Preparation method of Xiansheng pill dry extract powder

Abstract

The invention relates to a preparation method of Xiansheng pill dry extract powder, which is characterized by comprising the following steps: material preparation, extraction, concentration, belt type vacuum drying, crushing and packaging, and the belt type vacuum drying adopts a multi-stage drying mode. In the drying process of the Xiansheng pill extract, a multi-stage drying mode is adopted, effective components (such as saponin components and volatile oil components) in the Xiansheng pill dry extract powder are protected to the maximum extent, meanwhile, the drying time is shortened, the efficiency is improved, and the wall hanging phenomenon in the extract drying process is reduced.

Description

Technical Field

[0001] The present invention relates to the technical field of traditional Chinese medicine preparations, and in particular to a method for preparing a Zhongsheng Pill dry extract powder, in particular to a method for preparing a Zhongsheng Pill dry extract powder with high active ingredients, high stability and low moisture content through a multi-stage belt vacuum drying technology. Background Art

[0002] Zhongsheng Pills are one of the exclusive products of Guangdong Zhongsheng Pharmaceutical Co., Ltd. It is a traditional Chinese patent medicine with the effects of clearing away heat and detoxifying, promoting blood circulation and reducing swelling. It is widely used clinically to treat upper respiratory tract infections, sore throat, sores and swelling, and other diseases. Its formula contains 15 Chinese medicinal materials such as dandelion, windproof, Viola yedoensis, and Bupleurum. The combination of various medicinal materials synergistically exerts the effects of clearing heat and detoxifying, dispersing wind and evil, promoting blood circulation and reducing swelling.

[0003] Dandelion clears away heat and toxic substances, reduces swelling and resolves stagnation, and promotes dampness and relieves stranguria. It is used to treat sore throat, sores, and furuncles caused by excessive heat and toxicity. Saposhnikovia divaricata dispels wind and relieves exterior symptoms, overcomes dampness and relieves pain, relieves exogenous wind evil, and improves symptoms such as headaches and joint pain. Viola yedoensis clears away heat and toxic substances, cools blood and reduces swelling, and is commonly used for heat and toxicity syndromes such as carbuncles, furuncles, and snake bites. Bupleurum chinense soothes the liver and relieves depression, harmonizes and reduces fever, regulates Qi, and relieves symptoms such as fever and chest and flank fullness. Red peony root clears heat and cools blood, disperses blood stasis and relieves pain, and improves pain and swelling caused by blood heat and stasis. Scrophularia ningpoensis clears heat and cools blood, nourishes yin and reduces fire, and is used for sore throat, yin damage caused by febrile diseases, and other symptoms. Angelica sinensis replenishes blood and promotes blood circulation, regulates menstruation and relieves pain, promotes blood circulation, and assists in reducing swelling and resolving stagnation. Angelica dahurica dispels wind and resolves exterior symptoms, reduces swelling and discharges pus, and relieves headaches, nasal congestion, and sores and toxicity. Isatis root, clears heat and detoxifies, cools blood and relieves sore throat, and is commonly used for heat-toxic symptoms such as influenza and sore throat. Polygonum cuspidatum, clears heat and detoxifies, promotes blood circulation and dissipates blood stasis, promotes dampness and reduces jaundice, and improves damp-heat jaundice, traumatic injuries, and other symptoms. Prunella vulgaris, clears the liver and purges fire, disperses stagnation and reduces swelling, and is used for symptoms such as red and swollen eyes, scrofula, and goiter. Scutellaria baicalensis, clears heat and dries dampness, purges fire and detoxifies, and is used for symptoms such as lung heat cough and damp-heat jaundice. Gleditsia sinensis, reduces swelling and discharges pus, dispels wind and kills parasites, promotes the rupture and discharge of pus in sores and ulcers, and assists in reducing swelling. Rhizoma Cibotii, clears heat and detoxifies, promotes the production of body fluids and quenches thirst, and is commonly used for symptoms such as sore throat and dry mouth. Radix Trichosanthis, clears heat and promotes the production of body fluids, reduces swelling and discharges pus, and improves symptoms such as thirst due to fever, and sore and swollen sores.

[0004] The standard production process for Zhongsheng Pills involves boiling some of the medicinal ingredients in the recipe in water using a traditional multi-functional extraction tank. The extract is then concentrated into an extract using a triple-effect concentrator. The extract is then spray-dried into a dry paste powder using a spray dryer. The dry paste powder is then mixed with Arisaema consanguineum powder and artificial bezoar, and then formed into pills using a traditional plastic molding process. This production process has significant flaws. After the extract of the Zhongsheng Pills' medicinal ingredients is concentrated into an extract, the extract is spray-dried using a spray dryer with an inlet air temperature of 200-300°C. This high drying temperature destroys the active ingredients in the extract, significantly reducing the active ingredient content in the dry paste powder. Consequently, the therapeutic efficacy of Zhongsheng Pills formulated with this dry paste powder will be significantly reduced, even at the same dose as the original.

[0005] Traditional Chinese medicine extracts are thick, paste-like preparations obtained by extracting the active ingredients of medicinal materials with a suitable solvent and then concentrating them. These extracts retain all the active ingredients of herbal decoctions and are often used as raw materials for preparing other traditional Chinese medicine preparations. Currently, to facilitate the use and storage of traditional Chinese medicine extracts, they are often dried to produce dry powders.

[0006] Chinese patent ZL201010237529.7, issued on December 8, 2010, discloses a method for drying the extract of Zhongsheng Pills using a vacuum belt dryer. This gentle drying process (material temperature ranges from 40-80°C) involves adding optimal excipients and dosages to the dried extract powder, Arisaema consanguineum powder, and artificial bezoar, followed by pill pressing. This method significantly preserves the active ingredients in the Zhongsheng Pills formulation and significantly improves their efficacy.

