A freeze-dried mask based on yujian powder and a preparation method thereof

Abstract

The application discloses a freeze-dried mask based on Yuyong Powder and a preparation method thereof, and the preparation method comprises the following steps: after raw materials of the Yuyong Powder are crushed at low temperature, the raw materials are extracted at low temperature by using a composite solvent, and then the extracted solution is refined by flocculation clarification, centrifugation and microfiltration to obtain a refined extraction solution; the refined extraction solution is mixed with a humectant and a freeze-drying protective agent, and then is injected into a mask support, and gradient temperature control freeze-drying is carried out; finally, the freeze-dried mask is sealed and packaged under sterile conditions by using nitrogen. Through the whole low-temperature process and the synergistic effect of the composite freeze-drying protective agent, the heat-sensitive whitening components such as paeoniflorin, salvianolic acid and glabridin in the Yuyong Powder are effectively retained; impurities are removed through three-stage refining and purification, so that the irritability of the product is reduced; through freeze-drying and high-barrier packaging, the product can be stored at room temperature for a long time. The obtained freeze-dried mask can be quickly reconstituted when meeting water, has a refreshing skin feeling, and has remarkable effects of removing yellow and brown spots and whitening, and has the advantages of high activity, high stability, high convenience and high safety.

Description

Technical Field

[0001] This invention relates to the field of cosmetic technology, and in particular to a freeze-dried facial mask based on Yu Rong San and its preparation method. Background Technology

[0002] The removal of melasma is a core demand in the skincare market, with the key being to inhibit melanin production, even out skin tone, and lighten existing pigmentation. Currently, common solutions for melasma include oral anti-pigmentation agents, topical whitening cosmetics, and medical aesthetic treatments. Oral products are slow to take effect and cannot precisely target the melasma areas; traditional topical ingredients such as arbutin and kojic acid, while having some lightening effect, are highly irritating and unsuitable for the sensitive skin often associated with melasma; medical aesthetic procedures such as laser treatments and chemical peels are expensive and carry the risk of inducing post-inflammatory hyperpigmentation or damaging the skin barrier. Therefore, developing a product that is gentle, highly stable, and effectively removes melasma has become a current research hotspot in the industry.

[0003] Traditional Chinese medicine (TCM) topical preparations have shown great potential in the field of skin whitening due to their multi-target effects and minimal side effects. Among them, Yu Rong San, a classic TCM compound, has significant effects in improving dull skin tone and fading pigmentation. Its whitening mechanism involves the synergistic effects of multiple herbs, such as Poria cocos inhibiting melanoma cells, and Paeonia lactiflora and Salvia miltiorrhiza providing antioxidant effects.

[0004] However, existing Yu Rong San products suffer from the following technical bottlenecks: (1) Low activity and poor utilization of active ingredients: In traditional powder or paste dosage forms, it is difficult for active ingredients to be fully released and penetrated; in conventional aqueous solutions, heat-sensitive ingredients (such as paeoniflorin and glycyrrhizin) are easily degraded during production and storage.

[0005] (2) Poor product stability and short shelf life: Creams or wet masks rich in nutrients are prone to microbial growth, and the active ingredients are easily hydrolyzed and oxidized. They usually require the addition of a large amount of preservatives and rely on cold chain transportation, which is costly and inconvenient.

[0006] (3) Poor user experience and low user compliance: Traditional Yu Rong San requires temporary preparation, which has disadvantages such as difficulty in controlling the ratio, uneven application, sticky skin feel, and troublesome cleaning.

[0007] (4) Single carrier function: Ordinary mask base fabric only serves as a carrier for essence, lacking the ability to adsorb, control release and synergistic effect of effective ingredients.

[0008] Therefore, there is an urgent need for a freeze-dried facial mask based on Yu Rong San and its preparation method. Summary of the Invention

[0009] The purpose of this invention is to provide a freeze-dried facial mask based on Yu Rong San and its preparation method. Through specific processes and formulations, it achieves efficient retention of whitening active ingredients, improves the removal effect on melasma, enhances product stability, and provides an excellent user experience.

