Preparation method of white tea fermentation filtrate, white tea fermentation filtrate product and preparation method

Through the combined fermentation of fermented white tea extract, Ganoderma lucidum seed liquid and liquid culture medium, the problem of insufficient application of white tea fermentation in the prior art was solved, and the polyphenols and total flavonoid content in the white tea fermentation filtrate was significantly improved, achieving excellent antioxidant and skin care effects.

CN119679674APending Publication Date: 2025-03-25SHANGHAI CHUNZHIBAO BIOTECHNOLOGY CO LTD
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Patent Information

Application Number
CN202411871930.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-18
Publication Date
2025-03-25

AI Technical Summary

Technical Problem

Few research and products in the prior art involve fermented white tea, resulting in insufficient application in the field of plant cosmetics production, especially in obtaining high content of polyphenols and total flavonoids.

Method used

The white tea extract was obtained by ultrasonic extraction with airflow ultrasonic solution and aqueous butylene glycol, and fermented with Ganoderma lucidum seed liquid and liquid culture medium in a preferred ratio to prepare a white tea fermentation filtrate containing more polyphenols and total flavonoids.

Benefits of technology

It has achieved a significant increase in polyphenols and total flavonoids in the white tea fermentation filtrate, which has improved its antioxidant, anti-wrinkle and anti-photoaging effects, and provided better skin care effects, such as moisturizing, wrinkle removal and barrier repair.

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Abstract

The invention relates to a preparation method of a white tea fermentation filtrate, a white tea fermentation filtrate product and a preparation method. The preparation method sequentially comprises the following steps: (1) obtaining a white tea extract; (2) obtaining a ganoderma lucidum seed solution; (3) obtaining a white tea fermentation product: sterilizing and cooling the white tea extract liquid obtained in the step (1), uniformly mixing the white tea extract liquid with the ganoderma lucidum seed liquid obtained in the step (2) and the liquid culture medium obtained in the step (2) according to the volume ratio of (800-1000): (10-100): (20-100), and fermenting for 48-96 hours under the conditions that the temperature is 30-40 DEG C and the pH value is 5.0-7.0; and (4) obtaining white tea fermentation filtrate. The method overcomes the defects that related reports for researching fermented white tea exist in the market and more products of the fermented white tea exist, and the white tea extract prepared by adopting optimal preparation steps and technological parameters, the ganoderma lucidum seed liquid and the liquid culture medium are fermented according to an optimal proportion, so that the white tea with more polyphenol, total flavonoids and the like can be obtained. The white tea fermentation filtrate has the advantages of excellent oxidation resistance, wrinkle resistance and light aging resistance.
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Description

Technical Field

[0001] The invention relates to a preparation method of white tea fermentation filtrate, a white tea fermentation filtrate product and a preparation method, and the white tea fermentation filtrate product is applied in the field of plant cosmetic production. Background Art

[0002] As one of the six traditional teas in my country, white tea has a long history, which can be traced back to the Sui and Tang Dynasties. Its unique production method does not involve frying or kneading. The finished tea is covered with white hairs, so it is called white tea. It is generally divided into four types: Baihao Yinzhen, Bai Mudan, Gongmei, and Shoumei. Among them, Baihao Yinzhen is made from fat buds, which are fat, straight and even, covered with white hairs, white as silver, and shaped like needles. The hairs are not only an important feature of the appearance, but also a reflection of its quality. They sparkle like silver in the sun and are very ornamental, like a work of art among teas. It is the most precious category among white teas. Fuding has a unique natural environment suitable for the growth of white tea, such as the subtropical monsoon climate and mineral-rich soil, which makes the white tea produced here fat buds, white hairs, bright soup color, and mellow taste. Therefore, there is a saying that "the world's white tea can be seen in China, and China's white tea can be seen in Fuding".

[0003] Fermentation refers to the process of preparing products with the help of the life activities of microorganisms under aerobic or anaerobic conditions. Fermentation can effectively decompose plant cell walls, making it easier to release the effective ingredients in the cells, thereby improving the extraction efficiency. Fermentation can also transform some components in plants to generate new active substances, further enhancing the efficacy of plant extracts.

[0004] Ganoderma lucidum is the dried fruiting body of the Polyporaceae fungus Ganoderma lucidum (Leyss.ex Fr.) Karst. or Ganoderma sinense Zhao, Xu et Zhang. It has the effects of replenishing qi and calming the mind, relieving cough and asthma, and is mainly used to treat restlessness, insomnia, palpitations, cough, asthma, excessive sputum, and asthenia.

[0005] White tea tastes sweet and bitter, and is cold in nature. It has the effects of detoxification and purging fire. Ganoderma lucidum is a precious Chinese medicinal material, sweet in taste, neutral in nature, and enters the heart, lung, liver, and kidney meridians, and has the effect of strengthening the body. After the two are combined, the antioxidant capacity is enhanced. From the "holistic concept" of traditional Chinese medicine, it can regulate the body's qi and blood and the functions of the internal organs, and achieve the purpose of adjusting the complexion and delaying aging.

[0006] White tea is a naturally withered tea with a unique and simple production process, which retains most of the nutrients in tea. Modern research shows that white tea has high levels of flavonoids and polyphenols, and has good antioxidant and anti-radiation effects. At the same time, it can also improve eyesight, refresh the mind, resist oxidation, delay aging, regulate intestinal flora, improve immunity, and prevent allergies. In addition, white tea also has significant beauty and anti-aging effects. Invention patent application CN201611116033.8 discloses a white tea extract and its preparation method and application. The patent involves a white tea extract with multiple functions such as moisturizing, whitening, moisturizing, and anti-aging. However, there are few reports on fermented white tea. In order to further expand the application of white tea, the present invention aims to further utilize white tea resources in combination with modern fermentation technology and provide a new technical solution for the development of white tea.

