A kind of Poria cocos extract and its preparation method and application

Abstract

The present invention discloses a Poria cocos extract and a preparation method and application thereof. The Poria cocos extract is a mixture, which contains a water extract obtained by water extraction of Poria cocos and an alkali extract obtained by alkali extraction of Poria cocos residue after water extraction. The Poria cocos extract of the present invention contains Poria cocos alkali-soluble polysaccharides and Poria cocos water-soluble extract (including water-soluble polysaccharides) at the same time. The preparation method thereof is simple and easy, and has the effects of synergistic moisturizing and oil control (reducing skin oil secretion). The extract can be used as a moisturizing and oil control component in daily chemical products, and has broad application prospects.

Description

Technical Field

[0001] The invention relates to a Chinese herbal medicine extract, in particular to a Poria cocos extract, and also to a preparation method of the Poria cocos extract and application of the Poria cocos extract in the field of daily chemical products. Background Art

[0002] Poria cocos is a traditional Chinese herbal medicine with a history of more than 2,000 years in my country. It is an important component of many Chinese patent medicines and prescriptions, and was called "the magic medicine of the four seasons" by the ancients. Poria cocos is the dried sclerotium of the fungus Poria cocos (Schw.) Wolf of the Polyporaceae family. Chinese medicine believes that Poria cocos tastes sweet, light, and flat, and it enters the heart, spleen, and kidney meridians. It has the effects of promoting water and eliminating dampness, strengthening the spleen and calming the heart. It is mainly used clinically to treat symptoms such as edema and oliguria, phlegm and fluid, dizziness and palpitations, spleen deficiency and poor appetite, loose stools and diarrhea, restlessness, palpitations, and insomnia.

[0003] For decades, domestic and foreign scholars have conducted many studies on the effective components of Poria cocos. Literature reports show that Poria cocos contains a variety of chemical components, mainly triterpenes, polysaccharides, diterpenes and sterols, in addition to other compounds such as amino acids and fatty acids. Among them, the biologically active compounds are mainly concentrated in triterpenes and polysaccharides. Most of the triterpenes are tetracyclic triterpenes. Polysaccharides account for about 80% of the dry sclerotium of Poria cocos and are the main components of Poria cocos. They can be divided into water-soluble and alkali-soluble according to their solubility. Under normal circumstances, alkali-soluble polysaccharides are difficult to use, do not dissolve under acidic and neutral conditions, and only dissolve under alkaline conditions.

[0004] Poria cocos extract has good anti-inflammatory, whitening, moisturizing and antioxidant effects. It is used in cosmetics to moisturize the skin and prolong the life.

[0005] At present, Poria extract mainly refers to Poria polysaccharide, which includes simple alkali-soluble polysaccharide, simple water-soluble polysaccharide (Patent CN 114146019 A extracts Poria water-soluble polysaccharide and shows its application in anti-ultraviolet) or Poria total polysaccharide (Patent CN 114292346 A prepares Poria total polysaccharide, which is alkaline Poria polysaccharide and polysaccharide surface attachment obtained after alcohol washing, alkali dissolution and acid precipitation). These methods discard the initial water-soluble extract (content of about 15.516~41.107 mg·g-1) and alcohol-soluble extract (content of about 25.683~90.000 mg·g-1) of Poria [data referenced from "Study on Microscopic Quantification of Poria and Its Correlation with Active Ingredients of Medicinal Materials"]. The components in the extract are relatively single, resulting in a certain waste of Poria resources and loss of efficacy of Poria extract. Summary of the invention

[0006] The purpose of the present invention is to provide a Poria cocos extract, which is a mixture containing Poria cocos alkali-soluble polysaccharides and Poria cocos water-soluble extracts (including water-soluble polysaccharides and total triterpenes). The Poria cocos extract has significant effects of moisturizing and reducing skin oil secretion, and has better application prospects in daily chemical products.

[0007] The Poria cocos extract of the present invention contains both Poria cocos water extract and Poria cocos alkali extract, wherein the Poria cocos water extract is a water extract obtained by water extraction of Poria cocos, and the Poria cocos alkali extract is an alkali extract obtained by alkali extraction of Poria cocos residue after water extraction using Poria cocos residue as a raw material. The Poria cocos water extract contains Poria cocos water-soluble extracts, such as water-soluble Poria cocos polysaccharides and total triterpenes, and the main component of the Poria cocos alkali extract is alkali-soluble Poria cocos polysaccharides.

[0008] Furthermore, the Poria water extract is the filtrate obtained by filtering the Poria cocos after extracting the Poria cocos with water once or multiple times, and the alkaline extract is prepared by first dissolving the Poria cocos residue after the Poria cocos water extraction with a sodium hydroxide solution, and then precipitating the dissolved liquid part with alcohol, and the obtained alcohol precipitate is the Poria cocos alkaline extract.

