Yellow wine vinasse mask and preparation method thereof

Abstract

The invention relates to a yellow wine vinasse mask and a preparation method thereof, and belongs to the technical field of masks. The mask is prepared from the following raw materials in percentage by mass: 15%-27% of an oil phase component, 0.5%-1.5% of an emulsifier, 4% of a humectant, 1% of a penetration enhancer, 3% of nicotinamide, 6%-10% of a yellow wine vinasse extracting solution, 0.05%-0.15% of a preservative, 0.01%-0.05% of a chelating agent and the balance of purified water, the oil phase component comprises cetostearyl alcohol, liquid paraffin, squalane hydrogenated polyisobutene, glycerol monostearate and tocopheryl acetate in a mass ratio of 24: 8: 12: 1: 1. The preparation process parameters are optimized on the basis of single factor analysis and response surface experiments, the prepared yellow wine vinasse cream mask is good in sensory index, nutritional ingredients in the yellow wine vinasse can be effectively exerted, and the preparation method has important significance for improving secondary utilization of the yellow wine vinasse.

Description

Technical Field

[0001] The invention relates to the technical field of facial masks, and in particular to a rice wine lees facial mask and a preparation method thereof. Background Art

[0002] my country's yellow wine is one of the three major brewed wines in the world. It is made from rice, millet, corn, millet or wheat as the main raw materials, and is made through cooking, adding koji, saccharification, fermentation, pressing, clarification, filtration, frying, storage and blending. It is named for its yellow color. Yellow wine lees is the main by-product in the brewing process, and the lees yield is generally 20%-30%. Since the flavors of yellow wine from different regions and different manufacturers vary greatly, the substances remaining in the yellow wine lees are also different.

[0003] Studies have shown that rice wine lees are rich in kojic acid and flavonoids, which give them good antioxidant activity. However, at present, rice wine lees are only used in low economic value areas (such as animal husbandry feed).

[0004] Ran Yuzhou et al. studied the antioxidant properties of rice wine lees. The results showed that: with BHA as the positive control group, the total antioxidant capacity of rice wine lees was 74.6% of BHA, the reducing capacity was 19.76% of BHA, and the DPPH free radical scavenging capacity was 33.67% of BHA. Each 1g of rice wine lees contains 144μg of phenolic substances; the anti-superoxide anion activity of each 1g of lees is 119.2U. Yao Kaiyong et al. used Bacillus or yeast to re-ferment rice wine lees, and then studied the antioxidant activity of rice wine lees re-fermentation liquid. The results showed that the DPPH free radical scavenging capacity, superoxide free radical scavenging capacity, and hydroxyl free radical scavenging capacity of rice wine lees extract were significantly improved. Cao Longhui et al. isolated a short peptide component with antioxidant activity from rice wine, and the scavenging rates of the short peptide for ABTS free radicals and DPPH free radicals were 67.45% and 56.47%, respectively. The above studies show that rice wine lees have antioxidant capacity, and its antioxidant active ingredients may come from the polyphenols and peptides therein. Therefore, rice wine lees has considerable potential in the development of antioxidant and anti-aging cosmetics.

[0005] Most of the domestic applications of lees cosmetics are still limited to simple extraction, pretreatment and rough processing of lees. For example, Zhou Hualin et al. pretreated rice wine lees, extracted and concentrated with non-toxic organic solvents, and obtained a tyrosinase inhibitor extracted from rice wine lees, which can be used in the development of cosmetics. Liu Lu et al. extracted lees protein by vacuum extrusion, cooling, crushing, and sieving, and then extracted lees protein by alkali dissolution and acid precipitation. The lees protein extract was hydrolyzed with hydrolyzed protease, inactivated, filtered, concentrated, frozen, and dried to obtain lees small molecule peptides, which can be used in moisturizing and repairing skin care products. Chen Qingqing extracted lees with water, washed with dextran gel molecular sieves to remove impurities, eluted, and concentrated to obtain lees amino acid extracts, which were applied to cosmetics. Huang Dejian et al. ground highland barley lees with water, hydrolyzed with protease, and centrifuged to obtain supernatant. The obtained lees extract was used to prepare facial mask essence and applied to the production of facial masks. Zhu Xiuling et al. extracted anthocyanin extract and pectin extract from wine lees, and then prepared a wine lees extract facial mask according to the following weight percentage ratio: 1%-5% pectin extract, 0.5%-1% sodium chloride, 5%-10% stearic acid, 1%-5% glycerol, 1%-5% anthocyanin extract, 1%-5% sodium alginate, and 70%-80% deionized water.

[0006] Foreign research on wine lees cosmetics is relatively rich and mature. For example, the research results of Melanie et al. show that wine lees extracts are rich in phenolic substances, have excellent antioxidant capacity, and are also effective inhibitors of elastase, matrix metalloproteinase-1 and tyrosinase. The research results of Tsai et al. show that the yeast fermentation broth has a certain effect on inhibiting the production of inflammatory nitric oxide and repairing the epidermal damage induced by it.

[0007] Takahashi et al. determined the quantity and structure of glucosylceramide in sake lees, and the results showed that glucosylceramide has a good repair effect on skin damage. Sake lees are widely used in the production of skin care products abroad. Yukio et al. extracted sake lees as raw materials and applied the lees extract to the addition of cosmetics. Makio et al. used sake lees extract as raw material to develop a lees skin care product with anti-inflammatory effect.

[0008] The above existing research results show that wine lees has great potential in the development and application of cosmetics. Therefore, developing and manufacturing rice wine lees-based facial masks suitable for the general population based on rice wine lees can have whitening and anti-oxidation effects on users, and is beneficial to improving the reuse of nutrients in rice wine lees, and has broad application prospects and value. Summary of the invention

[0009] In view of the defects existing in the above-mentioned prior art, the present invention aims to provide a rice wine lees mask and a preparation method thereof to solve the problems existing in the background technology.

