. The amount of enzyme added, temperature, pH and time of hydrolysis also have a significant effect on the conversion efficiency.

[0015] The glycosidases mentioned include, but are not limited to, one or more of β-glucosidase, α-mannosidase, β-galactosidase, α-amylase, and β-glucanase. The applicant investigated the effects of various enzyme hydrolysates on elastase activity, type I collagen synthesis, and MMP-1 secretion by detecting the tannic acid and gallic acid content in the hydrolysates and by examining in vitro enzyme activity and cell experiments. Ultimately, α-mannosidase was selected as the optimal hydrolytic enzyme. This enzyme not only exhibits strong activity and high hydrolysis efficiency, but its hydrolysates also demonstrate higher activity in inhibiting elastase, promoting type I collagen synthesis, and reducing MMP-1 secretion, thus making it better suited for cosmetic applications.

[0016] More preferably, the enzyme content is 40-60 U / ml.

[0017] More preferably, the pH is 5-5.5.

[0018] More preferably, the hydrolysis temperature is 45-50℃.

[0019] More preferably, the hydrolysis time is 3-4 hours.

[0020] According to one embodiment of the present invention, a method for preparing a more effective gallnut extract is as follows:

[0021] (1) Take gallnut medicinal material, crush it and pass it through a 40-mesh sieve. Then add 15 times the weight of water and heat it to 60°C for warm soaking extraction. After 3 hours, filter it and centrifuge the filtrate with a tubular centrifuge at 5000 r / min. After vacuum concentration of the centrifuged liquid, freeze dry it and finally wash it with ether 3-5 times. After evaporating the residual organic solvent, obtain the crude gallnut extract.

[0022] (2) The crude extract was redissolved in water to prepare a solution with a solid content of 15%. Then, α-mannosidase was added to the aqueous solution to make the enzyme content reach 50 U / ml. The pH was adjusted to 5.5 with HCl or NaOH. The mixture was then heated to 45°C for reaction. After 4 hours, the mixture was boiled for 0.5 hours to inactivate the enzyme. The mixture was centrifuged at 5000 r / min, concentrated under vacuum, and then freeze-dried to obtain a gallnut extract rich in tannic acid and gallic acid.

[0023] The gallnut extract prepared under the above-mentioned optimal conditions also has the advantages of high product purity and high yield.

[0024] Preferably, the emulsifier is selected from one or more of polyglycerol-10 myristate, potassium lauryl phosphate, acrylate / acrylamide copolymer, polyglycerol-10 distearate, mineral oil, and polysorbate-85.

[0025] Preferably, the antioxidant is p-hydroxyacetophenone.

[0026] Preferably, the chelating agent is trisodium ethylenediamine disuccinate.

[0027] More preferably, the weight ratio of the raw materials is:

[0028]

[0029] The beneficial effects of this invention are:

[0030] This invention is the first to achieve the preparation of gallnut extract by using glycosidase, which not only enriches the types of tannic acid hydrolases and reduces the cost of hydrolases, but also, compared with existing hydrolases such as tanninase, the hydrolysate of this invention is rich in a variety of components, which enables the extract to better inhibit elastase, promote type I collagen synthesis and reduce MMP-1 secretion, and thus can be better applied to firming and anti-wrinkle cosmetics.

[0031] The face cream provided by this invention has a delicate texture, is comfortable and non-irritating to use, is quickly absorbed by the skin, has good product stability, and can be stored for 3 years at room temperature. Detailed Implementation

[0032] The present invention will be described in detail below with reference to specific embodiments.

[0033] All gallnut materials used in the examples were purchased from the same batch of products from the same company. β-glucosidase, β-galactosidase, α-amylase, β-glucanase, and tanninase were purchased from Shanghai Yuanye, and α-mannosidase was purchased from Macklin. The enzyme activities of all enzymes were between 10 and 600 U / mg. Other materials whose sources were not specified were all conventional materials in the art.

[0034] The methods for determining the content of tannic acid and gallic acid involved in the examples are as follows:

[0035] Tannic acid content determination: determined according to high performance liquid chromatography (General Rule 0512).

[0036] Chromatographic conditions and system suitability tests were conducted using octadecylsilane-bonded silica gel as the stationary phase; 1% phosphoric acid water: methanol (80:20) as the mobile phase; and a detection wavelength of 275 nm. The theoretical plate number, calculated based on the tannic acid peak, should be no less than 4000.