[0009] Further, when preparing the Poria cocos water extract, the extraction steps and process conditions can be used in the manner disclosed in the prior art, for example, the number of extractions can be once, twice or more than twice, and if it is multiple times, the water extracts can be combined and then concentrated to ensure the concentration of water-soluble components. In the final Poria cocos extract, the mass ratio of Poria cocos water extract to Poria cocos powder is 100:1-5. The extraction temperature can be 60°C-80°C, for example, the extraction can be carried out under oscillation, ultrasound or stirring to improve the extraction efficiency, for example, the extraction time is generally 4-6h, so that the water-soluble polysaccharide fully enters the water extract. In addition, in order to better precipitate the components in Poria cocos, Poria cocos powder is generally used as a raw material. Preferably, the mass ratio of Poria water extract to Poria powder can be 100:1, 100:1.5, 100:2, 100:2.5, 100:3, 100:3.5, 100:4, 100:4.5, 100:5; the extraction temperature can be 60°C, 61°C, 62°C, 63°C, 64°C, 65°C, 66°C, 67°C, 68°C, 69°C, 70°C, 71°C, 72°C, 73°C, 74°C, 75°C, 76°C, 77°C, 78°C, 79°C, 80°C.

[0010] Furthermore, when preparing the tuckahoe alkali extract, the raw material used is the tuckahoe dregs remaining after preparing the tuckahoe water extract. The tuckahoe dregs obtained after preparing the tuckahoe water extract once or multiple times are collected and used for the preparation of the tuckahoe alkali extract. The tuckahoe dregs are first fully dissolved with a 1-2wt% sodium hydroxide solution, and then the insoluble matter is filtered, and the remaining filtrate is added with alcohol for alcohol precipitation. The mass ratio of the sodium hydroxide solution to the tuckahoe dregs is 50:1-5, and the alcohol used for alcohol precipitation is generally ethanol, and the amount of ethanol used ensures that the concentration of alcohol in the filtrate is 55-70wt%. Preferably, the mass ratio of sodium hydroxide solution to Poria cocos residue can be 50:1, 50:1.5, 50:2, 50:2.5, 50:3, 50:3.5, 50:4, 50:2.5, 50:5; the concentration of ethanol in the filtrate can be 55 wt%, 56 wt%, 57 wt%, 58 wt%, 59 wt%, 60 wt%, 61 wt%, 62 wt%, 63 wt%, 64 wt%, 65 wt%, 66 wt%, 67wt%, 68 wt%, 69 wt%, 70wt%.

[0011] Further, in the Poria extract, the alkali extract (mainly alkali-soluble Poria polysaccharide) is suspended in the Poria water extract in the form of spherical small particles, and the Poria extract as a whole is in the state of a suspension. The spherical alkali extract can be formed by mixing the alkali extract with the water extract, then adding an appropriate amount of sodium hydroxide solution to completely dissolve the alkali extract in the water extract, and then adjusting the system pH to 6-8 with acid, at which time the alkali extract (mainly alkali-soluble Poria polysaccharide) will precipitate from the water extract in the form of spherical small particles and suspend in the water extract. Preferably, the pH can be 6.0, 6.5, 7.0, 7.5, 8.0.

[0012] Further, in the Poria cocos extract, the content of the alkaline extract in the Poria cocos water extract is 0.1-3wt%, for example, 0.1wt%, 0.5wt%, 1wt%, 1.5wt%, 2wt%, 2.5wt%, 3wt%, preferably 1 wt%.

[0013] In a specific embodiment of the present invention, a specific method for preparing a Poria cocos extract is provided, and the specific steps of the preparation method include:

[0014] (1) extracting the Poria powder with water, filtering after extraction to obtain a water extract, and using the filtered residue for later use;

[0015] (2) dissolving the filter residue fully with a sodium hydroxide solution, and then filtering to obtain an alkaline filtrate;

[0016] (3) adding alcohol to the alkaline filtrate for alcohol precipitation, washing the obtained precipitate with alcohol and drying it to obtain an alkaline extract;

[0017] (4) The water extract and the alkaline extract are mixed, and then sodium hydroxide solution is added to ensure that the alkaline extract is completely dissolved in the water extract. After the alkaline extract is completely dissolved, acid is added to adjust the pH to 6.0-8.0 so that the alkaline extract is suspended in the solution in the form of small spherical particles to obtain the Poria cocos extract.

[0018] Furthermore, in step (1), the Poria cocos sclerotia (i.e., Poria cocos pieces) can be sliced, powdered, and sieved to obtain Poria cocos powder. The Poria cocos used in the present invention can be shade-dried Poria cocos pieces or a dried product after steaming.

[0019] Furthermore, in step (1), the mass ratio of Poria powder to water is 1-5:100, the extraction temperature is 60°C-80°C, the extraction is carried out under shaking, ultrasound or stirring, and the extraction time is 4-6 hours. Preferably, the Poria powder is extracted once with water.

[0020] Furthermore, in step (1), the Poria residue obtained from preparing a single Poria water extract can be used to prepare the alkaline extract, the Poria residues obtained from multiple Poria water extracts can be combined together to prepare the alkaline extract, and a portion of the Poria residue obtained from a single Poria extract can be used to prepare the alkaline extract.