[0010] In order to achieve the above technical objectives, the technical solution of the present invention is as follows:

[0011] The first technical solution disclosed in the present invention is: a rice wine lees mask, comprising the following raw materials in mass fractions: 15% to 27% oil phase component, 0.5% to 1.5% emulsifier, 4% moisturizer, 1% transdermal absorption enhancer, 3% niacinamide, 6% to 10% rice wine lees extract, 0.05% to 0.15% preservative, 0.01% to 0.05% chelating agent, and the balance is purified water.

[0012] A further preferred embodiment of the above scheme is that the facial mask comprises the following raw materials in mass fractions: 21% oil phase component, 1% emulsifier, 4% moisturizer, 1% transdermal absorption enhancer, 3% niacinamide, 8% rice wine lees extract, 0.15% preservative, 0.02% chelating agent, and the remainder is purified water.

[0013] Among them, the oil phase components include cetearyl alcohol, liquid paraffin, squalane hydrogenated polyisobutene, glyceryl monostearate and tocopherol acetate, and the mass ratio of cetearyl alcohol: liquid paraffin: squalane hydrogenated polyisobutene: glyceryl monostearate: tocopherol acetate is 24:8:12:1:1; the emulsifier is Seppic M68, the moisturizer is glycerol, the transdermal absorption enhancer is laurocapram, the preservative is ethylparaben, and the chelating agent is EDTA-2Na.

[0014] As a further preferred embodiment: the preparation of the rice wine lees extract specifically comprises:

[0015] S1: treating rice wine lees to obtain rice wine lees powder;

[0016] S2: Weigh the rice wine lees powder, add the extraction solvent to the rice wine lees powder in proportion, heat and reflux for extraction for a set time, and then filter to obtain the rice wine lees extraction filtrate;

[0017] S3: Evaporate the rice wine lees extract filtrate to a fluid extract, dissolve it with a dissolving solution and make it constant to obtain a rice wine lees extract.

[0018] A further preferred embodiment of the above scheme is as follows: in step S1, the specific process of treating the rice wine lees is as follows: taking the preliminarily dried rice wine lees, crushing, sieving and drying them to obtain rice wine lees powder.

[0019] As a further preferred embodiment: in step S2, the extraction solvent is any one of deionized water, 40% ethanol, 80% ethanol, and ethyl acetate. Preferably, the extraction solvent is 80% ethanol.

[0020] As a further preferred embodiment: in step S2, the ratio of rice wine lees powder to extraction solvent is 1:40.

[0021] Furthermore: the dissolving liquid in step S3 is a 70% glycerol aqueous solution.

[0022] The second technical solution disclosed in the present invention is: a method for preparing a rice wine lees mask, comprising the following steps:

[0023] (1) preparing solution A: liquid paraffin, tocopherol acetate and squalane hydrogenated polyisobutylene are mixed and added into a beaker, and cetearyl stearate and glycerol monostearate are uniformly added and dispersed therein under constant stirring, sterilized by autoclaving at 100-120° C. for 10-20 min, and kept at 60-80° C. for later use;

[0024] (2) preparing solution B: dissolving the moisturizer, transdermal absorption enhancer, and nicotinamide, sterilizing by hot pressing at 100-120° C. for 10-20 min, and keeping at 60-80° C. for later use;

[0025] (3) Preparation of rice wine lees mask: 15% to 27% of solution A is added in a thin stream to 8% to 15% of solution B under sufficient stirring at 60 to 80°C. After solution A is completely added to solution B, 0.5% to 1.5% of emulsifier, 0.05 to 0.15% of preservative, 0.01 to 0.05% of chelating agent and 8% of rice wine lees extract are added and mixed evenly. Purified water is added to make up to 100 ml. The emulsified system is placed in an ultrasonic cell disruptor and ultrasonically emulsified with a probe at 60 to 80°C for 5 to 10 minutes to obtain an emulsion. After the emulsion is cooled to room temperature, it becomes semi-solid, thus obtaining a rice wine lees mask.

[0026] Based on the above scheme, further, in step (1), the mass ratio of cetearyl alcohol: liquid paraffin: squalane hydrogenated polyisobutylene: glycerol monostearate: tocopherol acetate is 24:8:12:1:1.

[0027] Based on the above scheme, further, in step (2), the mass ratio of moisturizer: transdermal absorption enhancer: niacinamide is 4:1:3.

[0028] Compared with the prior art, the technical solution of the present invention has the following beneficial effects:

[0029] 1. The present invention screens the whitening active effective parts of rice wine lees extract by tyrosinase inhibition rate method, and studies the dose-effect relationship of rice wine lees tyrosinase inhibition. The results show that the rice wine lees extract obtained by 80% ethanol extraction solvent has the best inhibitory effect on tyrosinase. The antioxidant active effective parts of rice wine lees extract are screened by superoxide radical scavenging method, and the dose-effect relationship of superoxide radical scavenging of rice wine lees is studied. The results show that the 80% ethanol extraction solvent has the best scavenging effect on superoxide radicals generated by pyrogallol self-oxidation. At the same time, the rice wine lees extract obtained by 80% ethanol extraction solvent has an average decolorization rate of 73.93% after decolorization by D101 macroporous resin, and the RSD is 1.23%, and the decolorization effect is good. Therefore, based on the whitening activity, antioxidant activity and dose-effect research results of rice wine lees, the present invention finally determines to use 80% ethanol extraction solvent to extract rice wine lees, and the concentration of rice wine lees extract added to the facial mask cosmetics is 40 mg / g.

