阅读说明：本技术 一种含金莲花活性成分保湿面膜及其制备方法 (Moisture mask containing active ingredients of trollius chinensis bunge and preparation method of moisture mask ) 是由 刘洋 简佳琦 陈梦玲 高林 郑丽雪 张扬 于 2021-10-13 设计创作，主要内容包括：本发明公开了一种含金莲花活性成分保湿面膜,包括以下质量百分比的原料：金莲花花茎复配提取物2.5％,1,2-丙二醇6％,甘油4％,透明质酸钠0.6％,玫瑰纯露4％,聚丙烯酰胺0.3％,余量为去离子水。对面膜稳定性及性能进行研究,结果表明,该产品具有耐寒、耐热性能,并且离心后不会产生分层状态,成品面膜表面细腻呈凝胶状态,经测试后测得pH为7.27,呈弱碱性,保湿率高达99.30％,香味持久不刺鼻,与其他产品对比保湿率较高。(The invention discloses a moisture mask containing active ingredients of trollius chinensis bunge, which comprises the following raw materials in percentage by mass: 2.5 percent of compound extract of the Chinese globeflower stems, 6 percent of 1, 2-propylene glycol, 4 percent of glycerin, 0.6 percent of sodium hyaluronate, 4 percent of rose hydrosol, 0.3 percent of polyacrylamide and the balance of deionized water. The stability and the performance of the facial mask are researched, and the result shows that the product has cold resistance and heat resistance, a layering state cannot be generated after centrifugation, the surface of the finished facial mask is fine and smooth and is in a gel state, the pH value is 7.27 after testing, the finished facial mask is alkalescent, the moisture retention rate is as high as 99.30%, the fragrance is lasting and not pungent, and the moisture retention rate is higher compared with other products.)

1. A moisture mask containing active ingredients of trollius chinensis bunge is characterized in that: comprises the following raw materials

The preparation method comprises the following steps of (1) compounding an extract of a trollius chinensis stem, 1, 2-propylene glycol, glycerin, sodium hyaluronate, rose hydrosol, polyacrylamide and deionized water;

the compound trollius chinensis stem extract is composed of trollius chinensis crude polysaccharide and trollius chinensis crude flavone extracted from trollius chinensis stems.

2. The trollius chinensis bunge active ingredient moisturizing mask as claimed in claim 1, wherein: the trollius chinensis moisture-preserving mask further comprises polyacrylamide and a preservative; the preservative is PE 9010.

3. The trollius chinensis bunge active ingredient moisturizing mask as claimed in claim 1, wherein:

the extraction method of the trollius chinensis bunge crude polysaccharide comprises the following steps: drying, crushing, sieving and leaching the trollius chinensis stems in hot water for 1-3 times, wherein the temperature of the hot water is 60-90 ℃, the extraction time is 1-3h, and the material-liquid ratio is 1: 20-1: 60 g/mL; centrifuging to obtain a solution, filtering, then carrying out vacuum concentration under reduced pressure, carrying out alcohol precipitation, carrying out centrifugal separation, carrying out low-temperature freeze drying to obtain globeflower stem polysaccharide, and carrying out freeze drying to obtain globeflower crude polysaccharide;

the extraction method of the trollius chinensis bunge crude flavone comprises the following steps: drying the cauliflower, crushing, sieving and placing into an ethanol water solution, wherein the temperature is 60-90 ℃, the extraction time is 2-5h, and the material-liquid ratio is 1: 30-1: 60g/mL, extracting the crude flavone of the trollius chinensis stems, and carrying out freeze drying to obtain the crude flavone of the trollius chinensis.

4. The trollius chinensis baill moisturizing mask as claimed in any one of claims 1 to 3, wherein: the weight ratio of the trollius chinensis crude polysaccharide to the trollius chinensis crude flavone in the compound extract of the trollius chinensis stems is 9:1-7: 3.

5. The trollius chinensis baill moisturizing mask as claimed in claim 4, wherein: the weight ratio of the trollius chinensis crude polysaccharide to the trollius chinensis crude flavone in the compound extract of the trollius chinensis stems is 7: 3.

6. The trollius chinensis baill moisturizing mask as claimed in claim 5, wherein: the trollius chinensis moisture-preserving mask comprises the following raw materials in percentage by weight: 1 to 5 percent of compound extract of the Chinese globeflower scape; 1% -8% of 1, 2-propylene glycol; 0.1 to 0.8 percent of sodium hyaluronate; 3% -5% of glycerin; 2% -6% of rose hydrosol; 0.1 to 0.7 percent of polyacrylamide; 0.1 to 0.7 percent of preservative; the balance being deionized water.