[0021] Furthermore, in step (2), the concentration of the sodium hydroxide solution is 1-2 wt %, and the mass ratio of the sodium hydroxide solution to the Poria cocos residue is 50:1-5.

[0022] Furthermore, in step (3), the alcohol precipitation is forward alcohol precipitation, and ethanol or other alcohol is added to the alkaline filtrate until the alcohol concentration is 55-70wt%.

[0023] Furthermore, in step (4), the concentration of the alkali extract in the water extract is 0.1-3wt%, specifically 0.1wt%, 0.2wt%, 0.3wt%, 0.4wt%, 0.5wt%, 0.6wt%, 0.7wt%, 0.8wt%, 0.9wt%, 1.0wt%, 1.1wt%, 1.2wt%, 1.3wt%, 1.4wt%, 1.5wt%, 1.6wt%, 1.7wt%, 1.8wt%, 1.9wt%, 2.0wt%, 2.1wt%, 2.2wt%, 2.3wt%, 2.4wt%, 2.5wt%, 2.6wt%, 2.7wt%, 2.8wt%, 2.9wt%, and 3.0wt%.

[0024] Furthermore, in step (4), the concentration of the sodium hydroxide solution is 1-2 wt %, and the acid used can be phosphoric acid, hydrochloric acid, acetic acid, lactic acid, citric acid, etc. Various acids have similar effects in the present invention.

[0025] Furthermore, in step (4), the Poria cocos extract finally obtained contains both Poria cocos water extract (including water-soluble Poria cocos polysaccharides and total triterpenes) and alkali-soluble Poria cocos polysaccharides, and the Poria cocos extract is a suspension containing small polysaccharide particles.

[0026] The Poria extract of the present invention retains the natural active substances in Poria to a large extent, and no other organic solvents are added except ethanol during the preparation of the extract, so it is highly safe and has no irritating byproducts, and can be used in daily chemical products. It has been verified that the Poria extract has excellent moisturizing and oil-controlling effects, can significantly increase the water content of the skin, reduce transepidermal water loss, and reduce oil secretion on the skin surface. Compared with simple alkali-soluble Poria polysaccharides and water-soluble Poria polysaccharides, it has better application prospects in the field of daily chemical products.

[0027] The present invention also provides the use of the Poria cocos extract as a moisturizing component and a skin oil-controlling component, especially as a moisturizing component and a skin oil-controlling component in daily chemical products.

[0028] The invention also provides a composition, comprising the Poria cocos extract.

[0029] Further, the above-mentioned Poria extract can be used as a moisturizing and oil-controlling ingredient in the composition. The amount of Poria extract added to the composition can be 1-20wt%, such as 1wt%, 2wt%, 3wt%, 4wt%, 5wt%, 6wt%, 7wt%, 8wt%, 9wt%, 10wt%, 11wt%, 12wt%, 13wt%, 14wt%, 15wt%, 16wt%, 17wt%, 18wt%, 19wt%, 20wt%, preferably 2-10wt%. It has been verified by experiments that within this addition range, it is safe and non-toxic.

[0030] Furthermore, the composition can be various types of daily chemical products, such as cosmetics, toothpaste, etc.

[0031] Furthermore, the cosmetics may be lotions, skin care lotions, skin care creams, essences, eye creams, facial masks, soaps, facial cleansers, shower gels, aerosols, sprays, shampoo products, hair care products, etc.

[0032] The present invention has the following advantages:

[0033] 1. The Poria cocos extract of the present invention contains both Poria cocos alkali-soluble polysaccharides and Poria cocos water-soluble extracts (including water-soluble polysaccharides and total triterpenes). The preparation method is simple and easy, and has synergistic moisturizing and oil-controlling (reducing skin oil secretion) effects. It can be used as a moisturizing and oil-controlling ingredient in daily chemical products, and has better application prospects in daily chemical products.

[0034] 2. The present invention obtains the Poria cocos extract through an improved extraction method, which fully utilizes the effective ingredients in the Poria cocos, not only improves the utilization rate of the Poria cocos, enriches the effective ingredients and product efficacy of the Poria cocos extract, but also reduces the water consumption in the preparation process of the Poria cocos extract, reduces the preparation cost and the amount of wastewater treatment.

[0035] 3. The present invention adopts a special processing method to make the alkaline extract in the Poria cocos extract stably suspended in the water extract in the form of spherical particles, so that the water-soluble components and alkaline-soluble components of Poria cocos can stably exist in one system. It not only has synergistic moisturizing and oil-control effects, but can also be directly added to daily chemical products as an effective ingredient, which is easy to use. DETAILED DESCRIPTION

[0036] The present invention is further described below in conjunction with examples, but the present invention is not limited by the following examples, wherein the Poria cocos used in the experiment is the traditional Chinese medicine Poria cocos (produced in Anhui).

[0037] In the following examples, unless otherwise specified, the concentrations are all in mass percentage.