[0037] Preparation of the reference solution: Take an appropriate amount of tannic acid reference standard (purity >98%, Shanghai Yuanye Biotechnology Co., Ltd.), accurately weigh it, add water to make a solution containing 100 μg per 1 mL.

[0038] Preparation of the test solution: Weigh approximately 1 mg of gallnut extract accurately, place it in a beaker, add water and stir until fully dissolved, transfer to a brown volumetric flask, add water to make up to 10 mL, shake well, and prepare a solution containing 100 μg per mL.

[0039] The assay involves precisely pipetting 10 μL of the reference solution and 10 μL of the test solution into a liquid chromatograph and measuring the results.

[0040] Gallic acid content determination: determined according to high performance liquid chromatography (General Rule 0512).

[0041] Chromatographic conditions and system suitability tests were conducted using octadecylsilane-bonded silica gel as the stationary phase; 1% phosphoric acid water: methanol (95:5) as the mobile phase; and a detection wavelength of 275 nm. The theoretical plate number, calculated based on the gallic acid peak, should be no less than 3000.

[0042] Preparation of the reference solution: Take an appropriate amount of gallic acid reference standard (China National Institutes for Food and Drug Control, content calculated as 91.5%), accurately weigh it, add water to prepare a solution containing 100 μg per 1 mL.

[0043] Preparation of the test solution: Take an appropriate amount of gallnut extract, accurately weigh it, add water to make a solution containing 100 μg per 1 mL.

[0044] The assay involves precisely pipetting 10 μL of the reference solution and 10 μL of the test solution into a liquid chromatograph and measuring the results.

[0045] Example 1: Preparation of Gallnut Extract

[0046] Studies have shown that gallnut is rich in tannins and polyphenols. Tannins have antibacterial and astringent effects, while polyphenols have antioxidant effects. Most naturally occurring plant polyphenols exist in the form of bound glycosides. Therefore, this invention uses the following process to extract gallnuts in order to obtain higher contents of tannins and polyphenols.

[0047] Process flow: After the raw material is crushed, it is extracted by soaking in water at a low temperature. The extract is centrifuged to remove impurities, concentrated and dried, washed and decolorized with ether, reconstituted with water, and hydrolyzed with glycosidase (screening for glycosidase types, hydrolysis temperature, pH and time). The extract is then heated to inactivate, centrifuged, concentrated and dried, and the content of tannic acid and gallic acid in the extract is detected.

[0048] Several commonly used hydrolytic enzymes were screened from literature reports, namely β-glucosidase, α-mannosidase, β-galactosidase, α-amylase, β-glucanase, and tanninase, a total of six enzymes. Their cleavage sites are different. Among them, β-glucosidase mainly hydrolyzes β-D-glucose bonds and releases β-D-glucose and the corresponding ligand; α-mannosidase catalyzes the hydrolysis of α-mannose residues at the end of mannoside; β-galactosidase can catalyze the hydrolysis of β-galactosides into monosaccharides; α-amylase can catalyze the hydrolysis of α-1,4-glycosidic bonds of starch; β-glucanase acts on the 1,3 and 1,4 glycosidic bonds of β-glucan to generate oligosaccharides and glucose; and tanninase can hydrolyze ester bonds, phenolic bonds and glycosidic bonds in the tannic acid molecule.

[0049] The test method is as follows:

[0050] (1) Extraction of medicinal materials: Gallnut medicinal materials were taken, pulverized, and passed through a 40-mesh sieve. Then, 15 times its weight of water was added and heated to 60℃ for warm extraction. After 3 hours, the mixture was filtered, and the filtrate was centrifuged in a tubular centrifuge at 5000 r / min. The centrifuged liquid was concentrated under vacuum and then freeze-dried. Finally, it was washed 3-5 times with ether to evaporate the residual organic solvent and obtain crude gallnut extract. The crude extract was found to contain 71.7% tannins and 4.9% gallic acid.

[0051] (2) The crude extract was redissolved in water to prepare a solution with a solid content of 15%. Different hydrolytic enzymes were added to the aqueous solution to make the enzyme content reach 50 U / ml. The pH was adjusted to 5.5 with HCl or NaOH. The reaction was then carried out at 45°C. After 4 hours, the solution was boiled for 0.5 hours to inactivate the enzymes. The solution was centrifuged at 5000 r / min, concentrated under vacuum, and then freeze-dried. The contents of tannic acid and gallic acid were detected. The results are shown in the table below.