7. The trollius chinensis baill moisturizing mask as claimed in claim 6, wherein: the trollius chinensis moisture-preserving mask comprises the following raw materials in percentage by weight: 2.5 percent of compound trollius chinensis stems extract; 6% of 1, 2-propylene glycol; 0.6 percent of sodium hyaluronate; 4% of glycerol; 4% of rose hydrosol; 0.3 percent of polyacrylamide; 0.3 percent of preservative; the balance being deionized water.

8. A preparation method of the trollius chinensis bunge moisturizing mask as claimed in claim 7, comprising the following steps:

s1, preparation of phase A:

weighing transparent acid sodium in a cup, adding a proper amount of water, and continuously stirring in a water bath at the temperature of 80 +/-5 ℃ until the transparent acid sodium is completely dissolved;

b, weighing the compound extract of the Chinese globeflower scape in the cup a, pouring the compound extract into the cup a, mixing the two solutions, adding the rose hydrosol, stirring to fully mix the three solutions, and putting the three solutions in a water bath kettle at the temperature of 80 +/-5 ℃ for heat preservation;

s2, preparation of phase B: dissolving glycerol and 1, 2-propylene glycol in deionized water;

s3, slowly mixing the phase A and the phase B, and adding a preservative PE9010 under slow stirring;

s4, weighing polyacrylamide, and dissolving the polyacrylamide in deionized water; adding into the mixed solution to obtain emulsion, sealing, and sterilizing in 80 + -5 deg.C water bath;

and S5, placing all required experimental articles in a sterile operating platform for sterilization, and filling in the sterile operating platform.

Technical Field

The invention relates to the technical field of daily cosmetics, and particularly relates to a moisture mask containing active ingredients of trollius chinensis bunge and a preparation method of the moisture mask.

Background

There are many other names of globeflower, also called dry globeflower, drynaria, keloid, and is a plant of globeflower of Ranunculaceae. Most growing sites are in grass slopes, loose jungles, or mountainous regions, and the elevation is usually 1000-. The habit is that the plant likes to grow in a cold and wet place, and can keep normal growth in a low-temperature environment of 2-15 ℃ throughout the year. The distribution is wide, and the western parts of Shanxi, Henan northern part, Hebei, inner Mongolia eastern part, Liaoning and Jilin all grow.

The trollius chinensis polysaccharide is a heteropolysaccharide, belongs to one of plant polysaccharides, and has the functions and properties of some plant polysaccharides. The plant polysaccharide has various biological activities of immunoregulation, anti-tumor effect, anti-aging effect, blood sugar reduction and the like, and has the advantages of small toxic and side effects, difficult residue generation and the like, so that the research range of the plant polysaccharide is enlarged, and nearly hundreds of plant polysaccharides are widely applied to health-care foods and medicines. At present, the trollius chinensis petals are often used as medicinal raw materials to be effectively utilized, but the stem height of the trollius chinensis petals can reach 80-100 cm at most, and effective research and utilization are not yet achieved. If the polysaccharide in the trollius chinensis flower stems is deeply developed, the utilization rate of the trollius chinensis by-products is greatly improved, and the application value of the trollius chinensis by-products is improved.

Disclosure of Invention

The invention aims to provide a moisturizing facial mask containing active ingredients of trollius chinensis bunge, and further provides a moisturizing facial mask with excellent oxidation resistance and moisturizing performance, which has excellent moisturizing rate in the early stage and the later stage of use compared with the traditional facial mask.

In order to achieve the purpose, the invention adopts the technical scheme that:

a moisture mask containing flos Trollii active ingredients comprises the following raw materials

The preparation method comprises the following steps of (1) compounding an extract of a trollius chinensis stem, 1, 2-propylene glycol, glycerin, sodium hyaluronate, rose hydrosol, polyacrylamide and deionized water; the compound trollius chinensis stem extract is composed of trollius chinensis (crude) polysaccharide and trollius chinensis (crude) flavone extracted from trollius chinensis stems.

