Cosmetic rose mud mask, rose flower mud and application
Rose petal mud, prepared by fermenting rose petal residue with a compound microbial strain, combined with moisturizers and thickeners, solves the problems of skin oil-water balance and sebum balance, achieving significant skin conditioning effects, including anti-wrinkle and improved skin elasticity.
Patent Information
- Application Number
- CN202511420141.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-30
- Publication Date
- 2025-12-23
- Estimated Expiration
- 2045-09-30
AI Technical Summary
In existing technologies, the integrity of the skin barrier depends on the dynamic regulation of keratinocytes rather than the periodic changes of sebaceous glands, resulting in plump and hydrated skin in infants and dry and loose skin in the elderly. Furthermore, the occurrence of acne is closely related to the function of sebaceous glands, and existing products are unable to effectively regulate the skin's oil-water balance and sebum balance.
Rose petal mud is prepared by fermenting rose petal residue and compound microbial strains (lactobacillus and yeast). Combined with moisturizers, thickeners and other auxiliary materials, a rose mud film is prepared. The fermentation and grinding process increases the water-soluble total flavonoid and polysaccharide content of the rose petal mud, thereby regulating the skin's oil-water balance and oil balance.
It significantly inhibits sebum secretion from sebaceous gland cells, improves oil-water balance and sebum balance, and has anti-wrinkle and skin elasticity-enhancing effects. The water-soluble total flavonoid content in rose mud is not less than 14.8 mg/mL, and the water-soluble total polysaccharide content is not less than 2.5 mg/mL.
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Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of microbial fermentation, and particularly relates to a rose mud mask for cosmetics, rose flower mud and application. BACKGROUND
[0002] In the classic 'brick wall model' of skin barrier, keratinocytes (bricks) and intercellular lipids (mortar) together constitute a physical barrier. Among them, the intercellular lipids are composed of hydrophilic polar lipids (such as ceramide, cholesterol) actively secreted by keratinocytes, and its core function is to maintain the hydration state of the epidermis and limit the loss of transdermal water. Unlike this, the hydrophobic neutral lipids (triglycerides, squalene, etc.) secreted by sebaceous glands are distributed on the skin surface to form a sebum film, which mainly participates in the lubrication and weakly acidic environment maintenance of the skin surface.
[0003] The function of sebaceous glands presents a 'bell-shaped curve' change: it is not mature in infancy, reaches the peak of secretion in adolescence, and gradually atrophies in old age. However, the skin barrier state presents significant differences at both ends of life - the baby's skin is moist and full, while the old skin is dry and loose. The contradiction is due to the difference in the activity of keratinocytes: in infancy, cell metabolism is vigorous, and polar lipids are synthesized in abundance, which can effectively lock water; in old age, cell proliferation slows down, and the secretion of polar lipids is insufficient, leading to the decline of barrier function. As can be seen, the integrity of the skin barrier depends more on the dynamic regulation of keratinocytes than on the periodic changes of sebaceous glands.
[0004] In addition, the occurrence of acne is closely related to the function of sebaceous glands: the over-secretion of non-polar lipids (such as wax esters, squalene) by sebaceous glands in adolescence leads to abnormal keratinization of hair follicles and proliferation of propionibacterium acnes. Although keratinocytes continuously synthesize polar lipids, the contribution of surface lipid detection data shows that it is less than 5% of the total lipids. This phenomenon suggests that the core cause of acne is focused on the imbalance of sebaceous gland-derived lipids, and the role of keratinocytes in barrier homeostasis tends to be more basic protection.
[0005] In summary, improving the secretion of polar lipids by keratinocytes and inhibiting the over-secretion of neutral lipids by sebaceous cells is of great significance to promote the oil balance and grease balance of the skin. SUMMARY
[0006] In view of the deficiencies in the prior art, the application provides a rose mud mask for cosmetics, rose flower mud and application.
[0007] In order to achieve the purpose of the application, the technical scheme adopted is as follows:
[0008] The cosmetic rose mud mask, raw materials of which include rose mud and auxiliary materials; the preparation raw materials of the rose mud include rose residue and compound bacteria, the compound bacteria include lactic acid bacteria and yeast bacteria with a mass ratio of 50-100:0.1-1, the yeast bacteria is bayaun yeast, and the lactic acid bacteria is lactobacillus plantarum; the auxiliary materials include moisturizing agent, thickening agent;
[0009] The mass ratio of the rose residue and the compound bacteria is 100:0.5-1;
[0010] The preparation method of the rose mud includes the following steps:
[0011] (1) inoculate the rose residue with the compound bacteria and ferment;
[0012] (2) sterilize and grind pulp;
[0013] (3) remove water with a filter membrane to obtain the rose mud;
[0014] In step (1), the fermentation is first carried out at 30-35 ℃ for 24-48 h, then the temperature is adjusted to 25-28 ℃, and the fermentation is continued for 48-72 h.
[0015] Preferably, examples of the moisturizing agent include, but are not limited to, one or more of glycerin, diglycerin, butylene glycol, propylene glycol, 1,3-propanediol, dipropylene glycol, 1,2-pentanediol, polyethylene glycol-8, polyethylene glycol-32, methyl gluceth-10, methyl gluceth-20, PEG / PPG-17 / 6 copolymer, glycereth-7, glycereth-26, glycerol glucoside, PPG-10 methyl glucose ether, PPG-20 methyl glucose ether, PEG / PPG / polybutylene glycol-8 / 5 / 3 glycerin, sucrose, trehalose, rhamnose, mannose, raffinose, betaine, erythritol, xylitol, urea, glycereth-5 lactate, sodium hyaluronate, hydrolyzed sodium hyaluronate, acetylated sodium hyaluronate, sodium polyglutamate, hydrolyzed sclerotium gum, pullulanase polysaccharide, tremella polysaccharide, and acid bean seed polysaccharide. The content of the moisturizing agent in the skin external use composition is known in the art.