[0007] Chinese patent CN201611160312.4, published on May 31, 2017, discloses a drying process for a compound Chinese herbal extract for treating insomnia, which uses a vacuum belt continuous dryer for drying and includes the following steps:

[0008] (1) Preheating the compound Chinese medicine extract for treating insomnia to 40-90° C., evenly coating the extract on a conveyor belt at a feeding rate of 4-12 L / h through a distributor, and running the conveyor belt at a speed of 6-30 m / h;

[0009] (2) Under vacuum conditions, the compound Chinese medicine extract for treating insomnia is sequentially moved through three heating sections and finally through a cooling section to form a porous, crispy cake-like dried product;

[0010] (3) crushing the dried material and sending it into the product collection tank through the discharging device;

[0011] The vacuum belt continuous dryer comprises a distributor, a conveyor belt, a crusher, three heating sections and a cooling section.

[0012] Guo Tiantian et al. published "Response Surface Methodology for Optimizing the Vacuum Belt Drying Process of Honeysuckle Extract." This paper notably combines single-factor experiments with response surface methodology to identify four influencing factors: relative density of honeysuckle extract, second-stage heating temperature, track speed, and material distribution speed. Using a comprehensive score of honeysuckle extract moisture and chlorogenic acid transfer rate as the evaluation criteria, the vacuum belt drying process parameters for honeysuckle extract were optimized. The first stage heats the material to a certain temperature; the second and third stages dry the material; and the fourth stage cools it down.

[0013] Zhongsheng Pills contain numerous medicinal ingredients. During the preparation of Zhongsheng Pills extract powder, the drying temperature and method are crucial to preserving the active ingredients. Improper heating and drying processes (such as high-temperature, prolonged baking or excessively high spray drying temperatures) can lead to the following problems:

[0014] 1. Degradation of heat-sensitive ingredients

[0015] Ingredients such as baicalin, saikosaponin, and chlorogenic acid (dandelion and viola yedoensis) are sensitive to high temperatures. Long-term high-temperature drying can easily lead to their oxidative decomposition and reduce their efficacy.

[0016] Volatile oil components (such as Angelica dahurica and Angelica sinensis) are easily volatilized and lost at high temperatures, affecting their efficacy in dispelling wind and activating blood circulation.

[0017] 2. Maillard reaction and browning

[0018] Sugars (such as lactose excipients) and amino acids (such as proteins in angelica and Scrophularia) undergo Maillard reaction at high temperatures, which not only causes the color of the extract to darken, but may also produce invalid or harmful products.

[0019] 3. Destruction of polysaccharide components

[0020] High-temperature drying may cause the structure of isatis root polysaccharide, fangfeng polysaccharide and other ingredients with immune-regulating effects to break and lose their activity.

[0021] 4. Uneven moisture residue and agglomeration

[0022] Traditional oven drying can easily cause surface hardening and internal moisture residue, making subsequent crushing difficult. It is also easy to absorb moisture and form lumps during storage, affecting the stability of the preparation.

[0023] From the above, we can see that due to the large number of medicinal materials and different characteristics of Zhongsheng Pills, the current preparation method of the dry extract powder of Zhongsheng Pills is still too simple. A more sophisticated method is needed to prepare the dry extract powder of Zhongsheng Pills, so as to further improve the quality standards of Zhongsheng Pills. Summary of the Invention

[0024] The purpose of the present invention is to overcome the deficiencies of the prior art and provide a method for preparing a dry extract powder of Zhongsheng Pills, characterized in that it comprises the following steps: batching, extraction, concentration, belt vacuum drying, pulverization, and packaging. Compared with conventional belt vacuum drying, the present invention adopts a multi-stage drying method. This method can shorten the drying time, improve efficiency, increase the content of active ingredients, and reduce the phenomenon of wall hanging during the drying process of the extract in the preparation process of Zhongsheng Pills. It can also significantly increase the content of the index components of the various medicinal materials of Zhongsheng Pills, providing a qualified dry extract powder for subsequent diversified processing.

[0025] The purpose of the present invention is achieved through the following technical solutions:

[0026] A method for preparing Zhongsheng Pills extract powder is characterized by comprising the following steps: batching, extraction, concentration, belt vacuum drying, crushing and packaging.

[0027] The belt vacuum drying adopts a multi-stage drying method:

[0028] The first stage: vacuum degree -0.35~-0.45MPa, drying temperature 40-50℃, conveyor speed 0.5-0.6m / min, drying time 10-20min;

[0029] The second stage: vacuum degree -0.15~-0.25MPa, drying temperature 55-65℃, conveyor speed 0.3-0.4m / min, drying time 5-15min;

[0030] The third stage: vacuum degree -0.05~-0.15MPa, drying temperature 70-80℃, conveyor belt speed 0.1-0.2m / min, drying time 5-10min, and the moisture content of the dry paste powder is less than 8.0%.

