WO2016184147A1 - Antrodia cinnamomea drop pill and preparation method thereof - Google Patents

Abstract

An Antrodia Cinnamomea drop pill and a preparation method thereof. The preparation method comprises the following steps: (1) crushing: freezing an Antrodia Cinnamomea body and Antrodia Cinnamomea hyphae, and then dehydrating and puffing the same by a temperature-changing differential pressure puffing equipment, and crushing, by a high power nanometer crushing mill, a powder mixture for 3 hours; (2) extracting: loading a crushed Antrodia Cinnamomea powder into an extractor vessel of a supercritical CO₂ extractor equipment and performing extraction; (3) condensing: mixing a separated liquid and an entrainer and evaporating an alcohol in a mixture of the separated liquid and entrainer to obtain an Antrodia Cinnamomea liquid extract; (4) preparing a drop pill: uniformly mixing the Antrodia Cinnamomea liquid extract, heating, melting, and dripping the same into a condensing coolant to perform gradient condensation, collecting a resultant drop pill as an Antrodia Cinnamomea drop pill. The preparation method is simple to operate, and produces a high activity and an easily absorbed product.

Description

Zhizhi dripping pill and preparation method thereof

 Technical field

 The invention relates to a health drink, in particular to a Zhizhi dripping pill with simple method, high biological activity of the product and beneficial to human body absorption and preparation method thereof .

 Background technique

 Antrodia Cinnamomea, also known as Antrodia camphorata, is a medicinal fungus with high medicinal value. In the era of 'Xiqi Medicine' in Taiwan, 500 years ago, indigenous people used it to detoxify, hangover and protect the liver, which was later promoted and used by the majority of Taiwan residents. In Taiwan, Yan Zhi is known as the 'King of Medicine', 'King of Cancer', 'King of Detoxification', 'King of Anti-Inflammation' and so on. Modern research and clinical practice have shown that the physiologically active ingredients such as polysaccharides, triterpenoids, sterols and antioxidants contained in Azolla have liver protection, anti-tumor, anti-oxidation, intensive immunity, anti-allergy, anti-inflammatory and antibacterial. , anti-virus and other effects, so in recent years has become a research and development hotspot. Dropping pills are preparations in which a solid or liquid drug is heated and melted and mixed with a substrate, dropped into an immiscible condensate, and shrunk and condensed. Pills have the characteristics of low dosage, disintegration and rapid dissolution, and are excellent dosage forms for extracts with small extraction amount and strong fat solubility. Because the carrier has a moist, hindered aggregation, solubilization and inhibition of the drug , The drug mainly exists in the matrix, microcrystal or colloidal state in the matrix, and the total surface area of the drug is increased, which not only increases the solubility, dissolution rate and absorption rate of the active components of the poorly soluble traditional Chinese medicine, but also improves the bioavailability of the active ingredient. Therefore, the dropping pills are essentially different from the traditional preparations, and have some advantages that other conventional dosage forms do not have.

 Summary of the invention

 In order to fully utilize the active ingredients in Antrodia camphorata and improve the absorption effect of Antrodia camphorata, one of the objects of the present invention is to provide a simple method and high bioactivity of the product. A method for preparing Antrodia sinensis pills for the absorption of the human body.

 The invention is achieved by the following technical measures, a preparation method of the Zhizhi dropping pill, comprising the following steps:

Step 1. Crushing: The A. camphorata fruit body and the Antrodia camphorata mycelium were frozen at minus 20 ° C for 60 minutes, and the frozen Aconite body and A. sinensis mycelium were dehydrated and expanded in a variable temperature and pressure expansion device. Adding dry ice particles having a particle size of less than 50 μm to the aphid body and the A. sinensis mycelium after dehydration and puffing at a ratio of 2:1, and pulverizing the mixed particles by a high-energy nano-impact mill for 3 hours;

Step 2. Extraction: 1 part by weight of the pulverized Antroil powder is charged into the extraction vessel of the supercritical CO ₂ extraction apparatus, and 4-8 parts by weight of absolute ethanol is added as an entraining agent to be extracted at 20 ° C to 60 ° C, and extracted. The extraction pressure of the autoclave is 10 MPa to 35 MPa, the flow rate of CO ₂ is 10 to 40 L/h, the extraction time is 1-1.5 hours, and after separation, it is separated into a separation vessel for separation. The pressure in the separation reactor I is 5MP-25MP, and the temperature is 20 °C. 30 ° C; the pressure in the separation tank II is 7MP ~ 15MP, the temperature is 20 ° C ~ 50 ° C;

 Step 3. Concentration: the separated liquid and the entrainer mixture are evaporated to dry ethanol at 80-90 ° C to obtain an extract of Antrodia camphorata;

 Step 4. Preparation of dropping pills: 1 part by weight of Antrodia camphorata extract and 3 parts by weight of the matrix are uniformly mixed, heated and melted, and then the melted Antrodia camphorata extract and substrate are dropped into the mixture at 8 ° C at 80-85 ° C - Gradient condensation in a 12 ° C condensing agent, The dropping pills are collected, the condensing agent on the pills is removed, and after drying for 24h-48h, the burdock is added.