[0016] Preferably, examples of the thickening agent include, but are not limited to, one or more of carbomer, acrylic acid (ester) and its derivatives, xanthan gum, gum arabic, polyethylene glycol-14M, polyethylene glycol-90M, succinyl polysaccharide, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, and other high molecular polymers. The content of the thickening agent in the skin external use composition is known in the art.
[0017] Preferably, the moisturizing agent is one or more of glycerin, 1,2-hexanediol, and arginine.
[0018] Preferably, the thickening agent is one or more of SEPIMAX ZEN, SEPINOV EMT10, SEPINOV WEO, Avicel PH-105, and xanthan gum.
[0019] Preferably, the adjuvant further comprises an emulsifier, an emulsion stabilizer, an antioxidant, an adsorbent, and an emollient, the emulsifier being Amphisol K.
[0020] Preferably, the emulsion stabilizer is cetyl alcohol or stearyl alcohol.
[0021] Preferably, the antioxidant is p-hydroxyacetophenone.
[0022] Preferably, the adsorbent is ImerCare 04K kaolin.
[0023] Preferably, the emollient is one or more of lanol 99, BYE SPTO, squalane, Myritol 318 RC, and DM10.
[0024] Preferably, the step (2) is a colloidal mill grinding to below 50 μm.
[0025] Preferably, the step (3) is a 100-300 dalton filter membrane water removal to a solid content of 20%, to obtain the rose mud.
[0026] Preferably, the rose residue in the step (1) is a rose residue byproduct after extraction of volatile oil by water vapor distillation technology, the rose being selected from Damask rose, Pingyin heavy petal rose, or Kusarose.
[0027] A second object of the present application is to provide a rose mud, which is the rose mud in the rose mud mask for cosmetics.
[0028] A third object of the present application is to provide a rose mud or the rose mud prepared by the preparation method for use in preparing a product having the effects of promoting skin oil balance, and / or sebum balance, and / or anti-wrinkle, and / or improving skin elasticity.
[0029] Compared with the prior art, the present application has the following advantages:
[0030] (1) The rose mud prepared by fermentation of rose residue by the complex bacterial strain of the present application has the effects of significantly synergistically inhibiting sebum secretion of sebaceous gland cells, improving oil balance, sebum balance, and anti-wrinkle, and improving skin elasticity.
[0031] (2) The rose mud prepared by the present application has a water-soluble total flavone content of not less than 14.8 mg / mL, a water-soluble total polysaccharide content of not less than 2.5 mg / mL, and a water-soluble solid content of about 4%.
[0032] (3) The mud film prepared from the rose mud of the application has the effect of regulating skin oil balance and sebum balance. DETAILED DESCRIPTION
[0033] The application will be further described in conjunction with specific embodiments. The following raw materials are all commercially available conventional raw materials; among them, the plant lactobacillus is Lactobacillus plantarum BNCC194165, the bayanus yeast is Saccharomyces bayanus BNCC374151, and the suppliers are both Henan Industrial Microbial Strain Engineering Technology Research Center of Beina Biological. Saccharomyces cerevisiae is purchased from China Industrial Microbial Strain Preservation Center, with the number CICC1002. Lactobacillus fermentum is purchased from Henan Industrial Microbial Strain Engineering Technology Research Center of Beina Biological, with the number BNCC194390.
[0034] Example 1
[0035] This example provides a rose mud film, the formula (see Table 1) and the preparation method are as follows:
[0036] Table 1
[0037]
[0038] The rose mud of phase B is prepared as follows:
[0039] (1) Take 2 kg of fresh distilled Pingyin heavy petal rose residue, inoculate plant lactobacillus and bayanus yeast (combined bacteria) with a mass ratio of 100:1, ferment at 30℃ for 36h, then adjust the temperature to 25℃ and continue to ferment for 60h; the mass ratio of rose residue to combined bacteria is 100:0.7; wherein the rose residue is the residue by-product (belonging to the waste resource utilization after extracting rose essential oil) after extracting rose essential oil from fresh rose for 3h by water vapor distillation technology;
[0040] (2) After high-temperature sterilization, grind to below 50μm by colloid mill;
[0041] (3) Remove water by using 200 dalton filter membrane, to a solid content of 20%, to obtain rose mud.
[0042] Example 2
[0043] This example provides a rose mud film, which is different from example 1 in that the preparation method of the rose mud of phase B is different, and the specific preparation method is as follows:
[0044] (1) Take fresh distilled Damascus rose residue 2 kg, inoculate the mass ratio of 50:1 of Lactobacillus plantarum and Bayanus yeast (combined bacteria), 35℃ fermentation for 24h, then adjust the temperature to 25℃, continue to ferment for 72h; the mass ratio of rose residue to combined bacteria is 100:0.5; wherein the rose residue is the remaining residue byproduct after extracting rose essential oil for 5h by water vapor distillation technology from fresh rose;
[0045] (2) After high temperature sterilization, grind to 50μm by colloid mill;
[0046] (3) Remove water by 100 Dalton filter membrane, to solid content of 20%, get rose mud.
[0047] Example 3
[0048] This example provides a rose mud mask, which is different from example 1 in that the preparation method of B phase rose mud is different, and the specific preparation method is as follows:
[0049] (1) Take fresh distilled bitter water rose residue 2 kg, inoculate the mass ratio of 100:0.1 of Lactobacillus plantarum and Bayanus yeast (combined bacteria), 30℃ fermentation for 48h, then adjust the temperature to 28℃, continue to ferment for 48h; the mass ratio of rose residue to combined bacteria is 100:0.9; wherein the rose residue is the remaining residue byproduct after extracting rose essential oil and rose hydrolate for 2h by water vapor distillation technology from fresh rose;
[0050] (2) After high temperature sterilization, grind to 50μm by colloid mill;
[0051] (3) Remove water by 300 Dalton filter membrane, to solid content of 20%, get rose mud.
