阅读说明：本技术 一种超微粉代替部分辅料的茯苓配方颗粒的制备方法 (Preparation method of poria cocos formula granules with ultrafine powder replacing part of auxiliary materials ) 是由 谢彦兵 李海兵 于 2021-02-02 设计创作，主要内容包括：本发明属于中药配方颗粒技术领域,具体涉及一种用超微粉代替部分辅料的茯苓配方颗粒的制备方法,包括如下步骤：(1)取茯苓饮片-研磨-静置-NaAc-HAc缓冲溶液调pH-混合酶液-酶解-灭活-室温下抽滤-滤渣-85％的乙醇微波-合并滤液,浓缩干燥,得到茯苓浓缩粉-NaOH-乙醇水浴提取-离心取上层清液浓缩-醇沉-离心,得到茯苓精制粉；(2)另取茯苓饮片,制得茯苓浓缩液-向茯苓浓缩液中加入药用辅料和辅料添加剂,制得茯苓超微研磨粉；(3)将茯苓精制粉和茯苓超微研磨粉混合均匀,经过10～30目筛,制粒,整粒,得到茯苓配方颗粒。本发明方法明显增加了有效成分茯苓多糖的含量,减少了辅料使用量。(The invention belongs to the technical field of traditional Chinese medicine formula granules, and particularly relates to a preparation method of poria cocos formula granules with ultrafine powder replacing part of auxiliary materials, which comprises the following steps: (1) taking poria cocos decoction pieces, grinding, standing, adjusting pH with NaAc-HAc buffer solution, mixing enzyme solution, performing enzymolysis, inactivating, performing suction filtration at room temperature, filtering residues, performing microwave treatment on 85% ethanol, mixing filtrate, concentrating and drying to obtain poria cocos concentrated powder, performing water bath extraction with NaOH-ethanol, centrifuging, taking supernatant, concentrating, performing alcohol precipitation, and centrifuging to obtain poria cocos refined powder; (2) preparing Poria decoction pieces into Poria concentrated solution, adding medicinal adjuvants and adjuvant additives into Poria concentrated solution, and making into Poria ultramicro ground powder; (3) and uniformly mixing the poria cocos refined powder and the poria cocos superfine grinding powder, sieving with a 10-30-mesh sieve, granulating, and finishing to obtain the poria cocos formula granules. The method of the invention obviously increases the content of the effective component pachyman and reduces the use amount of auxiliary materials.)

1. A preparation method of poria cocos formula granules with ultrafine powder replacing part of auxiliary materials is characterized by comprising the following steps:

(1) taking poria cocos decoction pieces, grinding the poria cocos decoction pieces into powder, adding 3-5 times of water, standing for 20-30 min, firstly adjusting the pH value to 5.6-6.2 by using NaAc-HAc buffer solution, then adding a proper amount of mixed enzyme solution, carrying out enzymolysis for 20-30 min at a constant temperature at the temperature of 45-50 ℃, inactivating at 100 ℃, and carrying out suction filtration at room temperature; adding 3-5 times of 85% ethanol into filter residue, performing microwave-assisted treatment for 10-20 min, mixing filtrates, concentrating, and drying to obtain Poria cocos concentrated powder;

adding 1.5mol/L NaOH-ethanol solution with the weight 1-3 times of the weight of the tuckahoe concentrated powder, extracting for 3-5 h in water bath at 95 ℃, centrifuging for 30-50 min, taking supernatant, concentrating to 30ml, adding 60-90 ml ethanol for precipitation, and centrifuging to obtain tuckahoe refined powder;

(2) crushing another poria cocos decoction piece by using a high-speed crusher, sieving the crushed poria cocos decoction piece by using a sieve of 80-120 meshes, then carrying out superfine crushing on the crushed decoction piece, adjusting the frequency of a grading impeller to be 30-40 Hz, collecting superfine powder with the particle size of 200-400 meshes, and adding deionized water with the weight of 1-3 times that of the poria cocos superfine powder to prepare a poria cocos concentrated solution;

under strong stirring, uniformly mixing reducing sugar and cyclodextrin, standing, precipitating crystals, and drying at 80-90 ℃ to obtain an auxiliary material additive;

adding medicinal auxiliary materials and auxiliary material additives into the poria cocos concentrated solution, heating and boiling for 10-20 min, standing for 20-30 min, uniformly stirring, grinding for 1-3 times by using a colloid mill for 40-50 min each time to obtain a poria cocos superfine grinding solution C, and performing spray drying to obtain poria cocos superfine grinding powder;

(3) and uniformly mixing the poria cocos refined powder and the poria cocos superfine grinding powder, sieving with a 10-30-mesh sieve, granulating, and finishing to obtain the poria cocos formula granules.

