CN115501271B - Preparation method of Qiqingbaidu granules - Google Patents
Preparation method of Qiqingbaidu granules Download PDFInfo
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- CN115501271B CN115501271B CN202210951278.1A CN202210951278A CN115501271B CN 115501271 B CN115501271 B CN 115501271B CN 202210951278 A CN202210951278 A CN 202210951278A CN 115501271 B CN115501271 B CN 115501271B
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- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
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- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
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Abstract
The invention relates to a preparation method of Qiqingbaidu granule, which consists of seven medicinal materials of baikal skullcap root, giant knotweed rhizome, chinese pulsatilla root, lightyellow sophora root, isatis root, rhizoma dryopterygii and dyers woad leaf, and has the functions of clearing heat and detoxicating, eliminating dampness and relieving diarrhea. It is mainly used for treating diarrhea due to damp-heat. Because the components in the formula are more, each medicinal material has the proper extraction conditions, the invention adopts a mode of grouping and step-by-step extraction, divides the medicinal materials which have the same extraction conditions and meet the compatibility rule of the traditional Chinese medicines into a group for grouping extraction, and concentrates the extraction liquid after grouping extraction together, and simultaneously, the whole process of grouping extraction before and after the extraction keeps the medicinal residues in an extraction tank to participate in the extraction of other medicinal materials added next. According to the invention, through a scientific extraction mode, the content of the active ingredients of each raw material of the Qiqing Baidu granule is comprehensively improved, the loss of the active ingredients in the medicinal materials is maximally reduced, and the quality of the granule can be ensured.
Description
Technical Field
The invention relates to the technical field of veterinary medicines, in particular to a preparation method of Qiqingbaidu granules.
Background
The QIQINGBAIDU granule is prepared from radix Scutellariae, rhizoma Polygoni Cuspidati, radix Pulsatillae, radix Sophorae Flavescentis, radix Isatidis, rhizoma Dryopteris Crassirhizomatis and folium Isatidis by extracting, concentrating and granulating. It has the functions of clearing away heat and toxic material, eliminating dampness and stopping diarrhea. It is mainly used for treating diarrhea due to damp-heat.
The traditional Qiqing antiphlogistic granule is prepared by decocting seven medicinal materials with water twice, the first time is 2 hours, the second time is 1 hour, the decoction is filtered, the filtrates are combined, and the extract and the dextrin are added for granulating after the concentration under reduced pressure at 80 ℃. However, the medicinal materials forming the Qiqing baidu granule are complex, the property difference among different medicinal materials is extremely large, the traditional preparation method cannot fully extract the main active ingredients of the medicinal materials in the extraction process, so that the content of the main active ingredients remained in the residues after extraction is higher, and the waste of resources is caused. In addition, the high temperature during decoction and concentration can decompose the effective components in the medicinal materials, thereby causing secondary waste of resources. Therefore, the optimum conditions of extraction and concentration of each medicinal material 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 grouping extraction, the extraction temperature, time, cost and stability of each effective component are comprehensively considered, a scientific and feasible set of preparation method which is controllable in cost and suitable for large-scale production is designed, the content of each effective component in the finished product of the Qijiao toxin-vanquishing granule is greatly improved, the preparation process is more controllable, and the method is required by the current traditional Chinese veterinary medicine market.
Disclosure of Invention
The invention aims to provide a preparation method of Qiqing antiphlogistic granules, which aims to maximally extract and retain active ingredients in various medicinal materials and improve the quality of products.
In order to achieve the above purpose, the present invention provides the following solutions:
the Qiqing baidu granule is prepared from the following seven medicinal materials: 100 parts of radix scutellariae, 100 parts of polygonum cuspidatum, 80 parts of pulsatilla chinensis, 80 parts of radix sophorae flavescentis, 100 parts of radix isatidis, 60 parts of rhizoma dryopteris crassirhizomae and 40 parts of dyers woad leaf. The formula is derived from the two parts of the pharmacopoeia 2020 of the people's republic of China, and the addition amount of each medicinal material is the total dosage of the medicinal material.
The QI QING BAI DU KE LI is prepared by extracting seven materials under three different extraction conditions, and extracting folium Isatidis and rhizoma Polygoni Cuspidati together, scutellariae radix, radix Sophorae Flavescentis and radix Pulsatillae together, and radix Isatidis and rhizoma Dryopteris Crassirhizomatis together. The extraction steps are divided into groups, only extracting solution is collected, and residues are always kept in an extraction tank until the extraction is completed in the whole process of front and rear group extraction. The method specifically comprises the following steps that the addition amounts of the medicinal materials are all the total dosage of the medicinal materials:
step one: extracting folium Isatidis and rhizoma Polygoni Cuspidati with ethanol solution, and collecting extractive solution.