[0010] The above-mentioned technical objective of the present invention is achieved through the following technical solution: A method for preparing a freeze-dried facial mask based on Yu Rong San includes the following steps: S1. Raw material pretreatment: The raw materials of Yu Rong San are screened, cleaned and pulverized at low temperature to obtain Chinese medicine powder; S2. Extraction of active ingredients: The Chinese herbal powder is extracted at low temperature using a compound solvent to obtain a crude extract; The crude extract is then purified by flocculation clarification, centrifugation and microfiltration to obtain a refined extract of Yu Rong San. S3. Matrix preparation: Mix the refined extract of Yu Rong San with a moisturizer and a freeze-drying protectant, and adjust the pH value to 5.5-6.5 to obtain the mask matrix solution. S4. Shaping: Inject the mask matrix liquid into the mask holder and spread it evenly; S5. Freeze-drying: The mask holder containing the mask matrix liquid is pre-frozen, sublimated and desorption dried in sequence to obtain a freeze-dried mask semi-finished product. S6. Post-processing: Under aseptic conditions, the freeze-dried mask semi-finished product is sealed and packaged to obtain the freeze-dried mask based on Yu Rong San.

[0011] More preferably, the raw materials of Yu Rong San by weight include: principal ingredient: 10 parts of white peony root, 9 parts of salvia miltiorrhiza, and 12 parts of white poria cocos; assistant ingredient: 9 parts of atractylodes macrocephala, 6 parts of silkworm pupae, 6 parts of licorice root, and 6 parts of notoginseng; adjuvant ingredient: 5 parts of white peony root, 5 parts of bletilla striata, and 6 parts of angelica sinensis; and guiding ingredient: 3 parts of nardostachys chinensis.

[0012] More preferably, in step S1, the temperature of the low-temperature pulverization is -20℃ to -10℃, and the pulverized material is passed through an 80-mesh sieve.

[0013] More preferably, in step S2, the composite solvent is a mixture of purified water and ethanol at a volume ratio of 7:3; the low-temperature extraction temperature is 40-45℃, the material-to-liquid ratio is 1:10-1:15 (g / ml), and the extraction is performed twice.

[0014] More preferably, in step S2, the specific steps of the purification are as follows: add 0.1%-0.2% chitosan to the crude extract, let it stand at 4±1℃ for 24 hours for flocculation and clarification, then centrifuge at 8000r / min for 15 minutes, and then filter through a 0.45μm filter membrane.

[0015] More preferably, in step S3, the humectant is glycerin and sodium hyaluronate, and the freeze-drying protectant is mannitol and maltodextrin.

[0016] More preferably, based on the mass of the refined extract of Yu Rong San, the amount of the moisturizer added is: 5% glycerin and 0.2% sodium hyaluronate; the amount of the freeze-drying protectant added is: 8% mannitol and 2% maltodextrin.

[0017] More preferably, in step S5, the specific conditions for freeze-drying are as follows: Pre-freezing: Lower the material temperature to -40℃ and pre-freeze at a constant temperature for 2 hours; Sublimation drying: Reduce the vacuum to below 10 Pa, raise the material temperature to -15℃, and dry at a constant temperature for 12 hours; Analysis drying: Maintain a vacuum of ≤10Pa, raise the material temperature to 25℃, and dry at a constant temperature for 6 hours until the final moisture content of the material is ≤3%.

[0018] In a further preferred embodiment, in step S6, after freeze-drying, sterile nitrogen gas filtered through a 0.22μm sterile filter is introduced to break the vacuum; under a C+A grade sterile environment, sterile aluminum foil composite film is used for packaging, and sterile nitrogen gas is filled into the packaging to replace the air, and then it is sealed.

[0019] The present invention also provides a freeze-dried facial mask based on Yu Rong San, which is prepared by the above-described preparation method.