[0031] In the present invention, the belt vacuum drying adopts a multi-stage drying method to achieve one of the key technologies for technical effects. The multi-stage drying is used to maximize the protection of the active ingredients (such as saponin components, volatile oil components, etc.) in the dried extract powder of Zhongsheng Pills. At the same time, it shortens the drying time, improves efficiency, and reduces the wall hanging phenomenon during the drying process of the extract. The first stage: vacuum degree -0.35~-0.45MPa, drying temperature 40-50℃, conveyor belt speed 0.5-0.6m / min, drying time 10-20min. For volatile oils (such as Angelica dahurica, Angelica sinensis) and heat-sensitive components (such as chlorogenic acid), the low temperature environment can reduce volatilization and oxidation, and the high vacuum degree (-0.4MPa) accelerates water evaporation, avoids long-term heating, and retains small molecular active substances. The second stage: vacuum degree -0.15 ~ -0.25MPa, drying temperature 55-65℃, conveyor speed 0.3-0.4m / min, drying time 5-15min, gradually increasing the temperature to promote the removal of bound water, while avoiding sudden heat-induced structural damage of polysaccharides (such as Radix Isatidis polysaccharides). Moderate vacuum (-0.2MPa) balances drying efficiency and material fluffiness to prevent surface filming. The third stage: vacuum degree -0.05 ~ -0.15MPa, drying temperature 70-80℃, conveyor speed 0.1-0.2m / min, drying time 5-10min, short-term high temperature to completely remove residual moisture (ultimately <5%), low vacuum (-1.0MPa) inhibits the Maillard reaction, prevents browning of sugars (lactose) and amino acids (angelica, Scrophularia), and ensures color and stability. Preferably, the belt vacuum drying adopts a multi-stage drying method, the first stage: vacuum degree -0.4MPa, drying temperature 45°C, conveyor belt speed 0.55m / min, drying time 15min; the second stage: vacuum degree -0.2MPa, drying temperature 60°C, conveyor belt speed 0.35m / min, drying time 10min; the third stage: vacuum degree -0.1MPa, drying temperature 75°C, conveyor belt speed 0.15m / min, drying time 5min, and the moisture content of the dry paste powder is less than 5.0%. Under these conditions, the temperature can be increased step by step to reduce thermal stress, and the loss rate of active ingredients is less than 10%, which is significantly better than traditional spray drying (loss rate of more than 30%), achieving the effect of ingredient retention. At the same time, the vacuum environment reduces the boiling point, shortens the drying time by more than 40%, and reduces energy consumption by more than 35%, achieving energy-saving and high-efficiency effects, and accurately controls the moisture gradient to avoid moisture absorption and agglomeration, extend the shelf life, and achieve the effect of stable quality.

[0032] In the present invention, the addition of lactose during the concentration process is one of the key technologies to achieve the technical effect. The current process of Zhongsheng Pills is to take the dried paste powder of Zhongsheng Pills, a premix of Arisaema consanguineum powder and lactose, artificial bezoar, hydroxypropyl cellulose, and microcrystalline cellulose, and then add silicon dioxide and magnesium stearate to a granulator at 45Hz through a 2.5mm sieve and put them together into a mixer for mixing for 30 minutes. Lactose is added after the dry paste powder is prepared, and then the mixture is mixed and pressed into pills. The inventors found that in the concentration process of Zhongsheng Pills extract, adding an appropriate amount of lactose allows the lactose and active ingredients to form a molecular-level dispersion, which improves bioavailability compared to the traditional drying and mixing process. At the same time, the amount of addition is strictly controlled, which ensures the function without affecting the material basis of the efficacy, in line with the principle of "excipients are used for the purpose" of traditional Chinese medicine preparations. Specifically, lactose, as an excellent pharmaceutical excipient, can significantly improve the physical properties of the extract and reduce its viscosity: the viscosity of Chinese herbal medicine extract increases sharply after concentration. The addition of lactose can interrupt the hydrogen bonds between polysaccharide chains, improve the fluidity of the concentrate, facilitate the transportation and spreading of the subsequent drying process, prevent agglomeration, and form a microcrystalline structure during the drying process. It acts as a physical isolation agent to prevent the melt adhesion of the extract particles, so that the final dry powder bulk density is controlled at 1.25-1.35g / cm 3 Ideal range. At the same time, lactose can play a role in thermal protection and antioxidant barrier. The glass transition temperature of lactose is about 101°C. It forms an amorphous protective layer during drying, which reduces the degradation rate of heat-sensitive ingredients such as baicalin to less than 5% (up to 15% when not added). Its reducing carbonyl group can preferentially react with oxygen to protect easily oxidized ingredients (such as saikosaponin). Secondly, the addition of lactose improves the drying efficiency. The hygroscopicity of lactose can promote moisture migration and shorten the belt drying time. As an inert carrier, it offsets the fluctuation of the solid content of medicinal extracts in different batches and ensures the consistency of the quality of the final product. Finally, lactose can reduce the contact angle of dry paste powder from 75° to 35°, significantly improve water solubility, and prevent moisture absorption and agglomeration through moisture regulation (balanced moisture 3.5-4.5%). Accelerated tests (40°C / RH75%) show that the shelf life is extended to 36 months. Preferably, the extract is concentrated at a temperature of 60-85°C, a steam pressure of 0.04-0.12 MPa, and a vacuum degree of 0.02-0.09 MPa, and lactose is added to concentrate the extract until the relative density is 1.25-1.35 g / cm 3 The amount of lactose is 0.5-0.9% of the total weight of the ingredients. More preferably, the extract is concentrated under the conditions of temperature 75°C, steam pressure 0.10 MPa, and vacuum degree 0.05 MPa, and lactose is added to concentrate until the relative density is 1.30 g / cm 3 The amount of lactose is 0.8% of the total weight of the ingredients. At this point, the concentration effect of the extract is optimal, the viscosity of the extract is reduced, no lumps are formed, and the active ingredients are protected to the maximum extent.

[0033] In the present invention, the extraction process is one of the important technologies to achieve the technical effect. Adding 2.0-4.0 times the amount of water as the medicinal material can not only ensure that the medicinal material is fully infiltrated and the effective ingredients are dissolved, but also avoid gelatinization caused by insufficient water or increased concentration energy consumption due to excessive water. By controlling the temperature at 99-101°C (corresponding to a steam pressure of 0.04-0.10MPa) through steam heating, it can not only maintain a slightly boiling state to promote the efficient dissolution of target components (such as flavonoids and saponins), but also avoid excessive temperature destroying heat-sensitive components or dissolving too many impurities. The setting of 2 hours per extraction covers the dissolution equilibrium point of most components, taking into account both extraction efficiency and energy consumption control. The process design of repeated extraction twice can recover more than 90% of the effective ingredients in the medicinal materials, achieving the best balance between extraction rate and production cost. The synergistic effect of these parameters not only ensures the material basis of the efficacy, but also meets the feasibility and stability requirements of industrial production. Preferably, the extraction process is to put the clean medicinal materials after the ingredients into the extraction tank, add 2.0-4.0 times the amount of water for the medicinal materials, turn on the steam heating to boil, keep warm and boil for 2 hours at a temperature of 99-101 ° C and a steam pressure of 0.04-0.10 MPa, collect the extract, filter, and place the filtrate in a clean storage tank for standby use, repeat the above extraction steps with the residue, perform a second extraction, collect the extract, filter, and merge the filtrate with the filtrate of the first extraction. More preferably, the clean medicinal materials after the ingredients are put into the extraction tank, add 3.0 times the amount of water for the medicinal materials, turn on the steam heating to boil, keep warm and boil for 2 hours at a temperature of 99-101 ° C and a steam pressure of 0.10 MPa, collect the extract, filter, and place the filtrate in a clean storage tank for standby use, repeat the above extraction steps with the residue, perform a second extraction, collect the extract, filter, and merge the filtrate with the filtrate of the first extraction.