2. The preparation method of the poria cocos formula particle with the ultrafine powder replacing part of auxiliary materials according to claim 1 is characterized in that the mixed enzyme liquid is prepared by mixing cellulase, plant hydrolase and amylase according to a mass ratio of 1-3: 4-8: 3-5, wherein the cellulase is food grade, the enzyme activity is 15000U/g, the plant hydrolase is food grade, the enzyme activity is 10000U/g, the amylase is food grade, and the enzyme activity is 10000-20000U/ml.

3. The method for preparing the poria cocos formula particle with the superfine powder replacing part of the auxiliary materials according to claim 1, wherein the reducing sugar is one of xylose, rhamnose and glucose.

4. The preparation method of the poria cocos formula particle with the superfine powder replacing part of auxiliary materials, as claimed in claim 1, is characterized in that the mass ratio of the reducing sugar to the cyclodextrin is 6-8: 1-3.

5. The preparation method of the poria cocos formula particle with the superfine powder replacing part of the auxiliary materials, as claimed in claim 1, is characterized in that the air inlet temperature of the spray drying in the step (2) is 120-140 ℃, the air outlet temperature is 100-110 ℃, and the feeding speed is 2-3 ml/min.

Technical Field

The invention relates to a preparation method of traditional Chinese medicine granules, in particular to a preparation method of poria cocos formula granules with ultrafine powder instead of part of auxiliary materials, and belongs to the technical field of traditional Chinese medicine formula granules.

Background

Poria is a common Chinese medicinal material, and more than 60% of the Chinese medicinal formulas are matched with Poria, so that the dosage is very large. Poria is a facultative parasitic bacterium, the wild Poria has a very small amount, most of the Poria used at present is cultivated, and the conventional cultivation adopts pine tree segment wood for production. According to the medical department, about 2 ten thousand tons of dried tuckahoe are required every year in China, and about 20 cubic meters of pine are required for producing 1 ton of dried tuckahoe, so that the pine used for producing tuckahoe reaches 40 ten thousand cubic meters every year. Under the condition that China has no plan for approval, if pine trees are cut down privately, the forestry department can collect high penalty, and thus the contradiction between tuckahoe planting and forestry is more and more prominent. However, in recent years, with the rapid development of economy in China, the living standard of people is greatly improved, the dual-purpose resource of medicine and food is more and more tense, and the price is continuously increased, so that the reasonable utilization of the poria cocos medicinal material resource is urgent.

The traditional Chinese medicine formula particle is an improvement of traditional Chinese medicine decoction piece dosage form guided by the traditional Chinese medicine theory, takes the traditional Chinese medicine decoction pieces processed according to the standard as raw materials, adopts the processes of dynamic extraction, low-temperature concentration, spray drying and the like to prepare the particle, and is clinically used for replacing the traditional Chinese medicine decoction pieces. The traditional Chinese medicine formula granule has the advantages of flexible formula, convenient taking, small dosage, controllable quality, easy storage, convenient carrying and the like.

The tuckahoe prescription granule is prepared by the traditional method that tuckahoe decoction pieces are extracted by adding water, concentrated, dried, granulated and the like, tuckahoe mainly contains beta-pachyman and is insoluble in water, the water extraction yield is very low and is usually only about 1 to 2 percent, the daily dosage of tuckahoe is 10 to 15g, each bag of tuckahoe prescription granule is equivalent to 10g of decoction pieces, each bag of tuckahoe prescription granule is only 0.1 to 0.2g of tuckahoe pure paste powder, the minimum packaging amount of the granule is 0.7g due to the limitation of a packaging machine, and at least 0.5g of auxiliary materials are required to be added into each bag according to the packaging amount. Therefore, on one hand, the extraction rate of the poria cocos decoction pieces is low, more than 10 kilograms of extract can be obtained per 1 ton of poria cocos decoction pieces, most of beta-pachyman is discarded as medicine residues, a large amount of medicinal materials are wasted, and a large amount of energy is consumed in the extraction process; on the other hand, in order to fill the package, a large amount of auxiliary materials are added, 50 tons of auxiliary materials are consumed each year according to the current sale amount of 1 hundred million bags each year, and a large amount of production cost is increased.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provides a preparation method of poria cocos formula granules with ultrafine powder replacing part of auxiliary materials.

