CN112516203A - Preparation method of Changtongshu granules - Google Patents

Preparation method of Changtongshu granules Download PDF

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CN112516203A
CN112516203A CN202011449982.4A CN202011449982A CN112516203A CN 112516203 A CN112516203 A CN 112516203A CN 202011449982 A CN202011449982 A CN 202011449982A CN 112516203 A CN112516203 A CN 112516203A
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parts
extraction
temperature
zone
parameters
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范福圣
胡锐敏
彭常春
刘慧星
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Jiangxi Jinshuibao Pharmaceutical Co ltd
Jiangxi Jimin Kexin Pharmaceutical Co Ltd
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Jiangxi Jinshuibao Pharmaceutical Co ltd
Jiangxi Jimin Kexin Pharmaceutical Co Ltd
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    • A61K36/704—Polygonum, e.g. knotweed
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    • A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/232—Angelica
    • A—HUMAN NECESSITIES
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    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
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    • A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605—Excipients; Inactive ingredients
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    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

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Abstract

The invention relates to a preparation method of Changtongshu granules, which comprises the following steps: the supercritical fluid extraction technology has the extraction pressure of 25MPa, the extraction temperature of 35 ℃, the extraction time of 1 hour and the flow rate of CO2 of 20 kg/hour. Centrifuging the extracting solution, wherein the centrifugation parameters are as follows: the temperature of the liquid medicine is 75-90 ℃, the centrifugal rotating speed is 6900r/min, and the feeding speed is 2.0m 3/h. The centrifugate is concentrated to a relative density of 1.08 (60-70 ℃). Cooling to room temperature, adding equal amount of ethanol, stirring, standing, and concentrating supernatant into fluid extract with relative density of 1.15-1.20 (60-70 deg.C). Vacuum belt drying, vacuum belt drying parameters: heating system temperature 1 zone 95 deg.C, 2 zone 90 deg.C, 3 zone 75 deg.C, 4 zone 30 deg.C, feeding speed 20L/h, crawler speed 8HZ, adding appropriate amount of dextrin and steviosin, making into 1000g granule, and drying.

Description

Preparation method of Changtongshu granules
Technical Field
The invention relates to a preparation method of a traditional Chinese medicine preparation, in particular to a preparation method of traditional Chinese medicine Changtongshu granules for relaxing bowel. Belongs to the technical field of medicine.
Technical Field
The Changtongshu granule is a Chinese patent medicine prepared by processing five medicinal materials of fleece-flower root, Chinese angelica, red paeony root, fructus cannabis and mulberry. The function and the main indications of the Changtongshu granules are as follows: nourish yin and blood, moisten intestines to relieve constipation. Can be used for treating habitual constipation, senile constipation and puerperal constipation.
The formula of the Changtongshu granules is as follows:
1250 parts of tuber fleeceflower root, 833 parts of angelica, 833 parts of red paeony root, 833 parts of fructus cannabis, 833 parts of mulberry, dextrin and stevioside.
The preparation method comprises the following steps:
decocting the five raw materials in water twice, each time for 1 hour, combining decoctions, filtering, and concentrating the filtrate to a relative density of 1.08 (60-70 ℃). Cooling to room temperature, adding equal amount of ethanol, stirring, standing, and concentrating supernatant into fluid extract with relative density of 1.15-1.20 (60-70 deg.C). Spray drying, adding appropriate amount of dextrin and steviosin, making into 1000g granule, and drying.
The Changtongshu granules contain active ingredients such as stilbene glucoside, ferulic acid, paeoniflorin and the like.
However, the prior art adopts a water boiling process to generate a large amount of water extract liquid clear paste, which brings difficulty to a spray drying granulation process and causes that sometimes the color of the granules does not meet the legal standard. In order to solve the problems, the invention greatly improves the prior art, develops a brand new technology through the selection of technical conditions and parameters, and provides a better quality Changtong comfortable granule product.