Preferably, the trollius chinensis bunge moisturizing facial mask further comprises polyacrylamide and a preservative; the preservative is preferably PE 9010;

preferably, the extraction method of the trollius chinensis bunge crude polysaccharide comprises the following steps: drying, crushing, sieving and leaching the trollius chinensis stems in hot water for 1-3 times, wherein the temperature of the hot water is 60-90 ℃, the extraction time is 1-3h, and the material-liquid ratio is 1: 20-1: 60 (g/mL); centrifuging to obtain a solution, filtering, then carrying out vacuum concentration under reduced pressure, carrying out alcohol precipitation, carrying out centrifugal separation, carrying out low-temperature freeze drying to obtain globeflower stem polysaccharide, and carrying out freeze drying to obtain globeflower crude polysaccharide; the extraction method of the trollius chinensis bunge crude flavone comprises the following steps: drying the cauliflower, crushing, sieving and placing into an ethanol water solution, wherein the temperature is 60-90 ℃, the extraction time is 2-5h, and the material-liquid ratio is 1: 30-1: 60(g/mL), extracting the crude flavone of the trollius chinensis stems, and carrying out freeze drying to obtain the crude flavone of the trollius chinensis.

Preferably, the weight ratio of the trollius chinensis crude polysaccharide to the trollius chinensis crude flavone in the compound extract of the trollius chinensis stems is 9:1-7: 3; further preferably 7: 3;

preferably, the trollius chinensis bunge active ingredient moisturizing mask comprises the following raw materials in percentage by weight: 1 to 5 percent of compound extract of the Chinese globeflower scape; 1% -8% of 1, 2-propylene glycol; 0.1 to 0.8 percent of sodium hyaluronate; 3% -5% of glycerin; 2% -6% of rose hydrosol; 0.1 to 0.7 percent of polyacrylamide; 0.1 to 0.7 percent of preservative; the balance being deionized water.

Preferably, the trollius chinensis bunge active ingredient moisturizing mask comprises the following raw materials in percentage by weight: 2.5 percent of compound trollius chinensis stems extract; 6% of 1, 2-propylene glycol; 0.6 percent of sodium hyaluronate; 4% of glycerol; 4% of rose hydrosol; 0.3 percent of polyacrylamide; 0.3 percent of preservative; the balance being deionized water.

According to another aspect of the invention, the invention also provides a preparation method of the trollius chinensis bunge active ingredient moisturizing facial mask, which comprises the following steps:

s1, preparation of phase A:

weighing a proper amount of transparent acid sodium in a cup, adding a proper amount of water, and continuously stirring in a water bath at the temperature of 80 +/-5 ℃ until the transparent acid sodium is completely dissolved;

b, weighing a proper amount of the compound extract of the trollius chinensis stems in the cup a, pouring the mixture into the cup a, mixing the two solutions, adding the rose hydrosol, stirring to fully mix the three solutions, and putting the three solutions in a water bath kettle at the temperature of 80 +/-5 ℃ for heat preservation.

S2, preparation of phase B: the glycerol and the 1, 2-propylene glycol are taken and added with a certain amount of water to be dissolved in the deionized water.

S3, slowly mixing the phase A and the phase B, and adding the preservative PE9010 under slow stirring.

S4, weighing polyacrylamide, and dissolving the polyacrylamide in deionized water. Adding into the mixed solution to obtain emulsion, sealing, and sterilizing in 80 + -5 deg.C water bath for 15 min.

And S5, placing all required experimental articles in a sterile operating platform, sterilizing for 30min, and filling in the sterile operating platform.

Compared with the prior art, the invention has the following advantages:

1) according to the invention, the trollius chinensis (crude) polysaccharide extracted from the trollius chinensis stems and the trollius chinensis (crude) flavone are compounded for the first time to form the trollius chinensis stem compound extract for preparing the moisturizing facial mask, and surprisingly, the moisturizing and antioxidant effects after compounding are remarkably superior to those of single use, especially when the weight ratio of the trollius chinensis (crude) polysaccharide to the trollius chinensis (crude) flavone is 7: 3;

2) compared with the traditional mask, the moisturizing mask prepared by the invention has excellent moisturizing rate in the early stage and the later stage of use;

3) the product prepared by the invention has cold resistance and heat resistance, does not generate a layered state after centrifugation, and the surface of the finished facial mask is fine and smooth and is in a gel state, and the pH value is 7.27 after testing, the finished facial mask is alkalescent, the moisture retention rate is as high as 99.30%, the fragrance is lasting and not pungent, and the moisture retention rate is higher compared with other products.

Drawings

FIG. 1 shows the effect of the compounding ratio of crude flos Trollii flavone and crude polysaccharide extract on the clearance rate of hydroxyl free radicals.

FIG. 2 shows the effect of the compound ratio of crude flavones and polysaccharide extracts of trollius chinensis on moisture retention.