[0052] Example 4
[0053] This example provides a rose mud mask, which is different from example 1 in that the formula is different, and the specific formula is as follows table 2:
[0054] Table 2
[0055]
[0056] The preparation method of B phase rose mud is the same as described in example 1.
[0057] Example 5
[0058] This example provides a rose mud mask, which is different from example 1 in that the formula is different, and the specific preparation method is as follows table 3:
[0059] Table 3
[0060]
[0061] The preparation method of the B-phase rose mud is the same as described in Example 1.
[0062] Example 6
[0063] This example provides a rose mud film, which is different from Example 1 in that the formula and the preparation method are different, and the specific preparation is shown in Table 4 below.
[0064] Table 4
[0065]
[0066] The preparation method of the D-phase rose mud is the same as described in Example 1.
[0067] Comparative Example 1
[0068] This comparative example provides a rose mud film, which is different from Example 1 in that the preparation method of the B-phase rose mud is different, and the specific preparation is as follows:
[0069] (1) Take 2 kg of fresh distilled Pingyin heavy petal rose residue;
[0070] (2) After high-temperature sterilization, grind the pulp to below 50 μm by a colloid mill;
[0071] (3) Remove water by using a 200 Dalton filter membrane, and the solid content is 20%, to obtain the rose mud.
[0072] Comparative Example 2
[0073] This comparative example provides a rose mud film, which is different from Example 1 in that the preparation method of the B-phase rose mud is different, and the specific preparation is as follows:
[0074] (1) Take 2 kg of fresh distilled Pingyin heavy petal rose residue, inoculate with Bayanus yeast, and after 36 h of fermentation at 30℃, adjust the temperature to 25℃ and continue to ferment for 60 h; the mass ratio of rose residue to Bayanus yeast is 100:0.7;
[0075] (2) After high-temperature sterilization, grind the pulp to below 50 μm by a colloid mill;
[0076] (3) Remove water by using a 200 Dalton filter membrane, and the solid content is 20%, to obtain the rose mud.
[0077] Comparative Example 3
[0078] This comparative example provides a rose mud film, which is different from Example 1 in that the preparation method of the B-phase rose mud is different, and the specific preparation is as follows:
[0079] (1) Take fresh distilled Pingyin double rose flower residue 2 kg, inoculate Lactobacillus plantarum, ferment at 30°C for 36 h, then adjust the temperature to 25°C, continue to ferment for 60 h; the mass ratio of rose flower residue to Lactobacillus plantarum is 100:0.7;
[0080] (2) After high-temperature sterilization, grind to 50 μm or less by colloid mill;
[0081] (3) Remove water by using 200 Dalton filter membrane, until the solid content is 20%, to obtain rose flower mud.
[0082] Comparative Example 4
[0083] This comparative example provides a rose mud mask, which is different from Example 1 in that the preparation method of the B-phase rose flower mud is different, and the specific preparation is as follows:
[0084] (1) Take fresh distilled Pingyin double rose flower residue 2 kg, inoculate the combined bacteria of Lactobacillus fermentum and Saccharomyces cerevisiae with a mass ratio of 100:1, ferment at 30°C for 72 h, then adjust the temperature to 25°C, continue to ferment for 24 h; the mass ratio of rose flower residue to combined bacteria is 100:0.7;
[0085] (2) After high-temperature sterilization, grind to 50 μm or less by colloid mill;
[0086] (3) Remove water by using 200 Dalton filter membrane, until the solid content is 20%, to obtain rose flower mud.
[0087] Comparative Example 5
[0088] This comparative example provides a rose mud mask, which is different from Example 1 in that the preparation method of the B-phase rose flower mud is different, and the specific preparation is as follows:
[0089] (1) Take fresh distilled Pingyin double rose flower residue 2 kg, inoculate the combined bacteria of Lactobacillus fermentum and Saccharomyces cerevisiae with a mass ratio of 100:1, ferment at 30°C for 36 h, then adjust the temperature to 25°C, continue to ferment for 60 h; the mass ratio of rose flower residue to combined bacteria is 100:0.7;
[0090] (2) After high-temperature sterilization, grind to 50 μm or less by colloid mill;
[0091] (3) Remove water by using 200 Dalton filter membrane, until the solid content is 20%, to obtain rose flower mud.
[0092] Comparative Example 6
[0093] This comparative example provides a rose mud mask, which is different from Example 1 in that the preparation method of the B-phase rose flower mud is different, and the specific preparation is as follows:
[0094] (1) Take fresh distilled Pingyin heavy petal rose dregs 2 kg, inoculate the combination of Lactobacillus plantarum and Bayanus yeast with a mass ratio of 100:1, ferment at 30°C for 36 h, then adjust the temperature to 25°C and continue to ferment for 60 h; the mass ratio of rose dregs to combination bacteria is 100:0.3;
[0095] (2) After high-temperature sterilization, grind the pulp to below 50 μm with a colloid mill;
[0096] (3) Remove water with a 200 dalton filter membrane to a solid content of 20% to obtain rose mud.
[0097] Effect Example 1: Efficacy Test of Rose Mud Film
[0098] 1. Experimental equipment
[0099] Multifunctional skin tester MPA580 (CK).
[0100] 2. Experimental method
[0101] Recruit 40 subjects for self-control experiment. After the subjects are enrolled, use a random number table to divide them into 4 groups. Group A uses rose mud film prepared from combination bacteria fermented flower mud (Example 1), group B uses rose mud film prepared from unfermented flower mud (Comparative Example 1), group C uses rose mud film prepared from Bayanus yeast fermented flower mud (Comparative Example 2), and group D uses rose mud film prepared from Lactobacillus plantarum fermented flower mud (Comparative Example 3). The subjects are required not to use other efficacy facial products during the test period, and are required to return for a visit. The test indicators are skin stratum corneum water content and skin surface oil content.