[0007] Therefore, it is urgent to provide a method for preparing white tea fermentation filtrate containing more polyphenols and total flavonoids and having excellent antioxidant, anti-wrinkle and anti-photoaging effects, a white tea fermentation filtrate product and a preparation method. Summary of the invention

[0008] In order to overcome the shortcomings that there are few reports on the research of fermented white tea and even fewer products of fermented white tea in the market, the present invention provides a method for preparing a white tea fermentation filtrate, a white tea fermentation filtrate product and a preparation method. The white tea extract prepared by adopting preferred preparation steps and process parameters and the ganoderma lucidum seed liquid are fermented with a liquid culture medium in a preferred proportion, which has the advantages of being able to obtain a white tea fermentation filtrate containing more polyphenols and total flavonoids, and the white tea fermentation filtrate product prepared by the white tea fermentation filtrate has excellent antioxidant, anti-wrinkle and anti-photoaging effects.

[0009] The technical solution of the present invention is as follows:

[0010] A method for preparing white tea fermentation filtrate comprises the following steps performed in sequence:

[0011] (1) The dried white tea is subjected to air flow ultrafine grinding and sieved through 380-420 meshes, and a 20% by mass concentration of butanediol aqueous solution is added and mixed at a material-liquid ratio of 1:20-30, and ultrasonic extraction is performed at 30-35° C. and an ultrasonic power of 180-220 W for 60-120 min; and then filtered through 350-450 meshes to obtain a white tea extract;

[0012] (2) inoculating the Ganoderma lucidum slant block into a sterilized liquid culture medium, and culturing in a shaker at 28-32° C. and a rotation speed of 100-200 rpm for 3-5 days to obtain Ganoderma lucidum seed liquid;

[0013] The liquid culture medium is prepared by adding 18-22 g of glucose, 11-18 g of malt extract powder, 3-8 g of corn steep liquor, 0.1-3 g of yeast extract powder and 0.5-3 g of peptone to each liter of water;

[0014] (3) sterilizing and cooling the white tea extract obtained in step (1), mixing it evenly with the ganoderma lucidum seed solution obtained in step (2) and the liquid culture medium in step (2) at a volume ratio of 800-1000:10-100:20-100, and fermenting it at 30-40° C. and a pH value of 5.0-7.0 for 48-96 hours to obtain a white tea fermentation product;

[0015] (4) sterilizing the white tea fermentation product obtained in step (3), cooling it, and filtering it to obtain a white tea fermentation filtrate.

[0016] The preparation method of the white tea fermentation filtrate of the present application is to ferment the white tea extract prepared by the preferred preparation steps and process parameters and the ganoderma lucidum seed liquid and liquid culture medium according to the preferred ratio, and has the advantages of being able to obtain a white tea fermentation filtrate containing more polyphenols and total flavonoids and having excellent antioxidant, anti-wrinkle and anti-photoaging effects. It creatively adopts airflow ultrafine grinding and ultrasonic extraction of 20% mass percentage concentration of butanediol aqueous solution to obtain white tea extract, and uses the white tea extract as a fermentation substrate, and optimizes the fermentation conditions to ferment the ganoderma lucidum mycelium. Compared with the existing white tea extract obtained only by ultrasonic extraction and the white tea fermentation liquid obtained by other fermentation methods, it not only retains the effective components of white tea to the greatest extent, but also greatly improves the release and conversion of the effective components in white tea, and can obtain a higher content of polyphenols and total flavonoids. Moreover, after the fermentation process conversion, the irritation of the product is further reduced, so that the obtained white tea fermentation filtrate has more excellent skin care effects, such as moisturizing, anti-wrinkle, barrier repair and brightening, etc. after being used as an active raw material.

[0017] The air flow ultrafine grinding in step (1) is carried out under nitrogen protection, and the specific conditions are: air pressure 0.5-1.0 MPa, system air volume 2.0-4.0 m3 / min, classifier speed 2500-4000 r / min, and feeding rate 3.0-5.0 kg / h.

[0018] The preferred air flow ultrafine grinding has a better grinding effect.

[0019] Airflow ultrafine grinding has higher crushing efficiency and better crushing degree than conventional crushers.

[0020] The wet weight content of Ganoderma lucidum mycelium in the Ganoderma lucidum seed liquid obtained in step (2) is 5-15 g / L.

[0021] The preferred ganoderma lucidum seed liquid can be combined with the white tea extract and liquid culture medium in a preferred ratio to obtain the best fermentation effect.

[0022] The filtration in step (4) is performed using a 1-5 μm filter membrane.

[0023] The preferred filtering conditions result in less impurities in the white tea fermentation filtrate.

[0024] The sterilization conditions of the liquid culture medium in step (2) and the white tea fermentation product in step (4) are both: sterilization at 115-121° C. for 15-30 min.

[0025] Preferably, the white tea is Fuding Baihao Yinzhen.

[0026] The preferred white tea fermentation filtrate prepared from white tea has high polyphenol and total flavonoid components.

[0027] A white tea fermentation filtrate product, which is a white tea fermentation filtrate cosmetic prepared using the white tea fermentation filtrate, wherein the white tea fermentation filtrate cosmetic is mainly prepared from the following components in the following mass proportions:

[0028]

[0029] In this case, white tea fermentation filtrate is used as the active ingredient, and other preferred components and preferred usage ratios are added to obtain white tea fermentation filtrate cosmetics. After human efficacy verification, it has good moisturizing, anti-wrinkle, excellent antioxidant, anti-photoaging, barrier repair and brightening effects, proving that it is safe and gentle and can be used for a long time.

