CN115501271A - Preparation method of Qiqing Baidu granules - Google Patents

Preparation method of Qiqing Baidu granules Download PDF

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CN115501271A
CN115501271A CN202210951278.1A CN202210951278A CN115501271A CN 115501271 A CN115501271 A CN 115501271A CN 202210951278 A CN202210951278 A CN 202210951278A CN 115501271 A CN115501271 A CN 115501271A
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extracting
extraction
qiqing
medicinal materials
baidu
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CN115501271B (en
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肖传明
张城玮
唐萌渝
谢方俊
曾艳
董荣鑫
黄远荣
王子安
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BEIJING KEEPYOUNG TECHNOLOGY CO LTD
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BEIJING KEEPYOUNG TECHNOLOGY CO LTD
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Abstract

The invention relates to a preparation method of Qiqing Baidu granules, which are prepared from seven medicinal materials of scutellaria baicalensis, polygonum cuspidatum, chinese pulsatilla root, radix sophorae flavescentis, isatis root, male fern rhizome and folium isatidis and have the functions of clearing heat, detoxifying, eliminating dampness and stopping diarrhea. It is used for treating diarrhea due to damp-heat. Because the ingredients in the formula are more, each medicinal material has suitable extraction conditions, the invention adopts a mode of extracting by groups step by step, the medicinal materials which have the same extraction conditions and accord with the compatibility rule of the traditional Chinese medicine are divided into a group for extracting by group, the extracting solutions after extracting by group are concentrated together, and meanwhile, the medicine dregs are kept in the extracting tank in the whole processes of the front and back extracting by group and participate in the extracting of other medicinal materials added next. The invention comprehensively improves the content of the effective components of each raw material of the Qiqing Baidu granules by a scientific extraction mode, maximally reduces the loss of the effective components in medicinal materials (the detailed data is shown in the specification), and can better ensure the quality of the granules.