[0102] 2.1 Subject requirements
[0103] According to the Helsinki Declaration, the selection of subjects follows the medical and ethical standards of human testing. All subjects must voluntarily participate in the test and sign an informed consent form before the test. Before signing the informed consent form, the test personnel need to inform the subjects of the purpose of the test, the possible benefits, potential risks and problems, and the relevant rights and obligations.
[0104] 2.2 Inclusion criteria
[0105] 1) Healthy women or men aged 18-45 years old;
[0106] 2) Informed consent, understanding of the test process, voluntary participation in the test, and signing of the informed consent form;
[0107] 3) Ability to return for a visit as required.
[0108] 2.3 Exclusion criteria:
[0109] 1) Pregnant or lactating women, and those who have a recent plan to get pregnant;
[0110] 2) Allergic or highly sensitive constitution;
[0111] 3) History of allergy to cosmetics or other external preparations;
[0112] 4) Allergic dermatosis, history of skin disease or illness, such as eczema, psoriasis, atopic dermatitis, severe acne, tinea, pityriasis, severe seborrheic dermatitis, bacterial or viral infection, etc;
[0113] 5) Those who are receiving dermatological treatment;
[0114] 6) Those who have received cosmetic surgery, laser and other cosmetic methods in the test area within the past six months, which may affect the test results;
[0115] 7) Those who have skin features in the test area that may affect the test results, such as birthmarks, scratches, white spots, pigments, moles, atrophy, scars or other blemishes;
[0116] 8) Those who have used antihistamines within the past week or hormones and immunosuppressants within the past month;
[0117] 9) Those who have used any anti-inflammatory drugs in the test area within the past two months;
[0118] 10) Those who have severe systemic diseases, immune deficiencies or autoimmune diseases;
[0119] 11) Insulin-dependent diabetes patients;
[0120] 12) Patients with asthma or other respiratory diseases who are receiving treatment;
[0121] 13) Those who have undergone bilateral mastectomy and bilateral axillary lymph node dissection;
[0122] 14) Those who have received anticancer chemotherapy within the past six months;
[0123] 15) Those who are not suitable for participating in the trial according to other clinical assessments;
[0124] 16) Those who are not willing to participate or cannot complete the required content according to the trial requirements.
[0125] 2.4 Exit (Dropout) Criteria
[0126] 1) The subject is lost or actively withdraws from the trial;
[0127] 2) The subject has poor compliance and cannot be followed up as required;
[0128] 3) The subject uses other products similar to the test sample during the study;
[0129] 4) The subject develops a new illness during the entire study period that directly impacts the assessment of the clinical status, including skin diseases;
[0130] 5) The subject develops a serious illness during the entire study period;
[0131] 6) The subject becomes pregnant during the study period;
[0132] 7) The subject develops a serious adverse reaction during the entire study period.
[0133] 3. Results of the experiment
[0134] 3.1 Number of subjects
[0135] A total of 40 subjects were enrolled, including 27 females and 13 males, with an average age of 32 ± 7 years.
[0136] 3.2 Skin surface oil content
[0137] The SM815 probe equipped with the multifunctional skin tester MPA580 of the German CK company was used to detect the oil content on the surface of the skin. The probe is built-in with a special extinction adhesive tape with a size of 8 mm in width and 0.1 mm in thickness. When the tape comes into contact with the oil on the skin, it will gradually become translucent and the light transmittance will increase. The degree of light transmittance is positively correlated with the oil content: the higher the oil content, the stronger the light transmittance. The test results range from 0 to 350 μg / cm², and the higher the value, the more active the oil secretion on the surface of the skin. The specific results are shown in Table 5.
[0138] Table 5 Test results of the oil content on the surface of the skin before and after using the sample
[0139]
[0140] Note: *p <0.05 vs before use.
[0141] Result description: Before the subjects use the product, there is no significant difference in the oil content on the surface of the skin between Example 1 and Comparative Examples 1-3; after the subjects use the product, the oil content on the surface of the skin significantly decreases after 4 weeks of using Example 1, and there is no significant change in the oil content on the surface of the skin after 4 weeks of using Comparative Examples 1-3.
[0142] 3.3 Skin stratum corneum water content
[0143] The multifunctional skin tester MPA580 produced by the German company CK is equipped with a Corneometer CM825 probe, which detects the moisture content of the skin surface layer using the capacitance method. The principle is that the dielectric constant of water in the skin surface layer is much greater than that of other components, so the change in the dielectric constant of the skin surface layer is mainly determined by the moisture content. By measuring the dielectric constant of the skin surface layer, the skin moisture level can be calculated. The measurement result is presented as a relative numerical value, with the unit of C.U. (Corneometer Units) being specifically used to measure the skin moisture content. The higher the value, the more adequate the moisture of the skin surface layer, and the specific results are shown in Table 6.
[0144] Table 6 Skin stratum corneum water content test results before and after using the sample
[0145]
[0146] Note: *p <0.05 vs before use, **p <0.01 vs before use.
[0147] Results description: there is no significant difference in the skin stratum corneum water content of Example 1 and Comparative Examples 1-3 before the subjects use the product; after the subjects use the product, the skin stratum corneum water content of Example 1 and Comparative Example 2 significantly increases after 4 weeks, and the effect of Example 1 is better than that of Comparative Example 2, and there is no significant difference in the change of the skin stratum corneum water content of Comparative Examples 1 and 3 after 4 weeks.
[0148] 3.4 Wrinkle length
[0149] The facial imaging system produced by the American company Canfield takes high-definition facial images from different angles through standard white light, ultraviolet light, polarized light and other light sources, and then the 3D skin analysis system produced by the Irish company Miravex analyzes and measures the wrinkle length. The wrinkle length is an evaluation index of the anti-wrinkle effect of cosmetics, and the higher the value of this index, the more serious the skin wrinkles. If the wrinkle length after using the sample is significantly reduced compared with that before using the sample, it can be explained that the sample has anti-wrinkle effect, and the specific results are shown in Table 7.