[0030] 2. When preparing the rice wine lees cream mask, the present invention uses squalane hydrogenated polyisobutylene and cetyl stearic acid with good skin compatibility as oil phase components, and adopts the composite emulsifier Seppic M68 which has good emulsification effect on the oil phase component, is mild and non-irritating, and has low foaming property for emulsification. Rice wine lees extract and niacinamide are used as effective ingredients to exert antioxidant and whitening effects. Probe ultrasonic emulsification is used, and on the basis of single factor analysis, the preparation process parameters are optimized as follows: the oil phase accounts for 21%, the emulsifier ratio is 1%, and the emulsification time is 5 minutes, so that a rice wine lees cream mask with good sensory indicators is prepared.

[0031] 3. The present invention uses hot and cold stability tests and centrifugation tests to investigate the stability of the rice wine lees cream mask, indicating that the hot and cold stability, centrifugation test and pH value of the rice wine lees cream mask all meet national standards, and the rice wine lees cream mask is easy to apply evenly, is mild and non-irritating, has good sensory indicators, and has excellent whitening and antioxidant effects. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art are briefly introduced below.

[0033] Figure 1 This is a comparison chart of tyrosinase inhibition rates of yellow wine lees extracts obtained by using different extraction solvents in the present invention;

[0034] Figure 2 This is a graph showing the relationship between the tyrosinase inhibition rate of the rice wine lees extract obtained by using 80% ethanol extraction solution and the concentration;

[0035] Figure 3A comparison chart of superoxide radical scavenging rates of yellow wine lees extracts obtained by using different extraction solvents of the present invention;

[0036] Figure 4 This is a graph showing the relationship between the superoxide radical scavenging rate of the rice wine lees extract obtained by using 80% ethanol extraction solution and the concentration;

[0037] Figure 5 The effect of the oil phase ratio in the rice wine lees cream mask of the present invention on the comprehensive sensory score;

[0038] Figure 6 The effect of the proportion of emulsifier in the rice wine lees cream mask of the present invention on the comprehensive sensory score;

[0039] Figure 7 The effect of the emulsification time of the rice wine lees cream mask on the comprehensive sensory score of the present invention;

[0040] Figure 8 The finished product of the yellow wine lees cream mask prepared by the present invention;

[0041] Fig. 9 The skin application of the rice wine lees cream mask, where A is before application, B is at the beginning of application, and C is after evenly applied;

[0042] Fig.10 Before the hot-cold alternating stability test of the rice wine lees cream mask (three groups of samples);

[0043] Fig.11 After conducting a hot-cold alternating stability test on the rice wine lees cream mask (three groups of samples);

[0044] Fig.12 This is a comparison chart of rice wine lees cream mask (three groups of samples) before and after centrifugation test, where A is before centrifugation test and B is after centrifugation test. DETAILED DESCRIPTION

[0045] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments.

[0046] Reference Figure 1-12 The present invention provides a rice wine lees facial mask, comprising the following raw materials in mass fractions: 15% to 27% of oil phase component, 0.5% to 1.5% of emulsifier, 4% of moisturizer, 1% of transdermal absorption promoter, 3% of niacinamide, 6% to 10% of rice wine lees extract, 0.05% to 0.15% of preservative, 0.01% to 0.05% of chelating agent, and the balance being purified water.

[0047] Preferably, the facial mask comprises the following raw materials in mass fractions: 21% oil phase component, 1% emulsifier, 4% moisturizer, 1% transdermal absorption enhancer, 3% niacinamide, 8% rice wine lees extract, 0.15% preservative, 0.02% chelating agent, and the remainder is purified water.

[0048] The oil phase components include cetearyl alcohol, liquid paraffin, squalane hydrogenated polyisobutene, glyceryl monostearate, and tocopherol acetate, and the mass ratio of cetearyl alcohol: liquid paraffin: squalane hydrogenated polyisobutene: glyceryl monostearate: tocopherol acetate is 24:8:12:1:1;

[0049] The emulsifier is Seppic M68, the moisturizer is glycerol, the transdermal absorption enhancer is laurocapram, the preservative is ethylparaben, the chelating agent is EDTA-2Na, and the mass ratio of glycerol: laurocapram: niacinamide is 4:1:3.

[0050] The ingredients and effects of the yellow wine lees mask of the present invention are shown in Table 1:

[0051] Table 1 Composition and function of rice wine lees mask

[0052] Element effect Cetearyl Alcohol oil phase Liquid paraffin oil phase Squalane Hydrogenated Polyisobutene oil phase Glyceryl Monostearate Oil phase, emulsifier Tocopheryl acetate Moisturizing ingredients Glycerol Moisturizer Laurocapram Skin permeation enhancer Niacinamide Whitening ingredients Seppic M68 O / W emulsifier Yellow wine lees extract (0.5g / mL) Whitening and antioxidant ingredients Ethylparaben preservative EDTA-2Na Metal ion chelators Purified water Water phase ingredients

[0053] Specifically, in the facial mask of the present invention, the rice wine lees extract is used as an effective ingredient with whitening and anti-oxidation effects, and the steps of preparing the rice wine lees extract specifically include:

[0054] a. Pre-treat the rice wine lees: take the rice wine lees after preliminary drying, crush them through an 80-mesh sieve, dry them to obtain rice wine lees powder, and set aside;

[0055] b. Preparation of yellow wine lees extract: The present invention prepares four yellow wine lees extracts:

[0056] 1) Preparation of yellow wine lees water extract:

[0057] Accurately weigh the rice wine lees powder, add deionized water at a solid-liquid ratio of 1:40 (g / mL), heat and reflux for extraction for 1.5 hours, and then filter to obtain the rice wine lees water extraction filtrate;