Disclosure of Invention
The invention aims to provide a preparation method of Changtongshu granules.
The purpose of the invention is realized as follows: the extraction method comprises the steps of continuously optimizing the process of the prescription, extracting the medicinal materials in the prescription in proportion, adopting a supercritical fluid extraction technology, and optimizing extraction parameters to ensure that the extraction is more sufficient. And a centrifugal technology is applied in the separation process, so that the impurity removal effect of the product is better, and the quality is easier to ensure. The spray drying granulation is changed into vacuum belt drying granulation, so that the problems of forming and particle color are solved.
The invention provides a preparation method of Changtongshu granules, which comprises the following steps:
the formula is as follows:
1250 parts of tuber fleeceflower root, 833 parts of angelica, 833 parts of red peony root, 833 parts of fructus cannabis, 833 parts of mulberry,
the preparation method comprises the following steps:
1) the method comprises the following steps of (1) extracting medicinal materials by adopting a supercritical fluid extraction technology to obtain an extracting solution, wherein the supercritical fluid extraction parameters are as follows: the extraction pressure is 25Mpa, the extraction temperature is 35 ℃, the extraction time is 1 hour, and the flow of CO2 is 20 kg/hour;
2) centrifuging the obtained extracting solution to obtain a supernatant, wherein the centrifugation parameters are as follows: the temperature of the liquid medicine is 75-90 ℃, the centrifugal rotating speed is 6900r/min, and the feeding speed is 2.0m 3/h;
3) concentrating the centrifugal supernatant until the relative density is 1.08 (60-70 ℃), and cooling to room temperature;
4) adding ethanol to make ethanol concentration in the solution reach 60-80%, stirring, standing, precipitating, and filtering to obtain supernatant
5) Concentrating the supernatant into clear paste with the relative density of 1.15-1.20 (60-70 ℃).
6) And (3) obtaining the particles by adopting vacuum belt drying, wherein the vacuum belt drying parameters are as follows: the temperature of the heating system is 95 ℃ in a 1 region, 90 ℃ in a 2 region, 75 ℃ in a 3 region, 30 ℃ in a 4 region, the feeding speed is 20L/h, the track speed is 8HZ,
7) adding appropriate amount of dextrin and steviosin, and making into granule.
The invention adopts various technical schemes, including:
1. and (3) carrying out process screening according to technical parameters in the extraction process, such as pressure, extraction temperature, extraction time and CO2 flow, and determining the optimal extraction process.
2. The separation process comprises the following steps: the temperature of the liquid medicine, the centrifugal rotating speed and the feeding speed are taken as investigation factors, each factor is set to 5 levels, whether the centrifugate is clear or not, the impurity removal rate and the paeoniflorin transfer rate are taken as indexes to carry out single-factor investigation, and the optimal centrifugal process parameters of the normal-open comfortable particles are preferably selected.
3. The preparation process comprises the following steps: and (3) carrying out process research aiming at the drying time and the drying temperature by adopting a vacuum belt type drying technology, carrying out process screening according to the parameters, and determining the optimal vacuum belt type drying process parameters.
Compared with the prior art, the particles obtained by the method of the invention have improved normal quality.
The process conditions of the present invention mentioned above are selected as follows:
1250 parts of tuber fleeceflower root, 833 parts of angelica, 833 parts of red paeony root, 833 parts of fructus cannabis and 833 parts of mulberry, and a supercritical fluid extraction technology is adopted. According to the detection results (refer to the detection method of YBZ03202003 normal-through particles and the determination of paeoniflorin content in normal-through particles by the national drug administration standard (trial) in reference to the reference (determination of paeoniflorin content in normal-through particles by the HPLC method in Zhouhua), experimental screening is carried out. See Table 1
The extraction in the step 1 is optimized in process, and a supercritical fluid extraction technology is adopted. The transfer rate of paeoniflorin is used as an investigation index, orthogonal experiments are carried out according to a 4-factor 3 level, and the process optimization experiment results and the variance analysis are shown in tables 1, 2 and 3 by using the content transfer rate as a reference index.