[0052] Sample number Types of hydrolytic enzymes Tannic acid content (%) Gallic acid content (%) Sample 1 β-glucosidase 21.7 51.3 Sample 2 α-Mannosidase 34.0 30.8 Sample 3 β-galactosidase 58.5 14.1 Sample 4 α-Amylase 41.3 9.9 Sample 5 β-glucanase 55.4 13.6 Sample 6 Tanninase 1.7 69.9

[0053] The experimental results showed that all five glycosidases could only partially hydrolyze tannic acid. In terms of hydrolysis capacity, β-glucosidase and α-mannosidase had stronger activities and produced more gallic acid; α-amylase produced more byproducts and less total tannic acid and gallic acid; β-galactosidase and β-glucanase had lower conversion capacity and produced less gallic acid; tanninase could almost completely hydrolyze tannic acid, producing a large amount of gallic acid. This result is basically consistent with the literature reports.

[0054] Example 2: Evaluation of the firming and anti-wrinkle effects of gallnut extract

[0055] To further investigate the firming and anti-wrinkle effects of different enzymatic hydrolysates, the following experiments were conducted on the six samples prepared in Example 1 to investigate their inhibitory activity on elastase and their effects on type I collagen and MMP-1.

[0056] I. Elastase Inhibition Experiment of Gallnut Extract

[0057] Elastase is a highly selective and specific protein-degrading enzyme that catalyzes the hydrolysis of many amino acids. It can break down elastin in connective tissue proteins. Inhibiting elastase activity can effectively slow down the degradation rate of elastin, reducing skin aging and the formation of wrinkles.

[0058] 1. Test materials

[0059]

[0060]

[0061] 2. Test methods

[0062] 2.1 Preparation of reagents and samples

[0063] Test sample solution: Dissolve the gallnut extract in water to prepare a test sample solution with a concentration of 50 mg / mL.

[0064] Positive control solution: Dissolve sodium cefotaxime in water to prepare a positive control solution with a concentration of 0.015 mg / mL.

[0065] Elastase solution: Weigh elastase, add Tris-HCl buffer (pH 8.2, preheated at 25℃) to dissolve, and prepare an enzyme solution with a concentration of 10 U / mL.

[0066] Substrate solution: Weigh N-succinyl-Ala-Ala-Ala-p-nitroanilide (NAAAPN), dissolve it in Tris-HCl buffer (pH 8.2, preheated at 25°C) to prepare a substrate solution with a concentration of 0.5 mg / mL.

[0067] 2.2 Experimental Procedure

[0068] Elastase can hydrolyze the substrate NAAAPN, and the resulting p-nitroaniline has absorbance at 405 nm. By using spectrophotometry to detect the absorbance value at 405 nm, the enzyme activity inhibition rate of the drug can be calculated.

[0069] In a 96-well plate, 25 μL of elastase solution was added to 50 μL of sample solution, followed by 100 μL of Tris-HCl buffer (pH 8.2), and incubated at 25 °C for 20 min. After incubation, 25 μL of substrate solution was added, the mixture was immediately vortexed, and the absorbance A1 was measured at 405 nm. The absorbance A2 was then measured again after incubation at 25 °C for 10 min. The value of ΔA(A2-A1) for each group was calculated to determine the enzyme inhibition rate.

[0070] Formula for calculating enzyme inhibition rate:

[0071]

[0072] In the formula: A: is the mean absorbance of the experimental group (T) or the positive control group (PC); A NC : Mean absorbance of the blank control group (NC group); A TC : Mean absorbance of the control group (TC group)

[0073] 3. Test Results

[0074] The elastase inhibition rates of each sample in Example 1 are shown in the table below.

[0075] Test sample Inhibition rate (%) Sample 1 40.0±0.19 Sample 2 46.5±0.18 Sample 3 36.7±0.22 Sample 4 23.3±0.13 Sample 5 28.6±0.07 Sample 6 17.1±0.18 Sample 7 8.8±0.05 Positive control 63.3±0.18

[0076] Sample 7 is the crude extract prepared in Example 1, which contains 71.7% tannic acid and 4.9% gallic acid.