 As a preferred mode, the mass ratio of the ball to the anthraquinone powder in the high energy nano impact mill in step 1 is 6-12:1.

 As a preferred mode, the pellet is cerium oxide.

 As a preferred mode, the temperature of the extraction in step 2 is from 40 ° C to 50 ° C.

As a preferred mode, the CO ₂ flow rate in step 2 is 22 to 32 L/h.

 As a preferred mode, the extraction pressure of the extraction vessel in step 2 is 15 MPa.

 As a preferred mode, in step 4, the drop distance of the Antrodia camphorata extract and the substrate into the condensing agent is 13 cm, and the temperature of the condensing agent is At 10 ° C, the formed pellets were removed from the surface condensing agent and dried to obtain Antrodia sinensis pills.

 As a preferred mode, the substrate in step 4 is polyethylene glycol 6000, and the condensing agent is liquid paraffin or dimethicone.

 Another object of the present invention is to protect the Zhizhi drop pills prepared by the above method.

The Antrodia camphorata fruit body and the Antrodia camphorata mycelium of the invention are subjected to temperature-variation pressure-expansion treatment after freezing, and the micro-crushing technology is used to carry out cell-level micro-pulverization of Antrodia camphorata so that the effective active ingredients in the cells are not destroyed. It can be fully exposed and can greatly increase the release rate and release amount of effective active ingredients. By using alcohol extraction combined with water extraction, it is possible to extract the active constituents such as triterpenoid which is easily soluble in alcohol and polysaccharide which is easily soluble in water. The extraction technique uses supercritical CO ₂ extraction to enable the active ingredients in Antrodia to be extracted at lower temperatures. This not only ensures that the active ingredient is sufficiently extracted, but also ensures that the extraction temperature is not too high, and protects the heat-sensitive component from being destroyed by high temperature. The dropping pills are prepared by the principle of dispersion, and the drug is highly dispersed in the drug matrix, and the drug exists in a high energy state such as a molecular state, colloidal crystallites or metastable microparticles, and the particle size of the poorly soluble drug can be greatly reduced. Increasing the diffusion area is beneficial to the dissolution of the drug, accelerates the dissolution rate of the active ingredient, and improves the absorption effect.

 detailed description

 The invention will now be further described in detail with reference to the examples and comparative examples.

 A method for preparing a Zhizhi drop pill, comprising the following steps:

Step 1. Crushing: The A. camphorata fruit body and the Antrodia camphorata mycelium were frozen at minus 20 ° C for 60 minutes, and the frozen Aconite body and A. sinensis mycelium were dehydrated and expanded in a variable temperature and pressure expansion device. Adding dry ice particles having a particle size of less than 50 μm to the aphid body and the A. sinensis mycelium after dehydration and puffing at a ratio of 2:1, and pulverizing the mixed particles by a high-energy nano-impact mill for 3 hours;

Step 2. Extraction: 1 part by weight of the pulverized Antroil powder is charged into the extraction vessel of the supercritical CO ₂ extraction apparatus, and 4-8 parts by weight of absolute ethanol is added as an entraining agent to be extracted at 20 ° C to 60 ° C, and extracted. The extraction pressure of the autoclave is 10 MPa to 35 MPa, the flow rate of CO ₂ is 10 to 40 L/h, the extraction time is 1-1.5 hours, and after separation, it is separated into a separation vessel for separation. The pressure in the separation reactor I is 5MP-25MP, and the temperature is 20 °C. 30 ° C; the pressure in the separation tank II is 7MP ~ 15MP, the temperature is 20 ° C ~ 50 ° C;

 Step 3. Concentration: the separated liquid and the entrainer mixture are evaporated to dry ethanol at 80-90 ° C to obtain an extract of Antrodia camphorata;

 Step 4. Preparation of dropping pills: 1 part by weight of Antrodia camphorata extract and 3 parts by weight of the matrix are uniformly mixed, heated and melted, and then the melted Antrodia camphorata extract and substrate are dropped into the mixture at 8 ° C at 80-85 ° C - Gradient condensation in a 12 ° C condensing agent, The dropping pills are collected, the condensing agent on the pills is removed, and after drying for 24h-48h, the burdock is added.

The method of the Antrodia camphorata fruit body and the Antrodia camphorata mycelium is subjected to temperature-variation pressure-expansion treatment after freezing, and the micro-crushing technology is used to carry out cell-level micro-pulverization of the Antrodia camphorata so that the effective active ingredients in the cells are not destroyed. It can be fully exposed and can greatly increase the release rate and release amount of effective active ingredients. By using alcohol extraction combined with water extraction, it is possible to extract the active constituents such as triterpenoid which is easily soluble in alcohol and polysaccharide which is easily soluble in water. The extraction technique uses supercritical CO ₂ extraction to enable the active ingredients in Antrodia to be extracted at lower temperatures. This not only ensures that the active ingredient is sufficiently extracted, but also ensures that the extraction temperature is not too high, and protects the heat-sensitive component from being destroyed by high temperature. The dropping pills are prepared by the principle of dispersion, and the drug is highly dispersed in the drug matrix, and the drug exists in a high energy state such as a molecular state, colloidal crystallites or metastable microparticles, and the particle size of the poorly soluble drug can be greatly reduced. Increasing the diffusion area is beneficial to the dissolution of the drug, accelerates the dissolution rate of the active ingredient, and improves the absorption effect.