In order to achieve the purpose, the technical scheme adopted by the invention is as follows:

a preparation method of Poria cocos formula granules with ultrafine powder replacing part of auxiliary materials comprises the following steps:

(1) taking poria cocos decoction pieces, grinding the poria cocos decoction pieces into powder, adding 3-5 times of water, standing for 20-30 min, firstly adjusting the pH value to 5.6-6.2 by using NaAc-HAc buffer solution, then adding a proper amount of mixed enzyme solution, carrying out enzymolysis for 20-30 min at a constant temperature at the temperature of 45-50 ℃, inactivating at 100 ℃, and carrying out suction filtration at room temperature; adding 3-5 times of 85% ethanol into filter residue, performing microwave-assisted treatment for 10-20 min, mixing filtrates, concentrating, and drying to obtain Poria cocos concentrated powder;

adding 1.5mol/L NaOH-ethanol solution with the weight 1-3 times of the weight of the tuckahoe concentrated powder, extracting for 3-5 h in water bath at 95 ℃, centrifuging for 30-50 min, taking supernatant, concentrating to 30ml, adding 60-90 ml ethanol for precipitation, and centrifuging to obtain tuckahoe refined powder;

(2) crushing another poria cocos decoction piece by using a high-speed crusher, sieving the crushed poria cocos decoction piece by using a sieve of 80-120 meshes, then carrying out superfine crushing on the crushed decoction piece, adjusting the frequency of a grading impeller to be 30-40 Hz, collecting superfine powder with the particle size of 200-400 meshes, and adding deionized water with the weight of 1-3 times that of the poria cocos superfine powder to prepare a poria cocos concentrated solution;

uniformly mixing reducing sugar and cyclodextrin under strong stirring, standing, precipitating crystals, and drying at 80-90 ℃ to obtain an auxiliary material additive;

adding medicinal auxiliary materials and auxiliary material additives into the poria cocos concentrated solution, heating and boiling for 10-20 min, standing for 20-30 min, uniformly stirring, grinding for 1-3 times by using a colloid mill for 40-50 min each time to obtain a poria cocos superfine grinding solution C, and performing spray drying to obtain poria cocos superfine grinding powder;

(3) and uniformly mixing the poria cocos refined powder and the poria cocos superfine grinding powder, sieving with a 10-30-mesh sieve, granulating, and finishing to obtain the poria cocos formula granules.

Preferably, the mixed enzyme solution is prepared by mixing cellulase, plant hydrolase and amylase according to the mass ratio of 1-3: 4-8: 3-5, wherein the cellulase is food-grade, the enzyme activity is 15000U/g, the plant hydrolase is food-grade, the enzyme activity is 10000U/g, the amylase is food-grade, and the enzyme activity is 10000-20000U/ml.

Preferably, the reducing sugar is one of xylose, rhamnose and glucose.

Preferably, the mass ratio of the reducing sugar to the cyclodextrin is 6-8: 1-3.

Preferably, the air inlet temperature of the spray drying in the step (2) is 120-140 ℃, the air outlet temperature is 100-110 ℃, and the feeding speed is 2-3 ml/min.

Compared with the prior art, the invention adopts the tuckahoe superfine grinding powder to replace auxiliary materials, thereby increasing the pachymaran content and reducing the consumption of the auxiliary materials; the main component of tuckahoe, beta-pachyman, belongs to water-insoluble pachyman, is insoluble in water, can be digested and absorbed by gastrointestinal tracts after being taken, and has pharmacological action; according to the traditional preparation process of the poria cocos formula granules, only a small amount of water-soluble polysaccharide ingredients can be extracted, most of beta-pachyman is discarded as medicine residues, the water extraction yield is low and is only 1-2%, and therefore a large amount of auxiliary materials are added. The invention adds a certain amount of tuckahoe superfine powder to replace a large amount of auxiliary materials and increase the content of tuckahoe polysaccharide components.

