CN107802543B - Roxburgh rose element skin-refreshing biological fiber mask and preparation method thereof - Google Patents
Roxburgh rose element skin-refreshing biological fiber mask and preparation method thereof Download PDFInfo
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- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
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- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
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Abstract
The invention belongs to the technical field of skin care product processing, and particularly relates to a roxburgh rose element skin-refreshing biological fiber mask; comprises a biological fiber membrane material, a roxburgh rose extract and rose water; the facial mask obtained by the special extraction process and the preparation method has good biocompatibility, high water retention and good wet flexibility, and has the effects of softening epidermal keratinase, promoting shedding of the epidermal keratinase, inhibiting growth of microorganisms in hair follicles, removing oxygen radicals, stimulating growth and division of cells, fading fine lines, reducing wrinkles and refreshing skin.
Description
Technical Field
The invention belongs to the technical field of skin care product processing, and particularly relates to a roxburgh rose essence skin-refreshing biological fiber mask and a preparation method thereof.
Background
With the development of economy, the pressure of life of more and more women is gradually increased, so that the women face irregular computer and life every day, and the physical function is gradually reduced. Free radicals are atoms, molecules or ions containing unpaired electrons produced during metabolism of biological cells, e.g. O2 -OH, etc., which have destructive effects on many biologically functional molecules, and normally, the production and elimination of free radicals in cells are in dynamic equilibrium. However, when the living organisms are injured, diseased and aged, the balance is broken, and the generated large amount of free radicals destroy important molecules with biological functions, such as proteins, lipids, polysaccharides and nucleic acids, so that facial skin problems, such as dullness, spots, uneven skin color, wrinkles, yellowing and the like, become increasingly significant, and thus, a safer and more effective skin care product needs to be found.
Rosa roxburghii Tratt is a wild plant of deciduous shrubs and is mainly distributed in southwest provinces of Guizhou, Yunnan and the like in China, wherein Guizhou resources are most abundant. In recent years, researches show that the high-grade rosa roxburghii tratt in Guizhou is rich in beauty vitamin C, E, anti-aging factors (SOD), trace elements such as Cu, Fe, Zn, Se, Mn and the like, wherein the contents of vitamin C, SOD and vitamin P are the best of fruits, and the rosa roxburghii tratt is known as 'Sanwang fruit' and has important beauty value. In addition, the roxburgh rose is also a national medicinal material in Guizhou province, and has the effects of invigorating stomach, helping digestion, nourishing, stopping diarrhea and the like; also has the medicinal values of improving immunity, resisting arteriosclerosis, delaying senility, reducing blood fat, preventing cancer, resisting cancer and the like.
Roses (Rosa rugosa Thumb.) are rare flowers, have high ornamental value and have high edible, medicinal and cosmetic values.
At present, a lot of documents and patents exist for applying rosa roxburghii tratt and rose to beauty and skin care products, but the production technology is simple, the formula is complex, and most of rosa roxburghii tratt and rose contain preservatives, so that the safety and the efficacy of the products are low, and the requirements of consumers are difficult to meet.
Disclosure of Invention
The invention provides a roxburgh rose element skin-refreshing biological fiber mask and a preparation method thereof, aiming at solving the technical problems.
The method is realized by the following technical scheme:
the roxburgh rose essence skin-refreshing biological fiber mask is characterized by comprising a biological fiber film material and natural extracted effective components, wherein the natural extracted effective components comprise, by mass, 55% -75% of roxburgh rose extract and 25% -45% of rose water.
Further, the roxburgh rose extract comprises the following preparation steps:
1) cleaning fresh roxburgh rose, and draining water for later use;
2) mixing the cleaned roxburgh rose and the solution 1 according to the mass ratio of 3:0.3-0.4, oscillating for 40-50min under the condition of 100-;
3) adding 30-47 times of 1 mass of filter residue into 3, performing ultrasonic extraction at 30-42 deg.C and 300-;
4) adding 15-20% fermentation liquid of precipitate 1 mass, mixing with precipitate 1, fermenting at 25-37 deg.C for 3-4 days to obtain fermentation material, adding clear water of 3-4 times of fermentation material mass, and reflux extracting for 3-4 hr to obtain extractive solution 3;
5) mixing the extractive solutions 1, 2 and 3, adding activated carbon decolorant 2-3 wt% of the mixture, and filtering.
Further, the solution 1 is 5-7.3% of glycerol by volume fraction, 6.7-8.0% of rock candy by mass fraction, 0.01-0.04 mol/L of potassium chloride by mass fraction, and 10-13% of beer by volume fraction.
Further, the solution 2 is 0.2-0.35 mol/L mol of sodium phosphate solution, and the volume fraction is 5-6% of glycerol.
Further, the solution 3 is an ethanol solution with the volume fraction of 55-70%.
Further, the fermentation liquor is prepared by mixing bacillus subtilis freeze-dried powder, acetic acid monomonas oxide freeze-dried powder, yeast freeze-dried powder, brandy, tribute vegetable powder, mushroom powder and clean water according to the mass ratio of 0.4-0.6:0.2-0.33:0.4-0.45:1-2.4:2.0-2.3:0.8-1.2:200, and culturing at 25-35 ℃ and 230r/min for 2-3 h.