[0150] Table 7 Wrinkle length (mm) test results before and after using the sample
[0151]
[0152] Note: *p <0.05 vs before use, **p <0.01 vs before use.
[0153] Results description: Before using the product, there was no significant difference in wrinkle length between Example 1 and Comparative Examples 1-3. After using the product, the wrinkle length was significantly reduced after 4 weeks using Example 1 and Comparative Examples 1-3, and the effect of Example 1 was significantly better than that of Comparative Examples 1-3.
[0154] 3.5 Skin elasticity R2
[0155] The skin elasticity tester produced by CK in Germany is based on the suction and stretching principle in physics, and measures the mechanical response of the skin to this through a precision sensor. The skin elasticity R2 is the ratio of the maximum rebound length to the maximum stretching length. The skin elasticity R2 is an evaluation index of the firming efficacy of cosmetics. The higher the value of this index, the better the skin elasticity. If the skin elasticity R2 after using the sample is significantly higher than that before using the sample, it indicates that the product has firming efficacy. The specific results are shown in Table 8.
[0156] Table 8 Test results of skin elasticity R2 before and after using the sample
[0157]
[0158] Note: *p<0.05 vs before use, **p<0.01 vs before use.
[0159] Results description: Before using the product, there was no significant difference in skin elasticity R2 between Example 1 and Comparative Examples 1-3. After using the product, the skin elasticity R2 was significantly increased after 4 weeks using Example 1 and Comparative Examples 1-3, and the effect of Example 1 was significantly better than that of Comparative Examples 1-3.
[0160] Effect Example 2: Efficacy test of rose mud mask
[0161] 1. Experimental equipment
[0162] Multifunctional skin tester MPA580 (CK).
[0163] 2. Experimental method
[0164] At least 60 subjects were recruited for the self-control experiment. After the subjects were enrolled, they were divided into 6 groups using a random number table. Groups A, B, and C used rose mud masks prepared from mixed bacteria fermented flower mud (Examples 1-3), group D used rose mud masks prepared from flower mud fermented for different times (Comparative Example 4), group E used rose mud masks prepared from flower mud fermented with different bacteria (Comparative Example 5), and group F used rose mud masks prepared from different mass ratios of rose residue and combined bacteria (Comparative Example 6). The subjects were required not to use other efficacious facial products during the test period, and were required to return for follow-up visits. The test indicators were the water content of the stratum corneum and the oil content on the skin surface.
[0165] Subject requirements, inclusion criteria, etc. Example 1.
[0166] 3. Experimental results
[0167] 3.1 Number of subjects
[0168] A total of 60 subjects were enrolled, including 45 females and 15 males, with an average age of 30 ± 6 years.
[0169] 3.2 Skin surface oil content
[0170] The SM815 probe of the multifunctional skin tester MPA580 from CK, Germany, was used to detect the oil content on the skin surface. The probe is equipped with a special extinction tape with a width of 8 mm and a thickness of 0.1 mm. When the tape comes into contact with the oil on the skin, it gradually becomes translucent and the light transmission increases. The degree of light transmission is positively correlated with the oil content: the higher the oil content, the stronger the light transmission. The test results range from 0 to 350 pg / cm2, and the higher the value, the more oil is secreted on the skin surface. The results are shown in Table 9.
[0171] Table 9 Test results of skin surface oil content before and after using the sample
[0172]
[0173] Note: *p <0.05 vs before use.
[0174] Results description: Before use, there was no significant difference in the skin surface oil content of Examples 1-3 and Comparative Examples 4-6. After use, the skin surface oil content of Examples 1-3 was significantly reduced after 4 weeks, while the skin surface oil content of Comparative Examples 4-6 showed no significant change after 4 weeks.
[0175] 3.3 Skin stratum corneum water content
[0176] The Corneometer CM825 probe of the multifunctional skin tester MPA580 from CK, Germany, was used to detect the water content on the skin surface. The principle is that the dielectric constant of water in the skin surface layer is much higher than that of other components, so the change in the dielectric constant of the skin surface layer is mainly determined by the water content. By measuring the dielectric constant of the skin surface layer, the water level of the skin can be calculated. The measurement results are presented as relative values, with units of C.U. (Corneometer Units), which are specifically used to measure the water content of the skin. The higher the value, the more water the skin surface layer contains. The results are shown in Table 10.
[0177] Table 10 Test results of skin stratum corneum water content before and after using the sample
[0178]
[0179] Note: *p<0.05 vs before use, **p<0.01 vs before use.
[0180] Result description: There was no significant difference in the skin horny layer water content of Examples 1-3 and Comparative Examples 4-6 before the subjects used the products; after the subjects used the products, the skin horny layer water content of Examples 1-3 and Comparative Example 4 significantly increased after 4 weeks, and the effect of Examples 1-3 was significantly better than that of Comparative Example 4, and there was no significant difference in the change in the skin horny layer water content of Comparative Examples 5-6 after 4 weeks.
[0181] 3.4 Wrinkle length
[0182] The facial imaging system produced by the American Canfield company takes high-definition facial images from different angles through standard white light, ultraviolet light, polarized light and other light sources, and then the 3D skin analysis system produced by the Irish Miravex company analyzes and measures the wrinkle length. The wrinkle length is an evaluation index of the anti-wrinkle effect of cosmetics. The higher the value of this index, the more serious the skin wrinkles. If the wrinkle length after using the sample is significantly reduced compared with before using the sample, it can be explained that the sample has an anti-wrinkle effect. The specific results are shown in Table 11.
[0183] Table 11 Test results of wrinkle length (mm) before and after using the sample
[0184]
[0185] Note: *p<0.05 vs before use, **p<0.01 vs before use.