Step two: adding a certain amount of water into an extraction tank, heating, adding three medicinal materials of radix Scutellariae, radix Sophorae Flavescentis and radix Pulsatillae, extracting, and collecting extractive solution.
Step three: adding radix Isatidis and rhizoma Dryopteris Crassirhizomatis into extraction tank, extracting with water, and collecting extractive solution.
Step four: and (3) uniformly mixing the extracting solutions in the first step to the third step, and concentrating to a certain degree to obtain extractum.
Step five: taking the extract in the step four, adding a proper amount of sucrose and dextrin to prepare a soft material, and granulating.
Preferably, the extraction conditions of the dyers woad leaf and the giant knotweed in the first step 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 folium Isatidis and rhizoma Polygoni Cuspidati, and extracting at 55-65deg.C for 1-3 hr.
Preferably, in the second step, when the radix scutellariae, the radix sophorae flavescentis and the radix pulsatillae are extracted, water which is equivalent to 10-15 times of the total mass of the five medicinal materials of the dyers woad leaf, the giant knotweed, the radix scutellariae, the radix sophorae flavescentis and the radix pulsatillae is heated to boiling, and then the medicinal materials are added, and the boiling state is maintained for 1-3 hours.
Preferably, in the third step, the medicinal materials of radix isatidis and rhizoma dryopteris crassirhizomae are added first, then water which is 10-15 times of the total mass of seven medicinal materials of dyers woad leaf, giant knotweed, baical skullcap root, lightyellow sophora root, chinese pulsatilla root, radix isatidis and rhizoma dryopteris crassirhizomae is added, the temperature is raised to 75-85 ℃, and the extraction is carried out for 1-3 hours.
Preferably, in the fourth step, the concentration temperature 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 15% -25%, 33% -38% and 42% -47%, respectively.
Compared with the prior art, the invention has the advantages that:
the invention has the advantage 1 that each medicinal material is extracted according to the optimal extraction condition by separating the components and then carrying out grouping extraction, compared with the traditional mixed water extraction method, the baicalin content is improved by 40%, and the indirubin content and the (R, S) -epigoitrin content are improved by one time. As shown by the examples, the experimental steps involve the comparison of the contents of the medicinal materials extracted by the optimal extraction method and the conventional water extraction method, and the effective components such as polydatin, emodin, indirubin, (R, S) -epigoitrin and the like are higher than those of the conventional methods.
The preparation method disclosed by the invention is more modern, provides a feasible route for improving the quality of the traditional Chinese veterinary medicine, and can be used for preparing Qiqing toxin-vanquishing particles and also is suitable for preparing other traditional Chinese medicines for animals.
The invention has the advantages of controllable cost, no need of adding new equipment on the basis of the original formula, and greatly reduced cost of process adjustment.
The invention has the advantages of improving the extraction efficiency of each medicinal material to 80% -95%, maximizing the utilization of resources, reducing other components in the medicinal residues and facilitating the subsequent treatment of the medicinal residues.
Detailed Description
The present invention will be described in detail with reference to the following specific examples, which are not intended to limit the present invention, but are merely illustrative of the present invention. The scope of the invention is defined by the appended claims. The materials and reagents used in the examples were commercially available unless otherwise specified.
Example 1: screening extraction conditions of radix Scutellariae in QIQING BAI DU KE LI.
And (3) condition presetting: the solvent parallel condition is water, 30% ethanol, 60% ethanol, 80% ethanol. The solvent multiple is ten times of the mass of the medicinal material. The temperature parallel conditions were set at 16 ℃,60 ℃,80 ℃,100 ℃. The extraction time-parallel conditions were set to 1 hour, 2 hours, 3 hours. The extraction rate of radix Scutellariae uses baicalin as a measurement standard. The experimental conditions were designed as follows:
experiments are carried out according to the conditions, and the extraction rate of baicalin in the baical skullcap root medicinal materials is detected, and the results are shown in the following table:
the experimental result shows that the optimum condition of the extraction of the baical skullcap root is that the solvent is water, the extraction temperature is 100 ℃ and the time is 2 hours.
Example 2: screening the extraction conditions of the kuh-seng in the Qiqing Baidu granules.
And (3) condition presetting: the solvent parallel condition is water, 0.1% hydrochloric acid and 1% acetic acid. The solvent multiple is ten times of the mass of the medicinal material. The temperature parallel conditions were set at 80 ℃,90 ℃,100 ℃. The extraction time was set to 1 hour, 2 hours, 3 hours. The extraction rate of radix Sophorae Flavescentis adopts the sum of matrine and oxymatrine as the measurement standard. The experimental conditions were designed as follows:
experiments are carried out according to the conditions, and the extraction rate of the total amount of matrine and oxymatrine in the kuh-seng medicinal materials is detected, and the results are shown in the following table:
note that: in the column of "vehicle influence", three numbers are expressed in order from top to bottom: average of all results in water as vehicle, average of all results in 0.1% hydrochloric acid as vehicle, average of all results in 1% acetic acid as vehicle. The "range" represents the difference between the maximum and minimum of the three numbers. The following is the same.