[0038] Example 1 Preparation of Poria cocos extract

[0039] 1. Take the naturally sweated and shade-dried Poria cocos, slice it, dry it at 40℃ until the water content is less than 4%, then crush it, sieve it, and collect the Poria cocos powder. Weigh the Poria cocos powder, add 1L of purified water to make a Poria cocos slurry with a Poria cocos powder content of 1wt%.

[0040] 2. Extract the Poria slurry at 60°C and 200 rpm for 4 h, and collect the water filtrate (save for later use) and the filter residue.

[0041] 3. Dissolve the filter residue with 0.5L of 1% NaOH solution and stir to fully dissolve it; after dissolution, filter through a 0.8-micron filter membrane to collect the alkali-soluble filtrate; add ethanol (to an ethanol concentration of 55%) to the alkali-soluble filtrate for forward alcohol precipitation, let it stand and collect the precipitate after alcohol precipitation, wash the precipitate with an equal amount of ethanol, collect the precipitate (mainly alkali-soluble polysaccharides), and dry it in vacuo at 30°C to obtain the alkali extract.

[0042] 4. Add the dried alkali extract to the water extract filtrate obtained in step 2, the amount of the alkali extract added to the water extract filtrate is 1% of the water extract filtrate, and in order to promote the complete dissolution of the alkali extract, add an appropriate 1% NaOH solution. After the alkali extract is completely dissolved, add phosphoric acid to adjust the pH value to 6. The alkali-soluble polysaccharides in the alkali extract are precipitated in the form of small spherical particles and suspended in the solution. The final suspension is the Poria cocos extract.

[0043] Example 2 Preparation of Poria cocos extract

[0044] 1. Take the steamed Poria cocos, slice it, dry it at 40℃ until the water content is less than 4%, then crush it, sieve it, and collect the Poria cocos powder. Weigh the Poria cocos powder, add 1L of purified water to make a Poria cocos slurry with a Poria cocos powder content of 1wt%.

[0045] 2. Extract the Poria slurry at 60°C and 200 rpm for 4 h, and collect the water filtrate (save for later use) and the filter residue.

[0046] 3. Dissolve the filter residue with 0.5L 1% NaOH solution and stir to fully dissolve it; after dissolution, filter through a 0.8-micron filter membrane to collect the alkali-soluble filtrate; add ethanol (to an ethanol concentration of 63%) to the alkali-soluble filtrate for forward alcohol precipitation, let it stand and collect the precipitate after alcohol precipitation, wash the precipitate with an equal amount of ethanol, collect the precipitate (mainly alkali-soluble polysaccharides), and dry it in vacuo at 30°C to obtain the alkali extract.

[0047] 4. Add the dried alkali extract to the water extract filtrate obtained in step 2, the amount of the alkali extract added is 1% of the water extract filtrate, and in order to promote the complete dissolution of the alkali extract, add a 1% NaOH solution of appropriate concentration, and after the alkali extract is completely dissolved, add phosphoric acid to adjust the pH value to 7, and the alkali-soluble polysaccharides in the alkali extract are precipitated in the form of small spherical particles and suspended in the solution. The final suspension is the Poria cocos extract.

[0048] Example 3 Preparation of Poria cocos extract

[0049] 1. Take the naturally sweated and shade-dried Poria cocos, slice it, dry it at 40℃ until the water content is less than 4%, then crush it, sieve it, and collect the Poria cocos powder. Weigh the Poria cocos powder, add 1L of purified water to make a Poria cocos slurry with a Poria cocos powder content of 5wt%.

[0050] 2. Extract the Poria slurry at 80°C and 200 rpm for 6 h, and collect the water filtrate (save for later use) and the filter residue.

[0051] 3. Dissolve the filter residue with 0.5L of 1% NaOH solution and stir to fully dissolve it; after dissolution, filter through a 0.8-micron filter membrane to collect the alkali-soluble filtrate; add ethanol (to an ethanol concentration of 70%) to the alkali-soluble filtrate for forward alcohol precipitation, let it stand and collect the precipitate after alcohol precipitation, wash the precipitate with an equal amount of ethanol, collect the precipitate (mainly alkali-soluble polysaccharides), and dry it in a vacuum at 30°C to obtain the alkali extract.

[0052] 4. Add the dried alkali extract to the water extract filtrate obtained in step 2, the amount of the alkali extract added is 1% of the water extract filtrate, and in order to promote the complete dissolution of the alkali extract, add a 1% NaOH solution of appropriate concentration, and after the precipitate is completely dissolved, add phosphoric acid to adjust the pH value to 8, and the alkali-soluble polysaccharides in the alkali extract are precipitated in the form of small spherical particles and suspended in the solution. The final suspension is the Poria cocos extract.

[0053] Example 4 Preparation of Poria cocos extract

[0054] 1. Take the naturally sweated and shade-dried Poria cocos, slice it, dry it at 40℃ until the water content is less than 4%, then crush it, sieve it, and collect the Poria cocos powder. Weigh the Poria cocos powder, add 1L of purified water to make a Poria cocos slurry with a Poria cocos powder content of 1wt%.