Description

Preparation method of Qiqing Baidu granules
Technical Field
The invention relates to the technical field of veterinary medicines, in particular to a preparation method of Qiqing Baidu granules.
Background
The Qiqing Baidu granule is prepared with seven kinds of Chinese medicinal materials, including skullcap root, giant knotweed, chinese pulsatilla root, flavescent sophora root, isatis root, male fern rhizome and isatis leaf, and through extraction, concentration and pelletizing. It has the functions of clearing away heat and toxic material, eliminating dampness and stopping diarrhea. It is used for treating diarrhea due to damp-heat.
The traditional preparation method of the Qiqing Baidu granules comprises the following steps of decocting seven medicinal materials in water twice, decocting for 2 hours for the first time and 1 hour for the second time, filtering, combining filtrates, concentrating under reduced pressure at 80 ℃, adding extractum and dextrin, and granulating. However, the medicinal materials for forming the Qiqing Baidu granules are complex, the property difference between different medicinal materials is great, and the traditional preparation method cannot fully extract the main effective components of the medicinal materials in the extraction process, so that the content of the main effective components of the residual medicinal residue after extraction is high, and the waste of resources is caused. In addition, the high temperature during decoction and concentration can also decompose the active ingredients in the medicinal materials, which causes secondary waste of resources. Therefore, the optimal conditions for extracting and concentrating the medicinal materials are selected, the medicinal materials which have the same extraction conditions and meet the compatibility rule of the traditional Chinese medicines are divided into a group for group extraction, the extraction temperature, the extraction time, the extraction cost and the stability of each effective component are comprehensively considered, and a set of scientific, feasible and cost-controllable preparation method suitable for large-scale production is designed, is used for greatly improving the content of each effective component in the finished product of the Qiqing Baidu granules, enables the preparation process to be more controllable, and is required by the market of traditional Chinese veterinary medicines.
Disclosure of Invention
The invention aims to provide a preparation method of Qiqing Baidu granules, which aims to maximally extract and retain effective components in medicinal materials and improve the product quality.
In order to achieve the purpose, the invention designs the following scheme:
the Qiqing Baidu granules are prepared from the following seven medicinal materials: 100 parts of scutellaria baicalensis, 100 parts of polygonum cuspidatum, 80 parts of Chinese pulsatilla root, 80 parts of sophora flavescens, 100 parts of isatis root, 60 parts of rhizoma dryopteris crassirhizomae and 40 parts of folium isatidis. The prescription is derived from the second part of 2020 edition of the animal pharmacopoeia of the people's republic of China, and the addition amount of each medicinal material is the total dosage of the medicinal material.
The Qiqing Baidu granules are extracted from seven medicinal materials by three different extraction conditions, the seven medicinal materials are divided into three groups, folium isatidis and polygonum cuspidatum are extracted together, scutellaria baicalensis, radix sophorae flavescentis and Chinese pulsatilla root are extracted together, and radix isatidis and rhizoma dryopteris crassirhizomae are extracted together. The extraction is divided into groups and step-by-step extraction, only extract is collected, and the herb residues in the whole process of the front and back group extraction are always kept in an extraction tank until the extraction is finished. The preparation method specifically comprises the following steps that the addition amount of each medicinal material is the total dosage of the medicinal material:
the method comprises the following steps: extracting folium Isatidis and rhizoma Polygoni Cuspidati with ethanol, and collecting extractive solution.
Step two: adding a certain amount of water into an extraction tank, heating, adding three medicinal materials of scutellaria baicalensis, sophora flavescens and Chinese pulsatilla root, extracting, and collecting an extracting solution.
Step three: adding radix Isatidis and rhizoma Dryopteris Crassirhizomatis into the extraction tank, extracting with water, and collecting extractive solution.
Step four: and (4) uniformly mixing the extracting solutions in the first step and the third step, and concentrating to a certain degree to obtain an extract.
Step five: taking the extract in the fourth step, adding a proper amount of cane sugar and dextrin to prepare a soft material and granulating.
Preferably, in the first step, the extraction conditions of folium isatidis and polygonum cuspidatum are as follows: adding ethanol with the mass fraction of 40% -55% which is 10-15 times of the total mass of the two medicinal materials of the dyers woad leaf and the giant knotweed rhizome, and extracting for 1-3 hours at the temperature of 55-65 ℃.
Preferably, in the second step, when the scutellaria baicalensis, the sophora flavescens and the pulsatilla chinensis are extracted, water which is 10-15 times of the total mass of the five medicinal materials including the folium isatidis, the polygonum cuspidatum, the scutellaria baicalensis, the sophora flavescens and the pulsatilla chinensis is heated to boiling, and then the medicinal materials are added into the mixture and kept at the boiling state for 1-3 hours.
Preferably, in the third step, the isatis root and the male fern rhizome are firstly added, and then water which is 10-15 times of the total mass of the seven medicinal materials of the isatis leaf, the giant knotweed rhizome, the baical skullcap root, the lightyellow sophora root, the Chinese pulsatilla root, the isatis root and the male fern rhizome is added, the temperature is raised to 75-85 ℃, and the extraction is carried out for 1-3 hours.
Preferably, the concentration temperature in the fourth step is 50-60 ℃, the pressure is-0.08-0.1 MPa, and the concentration is carried out until the relative density is 1.30-1.35 (55 ℃).
