A firming anti-wrinkle emulsion containing extract of myrobalan

Abstract

The application discloses a firming and anti-wrinkle emulsion containing a gallnut extract and belongs to the field of cosmetics. The gallnut medicinal material 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 the synthesis of type I collagen and reduce the secretion of MMP-1, and thus the prepared cosmetic has better firming and anti-wrinkle effects.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of cosmetics, and particularly relates to a firming anti-wrinkle emulsion containing extract of Chinese gallnut. BACKGROUND

[0002] Extract of Chinese gallnut is a common cosmetic raw material. Chinese gallnut contains abundant tannic acid (also known as tannin). Studies have shown that tannic acid has multiple pharmacological effects such as antibacterial and anti-inflammatory, astringent and hemostatic, and is a common pharmaceutical raw material. The structure of tannic acid is not yet clear. It is generally believed that tannic acid is an ester formed by the combination of five hydroxyl groups of glucose and galloyl. Tannic acid has good water solubility. A high concentration of tannic acid can be obtained by extracting and refining Chinese gallnut.

[0003] Tannic acid can be hydrolyzed to remove glycoside to generate gallic acid, which is a polyphenol compound. Studies have shown that plant polyphenols mostly have strong antioxidant effects, can scavenge free radicals, and protect cells from oxidative damage. At present, in order to realize the industrial production of gallic acid, the commonly used methods for hydrolysis of tannic acid mainly include acid-base method, fermentation method and enzyme method. Among them, the reaction of acid-base method and fermentation method is not easy to control, and by-products are easily produced. In comparison, the reaction condition of enzyme method is more mild, and the enzyme cutting site is accurate and controllable, which is conducive to reducing by-products.

[0004] The most commonly used enzyme for hydrolysis of tannic acid is tannase, which is a hydrolytic enzyme produced by mold (mainly Aspergillus niger) through extracellular induction. It can directional ly cleave the ester bond, phenolic bond and glycosidic bond in the tannic acid molecule to generate gallic acid. The enzymatic efficiency of tannase is very high. Literature shows that the conversion rate of tannic acid for preparing gallic acid using tannase can reach more than 98%. However, with the increasing shortage of mold and tannase resources, it is urgent to find other alternative tannic acid hydrolytic enzymes. Glycoside hydrolase is a class of enzymes that can hydrolyze glycosidic bonds in various sugar-containing compounds (including monosaccharide glycosides, oligosaccharides, polysaccharides, saponins and glycoproteins, etc.) in an endo or exo manner. It has been widely used in drug production and synthesis. For example, Zhang Liying et al. obtained a method for converting gardenoside to geniposide by using glycoside hydrolase through studying the role of glycoside hydrolase in the biological transformation of traditional Chinese medicine ingredients (Zhang Liying 2012).

[0005] Unlike tannase, glycoside hydrolase exists in almost all organisms, so the source is more extensive and the cost is more affordable. More importantly, glycoside hydrolase can only convert a part of tannic acid to gallic acid, resulting in a product rich in multiple chemical components and having multiple functions such as antibacterial and anti-inflammatory, astringent and hemostatic, and antioxidant, which is expected to play a better role in drugs.

[0006] Based on this, the application provides a firming and anti-wrinkle cream containing the extract of Chinese gallnut, which is rich in various components due to the use of glycosidase to hydrolyze the key raw material Chinese gallnut, and the prepared extract of Chinese gallnut can more effectively inhibit elastase, promote the synthesis of collagen type I and reduce the secretion of MMP-1, so that the extract can be used as the main component of firming and anti-wrinkle cosmetics and make the cosmetics have good effects. SUMMARY

[0007] The application aims to provide a firming and anti-wrinkle emulsion containing the extract of Chinese gallnut, so as to improve the firming and anti-wrinkle effects of the cosmetic.

[0008] The firming and anti-wrinkle emulsion provided by the application is prepared from the following raw materials in the following weight ratio:

[0009]

[0010] The efficacy component is the extract of Chinese gallnut; the auxiliary efficacy component is selected from one or more of the following: the fermentation product of the yeast of Schizosaccharomyces pompha, nicotinamide, hydroxypropyl tetrahydro pyran triol, biosaccharide gum-1, oat beta-glucan, extract of Qiongyufang, chlorella minutissima polysaccharide, tocopheryl acetate, and hydrolyzed collagen; the anti-allergic agent is the extract of Portulaca oleracea; the skin feel regulator is selected from one or more of the following: triolein, tocopherol, cetyl alcohol ethylhexanoate, trihydroxymethyl hexyl lactone cross-linked polymer, and vegetable oil; and the pH regulator is tetrahydroxypropyl ethylenediamine.