[0055] 2. Extract the Poria slurry at 60°C and 200 rpm for 4 h, and collect the water filtrate (save for later use) and the filter residue.

[0056] 3. Dissolve the filter residue with 0.5L of 1% NaOH solution and stir to fully dissolve it; after dissolution, filter through a 0.8-micron filter membrane to collect the alkali-soluble filtrate; add ethanol (to an ethanol concentration of 55%) to the alkali-soluble filtrate for forward alcohol precipitation, let it stand and collect the precipitate after alcohol precipitation, wash the precipitate with an equal amount of ethanol, collect the precipitate (mainly alkali-soluble polysaccharides), and dry it in vacuo at 30°C to obtain the alkali extract.

[0057] 4. Add the dried alkali extract to the water extract filtrate obtained in step 2, the amount of the alkali extract added to the water extract filtrate is 0.1% of the water extract filtrate, and in order to promote the complete dissolution of the alkali extract, add an appropriate 1% NaOH solution. After the alkali extract is completely dissolved, add phosphoric acid to adjust the pH value to 6. The alkali-soluble polysaccharides in the alkali extract are precipitated in the form of small spherical particles and suspended in the solution. The final suspension is the Poria cocos extract.

[0058] Example 5 Preparation of Poria cocos extract

[0059] 1. Take the naturally sweated and shade-dried Poria cocos, slice it, dry it at 40℃ until the water content is less than 4%, then crush it, sieve it, and collect the Poria cocos powder. Weigh the Poria cocos powder, add 1L of purified water to make a Poria cocos slurry with a Poria cocos powder content of 1wt%.

[0060] 2. Extract the Poria slurry at 60°C and 200 rpm for 4 h, and collect the water filtrate (save for later use) and the filter residue.

[0061] 3. Dissolve the filter residue with 0.5L of 1% NaOH solution and stir to fully dissolve it; after dissolution, filter through a 0.8-micron filter membrane to collect the alkali-soluble filtrate; add ethanol (to an ethanol concentration of 55%) to the alkali-soluble filtrate for forward alcohol precipitation, let it stand and collect the precipitate after alcohol precipitation, wash the precipitate with an equal amount of ethanol, collect the precipitate (mainly alkali-soluble polysaccharides), and dry it in vacuo at 30°C to obtain the alkali extract.

[0062] 4. Add the dried alkali extract to the water extract filtrate obtained in step 2, the amount of the alkali extract added to the water extract filtrate is 3% of the water extract filtrate, and in order to promote the complete dissolution of the alkali extract, add an appropriate 1% NaOH solution. After the alkali extract is completely dissolved, add phosphoric acid to adjust the pH value to 6. The alkali-soluble polysaccharides in the alkali extract are precipitated in the form of small spherical particles and suspended in the solution. The final suspension is the Poria cocos extract.

[0063] Comparative Example 1 Preparation of Poria cocos extract (water extract)

[0064] 1. Take the naturally sweated and shade-dried Poria cocos, slice it, dry it at 40℃ until the water content is less than 4%, then crush it, sieve it, and collect the Poria cocos powder. Weigh the Poria cocos powder, add 1L of purified water to make a Poria cocos slurry with a Poria cocos powder content of 1wt%.

[0065] 2. Extract the Poria cocos slurry at 60°C and 200 rpm for 4 h, and collect the water filtrate, which is the Poria cocos extract (water extract).

[0066] Comparative Example 2 Preparation of Poria cocos extract (alkali-soluble polysaccharide)

[0067] 1. Take the naturally sweated and shade-dried Poria cocos, slice it, dry it at 40℃ until the water content is less than 4%, then crush it, sieve it, and collect the Poria cocos powder. Weigh the Poria cocos powder, add purified water to make up to volume, and prepare 1L of Poria cocos slurry with a dry matter content of 1wt% of Cistanche deserticola.

[0068] 2. Extract the Poria slurry at 60°C and 200 rpm for 4 h, and collect the aqueous residue.

[0069] 3. Dissolve the filter residue with 0.5L 1% NaOH solution and stir to fully dissolve; after dissolution, filter through a 0.8 micron filter membrane to collect the alkali-soluble filtrate; add ethanol (to an ethanol concentration of 55%) to the alkali-soluble filtrate for positive alcohol precipitation: after alcohol precipitation, let it stand and collect the alcohol precipitate, add an equal amount of ethanol, wash it once with alcohol, and collect the precipitate (alkali-soluble polysaccharide); the obtained precipitate is vacuum dried at 30°C;

[0070] 4. Precipitation dissolution: Redissolve the dried alcohol precipitate with purified water, and add 1% of the precipitate extract. During the re-dissolution process, add NaOH solution appropriately to completely dissolve the precipitate. Then add phosphoric acid to adjust the pH value to 6 to precipitate the alkali-soluble polysaccharide to form polysaccharide granules. The resulting suspension is the Poria cocos extract.