Figure 3 is a graph of the effect of formulation dosage on moisturizing rate.

Fig. 4 shows the effect of 1,2 propylene glycol usage on moisturization.

Fig. 5 is a graph showing the effect of sodium hyaluronate dosage on moisturizing rate.

Fig. 6 is a graph showing the effect of glycerol usage on moisturizing efficiency.

FIG. 7 shows the effect of rose hydrosol dosage on moisture retention.

Figure 8 is a comparison of moisturizing effect of the samples and the control product.

Detailed Description

Raw material sources and specifications thereof:

1. polyacrylamide, often used as a thickener, of the formula (C)₃H₅NO) n, molecular weight of 1X 10⁴～2×10⁷Da. The density is 1.302g/cm³(23℃)。

2. Sodium hyaluronate of the formula (C)₁₄H₂₀NO₁₁Na) n, molecular weight of 5X 10⁵～12×10⁵Da。

Is an inherent component in human body, is a glucan aldehyde acid, has no species specificity and has the density of 1.78g/cm³。

The preservative PE9010, the phenoxyethanol and the ethylhexyl glycerin are compounded, have good inhibition effects on bacteria, yeasts and molds, are typical antibacterial and antiseptic products, and have a certain sterilization capacity.

1,2 propylene glycol of formula C₃H₈O₂Molecular weight of 76.09, density of 1.0381g/cm³. Can be used as raw material of unsaturated polyester resin, and can be used as humectant in cosmetics, toothpaste and soap in combination with glycerol or sorbitol.

Glycerol, formula C₃H₈O₃Molecular weight 92.09, density 1.261g/cm³(20 ℃ C.). Colorless, transparent, odorless, viscous liquid, sweet taste, and hygroscopicity. Mixing with water and alcohols, amines and phenols in any ratio, and making the aqueous solution neutral.

Rose hydrosol refers to the water left by the essential oil during the distillation and extraction process.

Extraction of trollius chinensis stem extract

Extraction of trollius chinensis crude polysaccharide

Drying the trollius chinensis stems, crushing the dried trollius chinensis stems by a crusher, sieving the crushed trollius chinensis stems by a sieve of 100 meshes, and leaching the washed trollius chinensis stems in hot water for 1 to 3 times, wherein the temperature of the hot water is 60 to 90 ℃, the extraction time is 1 to 3 hours, and the material-liquid ratio is 1: 20-1: 60 (g/mL); centrifuging to obtain filtrate, filtering, vacuum concentrating under reduced pressure to 1/10 of original volume, precipitating with ethanol, centrifuging, freeze drying at low temperature to obtain flos Trollii stem polysaccharide, and freeze drying to obtain flos Trollii crude polysaccharide;

extraction of trollflower crude flavone

Drying the cauliflower, crushing the cauliflower by a crusher, sieving the cauliflower by a 100-mesh sieve, adding an ethanol solution with the concentration of 60V%, extracting at the temperature of 60-90 ℃ for 2-5h, wherein the material-liquid ratio is 1: 30-1: 60(g/mL), extracting the crude flavone of the trollius chinensis stems, and freeze-drying the crude flavone of the trollius chinensis for later use to obtain the crude flavone of the trollius chinensis.

Measurement of in vitro moisture retention

The moisturizing activity of cosmetics such as a globeflower stem compound extract, chitosan, sodium alginate, sodium hyaluronate and the like is researched by commonly using a humectant. Drying the mixture in a 100 ℃ oven for 4h, placing the dried mixture in a dryer with the bottom added with dry allochroic silica gel, adding 20mL of distilled water into each sample, accurately weighing the mass, placing the sample in the dryer, placing the whole dryer in a constant-temperature incubator at 25 ℃, and accurately weighing the mass by using an analytical balance after placing the sample for 2h, 4h, 8h, 10h and 12h respectively.

Moisture retention (%) - (amount of decrease in sample moisture/original sample mass) × 100%

Determination of in vitro antioxidant Properties

Hydroxyl radicals can kill red blood cells, degrade DNA, cell membranes and polysaccharide compounds, damage normal cells, and produce new radicals to cause a series of chemical reactions. The free radicals attack normal cells and tissues indiscriminately, causing a chain peroxidation reaction, and leading the human body to have various degenerative syndromes, such as vascular fragility, immunologic function decline, brain cell aging, degenerative arthritis, cataract, skin relaxation and systemic aging. Therefore, the antioxidant activity of the compound extract of the cauliflower stems is evaluated according to the clearance rate of hydroxyl free radicals.