Further, the fermentation comprises spraying brown sugar water during the fermentation period, wherein the spraying amount is 20-24% of the mass of the precipitate 1, and the spraying is carried out for 3-4 times, and the spraying is carried out once a day.
Further, the rose water is prepared by mixing rose petals, egg white, yellow sugar and deionized water according to the mass ratio of 10-15:0.5-1:0.7-1.1:3-5, heating at 40-45 ℃ for 20-30min, standing at 25-30 ℃ for 15-17h to obtain a material 1, adding deionized water which is 50-100 times of the mass of the material 1, heating and refluxing for extraction for 60-80min, filtering the refluxed extract, and storing at 20-35 ℃ for later use.
The roxburgh rose essence skin-refreshing biological fiber mask further comprises the following preparation steps:
1) sterilizing the biological fiber membrane material and the aluminum bag for later use;
2) and (3) folding the membrane material in a 30-thousand air cleaning area, filling the membrane material into an aluminum bag, filling the roxburgh rose extract and rose water, and sealing the opening to obtain the rose flower water-containing film.
Further, the biological fiber membrane material is membrane cloth prepared by fermenting hypha from acetobacter xylinum, and is characterized by comprising the following preparation steps:
1) preparing a basic fermentation culture medium, namely 28-35 g/L of glucose, 3-5 g/L of glycerol, 6 g/L of yeast extract, 4-8 g/L of additive, 10-15 g/L of peptone, 1-1.3 g/L of sodium citrate, 2-2.5 g/L of magnesium sulfate, 2-3 g/L of calcium chloride, 0.3-0.5 g/L of zinc sulfate, pH6.3-7.0, and performing wet heat sterilization for 20-25min for later use;
2) culturing: inoculating activated acetobacter xylinum to a basic fermentation culture medium, oscillating for 1-2h under the conditions of 28-30 ℃ and 150-80 r/min, statically culturing for 6-8 days at 30 ℃, oscillating for 20-30min at 25-28 ℃ and 50-80r/min, irradiating by infrared light at 650nm for 15-20min at 630-;
3) taking out the cellulose membrane in the culture medium, washing with deionized water, soaking in 1 mol/L sodium hydroxide solution for 24-26h, pouring out the solution, boiling in 1 mol/L sodium hydroxide solution for 15-20min, repeatedly washing with water, treating with steam at 55-60 deg.C for 20-30min, soaking in 1% acetic acid for 10-13min, and repeatedly washing with water to obtain the final product;
wherein the additive is prepared by mixing tartary buckwheat, bananas and green tea according to the mass ratio of 3-5:1.2-1.5:0.3-0.6, crushing, adding an acetic acid solution which is 10-15% of the mass of the mixed powder and is 3-5 times of the mass of the mixed powder, standing at 30-35 ℃ for 20-22h to obtain a material 1, adding clear water which is 5-7 times of the mass of the material 1, decocting for 3-4h, filtering, and drying the filtrate.
The method has the beneficial effects that the active ingredients of the roxburgh rose are extracted in batches, the solution 1 is mixed with the roxburgh rose before the extraction is started, the mixture is oscillated and frozen for 2 hours, steam is introduced for treatment, and the solution 2 is extracted to ensure that the activity of the extracted SOD enzyme is kept well and the structure is complete. Through filtering, extracting the filter residue with ethanol, filtering, fermenting the filter residue with a special leaven and re-extracting, the SOD enzyme activity in the obtained roxburgh rose extract is up to 435.9g/u, oxygen free radical and OH can be effectively removed, the removal rate is respectively 96.3 percent and 95.0 percent, the skin aging is slowed down, in addition, the roxburgh rose filter residue is treated through fermentation, the obtained extract can inhibit pityrosporum orbiculare, propionibacterium acnes and staphylococcus aureus causing acne, and the inhibition rate is respectively up to 86.4 percent, 93.7 percent and 88.7 percent.
In addition, the prepared biological fiber membrane material has good biocompatibility, high water retention and good wet flexibility by culturing the acetobacter xylinum through a special culture medium and a special culture method, and the roxburgh rose extract and the rose water prepared by the method are matched, so that after the membrane material is used for 4 weeks, waste cutin on the outer layer of the skin is softened and peeled off, the growth of microorganisms in hair follicles is inhibited, redundant free radicals are eliminated, the growth and the division of cells are stimulated, and the skin percutaneous water loss value (TEW L value) is measured by a skin water loss instrument and is reduced to 15.5g/hm2The moisture content of the skin is as high as 68.2A.U., the R2 value of the skin elasticity is increased to 0.75, the skin barrier function is obviously improved, and the water locking capacity of the skin is improved; the elasticity value of the skin rises, and the fishtail lines and the wrinkles under the eyes of the volunteers are obviously reduced and lightened, which shows that the facial mask has the effects of lightening the fine lines, reducing the wrinkles and revitalizing the skin.
Detailed Description
The following is a detailed description of the embodiments of the present invention, but the present invention is not limited to these embodiments, and any modifications or substitutions in the basic spirit of the embodiments are included in the scope of the present invention as claimed in the claims.
Example 1
The roxburgh rose essence skin-refreshing biological fiber facial mask comprises a biological fiber facial mask material and natural extracted effective components, wherein the natural extracted effective components comprise, by mass, 55% of roxburgh rose extract and 45% of rose water.