[0071] Comparative Example 3 Preparation of Poria cocos extract (water extract after enzymatic hydrolysis)

[0072] 1. Take the naturally sweated and shade-dried Poria cocos, slice it, dry it at 40℃ until the water content is less than 4%, then crush it, sieve it, and collect the Poria cocos powder. Weigh the Poria cocos powder, add 1L of purified water to make a Poria cocos slurry with a Poria cocos powder content of 1wt%.

[0073] 2. After extracting the Poria cocos slurry at 60°C and 200 rpm shaking for 4 hours, add 0.2% alkaline protease, 0.1% chitinase, 0.5% cellulase, and 0.1% lysozyme to the Poria cocos slurry, and hydrolyze at 45°C for 12 hours. Collect the water filtrate after enzymolysis, which is the Poria cocos extract (water extract after enzymolysis).

[0074] Comparative Example 4 Preparation of Poria cocos Extract (Preparation of Poria cocos Extract after Alcohol Extraction)

[0075] 1. Take the naturally sweated and shade-dried Poria cocos, slice it, dry it at 40℃ until the moisture content is less than 4%, then crush it, sieve it, and collect the Poria cocos powder.

[0076] 2. Take 50g of Poria powder, add 1L of 96% (V / V) ethanol, extract repeatedly and filter. After the filter residue is dried at 40℃, add 1L of purified water to make up to the volume to prepare Poria slurry with a Poria powder content of 1wt%.

[0077] 3. Extract the Poria slurry at 60°C and 200 rpm for 4 h, and collect the water filtrate (save for later use) and the filter residue.

[0078] 4. Dissolve the filter residue with 0.5L of 1% NaOH solution and stir to fully dissolve it; after dissolution, filter through a 0.8-micron filter membrane to collect the alkali-soluble filtrate; add ethanol (to an ethanol concentration of 55%) to the alkali-soluble filtrate for forward alcohol precipitation, let it stand and collect the precipitate after alcohol precipitation, wash the precipitate with an equal amount of ethanol, collect the precipitate (mainly alkali-soluble polysaccharides), and dry it in vacuo at 30°C to obtain the alkali extract.

[0079] 5. Add the dried alkali extract to the water extract filtrate obtained in step 3, the amount of the alkali extract added is 1% of the water extract filtrate, and in order to promote the complete dissolution of the alkali extract, add a 1% NaOH solution of appropriate concentration, and after the alkali extract is completely dissolved, add phosphoric acid to adjust the pH value to 6, and the alkali-soluble polysaccharides in the alkali extract are precipitated in the form of small spherical particles and suspended in the solution. The final suspension obtained is the Poria cocos extract.

[0080] Test Example 1 Evaluation of cytotoxicity of Poria cocos extract

[0081] The cytotoxicity evaluation experiment refers to: GB / T16886.5-2017 Biological Evaluation of Medical Devices Part 5: In Vitro Cytotoxicity Test (ISO 10993-5:2009, IDT) and the "People's Republic of China Entry-Exit Inspection and Quarantine Industry Standard" SNT 2328-2009 Cosmetic Acute Toxicity Keratinocyte Test, and evaluates the cytotoxicity of the products prepared in the above examples and comparative examples. The detection index is the cell proliferation rate, and the detection method is the WST-1 method.

[0082] 1. Experimental Materials

[0083] Experimental samples: Poria extracts prepared in Examples 1-5 and Comparative Examples 1-4.

[0084] 2. Instruments and Equipment

[0085] Inverted microscope (OLYMPUS, CKX41), clean bench (Beijing Donglian Har Instrument Manufacturing Co., Ltd., SCB-1520), carbon dioxide incubator (SANYO), digital constant temperature water bath (Jintan Zhongda Instrument Factory), constant temperature microplate fast oscillator (Haimen Qilin Medical Instrument Factory), microplate reader (BIO-RAD), etc.

[0086] 3. Experimental process and evaluation criteria

[0087] Mouse embryonic fibroblasts BALB / 3T3 cells in logarithmic growth phase were collected and 5×10 4 The cells were inoculated in a 96-well plate at a density of 100 μL per well. The culture system was DMEM high-glucose culture medium supplemented with 10% fetal bovine serum. The samples were prepared with serum-free culture medium into 1.0%, 5.0%, 10.0%, and 20% concentration solutions, extracted overnight in a 4°C refrigerator, centrifuged at 5000 rpm for 10 min, and the supernatant was filtered and sterilized with a 0.22 μm filter membrane before use. After the inoculated cells were placed in a carbon dioxide incubator at 37°C and 5% CO2 for 24 hours, the culture medium was discarded and replaced with 100 μL sample solution, and the serum-containing culture medium was used as a normal control (control). Each sample had 5 concentration levels and 6 parallel wells at each level. After continuing to culture for 48 hours, the relative proliferation rate of cells was detected by the WST-1 method. The relative proliferation rate (RGR) is the ratio of the absorbance of the sample group to the absorbance of the normal control group. According to the requirements of GB / T16886.5-2017, when the RGR is lower than 70%, the sample is considered to be cytotoxic.