Table 1 4-factor 3 horizontal table affecting the extraction of always-on comfortable particles
1 2 3 4
Factors of the fact Pressure of extraction Temperature of extraction Time of extraction Flow rate of CO2
Level 1 20MPa 25 degree 1 hour 20 kg/h
Level 2 25MPa 30 degree 2 hours 30 kg/h
Level 3 30MPa 35 degree 3 hours 40 kg/h
TABLE 2 orthogonal Experimental tables for extraction factor screening
Figure BDA0002831717830000031
Figure BDA0002831717830000041
TABLE 3 analysis of variance of factors affecting content extraction transfer Rate
Figure BDA0002831717830000042
(F cutoff greater than 19, significant)
As can be seen from the above table: the extraction pressure is a significant factor. The optimal energy consumption requirement is combined, so that the optimal extraction process is adopted, wherein the extraction pressure is 25Mpa, the extraction temperature is 35 ℃, the extraction time is 1 hour, and the flow of CO2 is 20 kg/hour.
Because the current standard process of the Changtongshu granules is described as 'merging decoction and filtering', in the operation stage, when liquid medicine is filtered, the filtering speed is slow, the filtering time is long, the impurity removal effect is poor, the granule dissolubility is easy to generate a turbid phenomenon, and the product quality is not ensured. Experimental research shows that the problems can be solved by adopting a centrifugal process instead of a filtering process, the change of the material basis of the medicine cannot be caused, and the absorption and the utilization of the medicine cannot be obviously influenced. Therefore, the centrifugal technology is adopted, the liquid medicine temperature, the centrifugal rotating speed and the feeding speed are respectively taken as investigation factors, each factor is set to 5 levels, whether the centrifugal liquid is clear or not, the impurity removal rate and the paeoniflorin transfer rate are taken as indexes to carry out single-factor investigation, and the optimal centrifugal process parameters of the always-on comfortable particles are preferably selected.
TABLE 4 influence of temperature of liquid medicine on clarification, impurity removal rate and transfer rate
Figure BDA0002831717830000043
TABLE 5 influence of the centrifugal speed on the clarification, impurity removal and transfer efficiency
Figure BDA0002831717830000044
Figure BDA0002831717830000051
TABLE 6 influence of the feed rate on the effect of clarification, impurity removal and transfer rates
Figure BDA0002831717830000052
According to the result of each single-factor experimental investigation, the optimal centrifugal process of the normally-open comfortable particles is determined as follows: the temperature of the liquid medicine is 75-90 ℃, the centrifugal rotating speed is 6900r/min, and the feeding speed is 2.0m 3/h.
The preparation process comprises the following steps: and (3) carrying out process research aiming at the drying time and the drying temperature by adopting a vacuum belt type drying technology, carrying out process screening according to the parameters, and determining the optimal vacuum belt type drying process parameters.
According to material properties and equipment performance, relevant documents are referred, on the basis of pre-tests, production experience is combined, the temperature of a heating system, the feeding speed and the track speed which have great influence on the vacuum belt type drying process are considered as factors, other conditions are fixed to be that the relative density of clear paste is 1.15-1.20 (60-70 ℃), the feeding temperature is 40 +/-2 ℃), the feeding swing frequency is 5Hz, the temperature of a cooling area is 40 ℃, the vacuum degree is-0.10-0.09 MPa, the moisture content of the dry paste is used as an evaluation index, an orthogonal test method is adopted for process optimization, and the factor level table is shown in table 1.