The roxburgh rose extract comprises the following preparation steps:
1) cleaning fresh roxburgh rose, and draining water for later use;
2) mixing the cleaned roxburgh rose and the solution 1 according to a mass ratio of 3:0.3, oscillating for 40min at 100r/min, freezing for 1h at minus 10 ℃, introducing 120 ℃ steam for processing for 2min, homogenizing the roxburgh rose at 2 ℃, adding 10 times of roxburgh rose mass solution 2, performing ultrasonic extraction for 30min at 250w ultrasonic power and 2 ℃, performing ultrasonic 5s during ultrasonic processing, pausing for 10s, and filtering to obtain an extracting solution 1 and a filter residue 1;
3) adding 30 times of 1 mass of filter residue into 3, ultrasonic extracting at 30 deg.C and 300w for 40min, centrifuging at 8000rpm for 40min to obtain supernatant and precipitate 1, and recovering ethanol from the supernatant under reduced pressure and reflux to obtain extractive solution 2;
4) adding 15% of fermentation liquor with the mass of 1 precipitate, mixing with the precipitate 1, fermenting at 25 ℃ for 3 days to obtain a fermentation material, adding clear water with the mass of 3 times of the fermentation material, and performing reflux extraction for 3 hours to obtain an extracting solution 3;
5) mixing the extract solutions 1, 2 and 3, adding activated carbon decolorant with the mass of 2% of the mixed solution, and filtering to obtain the product.
The solution 1 is 5% of glycerol by volume fraction, 6.7% of rock candy by mass fraction, 0.01 mol/L of potassium chloride by mass fraction, and 10% of beer by volume fraction.
The solution 2 is 0.2 mol/L sodium phosphate solution, and the volume fraction is 5% of glycerol.
The solution 3 is an ethanol solution with the volume fraction of 55%.
The fermentation liquor is prepared by mixing bacillus subtilis freeze-dried powder, acetic acid monomonas oxide freeze-dried powder, yeast freeze-dried powder, brandy, ivy mosses powder, mushroom powder and clean water according to the mass ratio of 0.4:0.2:0.4:1:2.0:0.8:200, and culturing at 25 ℃ and 200r/min for 2 hours.
The fermentation comprises spraying brown sugar water in an amount of 20% of the mass of the precipitate 1 during the fermentation, and spraying for 3 times, once a day.
The rose water is prepared by mixing rose petals, egg white, brown sugar and deionized water according to a mass ratio of 10:0.5:0.7:3, heating at 40 ℃ for 20min, standing at 25 ℃ for 15h to obtain a material 1, adding 50 times of deionized water by mass of the material 1, heating and refluxing for extraction for 60min, filtering the refluxed extracting solution, and storing at 20 ℃ for later use.
The roxburgh rose essence skin-refreshing biological fiber mask comprises the following preparation steps:
1) sterilizing the biological fiber membrane material and the aluminum bag for later use;
2) and (3) folding the membrane material in a 30-thousand air cleaning area, filling the membrane material into an aluminum bag, filling the roxburgh rose extract and rose water, and sealing the opening to obtain the rose flower water-containing film.
The biological fiber membrane material is membrane cloth prepared by fermenting hypha from acetobacter xylinum, and comprises the following preparation steps:
1) preparing a basic fermentation culture medium, namely 28 g/L glucose, 3 g/L glycerol, 6 g/L yeast extract, 4 g/L additive, 10 g/L peptone, 1 g/L sodium citrate, 2 g/L magnesium sulfate, 2 g/L calcium chloride, 0.3 g/L zinc sulfate, pH6.3, and performing moist heat sterilization for 205min for later use;
2) culturing: inoculating activated acetobacter xylinum to a basic fermentation culture medium, oscillating for 1h under the conditions of 28 ℃ and 150r/min, statically culturing for 6 days at 30 ℃, oscillating for 20min at 25 ℃ and 50r/min, irradiating by using infrared light of 630nm for 15min, and statically culturing for 2 days at 30 ℃ to obtain a cellulose membrane;
3) taking out the cellulose membrane in the culture medium, washing with deionized water, soaking in 1 mol/L sodium hydroxide solution for 24h, pouring out the solution, boiling in 1 mol/L sodium hydroxide solution for 15min, washing with water repeatedly, treating with 55 deg.C steam for 20min, soaking in 1% acetic acid for 10min, and washing with water repeatedly to obtain the final product;
wherein the additive is prepared by mixing tartary buckwheat, bananas and green tea according to the mass ratio of 3:1.2:0.3, crushing, adding an acetic acid solution which is 10% of the mass of the mixed powder and is 3 times of the mixed powder, standing at 30 ℃ for 20 hours to obtain a material 1, adding clear water which is 5 times of the material 1 in mass, decocting for 3 hours, filtering, and drying the filtrate.
Example 2
A roxburgh rose essence skin-refreshing biological fiber facial mask comprises a biological fiber facial mask material and natural extracted effective components, wherein the natural extracted effective components comprise, by mass, 65% of roxburgh rose extract and 35% of rose water.