Detailed Description

The present invention will be further described with reference to specific embodiments for making the objects, technical solutions and advantages of the present invention more apparent, but the present invention is not limited to these examples. It should be noted that, without conflict, any combination between the embodiments or technical features described below may form a new embodiment. In the invention, all parts and percentages are mass units, and the adopted equipment, raw materials and the like can be purchased from the market or are commonly used in the field. The methods in the following examples are conventional in the art unless otherwise specified.

Example 1

A preparation method of Poria cocos formula granules with ultrafine powder replacing part of auxiliary materials comprises the following steps:

(1) grinding Poria decoction pieces into powder, adding 4 times of water, standing for 25min, adjusting pH to 5.9 with NaAc-HAc buffer solution, adding appropriate amount of mixed enzyme solution, performing enzymolysis at 48 deg.C for 25min, inactivating at 100 deg.C, and vacuum filtering at room temperature; adding 4 times of 85% ethanol into the residue, performing microwave-assisted treatment for 15min, mixing the filtrates, concentrating, and drying to obtain Poria concentrated powder;

the mixed enzyme solution is formed by mixing cellulase, plant hydrolase and amylase according to the mass ratio of 2: 6: 4, wherein the cellulase is food-grade, the enzyme activity is 15000U/g, the plant hydrolase is food-grade, the enzyme activity is 10000U/g, the amylase is food-grade, and the enzyme activity is 15000U/ml;

adding 2 times of 1.5mol/L NaOH-ethanol solution into Poria concentrated powder, extracting in water bath at 95 deg.C for 4 hr, centrifuging for 40min, collecting supernatant, concentrating to 30ml, adding 75ml ethanol for precipitation, and centrifuging to obtain Poria refined powder;

(2) pulverizing Poria decoction pieces with high-speed pulverizer, sieving with 100 mesh sieve, micronizing, regulating impeller frequency to 35Hz, collecting micropowder with particle diameter of 300 meshes, and adding deionized water 2 times the weight of the micropowder to obtain Poria concentrated solution;

uniformly mixing rhamnose and cyclodextrin according to the mass ratio of 6-8: 1-3 under strong stirring, standing, precipitating crystals, and drying at 85 ℃ to obtain an auxiliary material additive;

adding medicinal adjuvants and adjuvant additives into Poria concentrated solution, boiling for 15min, standing for 25min, stirring, grinding with colloid mill for 2 times, and grinding for 45min each time to obtain Poria micropowder grinding solution C, and spray drying to obtain Poria micropowder grinding powder;

the air inlet temperature of the spray drying is 130 ℃, the air outlet temperature is 105 ℃, and the feeding speed is 2.5 ml/min;

(3) mixing Poria refined powder and Poria ultramicro grinding powder uniformly, sieving with 20 mesh sieve, granulating, and grading to obtain Poria granule.

Example 2

A preparation method of Poria cocos formula granules with ultrafine powder replacing part of auxiliary materials comprises the following steps:

(1) grinding Poria decoction pieces into powder, adding 5 times of water, standing for 20min, adjusting pH to 6.2 with NaAc-HAc buffer solution, adding appropriate amount of mixed enzyme solution, performing enzymolysis at 45 deg.C for 30min, inactivating at 100 deg.C, and vacuum filtering at room temperature; adding 3 times of 85% ethanol into the residue, performing microwave-assisted treatment for 20min, mixing the filtrates, concentrating, and drying to obtain Poria concentrated powder;

the mixed enzyme liquid is formed by mixing cellulase, plant hydrolase and amylase according to the mass ratio of 3: 4: 5, wherein the cellulase is food-grade, the enzyme activity is 15000U/g, the plant hydrolase is food-grade, the enzyme activity is 10000U/g, the amylase is food-grade, and the enzyme activity is 20000U/ml;

adding 1.5mol/L NaOH-ethanol solution 3 times the weight of the Poria concentrated powder, extracting in water bath at 95 deg.C for 3 hr, centrifuging for 50min, collecting supernatant, concentrating to 30ml, adding 60ml ethanol for precipitation, and centrifuging to obtain Poria refined powder;