[0020] In summary, the present invention has the following beneficial effects: Firstly, this invention employs a low-temperature processing technology throughout the entire process, combined with a composite freeze-drying protectant, which maximizes the protection of heat-sensitive whitening ingredients such as paeoniflorin, salvianolic acid, and glycyrrhizin in Yu Rong San, ensuring a retention rate of ≥90%. The product can be quickly reconstituted upon contact with water, and the effective ingredients can be rapidly released, guaranteeing the whitening effect and the effect of removing age spots.

[0021] Secondly, this invention uses freeze-drying technology to control the product's moisture content to below 3%, and combines this with sterile nitrogen filling and high-barrier aluminum foil packaging to effectively isolate oxygen and moisture, preventing the oxidative degradation of active ingredients and the growth of microorganisms. The product can be stably stored at room temperature for 24 months, solving the problem of traditional Chinese medicine facial masks requiring refrigeration and being prone to spoilage.

[0022] Thirdly, the freeze-dried mask of this invention has a loose and porous structure, good rehydration properties, and a refreshing and non-sticky feel on the skin. Combined with the modified base fabric, the product has high adhesion, no dripping, and is convenient to use, greatly enhancing the user's skincare experience.

[0023] Fourth, this invention uses a three-stage refining process of chitosan flocculation, high-speed centrifugation, and microfiltration to effectively remove irritating impurities such as proteins and tannins from the extract. At the same time, it adjusts the pH value of the product to 5.5-6.5, which is in line with the physiological environment of the skin, significantly reducing the risk of skin irritation and making it suitable for people with sensitive skin. Detailed Implementation

[0024] Example: A method for preparing a freeze-dried facial mask based on Yu Rong San, the specific steps of which are as follows: S1. Raw material pretreatment: Weigh out the following herbs by weight: 10g of white peony root, 9g of salvia miltiorrhiza, 12g of poria cocos; 9g of atractylodes macrocephala, 6g of silkworm pupae, 6g of licorice root, 6g of notoginseng; 5g of white peony root, 5g of bletilla striata, 6g of angelica sinensis; and 3g of nardostachys chinensis. Remove impurities, rinse twice quickly with purified water at 32℃ for 30 seconds each time, and drain. Place the washed herbs in a low-temperature grinder and grind at -15℃. Pass the powder through an 80-mesh sieve and collect the sieve-through powder.

[0025] S2. Extraction of active ingredients: Take the above-mentioned Chinese herbal powder and add purified water-ethanol (7:3, v / v) composite solvent at a material-liquid ratio of 1:12 (g / ml). Extract twice at a constant temperature of 42℃ and 0.1MPa, the first time for 1.5 hours and the second time for 1 hour. After each extraction, filter through a 120-mesh filter cloth and combine the two filtrates to obtain the crude extract.

[0026] The crude extract was cooled to 25°C, and 0.15% chitosan was added. After stirring evenly, the mixture was refrigerated at 4°C for 24 hours. Then, it was centrifuged at 8000 rpm for 15 minutes, and the supernatant was collected. Finally, the supernatant was filtered through a 0.45 μm organic phase filter membrane to obtain the refined extract of Yu Rong San.

[0027] S3, Matrix Preparation: Place the purified extract in a mixing tank and heat to 38°C. While stirring at 300 rpm, add glycerol (5%), sodium hyaluronate (0.2%), mannitol (8%), and maltodextrin (2%) in sequence, stirring for 20 minutes until completely dissolved. Adjust the pH to 6.0 with citric acid and cool to room temperature.

[0028] S4, Molding: Pour the prepared mask base solution into a food-grade PP mask holder that has been sterilized by high-pressure steam at 121℃ for 20 minutes. The amount injected into each mask is 25mL. Gently shake the mask to spread the base solution evenly without air bubbles.

[0029] S5, freeze-drying: Place the mask containing the substrate solution onto the material rack of the freeze dryer, which has been pre-cooled to -10°C, and close the door. Perform freeze drying. Pre-freezing: Lower the material temperature to -40℃ and maintain a constant temperature for 2 hours for pre-freezing.