The roxburgh rose extract comprises the following preparation steps:
1) cleaning fresh roxburgh rose, and draining water for later use;
2) mixing the cleaned roxburgh rose and the solution 1 according to the mass ratio of 3:0.35, oscillating for 45min at 160r/min, freezing for 1.2h at minus 13 ℃, introducing 130 ℃ steam for treating for 2.2min, homogenizing the roxburgh rose at 4 ℃, adding 11 times of roxburgh rose mass solution 2, performing ultrasonic extraction at 260w and 4 ℃ for 35min, performing ultrasonic extraction for 6s during ultrasonic treatment, pausing for 10s, and filtering to obtain an extracting solution 1 and a filter residue 1;
3) adding 38 times of 1 mass of residue into 3, ultrasonic extracting at 36 deg.C under 310w for 43min, centrifuging at 8200rpm for 46min to obtain supernatant and precipitate 1, and recovering ethanol from the supernatant under reduced pressure under reflux to obtain extract 2;
4) adding 17% of fermentation liquor with the mass of 1 precipitate, mixing with the precipitate 1, fermenting at 32 ℃ for 3.4 days to obtain a fermentation material, adding clear water with the mass of 3.4 times of the fermentation material, and performing reflux extraction for 3.4h to obtain an extracting solution 3;
5) mixing the extractive solutions 1, 2 and 3, adding 2.3% of activated carbon decolorization, and filtering.
The solution 1 is 6% of glycerol by volume fraction, 7.7% of rock candy by mass fraction, 0.03 mol/L of potassium chloride by mass fraction, and 12% of beer by volume fraction.
The solution 2 is 0.3 mol/L sodium phosphate solution, and the volume fraction is 5.6% of glycerol.
The solution 3 is an ethanol solution with the volume fraction of 65 percent.
The fermentation liquor is prepared by mixing bacillus subtilis freeze-dried powder, acetic acid monomonas oxide freeze-dried powder, yeast freeze-dried powder, brandy, ivy mosses powder, mushroom powder and clean water according to the mass ratio of 0.5:0.27:0.43:2.0:2.2:1.0:260, and culturing at 30 ℃ and 220r/min for 2.3 hours.
The fermentation comprises spraying brown sugar water during fermentation, wherein the spraying amount is 23% of the mass of the precipitate 1, and the spraying is carried out for 3 times, and the spraying is carried out once a day.
The rose water is prepared by mixing rose petals, egg white, brown sugar and deionized water according to a mass ratio of 13:0.7:0.9:4, heating at 43 ℃ for 25min, standing at 27 ℃ for 16h to obtain a material 1, adding deionized water accounting for 70 times of the material 1 by mass, heating, refluxing and extracting for 70min, filtering the refluxed and extracted solution, and storing at 30 ℃ for later use.
The roxburgh rose essence skin-refreshing biological fiber mask comprises the following preparation steps:
1) sterilizing the biological fiber membrane material and the aluminum bag for later use;
2) and (3) folding the membrane material in a 30-thousand air cleaning area, filling the membrane material into an aluminum bag, filling the roxburgh rose extract and rose water, and sealing the opening to obtain the rose flower water-containing film.
The biological fiber membrane material is membrane cloth prepared by fermenting hypha from acetobacter xylinum, and comprises the following preparation steps:
1) preparing a basic fermentation culture medium of 30 g/L glucose, 4 g/L glycerol, 6 g/L yeast extract, 6 g/L additive, 13 g/L peptone, 1.1 g/L sodium citrate, 2.0 g/L magnesium sulfate, 2.3 g/L calcium chloride, 0.4 g/L zinc sulfate, pH6.8, and performing moist heat sterilization for 23min for later use;
2) culturing: inoculating activated acetobacter xylinum to a basic fermentation culture medium, oscillating for 1.2h under the conditions of 29 ℃ and 170r/min, statically culturing for 7 days at 30 ℃, oscillating for 25min at 27 ℃ and 70r/min, irradiating by infrared light of 640nm for 17min, and statically culturing for 2.3 days at 30 ℃ to obtain a cellulose membrane;
3) taking out the cellulose membrane in the culture medium, washing with deionized water, soaking in 1 mol/L sodium hydroxide solution for 25h, pouring off the solution, boiling in 1 mol/L sodium hydroxide solution for 17min, washing with water repeatedly, treating with 57 deg.C steam for 25min, soaking in 1% acetic acid for 12min, and washing with water repeatedly to obtain the final product;
wherein the additive is prepared by mixing tartary buckwheat, bananas and green tea according to the mass ratio of 4:1.4:0.4, crushing, adding an acetic acid solution with the mass of 13% of that of 4 times of the mixed powder, standing at 33 ℃ for 21 hours to obtain a material 1, adding clear water with the mass of 6 times of that of the material 1, decocting for 3.4 hours, filtering, and drying the filtrate.
Example 3
The roxburgh rose essence skin-refreshing biological fiber facial mask comprises a biological fiber facial mask material and natural extracted effective components, wherein the natural extracted effective components comprise, by mass, 75% of roxburgh rose extract and 25% of rose water.