(2) pulverizing Poria decoction pieces with high-speed pulverizer, sieving with 120 mesh sieve, micronizing, regulating impeller frequency to 30Hz, collecting micropowder with particle diameter of 400 meshes, and adding deionized water 1 times the weight of the micropowder to obtain Poria concentrated solution;

uniformly mixing glucose and cyclodextrin according to the mass ratio of 8: 1 under strong stirring, standing, precipitating crystals, and drying at 90 ℃ to obtain an auxiliary material additive;

adding medicinal adjuvants and adjuvant additives into Poria concentrated solution, boiling for 20min, standing for 20min, stirring, grinding with colloid mill for 3 times (40 min each time) to obtain Poria micropowder grinding fluid C, and spray drying to obtain Poria micropowder grinding powder;

the air inlet temperature of the spray drying is 140 ℃, the air outlet temperature is 100 ℃, and the feeding speed is 3 ml/min;

(3) and uniformly mixing the poria cocos refined powder and the poria cocos superfine grinding powder, sieving with a 10-30-mesh sieve, granulating, and finishing to obtain the poria cocos formula granules.

Example 3

A preparation method of Poria cocos formula granules with ultrafine powder replacing part of auxiliary materials comprises the following steps:

(1) grinding Poria decoction pieces into powder, adding 3 times of water, standing for 30min, adjusting pH to 5.6 with NaAc-HAc buffer solution, adding appropriate amount of mixed enzyme solution, performing enzymolysis at 50 deg.C for 20min, inactivating at 100 deg.C, and vacuum filtering at room temperature; adding 5 times of 85% ethanol into the residue, performing microwave-assisted treatment for 10min, mixing the filtrates, concentrating, and drying to obtain Poria concentrated powder;

the mixed enzyme solution is formed by mixing cellulase, plant hydrolase and amylase according to the mass ratio of 1: 8: 3, wherein the cellulase is food-grade, the enzyme activity is 15000U/g, the plant hydrolase is food-grade, the enzyme activity is 10000U/g, the amylase is food-grade, and the enzyme activity is 10000U/ml;

adding 1.5mol/L NaOH-ethanol solution 1 times the weight of the Poria concentrated powder, extracting in water bath at 95 deg.C for 5 hr, centrifuging for 30min, collecting supernatant, concentrating to 30ml, adding 90ml ethanol for precipitation, and centrifuging to obtain Poria refined powder;

(2) pulverizing Poria decoction pieces with high-speed pulverizer, sieving with 80 mesh sieve, micronizing, regulating impeller frequency to 40Hz, collecting micropowder with particle diameter of 200 meshes, and adding deionized water 3 times the weight of the micropowder to obtain Poria concentrated solution;

uniformly mixing xylose and cyclodextrin according to the mass ratio of 6: 3 under strong stirring, standing, precipitating crystals, and drying at 80 ℃ to obtain an auxiliary material additive;

adding medicinal adjuvants and adjuvant additives into Poria concentrated solution, boiling for 10min, standing for 30min, stirring, grinding with colloid mill for 1 time and 50min each time to obtain Poria superfine powder C, and spray drying to obtain Poria superfine powder;

the air inlet temperature of the spray drying is 120 ℃, the air outlet temperature is 110 ℃, and the feeding speed is 2 ml/min;

(3) mixing Poria refined powder and Poria ultramicro grinding powder uniformly, sieving with 10 mesh sieve, granulating, and grading to obtain Poria granule.

Comparative example 1

A preparation method of Poria cocos formula granules with ultrafine powder replacing part of auxiliary materials comprises the following steps:

(1) grinding Poria decoction pieces into powder, adding 4 times of water, standing for 25min, adjusting pH to 5.9 with NaAc-HAc buffer solution, adding appropriate amount of mixed enzyme solution, performing enzymolysis at 48 deg.C for 25min, inactivating at 100 deg.C, and vacuum filtering at room temperature; adding 4 times of 85% ethanol into the residue, performing microwave-assisted treatment for 15min, mixing the filtrates, concentrating, and drying to obtain Poria concentrated powder;

the mixed enzyme solution is formed by mixing cellulase, plant hydrolase and amylase according to the mass ratio of 2: 6: 4, wherein the cellulase is food-grade, the enzyme activity is 15000U/g, the plant hydrolase is food-grade, the enzyme activity is 10000U/g, the amylase is food-grade, and the enzyme activity is 15000U/ml;