[0077] The results showed that the gallnut extract prepared by the five glycosidases inhibited the activity of elastase much more than that of tanninase. This result may be related to the fact that the extract contains both tannic acid and gallic acid.

[0078] II. Effects of Gallnut Extract on Type I Collagen and MMP-1

[0079] Type I collagen is a major component of the dermal extracellular matrix, and human dermal fibroblasts can serve as a cell model for studying how cosmetics can increase type I collagen levels. Matrix metalloproteinase-1 (MMP-1) has the ability to degrade the extracellular matrix; increased MMP-1 secretion accelerates collagen degradation, leading to collagen loss in the skin, resulting in sagging skin, decreased elasticity, and increased fine lines. Therefore, the anti-wrinkle efficacy of extracts and cosmetics can be evaluated by measuring the type I collagen and MMP-1 content in dermal fibroblasts.

[0080] 1. Experimental materials

[0081]

[0082]

[0083] 2. Experimental Methods

[0084] 2.1 Preparation of reagents and samples

[0085] The cryopreserved human skin fibroblast culture was passaged once in the culture medium, and then seeded into the culture medium at an appropriate density for the experiment. The cell seeding density should ensure that the confluence reaches 45-60% after 24 hours of seeding.

[0086] The gallnut extract prepared in Example 1 was dissolved in PBS, centrifuged at 5000 r / min for 5 min, and the supernatant was collected and filtered through a 0.22 μm microporous membrane. Then it was diluted with culture medium to a test sample solution with a concentration of 5 mg / mL.

[0087] Positive control: 200 ng / mL TGF-β1;

[0088] Blank control: Added with normal cell culture medium

[0089] 2.2 Experimental Procedure

[0090] Plate 96-well plates and incubate for 24 hours in an incubator (37°C, 5% CO2). Discard the culture medium from the 96-well plates and proceed with the drug administration. Add culture medium containing the test substance to the test wells, culture medium containing the positive control to the positive control wells, and normal cell culture medium to the blank control wells, 100 μL per well. After drug administration, incubate the 96-well plates in a CO2 incubator for 24 h ± 2 h. After incubation, collect approximately 100 μL of cell culture supernatant from each well into a 1.5 mL sterile centrifuge tube, and then perform ELISA assays according to the kit instructions.

[0091] 3. Experimental Results

[0092] The type I collagen content measured in each sample in Example 1 is shown in the table below.

[0093] Test sample COLⅠ content (ng / ml) Sample 1 17.3±0.12 Sample 2 16.8±0.09 Sample 3 13.9±0.11 Sample 4 13.5±0.17 Sample 5 14.0±0.13 Sample 6 12.1±0.04 Sample 7 14.3±0.15 Positive control 18.3±0.19 Blank control 10.9±0.15

[0094] Sample 7 is the crude extract prepared in Example 1, which contains 71.7% tannic acid and 4.9% gallic acid.

[0095] The results showed that, compared with the blank control, the content of type I collagen in each experimental group and the positive control group was significantly upregulated (P<0.05), indicating that gallnut extract has the ability to promote the synthesis of type I collagen, and the activity of glycosidase hydrolysis products is significantly higher than that of tanninase.

[0096] The MMP-1 content measured in each sample in Example 1 is shown in the table below.

[0097] Test sample MMP-1 content (ng / ml) Sample 1 61.3±0.17 Sample 2 60.7±0.06 Sample 3 62.5±0.11 Sample 4 63.1±0.16 Sample 5 62.2±0.22 Sample 6 63.4±0.19 Sample 7 62.9±0.20 Blank control 64.5±0.17

[0098] Sample 7 is the crude extract prepared in Example 1, which contains 71.7% tannic acid and 4.9% gallic acid.

[0099] The results showed that MMP-1 levels were downregulated in all experimental groups compared to the blank control, indicating that gallnut extract has the effect of reducing MMP-1 secretion.

[0100] Since the hydrolysis products of α-mannosidase have higher activity than other glycosidases, sample 2 was selected, that is, α-mannosidase was used as the hydrolase to hydrolyze gallnut.

[0101] Example 3: Preparation of Gallnut Extract

[0102] (1) Extraction of medicinal materials: Gallnut medicinal materials were crushed and passed through a 40-mesh sieve. Then, 12 times its weight of water was added and heated to 70℃ for warm extraction. After 2 hours, the mixture was filtered, and the filtrate was centrifuged in a tubular centrifuge at 5000 r / min. The centrifuged liquid was concentrated under vacuum and then freeze-dried. Finally, it was washed 3-5 times with ether to evaporate the residual organic solvent and obtain crude gallnut extract. The crude extract was found to contain 65.2% tannic acid and 3.7% gallic acid.