The roxburgh rose extract comprises the following preparation steps:
1) cleaning fresh roxburgh rose, and draining water for later use;
2) mixing the cleaned roxburgh rose and the solution 1 according to the mass ratio of 3:0.4, oscillating for 50min at 200r/min, freezing for 2h at-15 ℃, introducing steam at 140 ℃ for 2.5min, homogenizing at 6 ℃, adding the solution 2 with the mass of 12 times of the roxburgh rose, performing ultrasonic extraction for 37min at 280w and 6 ℃, performing ultrasonic extraction for 7s during ultrasonic treatment, pausing for 10s, and filtering to obtain an extracting solution 1 and a filter residue 1;
3) adding 47 times of 1 mass of the residue into 3, ultrasonic extracting at 42 deg.C and 330w for 45min, centrifuging at 8500rpm for 50min to obtain supernatant and precipitate 1, and recovering ethanol from the supernatant under reduced pressure and reflux to obtain extractive solution 2;
4) adding 20% of fermentation liquor with the mass of 1 precipitate, mixing with the precipitate 1, fermenting at 37 ℃ for 4 days to obtain a fermentation material, adding clear water with the mass of 4 times of the fermentation material, and performing reflux extraction for 4 hours to obtain an extracting solution 3;
5) mixing the extract solutions 1, 2 and 3, adding activated carbon decolorant with the mass of 3% of the mixed solution, and filtering to obtain the product.
The solution 1 is composed of 7.3% of glycerin by volume fraction, 8.0% of rock candy by mass fraction, 0.04 mol/L of potassium chloride by mass fraction, and 13% of beer by volume fraction.
The solution 2 is 0.35 mol/L sodium phosphate solution, and the volume fraction is 6% of glycerol.
The solution 3 is ethanol solution with the volume fraction of 70 percent.
The fermentation liquor is prepared by mixing bacillus subtilis freeze-dried powder, acetic acid monomonas oxide freeze-dried powder, yeast freeze-dried powder, brandy, ivy mosses powder, mushroom powder and clean water according to the mass ratio of 0.6:0.33:0.45:2.4:2.3:1.2:300, and culturing at 35 ℃ and 230r/min for 3 hours.
The fermentation comprises spraying brown sugar water in an amount of 24% of the mass of the precipitate 1 during the fermentation, 4 times and once a day.
The rose water is prepared by mixing rose petals, egg white, yellow sugar and deionized water according to a mass ratio of 15:1:1.1:5, heating at 45 ℃ for 30min, standing at 30 ℃ for 17h to obtain a material 1, adding 100 times of deionized water of the mass of the material 1, heating and refluxing for extraction for 80min, filtering the refluxed extract, and storing at 35 ℃ for later use.
The roxburgh rose essence skin-refreshing biological fiber mask comprises the following preparation steps:
1) sterilizing the biological fiber membrane material and the aluminum bag for later use;
2) and (3) folding the membrane material in a 30-thousand air cleaning area, filling the membrane material into an aluminum bag, filling the roxburgh rose extract and rose water, and sealing the opening to obtain the rose flower water-containing film.
The biological fiber membrane material is membrane cloth prepared by fermenting hypha from acetobacter xylinum, and comprises the following preparation steps:
1) preparing a basic fermentation culture medium, namely 35 g/L of glucose, 5 g/L of glycerol, 6 g/L of yeast extract, 8 g/L of additive, 15 g/L of peptone, 1.3 g/L of sodium citrate, 2.5 g/L of magnesium sulfate, 3 g/L of calcium chloride, 0.5 g/L of zinc sulfate, pH7.0, and performing wet heat sterilization for 25min for later use;
2) culturing: inoculating activated acetobacter xylinum to a basic fermentation culture medium, oscillating for 2h under the conditions of 30 ℃ and 200r/min, statically culturing for 8 days at 30 ℃, oscillating for 30min at 28 ℃ and 80r/min, irradiating for 20min by using 650nm infrared light, and statically culturing for 3 days at 30 ℃ to obtain a cellulose membrane;
3) taking out the cellulose membrane in the culture medium, washing with deionized water, soaking in 1 mol/L sodium hydroxide solution for 26h, pouring out the solution, boiling in 1 mol/L sodium hydroxide solution for 20min, washing with water repeatedly, treating with 60 deg.C steam for 30min, soaking in 1% acetic acid for 13min, and washing with water repeatedly to obtain the final product;
wherein the additive is prepared by mixing tartary buckwheat, bananas and green tea according to the mass ratio of 5:1.5:0.6, crushing, adding an acetic acid solution which is 15% of the mass of the mixed powder and is 3-5 times of that of the mixed powder, standing at 35 ℃ for 22h to obtain a material 1, adding clear water which is 7 times of the mass of the material 1, decocting for 4h, filtering, and drying the filtrate.
Example 4
Example 4 differs from example 3 in that the Rosa roxburghii extract solution comprises the following preparation steps: 2) homogenizing cleaned roxburgh rose at 6 ℃, adding clear water with the mass being 12 times of that of the roxburgh rose, performing ultrasonic extraction at the ultrasonic power of 280w and the temperature of 6 ℃ for 37min, performing ultrasonic extraction for 7s during ultrasonic extraction, pausing for 10s, and filtering to obtain an extracting solution 1 and filter residue 1; the other processing preparation steps are the same as in example 3.
Example 5
In the Rosa roxburghii Tratt extracting solution, in the step 4), 17% of fermentation liquor with the mass of 1 precipitate is not added and is mixed with the 1 precipitate, the mixture is fermented for 3.4 days at 32 ℃ to obtain a fermentation material, clear water with the mass 3.4 times that of the fermentation material is added, and the reflux extraction is carried out for 3.4 hours to obtain an extracting solution 3; the other processing steps are the same as in example 3.