 In an embodiment of the preparation method of the Zhizhi drop pill, the specific technical solution may also be based on the foregoing technical solution. The mass ratio of the ball to the anthraquinone powder in the high energy nano impact mill in step 1 is 6-12:1.

 In an embodiment of the preparation method of the Zhizhi drop pill, in addition to the foregoing technical solution, the ball material may be ceria.

 In an embodiment of the preparation method of the Zhizhi drop pill, the specific technical solution may also be based on the foregoing technical solution. The temperature of the extraction in step 2 is 40 ° C to 50 ° C.

In the embodiment of the method for preparing the sapphire granules, in the foregoing technical solution, the CO ₂ flow rate in the step 2 is 22 to 32 L/h.

 In an embodiment of the preparation method of the Zhizhi drop pill, the specific technical solution may also be based on the foregoing technical solution. The extraction pressure of the extraction vessel in step 2 is 15 MPa.

 In an embodiment of the preparation method of the Zhizhi drop pill, the specific technical solution may also be based on the foregoing technical solution. In step 4, the drop distance between the Antrodia camphorata extract and the substrate into the condensing agent is 13 cm, the temperature of the condensing agent is 10 ° C, and the formed pellets are removed from the surface condensing agent and dried to obtain Anthracis chinensis pills.

 In an embodiment of the preparation method of the Zhizhi drop pill, according to the foregoing technical solution, the substrate in the step 4 is polyethylene glycol. 6000, the condensing agent is liquid paraffin or dimethicone.

 The above is a description of the present invention, and the preparation method thereof is used to help understand the present invention. However, the embodiments of the present invention are not limited by the above-described embodiments, and any changes, modifications, substitutions, combinations, and simplifications that are made without departing from the principles of the present invention should be equivalently substituted, and are included in the protection of the present invention. Within the scope.

Claims (9)

A method for preparing an Antrodia sinensis dropping pill, comprising the steps of: Step 1. Crushing: The A. camphorata fruit body and the Antrodia camphorata mycelium were frozen at minus 20 ° C for 60 minutes, and the frozen Aconite body and A. sinensis mycelium were dehydrated and expanded in a variable temperature and pressure expansion device. Adding dry ice particles having a particle size of less than 50 μm to the aphid body and the A. sinensis mycelium after dehydration and puffing at a ratio of 2:1, and pulverizing the mixed particles by a high-energy nano-impact mill for 3 hours; Step 2. Extraction: 1 part by weight of the pulverized Antroil powder is charged into the extraction vessel of the supercritical CO ₂ extraction apparatus, and 4-8 parts by weight of absolute ethanol is added as an entraining agent to be extracted at 20 ° C to 60 ° C, and extracted. The extraction pressure of the autoclave is 10 MPa to 35 MPa, the flow rate of CO ₂ is 10 to 40 L/h, the extraction time is 1-1.5 hours, and after separation, it is separated into a separation vessel for separation. The pressure in the separation reactor I is 5MP-25MP, and the temperature is 20 °C. 30 ° C; the pressure in the separation tank II is 7MP ~ 15MP, the temperature is 20 ° C ~ 50 ° C; Step 3. Concentration: the separated liquid and the entrainer mixture are evaporated to dry ethanol at 80-90 ° C to obtain an extract of Antrodia camphorata; Step 4. Preparation of dropping pills: 1 part by weight of Antrodia camphorata extract and 3 parts by weight of the matrix are uniformly mixed, heated and melted, and then the melted Antrodia camphorata extract and substrate are dropped into the mixture at 8 ° C at 80-85 ° C - Gradient condensation in a 12 ° C condensing agent, The dropping pills are collected, the condensing agent on the pills is removed, and after drying for 24h-48h, the burdock is added. The preparation method according to claim 1, wherein in the high energy nano impact mill, the mass ratio of the ball to the anthraquinone powder in the high energy nano impact mill is 6-12:1. The preparation method according to claim 2, wherein the pellet is cerium oxide. The preparation method according to claim 1, wherein the extraction temperature in the step 2 is 40 ° C to 50 ° C. The preparation method according to claim 1, wherein the flow rate of the CO ₂ in the step 2 is 22 to 32 L/h. The preparation method according to claim 1, wherein in the step 2, the extraction pressure of the extraction vessel is 15 MPa. The preparation method according to claim 1, wherein in step 4, the drop distance of the antrodia camphora extract and the substrate into the condensing agent is 13 cm, and the temperature of the condensing agent is At 10 ° C, the formed pellets were removed from the surface condensing agent and dried to obtain Antrodia sinensis pills. The preparation method according to claim 1, wherein the substrate in the step 4 is polyethylene glycol 6000, and the condensing agent is liquid paraffin or dimethicone. An anthraquinone dropping pill prepared according to any one of claims 1-8.