TABLE 7 factors of the level of the factors of the orthogonal test of the vacuum belt drying process
Figure BDA0002831717830000053
TABLE 8 vacuum Belt drying orthogonal test setup and results
Figure BDA0002831717830000054
Figure BDA0002831717830000061
TABLE 9 analysis of variance of results of orthogonal tests of vacuum belt drying process
Figure BDA0002831717830000062
(F cutoff greater than 19, significant)
As can be seen from the above table: the influence of the C factor caterpillar band speed on the moisture content of the dry paste is obvious. The optimal energy consumption requirement is combined, so that the optimal extraction process is adopted, wherein the temperature of the heating system is 1 zone 95 ℃, 2 zone 90 ℃, 3 zone 75 ℃, 4 zone 30 ℃, the feeding speed is 20L/h, and the track speed is 8 HZ.
The preferred optimal process is therefore: 1250 parts of tuber fleeceflower root, 833 parts of angelica, 833 parts of red peony root, 833 parts of fructus cannabis and 833 parts of mulberry, and the steps are as follows: the supercritical fluid extraction technology has the extraction pressure of 25MPa, the extraction temperature of 35 ℃, the extraction time of 1 hour and the flow rate of CO2 of 20 kg/hour. Centrifuging the extracting solution, wherein the centrifugation parameters are as follows: the temperature of the liquid medicine is 75-90 ℃, the centrifugal rotating speed is 6900r/min, and the feeding speed is 2.0m 3/h. The centrifugate is concentrated to a relative density of 1.08 (60-70 ℃). Cooling to room temperature, adding equal amount of ethanol, stirring, standing, and concentrating supernatant into fluid extract with relative density of 1.15-1.20 (60-70 deg.C). Vacuum belt drying, vacuum belt drying parameters: heating system temperature 1 zone 95 deg.C, 2 zone 90 deg.C, 3 zone 75 deg.C, 4 zone 30 deg.C, feeding speed 20L/h, crawler speed 8HZ, adding appropriate amount of dextrin and steviosin, making into 1000g granule, and drying.
Selecting a sample prepared by an optimal process to prepare a finished product of the Changtong comfortable granule, and carrying out accelerated stability investigation under the following investigation conditions: standing at 40 + -2 deg.C and 75% + -5% relative humidity for 6 months. Samples were taken at month 0, month 1, month 2, month 3 and month 6 of the test period and examined.
Accelerated stability data for the scheme of Table 10
Figure BDA0002831717830000071
From all the data analyses above, it follows: the sample prepared by the optimal process has better stability than the paeoniflorin prepared by the standard process, and the obtained product has strong moisture-attracting resistance, strong stability and stable curative effect; the whole process is easy to operate and suitable for popularization and application.
Compared with the prior art, the invention has the beneficial effects that:
according to the method provided by the invention, the transfer rate of paeoniflorin from a red paeony root medicinal material to an extracted liquid medicine reaches 30% by virtue of a supercritical fluid extraction technology, while the transfer rate of paeoniflorin in the prior art is about 15%, so that the loss of effective components of paeoniflorin is effectively reduced;
the invention solves the problems that the impurity removal effect is poor, the filtering time is long, the particle dissolubility is easy to generate turbidity and the product quality is not easy to ensure when the liquid medicine is filtered through a centrifugal technology, and the product quality is more stable; according to the invention, the problem of large clear paste amount of the preparation is solved through a vacuum belt drying technology, namely, the paste yield is 50%, the preparation method in the prior art cannot prepare a clear paste according to batches, and the vacuum belt drying technology can prepare a clear paste according to batches, so that the preparation is easier to form and a more qualified product is obtained;
the invention ensures the quality of the Changtongshu granules by increasing the control on the content of paeoniflorin, and the product quality is more stable and reliable.
In order to better embody the advancement of the invention, the invention adopts a comparative research form and carries out comparative research with other samples.