[0058] 2) Preparation of yellow wine lees ethanol extract:

[0059] Accurately weigh the yellow wine lees powder, add 40% ethanol and 80% ethanol as extraction solvents according to the solid-liquid ratio of 1:40 (g / mL), heat reflux extraction for 1.5 hours and then filter to obtain two yellow wine lees ethanol extraction filtrates;

[0060] 3) Preparation of yellow wine lees ethyl acetate extract:

[0061] Accurately weigh the yellow wine lees powder, use ethyl acetate as the extraction solvent, and the solid-liquid ratio is 1:40 (g / mL). Heat and reflux for extraction for 1.5 hours and then filter to obtain the yellow wine lees ethyl acetate extraction filtrate;

[0062] c. The various rice wine lees extract filtrates in b above were rotary evaporated to a fluid extract, and then fully dissolved with 70% glycerol aqueous solution and fixed to volume to obtain four rice wine lees extracts.

[0063] The four different solvent extracts obtained above were respectively tested and compared for tyrosinase inhibition activity, antioxidant capacity, decolorization and decolorization rate to obtain the best rice wine lees extract, as follows:

[0064] 1) Determination and comparison of the inhibition of tyrosinase activity by rice wine lees extract:

[0065] The mother solution of the extract was diluted with PBS buffer solution (pH 7.4) to the corresponding concentration to prepare the test sample. According to Table 2, the four sample solutions of a, b, c, and d were accurately transferred into 1.5 mL centrifuge tubes using a pipette, and the tubes were shaken well. After being placed in a 37°C water bath for 10 minutes, 60 μL of tyrosinase solution with an enzyme activity of 180 U / mL was quickly added to each tube and shaken well. The tubes were placed in a 37°C water bath for 5 minutes. After the insulation, the tubes were shaken well. The absorbance was immediately measured at 475 nm using an ultra-micro UV-visible spectrophotometer. The tyrosinase activity inhibition rate was calculated using the following formula. The results are shown in Table 2:

[0066] Tyrosinase activity inhibition rate (%) = [1-(Ad-Ac) / (Ab-Aa)] × 100%

[0067] Table 2 Tyrosinase inhibition rate determination reagent addition amount in each tube

[0068] a b c d L-Dopa 0 440μL 0 440μL sample PBS 200 μL PBS 200 μL Extraction solution 200 μL Extraction solution 200 μL PBS 740μL 300μL 740μL 300μL Tyrosinase 60μL 60μL 60μL 60μL

[0069] After determining the extract with the best tyrosinase inhibition effect, the tyrosinase inhibition rate of the extract at different concentrations was determined. L-ascorbic acid (L-Dopa) was used as a positive control to study the relationship between the tyrosinase inhibition rate of rice wine lees extract and its concentration. Three groups of experiments were conducted in parallel. The obtained data were logarithmized and regressed using GraphPadPrism 9 to calculate the IC 50 .

[0070] When the concentration of rice wine lees extracts with different extraction solvents was 30 mg / mL, the 80% ethanol extract had the best inhibitory effect on tyrosinase, which was 26.217%, followed by the water extract, which was 19.534%. At this concentration, the tyrosinase inhibition rate of the extracts with different solvents was significantly different among the groups (P<0.001, α=0.05). Figure 1 , tyrosinase inhibition rate: 80% ethanol extract > water extract > 40% ethanol extract > ethyl acetate extract. The results showed that 80% ethanol rice wine lees extract had the highest inhibition efficiency on tyrosinase activity. The reason is that the polarity of the components in rice wine lees that have tyrosinase activity inhibition is close to 80% ethanol and is easier to dissolve in it; in addition, 80% ethanol is easier to penetrate the plant cell structure in rice wine lees, allowing the effective components in the cells to dissolve more fully in it.

[0071] On this basis, the dose-effect relationship between rice wine lees extract and tyrosinase inhibition activity was further studied. A concentration gradient was set to measure the inhibition rate of 80% ethanol extract of rice wine lees on tyrosinase at different concentrations to study the relationship between tyrosinase inhibition rate and concentration. Figure 2 As shown in the figure, within the concentration range of 15 to 75 mg / mL, L-ascorbic acid exhibits good and stable tyrosinase inhibition activity, and its tyrosinase inhibition rate is close to 100% and does not change much with concentration; the 80% ethanol extract of rice wine lees has a dose-dependent inhibition on tyrosinase within the mass concentration range of 15 to 45 mg / mL. As the mass concentration of the lees extract increases, its tyrosinase inhibition rate also gradually increases, and the mass concentration of the lees extract and the tyrosinase inhibition rate show a linear relationship (r=0.9960). When the mass concentration of the lees extract reaches 45 mg / mL, its tyrosinase inhibition rate reaches the maximum, which is 59.50%. However, the mass concentration of the 80% ethanol extract of rice wine lees and its tyrosinase inhibition rate do not only show a unidirectional increase and decrease relationship. After the mass concentration of the lees extract reaches 45 mg / mL, the tyrosinase inhibition rate shows a downward trend when its concentration continues to increase, and when the mass concentration of the lees extract reaches 75 mg / mL, its tyrosinase inhibition rate drops to 16.815%. The reason is that, in addition to the tyrosinase activity inhibitory components, the 80% ethanol extract of rice wine lees may also contain other impurities that interfere with the inhibition process of the tyrosinase activity inhibitory components and impurities that may activate the tyrosinase activity. When the concentration reaches a certain level, the tyrosinase inhibition rate gradually tends to be flat as the concentration of the tyrosinase activity inhibitory components in the extract increases. Continuing to increase the concentration of the extract will increase the concentration of impurities, increase the interference with the tyrosinase inhibition effect, and cause a decrease in the tyrosinase inhibition rate. The effective part of its tyrosinase inhibitory activity may come from kojic acid and polyphenols in rice wine lees. The IC value of 80% ethanol extract of rice wine lees on tyrosinase is 50 It is 39.5mg / mL.