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

[0012] (1) Chinese gallnut medicinal materials are taken, crushed, and then extracted by warm immersion with water, the extract is filtered, centrifuged, and concentrated and dried, and then washed with diethyl ether to obtain the crude extract of Chinese gallnut;

[0013] (2) the crude extract is redissolved with water to prepare a solution containing 10-30% of solid content, then glycosidase is added to make the enzyme content be 20-100 U / ml, and the pH is adjusted to 4-6, then heated to 40-60 DEG C for hydrolysis, boiled after 2-5 h to inactivate the enzyme, and then centrifuged, concentrated and dried to obtain the extract of Chinese gallnut rich in tannic acid and gallic acid.

[0014] In the above preparation method of the extract of Chinese gallnut, step (1) is to extract tannic acid, and the high-content tannic acid crude extract can be obtained by defatting and decoloring treatment, and the extraction temperature, water amount and time have influences on the purity and yield of the product, which can be further optimized; step (2) is to hydrolyze and convert tannic acid, and the extract of Chinese gallnut containing tannic acid and gallic acid can be obtained by using glycosidase to control the conversion efficiency, and the enzyme amount, temperature, pH and time of hydrolysis have great influences on the conversion efficiency.

[0015] The glycosidase includes, but is not limited to, one or more of β-glucosidase, α-mannosidase, β-galactosidase, α-amylase, and β-glucanase. The applicants detect the content of tannic acid and gallic acid in the hydrolysis product, and investigate the effect of the hydrolysis product of various enzymes on elastase activity, type I collagen synthesis, and MMP-1 secretion through in vitro enzyme activity and cell tests, and finally select α-mannosidase as the best hydrolysis enzyme. The enzyme has higher activity and higher hydrolysis efficiency, and the hydrolysis product has higher activity in inhibiting elastase, promoting type I collagen synthesis, and reducing MMP-1 secretion, and thus can be better applied to cosmetics.

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

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

[0018] Further preferably, the hydrolysis temperature is 45-50°C.

[0019] Further preferably, the hydrolysis time is 3-4 h.

[0020] According to one embodiment of the present application, an effective gallnut extract preparation method is as follows:

[0021] (1) Take gallnut medicinal materials, crush them, pass them through a 40-mesh sieve, then add 15 times the weight of water and heat to 60°C for warm infusion extraction, filter after 3 h, centrifuge the filtrate at a speed of 5000 r / min using a tubular centrifuge, vacuum concentrate the centrifugate, freeze-dry it, and finally wash it with ether 3-5 times, and then evaporate the residual organic solvent to obtain a crude gallnut extract;

[0022] (2) Resuspend the crude extract in water to prepare a solution with a solid content of 15%, then add α-mannosidase to the aqueous solution to make the enzyme content reach 50 U / ml, adjust the pH to 5.5 with HCl or NaOH, then heat to 45°C for reaction, boil for 0.5 h after 4 h to inactivate the enzyme, centrifuge at 5000 r / min, vacuum concentrate, and freeze-dry to obtain a gallnut extract rich in tannic acid and gallic acid.

[0023] The gallnut extract prepared according to the above preferred conditions also has the advantages of high product purity and high yield.

[0024] Preferably, the emulsifier is polyglyceryl-10 myristate.

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

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

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

[0028]

[0029]

[0030] The present application has the following advantages:

[0031] The present application first realizes the preparation of gallnut extract by using glycosidase, which not only enriches the types of tannin hydrolase and reduces the cost of the hydrolase, but also enriches various components in the hydrolysis product compared with the existing hydrolase such as tannase, so that the extract can better inhibit elastase, promote the synthesis of type I collagen and reduce the secretion of MMP-1, and thus can be better applied to firming and anti-wrinkle cosmetics.

[0032] The emulsion formula provided by the present application is stable and will not flocculate, delaminate or break emulsion, and can be stored for 3 years under room temperature conditions and is comfortable and non-irritating to use. DETAILED DESCRIPTION

[0033] The present application will be described in detail below in combination with specific examples.