Preferably, in the fifth step, the mass percentages of the extract, the sucrose and the dextrin are respectively 15% -25%, 33% -38% and 42% -47%.
Compared with the prior art, the invention has the advantages that:
the method has the advantages that 1, each medicinal material is extracted according to the optimal extraction condition by a mode of extracting the medicinal materials in groups after the components are disassembled, and compared with the traditional mixed water extraction method, the content of the baicalin is improved by 40 percent, and the content of the indirubin and the content of (R, S) -goitrin are improved by one time. As can be seen from the examples, the experimental steps all relate to the content comparison of the medicinal materials extracted according to the optimal extraction method and the traditional water extraction method, and the effective components such as polydatin, emodin, indirubin and (R, S) -goitrin are all higher than those of the traditional method.
The preparation method is more modern, provides a feasible route for improving the quality of the traditional Chinese veterinary medicine, can be used for preparing the Qiqing toxin-vanquishing granules, and is also suitable for preparing other traditional Chinese veterinary medicines.
The method has the advantages that the cost is controllable, the method is upgraded on the basis of the original recipe, new equipment does not need to be added, and the cost of process adjustment is greatly reduced.
The method has the advantages that the extraction efficiency of each medicinal material is improved, the extraction efficiency reaches 80-95%, resources are utilized to the maximum degree, other components in the decoction dregs are reduced, and the subsequent treatment of the decoction dregs is facilitated.
Detailed Description
The present invention will be described in detail with reference to specific examples, which are not intended to limit the present invention but are merely illustrative thereof. The scope of the invention is defined by the appended claims. The medicinal materials and reagents used in the examples are purchased from the market unless otherwise specified.
Example 1: screening the extraction conditions of the scutellaria baicalensis in the Qiqing toxin-vanquishing granules.
Presetting conditions: the solvent parallel condition is water, 30% ethanol, 60% ethanol, 80% ethanol. The multiple of solvent is ten times of the mass of the medicinal materials. The temperature parallel conditions were 16 ℃,60 ℃,80 ℃ and 100 ℃. Extraction time parallel conditions were set to 1 hour, 2 hours, 3 hours. The extraction rate of Scutellariae radix is measured by baicalin. The experimental conditions thus designed are as follows:
Figure BDA0003788525520000021
experiments are carried out according to the conditions, the extraction rate of the baicalin in the scutellaria baicalensis medicinal material is detected, and the results are shown in the following table:
Figure BDA0003788525520000031
the experimental result shows that the optimum condition for extracting the scutellaria baicalensis is that the solvent is water, the extraction temperature is 100 ℃, and the extraction time is 2 hours.
Example 2: screening the extraction conditions of the radix sophorae flavescentis in the Qiqing toxin-vanquishing granules.
Presetting conditions: the solvent parallel conditions were water, 0.1% hydrochloric acid, 1% acetic acid. The multiple of the solvent is ten times of the mass of the medicinal materials. The temperature parallel conditions were set at 80 ℃,90 ℃,100 ℃. The extraction time was set to 1 hour, 2 hours, and 3 hours. The extraction rate of radix Sophorae Flavescentis is measured by the total amount of matrine and oxymatrine. The experimental conditions thus designed are as follows:
Figure BDA0003788525520000032
the experiment is carried out according to the conditions, the extraction rate of the total amount of the matrine and the oxymatrine in the radix sophorae flavescentis medicinal material is detected, and the result is shown in the following table:
Figure BDA0003788525520000041
note: in the column "influence of solvent", from top to bottom, the three numbers are indicated as follows: the average value of all results with water as the solvent, the average value of all results with 0.1% hydrochloric acid as the solvent, and the average value of all results with 1% acetic acid as the solvent. "range" means the difference between the maximum and minimum of three numbers. The same is applied below.
The experimental result shows that the water extraction at 100 ℃ for 2h is the best extraction condition of the radix sophorae flavescentis and is consistent with the radix scutellariae.
Example 3: screening the extraction conditions of isatis root and indigowoad leaf in the Qiqing toxin-vanquishing granules.
Presetting conditions: the solvent parallel condition is water, 50% ethanol, 70% ethanol. The multiple of the solvent is ten times of the mass of the medicinal materials. The temperature parallel conditions were 60 ℃ and 80 ℃. The extraction time was set to 1 hour, 2 hours, and 3 hours. The extraction rate of radix Isatidis is measured by (R, S) -goivochen, and the extraction rate of folium Isatidis is measured by indirubin. The experimental conditions thus designed are as follows:
Figure BDA0003788525520000051
the experiment is carried out according to the experimental conditions, the extraction rate of the indirubin in the indigowoad leaf medicinal material is detected, and the results are shown in the following table:
Figure BDA0003788525520000052
as can be seen from the experimental results, 50% ethanol extraction at 80 deg.C for 1h is most effective, and 50% extraction at 60 deg.C for 2h is similar to the former.
The test was carried out according to the above test table conditions, and the extraction rate of (R, S) -goitrin in the radix isatidis medicinal material was detected, and the results are shown in the following table:
Figure BDA0003788525520000061
according to experimental results, the water extraction at 80 ℃ for 2 hours has the best effect.
Example 4: screening the isatis root pretreatment conditions in Qiqing Baidu granules.