[0034] In the present invention, the dry extract after extraction, concentration and drying is pulverized, and the dry extract is pulverized through 40-80 meshes before discharging to achieve uniform fineness of dry extract powder, and the pulverized dry extract powder is collected and packaged.

[0035] In the present invention, the ingredients are 15 pure medicinal materials in the Zhongsheng Pills, including dandelion, siler, viola yedoensis, bupleurum, red peony root, scrophularia, angelica, angelica dahurica, isatis root, knotweed, selfheal, scutellaria, honeysuckle, mulberry and trichosanthes.

[0036] In a preferred embodiment of the present invention, a method for preparing a dry powder of Zhongsheng Wan extract is provided, comprising the following steps: batching, extraction, concentration, belt vacuum drying, pulverization and packaging.

[0037] The ingredients are 15 kinds of pure medicinal materials, including dandelion, siler, viola yedoensis, bupleurum, red peony root, figwort, angelica, angelica dahurica, isatis root, knotweed, selfheal, scutellaria, honeysuckle, mulberry, and trichosanthes root.

[0038] Put the clean medicinal materials after batching into the extraction tank, add 3.0 times the amount of water of the medicinal materials, turn on the steam and heat to boiling, keep warm and decoct for 2 hours at a temperature of 99-101 ° C and a steam pressure of 0.10 MPa, collect the extract, filter, and place the filtrate in a clean storage tank for later use. Repeat the above extraction steps with the medicinal residue for the second extraction, collect the extract, filter, and combine the filtrate with the filtrate of the first extraction;

[0039] The concentration is to add lactose to the extract under the conditions of temperature 75°C, steam pressure 0.10MPa and vacuum degree 0.05MPa, and concentrate to a relative density of 1.30g / cm 3 , the amount of lactose is 0.8% of the total mass of the ingredient medicinal materials;

[0040] The belt vacuum drying adopts a multi-stage drying method:

[0041] Stage 1: vacuum degree -0.4MPa, drying temperature 45℃, conveyor speed 0.55m / min, drying time 15min;

[0042] The second stage: vacuum degree -0.2MPa, drying temperature 60℃, conveyor speed 0.35m / min, drying time 10min;

[0043] The third stage: vacuum degree -0.1MPa, drying temperature 75℃, conveyor belt speed 0.15m / min, drying time 5min, the moisture content of the dry paste powder is less than 5.0%;

[0044] The crushing and packaging are as follows: the dry extract is crushed through 40-80 meshes during the discharge process, and the crushed dry extract is collected and packaged.

[0045] The present invention has the following beneficial effects compared to the prior art:

[0046] 1. In the drying process of the Zhongsheng Pills extract, the present invention adopts a multi-stage drying method to maximize the protection of the effective ingredients (such as saponins, volatile oils, etc.) in the Zhongsheng Pills dry extract powder. At the same time, it shortens the drying time, improves efficiency, and reduces the wall hanging phenomenon during the extract drying process.

[0047] 2. The present invention adds lactose during the concentration process of the Zhongsheng Pills extract, thereby reducing the viscosity of the extract and preventing agglomeration, thereby improving work efficiency and ensuring maximum protection of the active ingredients.

[0048] 3. The content of active ingredients in the Zhongsheng Pills prepared by the present invention is high, and the active ingredients contained in each medicinal material can be utilized to a greater extent, and they can better play a synergistic role, more effectively exert antibacterial activity, enhance the body's immune function, and have better efficacy. DETAILED DESCRIPTION

[0049] The present invention will be further described in detail below with reference to examples, but the embodiments of the present invention are not limited thereto.

[0050] Example 1

[0051] 1. Ingredients: 330g of dandelion, 100g of siler, 330g of violet yedoensis, 100g of bupleurum, 100g of red peony root, 100g of figwort, 100g of angelica, 30g of angelica dahurica, 130g of isatis root, 130g of knotweed, 65g of prunella vulgaris, 100g of scutellaria, 130g of soapberry thorn, 130g of mulberry, 100g of radix trichosanthis,

[0052] 2. Extraction: Put the clean medicinal materials after batching into the extraction tank, add 6L of water, turn on the steam and heat to boiling, keep warm and decoct at a temperature of 99-101℃ and a steam pressure of 0.10MPa for 2 hours, collect the extract, filter, and place the filtrate in a clean storage tank for later use. Repeat the above extraction steps with the medicinal residue for the second extraction, collect the extract, filter, and combine the filtrate with the filtrate from the first extraction;

[0053] 3. Concentration: Add 15.8g lactose to the extract at a temperature of 75℃, a steam pressure of 0.10MPa, and a vacuum degree of 0.05MPa, and concentrate to a relative density of 1.30g / cm 3 ;

[0054] 4. Drying: Belt vacuum drying adopts multi-stage drying method

[0055] Stage 1: vacuum degree -0.4MPa, drying temperature 45℃, conveyor speed 0.55m / min, drying time 15min;

[0056] The second stage: vacuum degree -0.2MPa, drying temperature 60℃, conveyor speed 0.35m / min, drying time 10min;

[0057] The third stage: vacuum degree -0.1MPa, drying temperature 75℃, conveyor belt speed 0.15m / min, drying time 5min, the moisture content of the dry paste powder is less than 5.0%;

[0058] 5. Crushing and packaging: During the discharge process, the dry extract is crushed through 40-80 mesh, and 405g of the crushed dry extract powder is collected and packaged.