[0030] The polyol is one of 1,3-butylene glycol, 1,3-propylene glycol or glycerol or any combination of any two or more thereof, and the thickener is xanthan gum or carbomer.

[0031] The preferred polyols and thickeners are the polyols and thickeners commonly used in the market, which have good effects and are safe to use.

[0032] The oil is one of white oil, caprylic / capric triglyceride, squalane, cetearyl alcohol or beeswax, or any combination of any two or more thereof; the emulsifier is one of polyglycerol fatty acid ester or glyceryl stearate / PEG-100 stearate, or any combination of any two thereof.

[0033] The preferred oils and emulsifiers are all commonly used raw materials on the market, with high frequency of use and high safety.

[0034] The method for preparing the white tea fermentation filtrate product comprises the following steps performed in sequence:

[0035] 1) adding white tea fermentation filtrate, polyol, thickener and water into a container and mixing them evenly at 80-85° C. to obtain a water phase material;

[0036] 2) Add the oil and emulsifier into a container, mix them evenly while stirring at 80-95° C. to obtain the oil phase material;

[0037] 3) Adding the oil phase material to the water phase material at 80-85° C. while stirring, and mixing for 25-35 minutes; then cooling to 40-45° C., adding a preservative, and stirring evenly to obtain white tea fermentation filtrate cosmetics.

[0038] The preferred preparation method of the white tea fermentation filtrate product is simple to operate and suitable for industrial production.

[0039] Compared with the prior art, the present invention has the following advantages:

[0040] 1) The method for preparing the white tea fermentation filtrate of the present application has the advantages of being able to obtain a white tea fermentation filtrate containing more polyphenols and total flavonoids and having excellent antioxidant, anti-wrinkle and anti-photoaging effects by fermenting the white tea extract prepared by the preferred preparation steps and process parameters and the ganoderma lucidum seed liquid and liquid culture medium according to the preferred ratio. ;

[0041] 2) In this case, white tea fermentation filtrate is used as the active ingredient, and other preferred components and preferred usage ratios are added to obtain white tea fermentation filtrate cosmetics. The human body efficacy test shows that it has good moisturizing, wrinkle removal, excellent antioxidant, anti-photoaging, barrier repair and brightening effects, proving that it is safe and mild and can be used for a long time;

[0042] 3) The method for preparing the white tea fermentation filtrate product is simple to operate and suitable for industrial production. BRIEF DESCRIPTION OF THE DRAWINGS

[0043] Figure 1 This is the appearance of the white tea extract prepared in Comparative Example 4;

[0044] Figure 2 This is an appearance diagram of the white tea fermentation filtrate prepared in Example 1 of the preparation method of the white tea fermentation filtrate, the white tea fermentation filtrate product and the preparation method of the present invention;

[0045] Figure 3 It is a bar graph of DPPH free radical scavenging rate test results of various embodiments and comparative examples of the preparation method of white tea fermentation filtrate, white tea fermentation filtrate product and preparation method of the present invention;

[0046] Figure 4 It is a bar graph of the test results of elastase inhibition rate of various embodiments and comparative examples of the preparation method of white tea fermentation filtrate, white tea fermentation filtrate product and preparation method of the present invention;

[0047] Figure 5 It is a bar chart of the cell viability test results of the preparation method of the white tea fermentation filtrate, the white tea fermentation filtrate product and the preparation method of each embodiment and comparative example of the present invention;

[0048] Figure 6 It is a bar graph of the test results of the skin wrinkle quantity change rate of the white tea fermentation filtrate preparation method of the present invention, the white tea fermentation filtrate product and the preparation method, and the comparative example 1 and the placebo;

[0049] Figure 7 It is a bar graph of the test results of skin brightness change rate using comparative example 1 and placebo for the preparation method of the white tea fermentation filtrate of the present invention, the white tea fermentation filtrate product and the various embodiments of the preparation method;

[0050] Figure 8 It is a bar graph of the test results of the skin moisture content change rate of the white tea fermentation filtrate preparation method of the present invention, the white tea fermentation filtrate product and the embodiments of the preparation method, and the application of comparative example 1 and placebo.

[0051] Fig. 9 It is a bar graph of the test results of the transepidermal water loss change rate of the white tea fermentation filtrate preparation method of the present invention, the white tea fermentation filtrate product and the various embodiments of the preparation method, and the application of comparative example 1 and placebo. DETAILED DESCRIPTION

[0052] The technical solution of the present invention will be clearly and completely described below in conjunction with specific embodiments.

[0053] Example 1

[0054] The method for preparing white tea fermentation filtrate of the present invention comprises the following steps performed in sequence:

[0055] (1) The dried white tea is subjected to air flow ultrafine grinding and 400-mesh sieve in sequence, and a 20% by mass concentration of butanediol aqueous solution is added and mixed at a material-liquid ratio of 1:25, and ultrasonic extraction is performed at 32° C. and an ultrasonic power of 200 W for 100 min; then, the mixture is filtered through 400 mesh to obtain a white tea extract;

[0056] (2) inoculating the Ganoderma lucidum slant block into a sterilized liquid culture medium, and culturing in a shaker at 30° C. and 150 rpm for 4 days to obtain Ganoderma lucidum seed liquid;

[0057] The liquid culture medium is prepared by adding 20g of glucose, 15g of malt extract powder, 5g of corn steep powder, 1g of yeast extract powder and 1g of peptone into each liter of water;

[0058] (3) sterilizing and cooling the white tea extract obtained in step (1), uniformly mixing it with the ganoderma lucidum seed solution obtained in step (2) and the liquid culture medium in step (2) at a volume ratio of 1000:40:20, and fermenting it at 40° C. and pH 7.0 for 96 hours to obtain a white tea fermentation product; (4) sterilizing the white tea fermentation product obtained in step (3), cooling it, and filtering it to obtain a white tea fermentation filtrate.