The experimental result shows that the water extraction at 100 ℃ for 2 hours is the optimal extraction condition of the kuh-seng, and is consistent with the baical skullcap root.
Example 3: screening extraction conditions of radix Isatidis and folium Isatidis in QINGBAIDU granule.
And (3) condition presetting: the solvent parallel condition is water, 50% ethanol, 70% ethanol. The solvent multiple is ten times of the mass of the medicinal material. The temperature parallel conditions were set at 60℃and 80 ℃. The extraction time was set to 1 hour, 2 hours, 3 hours. The extraction rate of radix Isatidis uses (R, S) -epigoitrin as a measurement standard, and the extraction rate of folium Isatidis uses indirubin as a measurement standard. The experimental conditions were designed as follows:
the extraction rate of indirubin in dyers woad leaf medicinal materials is detected by experiments according to the experimental conditions, and the results are shown in the following table:
as shown by the experimental results, 50% ethanol has the best effect of extracting for 1h at 80 ℃ and 50% ethanol is extracted for 2h at 60 ℃ which is close to the former.
The extraction rate of (R, S) -epigoitrin in the isatis root medicinal material is detected by performing experiments according to the conditions of the experimental table, and the results are shown in the following table:
as shown by the experimental results, the water extraction for 2 hours at 80 ℃ has the best effect.
Example 4: screening pretreatment conditions of radix isatidis in QINGBAIDU granule.
And (3) condition presetting: the solvent condition is water. The solvent multiple is ten times of the mass of the medicinal material. The temperature conditions were set at 80 ℃. The extraction time was set to 2 hours. The extraction rate of radix Isatidis uses (R, S) -epigoitrin as a measurement standard. Experiments were designed with the variables being only whether or not to soak for 2 hours prior to extraction. No. 1 is not soaked, and No. 2 is soaked.
The extraction rate of (R, S) -epigoitrin in the isatis root medicinal material is detected by experiments according to the experimental conditions, and the results are shown in the following table:
the experimental result shows that the soaking effect for 2 hours is better than that without soaking.
Example 5: screening extraction conditions of giant knotweed rhizome in the Qiqing Baidu granule.
And (3) condition presetting: the solvent conditions were water and 50% ethanol. The solvent multiple is ten times of the mass of the medicinal material. The temperature conditions were set at 60℃and 80℃and 100 ℃. The extraction time was set to 2 hours. The extraction rate of radix Isatidis uses polydatin and emodin as measurement standard. The experimental conditions are designed according to the following table
The extraction rate of polydatin in the giant knotweed medicinal material is detected by experiments according to the experimental conditions, and the results are shown in the following table:
as shown by the experimental results, the optimal extraction condition of the polydatin is that 50% ethanol is extracted for 2 hours at 60 ℃.
The extraction rate of the emodin in the giant knotweed medicinal material is detected by experiments according to the experimental conditions, and the results are shown in the following table:
as shown by the experimental results, the optimal extraction condition of the emodin is 50% ethanol at 80 ℃ for 1 hour or 50% ethanol at 60 ℃ for 2 hours.
Example 6: the Qiqingbaidu granule is prepared in a laboratory according to the preparation method of Qiqingbaidu granule.
The first step: weighing 24g of dyers woad leaf medicinal material, 60g of giant knotweed medicinal material, adding 45% ethanol 84ml by mass fraction, and preserving heat for 2 hours at 60 ℃. The extract was collected and the residue was retained.
And a second step of: 2400mL of water is added, 60g of baical skullcap root, 48g of kuh-seng and 48g of Chinese pulsatilla root are added after the temperature is raised to 100 ℃, and the extract is collected and the dregs are reserved after 2 hours of decoction.
And a third step of: 60g of radix isatidis, 36g of rhizoma drynariae, 3360mL of water and the like are added, the temperature is raised to 80 ℃, and the extracting solution is collected after 2 hours of heat preservation.
Fourth step: mixing the extractive solutions collected in the first to third steps, concentrating under reduced pressure at 60deg.C and pressure of-0.1 MPa to obtain extract with relative density of 1.18 (55deg.C), and centrifuging the concentrated extract.
Fifth step: concentrating the centrifuged extract under reduced pressure at 60deg.C and pressure of-0.1 MPa to obtain extract with relative density of 1.31 (55deg.C). 75g of extract is obtained.
Sixth step: weighing 90g of sucrose and 110g of medicinal dextrin, uniformly mixing, adding 55g of extract, and wet mixing for 8 minutes to obtain a soft material. Granules were prepared using a rotary granulator at a rotational speed of 200 r/min. Oven-dried at 45 ℃. 210.5g of granules were finally obtained.