[0072] 2) Determination of the antioxidant capacity of rice wine lees extract:

[0073] The antioxidant capacity of the sample was determined by the superoxide free radical scavenging rate method. 2950 μL of Tris-HCl buffer solution (pH = 7.4) was accurately measured and added to a quartz cuvette, and then 50 μL of 60 mmol / L pyrogallol solution was added. After rapid inversion mixing, the mixture was placed in an ultraviolet spectrophotometer. The absorbance at λ = 325 nm was measured with a blank adjustment of Tris-HCl buffer (pH = 7.4). The measurement was performed every 30 seconds for 300 seconds, and ΔA0 = A was calculated. 300s -A 30s ; Then accurately measure 500 μL of each rice wine lees extract into another quartz cuvette, add 2450 μL of Tris-HCl buffer solution (pH=7.4), then add 50 μL of 60 mmol / L pyrogallol solution, quickly mix by inverting, and place in an ultraviolet spectrophotometer, use Tris-HCl buffer (pH=7.4) to adjust the blank to zero and measure the absorbance at λ=325 nm, measure once every 30 seconds, and measure continuously for 300 seconds, and calculate its ΔA=A 300s -A 30s .

[0074] O 2- The calculation expression of the clearance rate S (%) is as follows:

[0075]

[0076] Where: ΔA0 is the absorbance of pyrogallol solution at λ = 325nm. The measurement is performed every 30 seconds for 300 seconds. Calculate ΔA0 = A 300s -A 30s； ΔA is the absorbance of each extract of rice wine lees at λ = 325nm. The measurement is carried out every 30 seconds for 300 seconds. Calculate ΔA = A 300s -A 30s After determining the extract with the best antioxidant effect, the mother liquor of rice wine lees extract was diluted with deionized water to different concentration gradients. L-ascorbic acid was used as a positive control to study the relationship between the superoxide radical scavenging rate of rice wine lees extract and its concentration. Three groups of experiments were conducted in parallel. The obtained data were logarithmized and regressed using GraphPad Prism 9 to calculate its IC 50 .

[0077] like Figure 3As shown, when the concentration of rice wine lees extracts from different solvents was 5 mg / mL, the 80% ethanol extract had the best scavenging effect on superoxide radicals generated by self-oxidation of pyrogallol, which was 55.943%, followed by the 40% ethanol extract, which was 48.754%. At this concentration, the superoxide radical scavenging rate of extracts from different solvents was significantly different among the groups (P<0.05, α=0.05), and the superoxide radical scavenging rate was: 80% ethanol extract>40% ethanol extract>water extract>ethyl acetate extract.

[0078] On this basis, the dose-effect relationship between rice wine lees extract and superoxide radical scavenging rate was further studied. A concentration gradient was set to measure the scavenging rate of superoxide radicals produced by pyrogallol autooxidation at different concentrations of 80% ethanol extract of rice wine lees to study the relationship between superoxide radical scavenging rate and concentration. Figure 4 As shown in the results, within the concentration range of 3.5-6 mg / mL, L-ascorbic acid exhibited good and stable superoxide radical scavenging activity, and its superoxide radical scavenging rate did not change much with the concentration. The scavenging ability of 80% ethanol extract of rice wine lees on superoxide radicals showed a dose-dependent relationship within this concentration range. With the increase of the mass concentration of lees extract, its superoxide radical scavenging rate also gradually increased, and the mass concentration of lees extract and its superoxide radical scavenging rate showed a linear relationship (r=0.9960). When the mass concentration of lees extract was 6 mg / mL, its superoxide radical scavenging rate was 70.839%, showing a good in vitro antioxidant effect. The effective part of its antioxidant activity may come from the polyphenols and peptides in rice wine lees. The IC value of 80% ethanol extract of rice wine lees on superoxide radicals is 50 It is 4.903mg / mL.

[0079] 3) Decolorization of rice wine lees extract and decolorization rate determination:

[0080] Take 70% glycerol extract of yellow wine lees equivalent to 5g of original yellow wine lees, dissolve it in water and make it up to 100mL, scan the maximum absorption wavelength on a spectrophotometer, and measure the absorbance A0 at this wavelength; place an equal amount of yellow wine lees extract on a D101 macroporous resin ion exchange column, elute it with 80mL of water, collect the eluate, add water to make it up to 100mL, measure its absorbance A1 at the maximum absorption wavelength, and calculate the decolorization rate of the yellow wine lees extract:

[0081] ω(%)=1-A1 / A0×100%

[0082] Where: A0 is the absorbance of original rice wine lees; A1 is the absorbance of lees after decolorization.

[0083] The average decolorization rate of 80% ethanol extract of rice wine lees after decolorization by D101 macroporous resin was 73.927%, and the RSD was 1.232%, indicating that the pigment in rice wine lees is a non-polar substance that can be adsorbed by D101 macroporous resin. This method has good effect and repeatability in removing pigments from rice wine lees extract. The decolorization data are shown in Table 3.