[0059] The air flow ultrafine grinding in step (1) is carried out under nitrogen protection, and the specific conditions are: air pressure 0.8MPa, system air volume 3m 3 / min, classifier speed 3500r / min, feeding speed 4kg / h.

[0060] The wet weight content of Ganoderma lucidum mycelium in the Ganoderma lucidum seed liquid obtained in step (2) is 10 g / L.

[0061] The filtration in step (4) is performed using a 3.5 μm filter membrane.

[0062] The sterilization conditions of the liquid culture medium in step (2) and the white tea fermentation product in step (4) are both: sterilization at 118° C. for 25 minutes.

[0063] The white tea is Fuding Baihao Yinzhen.

[0064] A white tea fermentation filtrate product, which is a white tea fermentation filtrate cosmetic prepared using the white tea fermentation filtrate, wherein the white tea fermentation filtrate cosmetic is mainly prepared from the following components in the following mass proportions:

[0065]

[0066] The polyol includes 2 parts of 1,3-butylene glycol, 0.5 parts of 1,3-propylene glycol and 0.5 parts of glycerol, and the thickener is 0.05 parts of xanthan gum.

[0067] The oil includes 1.1 parts of white oil, 1.2 parts of caprylic / capric triglyceride, 1 part of semisqualane, 1 part of cetearyl alcohol and 0.2 parts of beeswax, and the emulsifier includes 0.5 parts of polyglycerol fatty acid ester and 1.2 parts of glyceryl stearate / PEG-100 stearate.

[0068] The method for preparing the white tea fermentation filtrate product is characterized by comprising the following steps performed in sequence:

[0069] 1) adding white tea fermentation filtrate, polyol, thickener and water into a container and mixing them evenly at 83° C. to obtain a water phase material;

[0070] 2) Add oil and emulsifier into a container and mix them evenly while stirring at 90° C. to obtain an oil phase material;

[0071] 3) Adding the oil phase material to the water phase material at 83° C. while stirring, and mixing for 30 minutes; then cooling to 42° C., adding a preservative, and stirring evenly to obtain white tea fermentation filtrate cosmetics.

[0072] Example 2

[0073] The method for preparing white tea fermentation filtrate of the present invention comprises the following steps performed in sequence:

[0074] (1) The dried white tea is subjected to air flow ultrafine grinding and sieved through 380 meshes, and a 20% by mass concentration of butanediol aqueous solution is added and mixed at a material-liquid ratio of 1:20, and ultrasonic extraction is performed at 35° C. and an ultrasonic power of 180 W for 120 min; and then filtered through 350 meshes to obtain a white tea extract;

[0075] (2) inoculating the Ganoderma lucidum slant block into a sterilized liquid culture medium, and culturing in a shaker at 32° C. and 100 rpm for 5 days to obtain Ganoderma lucidum seed liquid;

[0076] The liquid culture medium is prepared by adding 18g of glucose, 18g of malt extract powder, 3g of corn steep liquor, 3g of yeast extract powder and 0.5g of peptone into each liter of water;

[0077] (3) sterilizing and cooling the white tea extract obtained in step (1), uniformly mixing it with the ganoderma lucidum seed solution obtained in step (2) and the liquid culture medium in step (2) at a volume ratio of 800:10:50, and fermenting it at 30° C. and pH 5.0 for 48 hours to obtain a white tea fermentation product; (4) sterilizing the white tea fermentation product obtained in step (3), cooling it, and filtering it to obtain a white tea fermentation filtrate.

[0078] The air flow ultrafine grinding in step (1) is carried out under nitrogen protection, and the specific conditions are: air pressure 1.0 MPa, system air volume 2.0 m 3 / min, classifier speed 4000r / min, feeding speed 3.0kg / h.

[0079] The wet weight content of Ganoderma lucidum mycelium in the Ganoderma lucidum seed liquid obtained in step (2) is 15 g / L.

[0080] The filtration in step (4) is performed using a 1 μm filter membrane.

[0081] The sterilization conditions of the liquid culture medium in step (2) and the white tea fermentation product in step (4) are both: sterilization at 121° C. for 15 min.

[0082] The white tea is Fuding Baihao Yinzhen.

[0083] A white tea fermentation filtrate product, which is a white tea fermentation filtrate cosmetic prepared using the white tea fermentation filtrate, wherein the white tea fermentation filtrate cosmetic is mainly prepared from the following components in the following mass proportions:

[0084]

[0085]

[0086] The polyol includes 1 part of 1,3-butylene glycol, 1 part of 1,3-propylene glycol and 1 part of glycerol, and the thickener is 0.2 part of xanthan gum.

[0087] The oil comprises 0.1 part of white oil, 0.1 part of caprylic / capric triglyceride and 0.3 part of semisqualane, and the emulsifier is 0.5 part of polyglycerol fatty acid ester.

[0088] The method for preparing the white tea fermentation filtrate product is characterized by comprising the following steps performed in sequence:

[0089] 1) adding white tea fermentation filtrate, polyol, thickener and water into a container and mixing them evenly at 80° C. to obtain a water phase material;

[0090] 2) Add oil and emulsifier into a container and mix them evenly at 95°C while stirring to obtain an oil phase material;

[0091] 3) Add the oil phase material to the water phase material at 80° C. while stirring, and mix for 35 minutes; then cool to 40° C., add the preservative, and stir evenly to obtain the white tea fermentation filtrate cosmetic.