[0059] Example 2

[0060] 1. Ingredients: The ingredients and steps are as shown in Example 1;

[0061] 2. Extraction: Place the cleaned medicinal materials after batching into an extraction tank, add 4L of water, turn on the steam and heat to boiling, keep warm and decoct at a temperature of 99-101°C and a steam pressure of 0.04MPa for 2 hours, collect the extract, filter, and place the filtrate in a clean storage tank for later use. Repeat the above extraction steps with the medicinal residue for a second extraction, collect the extract, filter, and combine the filtrate with the filtrate from the first extraction;

[0062] 3. Concentration: Add 9.9g lactose to the extract at a temperature of 60℃, a steam pressure of 0.04MPa, and a vacuum degree of 0.02MPa, and concentrate to a relative density of 1.25g / cm 3 ;

[0063] 4. Drying: Belt vacuum drying adopts multi-stage drying method

[0064] The first stage: vacuum degree -0.35MPa, drying temperature 40℃, conveyor speed 0.5m / min, drying time 10min;

[0065] The second stage: vacuum degree -0.15MPa, drying temperature 55℃, conveyor speed 0.3m / min, drying time 5min;

[0066] The third stage: vacuum degree -0.05MPa, drying temperature 70℃, conveyor belt speed 0.1m / min, drying time 5min, the moisture content of the dry paste powder is less than 5.0%;

[0067] 5. Crushing and packaging: During the discharge process, the dry extract is crushed through 40-80 mesh, and 385g of the crushed dry extract powder is collected and packaged.

[0068] Example 3

[0069] 1. Ingredients: The ingredients and steps are as shown in Example 1;

[0070] 2. Extraction: Place the cleaned medicinal materials after batching into an extraction tank, add 8L of water, turn on the steam and heat to boiling, keep warm and decoct at a temperature of 99-101°C and a steam pressure of 0.10MPa for 2 hours, collect the extract, filter, and place the filtrate in a clean storage tank for later use. Repeat the above extraction steps with the medicinal residue for a second extraction, collect the extract, filter, and combine the filtrate with the filtrate from the first extraction;

[0071] 3. Concentration: Add 17.8g lactose to the extract at a temperature of 85℃, a steam pressure of 0.12MPa, and a vacuum degree of 0.09MPa, and concentrate to a relative density of 1.35g / cm 3 ;

[0072] 4. Drying: Belt vacuum drying adopts multi-stage drying method

[0073] The first stage: vacuum degree -0.45MPa, drying temperature 50℃, conveyor speed 0.6m / min, drying time 20min;

[0074] The second stage: vacuum degree -0.25MPa, drying temperature 65℃, conveyor speed 0.4m / min, drying time 15min;

[0075] The third stage: vacuum degree -0.15MPa, drying temperature 80℃, conveyor belt speed 0.2m / min, drying time 10min, the moisture content of the dry paste powder is less than 5.0%;

[0076] 5. Crushing and packaging: During the discharge process, the dry extract is crushed through 40-80 mesh, and 398g of the crushed dry extract powder is collected and packaged.

[0077] Example 4

[0078] 1. Ingredients: The ingredients and steps are as shown in Example 1;

[0079] 2. Extraction: Put the clean medicinal materials after batching into the extraction tank, add 5L of water, turn on the steam and heat to boiling, keep warm and decoct at a temperature of 99-101℃ and a steam pressure of 0.06MPa for 2 hours, collect the extract, filter, and place the filtrate in a clean storage tank for later use. Repeat the above extraction steps with the medicinal residue for the second extraction, collect the extract, filter, and combine the filtrate with the filtrate from the first extraction;

[0080] 3. Concentration: Add 11.9g lactose to the extract at a temperature of 65℃, a steam pressure of 0.06MPa, and a vacuum degree of 0.04MPa, and concentrate to a relative density of 1.32g / cm 3 ;

[0081] 4. Drying: Belt vacuum drying adopts multi-stage drying method

[0082] Stage 1: vacuum degree -0.4MPa, drying temperature 45℃, conveyor speed 0.55m / min, drying time 15min;

[0083] The second stage: vacuum degree -0.15MPa, drying temperature 55℃, conveyor speed 0.3m / min, drying time 5min;

[0084] The third stage: vacuum degree -0.05MPa, drying temperature 70℃, conveyor belt speed 0.1m / min, drying time 5min, the moisture content of the dry paste powder is less than 5.0%;

[0085] 5. Crushing and packaging: During the discharge process, the dry extract is crushed through 40-80 mesh, and 392g of the crushed dry extract powder is collected and packaged.

[0086] Example 5

[0087] 1. Ingredients: The ingredients and steps are as shown in Example 1;

[0088] 2. Extraction: Place the cleaned medicinal materials after batching into an extraction tank, add 7L of water, turn on the steam and heat to boiling, keep warm and decoct at a temperature of 99-101°C and a steam pressure of 0.08MPa for 2 hours, collect the extract, filter, and place the filtrate in a clean storage tank for later use. Repeat the above extraction steps with the medicinal residue for a second extraction, collect the extract, filter, and combine the filtrate with the filtrate from the first extraction;

[0089] 3. Concentration: Add 13.8g lactose to the extract at a temperature of 80℃, a steam pressure of 0.08MPa, and a vacuum degree of 0.08MPa, and concentrate to a relative density of 1.34g / cm 3 ;

[0090] 4. Drying: Belt vacuum drying adopts multi-stage drying method

[0091] The first stage: vacuum degree -0.35MPa, drying temperature 40℃, conveyor speed 0.6m / min, drying time 20min;

[0092] The second stage: vacuum degree -0.25MPa, drying temperature 65℃, conveyor speed 0.35m / min, drying time 15min;

[0093] The third stage: vacuum degree -0.1MPa, drying temperature 80℃, conveyor belt speed 0.2m / min, drying time 5min, the moisture content of the dry paste powder is less than 5.0%;

[0094] 5. Crushing and packaging: During the discharge process, the dry extract is crushed through 40-80 mesh, and 387g of the crushed dry extract powder is collected and packaged.