[0084] Table 3 Decolorization rate of yellow wine lees

[0085]

[0086] On the other hand, the present invention provides a method for preparing a rice wine lees facial mask, comprising the following steps:

[0087] (1) preparing solution A: liquid paraffin, tocopherol acetate and squalane hydrogenated polyisobutylene were mixed and added into a beaker, and cetearyl alcohol and glycerol monostearate were uniformly added and dispersed therein under constant stirring as an oil phase, and sterilized by hot pressing at 120° C. for 15 min, and kept warm at 75° C. for later use; wherein the mass ratio of cetearyl alcohol: liquid paraffin: squalane hydrogenated polyisobutylene: glycerol monostearate: tocopherol acetate was 24:8:12:1:1;

[0088] (2) preparing solution B: dissolving glycerol, laurocapram and niacinamide, sterilizing by hot pressing at 120°C for 15 min, and keeping at 75°C for later use; wherein the mass ratio of glycerol: laurocapram: niacinamide is 4:1:3;

[0089] (3) Preparation of rice wine lees mask: 15% to 27% of solution 1 was added to 8% to 15% of solution B in a thin stream under 75°C heat preservation and sufficient stirring. After solution 1 was completely added to solution 2, 1% of Seppic M68, 0.15% of ethylparaben, 0.02% of EDTA-2Na and 8% of rice wine lees extract were added and mixed evenly. Purified water was added to make up to 100 mL. The emulsified system was placed in an ultrasonic cell disruptor and ultrasonically emulsified with a probe at 75°C for 5 minutes to obtain an emulsion. After the emulsion was cooled to room temperature and became semi-solid, a rice wine lees mask was obtained.

[0090] The facial mask prepared by the present invention is a rice wine lees cream mask. Single factor experiments are carried out from the aspects of oil phase proportion, emulsifier proportion, and emulsification time. Response surface experiments are carried out on the basis of the single factor experiments to analyze and obtain the optimal prescription ratio.

[0091] (1) Influence of oil phase ratio:

[0092] The proportion of oil phase has an influence on the viscosity of cream masks in the emulsified system, and also has an influence on the sensory index of the refreshing and greasy degree of cosmetics. In the present invention, the influence of different oil-water phase ratios on the total score of the sensory evaluation of rice wine lees cream masks is studied with the oil phase proportions of 15%, 18%, 21%, 24% and 27%.

[0093] Depend on Figure 5 It can be seen that when the oil phase accounts for 15%, the sensory comprehensive score of the rice wine lees cream mask is low. The reason is that the oil phase accounts for too low a proportion, the viscosity of the rice wine lees cream mask is too low, it is in a fluid state, and the skin adhesion is poor; increasing the oil phase proportion, the sensory comprehensive score of the rice wine lees cream mask improves, and the maximum value appears when the oil phase accounts for 21%; continuing to increase the oil phase ratio, the sensory score of the rice wine lees cream mask shows a downward trend. The reason is that the excessively high oil phase proportion makes the rice wine lees cream mask too viscous, making it difficult to apply evenly on the skin surface, and the skin feels greasy, and the sensory score is poor. Taking all factors into consideration, it is more appropriate to choose an oil phase proportion of 21%.

[0094] (2) Impact of emulsifier proportion:

[0095] The amount of emulsifier used is related to the stability of the emulsified system. The emulsifier plays a role in reducing the surface tension in the emulsified system. When the amount of the emulsifier in the emulsified system increases to a certain extent, the emulsifier molecules form micelles in the aqueous solution and reach a critical micelle concentration, which is conducive to the stability of the emulsified system. In the present invention, the proportion of Seppic M68 is 0.5%, 0.75%, 1.0%, 1.25% and 1.5%, and the influence of the proportion of emulsifier on the total sensory score of rice wine lees cream mask is studied.

[0096] Depend on Figure 6 It can be seen that the addition ratio of compound emulsifier Seppic M68 and the comprehensive sensory score show a positive correlation in the range of 0.5% to 1%. The reason is that at low dosage, the emulsifier molecules are sparsely arranged at the oil-water interface, the surface tension is not completely reduced, and the emulsification system is unstable. In the finished cosmetics, oil-water separation and incomplete emulsification are shown, and the texture of the cosmetics is uneven, resulting in a low comprehensive sensory score; when the addition ratio of Seppic M68 reaches 1%, the comprehensive sensory score is the largest. If the emulsifier is continued to be added, the comprehensive sensory score will decrease. The reason is that the excessive emulsifier addition causes a foaming effect. When the mask is applied to the skin, it is easy to produce white and delicate foam, which is difficult to apply evenly, which reduces the comprehensive sensory score. Taking all factors into consideration, it is more appropriate to choose an addition amount of 1% emulsifier Seppic M68.

[0097] (3) Influence of emulsification time:

[0098] Emulsification time has an influence on the stability of the emulsification system. The probe ultrasonic emulsification time was changed to 1min, 3min, 5min, 7min, and 9min, and the influence of the emulsification time on the total sensory score of the obtained rice wine lees cream mask was studied. In the present invention, the emulsification process adopts the probe ultrasonic emulsification process, the ultrasonic frequency is 20kHz, the ultrasonic power is 600W, the ultrasonic cycle working time is 5s, the cycle interval time is 10s, and the amplitude rod specification is selected as 10Φ.

[0099] Depend on Figure 7 It can be seen that within the emulsification time of 1 to 5 minutes, the comprehensive sensory score of the cream mask shows an increasing trend. The reason is that too short an emulsification time will lead to instability of the emulsification system, uneven dispersion of the oil phase, uneven texture of the cream cosmetics, and easy oil-water separation. After the emulsification time reaches 5 minutes, the ultrasonic emulsification time continues to increase, and the comprehensive sensory score shows a downward trend. The reason is that the cavitation effect caused by the ultrasonic emulsification of the probe lasts too long and enhances the foaming phenomenon of the emulsifier, leaving a certain amount of tiny bubbles in the emulsification system, so that bubbles remain in the middle of the cream emulsification system after cooling and solidification, affecting its sensory score and cream texture. Taking all factors into consideration, it is more reasonable to use an emulsification time of 5 minutes.