[0034] The gallnut medicinal materials used in the examples are all from the same batch of products purchased from the same company. The β-glucosidase, β-galactosidase, α-amylase, β-glucanase and tannase are purchased from Shanghai Yuan Ye, and the α-mannosidase is purchased from Macklin, and the enzyme activity of all the enzymes is between 10-600 U / mg. The materials not mentioned in the source are all conventional materials in the field.

[0035] The tannic acid and gallic acid content determination method involved in the examples is as follows:

[0036] Tannic acid content determination: determined according to high performance liquid chromatography (general rule 0512)

[0037] Chromatographic conditions and system suitability test: octadecylsilane bonded silica gel as the filler; 1% phosphoric acid water:methanol (80:20) as the mobile phase; the detection wavelength is 275 nm. The theoretical plate number should not be less than 4000 calculated according to the tannic acid peak.

[0038] Preparation of the reference solution: take tannic acid reference substance (purity > 98%, Shanghai Yuan Ye Biotechnology Co., Ltd.) in an appropriate amount, accurately weigh and add water to prepare a solution containing 100 μg per 1 mL, and obtain it.

[0039] Preparation of test solution: accurately weigh about 1 mg of the extract of gallnut, add water to dissolve it, transfer to a brown volumetric flask, add water to make up to 10 mL, shake well, and obtain a solution containing 100 μg per 1 mL.

[0040] Determination: accurately pipette 10 μL of the control solution and 10 μL of the test solution, inject into the liquid chromatograph, and determine.

[0041] Determination of gallic acid content: determine according to the high performance liquid chromatography (General Rule 0512)

[0042] Chromatographic conditions and system suitability test: use octadecylsilane bonded silica gel as the filler; use 1% phosphoric acid water:methanol (95:5) as the mobile phase; and the detection wavelength is 275 nm. The theoretical plate number calculated according to the gallic acid peak should not be less than 3000.

[0043] Preparation of control solution: accurately weigh an appropriate amount of the gallic acid control (China Institute for Drug Control, content is 91.5%) and add water to make up to 100 μg per 1 mL, and obtain the solution.

[0044] Preparation of test solution: accurately weigh an appropriate amount of the extract of gallnut and add water to make up to 100 μg per 1 mL, and obtain the solution.

[0045] Determination: accurately pipette 10 μL of the control solution and 10 μL of the test solution, inject into the liquid chromatograph, and determine.

[0046] Example 1: Preparation of the extract of gallnut

[0047] Researches show that the gallnut is rich in tannic acid and polyphenol, wherein the tannic acid has antibacterial and astringent effects, and the polyphenol has antioxidant effect. Most of the naturally existing plant polyphenol is in the form of combined glycoside, therefore, the gallnut is extracted by using the following process, so as to obtain higher content of tannic acid and polyphenol.

[0048] Process flow: after the raw material is crushed, it is extracted by water warm extraction, the extract is centrifuged to remove impurities, concentrated and dried, washed and decolorized by using ether, redissolved by adding water, and hydrolyzed by adding glycosidase (selecting the type of glycosidase, temperature, pH, and time of enzymolysis), heated to inactivate, centrifuged, the solution is concentrated and dried, and the contents of tannic acid and gallic acid in the extract are detected.

[0049] From the literature reports, several commonly used hydrolytic enzymes were screened, namely β-glucosidase, α-mannosidase, β-galactosidase, α-amylase, β-glucanase, and tannase. The enzyme cleavage sites of these enzymes 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 mannose; β-galactosidase can catalyze the hydrolysis of β-galactosidase into monosaccharides; α-amylase can catalyze the hydrolysis of α-1,4-glucosidic bonds of starch; β-glucanase acts on 1,3 and 1,4 glucosidic bonds of β-glucan and generates oligosaccharides and glucose; and tannase can hydrolyze the ester bond, phenolic bond, and glycosidic bond in the molecular structure of tannic acid.

[0050] The test method is as follows:

[0051] (1) Extraction of medicinal materials: Take the gallnut medicinal material, crush it, pass it through a 40-mesh sieve, then add 15 times the weight of water and heat to 60°C for warm infusion extraction. After 3 hours, filter, centrifuge the filtrate at 5000 r / min using a tubular centrifuge, vacuum concentrate the centrifugate, freeze-dry it, and finally wash it with ether for 3-5 times, and then dry the residual organic solvent to obtain the crude extract of gallnut. The detection shows that the content of tannic acid in the crude extract is 71.7%, and the content of gallic acid is 4.9%.