Example 6
Example 6 differs from example 3 in that the rose water was prepared by mixing rose petals and deionized water at a mass ratio of 1:15, heating and refluxing for 80min, filtering the refluxed extract, and storing at 35 ℃ for later use, with the other preparation steps being the same as example 3.
Example 7
The biofabric membrane material of example 7 and example 3, in step 1), the basic fermentation medium of 35 g/L glucose, 6 g/L yeast extract, 15 g/L peptone, 1.3 g/L sodium citrate, 2.5 g/L magnesium sulfate, pH7.0, moist heat sterilization for 25min, and other preparation steps are the same as example 3.
Example 8
Example 8 differs from example 3 in that step 2) of cultivation: inoculating activated acetobacter xylinum to a basic fermentation culture medium, and statically culturing for 10 days at 30 ℃ to obtain a cellulose membrane; the other preparation method is the same as example 3.
Example 9
Example 9 differs from example 3 in that step 3) cellulose membrane treatment, which is to take out the cellulose membrane in the culture medium, wash the cellulose membrane with deionized water, soak the cellulose membrane in 1 mol/L sodium hydroxide solution for 26h, pour the solution, boil the cellulose membrane in 1 mol/L sodium hydroxide solution for 20min, repeatedly wash the cellulose membrane with water, soak the cellulose membrane in 1% acetic acid for 13min, and repeatedly wash the cellulose membrane with water, is obtained.
Example 10
Example 10 differs from example 3 in that the Rosa roxburghii Tratt extract solution of example 10 comprises the following preparation steps:
1) cleaning fresh roxburgh rose, and draining water for later use;
2) homogenizing cleaned fructus Rosae Normalis at 6 deg.C, adding 30 times of deionized water, ultrasonic extracting at 6 deg.C for 37min at 280w ultrasonic power for 7s, suspending for 10s, filtering to obtain extractive solution 1, decolorizing with 2% of active carbon (by mass of 1) and filtering to obtain final product, wherein the other preparation steps are the same as those in example 3.
Examples of the experiments
1. Performance testing of BioCellulose films
Biological cellulose films were prepared according to the methods of examples 1 to 10, and the mask base materials were prepared as a control group with reference to the methods reported in the literature (Zhangzheng, Zhang Yunzao, Liyutao, etc.. fermentation conditions for producing bacterial cellulose by Acetobacter xylinum are optimized [ J ]. proceedings of Hebei university of Industrial science, 2013,42(2):49-54.) while referring to application No. CN201610731868.8, a method for preparing mask base materials, and the results of the test for correlation properties were as shown in Table 1.
TABLE 1 Biocellulosic film Performance test results
| Yield g/L of biological cellulose | Has water content of% | Tensile strength MPa | |
| Example 1 | 10.25 | 98.4 | 2.01 |
| Example 2 | 11.13 | 98.0 | 1.96 |
| Example 3 | 10.78 | 97.6 | 1.98 |
| Example 4 | 10.25 | 98.2 | 1.99 |
| Example 5 | 10.58 | 97.5 | 2.03 |
| Example 6 | 11.29 | 98.0 | 2.07 |
| Example 7 | 7.29 | 93.7 | 1.67 |
| Example 8 | 5.36 | 92.1 | 1.53 |
| Example 9 | 5.87 | 93.6 | 1.50 |
| Example 10 | 10.36 | 98.0 | 1.96 |
| Control group | 6.29 | 95.4 | 1.69 |
2. Activity test of Rosa roxburghii extract
Experimental tests for scavenging free radicals were carried out on the Rosa roxburghii extract extracted in examples 1-10, the test methods refer to the methods reported in the literature (Huifen, Zhuheng, Korea, etc.. Rose extract has scavenging effect on oxygen free radicals [ J ]. Henan agricultural science, 2008,37(12):102 Sunzhai 103.), and the methods reported in the literature (Hongyan, Hukai, Guogilong, etc.. Process optimization for extracting Rosa roxburghii polyphenol by ultrasonic method and in vitro antibacterial activity research [ J ]. Chinese food additive, 2016(2):57-61, Rayanping, XilinKetoconazole lotion has inhibitory effect on Pityrosporum orbiculare [ J ]. Chinese dermatological journal, 2000,33(1):67-67., Jianglili, Spirodela, Shenchong, etc.. in vitro antibacterial activity research on acne pathogenic bacteria of Chinese medicines [ J ]. pharmaceutical and clinical research, 2014,22(4): 315-.
TABLE 2 analysis of active ingredients of Rosa roxburghii Tratt extract
3. Analysis of fragrance components of rose water
The rose petal, egg white, yellow sugar and deionized water are mixed according to the mass ratio, heated, placed and distilled, so that the prepared rose water has the fragrance component with the relative content as high as 97.69 percent, the relative content of the fragrance component is 92.72 percent with the highest alcohol compound content, the phenethyl alcohol content is 39.78 percent, the rose water has the fragrance characteristics of fresh bread and fresh and sweet rose-like fragrance, the geraniol content is 10.25 percent, and the rose water has the fragrance characteristics of sweet fragrance, elecampane, citrus fragrance and lemon fragrance. In addition, when the rose water is subjected to an antioxidant activity test, the result shows that the clearance rate of oxygen anions and hydroxide ions is up to more than 96.4% when the test amount is 80 ml.