[0088] 4. Experimental results

[0089]

[0090] It is generally believed that when the relative proliferation rate (RGR) is lower than 70%, there is cytotoxicity. As shown in Table 1, the Poria extracts prepared in Examples 1-5 and Comparative Examples 1-4 have no obvious cytotoxicity when the addition amount is 1%-20%, and the relative proliferation rate of fibroblasts of the Poria extracts in Examples 1-5 is maintained above 100% when the addition amount is as high as 20%, indicating that the Poria extract prepared by the present invention is not only non-toxic, but also highly safe and can be used in daily chemical products.

[0091] Test Example 2 Moisturizing effect of Poria cocos extract

[0092] The moisturizing effect of Poria cocos extract was evaluated with reference to QB / T 4256-2011 Guidelines for Evaluation of Moisturizing Efficacy of Cosmetics and T / ZHCA003-2018 Test Method for Transdermal Water Loss of Cosmetics.

[0093] 1. Experimental Materials

[0094] Experimental samples: Poria extracts prepared in Examples 1-5 and Comparative Examples 1-4.

[0095] 2. Instruments and Equipment

[0096] Skin moisture tester Corneometer CM 825 (Courage Khazaka, Germany).

[0097] 3 Experimental methods:

[0098] 3.1. Emulsion sample preparation

[0099] The Poria extract prepared in Examples 1-5 and Comparative Examples 1-4 was added to a basic moisturizing lotion (5% pentylene glycol, 0.2% glycerol) at an addition amount of 1%, 2%, 5%, 10%, and 20% to prepare a test lotion.

[0100] 3.2. Determination of moisture retention

[0101] The moisturizing test recruited 100 volunteers aged 20-50 years old, regardless of gender. The volunteers who met the requirements were divided into 5 groups, and each group tested a moisturizing lotion containing Poria cocos extract (prepared in Examples 1-5 and Comparative Examples 1-4) with a concentration gradient. The flexor side of the subject's forearm cannot be exposed to water 1-3 hours before the test, and it must be wiped clean with dry facial tissue before the experiment. Mark 9 experimental areas of 3 cm x 3 cm and 1 control area at the same position on the flexor side of the subject's left and right forearms. The test part must be exposed to the test environment for at least 20 minutes before the test. The initial value of the stratum corneum water content in the marked areas of the left and right arms was detected, and the experimental area was measured at 2.0±0.1 mg / cm 2 The test sample containing Poria cocos extract was applied once, and the control area was coated with a basic moisturizing lotion control sample without Poria cocos extract. All indicators were tested again 0.5h and 6h after use. The increase rate of skin moisture content of each volunteer was calculated and then the average value was taken.

[0102] Data processing

[0103]

[0104] 4. Experimental Results

[0105]

[0106]

[0107] The data in Tables 2 and 3 show that the Poria extracts prepared in Examples 1-5 all have good moisturizing effects. In the case of the same addition amount, the effects of the Poria extracts prepared in Examples 1-5 of the present invention are better than those prepared in Comparative Examples 1, 2, 3, and 4. It can be seen from the analysis data that the Poria extract prepared in Comparative Example 2 has a good moisturizing effect, indicating that the Poria alkali-soluble polysaccharide has a good moisturizing effect, and the Poria extracts prepared in Comparative Examples 1 and 3 do not have a moisturizing effect, and can reduce the moisture content of the skin, indicating that the water extract of Poria may promote transdermal water loss, causing the moisture content of the skin to decrease. The moisturizing effect of the Poria extract after alcohol extraction prepared in Comparative Example 4 is close to that of Comparative Example 2, but lower than that of Examples 1-5, indicating that alcohol extraction before preparing the Poria extract will lose a part of the effective substances. The moisturizing effect of the Poria extract prepared in Examples 1-5 is significantly improved compared with that of Comparative Example 2, which indicates that the mixture of the Poria water extract and the Poria alkali-soluble polysaccharide has an unexpected synergistic effect on the moisturizing effect. This may be because the introduction of the Poria water extract in Examples 1-5 promotes the absorption of some extract components, while the film-forming property of the alkali-soluble polysaccharide particles reduces water loss, and together they form a good moisturizing effect.

[0108] Test Example 3 Oil Control Effect of Poria Extract

[0109] The oil control effect of Poria cocos extract was evaluated with reference to T / ZHCA 002-2018 cosmetic oil control efficacy determination method.

[0110] 1. Experimental Materials

[0111] Experimental samples: The Poria extracts prepared in Examples 1-5 and Comparative Examples 1-4 were added to a basic moisturizing lotion (5% pentylene glycol, 0.2% glycerol) at an addition amount of 5% to prepare a test lotion.

[0112] 2. Instruments and Equipment

[0113] Multi-probe skin testing system MPA580 (Courage + Khazaka, Germany).