[0052] (2) The above crude extract is redissolved with water to prepare a solution containing 15% solid content. Then different hydrolytic enzymes are added to the aqueous solution to make the enzyme content reach 50 U / ml, and the pH is adjusted to 5.5 with HCl or NaOH. Then heat to 45°C for reaction. After 4 hours, heat to boiling for 0.5 hours to inactivate the enzyme, centrifuge at 5000 r / min, vacuum concentrate, and freeze-dry. Detect the contents of tannic acid and gallic acid, and the results are shown in the table below.

[0053] Sample No. Hydrolase class Tannin 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 Tannase 1.7 69.9

[0054] The test results show that the five glycosidases can only partially hydrolyze tannic acid. In terms of hydrolysis ability, β-glucosidase and α-mannosidase have stronger activity and generate more gallic acid; α-amylase generates more byproducts and less total amount of tannic acid and gallic acid; β-galactosidase and β-glucanase have lower conversion ability and generate less gallic acid; and tannase can almost completely hydrolyze tannic acid to generate a large amount of gallic acid. This result is basically consistent with the literature reports.

[0055] Example 2: Evaluation of the firming and anti-wrinkle efficacy of gallnut extract

[0056] To further investigate the firming and anti-wrinkle effects of different enzymatic products, the following tests were conducted on the six samples prepared in Example 1 to investigate their inhibitory activity on elastase and their effects on collagen type I and MMP-1, respectively.

[0057] I. Elastase Inhibition Test of Extract of Chinese Gall

[0058] Elastase is a protein-decomposing enzyme with very high selectivity and specificity. It has catalytic hydrolysis effect on many amino acids and can decompose elastin in bound tissue proteins. Inhibition of the activity of elastase can effectively slow down the degradation of elastin and reduce skin aging and wrinkle formation.

[0059] 1. Test Materials

[0060]

[0061] 2. Test Method

[0062] 2.1 Preparation of Reagents and Samples

[0063] Test sample solution: The extract of Chinese gall was dissolved in water to prepare a test sample solution with a concentration of 50 mg / mL.

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

[0065] Elastase solution: Elastase was weighed and dissolved in Tris-HCL buffer (pH 8.2, preheated at 25°C) to prepare an enzyme solution with a concentration of 10 U / mL.

[0066] Reaction substrate solution: N-succinyl-Ala-Ala-Ala-p-nitroanilide (NAAAPN) was weighed and dissolved 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 p-nitroaniline decomposed has absorbance at 405 nm. The absorbance value at 405 nm can be detected using spectrophotometry, and the enzyme activity inhibition rate of the drug can be calculated.

[0069] In 96-well plates, 25 μL elastase solution was added to 50 μL sample solution, and then 100 μL Tris-HCL buffer (pH 8.2) was added, and incubated at 25°C for 20 min. After the end, 25 μL substrate solution was added, immediately mixed and measured absorbance A1 at 405 nm, and then incubated at 25°C for 10 min and measured absorbance A2. The value of ΔA (A2-A1) of each group was calculated for calculating the enzyme inhibition rate.

[0070] Enzyme inhibition rate calculation formula:

[0071]

[0072] In the formula: A: the average absorbance of the test group (T) or the positive control group (PC); A NC : the average absorbance of the blank control group (NC group); A TC : the average absorbance of the control group (TC group)

[0073] 3. Test results

[0074] The elastase inhibition rate of each sample in Example 1 is shown in the following table.

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

[0077] The results show that the enzyme activity inhibition rate of the five kinds of sumac extract prepared by glycosidase is much higher than that of tannase, which may be related to the fact that the extract contains tannic acid and gallic acid at the same time.

[0078] II. Effects of sumac extract on type I collagen and MMP-1

[0079] Type I collagen is one of the main components of the extracellular matrix of the dermis, and human dermal fibroblasts can be used as a cell model for studying the effect of cosmetics on increasing the content of type I collagen. Matrix metalloproteinase (MMP-1) has the ability to degrade extracellular matrix, and increased secretion of MMP-1 will accelerate the degradation of collagen, causing the loss of skin collagen, making the skin loose, the elasticity decreased, and the fine lines increased. Therefore, the anti-wrinkle effect of the extract and cosmetics can be evaluated by measuring the content of type I collagen and MMP-1 of skin fibroblasts.