[0092] Example 3

[0093] The method for preparing white tea fermentation filtrate of the present invention comprises the following steps performed in sequence:

[0094] (1) The dried white tea is subjected to air flow ultrafine grinding and sieved through 420 meshes, and a 20% by mass concentration of butanediol aqueous solution is added and mixed at a material-liquid ratio of 1:30, and ultrasonic extraction is performed at 30° C. and an ultrasonic power of 220 W for 60 minutes; then filtered through 450 meshes to obtain a white tea extract;

[0095] (2) inoculating the Ganoderma lucidum slant block into a sterilized liquid culture medium, and culturing in a shaker at 28° C. and 200 rpm for 3 days to obtain Ganoderma lucidum seed liquid;

[0096] The liquid culture medium is prepared by adding 22g of glucose, 11g of malt extract powder, 8g of corn steep liquor, 0.1g of yeast extract powder and 3g of peptone into each liter of water;

[0097] (3) sterilizing and cooling the white tea extract obtained in step (1), uniformly mixing it with the ganoderma lucidum seed solution obtained in step (2) and the liquid culture medium in step (2) at a volume ratio of 900:100:100, and fermenting it at 35° C. and pH 6.0 for 72 hours to obtain a white tea fermentation product; (4) sterilizing the white tea fermentation product obtained in step (3), cooling it, and filtering it to obtain a white tea fermentation filtrate.

[0098] The air flow ultrafine grinding in step (1) is carried out under nitrogen protection, and the specific conditions are: air pressure 0.5MPa, system air volume 4.0m 3 / min, classifier speed 2500r / min, feeding speed 5.0kg / h.

[0099] The wet weight content of Ganoderma lucidum mycelium in the Ganoderma lucidum seed liquid obtained in step (2) is 5 g / L.

[0100] The filtration in step (4) is performed using a 5 μm filter membrane.

[0101] The sterilization conditions of the liquid culture medium in step (2) and the white tea fermentation product in step (4) are both: sterilization at 115° C. for 30 minutes.

[0102] The white tea is Fuding Baihao Yinzhen.

[0103] A white tea fermentation filtrate product, which is a white tea fermentation filtrate cosmetic prepared using the white tea fermentation filtrate, wherein the white tea fermentation filtrate cosmetic is mainly prepared from the following components in the following mass proportions:

[0104]

[0105]

[0106] The polyol includes 4 parts of 1,3-butylene glycol and 1.5 parts of glycerol, and the thickener is 0.5 parts of carbomer.

[0107] The oil includes 1.2 parts of white oil, 1 part of caprylic / capric triglyceride, 1 part of semisqualane, 1 part of cetearyl alcohol and 0.8 part of beeswax, and the emulsifier includes 1 part of polyglycerol fatty acid ester and 1 part of glyceryl stearate / PEG-100 stearate.

[0108] The method for preparing the white tea fermentation filtrate product is characterized by comprising the following steps performed in sequence:

[0109] 1) adding white tea fermentation filtrate, polyol, thickener and water into a container and mixing them evenly at 85° C. to obtain a water phase material;

[0110] 2) Add the oil and emulsifier into a container and mix them evenly while stirring at 80° C. to obtain the oil phase material;

[0111] 3) Add the oil phase material to the water phase material at 85° C. while stirring, and mix for 25 minutes; then cool to 45° C., add the preservative, and stir evenly to obtain the white tea fermentation filtrate cosmetic.

[0112] Example 4

[0113] The method for preparing white tea fermentation filtrate of the present invention comprises the following steps performed in sequence:

[0114] (1) The dried white tea is subjected to air flow ultrafine grinding and 400-mesh sieve in sequence, and a 20% by mass concentration of butanediol aqueous solution is added and mixed at a material-liquid ratio of 1:25, and ultrasonic extraction is performed at 32° C. and an ultrasonic power of 200 W for 80 minutes; then, the mixture is filtered through 400 mesh to obtain a white tea extract;

[0115] (2) inoculating the Ganoderma lucidum slant block into a sterilized liquid culture medium, and culturing in a shaker at 30° C. and 180 rpm for 4 days to obtain Ganoderma lucidum seed liquid;

[0116] The liquid culture medium is prepared by adding 20g of glucose, 12g of malt extract powder, 8g of corn steep liquor, 1g of yeast extract powder and 2g of peptone into each liter of water;

[0117] (3) sterilizing and cooling the white tea extract obtained in step (1), uniformly mixing it with the ganoderma lucidum seed solution obtained in step (2) and the liquid culture medium in step (2) in a volume ratio of 850:25:100, and fermenting it at 38° C. and pH 6.5 for 80 hours to obtain a white tea fermentation product; (4) sterilizing the white tea fermentation product obtained in step (3), cooling it, and filtering it to obtain a white tea fermentation filtrate.

[0118] The air flow ultrafine grinding in step (1) is carried out under nitrogen protection, and the specific conditions are: air pressure 0.8MPa, system air volume 3m 3 / min, classifier speed 3500r / min, feeding speed 3.5kg / h.

[0119] The wet weight content of Ganoderma lucidum mycelium in the Ganoderma lucidum seed liquid obtained in step (2) is 10 g / L.

[0120] The filtration in step (4) is performed using a 3 μm filter membrane.

[0121] The sterilization conditions of the liquid culture medium in step (2) and the white tea fermentation product in step (4) are both: sterilization at 120° C. for 18 min.

[0122] The white tea is Fuding Baihao Yinzhen.

[0123] A white tea fermentation filtrate product, which is a white tea fermentation filtrate cosmetic prepared using the white tea fermentation filtrate, wherein the white tea fermentation filtrate cosmetic is mainly prepared from the following components in the following mass proportions:

[0124]

[0125] The polyol includes 5 parts of 1,3-butylene glycol and 2 parts of glycerol, and the thickener is 0.01 part of carbomer.