4. Evaluation of mask use Effect
1000 volunteers, half of each male and half of each female, were divided into 10 groups, each group was applied with the mask 3 times per week for 25min each time, after 4 weeks, the application effect evaluation was performed on the masks prepared in examples 1 to 10 with reference to a method reported in the literature (julieng, grandma, plum safety, ginseng anti-aging mask clinical efficacy test and analysis [ J ]. journal of cosmetic medicine china, 2016,25(2):33-36.), and the average value was obtained after measurement of each volunteer, with the results shown in table 3.
TABLE 3 evaluation of the effects of the mask application
Further, the mask of example 1 is applied to volunteers with acne on face, after 4 weeks of application, the total skin damage is faded over 90%, and the effective rate is as high as 95.6%.
Through the analysis, the active ingredients of the rosa roxburghii tratt are extracted in batches, the solution 1 is mixed with the rosa roxburghii tratt before the extraction is started, the oscillation and the freezing are carried out for 2 hours, the steam is introduced for treatment, and the solution 2 is extracted, so that the activity of the extracted SOD enzyme is kept better and the structure is complete. Through filtering, extracting the filter residue with ethanol, filtering, fermenting the filter residue with a special leaven and re-extracting, the SOD enzyme activity in the obtained roxburgh rose extract is up to 435.9g/u, oxygen free radical and OH can be effectively removed, the removal rate is respectively 96.3 percent and 95.0 percent, the skin aging is slowed down, in addition, the roxburgh rose filter residue is treated through fermentation, the obtained extract can inhibit pityrosporum orbiculare, propionibacterium acnes and staphylococcus aureus causing acne, and the inhibition rate is respectively up to 86.4 percent, 93.7 percent and 88.7 percent.
In addition, the prepared biological fiber membrane material has good biocompatibility, high water retention and good wet flexibility by culturing the acetobacter xylinum through a special culture medium and a special culture method, and the roxburgh rose extract and the rose water prepared by the method are matched, so that after the membrane material is used for 4 weeks, waste cutin on the outer layer of the skin is softened and peeled off, the growth of microorganisms in hair follicles is inhibited, redundant free radicals are eliminated, the growth and the division of cells are stimulated, and the skin percutaneous water loss value (TEW L value) is measured by a skin water loss instrument and is reduced to 15.5g/hm2The moisture content of the skin is as high as 68.2A.U., the R2 value of the skin elasticity is increased to 0.75, the skin barrier function is obviously improved, and the water locking capacity of the skin is improved; the elasticity value of the skin rises, and the fishtail lines and the wrinkles under the eyes of the volunteers are obviously reduced and lightened, which shows that the facial mask has the effects of lightening the fine lines, reducing the wrinkles and revitalizing the skin.
Claims (5)
1. The roxburgh rose essence skin-refreshing biological fiber mask is characterized by comprising a biological fiber mask material and natural extracted effective components, wherein the natural extracted effective components comprise, by mass, 55-75% of roxburgh rose extract and 25-45% of rose water;
the roxburgh rose extract comprises the following preparation steps:
1) cleaning fresh roxburgh rose, and draining water for later use;
2) mixing the cleaned roxburgh rose and a solution 1 according to a mass ratio of 3:0.3-0.4, oscillating for 40-50min under the condition of 100-;
3) adding 30-47 times of 1 mass of filter residue into 3, performing ultrasonic extraction at 30-42 deg.C and 300-; the solution 3 is an ethanol solution with the volume fraction of 55-70%;
4) adding 15-20% fermentation liquid of precipitate 1 mass, mixing with precipitate 1, fermenting at 25-37 deg.C for 3-4 days to obtain fermentation material, adding clear water of 3-4 times of fermentation material mass, and reflux extracting for 3-4 hr to obtain extractive solution 3; the fermentation liquor is prepared by mixing bacillus subtilis freeze-dried powder, acetic acid monomonas oxide freeze-dried powder, yeast freeze-dried powder, brandy, tribute vegetable powder, mushroom powder and clean water according to the mass ratio of 0.4-0.6:0.2-0.33:0.4-0.45:1-2.4:2.0-2.3:0.8-1.2:200, and culturing at 25-35 ℃ and 230r/min for 2-3 h;
5) mixing the extractive solutions 1, 2 and 3, adding activated carbon decolorization 2-3% of the mixed solution, and filtering.
2. The roxburgh rose element peel biofiber mask of claim 1, wherein the fermentation comprises spraying brown sugar water during fermentation in an amount of 20-24% by mass of the precipitate 1, 3-4 times, once a day.
3. The roxburgh rose element skin-refreshing biological fiber mask as claimed in claim 1, wherein the rose water is prepared by mixing rose petals, egg white, yellow sugar and deionized water according to a mass ratio of 10-15:0.5-1:0.7-1.1:3-5, heating at 40-45 ℃ for 20-30min, standing at 25-30 ℃ for 15-17h to obtain material 1, adding deionized water 50-100 times of the mass of material 1, heating and refluxing for extraction for 60-80min, filtering the refluxed extracted solution, and storing at 20-35 ℃ for later use.