[0030] Sublimation drying: Start the vacuum system to reduce the vacuum level inside the chamber to below 10 Pa, then raise the material temperature to -15°C and maintain this temperature and vacuum level for constant drying for 12 hours.

[0031] Analysis and drying: Maintain the vacuum degree in the chamber ≤10Pa, raise the material temperature to 25℃, and keep the temperature constant for 6 hours until the material moisture content ≤3%.

[0032] S6. Post-processing: After freeze-drying, sterile nitrogen gas filtered through a 0.22μm sterile filter is introduced to break the vacuum, followed by the introduction of sterile nitrogen gas with a purity ≥99.99% to atmospheric pressure. Under a C+A grade aseptic environment, the freeze-dried masks are quickly removed and immediately sealed in aluminum foil composite bags in a sterile packaging workshop with humidity ≤45% and temperature 22℃, one mask per bag. After packaging, the finished product undergoes inspection. Those that pass inspection are then stored at 20℃ and humidity ≤50%.

[0033] Comparative Example: This comparative example provides a method for preparing an existing Yu Rong San medicated cloth, specifically: the crude extract that has not been refined and purified in the example is directly adsorbed onto an ordinary non-woven fabric base, and then sealed and packaged.

[0034] Effect verification 1. Active ingredient retention rate test: The content of key active ingredients (paeoniflorin, salvianolic acid, and glycyrrhizin) in the purified extract and the final freeze-dried facial mask in the examples was determined by high performance liquid chromatography (HPLC), and the retention rates were calculated. The results showed that the retention rates of each component were all above 92%.

[0035] 2. Stability Test: The products of the examples and comparative examples were subjected to accelerated testing in a constant temperature and humidity chamber at 40°C and 75%RH for 6 months, and then placed at room temperature for 24 months, respectively. The test results showed that after 3 months of accelerated testing, the content of the active ingredient in the comparative example product decreased by more than 20%, and a rancid odor appeared. In contrast, after 6 months of accelerated testing and 24 months of storage at room temperature, the products of the examples showed no significant changes in appearance, odor, pH value, or content of the active ingredient, and met the quality standards.

[0036] 3. Test on the efficacy of removing age spots and whitening skin: Thirty volunteers with melasma and dull skin were recruited and randomly divided into two groups. One group used the freeze-dried mask (reconstituted with purified water and applied to the face) from the example group, while the other group used the medicated handkerchief (applied directly to the face) from the control group. Both groups used the mask once daily for eight weeks. Melanin and red pigmentation were measured using a skin melanin and red pigmentation analyzer before the experiment and at weeks 4 and 8 after the experiment. Changes in the area and color of the melasma were also observed. Results showed that the MI value of the melasma area in volunteers using the example group significantly decreased after four weeks (P<0.05), with an average decrease rate of 8.5%-10% after eight weeks. The melasma color lightened significantly, and the area decreased. In contrast, the MI value of volunteers using the control group decreased by an average of 7.2% after eight weeks, with less improvement than the example group. The difference between the two groups was statistically significant (P<0.01). This indicates that the example group's product has a significantly better effect on removing melasma and overall whitening than the control group.

[0037] In summary, this invention provides a freeze-dried facial mask based on Yu Rong San and its preparation method. Through specific processes and formulations, it effectively solves the problems of easy degradation of active ingredients, poor stability, and unsatisfactory user experience in traditional Yu Rong San products. The product has advantages such as high retention rate of active ingredients, good stability at room temperature, convenient use, refreshing feel, significant whitening and spot-removing effects, and high safety, and has broad market application prospects.

[0038] This specific embodiment is merely an explanation of the present invention and is not intended to limit the invention. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but such modifications are protected by patent law as long as they are within the scope of the claims of the present invention.