[0095] Comparative Example 1

[0096] 1. Ingredients: The ingredients and steps are as shown in Example 1;

[0097] 2. Extraction: Put the clean medicinal materials after batching into the extraction tank, add 2L of water, turn on the steam and heat to boiling, keep warm and decoct at a temperature of 99-101℃ and a steam pressure of 0.02MPa for 2 hours, collect the extract, filter, and place the filtrate in a clean storage tank for later use. Repeat the above extraction steps with the medicinal residue for the second extraction, collect the extract, filter, and combine the filtrate with the filtrate from the first extraction;

[0098] 3. Concentration: Add 5.9g lactose to the extract at a temperature of 50℃, a steam pressure of 0.02MPa, and a vacuum degree of 0.01MPa, and concentrate to a relative density of 1.00g / cm 3;

[0099] 4. Drying: Belt vacuum drying adopts multi-stage drying method

[0100] Stage 1: vacuum degree -0.3MPa, drying temperature 35℃, conveyor speed 0.4m / min, drying time 5min;

[0101] The second stage: vacuum degree -0.1MPa, drying temperature 50℃, conveyor speed 0.2m / min, drying time 3min;

[0102] The third stage: vacuum degree -0.01MPa, drying temperature 65℃, conveyor belt speed 0.05m / min, drying time 3min, the moisture content of the dry paste powder is less than 5.0%;

[0103] 5. Crushing and packaging: During the discharge process, the dry extract is crushed through 40-80 mesh, and 250g of the crushed dry extract powder is collected and packaged.

[0104] Compared with Example 1, the amount of lactose added in the concentration process of Comparative Example 1 is less, and the vacuum degree, temperature, conveyor speed and drying time are shorter during the multi-stage drying process.

[0105] Comparative Example 2

[0106] 1. Ingredients: The ingredients and steps are as shown in Example 1;

[0107] 2. Extraction: Put the clean medicinal materials after batching into the extraction tank, add 10L of water, turn on the steam heating to boiling, keep warm and decoct at a temperature of 99-101℃ and a steam pressure of 0.15MPa for 2 hours, collect the extract, filter, and place the filtrate in a clean storage tank for later use. Repeat the above extraction steps with the medicinal residue for the second extraction, collect the extract, filter, and combine the filtrate with the filtrate from the first extraction;

[0108] 3. Concentration: Add 23.7g lactose to the extract at a temperature of 90℃, a steam pressure of 0.15MPa, and a vacuum degree of 0.15MPa, and concentrate to a relative density of 1.50g / cm 3 ;

[0109] 4. Drying: Belt vacuum drying adopts multi-stage drying method

[0110] The first stage: vacuum degree -0.5MPa, drying temperature 60℃, conveyor speed 0.7m / min, drying time 30min;

[0111] The second stage: vacuum degree -0.3MPa, drying temperature 70℃, conveyor speed 0.5m / min, drying time 20min;

[0112] The third stage: vacuum degree -0.2MPa, drying temperature 90℃, conveyor belt speed 0.3m / min, drying time 15min, the moisture content of the dry paste powder is less than 5.0%;

[0113] 5. Crushing and packaging: During the discharge process, the dry extract is crushed through 40-80 mesh, and 356g of the crushed dry extract powder is collected and packaged.

[0114] Compared with Example 1, in Comparative Example 2, a larger amount of lactose was added during the concentration process, and during the multi-stage drying process, the vacuum degree was higher, the temperature was higher, the conveyor belt speed was faster, and the drying time was longer.

[0115] Comparative Example 3

[0116] 1. Ingredients: The ingredients and steps are as shown in Example 1;

[0117] 2. Extraction: Put the clean medicinal materials after batching into the extraction tank, add 6L of water, turn on the steam and heat to boiling, keep warm and decoct at a temperature of 99-101℃ and a steam pressure of 0.10MPa for 2 hours, collect the extract, filter, and place the filtrate in a clean storage tank for later use. Repeat the above extraction steps with the medicinal residue for the second extraction, collect the extract, filter, and combine the filtrate with the filtrate from the first extraction;

[0118] 3. Concentration: Add 15.8g lactose to the extract at a temperature of 75℃, a steam pressure of 0.10MPa, and a vacuum degree of 0.05MPa, and concentrate to a relative density of 1.30g / cm 3 ;

[0119] 4. Drying: vacuum degree -0.1MPa, drying temperature 80℃, conveyor speed 0.25m / min, drying time 50min;

[0120] 5. Crushing and packaging: During the discharge process, the dry extract is crushed through 40-80 mesh, and 323g of the crushed dry extract powder is collected and packaged.

[0121] Compared with Example 1, Comparative Example 3 did not adopt multi-stage drying during the drying process.

[0122] Comparative Example 4

[0123] The preparation steps were as described in Example 1. In Comparative Example 4, compared with Example 1, no lactose was added during the concentration process, and 303 g of dry paste powder was finally collected.