[0103] (2) The crude extract was reconstituted with water to prepare a solution with a solid content of 12.5%. Then, α-mannosidase was added to the aqueous solution to achieve an enzyme concentration of 70 U / ml. The pH was adjusted to 5.0 with HCl or NaOH. The mixture was then heated to 50°C for 2.5 h, followed by boiling for 0.5 h to inactivate the enzyme. The mixture was then centrifuged at 5000 r / min, concentrated under vacuum, and freeze-dried. The product contained 26.5% tannic acid and 29.7% gallic acid.

[0104] Example 4: Preparation of Gallnut Extract

[0105] (1) Extraction of medicinal materials: Gallnut medicinal materials were crushed and passed through a 40-mesh sieve. Then, 8 times its weight of water was added and heated to 55℃ for warm extraction. After 5 hours, the mixture was filtered, and the filtrate was centrifuged in a tubular centrifuge at 5000 r / min. The centrifuged liquid was concentrated under vacuum and then freeze-dried. Finally, it was washed 3-5 times with ether to evaporate the residual organic solvent and obtain crude gallnut extract. The crude extract was found to contain 69.3% tannic acid and 4.1% gallic acid.

[0106] (2) The crude extract was reconstituted with water to prepare a solution with a solid content of 20%. Then, α-mannosidase was added to the aqueous solution to achieve an enzyme concentration of 25 U / ml. The pH was adjusted to 6.0 with HCl or NaOH. The mixture was then heated to 40°C for 5 hours, followed by boiling for 0.5 hours to inactivate the enzyme. The mixture was then centrifuged at 5000 r / min, concentrated under vacuum, and freeze-dried. The product contained 24.5% tannic acid and 22.6% gallic acid.

[0107] Example 5: Firming and Anti-wrinkle Face Cream Containing Gallnut Extract

[0108] formula:

[0109]

[0110]

[0111] Raw material description:

[0112] Vifuzhi: Composed of multiple active peptides, it can block the nerve signal transmission that leads to wrinkle formation at multiple targets, thereby exerting an anti-wrinkle effect. Purchased from Foshan Kejia Biotechnology Co., Ltd.

[0113] Glycosphingolipids: These are compounds of N-acylsphingosine and oligosaccharides, which can improve skin hydration and enhance the skin barrier.

[0114] Anti-aging and skin-sculpting formula extract: Extracts from eight herbs including Ophiopogon japonicus, Tremella fuciformis, Dendrobium nobile, Carthamus tinctorius, Ganoderma lucidum, Astragalus membranaceus, Ginseng, and Salvia miltiorrhiza. Traditional Chinese medicine believes it has the effects of replenishing qi and blood, promoting blood circulation, and delaying aging. Modern medicine has found that it has the effects of scavenging free radicals, reducing cell apoptosis, and anti-aging. Purchased from Shanghai Zhina Biotechnology Co., Ltd.

[0115] Preparation process:

[0116] 1. Mix the raw materials polyglycerol-10 myristate, polyglycerol-10 distearate, behenol, trimethylolhexyl lactone crosspolymer, silica, cetyl ethylhexanoate, triolein, tocopherol, and vegetable oil evenly and heat to 85°C to obtain phase A;

[0117] 2. Mix the raw materials carbomer, acrylate / C10-30 alkyl acrylate crosspolymer, trisodium ethylenediamine disuccinate, cyclodextrin, PEG-40 hydrogenated castor oil, diglycerides, sodium hyaluronate, butanediol, and water until homogenized, and heat to 80°C to obtain phase B.

[0118] 3. Add phase B to phase A, reheat to 85℃ and homogenize for 10 min, keep warm for 10 min, then cool to 75℃ and add raw materials potassium lauryl phosphate, acrylate / acrylamide copolymer, mineral oil, polysorbate-85, and CPE. Homogenize for 5 min and cool to below 45℃.

[0119] 4. Add all remaining raw materials at 45℃, stir evenly, and discharge the material after passing the test (pH value 6-6.8).