Claims

1. A method for preparing a freeze-dried facial mask based on Yu Rong San, characterized in that, Includes the following steps: S1. Raw material pretreatment: The raw materials of Yu Rong San are screened, cleaned and pulverized at low temperature to obtain Chinese medicine powder; S2. Extraction of active ingredients: The Chinese herbal powder is extracted at low temperature using a compound solvent to obtain a crude extract; The crude extract is then purified by flocculation clarification, centrifugation and microfiltration to obtain a refined extract of Yu Rong San. S3. Matrix preparation: Mix the refined extract of Yu Rong San with a moisturizer and a freeze-drying protectant, and adjust the pH value to 5.5-6.5 to obtain the mask matrix solution. S4. Shaping: Inject the mask matrix liquid into the mask holder and spread it evenly; S5. Freeze-drying: The mask holder containing the mask matrix liquid is pre-frozen, sublimated and desorption dried in sequence to obtain a freeze-dried mask semi-finished product. S6. Post-processing: Under aseptic conditions, the freeze-dried mask semi-finished product is sealed and packaged to obtain the freeze-dried mask based on Yu Rong San.

2. The method for preparing a freeze-dried facial mask based on Yu Rong San according to claim 1, characterized in that, The ingredients of Yu Rong San, by weight, include: principal ingredient: 10 parts white peony root, 9 parts salvia miltiorrhiza, and 12 parts white poria cocos; assistant ingredient: 9 parts atractylodes macrocephala, 6 parts silkworm pupae, 6 parts licorice root, and 6 parts notoginseng; adjuvant ingredient: 5 parts white peony root, 5 parts bletilla striata, and 6 parts angelica sinensis; and guiding ingredient: 3 parts nardostachys chinensis.

3. The method for preparing a freeze-dried facial mask based on Yu Rong San according to claim 1, characterized in that: In step S1, the temperature of the low-temperature pulverization is -20℃ to -10℃, and the pulverized material is passed through an 80-mesh sieve.

4. The method for preparing a freeze-dried facial mask based on Yu Rong San according to claim 1, characterized in that: In step S2, the composite solvent is a mixture of purified water and ethanol at a volume ratio of 7:3; the low-temperature extraction temperature is 40-45℃, the material-to-liquid ratio is 1:10-1:15 (g / ml), and the extraction is performed twice.

5. The method for preparing a freeze-dried facial mask based on Yu Rong San according to claim 4, characterized in that: In step S2, the specific steps of purification are as follows: add 0.1%-0.2% chitosan to the crude extract, let it stand at 4±1℃ for 24 hours for flocculation and clarification, then centrifuge at 8000r / min for 15 minutes, and then filter through a 0.45μm filter membrane.

6. The method for preparing a freeze-dried facial mask based on Yu Rong San according to claim 1, characterized in that: In step S3, the humectant is glycerin and sodium hyaluronate, and the freeze-drying protectant is mannitol and maltodextrin.

7. The method for preparing a freeze-dried facial mask based on Yu Rong San according to claim 6, characterized in that: Based on the quality of the refined extract of Yu Rong San, the amount of the moisturizing agent added is: 5% glycerin and 0.2% sodium hyaluronate; the amount of the freeze-drying protectant added is: 8% mannitol and 2% maltodextrin.

8. The freeze-dried facial mask based on Yu Rong San and its preparation method according to claim 1, characterized in that: In step S5, the specific conditions for freeze-drying are as follows: Pre-freezing: Lower the material temperature to -40℃ and pre-freeze at a constant temperature for 2 hours; Sublimation drying: Reduce the vacuum to below 10 Pa, raise the material temperature to -15℃, and dry at a constant temperature for 12 hours; Analysis drying: Maintain a vacuum of ≤10Pa, raise the material temperature to 25℃, and dry at a constant temperature for 6 hours until the final moisture content of the material is ≤3%.

9. The freeze-dried facial mask based on Yu Rong San and its preparation method according to claim 1, characterized in that: In step S6, after freeze-drying, sterile nitrogen gas filtered through a 0.22μm sterile filter is introduced to break the vacuum; under a C+A grade sterile environment, sterile aluminum foil composite film is used for packaging, and sterile nitrogen gas is filled into the packaging to replace the air, and then it is sealed.

10. A freeze-dried facial mask based on Yu Rong San, characterized in that, It is prepared by the preparation method according to any one of claims 1-9.