TABLE 11 comparative experimental conditions
Figure BDA0002831717830000081
From all the data analyses above, it follows: the sample prepared by the optimal process has better stability than the standard process, and the obtained product has strong moisture-attracting resistance, strong stability and stable curative effect; the whole process is easy to operate and suitable for popularization and application.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1: 1250 parts of tuber fleeceflower root, 833 parts of angelica, 833 parts of red peony root, 833 parts of fructus cannabis and 833 parts of mulberry, and the steps are as follows: the supercritical fluid extraction technology has the extraction pressure of 25MPa, the extraction temperature of 35 ℃, the extraction time of 1 hour and the flow rate of CO2 of 20 kg/hour. Centrifuging the extracting solution, wherein the centrifugation parameters are as follows: the temperature of the liquid medicine is 75-90 ℃, the centrifugal rotating speed is 6900r/min, and the feeding speed is 2.0m 3/h. The centrifugate is concentrated to a relative density of 1.08 (60-70 ℃). Cooling to room temperature, adding equal amount of ethanol, stirring, standing, and concentrating supernatant into fluid extract with relative density of 1.15-1.20 (60-70 deg.C). Vacuum belt drying, vacuum belt drying parameters: heating system temperature 1 zone 95 deg.C, 2 zone 90 deg.C, 3 zone 75 deg.C, 4 zone 30 deg.C, feeding speed 20L/h, crawler speed 8HZ, adding appropriate amount of dextrin and steviosin, making into 1000g granule, and drying.
Example 2: 1250 parts of tuber fleeceflower root, 833 parts of angelica, 833 parts of red peony root, 833 parts of fructus cannabis and 833 parts of mulberry, and the steps are as follows: the supercritical fluid extraction technology has the extraction pressure of 25MPa, the extraction temperature of 35 ℃, the extraction time of 1 hour and the flow rate of CO2 of 20 kg/hour. Centrifuging the extracting solution, wherein the centrifugation parameters are as follows: the temperature of the liquid medicine is 75-90 ℃, the centrifugal rotating speed is 6900r/min, and the feeding speed is 2.0m 3/h. The centrifugate is concentrated to a relative density of 1.08 (60-70 ℃). Cooling to room temperature, adding equal amount of ethanol, stirring, standing, and concentrating supernatant into fluid extract with relative density of 1.15-1.20 (60-70 deg.C). Vacuum belt drying, vacuum belt drying parameters: heating system temperature 1 zone 95 deg.C, 2 zone 90 deg.C, 3 zone 75 deg.C, 4 zone 30 deg.C, feeding speed 20L/h, track speed 10HZ, adding appropriate amount of dextrin and steviosin, making into 1000g granule, and drying.
Example 3: 1250 parts of tuber fleeceflower root, 833 parts of angelica, 833 parts of red peony root, 833 parts of fructus cannabis and 833 parts of mulberry, and the steps are as follows: the supercritical fluid extraction technology has the extraction pressure of 25MPa, the extraction temperature of 35 ℃, the extraction time of 1 hour and the flow rate of CO2 of 25 kg/hour. Centrifuging the extracting solution, wherein the centrifugation parameters are as follows: the temperature of the liquid medicine is 75-90 ℃, the centrifugal rotating speed is 6900r/min, and the feeding speed is 2.0m 3/h. The centrifugate is concentrated to a relative density of 1.08 (60-70 ℃). Cooling to room temperature, adding equal amount of ethanol, stirring, standing, and concentrating supernatant into fluid extract with relative density of 1.15-1.20 (60-70 deg.C). Vacuum belt drying, vacuum belt drying parameters: heating system temperature 1 zone 95 deg.C, 2 zone 90 deg.C, 3 zone 75 deg.C, 4 zone 30 deg.C, feeding speed 20L/h, crawler speed 8HZ, adding appropriate amount of dextrin and steviosin, making into 1000g granule, and drying.