Through detection of the Qiqing toxin-vanquishing particles prepared in a laboratory, the content of baicalin in the Qiqing toxin-vanquishing particles is 0.73%, and the total amount of matrine and oxymatrine is 0.14%. Other detection items meet the regulations. Compared with the standard, the baicalin content of the Qiqingbaidu granules prepared in the laboratory is 146 percent of the standard, and the content and quality of the active ingredients in the Qiqingbaidu granules are greatly improved.
Example 7: workshop pilot-plant tests were carried out according to the preparation method of the Qiqing antiphlogistic granules.
The first step: taking 9kg of dyers woad leaf medicinal material, 22.5kg of giant knotweed medicinal material, adding 315kg of 45% ethanol, and preserving heat for 2 hours at 60 ℃. The extract was collected and the residue was retained.
And a second step of: adding 900L of water, heating to 100deg.C, adding 22.5kg of Scutellariae radix, 18kg of radix Sophorae Flavescentis, and 18kg of radix Pulsatillae, decocting for 2 hr, collecting extractive solution, and retaining residue.
And a third step of: adding radix Isatidis 22.5kg, rhizoma Dryopteris Crassirhizomatis 13.5kg, adding water 1260L, heating to 80deg.C, maintaining for 2 hr, and collecting extractive solution.
Fourth step: mixing the extractive solutions collected in the first to third steps, concentrating under reduced pressure at 60deg.C and pressure of-0.08 MPa to obtain extract with relative density of 1.18 (55deg.C), and centrifuging the concentrated extract.
Fifth step: concentrating the centrifuged extract under reduced pressure at 60deg.C and pressure of-0.08 MPa to obtain extract with relative density of 1.31 (55deg.C). 33.2kg of extract was obtained.
Sixth step: weighing 18kg of sucrose and 22kg of medicinal dextrin, mixing uniformly, adding 11kg of extract, and wet mixing for 8 minutes to obtain a soft material. Granules were prepared using a rocking granulator.
The sixth step is repeated until all the extractum is used completely. The total amount of the particles obtained after drying is 125.73kg, which accords with the material balance regulation. The granule has yellow brown color and bitter taste. The content of baicalin in the detection result is 0.70% and exceeds 40% of the standard. The moisture was 4.4%. Other detection results all meet the standard.
As can be seen from workshop pilot-plant test results and laboratory results, the content of the Qiqing toxin-vanquishing granule prepared by the invention is far higher than that of standard components in the market. And the process is stable and easy to produce.
Claims (3)
1. A preparation method of Qiqing Baidu granule is characterized in that seven medicinal materials are extracted under three different extraction conditions, folium isatidis and giant knotweed rhizome are extracted together, radix scutellariae, radix sophorae flavescentis and Chinese pulsatilla root are extracted together, radix isatidis and rhizoma dryopteris crassirhizomae are extracted together, extracting solutions are only collected after each step of extraction according to a front-back three-component extraction mode, and dregs are always reserved in an extraction tank until the extraction is completed, and the preparation method specifically comprises the following steps that the adding amount of each medicinal material is the total dosage of the medicinal material:
step one: adding 10-15 times of ethanol with the mass fraction of 40% -55% into folium Isatidis and rhizoma Polygoni Cuspidati, extracting at 55-65deg.C for 1-3 hr, and collecting extractive solution;
step two: adding a certain amount of water into an extraction tank, heating to boil, adding three medicinal materials of radix Scutellariae, radix Sophorae Flavescentis and radix Pulsatillae for extraction, wherein the water content is 10-15 times of the total mass of folium Isatidis, rhizoma Polygoni Cuspidati, radix Scutellariae, radix Sophorae Flavescentis and radix Pulsatillae, keeping boiling state for 1-3 hr, and collecting extractive solution;
step three: adding radix Isatidis and rhizoma Dryopteris Crassirhizomatis into an extraction tank, adding water 10-15 times of the total mass of folium Isatidis, rhizoma Polygoni Cuspidati, scutellariae radix, radix Sophorae Flavescentis, radix Pulsatillae, radix Isatidis and rhizoma Dryopteris Crassirhizomatis, heating to 75-85deg.C, extracting for 1-3 hr, and collecting extractive solution;
step four: uniformly mixing the extracting solutions in the first to third steps, and concentrating to obtain extractum;
step five: taking the extract in the step four, adding a proper amount of sucrose and dextrin to prepare a soft material, and granulating.
2. The method for preparing the Qiqingbaidu granule according to claim 1, which is characterized in that: in the fourth step, the concentration temperature 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 at 55 ℃.
3. The method for preparing the Qiqingbaidu granule according to claim 1, which is characterized in that: in the fifth step, the mass percentages of the extractum, the sucrose and the dextrin are respectively 15% -25%, 33% -38% and 42% -47%.
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