Presetting conditions: the solvent condition was water. The multiple of solvent is ten times of the mass of the medicinal materials. The temperature condition was set to 80 ℃. The extraction time was set to 2 hours. The extraction rate of radix Isatidis is measured as (R, S) -goivochun. Experiments were designed with this variable as to whether soaking for 2h before extraction was only performed. No. 1 indicates no immersion, and No. 2 indicates immersion.
The experiment is carried out according to the experimental conditions, the extraction rate of (R, S) -goitrin in the isatis root medicinal material is detected, and the results are shown in the following table:
Figure BDA0003788525520000062
the experimental results show that the effect of soaking for 2 hours is better than that of not soaking.
Example 5: screening the extraction conditions of the giant knotweed rhizome in the Qiqing toxin-vanquishing particles.
Presetting conditions: the solvent conditions were water and 50% ethanol. The multiple of solvent is ten times of the mass of the medicinal materials. The temperature conditions were 60 ℃,80 ℃ and 100 ℃. The extraction time was set to 2 hours. The extraction rate of radix Isatidis is measured by polydatin and emodin. The experimental conditions designed by the method are shown in the following table
Figure BDA0003788525520000063
Experiments are carried out according to the experimental conditions, the extraction rate of polydatin in the giant knotweed medicinal material is detected, and the results are shown in the following table:
Figure BDA0003788525520000071
the experimental result shows that the best extraction condition of the polydatin is that 50% ethanol is extracted for 2 hours at 60 ℃.
Experiments are carried out according to the experimental conditions, the extraction rate of the emodin in the giant knotweed medicinal material is detected, and the results are shown in the following table:
Figure BDA0003788525520000072
according to the experimental result, the optimal extraction condition of the emodin is that the emodin is extracted by 50% ethanol at 80 ℃ for 1 hour, or extracted by 50% ethanol at 60 ℃ for 2 hours.
Example 6: according to the preparation method of the Qiqing Baidu granules, the Qiqing Baidu granules are prepared in a laboratory.
The first step is as follows: 24g of folium isatidis and 60g of polygonum cuspidatum are weighed, 840mL of 45% ethanol is added in parts by mass, and heat preservation is carried out for 2 hours at the temperature of 60 ℃. Collecting extractive solution and collecting residue.
The second step is that: adding 2400mL of water, heating to 100 ℃, adding 60g of scutellaria baicalensis, 48g of sophora flavescens and 48g of Chinese pulsatilla root, decocting for 2 hours, collecting an extracting solution, and keeping dregs of a decoction.
The third step: adding radix Isatidis 60g, rhizoma Dryopteris Crassirhizomatis 36g, adding water 3360mL, heating to 80 deg.C, keeping the temperature for 2 hr, and collecting the extractive solution.
The fourth step: mixing the extractive solutions collected in the first to third steps, concentrating under reduced pressure at 60 deg.C and-0.1 MPa to relative density of 1.18 (55 deg.C), and centrifuging.
The fifth step: concentrating the centrifuged extract under reduced pressure at 60 deg.C and-0.1 MPa until the relative density of the extract is 1.31 (55 deg.C). 75g of extract is obtained.
And a sixth step: weighing 90g of sucrose and 110g of medical dextrin, uniformly mixing, adding 55g of the extract, and wet mixing for 8 minutes to obtain a soft material. The granules were prepared using a rotary granulator at a speed of 200 r/min. Drying in a 45 ℃ oven. Finally, 210.5g of granules were obtained.
Through the detection of the Qiqing toxin-vanquishing particles prepared in a laboratory, the content of baicalin in the Qiqing toxin-vanquishing particles is 0.73 percent, and the total amount of matrine and oxymatrine is 0.14 percent. All other items meet the specification. Compared with the standard, the baicalin content of the Qiqing toxin-vanquishing particles prepared in a laboratory is 146 percent of the standard, so that the content and the quality of the effective components in the Qiqing toxin-vanquishing particles are greatly improved.
Example 7: the pilot plant test is carried out according to the preparation method of the Qiqing toxin-vanquishing particles.
The first step is as follows: taking 9kg of folium isatidis medicinal material and 22.5kg of giant knotweed medicinal material, adding 315kg of ethanol with the mass fraction of 45%, and preserving heat for 2 hours at 60 ℃. Collecting the extractive solution and collecting the residue.
The second step: adding 900L water, heating to 100 deg.C, adding Scutellariae radix 22.5kg, radix Sophorae Flavescentis 18kg, and radix Pulsatillae 18kg, decocting for 2 hr, collecting extractive solution, and keeping residue.
The third step: adding radix Isatidis 22.5kg, rhizoma Dryopteris Crassirhizomatis 13.5kg, adding water 1260L, heating to 80 deg.C, keeping the temperature for 2 hr, and collecting extractive solution.
The fourth step: mixing the extractive solutions collected in the first to third steps, concentrating under reduced pressure at 60 deg.C and-0.08 MPa to relative density of 1.18 (55 deg.C), and centrifuging.
The fifth step: concentrating the centrifuged extract under reduced pressure at 60 deg.C and-0.08 MPa to relative density of 1.31 (55 deg.C). 33.2kg of extract is obtained.
And a sixth step: weighing 18kg of sucrose and 22kg of medical dextrin, uniformly mixing, adding 11kg of extract, and wet mixing for 8 minutes to obtain a soft material. Granules were prepared using an oscillating granulator.
Repeating the sixth step until all the extractum is completely used. The total amount of the particles obtained after drying is 125.73kg, which meets the material balance regulation. The granule color is yellow brown and bitter. The detection result shows that the content of baicalin is 0.70 percent and exceeds the standard by 40 percent. The water content was 4.4%. And other detection results all meet the standard.
As can be seen from the test results in a workshop and the laboratory results, the content of the component of the Qiqing toxin-vanquishing particle prepared by the invention is far higher than that of the standard component in the market. And the process is stable and easy to produce.