4. The roxburgh rose element peel biofiber mask of claim 1, comprising the following preparation steps:
1) sterilizing the biological fiber membrane material and the aluminum bag for later use;
2) and (3) folding the membrane material in a 30-thousand air cleaning area, filling the membrane material into an aluminum bag, filling the roxburgh rose extract and rose water, and sealing the opening to obtain the rose water-containing film.
5. The roxburgh rose element skin-refreshing biological fiber mask as claimed in claim 1, wherein the biological fiber mask material is a film cloth prepared by fermenting hypha from acetobacter xylinum, and the preparation method comprises the following preparation steps:
1) preparing a basic fermentation culture medium, namely 28-35 g/L of glucose, 3-5 g/L of glycerol, 6 g/L of yeast extract, 4-8 g/L of additive, 10-15 g/L of peptone, 1-1.3 g/L of sodium citrate, 2-2.5 g/L of magnesium sulfate, 2-3 g/L of calcium chloride, 0.3-0.5 g/L of zinc sulfate, pH6.3-7.0, and performing wet heat sterilization for 20-25min for later use;
2) culturing: inoculating activated acetobacter xylinum to a basic fermentation culture medium, oscillating for 1-2h under the conditions of 28-30 ℃ and 150-80 r/min, statically culturing for 6-8 days at 30 ℃, oscillating for 20-30min at 25-28 ℃ and 50-80r/min, irradiating by infrared light at 650nm for 15-20min at 630-;
3) and (2) treating the biological cellulose membrane, namely taking out the cellulose membrane in the culture medium, washing the cellulose membrane with deionized water, soaking the cellulose membrane in 1 mol/L sodium hydroxide solution for 24-26h, pouring out the solution, putting the solution into 1 mol/L sodium hydroxide solution, boiling the solution for 15-20min, repeatedly washing the solution with water, treating the solution with steam at 55-60 ℃ for 20-30min, soaking the solution in 1% acetic acid for 10-13min, and repeatedly washing the solution with water to obtain the biological cellulose membrane, wherein the additive is prepared by mixing, crushing, adding acetic acid solution which is 10-15% of the mixed powder by mass according to the mass ratio of 3-5:1.2-1.5:0.3-0.6, standing the mixture at 30-35 ℃ for 20-22h to obtain material 1, adding 5-7 times of clear water by mass of material 1, decocting the mixture for 3-4h, filtering, and drying the filtrate.
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| CN109966212A (en) * | 2019-05-06 | 2019-07-05 | 六盘水职业技术学院 | A kind of preparation and its application method of edible Rosa roxburghii Tratt facial mask |
| CN111297763B (en) * | 2020-04-14 | 2022-02-22 | 张丽 | Composition with whitening and spot-fading effects and application thereof |
| CN112315874A (en) * | 2020-10-29 | 2021-02-05 | 贵州真阳纳米医药科技有限公司 | Rosa roxburghii and dendrobium nobile compound for skin care product and application thereof |
| CN114469823B (en) * | 2021-06-24 | 2024-02-23 | 重庆米洛诊所管理有限公司 | Novel moisturizing factor composition and preparation and application thereof |
| CN113499288B (en) * | 2021-07-08 | 2023-01-20 | 北京工商大学 | Fermented product of fructus Rosae Normalis for cosmetic and its preparation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102911982A (en) * | 2012-11-23 | 2013-02-06 | 海南椰国食品有限公司 | Application of bananas in biocellulose fermentation media |
| CN103110556A (en) * | 2013-03-11 | 2013-05-22 | 郭茂祥 | Bio-fiber aloe mask and preparation method thereof |
| US20140010901A1 (en) * | 2011-03-15 | 2014-01-09 | Shiseido Company, Ltd. | Bleomycin hydrolase production promotor |
-
2017
- 2017-12-05 CN CN201711266561.6A patent/CN107802543B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140010901A1 (en) * | 2011-03-15 | 2014-01-09 | Shiseido Company, Ltd. | Bleomycin hydrolase production promotor |
| CN102911982A (en) * | 2012-11-23 | 2013-02-06 | 海南椰国食品有限公司 | Application of bananas in biocellulose fermentation media |
| CN103110556A (en) * | 2013-03-11 | 2013-05-22 | 郭茂祥 | Bio-fiber aloe mask and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 产品创新 再传喜讯——首款刺梨素（酵素）今日成功生产下线;未知;《贵州四季常青药业有限公司（http://www.sjcq.com/article/20171204.html）》;20171204;第1-2页 * |
| 木醋杆菌生产细菌纤维素发酵条件优化;张朝正等;《河北工业大学学报》;20130430;第42卷(第2期);49-54 * |
| 未知.产品创新 再传喜讯——首款刺梨素（酵素）今日成功生产下线.《贵州四季常青药业有限公司（http://www.sjcq.com/article/20171204.html）》.2017,第1-2页. * |
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Address after: No.1 Changqing Road, Shangba Industrial Park, Daozhen Autonomous County, Zunyi City, Guizhou Province Applicant after: GUIZHOU EVERGREEN PHARMACEUTICAL Co.,Ltd. Address before: 563500 Guizhou city in Zunyi Province, Daozhen yilao and Miao Autonomous County Xintian Village Center BA Xiang Group Applicant before: GUIZHOU EVERGREEN PHARMACEUTICAL Co.,Ltd. |
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