[0114] 3. Experimental Methods

[0115] 180 volunteers were recruited, aged 20-50 years old, both men and women. The volunteers who met the requirements were randomly divided into 9 groups, and each group used an emulsion containing 5% Poria extract (prepared in Examples 1-5 and Comparative Examples 1-4). Using the half-face control method, the left and right halves of the subjects used an emulsion containing Poria extract and a placebo, respectively. After the volunteers cleansed their faces for 15 minutes, the skin oil content of the left and right foreheads was detected as the initial value. After that, the left and right halves of the face were respectively used with an emulsion containing Poria extract and a placebo in the morning and evening, and the dosage was kept consistent. All indicators were tested again 1 week, 2 weeks, and 4 weeks after use. The relative value of the skin oil content of each volunteer was calculated, and then the average was taken.

[0116]

[0117] 4. Experimental results

[0118]

[0119] As can be seen from the data in Table 4, the Poria extracts prepared in Examples 1-5 all have good oil control effects, can effectively reduce the oil content on the skin surface, and the effects are significantly better than the Poria extracts prepared in Comparative Examples 1, 2, 3, and 4. From the analysis of the data, it can be seen that the Poria extracts prepared in Comparative Examples 1-4 all have partial oil control effects, but the effects are poor and not significant. The oil control effects of the Poria extracts prepared in Examples 1-5 are unexpectedly improved compared with Comparative Examples 1-4, and are significantly different from the placebo, and can be used in daily chemical products with oil control requirements.

[0120] In summary, the preparation method of the Poria cocos extract of the present invention is simple and easy, and it contains both Poria cocos alkali-soluble polysaccharides and Poria cocos water-soluble extracts (including water-soluble polysaccharides). Compared with single Poria cocos alkali-soluble polysaccharides and Poria cocos water-soluble extracts, the Poria cocos extract has synergistic moisturizing and reducing skin oil secretion effects, and has better application prospects in daily chemical products.

Claims

1. A Poria cocos extract, characterized in that: The Poria cocos extract contains both Poria cocos water extract and Poria cocos alkali extract. The Poria cocos water extract is obtained by extracting Poria cocos with water. After extracting Poria cocos with water once or multiple times, the filtrate obtained by filtering is the water extract. The mass ratio of Poria cocos to the Poria cocos water extract is 1-5:

100. The Poria cocos alkali extract is an alcohol precipitate obtained by alkali extraction and alcohol precipitation with Poria cocos residue after water extraction as a raw material. The concentration of Poria cocos alkali extract in the Poria cocos water extract is 1-3wt%.

2. The Poria cocos extract according to claim 1, characterized in that: When preparing the Poria cocos alkali extract, the Poria cocos residue after water extraction is first fully dissolved in a sodium hydroxide solution, and then the dissolved liquid is precipitated with alcohol to obtain the alcohol precipitate, which is the Poria cocos alkali extract. The mass ratio of the Poria cocos residue after water extraction to the sodium hydroxide solution is 1-5:

50.

3. The Poria cocos extract according to claim 1 or 2, characterized in that: The tuckahoe alkali extract is suspended in the tuckahoe water extract in the form of spherical particles.

4. The Poria cocos extract according to claim 3, characterized in that: The tuckahoe alkali extract is mixed with the tuckahoe water extract, and then sodium hydroxide solution is added to completely dissolve the tuckahoe alkali extract, and then acid is added to adjust the pH to 6-8, so that the tuckahoe alkali extract is suspended in the tuckahoe water extract in the form of spherical particles.

5. A method for preparing the Poria cocos extract according to any one of claims 1 to 4, characterized in that The following steps are involved: (1) extracting the Poria powder with water, filtering after extraction to obtain a water extract, and filtering the obtained filter residue for later use; (2) dissolving the filter residue fully with sodium hydroxide solution, and then filtering to obtain an alkaline filtrate; (3) adding alcohol to the alkaline filtrate for alcohol precipitation, washing the obtained precipitate with alcohol and drying it to obtain an alkaline extract; (4) adding the alkaline extract of step (3) to the water extract of step (1), adding sodium hydroxide solution to dissolve the alkaline extract in the water extract, and after the alkaline extract is dissolved, adding acid to adjust the pH to 6.0-8.0 to obtain a Poria cocos extract.

6. The method according to claim 5, characterized in that: At least one of the following conditions is met: Condition 1: In step (1), Poria powder and water are mixed in a mass ratio of 1-5:100; Condition 2: In step (2), the concentration of the sodium hydroxide solution is 1-2wt%; Condition 3: In step (2), the mass ratio of sodium hydroxide solution to filter residue is 50:1-5; Condition 4: In step (4), the concentration of the alkali extract in the water extract is 1-3 wt %; Condition 5: In step (4), the concentration of the sodium hydroxide solution is 1-2 wt %.

7. Use of the Poria cocos extract according to any one of claims 1 to 4 in the preparation of moisturizing products and skin oil control products.

8. A composition, characterized in that: The invention comprises the Poria cocos extract according to any one of claims 1 to 4.

9. The composition according to claim 8, characterized in that: The amount of Poria cocos extract added to the composition is 1-20wt%.

10. The composition according to claim 9, characterized in that: The amount of Poria cocos extract added to the composition is 2-10wt%.

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