[0126] The oil includes 0.1 part of white oil, 0.1 part of caprylic / capric triglyceride, 0.1 part of semisqualane, 0.1 part of cetearyl alcohol and 0.1 part of beeswax, and the emulsifier includes 0.25 part of polyglycerol fatty acid ester and 0.25 part of glyceryl stearate / PEG-100 stearate.

[0127] The method for preparing the white tea fermentation filtrate product is characterized by comprising the following steps performed in sequence:

[0128] 1) adding white tea fermentation filtrate, polyol, thickener and water into a container and mixing them evenly at 80° C. to obtain a water phase material;

[0129] 2) Add the oil and emulsifier into a container and mix them evenly while stirring at 80° C. to obtain the oil phase material;

[0130] 3) Add the oil phase material to the water phase material at 85° C. while stirring, and mix for 35 minutes; then cool to 40° C., add the preservative, and stir evenly to obtain the white tea fermentation filtrate cosmetic.

[0131] Raw material information involved in each embodiment:

[0132] Ganoderma lucidum slant block: The strain is provided by Shanghai Baolong Zhongcheng Technology Co., Ltd. (deposited in China General Microbiological Culture Collection Center CGMCC, deposit number NO: 30854). It is a strain identified by the Edible Fungi Center of the Institute of Agricultural Resources and Agricultural Zoning, Chinese Academy of Agricultural Sciences. It is mainly used for health care and medicine and is suitable for liquid fermentation.

[0133] Experimental data:

[0134] 1. Test of related properties of white tea fermentation filtrate

[0135] Comparative Example 1:

[0136] The difference between this comparative example and Example 1 is that the solid-liquid ratio of ultrasonic extraction in step (1) of preparing white tea fermentation filtrate is 1:100.

[0137] Comparative Example 2:

[0138] The difference between this comparative example and Example 1 is that the fermentation temperature of step (3) of preparing white tea fermentation filtrate is 20°C.

[0139] Comparative Example 3:

[0140] The difference between this comparative example and Example 1 is that the fermentation pH value of step (3) of preparing the white tea fermentation filtrate is 4.2.

[0141] Comparative Example 4:

[0142] The difference between this comparative example and Example 1 is that a white tea extract is prepared instead of a white tea fermentation filtrate, and the steps only include step (1) and do not include steps (2) to (4).

[0143] (I) Determination of appearance, odor, polyphenol content, and flavonoid content

[0144] Determination of white tea polyphenol content: ammonium molybdate spectrophotometry (reference Liao Xiaoling, Lang Huiyun, Xu Wenfeng, Shen Yehua. Determination of tea polyphenols in green tea by ammonium molybdate spectrophotometry. Analytical Laboratory. DOI: 10.3969 / j.issn.1000-0720.2003.05.020);

[0145] Determination of total flavonoids content: spectrophotometry, detection wavelength 504nm (reference He Shumei, Liu Jinglan. Research on the determination method of total flavonoids content in tea [J / OL]. Analytical Chemistry. DOI: 10.3321 / j.issn:0253-3820.2007.09.028).

[0146] The results are shown in Table 1. Figure 1-2 :

[0147] Figure 1 This is the appearance of the white tea extract prepared in Comparative Example 4. Figure 2 This is the appearance of the white tea fermentation filtrate prepared in Example 1 of this case.

[0148] Table 1 Determination results of appearance, odor, polyphenol content and total flavonoid content

[0149] Group Appearance odor Polyphenol content Total flavonoids content Example 1 Brown transparent liquid Slight fermentation characteristic smell 2.34mg / mL 1.88mg / mL Example 2 Brown transparent liquid Slight fermentation characteristic smell 2.18mg / mL 1.70mg / mL Example 3 Brown transparent liquid Slight fermentation characteristic smell 2.23mg / mL 1.76mg / mL Example 4 Brown transparent liquid Slight fermentation characteristic smell 2.23mg / mL 1.82mg / mL Comparative Example 1 Light yellow transparent liquid Slight fermentation characteristic smell 1.68mg / mL 1.28mg / mL Comparative Example 2 Light yellow transparent liquid Slight fermentation characteristic smell 1.39mg / mL 1.34mg / mL Comparative Example 3 Light yellow transparent liquid Slight fermentation characteristic smell 1.55mg / mL 1.27mg / mL Comparative Example 4 Light yellow transparent liquid Characteristic smell 1.25mg / mL 1.31mg / mL

[0150] According to the data in Table 1, Figure 1-2 It can be seen that the white tea fermentation filtrate obtained by the preparation method and preferred process parameters of each embodiment of the present invention has a higher content of polyphenols and total flavonoids, which provides a certain material basis for its excellent skin care effects in terms of moisturizing, anti-oxidation, anti-wrinkle, anti-photoaging, and brightening.

[0151] (II) Tests on DPPH free radical scavenging rate, elastase inhibition rate, cell photoaging and irritation

[0152] Sample pretreatment: First, the samples to be tested in Examples 1-4 and Comparative Examples 1-4 were dissolved with 5‰ DMSO (v / v), and then filtered with a 0.22 μm filter membrane. After filtration, the samples were used as the mother solutions to be tested in Examples 1-4 and Comparative Examples 1-4.

[0153] DPPH scavenging experiment: According to the "Cosmetics-Free Radical (DPPH) Scavenging Experiment Method (T / SHRH006-2018)", the DPPH free radical scavenging rate (%) of the products prepared in the above Examples 1-4 and Comparative Examples 1-4 and the blank control group was tested respectively.

[0154] Calculation method of clearance rate: Clearance rate (%) = [(A1-A2) / A1]*100%, A1 is the absorbance of the control group, A2 is the absorbance of the sample.