Gradient solutions with different ratios of crude flos Trollii flavone and crude flos Trollii polysaccharide are added into 2.5mL phosphoric acid buffer solution with pH of 6.6, respectively, i.e. the ratio of crude flavone to crude polysaccharide is 9:1, 7:3, 5: 4, 4: 5, 3: 7, 1: 9. Taking 1.0mL of gradient solution with different proportions, respectively adding 1.0mL of 6mmol/L FeSO₄Adding 1.0mL of 6mmol/L hydrogen peroxide solution into the solution, fully oscillating and shaking the solution, standing the solution for 10min, then respectively adding 1.0mL of 6mmol/L salicylic acid (50% alcohol is used as a solvent), standing the solution for 30min, placing the solution at a wavelength of 510nm to measure absorbance, and taking an average value after 3 experiments. Wherein, distilled water replaces the sample solution as a blank, distilled water replaces the hydrogen peroxide solution as a sample control, and ascorbic acid is used as a positive control. The OH radical clearance was calculated by the following formula and the data was analyzed using one-way anova.

In the formula: a. the₀The hydrogen peroxide solution system is replaced by distilled water; a. the₁The light absorption value of the sample group to be detected; a. the₂The distilled water is used for replacing the light absorption value of the sample solution system.

Examples

Determination of compounding ratio of trollius chinensis bunge extract

The hydroxyl radical clearance results of the trollius chinensis crude flavone and the trollius chinensis crude polysaccharide after being compounded according to the proportion are shown in figure 1. When the compounding ratio (mass ratio) of the trollius chinensis crude flavone to the trollius chinensis polysaccharide crude extract is 7:3, the hydroxyl free radical clearance rate is highest and is higher than that of uncomplexed trollius chinensis single flavone (namely trollius chinensis crude flavone) and polysaccharide (namely trollius chinensis crude polysaccharide), and the antioxidant activity is better.

The trollius chinensis bunge crude flavone and the trollius chinensis bunge crude polysaccharide are compounded according to a proportion to prepare the concentration with the mass fraction of 5%, and the moisturizing result is shown in figure 2. When the compounding ratio of the trollius chinensis bunge crude flavone to the polysaccharide crude extract is 7: and 3, the moisturizing activity reaches 73.08 +/-2.4%, and the moisturizing activity is higher than that of single flavone and polysaccharide of the uncomplexed trollius chinensis, and the glycerin moisturizing rate is close to 5%.

The applicant surprisingly found that when the weight ratio of the compound of the crude flavone and the crude polysaccharide extract of the trollius chinensis is 7:3, the antioxidant has excellent antioxidant activity and excellent moisturizing performance.

Determination of polyacrylamide weight percentage in trollius chinensis moisture-preserving mask

To increase the product stability, an emulsifier, namely polyacrylamide, is added. The polyacrylamide is divided into four groups of 0.7%, 0.5%, 0.3% and 0.1%, essence is prepared respectively, the obtained finished product is selected according to the viscosity, the extensibility during smearing and the stability, the comprehensive score is calculated after 6-person evaluation, and the optimal proportion is selected according to the grade. The sensory evaluation is mainly carried out by making a sensory evaluation standard table, making a sensory evaluation table, selecting sensory evaluators, training the evaluators, and finally carrying out sensory evaluation on the sample, wherein the standard is shown in table 1.

TABLE 1 sensory evaluation scoring criteria

Single-factor experimental design of trollius chinensis moisturizing mask

The determination of the amount of the compound extract of the trollius chinensis stems (the compound weight ratio of the crude flavone and the crude polysaccharide extract of the trollius chinensis stems is 7: 3) takes the compound extract of the trollius chinensis stems as a variable, and the other components are kept unchanged, wherein the total mass is 10g, and the weight percentage of the compound extract of the trollius chinensis stems comprises 4% of 1, 2-propylene glycol, 0.3% of sodium hyaluronate, 4% of glycerol, 4% of rose hydrosol and the balance of deionized water. The compound extract of the Chinese globeflower stems is used as a variable, 1 percent, 2 percent, 3 percent, 4 percent and 5 percent of the mixed material are respectively taken, the mixed material is put into an aluminum box, the weighed aluminum box is put into a drier filled with allochroic silica gel, and the weight of the aluminum box is measured after 12 hours. And calculating the moisture retention rate.