[0100] (4) Response surface analysis and ratio optimization

[0101] On the basis of the above single factor experiment, the three factors of oil phase proportion (A), emulsifier proportion (B) and ultrasonic emulsification time (C) were set as independent variables, and the total sensory score was used as the response value (Y). The relevant factor development level was formulated according to the design principle of Box-Behnken experiment, and a response surface experiment was conducted. The obtained data were analyzed by Design Expert 13.0 to obtain the optimal ingredient ratio. The sensory comprehensive evaluation table is shown in Table 4. The total sensory score is the sum of the average scores of each group. Three volunteer subjects were selected, and a single-blind experimental method was used to let the subjects evaluate their feelings after using the rice wine lees mask. Table 5 shows the response surface test design and results, and Table 6 shows the variance and significance analysis of the response surface model.

[0102] Table 4 Sensory score evaluation table of rice wine lees mask

[0103]

[0104] Table 5 Response surface design and results of rice wine lees mask

[0105]

[0106]

[0107] The three factors and the response value Y were regressed and fitted by Design Expert v13.0 software to obtain the multivariate quadratic regression fitting equation of the comprehensive sensory score of rice wine lees mask (the level values ​​of each factor are coded):

[0108] Y=53.76-0.9875A+0.1625B+0.0750C-0.0250AB-0.1500AC-1.50BC-7.44A 2 -4.4

[0109] 9B 2 -4.47C 2

[0110] By statistically analyzing the predicted values ​​and the actual values, the goodness of fit of the model R 2 =0.9831, indicating that the two are close, the deviation between the model prediction and the actual value is small, and the model prediction is accurate.

[0111] Table 6 Response surface variance analysis and significance test of rice wine lees mask

[0112]

[0113]

[0114] It can be seen from Table 6 that the F value of the response surface mathematical model is 45.32, and the P value is <0.0001, indicating that the level difference of the response surface model of this experiment is significant (P<0.05), and it is more reasonable to optimize the process level of the rice wine lees mask by response surface; the F value of the lack of fit term of this model is 3.78, and the P value is 0.1160 (P>0.05), and the lack of fit term is not significant, indicating that the model has a high degree of fit.

[0115] In the variance analysis, factor A, oil phase ratio, had a significant effect on the comprehensive sensory score of rice wine lees cream mask (P<0.05), while emulsification time and emulsifier ratio had no significant effect. The quadratic terms all had a very significant effect on the comprehensive sensory score of rice wine lees cream mask (P<0.01). Among the interaction terms, factor B, emulsifier ratio and factor C, emulsification time, had a significant interactive effect on the comprehensive sensory score of rice wine lees cream mask (P<0.05), indicating that the effects of the two on the sensory indicators of rice wine lees cream mask were not independent, and the two showed an interactive effect. The other interaction terms had no significant effect (P>0.05). The influence intensity of each factor on the comprehensive sensory score of rice wine lees mask is: A>B>C, that is, oil phase proportion>emulsifier proportion>emulsification time; the influence intensity of factor interaction on the comprehensive sensory score of rice wine lees cream mask is: BC>AC>AB, that is, the interaction of emulsifier proportion and emulsification time>interaction of oil phase proportion and emulsification time>interaction of oil phase proportion and emulsifier proportion.

[0116] The regression model analysis by Design Expert v13.0 software showed that the predicted value of the comprehensive sensory score of the prepared rice wine lees cream mask was 53.794 when the oil phase accounted for 20.799%, the emulsifier ratio was 1.017%, and the emulsification time was 5.012 min. Considering the actual conditions of the preparation process, the preparation parameters of the mask were optimized as follows: the oil phase accounted for 21%, the emulsifier ratio was 1%, and the emulsification time was 5 min. The rice wine lees cream mask was prepared, and five volunteers were selected for single-blind comprehensive sensory scoring according to Table 3. The average comprehensive sensory score was 54.2, the RSD value was 2.74%, the relative standard deviation between parallel groups was small, and the actual value was 100.75% of the predicted value, which was close to the two, confirming the reliability of the process parameters after prescription.

[0117] Example:

[0118] According to the preparation method of the present invention and the optimal parameters determined after the above optimization, a finished product of a yellow wine lees cream mask is prepared, such as Figure 8 As shown, the finished product is a milky white, fine and uniform semi-solid cream with a special aroma of rice wine, moderate viscosity, and easy to apply evenly on the skin. Fig. 9 No skin irritation or local allergic reaction was observed within 24 hours after application on the subjects' skin.

[0119] The quality and stability test of the finished product of rice wine lees cream mask was evaluated. Figure 10 to Figure 12 As shown, the details are as follows:

[0120] (1) Hot and cold stability test:

[0121] The following thermal stability, cold stability and hot and cold alternating stability samples were tested using three sets of parallel samples. The results are as follows:

[0122] Thermal stability: The test samples of rice wine lees cream mask were placed in a constant temperature incubator at 40°C for 24 hours and then taken out to return to room temperature. There was no obvious difference in properties compared with the control group placed at room temperature for 24 hours; the test samples did not show oil-water separation after heating, proving that their thermal stability meets the national standards.

[0123] Cold stability: The rice wine lees cream mask samples were placed in a refrigerator at -5°C for 24 hours, taken out and brought to room temperature. There was no obvious difference in properties compared with the control group placed at room temperature for 24 hours; no oil-water separation phenomenon occurred in the test samples after refrigeration, proving that its cold stability meets the national standards.