[0186] Result description: There was no significant difference in the wrinkle length of Examples 1-3 and Comparative Examples 4-6 before the subjects used the products; after the subjects used the products, the wrinkle length of Examples 1-3 and Comparative Examples 4-6 significantly decreased after 4 weeks, and the effect of Examples 1-3 was significantly better than that of Comparative Examples 4-6.
[0187] 3.5 Skin elasticity R2
[0188] The skin elasticity tester produced by the German CK is based on the suction and stretching principle in physics, which measures the mechanical response of the skin to this through a precision sensor. The skin elasticity R2 is the ratio of the maximum rebound length to the maximum stretching length. The skin elasticity R2 is an evaluation index of the firming effect of cosmetics. The higher the value of this index, the better the skin elasticity. If the skin elasticity R2 after using the sample is significantly increased compared with before using the sample, it can be explained that the product has a firming effect. The specific results are shown in Table 12.
[0189] Table 12 Test results of skin elasticity R2 before and after using the sample
[0190]
[0191] Note: *p<0.05 vs before use, **p<0.01 vs before use.
[0192] Results description: Before using the product, there was no significant difference in skin elasticity R2 among Example 1-3 and Comparative Example 4-6; after using the product, the skin elasticity R2 of Example 1-3 and Comparative Example 4-6 increased significantly after 4 weeks, and the effect of Example 1-3 was significantly better than that of Comparative Example 4-6.
[0193] Effect Example 3: Improvement of mud mask on skin condition
[0194] 1. Experimental equipment
[0195] Multifunctional skin tester MPA580 (CK), facial imaging system (Canfield), 3D skin analysis system (Miravex), skin elasticity tester (CK).
[0196] 2. Experimental method
[0197] At least 120 volunteers were recruited for self-control, and were divided into 4 groups using a random number table, group A used Example 1, group B used Example 4, group C used Example 5, and group D used Example 6. After cleaning the face, the subjects took an appropriate amount of mud mask and evenly applied it to the test area, and then washed it off after 15 minutes of standing. The subjects were required to adapt to the conditions of maintaining temperature at 20-22°C and relative humidity at 40%-60% for 30 minutes, and then the skin surface oil content, skin stratum corneum water content, wrinkle length and skin elasticity R2 were detected respectively. The subjects were required not to use other efficacious facial products during the test period, and were required to return for follow-up, and the test indicators were skin surface oil content, skin stratum corneum water content, wrinkle length and skin elasticity R2.
[0198] The requirements and inclusion criteria of the subjects were the same as those of Effect Example 1.
[0199] 3. Experimental results
[0200] 3.1 Number of subjects
[0201] A total of 120 subjects were enrolled, including 100 females and 20 males, with an average age of 35±9 years.
[0202] 3.2 Skin surface oil content
[0203] The MPA580 multifunctional skin analyzer from the German company CK is equipped with the SM815 probe, which is used to detect the oil content of the skin surface. This probe incorporates a special matte adhesive tape, 8 mm wide and 0.1 mm thick. When the tape comes into contact with the oil on the skin, it gradually becomes translucent, and its light transmittance increases. The degree of light transmittance is positively correlated with the oil content: the higher the oil content, the stronger the light transmittance. The test results range from 0-350 μg / cm², with higher values indicating more vigorous oil secretion on the skin surface. Specific results are shown in Table 13.
[0204] Table 13 Results of skin surface oil content test before and after sample use
[0205]
[0206] Note: *p<0.05 vs before use, **p<0.01 vs before use.
[0207] Results description: Before the subjects used the product, there was no significant difference in the skin surface oil content between Examples 1 and 4-6; after the subjects used the product, the skin surface oil content of Examples 1 and 4-5 was significantly reduced after the 4th week, and there was no significant difference between Examples 1 and 4-5.
[0208] 3.3 Skin stratum corneum water content
[0209] The MPA580 multifunctional skin analyzer manufactured by CK GmbH in Germany is equipped with a Corneometer CM825 probe, which uses capacitance to detect the moisture content of the skin's surface. The principle is that the dielectric constant of water in the skin's surface is much higher than that of other components, so the change in the dielectric constant of the skin's surface is mainly determined by its moisture content. By measuring the dielectric constant of the skin's surface, the skin's moisture level can be calculated. The measurement results are presented as relative values in CU (Corneometer Units), specifically used to measure skin moisture content. The higher the value, the more hydrated the skin's surface. See Table 14 for specific results.
[0210] Table 14 Results of skin stratum corneum water content test before and after sample use
[0211]
[0212] Note: *p<0.05 vs before use, **p<0.01 vs before use.
[0213] Results description: Before the subjects used the product, there was no significant difference in the stratum corneum water content of the skin in Examples 1 and 4-6; after the subjects used the product, the stratum corneum water content of the skin in Examples 1 and 4-5 was significantly increased after the 4th week, and there was no significant difference between Examples 1 and 4-5.
[0214] 3.4 Wrinkle length
[0215] The facial imaging system produced by the American company Canfield takes high-definition facial images from different angles through standard white light, ultraviolet light, polarized light, etc. The 3D skin analysis system produced by the Irish company Miravex analyzes and measures the wrinkle length. The wrinkle length is an evaluation index of the anti-wrinkle effect of cosmetics. The higher the value of this index, the more serious the skin wrinkles. If the wrinkle length after using the sample is significantly reduced compared with before using the sample, it means that the sample has anti-wrinkle effect. The specific results are shown in Table 15.
[0216] Table 15 Test results of wrinkle length (mm) before and after using the sample
[0217]
[0218] Note: *p <0.05 vs before use, **p <0.01 vs before use.
[0219] Result description: Before using the product, there was no significant difference in the wrinkle length of Examples 1, 4-6. After using the product, the wrinkle length of Examples 1, 4-5 was significantly reduced after 4 weeks, and there was no obvious difference between Examples 1, 4-5.