Determination of the amount of 1, 2-propanediol used

1, 2-propylene glycol is used as a variable, other components are kept unchanged, and the compound extract of the Chinese globeflower stems accounts for 2% by weight, the sodium hyaluronate accounts for 0.3% by weight, the glycerin accounts for 4% by weight, the rose hydrosol accounts for 4% by weight, and the balance is deionized water. Selecting 1, 2-propylene glycol as a humectant, adding 1, 2-propylene glycol as a variable into the components to prepare 5 groups of solutions, wherein the dosages are respectively 2%, 3%, 4%, 5% and 6%, putting the solutions into an aluminum box, weighing the solutions, putting the aluminum box into the aluminum box for 12 hours, weighing the aluminum box again, and calculating the moisture retention rate.

Determination of the amount of sodium hyaluronate

Taking sodium hyaluronate as a variable, keeping other components unchanged, and calculating by weight percentage, wherein the amount of the compound extract of the Chinese globeflower stems is 2%, the amount of 1, 2-propylene glycol is 4%, the amount of glycerin is 4%, the amount of rose hydrosol is 4%, and the balance is deionized water. Sodium hyaluronate is selected as a humectant, added into the components according to the variable quantity of sodium hyaluronate to prepare 5 groups of solutions, the dosage of the solutions is 0.1%, 0.2%, 0.3%, 0.4% and 0.5%, the solutions are respectively put into an aluminum box, the aluminum box is weighed, the aluminum box is put into the aluminum box for 12 hours, then the aluminum box is weighed again, and the moisturizing rate is calculated.

Determination of the amount of Glycerol

Taking glycerin as a variable, keeping other components unchanged, and calculating by weight percentage, wherein the amount of the compound extract of the Chinese globeflower stems is 2%, the amount of 1, 2-propylene glycol is 4%, the amount of sodium hyaluronate is 0.3%, the amount of hydrolat is 4%, and the balance is deionized water. Glycerin is selected as a humectant, is added into the components according to the variable of the glycerin to prepare 5 groups of solutions, the dosage of the solutions is 3%, 3.5%, 4%, 4.5% and 5%, the solutions are respectively put into an aluminum box and weighed, the aluminum box is put into the aluminum box for 12 hours and then weighed again, and the moisturizing rate of the solutions is calculated.

Determination of rose hydrosol dosage

Taking rose hydrosol as a variable, keeping other components unchanged, and calculating by weight percentage, wherein the amount of the compound extract of the Chinese globeflower stems is 2%, the amount of 1, 2-propylene glycol is 4%, the amount of sodium hyaluronate is 0.3%, and the balance is deionized water. Rose hydrosol is selected as a humectant and a flavoring agent, and is added into the components according to the rose hydrosol as variables to prepare 5 groups of solutions, the dosage of the solutions is respectively 2%, 3%, 4%, 5% and 6%, the solutions are put into an aluminum box and weighed, the aluminum box is put into the aluminum box for 12 hours and then weighed again, and the moisturizing rate is calculated.

Orthogonal experimental design of trollflower moisturizing mask

On the basis of a single-factor test, taking the addition amount of the trollius chinensis bunge extract in the humectant and the essence and the addition amount of the rose hydrosol as factors to prepare L₁₆(4⁵) And (4) performing a five-factor four-level orthogonal test, and screening the optimal formula of the optimal essence by taking the moisture retention rate of the essence as an index. The levels of orthogonal experimental factors are shown in table 2:

TABLE 2 orthogonal experiment factor horizon

Evaluation of performance of trollius chinensis rose moisturizing mask

Heat and Cold resistance stability test

Putting 10.0g of trollius chinensis moisturizing mask essence into a test tube with the volume of 20mL, sealing the opening of the test tube, placing the test tube at a high temperature of over 80 ℃, taking out after placing for 24 hours, and observing the change condition after placing for 20 minutes at room temperature; similarly, the sealed test tube is placed at a low temperature of above-40 ℃ for 24 hours and observed at room temperature.

Centrifugal test

Dividing 5.0g of flos Trollii essence into two groups at normal temperature, respectively placing into 5mL centrifuge tubes, centrifuging at 1000, 2000, 3000, 4000, 5000r/min for 10min, taking out, and observing whether the sample is stratified.

Character and fineness

10.0g of trollius chinensis bunge essence is placed in a 50mL beaker, and appearance characters of the trollius chinensis bunge essence are observed. The trollius chinensis essential liquid is coated on the skin, and the research is carried out by taking the fineness as an evaluation index.

pH value

The pH value of the sample is measured according to GB/T13531.1-2008 universal detection method for cosmetics. Dissolving 10.0g of trollius chinensis bunge essence in 100mL of distilled water, heating for slightly boiling, cooling to room temperature, and measuring the pH value by using a pH meter.