[0124] Stability of alternating hot and cold conditions: After placing the test sample of the rice wine lees cream mask in a refrigerator at -5°C for 24 hours, the test sample was placed in a constant temperature incubator at 40°C for 24 hours. After being taken out, it was compared with the control group sample placed at room temperature. There was no obvious difference in properties, such as Fig.10 , Fig.11 As shown, there is no obvious oil-water separation phenomenon in the tested samples after the hot-cold alternating test, proving that its hot-cold alternating stability meets the national standards.

[0125] (2) Centrifugal test:

[0126] Take the rice wine lees cream mask in a test tube to make three sets of parallel samples for centrifugal test, control the centrifugal speed to 2000r / min, set the centrifugal time to 30min, and Fig.12 It can be seen that there is no obvious difference in the properties of the three groups of parallel samples before and after the centrifugal test. After centrifugation, no oil-water separation phenomenon was observed in the three groups of parallel samples, proving that their centrifugal test meets the national standards.

[0127] (3) pH determination:

[0128] Take one sample of rice wine lees mask (accurate to 0.1g), add nine parts of deionized water, heat to 40℃, stir until uniform, cool to room temperature, test pH value with a calibrated pH meter, test three groups of samples in parallel, and take the average value. After testing, the average pH value of the three groups of samples was 5.04, and the RSD value was 0.75%, which meets the national standard for mask cosmetics pH of 4.0 to 8.5.

[0129] The above shows and describes the basic principles, main features and advantages of the present invention. It should be understood by those skilled in the art that the present invention is not limited to the above embodiments, and the above embodiments and descriptions are only for explaining the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, which fall within the scope of the present invention to be protected. The scope of protection of the present invention is defined by the attached claims and their equivalents.

Claims

1. A yellow wine lees facial mask, characterized in that: The invention comprises the following raw materials in mass fractions: 15% to 27% of oil phase component, 0.5% to 1.5% of emulsifier, 4% of moisturizer, 1% of skin permeation enhancer, 3% of nicotinamide, 6% to 10% of rice wine lees extract, 0.05% to 0.15% of preservative, 0.01% to 0.05% of chelating agent and the balance is purified water.

2. A yellow wine lees facial mask according to claim 1, characterized in that: The invention comprises the following raw materials in mass fractions: 21% of oil phase component, 1% of emulsifier, 4% of moisturizer, 1% of skin permeation enhancer, 3% of nicotinamide, 8% of rice wine lees extract, 0.15% of preservative, 0.02% of chelating agent and the balance of purified water.

3. A yellow wine lees facial mask according to claim 2, characterized in that: The oil phase ingredients include cetearyl alcohol, liquid paraffin, squalane hydrogenated polyisobutene, glyceryl monostearate and tocopherol acetate, and the mass ratio of cetearyl alcohol: liquid paraffin: squalane hydrogenated polyisobutene: glyceryl monostearate: tocopherol acetate is 24:8:12:1:

1.

4. A yellow wine lees facial mask according to claim 3, characterized in that: The preparation of yellow wine lees extract specifically includes: S1: treating rice wine lees to obtain rice wine lees powder; S2: Weigh the rice wine lees powder, add the extraction solvent to the rice wine lees powder in proportion, heat and reflux for extraction for a set time, and then filter to obtain the rice wine lees extraction filtrate; S3: Evaporate the rice wine lees extract filtrate to a fluid extract, dissolve it with a dissolving solution and make it constant to obtain a rice wine lees extract.

5. The yellow wine lees facial mask according to claim 4, characterized in that: In step S2, the extraction solvent is any one of deionized water, 40% ethanol, 80% ethanol, and ethyl acetate.

6. The yellow wine lees facial mask according to claim 4, characterized in that: In step S2, the ratio of rice wine lees powder to extraction solvent is 1:

40.

7. The yellow wine lees facial mask according to claim 4, characterized in that: The dissolving liquid in step S3 is a 70% glycerol aqueous solution.

8. The method for preparing a rice wine lees facial mask according to any one of claims 1 to 7, characterized in that: The following steps are involved: (1) Preparation of solution A: Liquid paraffin, tocopherol acetate and squalane hydrogenated polyisobutylene are mixed and added into a beaker, and cetearyl stearate and glycerol monostearate are uniformly added and dispersed therein under constant stirring, and sterilized by hot pressing at 100-120°C for 10-20 min, and kept warm at 60-80°C for later use (2) preparing solution B: dissolving the moisturizer, transdermal absorption enhancer, and nicotinamide, sterilizing by hot pressing at 100-120° C. for 10-20 min, and keeping at 60-80° C. for later use; (3) Preparation of rice wine lees mask: 15% to 27% of solution A is added in a thin stream to 8% to 15% of solution B under sufficient stirring at 60 to 80°C. After solution A is completely added to solution B, 0.5% to 1.5% of emulsifier, 0.05 to 0.15% of preservative, 0.01 to 0.05% of chelating agent and 8% of rice wine lees extract are added and mixed evenly. Purified water is added to make up to 100 ml. The emulsified system is placed in an ultrasonic cell disruptor and ultrasonically emulsified with a probe at 60 to 80°C for 5 to 10 minutes to obtain an emulsion. After the emulsion is cooled to room temperature, it becomes semi-solid, thus obtaining a rice wine lees mask.

9. The method for preparing a rice wine lees facial mask according to claim 8, characterized in that: In step (1), the mass ratio of cetearyl alcohol: liquid paraffin: squalane hydrogenated polyisobutylene: glycerol monostearate: tocopherol acetate is 24:8:12:1:

1.

10. The method for preparing a rice wine lees facial mask according to claim 8, characterized in that: In step (2), the mass ratio of moisturizer: skin permeation enhancer: niacinamide is 4:1:3.

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