[0120] Stability test: The incubator temperatures were pre-adjusted to -10℃ and 40℃. The frosting packaged in glass bottles was placed in the -10℃ incubator for 24 hours, then incubated in the 40℃ incubator for 24 hours, and this process was repeated for 28 days. The color, odor, and presence of stratification, flocculation, and demulsification were observed daily. The tannin and gallic acid content was also periodically tested. The results are as follows:

[0121] (1) Appearance: Formulas 1 and 2 did not change color or taste during the 28-day observation period. The cream was uniform in nature and did not show any layering, flocculation or demulsification. It was stable.

[0122] (2) Content. The results are as follows.

[0123]

[0124] The content of tannic acid and gallic acid changed little during the observation period, and the chemical properties of the prepared cream were stable.

Claims

1. A firming and anti-wrinkle face cream containing gallnut extract, characterized in that... Made from the following raw materials in the following weight ratio: Active ingredient 0.05~0.5% 1-10% of auxiliary functional ingredients Anti-allergen 0.5-3% Skin feel modifier 5-15% Thickener 1~5% Emulsifier 1~5% Moisturizer 5-10% Antioxidant 0.1~1% pH adjuster 0.1~1% Chelating agent 0.01~0.1% Preservative 0.05~0.2% Solvent balance The active ingredient is gallnut extract; the auxiliary active ingredients are selected from one or more of caffeine, horse chestnut extract, hydroxypropyl tetrahydropyrantriol, glycosphingolipids, allantoin, anti-aging and skin-sculpting extract, tocopheryl acetate, and vitrazol; the anti-allergic agent is selected from one or more of betaine, dipotassium glycyrrhizate, and water-soluble total glycosides of Centella asiatica; the skin feel modifier is selected from one or more of behenol, triolein, tocopherol, cetyl ethylhexanoate, trimethylolpropionyl lactone crosspolymer, silica, and plant oils; and the pH adjuster is tetrahydroxypropyl ethylenediamine. The preparation method of the gallnut extract includes the following steps: (1) Take gallnut medicinal material, crush it, add water for warm soaking and extraction, filter the extract, centrifuge and concentrate and dry it, wash with ether to obtain crude gallnut extract; (2) The crude extract is redissolved in water to prepare a solution with a solid content of 10-30%. Then, glycosidase is added to make the enzyme content 20-100 U / ml and the pH is adjusted to 4-6. Then, it is heated to 40-60℃ for hydrolysis. After 2-5 hours, it is heated to boiling to inactivate the enzyme. After centrifugation, it is concentrated and dried to obtain a gallnut extract rich in tannic acid and gallic acid. The glycosidase is one or more of β-glucosidase and α-mannosidase.

2. The firming and anti-wrinkle face cream as described in claim 1, characterized in that: The enzyme content is 40-60 U / ml.

3. The firming and anti-wrinkle face cream as described in claim 1, characterized in that: The pH is 5-5.

5.

4. The firming and anti-wrinkle face cream as described in claim 1, characterized in that: The hydrolysis temperature is 45-50℃.

5. The firming and anti-wrinkle face cream as described in claim 1, characterized in that: The hydrolysis time is 3-4 hours.

6. The firming and anti-wrinkle face cream as described in claim 1, characterized in that: The emulsifier is selected from one or more of polyglycerol-10 myristate, potassium lauryl phosphate, acrylate / acrylamide copolymer, polyglycerol-10 distearate, mineral oil, and polysorbate-85.

7. The firming and anti-wrinkle face cream as described in claim 1, characterized in that: The antioxidant is p-hydroxyacetophenone.

8. The firming and anti-wrinkle face cream as described in claim 1, characterized in that: The chelating agent is trisodium ethylenediamine disuccinate.

9. The firming and anti-wrinkle face cream as described in claim 1, characterized in that, The weight ratio of the raw materials is: Active ingredient: 0.1-0.3% 3-5% of auxiliary functional ingredients Anti-allergen 1-2% Skin feel modifier 9-12% Thickener 3-5% Emulsifier 3-5% Moisturizer 7~9% Antioxidant 0.3~0.6% pH adjuster 0.1~0.3% Chelating agent 0.05~0.1% Preservative 0.08~0.15% Solvent balance.

Citation Information

Patent Citations

  • Natural anti-aging cream

    CN102871944A

  • A composition comprising pentaphylloides fruticosa extract as an active ingredient

    WO2009054606A1