Skin moisture determination

Selecting 10 subjects to carry out an experiment by using a skin moisture tester, wherein the forearm is a test area; the subject is asked to be free of severe systemic disease, immunodeficiency, or autoimmune disease; an inactive allergic disease; no serious allergic history exists on skin care cosmetics; hormone medicines and immunosuppressants are not used in about 1 month; no other clinical trials were enrolled. The temperature of the test environment is kept at (22 +/-1) ° C, and the relative humidity is kept at (40 +/-5)%. Before testing, the testee uses clear water with the temperature of about 35 ℃ to wipe the two arms, then enters the testing environment to rest for 30min, and then starts testing. The measured data are divided into four parts, namely, before smearing, after smearing for 15min and after washing.

Experimental results and discussion

Determination of acrylamide

After the finished product is successfully prepared and stored in a sealed manner for a period of time, the bottle bottom can be precipitated to form a trollius chinensis bunge compound, in order to increase the stability of the finished product, an emulsifier, namely polyacrylamide, is added into the finished product, the polyacrylamide comprises four components which are 0.7 wt%, 0.5 wt%, 0.3 wt% and 0.1 wt% of the total weight of the moisturizing mask, the essence is prepared respectively, and the obtained finished product is selected according to the wire drawing degree, the extension degree during smearing and the stability, and the result is shown in table 3.

TABLE 3 Polyacrylamide sensory evaluation scores

According to the scores of the sensory evaluation table, when the dosage of the polyacrylamide is 0.3%, the finished product has better stringiness, viscosity, extensibility and stability, so that the dosage of the polyacrylamide is determined to be 0.3%.

Analysis of Single factor Experimental results

Influence of adding amount of compound extract of Chinese globeflower stems on moisture retention rate

As can be seen from fig. 3, when the amount of the compound is 1% to 2%, the moisture retention rate increases with the increase of the amount of the compound, when the amount reaches 2% to 3%, the moisture retention rate decreases with the increase of the amount of the compound, when the amount reaches 3% to 5%, the moisture retention rate increases with the increase of the amount of the compound, but the increase tendency is smaller than the increase tendency with the amount of 1% to 2%, when the amount is 2%, the moisture retention rate reaches the highest, and part of research proves that the moisture retention rate is related to the number of hydrophilic groups and the strength of hydrophilicity, the higher the concentration of the hydroxyl group is, the bonding ability with hydrogen bonds is weakened, the moisture retention rate decreases, and the research shows that the moisture retention rate is obviously decreased after the concentration exceeds 5%. Therefore, 2% of the addition amount of the compound is determined to be used as a single-factor index.

Influence of 1, 2-propylene glycol addition amount on moisturizing rate

As can be seen from fig. 4, when the amount of 1, 2-propanediol is 1% to 3%, the moisture retention rate decreases with increasing amount, when the amount of 1, 2-propanediol is 3% to 5%, the moisture retention rate increases with increasing amount, and when the amount reaches 5%, the moisture retention rate is the highest, and some documents report that the amount of 1, 2-propanediol is generally not more than 5%, and therefore, the amount of 1, 2-propanediol added is determined to be 5% as a one-factor indicator.

Effect of sodium hyaluronate addition on moisture retention

As can be seen from fig. 5, when the amount of sodium hyaluronate is less than 0.5%, the moisturizing rate increases with the increase of the amount, so when the amount is 0.5%, the moisturizing rate is the highest, and since the cost price of sodium hyaluronate is high, the amount is selected to be 0.5% for cost saving, and the specific amount is determined by an orthogonal test.

Effect of Glycerol addition amount on moisture retention

As can be seen from fig. 6, when the amount of glycerin was in the range of 3% to 3.5%, the moisturizing rate decreased with an increase in the amount of glycerin, and when the amount was in the range of 3.5% to 4.5%, the moisturizing rate tended to increase with an increase in the amount of glycerin. When the amount of glycerin reaches 5%, the moisturizing rate gradually decreases with the increase of the amount of glycerin. Therefore, the addition amount of glycerin is 4.5% as a single factor index.