[0080] 1. Experimental materials

[0081]

[0082]

[0083] 2. Experimental method

[0084] 2.1 Preparation of reagents and samples

[0085] The frozen human skin fibroblast culture was subcultured once in the culture medium and then inoculated into the culture medium at a suitable density for the test, and the cell inoculation density should ensure that the confluence reached 45-60% after 24h of inoculation.

[0086] The extract prepared in Example 1 was dissolved in PBS, and after centrifugation at 5000r / min for 5min, the supernatant was taken and passed through a 0.22μm microporous filter, and then diluted with the culture medium to prepare a test sample solution with a concentration of 5mg / mL.

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

[0088] Blank control: normal cell culture medium was added

[0089] 2.2 Experimental procedure

[0090] The 96-well plate was prepared and incubated in an incubator (37℃, 5% CO2) for 24h, and the culture medium in the 96-well plate was discarded, and the drug administration was carried out. The test sample was added to the test sample well, the positive control was added to the positive control well, and the normal cell culture medium was added to the blank control well, 100μL per well. After the drug administration was completed, the 96-well plate was placed in a CO2 incubator for 24h±2h. After the incubation was completed, about 100μL of cell culture supernatant was collected in a 1.5mL sterile centrifuge tube, and then ELISA detection was carried out according to the instructions of the kit.

[0091] 3. Experimental results

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

[0093] Test sample COL I 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] Among them, sample 7 is the crude extract prepared in Example 1, which contains 71.7% tannic acid and 4.9% gallic acid.

[0095] The results show that compared with the blank control, the content of collagen type I in each test group and the positive control group is significantly increased (P<0.05), indicating that the extract of Galla chinensis has the ability to promote the synthesis of collagen type I, and the activity of the glycosidase hydrolysate is significantly higher than that of tannase.

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

[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] wherein sample 7 is the crude extract prepared in example 1, which contains 71.7% tannic acid and 4.9% gallic acid.

[0099] The results show that the MMP-1 of each test group is down-regulated compared with the blank control, indicating that the extract of Chinese gall has the effect of reducing the secretion of MMP-1.

[0100] Since the hydrolysis product of α-mannosidase has higher activity than other glycosidases, sample 2, i.e. α-mannosidase as the hydrolysis enzyme, is selected to hydrolyze Chinese gall.

[0101] Example 3 Preparation of Chinese gall extract

[0102] (1) Extracting medicinal materials: Take Chinese gall medicinal materials, crush them through a 40-mesh sieve, then add 12 times the weight of water and heat to 70°C for warm extraction. After 2 hours, filter, centrifuge the filtrate at a speed of 5000 r / min using a tubular centrifuge, vacuum concentrate the centrifugate, freeze-dry, and finally wash 3-5 times with ether, and dry the residual organic solvent to obtain the crude extract of Chinese gall. The detection shows that the content of tannic acid in the crude extract is 65.2%, and the content of gallic acid is 3.7%.

[0103] (2) Dissolve the above crude extract in water to prepare a solution containing 12.5% solid content, then add α-mannosidase to the aqueous solution to make the enzyme content reach 70 U / ml, and adjust the pH to 5.0 with HCl or NaOH, then heat to 50°C for reaction. After 2.5 hours, inactivate the enzyme by boiling for 0.5 hour, centrifuge at 5000 r / min, vacuum concentrate, and freeze-dry. The content of tannic acid in the product is 26.5%, and the content of gallic acid is 29.7%.

[0104] Example 4 Preparation of Chinese gall extract

[0105] (1) Extracting medicinal materials: Take Chinese gall medicinal materials, crush them through a 40-mesh sieve, then add 8 times the weight of water and heat to 55°C for warm extraction. After 5 hours, filter, centrifuge the filtrate at a speed of 5000 r / min using a tubular centrifuge, vacuum concentrate the centrifugate, freeze-dry, and finally wash 3-5 times with ether, and dry the residual organic solvent to obtain the crude extract of Chinese gall. The detection shows that the content of tannic acid in the crude extract is 69.3%, and the content of gallic acid is 4.1%.