Claims (6)

1. A preparation method of Qiqing Baidu granules is characterized in that seven medicinal materials are extracted under three different extraction conditions and divided into three groups, folium isatidis and polygonum cuspidatum are extracted together, radix scutellariae, radix sophorae flavescentis and Chinese pulsatilla root are extracted together, and radix isatidis and rhizoma dryopteris crassirhizomae are extracted together. According to the front and back three groups of step-by-step extraction modes, only the extracting solution is collected after each step of extraction, and the medicine dregs are always kept in the extracting tank until the extraction is finished. The method specifically comprises the following steps that the adding amount of each medicinal material is the total dosage of the medicinal material:
the method comprises the following steps: extracting folium Isatidis and rhizoma Polygoni Cuspidati with ethanol, and collecting extractive solution.
Step two: adding a certain amount of water into an extraction tank, heating, adding three medicinal materials of scutellaria baicalensis, sophora flavescens and Chinese pulsatilla root, extracting, and collecting an extracting solution.
Step three: adding radix Isatidis and rhizoma Dryopteris Crassirhizomatis into the extraction tank, extracting with water, and collecting extractive solution.
Step four: and (4) uniformly mixing the extracting solutions in the first step and the third step, and concentrating to a certain degree to obtain an extract.
Step five: taking the extract obtained in the fourth step, adding a proper amount of sucrose and dextrin to prepare a soft material, and granulating.
2. The Qiqing Baidu granule according to claim 1, wherein: in the first step, the extraction conditions of the dyers woad leaf and the giant knotweed rhizome are as follows: adding ethanol with the mass fraction of 40-55 percent, which is 10-15 times of the total mass of the two medicinal materials of the dyers woad leaf and the giant knotweed rhizome, and extracting for 1-3 hours at the temperature of 55-65 ℃.
3. The Qiqing Baidu granule according to claim 1, wherein: in the second step, when the scutellaria baicalensis, the sophora flavescens and the Chinese pulsatilla root are extracted, water which is 10-15 times of the total mass of the five medicinal materials of the folium isatidis, the giant knotweed rhizome, the scutellaria baicalensis, the sophora flavescens and the Chinese pulsatilla root is heated to boiling, then the medicinal materials are added, and the boiling state is kept for 1-3 hours.
4. The Qiqing Baidu granule according to claim 1, wherein: in the third step, the isatis root and the male fern rhizome are added, and water which is 10-15 times of the total mass of the seven medicinal materials of the isatis leaf, the giant knotweed rhizome, the baical skullcap root, the lightyellow sophora root, the Chinese pulsatilla root, the isatis root and the male fern rhizome is added, the temperature is raised to 75-85 ℃, and the extraction is carried out for 1-3 hours.
5. The Qiqing Baidu granule according to claim 1, wherein: in the fourth step, the concentration temperature is 50-60 ℃, the pressure is-0.08 to-0.1 MPa, and the concentration is carried out until the relative density is 1.30 to 1.35 (55 ℃).
6. The Qiqing Baidu granule according to claim 1, wherein: in the fifth step, the mass percentages of the extract, the cane sugar and the dextrin are respectively 15% -25%, 33% -38% and 42% -47%.
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Citations (2)

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CN106236713A (en) * 2016-08-30 2016-12-21 林州中农颖泰生物肽有限公司 A kind of seven relieve internal heat clearly effervescent granule and preparation method thereof
CN114366770A (en) * 2020-10-14 2022-04-19 洛阳瑞华动物保健品有限公司 Preparation method of Qiqing Baidu granules

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CN106236713A (en) * 2016-08-30 2016-12-21 林州中农颖泰生物肽有限公司 A kind of seven relieve internal heat clearly effervescent granule and preparation method thereof
CN114366770A (en) * 2020-10-14 2022-04-19 洛阳瑞华动物保健品有限公司 Preparation method of Qiqing Baidu granules

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