Example 4: 1250 parts of tuber fleeceflower root, 833 parts of angelica, 833 parts of red peony root, 833 parts of fructus cannabis and 833 parts of mulberry, and the steps are as follows: the supercritical fluid extraction technology has the extraction pressure of 25MPa, the extraction temperature of 35 ℃, the extraction time of 1 hour and the flow of CO2 of 30 kg/hour. Centrifuging the extracting solution, wherein the centrifugation parameters are as follows: the temperature of the liquid medicine is 75-90 ℃, the centrifugal rotating speed is 6900r/min, and the feeding speed is 2.0m 3/h. The centrifugate is concentrated to a relative density of 1.08 (60-70 ℃). Cooling to room temperature, adding equal amount of ethanol, stirring, standing, and concentrating supernatant into fluid extract with relative density of 1.15-1.20 (60-70 deg.C). Vacuum belt drying, vacuum belt drying parameters: heating system temperature 1 zone 95 deg.C, 2 zone 90 deg.C, 3 zone 75 deg.C, 4 zone 30 deg.C, feeding speed 20L/h, crawler speed 8HZ, adding appropriate amount of dextrin and steviosin, making into 1000g granule, and drying.
Example 5: 1250 parts of tuber fleeceflower root, 833 parts of angelica, 833 parts of red peony root, 833 parts of fructus cannabis and 833 parts of mulberry, and the steps are as follows: the supercritical fluid extraction technology has the extraction pressure of 25MPa, the extraction temperature of 25 ℃, the extraction time of 1 hour and the flow rate of CO2 of 20 kg/hour. Centrifuging the extracting solution, wherein the centrifugation parameters are as follows: the temperature of the liquid medicine is 75-90 ℃, the centrifugal rotating speed is 6900r/min, and the feeding speed is 2.0m 3/h. The centrifugate is concentrated to a relative density of 1.08 (60-70 ℃). Cooling to room temperature, adding equal amount of ethanol, stirring, standing, and concentrating supernatant into fluid extract with relative density of 1.15-1.20 (60-70 deg.C). Vacuum belt drying, vacuum belt drying parameters: heating system temperature 1 zone 95 deg.C, 2 zone 90 deg.C, 3 zone 75 deg.C, 4 zone 30 deg.C, feeding speed 20L/h, crawler speed 8HZ, adding appropriate amount of dextrin and steviosin, making into 1000g granule, and drying.
Example 6: 1250 parts of tuber fleeceflower root, 833 parts of angelica, 833 parts of red peony root, 833 parts of fructus cannabis and 833 parts of mulberry, and the steps are as follows: the supercritical fluid extraction technology has the extraction pressure of 25MPa, the extraction temperature of 30 ℃, the extraction time of 1 hour and the flow rate of CO2 of 20 kg/hour. Centrifuging the extracting solution, wherein the centrifugation parameters are as follows: the temperature of the liquid medicine is 75-90 ℃, the centrifugal rotating speed is 6900r/min, and the feeding speed is 2.0m 3/h. The centrifugate is concentrated to a relative density of 1.08 (60-70 ℃). Cooling to room temperature, adding equal amount of ethanol, stirring, standing, and concentrating supernatant into fluid extract with relative density of 1.15-1.20 (60-70 deg.C). Vacuum belt drying, vacuum belt drying parameters: heating system temperature 1 zone 95 deg.C, 2 zone 90 deg.C, 3 zone 75 deg.C, 4 zone 30 deg.C, feeding speed 20L/h, crawler speed 8HZ, adding appropriate amount of dextrin and steviosin, making into 1000g granule, and drying.
Example 7: 1250 parts of tuber fleeceflower root, 833 parts of angelica, 833 parts of red peony root, 833 parts of fructus cannabis and 833 parts of mulberry, and the steps are as follows: the supercritical fluid extraction technology has the extraction pressure of 25MPa, the extraction temperature of 35 ℃, the extraction time of 2 hours and the flow rate of CO2 of 20 kg/hour. Centrifuging the extracting solution, wherein the centrifugation parameters are as follows: the temperature of the liquid medicine is 75-90 ℃, the centrifugal rotating speed is 6900r/min, and the feeding speed is 2.0m 3/h. The centrifugate is concentrated to a relative density of 1.08 (60-70 ℃). Cooling to room temperature, adding equal amount of ethanol, stirring, standing, and concentrating supernatant into fluid extract with relative density of 1.15-1.20 (60-70 deg.C). Vacuum belt drying, vacuum belt drying parameters: heating system temperature 1 zone 95 deg.C, 2 zone 90 deg.C, 3 zone 75 deg.C, 4 zone 30 deg.C, feeding speed 20L/h, crawler speed 8HZ, adding appropriate amount of dextrin and steviosin, making into 1000g granule, and drying.