[0220] 3.5 Skin elasticity R2
[0221] The skin elasticity tester produced by the German company CK is based on the suction and stretching principle in physics. The mechanical response of the skin to this is measured by a precision sensor. The skin elasticity R2 is the ratio of the maximum rebound length to the maximum stretching length. The skin elasticity R2 is an evaluation index of the firming effect of cosmetics. The higher the value of this index, the better the skin elasticity. If the skin elasticity R2 after using the sample is significantly increased compared with before using the sample, it means that the product has firming effect. The specific results are shown in Table 16.
[0222] Table 16 Test results of skin elasticity R2 before and after using the sample
[0223]
[0224] Note: *p <0.05 vs before use, **p <0.01 vs before use.
[0225] Result description: Before using the product, there was no significant difference in the skin elasticity R2 of Examples 1, 4-6. After using the product, the skin elasticity R2 of Examples 1, 4-5 was significantly increased after 4 weeks, and there was no obvious difference between Examples 1, 4-5.
[0226] Effect Example 4: Property detection of rose mud
[0227] 1 Experimental method
[0228] The water-soluble total flavonoids, total polysaccharides and total solids content of the rose mud described in Examples 1-3 and Comparative Examples 1-6 were detected.
[0229] Experimental materials
[0230] UV spectrophotometer (TU-1900), Nessler colorimetric tube, quartz colorimetric dish, electronic balance, rutin, sodium nitrite, aluminum nitrate, sodium hydroxide, anhydrous glucose, phenol, concentrated sulfuric acid, electronic balance, oven, flat weighing bottle, dryer, filter paper, funnel, vacuum filtration apparatus, constant temperature water bath. The reagent preparation method is shown in Tables 17 and 18.
[0231] Table 17 Reagent preparation method for testing water-soluble total flavonoids content
[0232]
[0233] Table 18 Reagent preparation method for testing water-soluble total polysaccharides content
[0234]
[0235] 1.1 Water-soluble total flavonoids content test
[0236] Take 6 25mL colorimetric tubes numbered 0#-5#, respectively, and accurately transfer 0mL, 1.0mL, 2.0mL, 3.0mL, 4.0mL and 5.0mL of rutin standard solution into 0#-5# groups in turn, respectively, and each tube is supplemented with deionized water to 6.0mL and mixed. Add 1.0mL of 5% sodium nitrite solution to each group and mix, and place at room temperature for 6min; then add 1.0mL of 10% aluminum nitrate solution to each group and mix, and place at room temperature for 6min; add 10.0mL of 4% sodium hydroxide solution to each group, and supplement with deionized water to 25mL and mix, and place at room temperature for 15min. Take the 0# group as the blank control group, and measure the absorbance of the reaction solution of each group at 510nm wavelength, and draw the standard curve with the concentration of the rutin standard solution as the horizontal coordinate and the absorbance as the vertical coordinate. The standard curve equation is y=ax+b.
[0237] 1.2 Water-soluble total polysaccharides content test
[0238] Precisely weigh 10 mg of anhydrous grape standard, dilute with deionized water to 100 mL, take 0.4 mL, 0.6 mL, 0.8 mL, 1.0 mL, 1.2 mL, 1.4 mL standard solution into 6 colorimetric tubes, and add deionized water to 2.0 mL; take another 2 test tubes and add deionized water 2.0 mL as blank control. Add 1.0 mL of 5% phenol solution, shake well and quickly add 5.0 mL of concentrated sulfuric acid, shake well, react for 30 min, then cool to room temperature, and measure the absorbance at 490 nm. Linear regression is performed with the standard solution concentration as X value and the absorbance as Y value to draw the standard curve.
[0239] 1.3 Detection of water-soluble total flavonoids content of sample
[0240] Take 1.0 mL of test solution, add deionized water to 6 mL, add 1 mL of 5% sodium nitrite solution, mix well, and stand at room temperature for 6 min, then add 1 mL of 10% aluminum nitrate solution, mix well, and stand at room temperature for 6 min; add 10 mL of 4% sodium hydroxide solution, mix well with deionized water to 25 mL, stand at room temperature for 15 min. Measure the absorbance of the reaction solution at 510 nm, with 0# as the blank control group, and each test solution group is done in duplicate. Calculate the water-soluble total flavonoids content according to the following formula, and finally convert the total flavonoids content unit to mg / mL.
[0241] X=c*N;
[0242] X is the content of flavonoids in the sample, with unit of mg / g;
[0243] c=(y-b) / a, is the mass concentration of flavonoids in the test solution measured by the standard curve, with unit of mg / mL;
[0244] N is the dilution multiple of the test solution.
[0245] 1.4 Detection of water-soluble total polysaccharide content of sample
[0246] Precisely weigh 0.2 g of the sample to be tested, dissolve with 50 mL of boiling water, cool to room temperature, and dilute to 100 mL. Take 2.0 mL of sample solution and add 10 mL of 70% ethanol, shake well and precipitate and flocculate overnight, centrifuge at 10000 rpm for 10 min, take the precipitate and dilute to 100 mL, shake well. Take 2.0 mL of the sample to be tested and add 1 mL of 5% phenol solution, shake well, then add 5 mL of concentrated sulfuric acid, mix well, and stand at room temperature for 30 min. After cooling to room temperature, measure the absorbance at 490 nm. Calculate the water-soluble total polysaccharide content according to the following formula, and finally convert the polysaccharide content unit to mg / mL.
[0247] X=c*V*0.9 / m*100%
[0248] X is the content of polysaccharide in the sample, %.
[0249] c is the content of the multiple lines measured in the standard curve, in mg / mL;
[0250] 0.9 is the correction coefficient;
[0251] V is the total volume of the sample after dilution, in mL;
[0252] m is the mass of the sample, in mg.