[0124] Example 6 Quality Inspection of Zhongsheng Pills Dry Extract

[0125] The quality of the dried extracts of the Zhongsheng Pills prepared in Examples 1-5 and Comparative Examples 1-4 was investigated. The results are as follows:

[0126] Table 1 Quality inspection of Zhongsheng pills dry extract

[0127]

[0128]

[0129] From the above results, it can be seen that the dry extracts of the living beings pills prepared in Examples 1-5 and Comparative Examples 1-4 are all brown in color, and Comparative Example 2 is dark brown. The analysis shows that this is because the concentration and drying temperatures are high, the time is long, and some of the active substances are oxidized. The dry extract of the living beings pills obtained in Comparative Example 1 is compacted in shape, easy to absorb moisture, sticky in texture, and has a moist feeling. Analysis shows that the amount of lactose added is small, the concentration and drying temperatures are low, the time is short, and the humidity of the dry extract of the living beings pills is high. The dry extract of the living beings pills obtained in Comparative Example 4 is compacted in shape, easy to absorb moisture, sticky in texture, and has a moist feeling. Analysis shows that no lactose was added during the concentration process, and the extract particles melted and adhered during the drying process. At the same time, part of the extract adhered to the conveyor belt, affecting the yield. Examples 1-5 are preferred schemes in this scheme, and various parameters in Example 1, including various parameters in the concentration and drying processes, are all the most preferred. For example, suitable lactose is used in the concentration process to improve the physical properties of the extract, reduce the viscosity, and at the same time improve the fluidity of the concentrate, facilitate the transportation and spreading of the drying process, and prevent agglomeration. Multi-stage drying is used in the belt vacuum drying process to protect the effective ingredients in the Zhongsheng Pills dry extract powder (such as saponin components, volatile oil components, etc.). At the same time, the drying time is shortened, the efficiency is improved, and the wall hanging phenomenon during the extract drying process is reduced. The overall combination of the above conditions makes the obtained Zhongsheng Pills dry extract reach the optimal level.

[0130] Example 7 Quality Inspection of Zhongsheng Pills Dry Extract

[0131] The dry extract of Zhongsheng Pills prepared in Example 1 and Comparative Example 3 was used to prepare Zhongsheng Pills with reference to the preparation method of Zhongsheng Pills in Chinese Patent ZL201010237529.7. The active content of the Zhongsheng Pills preparation was determined and compared according to high performance liquid chromatography (Appendix VID of Part 1 of the Pharmacopoeia of the People's Republic of China 2020 edition).

[0132] Table 2 Test results of each component of each group of Zhongsheng pill preparations (unit: mg / pill)

[0133]

[0134] The above results indicate that the active ingredient content of the Zhongsheng Pills prepared in Example 1 is further improved compared to the new Zhongsheng Pills prepared in ZL201010237529.7. Compared to the new Zhongsheng Pills prepared in ZL201010237529.7, the main active ingredient content of the Zhongsheng Pills prepared in Example 1 has increased by 136%, caffeic acid by 97%, ferulic acid by 119%, polydatin by 51%, baicalin by 33%, paeoniflorin by 45%, and harpagoside by 68%. Since the Zhongsheng Pills prepared in Comparative Example 3 did not employ multi-stage drying, the main active ingredient content was not significantly improved compared to the new Zhongsheng Pills prepared in ZL201010237529.7.

[0135] Example 8 Antibacterial effect experiment

[0136] With reference to Chinese ZL201010237529.7, nine representative strains, primarily common pathogens and opportunistic pathogens of respiratory tract infections, were selected for this experiment. These strains include Staphylococcus aureus (26112-5), beta-hemolytic Streptococcus (32210), Escherichia coli (44113-5), Pseudomonas aeruginosa (10211), Candida albicans (98001), alpha-hemolytic Streptococcus (32209), Corynebacterium diphtheriae (38101), Streptococcus pneumoniae (31001), and Coccus catarrhalis. Coccus catarrhalis was isolated from a throat specimen by the bacteriological laboratory. Candida albicans was kindly provided by the Guangzhou Institute for Drug Control. The remaining strains were obtained from the National Institute for the Control of Pharmaceutical and Biological Products in Beijing. During the experiment, the Zhongsheng Pills prepared in Example 1 and the new Zhongsheng Pills prepared in ZL201010237529.7 were prepared in meat paste soup to a concentration of 5.5g of the raw medicinal material per 5.5ml, i.e., 1g / ml. The mixture was sterilized by circulating steam. For tests on Streptococci, 1% glucose was added to the sterilized solution. For tests on Pneumococci and Corynebacterium diphtheriae, 10% rabbit serum was added. For tests on Candida albicans, the solution was diluted with Sabouraud broth. The blank control consisted of a medium containing no drug. 0.1ml of the test bacterial solution (8-hour culture) at a 1:2000 dilution was added to each concentration tube in each row of the drug solution and the blank control tube. The tubes were incubated at 37°C for 24 hours and the results were observed. The minimum inhibitory concentration (MIC) was determined. The MIC is the minimum drug concentration required to completely inhibit the growth of the test bacteria. The results are shown in Table 3.

[0137] Table 3 Antibacterial effect of Zhongsheng Pills

[0138]

[0139] From the above results, it can be seen that Zhongsheng Pills have a certain antibacterial effect on the tested bacteria, mainly the common pathogens and conditional pathogens that cause respiratory tract infections. The minimum inhibitory concentration (MIC) of the new Zhongsheng Pills prepared by ZL201010237529.7 for each bacteria is between 0.025g / ml and 0.4g / ml, among which it has no inhibitory effect on Escherichia coli. The minimum inhibitory concentration (MIC) of the Zhongsheng Pills prepared in Example 1 for each bacteria is between 0.010g / ml and 0.3g / ml. For common pathogens and conditional pathogens that cause respiratory tract infections, the Zhongsheng Pills prepared in Example 1 show a better antibacterial effect. The above shows that the content of the pharmacologically active components of the prepared Zhongsheng Pills is high when using the dry extract of the Zhongsheng Pills prepared by the present invention, and the active ingredients contained in each medicinal material can be utilized to a greater extent, and they can better play a synergistic role with more effective antibacterial activity.