[0155] Elastase inhibition assay:

[0156] Elastase was used as the research object. It was divided into a sample group (example sample and comparative sample) and a blank control group. Each sample was made in 3 parallels, and 10 μL of the sample to be tested was added to a 96-well plate, and then 20 μL of elastase with a concentration of 0.1 U / mL was added. The 96-well plate was placed in a 25°C constant temperature incubator for 15 minutes, and then 50 μL of a substrate with a concentration of 1 mg / mL (98% N-succinyl-alanine-alanine-alanine-p-nitroaniline) was added, and the absorbance of the sample at a wavelength of 410 nm was measured using an ELISA reader, and the inhibition rate of the sample to be tested on the activity of elastase was calculated.

[0157] Elastase activity inhibition rate (%) = [(A1-A2) / A1]*100%, A1 represents the absorbance value of the blank control, and A2 represents the absorbance value of the sample.

[0158] The higher the elastase inhibition rate, the better the anti-wrinkle effect of the product.

[0159] Cell photoaging test:

[0160] HaCaT cells (2*104 per well) were inoculated in a 96-well plate and cultured overnight in an incubator. When the HaCaT cells reached about 60% confluence, each group of samples was diluted to a concentration of 5% with complete culture medium. The old culture medium was discarded, and complete culture medium without sample was added to the untreated group and UVA group. 100 μL of cell culture medium containing 5% sample concentration was added to each well of the drug-treated group, and culture was continued for 4 hours.

[0161] Establishment of photoaging HaCaT cell model: discard the old culture medium, wash once with PBS, add 50uL PBS to each well to cover the cells, irradiate with UVA (UVA ultraviolet light wavelength 320-400nm, peak at 368nm), irradiation dose of 15J / cm2, and cover the blank control group with tin foil. After irradiation, aspirate PBS, add 100μL serum-free DMEM culture medium to each well, and return to the incubator to continue culturing for 24h.

[0162] Detect the protective effect of the sample on photoaged HaCaT cells: discard the old culture medium, wash once with PBS, add 100uL of DMEM culture medium containing 10% CCK-8 to each well, incubate at 37℃ for 1.5h, and detect the OD value at 450nm with a microplate reader. The blank control group does not contain cells, and only 100ul of 10% CCK-8 working solution is added during the detection.

[0163] Cell survival rate (%) = 100%*(OD experimental group-OD blank control group) / (OD untreated group-OD blank control group).

[0164] The higher the cell survival rate, the better the anti-photoaging effect of the product.

[0165] Irritation test:

[0166] The products obtained in Examples 1-4 and Comparative Examples 1-4 were subjected to multiple skin irritation tests according to the method of Chapter 6.4 of the "Technical Specification for Safety of Cosmetics" (2015 Edition), and the acute eye irritation test was carried out according to the method of Chapter 6.5 of the "Technical Specification for Safety of Cosmetics" (2015 Edition).

[0167] The test results are shown in Table 2 and Figure 3-5 :

[0168] Table 2 Test results of DPPH free radical scavenging rate, elastase inhibition rate, cell photoaging and irritation

[0169]

[0170]

[0171] Among them, “-” in the table means not measured.

[0172] From Table 2 and Figure 3-5 It can be seen from the data that the white tea fermentation filtrate obtained by the preparation method of each embodiment of the present invention has excellent antioxidant, anti-wrinkle and anti-photoaging effects, and its preferred preparation process conditions and ratios can affect the above effects.

[0173] 2. Performance test of white tea fermentation filtrate application products (cosmetics prepared with white tea fermentation filtrate)

[0174] Application Comparative Example 1: The difference between this application comparative example 1 and Example 1 is that the white tea fermentation filtrate is replaced by the white tea extract of comparative example 4;

[0175] Placebo: A blank control, that is, no white tea fermentation filtrate or white tea extract is added to the raw materials.

[0176] Table 3 Ratio system of application example 1 and placebo

[0177]

[0178] The preparation method of Comparative Example 1 was applied according to Example 1.

[0179] Preparation method of placebo: The difference from Example 1 is that in step (1), the white tea extract of Comparative Example 4 is used to replace the white tea fermentation filtrate.

[0180] (I) Human efficacy test

[0181] Test method:

[0182] (1) Test subjects: A total of 120 volunteers aged 25-35 years were randomly divided into 6 groups.

[0183] (2) Usage: After cleansing the face every morning and evening, use equal amounts of skin care essence and massage until completely absorbed. Twice a day, once in the morning and once in the evening. Test once in week 0 and once in week 4. Do not use any other skin care products during the test to avoid interfering with the test results. (3) Test instrument: Before the test, the volunteers sit quietly in the room for 30 minutes, and use the VISIA full face analyzer to take test pictures. The instrument analyzes the changes in facial wrinkles. Use a skin tester to test skin indicators (brightness, moisture content, transepidermal water loss), compare the test results with the aforementioned initial skin indicators, and obtain the corresponding change rates (skin brightness change rate, skin moisture content change rate, transepidermal water loss change rate) as shown in Table 4.

[0184] The test results are shown in Table 4. Figure 6-9 As shown:

[0185] Table 4 Human efficacy test results

[0186]

[0187] Among them, positive values ​​indicate an increase in value, and negative values ​​indicate a decrease in value.