[0253] 1.5 Test the water-soluble total solid content of the sample
[0254] Accurately weigh 5 g of rose mud sample, add water to make up to 50 mL, mix well to obtain the sample to be tested; filter the sample to be tested with a vacuum filter to remove the non-water-soluble solids; take the weighing bottle into the oven at (105±2) °C and dry for 1.5 h, then cool in the desiccator for 30 min, and weigh, recorded as M0; place the water phase obtained after filtration in a weighing bottle, and place the weighing bottle in an oven at (105±2) °C with the lid slightly open, dry for 6 h, take it out and cover the lid, and place it in a desiccator to cool for 30 min; then place it in an oven at (105±2) °C with the lid slightly open, dry for 30 min, take it out and cover the lid, and place it in a desiccator to cool for 30 min, until the difference between the two consecutive weighings is ≤1 mg, recorded as M. Each group of samples is tested in duplicate. The water-soluble solid content is calculated according to the following formula:
[0255] Water-soluble solid content%= (M-M0) / 5*100%.
[0256] 2 Experimental results
[0257] The results are shown in Tables 19-21.
[0258] Table 19 Test results of water-soluble total flavone content
[0259]
[0260] Table 20 Test results of water-soluble total polysaccharide content
[0261]
[0262] Table 21 Test results of water-soluble solid content
[0263]
[0264] Result description: The water-soluble total flavone, total polysaccharide, and water-soluble solid contents of Examples 1-3 are all higher than those of Comparative Examples 1-6.
[0265] Example 5: Efficacy test of rose mud
[0266] 1 Experimental method
[0267] DPPH (1, 1-Diphenyl-2-picrylhydrazyl) is a stable nitrogen-centered free radical, its alcohol solution is purple, and has a maximum absorption peak at a wavelength of 517 nm. When an antioxidant is present, the single electron of the DPPH free radical is captured, making its color lighter, the absorbance decreases, and the degree of decrease is proportional to the degree of free radical scavenging, so that the antioxidant capacity of the sample can be evaluated. According to the instructions of the reagent manufacturer, the sample to be tested is dissolved in 80% anhydrous ethanol and diluted to the concentration to be tested, a certain amount of sample solution and DPPH working solution are added in a 96-well plate, mixed, and then placed in the dark at room temperature for 30 minutes, and the absorbance is read at 517 nm.
[0268] Scavenging rate (%) = (1 - OD value of sample group / OD value of blank control group) * 100%.
[0269] The experimental results are expressed as mean ± standard deviation (x ± s), ANOVA test is used for statistical analysis, and Dunnett's multiple comparison test is used for post-hoc test, with a significance level of α = 0.05.
[0270] 2 Experimental results
[0271] The results are shown in Table 22.
[0272] Table 22 Results of sample (0.5%) scavenging DPPH free radicals
[0273]
[0274] Note: *p <0.05 vs Example 1, **p <0.01 vs Example 1.
[0275] Result description: Examples 1-3 and Comparative Examples 1-6 can significantly scavenge DPPH free radicals at a concentration of 0.5%, and the effect of Examples 1-3 is significantly better than that of Comparative Example 1-Comparative Example 6.
[0276] The above detailed description is a specific description of one of the feasible embodiments of the present application, and is not used to limit the patent scope of the present application. Any equivalent implementation or change that does not deviate from the present application shall be included in the scope of the technical solutions of the present application.
Claims
1. A cosmetic rose clay mask, characterized by, The raw materials include rose mud and auxiliary materials; the preparation raw materials of the rose mud include rose residue and compound bacteria, the compound bacteria include lactic acid bacillus and yeast with a mass ratio of 50-100:0.1-1, the yeast is Bayanus, and the lactic acid bacillus is lactobacillus plantarum; the auxiliary materials include moisturizing agent, thickening agent; The mass ratio of the rose residue and the compound bacteria is 100:0.5-1; The preparation method of the rose mud comprises the following steps: (1) inoculating the rose residue with the compound bacteria and fermenting; (2) sterilizing and grinding pulp; (3) removing water by filter membrane to obtain the rose mud; The fermentation in step (1) is first fermenting at 30-35 DEG C for 24-48 h, then adjusting the temperature to 25-28 DEG C and continuing to ferment for 48-72 h.
2. The cosmetic rose clay mask according to claim 1, characterized in that, The moisturizing agent is one or more of glycerol, 1,2-hexanediol and arginine, and the thickening agent is one or more of SEPIMAX ZEN, SEPINOV EMT10, SEPINOV WEO, microcrystalline cellulose PH-105 and Hamsen gum.
3. The cosmetic rose clay mask according to claim 1, characterized in that, The auxiliary materials further include emulsifying agent, emulsion stabilizer, antioxidant, adsorbent and emollient.
4. The cosmetic rose clay mask according to claim 3, characterized in that, The emulsifying agent is Amphisol K, and / or the emulsion stabilizer is cetyl alcohol or stearyl alcohol, and / or the antioxidant is p-hydroxyacetophenone, and / or the adsorbent is ImerCare 04K kaolin, and / or the emollient is one or more of lanol 99, BYE SPTO, squalane, Myritol 318RC and DM10.
5. The cosmetic rose clay mask according to claim 1, characterized in that, The grinding pulp in step (2) is ground by a colloid mill to below 50 mu m, and / or the water is removed by a filter membrane with a molecular weight of 100-300 daltons in step (3) to obtain the rose mud with a solid content of below 20%, and / or the rose residue in step (1) is the residue by-product after extracting volatile oil from fresh rose by steam distillation, and the fresh rose is selected from Damask rose, Pingyin heavy petal rose or Kusyu rose.
6. A rose petal mud, characterized in that, It is the rose mud in the rose mud mask for cosmetics in any one of claims 1-5.
7. Use of the rose mud mask for cosmetics in any one of claims 1-5 or the rose mud in claim 6 in the preparation of a product with the efficacy of promoting skin oil balance, and / or sebum balance, and / or anti-wrinkle, and / or improving skin elasticity.
Citation Information
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