[0140] The above embodiments are preferred implementation modes of the present invention, but the implementation modes of the present invention are not limited to the above embodiments. Any other changes, modifications, substitutions, combinations, and simplifications that do not deviate from the spirit and principles of the present invention should be considered as equivalent replacement methods and are included in the scope of protection of the present invention.

Claims

1. A method for preparing a dry extract powder of Zhongsheng Pills, characterized in that: The method comprises the following steps: batching, extraction, concentration, belt vacuum drying, crushing and packaging, wherein the belt vacuum drying adopts a multi-stage drying method.

2. The preparation method according to claim 1, characterized in that The belt vacuum drying adopts a multi-stage drying method: The first stage: vacuum degree -0.35~-0.45MPa, drying temperature 40-50℃, conveyor speed 0.5-0.6m / min, drying time 10-20min; The second stage: vacuum degree -0.15~-0.25MPa, drying temperature 55-65℃, conveyor speed 0.3-0.4m / min, drying time 5-15min; The third stage: vacuum degree -0.05~-0.15MPa, drying temperature 70-80℃, conveyor belt speed 0.1-0.2m / min, drying time 5-10min, and the moisture content of the dry paste powder is less than 8.0%.

3. The preparation method according to claim 2, characterized in that The belt vacuum drying adopts a multi-stage drying method: Stage 1: vacuum degree -0.4MPa, drying temperature 45℃, conveyor speed 0.55m / min, drying time 15min; The second stage: vacuum degree -0.2MPa, drying temperature 60℃, conveyor speed 0.35m / min, drying time 10min; The third stage: vacuum degree -0.1MPa, drying temperature 75℃, conveyor belt speed 0.15m / min, drying time 5min, moisture content of dry paste powder is less than 5.0%.

4. The preparation method according to claim 1, characterized in that The extraction is: Put the clean medicinal materials after batching into the extraction tank, add 2.0-4.0 times the amount of water of the medicinal materials, turn on the steam and heat to boiling, keep warm and decoct at a temperature of 99-101 ° C and a steam pressure of 0.04-0.10 MPa for 2 hours, collect the extract, filter, and place the filtrate in a clean storage tank for later use. Repeat the above extraction steps with the medicinal residue for the second extraction, collect the extract, filter, and combine the filtrate with the filtrate of the first extraction.

5. The preparation method according to claim 1, characterized in that The extraction is: Put the clean medicinal materials after batching into the extraction tank, add 3.0 times the amount of water of the medicinal materials, turn on the steam and heat to boiling, keep warm and decoct at a temperature of 99-101℃ and a steam pressure of 0.10MPa for 2 hours, collect the extract, filter, and place the filtrate in a clean storage tank for later use. Repeat the above extraction steps with the medicinal residue for the second extraction, collect the extract, filter, and combine the filtrate with the filtrate of the first extraction.

6. The preparation method according to claim 1, characterized in that The concentration is to add lactose to the extract under the conditions of temperature of 60-85°C, steam pressure of 0.04-0.12MPa and vacuum degree of 0.02-0.09MPa, and concentrate to a relative density of 1.25-1.35g / cm 3 The amount of lactose is 0.5-0.9% of the total mass of the medicinal materials.

7. The preparation method according to claim 6, characterized in that The concentration is to add lactose to the extract under the conditions of temperature 75°C, steam pressure 0.10MPa and vacuum degree 0.05MPa, and concentrate to a relative density of 1.30g / cm 3 The amount of lactose is 0.8% of the total mass of the ingredient medicinal materials.

8. The preparation method according to claim 1, characterized in that The crushing and packaging are as follows: the dry extract is crushed through 40-80 meshes during the discharge process, and the crushed dry extract is collected and packaged.

9. The preparation method according to claim 1, characterized in that The ingredients are 15 pure medicinal materials including dandelion, siler, viola yedoensis, bupleurum, red peony root, scrophularia, angelica, angelica dahurica, isatis root, knotweed, selfheal, scutellaria, soapberry thorn, mulberry and trichosanthes root.

10. A method for preparing a dry extract powder of Zhongsheng Pills, characterized in that: The process includes the following steps: batching, extraction, concentration, belt vacuum drying, crushing and packaging. The ingredients are 15 kinds of pure medicinal materials, including dandelion, siler, viola yedoensis, bupleurum, red peony root, figwort, angelica, angelica dahurica, isatis root, knotweed, selfheal, scutellaria, honeysuckle, mulberry, and trichosanthes root. Put the clean medicinal materials after batching into the extraction tank, add 3.0 times the amount of water of the medicinal materials, turn on the steam and heat to boiling, keep warm and decoct for 2 hours at a temperature of 99-101 ° C and a steam pressure of 0.10 MPa, collect the extract, filter, and place the filtrate in a clean storage tank for later use. Repeat the above extraction steps with the medicinal residue for the second extraction, collect the extract, filter, and combine the filtrate with the filtrate of the first extraction; The concentration is to add lactose to the extract under the conditions of temperature 75°C, steam pressure 0.10MPa and vacuum degree 0.05MPa, and concentrate to a relative density of 1.30g / cm 3 , the amount of lactose is 0.8% of the total mass of the ingredient medicinal materials; The belt vacuum drying adopts a multi-stage drying method: Stage 1: vacuum degree -0.4MPa, drying temperature 45℃, conveyor speed 0.55m / min, drying time 15min; The second stage: vacuum degree -0.2MPa, drying temperature 60℃, conveyor speed 0.35m / min, drying time 10min; The third stage: vacuum degree -0.1MPa, drying temperature 75℃, conveyor belt speed 0.15m / min, drying time 5min, the moisture content of the dry paste powder is less than 5.0%; The crushing and packaging are as follows: the dry extract is crushed through 40-80 meshes during the discharge process, and the crushed dry extract is collected and packaged.

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