[0188] From Table 4 and Figure 6-9The data show that: the number of skin wrinkles of the subjects using the skin care essence of the product of the present invention is reduced. Compared with the placebo, the skin wrinkle change rate of Examples 1-4 is at least reduced by 6.5%, and can be reduced by up to 8.6%. Compared with the placebo, the skin wrinkle change rate of Comparative Example 1 is reduced by an average of 2.8%, and the effect of Comparative Example 1 is significantly inferior to that of Examples 1-4; the skin brightness of the subjects using the skin care essence of the product of the present invention is increased. Compared with the placebo, the skin brightness change rate is increased by at least 3.1%, and can be increased by up to 3.8%. Compared with the placebo, the skin brightness change rate of Comparative Example 1 is increased by an average of 1.0%, and the effect of Comparative Example 1 is significantly inferior to that of Examples 1-4; the skin moisture content of the subjects using the skin care essence of the product of the present invention is increased, and compared with the placebo, the skin moisture content of the subjects using the skin care essence of the product of the present invention is increased. Compared with the placebo, the skin moisture content change rate of comparative example 1 increased by at least 9.1%, and could increase by up to 11.5%. Compared with the placebo, the skin moisture content change rate of comparative example 1 increased by an average of 2.7%, and the effect of comparative example 1 was significantly inferior to that of examples 1-4; for the subjects using the skin care essence of the product of the present invention, the skin transepidermal moisture was reduced, and compared with the placebo, the transepidermal water loss rate change rate was reduced by at least 11.1%, and could be reduced by up to 13.5%. Compared with the placebo, the skin moisture content change rate of comparative example 1 was reduced by an average of 3.4%, and the effect of comparative example 1 was significantly inferior to that of examples 1-4; it can be seen that the cosmetics (essence) prepared from the white tea fermentation filtrate prepared by the preparation method and process parameters of the present case have significant wrinkle removal, brightening, moisturizing and repairing effects.

Claims

1. A method for preparing white tea fermentation filtrate, characterized in that: The steps are as follows: (1) The dried white tea is subjected to air flow ultrafine grinding and sieved through 380-420 meshes, a 20% mass percentage concentration of butanediol aqueous solution is added, the mixture is mixed at a material-liquid ratio of 1:20-30, and ultrasonic extraction is performed at 30-35° C. and an ultrasonic power of 180-220 W for 60-120 min; and then filtered through 350-450 meshes to obtain a white tea extract; (2) inoculating the Ganoderma lucidum slant block into a sterilized liquid culture medium, and culturing in a shaker at 28-32° C. and a rotation speed of 100-200 rpm for 3-5 days to obtain Ganoderma lucidum seed liquid; The liquid culture medium is prepared by adding 18-22 g of glucose, 11-18 g of malt extract powder, 3-8 g of corn steep liquor, 0.1-3 g of yeast extract powder and 0.5-3 g of peptone to each liter of water; (3) sterilizing and cooling the white tea extract obtained in step (1), mixing it evenly with the ganoderma lucidum seed solution obtained in step (2) and the liquid culture medium in step (2) at a volume ratio of 800-1000:10-100:20-100, and fermenting it at 30-40° C. and a pH value of 5.0-7.0 for 48-96 hours to obtain a white tea fermentation product; (4) sterilizing the white tea fermentation product obtained in step (3), cooling it, and filtering it to obtain a white tea fermentation filtrate.

2. The method for preparing white tea fermentation filtrate according to claim 1, characterized in that: The air flow ultrafine grinding in step (1) is carried out under nitrogen protection, and the specific conditions are: air pressure 0.5-1.0 MPa, system air volume 2.0-4.0 m3 / min, classifier speed 2500-4000 r / min, and feeding rate 3.0-5.0 kg / h.

3. The method for preparing white tea fermentation filtrate according to claim 1, characterized in that: The wet weight content of Ganoderma lucidum mycelium in the Ganoderma lucidum seed liquid obtained in step (2) is 5-15 g / L.

4. The method for preparing white tea fermentation filtrate according to claim 1, characterized in that: The filtration in step (4) is performed using a 1-5 μm filter membrane.

5. The method for preparing white tea fermentation filtrate according to claim 1, characterized in that: The sterilization conditions of the liquid culture medium in step (2) and the white tea fermentation product in step (4) are both: sterilization at 115-121° C. for 15-30 min.

6. The method for preparing white tea fermentation filtrate according to claim 1, characterized in that: The white tea is Fuding Baihao Yinzhen.

7. A white tea fermentation filtrate product, characterized in that: The white tea fermentation filtrate product is a white tea fermentation filtrate cosmetic prepared using the white tea fermentation filtrate according to any one of claims 1 to 6, and the white tea fermentation filtrate cosmetic is mainly prepared from the following components in the following mass proportions:

8. The white tea fermentation filtrate product according to claim 7, characterized in that: The polyol is one of 1,3-butylene glycol, 1,3-propylene glycol or glycerol or any combination of any two or more thereof, and the thickener is xanthan gum or carbomer.

9. The white tea fermentation filtrate product according to claim 7, characterized in that: The oil is one of white oil, caprylic / capric triglyceride, squalane, cetearyl alcohol or beeswax, or any combination of any two or more thereof; the emulsifier is one of polyglycerol fatty acid ester or glyceryl stearate / PEG-100 stearate, or any combination of any two thereof.

10. The method for preparing the white tea fermentation filtrate product according to claim 7, characterized in that: The steps are as follows: 1) adding white tea fermentation filtrate, polyol, thickener and water into a container and mixing them evenly at 80-85° C. to obtain a water phase material; 2) Add the oil and emulsifier into a container, mix them evenly while stirring at 80-95° C. to obtain the oil phase material; 3) Adding the oil phase material to the water phase material at 80-85° C. while stirring, and mixing for 25-35 minutes; then cooling to 40-45° C., adding a preservative, and stirring evenly to obtain white tea fermentation filtrate cosmetics.

Citation Information

Patent Citations

  • White tea extract and preparation method and application thereof

    CN106726898A