Example 8: 1250 parts of tuber fleeceflower root, 833 parts of angelica, 833 parts of red peony root, 833 parts of fructus cannabis and 833 parts of mulberry, and the steps are as follows: the supercritical fluid extraction technology has the extraction pressure of 25MPa, the extraction temperature of 35 ℃, the extraction time of 3 hours and the flow rate of CO2 of 20 kg/hour. Centrifuging the extracting solution, wherein the centrifugation parameters are as follows: the temperature of the liquid medicine is 75-90 ℃, the centrifugal rotating speed is 6900r/min, and the feeding speed is 2.0m 3/h. The centrifugate is concentrated to a relative density of 1.08 (60-70 ℃). Cooling to room temperature, adding equal amount of ethanol, stirring, standing, and concentrating supernatant into fluid extract with relative density of 1.15-1.20 (60-70 deg.C). Vacuum belt drying, vacuum belt drying parameters: heating system temperature 1 zone 95 deg.C, 2 zone 90 deg.C, 3 zone 75 deg.C, 4 zone 30 deg.C, feeding speed 20L/h, crawler speed 8HZ, adding appropriate amount of dextrin and steviosin, making into 1000g granule, and drying.

Claims (1)

1. A preparation method of the Changtongshu granules comprises the following steps: 1250 parts of tuber fleeceflower root, 833 parts of Chinese angelica, 833 parts of red paeony root, 833 parts of fructus cannabis and 833 parts of mulberry; the method is characterized by comprising the following steps:
1) the method comprises the following steps of (1) extracting medicinal materials by adopting a supercritical fluid extraction technology to obtain an extracting solution, wherein the supercritical fluid extraction parameters are as follows: the extraction pressure is 25Mpa, the extraction temperature is 35 ℃, the extraction time is 1 hour, and the flow of CO2 is 20 kg/hour;
2) centrifuging the obtained extracting solution to obtain a supernatant, wherein the centrifugation parameters are as follows: the temperature of the liquid medicine is 75-90 ℃, the centrifugal rotating speed is 6900r/min, and the feeding speed is 2.0m 3/h;
3) concentrating the centrifugal supernatant until the relative density is 1.08 (60-70 ℃), and cooling to room temperature;
4) adding ethanol to make ethanol concentration in the solution reach 60-80%, stirring, standing, precipitating, and filtering to obtain supernatant;
5) concentrating the supernatant into clear paste with the relative density of 1.15-1.20 (60-70 ℃);
6) and (3) obtaining the particles by adopting vacuum belt drying, wherein the vacuum belt drying parameters are as follows: the temperature of the heating system is 95 ℃ in a 1 region, 90 ℃ in a 2 region, 75 ℃ in a 3 region, 30 ℃ in a 4 region, the feeding speed is 20L/h, and the track speed is 8 HZ;
7) adding appropriate amount of dextrin and steviosin, and making into granule.
CN202011449982.4A 2020-12-12 2020-12-12 Preparation method of Changtongshu granules Pending CN112516203A (en)

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Citations (1)

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Publication number Priority date Publication date Assignee Title
CN110960663A (en) * 2019-12-21 2020-04-07 江西济民可信金水宝制药有限公司 Preparation method of Xiaochaihu granules

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110960663A (en) * 2019-12-21 2020-04-07 江西济民可信金水宝制药有限公司 Preparation method of Xiaochaihu granules

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