[0106] (2) The above crude extract is dissolved in water to prepare a solution containing 20% solid content, then α-mannosidase is added to the aqueous solution to make the enzyme content reach 25 U / ml, and the pH is adjusted to 6.0 with HCl or NaOH, then heated to 40°C for reaction, heated and boiled for 0.5 h after 5 h to inactivate the enzyme, centrifuged at 5000 r / min, vacuum concentrated and freeze-dried. The tannic acid content in the product is 24.5%, and the gallic acid content is 22.6%.

[0107] Example 5 Tightening Anti-wrinkle Emulsion Containing Gallnut Extract

[0108] Formulation:

[0109]

[0110]

[0111] Qiongyu Fang extract: is extracted from three medicinal materials, including Poria cocos, Rehmannia glutinosa and Panax ginseng, and has excellent whitening, even skin tone and free radical removal effects.

[0112] Preparation process:

[0113] 1. Mix the raw materials cetyl ethylhexanoate, tocopherol, triolein, trihydroxymethyl hexyl lactone cross-linked polymer, vegetable oil and polyglyceryl-10 myristate uniformly and heat to 80°C to obtain phase A;

[0114] 2. Mix the raw materials carbomer, acrylates / C10-30 alkyl acrylate cross-linked polymer, CPE, ethylenediamine disuccinate trisodium, hyaluronic acid, glycerol, erythritol, 1,2-pentanediol and water uniformly, and heat to 85°C to obtain phase B;

[0115] 3. Add phase A to phase B, warm to 85°C, keep for 10 min, homogenize for 10 min, then keep for another 10 min, cool to below 45°C, and then add tetrahydroxypropyl ethylenediamine, homogenize for 5 min, and cool to below 45°C;

[0116] 4. At 45°C, add the remaining raw materials, stir uniformly, and detect for quality control.

[0117] Stability test: The temperature of the incubator is adjusted to -10°C and 40°C respectively, the emulsion packaged with glass bottles is placed in the -10°C incubator for 24 hours, then placed in the 40°C incubator for 24 hours, and the operation is repeated for 28 days. The color, odor, whether layered, flocculated, broken, and the contents of tannic acid and gallic acid are detected regularly. The results are as follows:

[0118] (1) Appearance: Formula 1 showed slight turbidity on the 19th day, and delamination and demulsification on the 22nd day. Formula 2 showed slight turbidity on the 25th day, and a small amount of delamination on the 27th day. The stability of Formula 2 at high and low temperatures was slightly better than that of Formula 1.

[0119] (2) Content. The test results are as follows.

[0120]

[0121] From the test results, the tannin content showed a downward trend, while the gallic acid content was relatively stable. At the end of the test, the tannin content of Formula 1 decreased by 24.2%, and the tannin content of Formula 2 decreased by 5.9%. The tannin in Formula 2 was more stable than that in Formula 1.

Claims

1. A firming and anti-wrinkle lotion 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 0.001~0.1% Skin feel modifier 5-20% Thickener 3-8% Emulsifier 0.5-5% Moisturizer 3~15% Antioxidant 0.1~1% pH adjuster 0.1~1% Chelating agent 0.01~0.15% Preservative 0.05~0.2% Solvent balance The active ingredient is gallnut extract; the auxiliary active ingredient is selected from one or more of the following: Bifida ferment lysate, niacinamide, hydroxypropyl tetrahydropyrantriol, biosaccharide gum-1, oat β-glucan, *Gynostemma pentaphyllum* extract, Euglena gracilis polysaccharide, tocopheryl acetate, and hydrolyzed collagen; the anti-allergic agent is purslane extract; the skin feel modifier is selected from one or more of the following: triolein, tocopherol, cetyl ethylhexanoate, trimethylolpropionyl lactone crosspolymer, 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 emulsion as described in claim 1, characterized in that: The enzyme content is 40-60 U / ml.

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

5.

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

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

6. The firming and anti-wrinkle emulsion as described in claim 1, characterized in that: The emulsifier is polyglycerol-10 myristate.

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

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

9. The firming and anti-wrinkle emulsion according to any one of claims 1-8, characterized in that, The weight ratio of the raw materials is: Active ingredient: 0.1-0.3% 5-8% of auxiliary functional ingredients Anti-allergen 0.001~0.01% Skin feel modifier 10-15% Thickener 4-6% Emulsifier 1~3% Moisturizer 5-10% Antioxidant 0.3~0.8% pH adjuster 0.1~0.5% Chelating agent 0.05~0.1% Preservative 0.08~0.12% Solvent balance.

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