Influence of rose hydrosol addition on moisture retention rate

As shown in fig. 7, the moisture retention rate increases with the increase of the amount of the hydrolat when the amount of the hydrolat reaches 4%, the moisture retention rate gradually decreases with the amount of the hydrolat between 4% and 5%, and the moisture retention rate gradually increases but the increase is decreased with the amount of the hydrolat exceeding 5% to 6%, so that the moisture retention rate reaches the maximum when the amount of the hydrolat reaches 4%. Since the hydrolat is also used as an essence component in the essence, and the whole aroma of the mask can be influenced if the concentration is high, 4% of the hydrolat is selected as a single-factor index.

Orthogonal experiment and verification experiment result analysis

Analysis of results of orthogonal experiments

Optimizing the facial mask formula on the basis of single factor, and designing five-factor four-level L16 (4)⁵) The specific experimental results of the orthogonal test are shown in table 4:

TABLE 4 results of orthogonal experiments

On the basis of a compound, sodium hyaluronate, glycerin, hydrolat and 1,2 propylene glycol single-factor experiment, a five-factor four-level orthogonal experiment is carried out, the orthogonal experiment result table for obtaining the moisture retention rate is shown in table 4, and according to the orthogonal experiment result table 4, D can be found by comparing the extreme difference result R values of all columns>C>B>E>And A, among the factors set by the test, the glycerol has the largest influence on the moisture retention rate of the mask, and the sodium hyaluronate, the 1, 2-propylene glycol, the hydrolat and the compound are used, and the hydrolat has the smallest influence on the moisture retention rate of the mask. By comparing the k values, the optimal combination is determined to be A₄B₂C₂D₂E₄Not shown in the table, the moisture retention rate was determined to be 99.12% + -3.42% by empirical test, slightly worse than A in the orthogonal table₄B₄C₁D₃E₂And (4) combining. Thus, A is selected₄B₄C₁D₃E₂The combination is the optimal level, namely the addition of the trollius chinensis bunge compound is 2.5 percent, the addition of 1, 2-propylene glycol is 6.0 percent, the addition of sodium hyaluronate is 0.6 percent, the addition of glycerin is 4.0 percent, the addition of pure dew is 4.0 percent, and the moisture retention rate can reach 99.30 percent.

Evaluation results of stability and Performance of mask

Optimal formulation according to orthogonal test (A)₄B₄C₁D₃E₂) The stability results of the prepared mask product are shown in table 5, the mask has good cold resistance and heat resistance, no layering is performed after centrifugation, the stability is good, the product is light brown, has light rose fragrance, and is uniform, fine and smooth in texture, and the pH value of the finished product is 7.27 and is alkalescent.

Table 5 evaluation results of mask stability

Comparison result of trollflower rose moisturizing mask and traditional mask

Moisture retention rate measurement

The product was compared with four other products, five different products of the same amount were put in an aluminum box and all put in a desiccator, and the moisture retention rates of the five products were measured and compared after 2h and 4h, respectively, with the results shown in table 6.

TABLE 6 comparison of sample to moisturizing ratio of four products

Through test analysis, the products 1 and 3 have better effects immediately after use, but the moisture retention rate is reduced faster. Although the moisture retention rate of the products 2 and 4 at the early stage is lower than that of the products 1 and 3, the moisture retention rate is reduced slowly, and the moisture retention rate is relatively high after 4 hours. The moisture retention rate of the product in the early stage is higher than that of the other four products, and the moisture retention rate after 4 hours is also higher than that of the other four products. Compared with other moisturizing essences, the moisturizing essence has a good moisturizing effect. Among other four products, 2 # and 4 moisturizing effects are equivalent, are slightly more than 1 # and 3 # and select 1 # product at last to carry out moisture test contrast with this product.

The temperature of the test environment is kept at (22 +/-1) ° C, and the relative humidity is kept at (40 +/-5)%. Before testing, the testee uses clear water with the temperature of about 35 ℃ to wipe the two arms, then enters the testing environment to rest for 30min, and then starts testing. The measured data are divided into four parts, namely before smearing, after smearing for 15min and after washing. The test results are shown in table 7, with the test results for the comparative product applied to the left hand and the test result for the product applied to the right hand of the subject:

table 7 comparative table for skin moisture test of products

As can be seen from FIG. 8, the product and the comparative product showed good moisturizing effect after being applied by the testers. After the product is smeared for 15min, the moisture retention rate of the product is close to that of a comparison product, but the moisture retention rate difference of the two products is reduced, and the moisture retention rate and the stability of the product after washing are also obviously higher than those of the comparison product. Therefore, the product has better overall moisture retention rate than a control product immediately after being smeared to be cleaned.

The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.