(2) pulverizing Poria decoction pieces with high-speed pulverizer, sieving with 100 mesh sieve, micronizing, regulating impeller frequency to 35Hz, collecting micropowder with particle diameter of 300 meshes, and adding deionized water 2 times the weight of the micropowder to obtain Poria concentrated solution;

uniformly mixing rhamnose and cyclodextrin according to the mass ratio of 6-8: 1-3 under strong stirring, standing, precipitating crystals, and drying at 85 ℃ to obtain an auxiliary material additive;

adding medicinal adjuvants and adjuvant additives into Poria concentrated solution, boiling for 15min, standing for 25min, stirring, grinding with colloid mill for 2 times, and grinding for 45min each time to obtain Poria micropowder grinding solution C, and spray drying to obtain Poria micropowder grinding powder;

the air inlet temperature of the spray drying is 130 ℃, the air outlet temperature is 105 ℃, and the feeding speed is 2.5 ml/min;

(3) mixing Poria concentrated powder and Poria ultramicro ground powder uniformly, sieving with 20 mesh sieve, granulating, and grading to obtain Poria granule.

Comparative example 2

A preparation method of Poria cocos formula granules with ultrafine powder replacing part of auxiliary materials comprises the following steps:

(1) grinding Poria decoction pieces into powder, adding 4 times of water, standing for 25min, adjusting pH to 5.9 with NaAc-HAc buffer solution, adding appropriate amount of mixed enzyme solution, performing enzymolysis at 48 deg.C for 25min, inactivating at 100 deg.C, and vacuum filtering at room temperature; adding 4 times of 85% ethanol into the residue, performing microwave-assisted treatment for 15min, mixing the filtrates, concentrating, and drying to obtain Poria concentrated powder;

the mixed enzyme solution is formed by mixing cellulase, plant hydrolase and amylase according to the mass ratio of 2: 6: 4, wherein the cellulase is food-grade, the enzyme activity is 15000U/g, the plant hydrolase is food-grade, the enzyme activity is 10000U/g, the amylase is food-grade, and the enzyme activity is 15000U/ml;

adding 2 times of 1.5mol/L NaOH-ethanol solution into Poria concentrated powder, extracting in water bath at 95 deg.C for 4 hr, centrifuging for 40min, collecting supernatant, concentrating to 30ml, adding 75ml ethanol for precipitation, and centrifuging to obtain Poria refined powder;

(2) pulverizing Poria decoction pieces with high-speed pulverizer, sieving with 100 mesh sieve, micronizing, regulating impeller frequency to 35Hz, collecting micropowder with particle diameter of 300 meshes, and adding deionized water 2 times the weight of the micropowder to obtain Poria concentrated solution;

adding medicinal adjuvants into Poria concentrated solution, heating and boiling for 15min, standing for 25min, stirring, grinding with colloid mill for 2 times, each for 45min to obtain Poria micropowder grinding fluid C, and spray drying to obtain Poria micropowder grinding powder;

the air inlet temperature of the spray drying is 130 ℃, the air outlet temperature is 105 ℃, and the feeding speed is 2.5 ml/min;

(3) mixing Poria refined powder and Poria ultramicro grinding powder uniformly, sieving with 20 mesh sieve, granulating, and grading to obtain Poria granule.

The poria cocos formula granules are 0.7g in each bag, and the pachymaran content and the auxiliary material amount of the process of the embodiment 1, the process of the application number CN201210018572.3 and the conventional process are shown in the following table:

TABLE 1 pachymaran content and adjuvant amount for three processes

As can be seen from the above table, the amount of the auxiliary material of the invention is 0.43g per bag, while the amount of the auxiliary material of the traditional process is 0.22g per bag, and the amount of the auxiliary material of the invention CN201210018572.3 is 0.31 g; in the aspect of pachymaran content, the pachymaran content of the invention is 0.48g, which is obviously increased.

The above embodiments are merely preferred embodiments of the present invention, and any simple modification, modification and substitution changes made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.