CN114288252A - Buffalo horn formula particle and preparation method thereof - Google Patents

Buffalo horn formula particle and preparation method thereof Download PDF

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Publication number
CN114288252A
CN114288252A CN202210187031.7A CN202210187031A CN114288252A CN 114288252 A CN114288252 A CN 114288252A CN 202210187031 A CN202210187031 A CN 202210187031A CN 114288252 A CN114288252 A CN 114288252A
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buffalo horn
preparation
extract
filter residue
extraction
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高亮
徐宝信
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Heilongjiang Forest Industry Pharmaceutical Co ltd
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Heilongjiang Forest Industry Pharmaceutical Co ltd
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Abstract

The invention relates to buffalo horn formula particles and a preparation method thereof. The preparation method comprises the following steps: extracting cornu Bubali decoction pieces with water, and filtering to obtain extractive solution; concentrating the extracting solution to obtain a concentrated solution; stirring and heating the concentrated solution, adding auxiliary materials, and performing spray drying to obtain dry powder; and mixing the dry powder with auxiliary materials, granulating by adopting a dry method, and sieving to obtain the buffalo horn formula granules. According to the preparation method, the obtained buffalo horn formula particles can completely meet the requirements through water extraction, concentration, spray drying and dry granulation processes, the dissolubility of the product is effectively improved, and the production efficiency and the product quality are also ensured.

Description

Buffalo horn formula particle and preparation method thereof
Technical Field
The invention belongs to the field of traditional Chinese medicine preparation, and particularly relates to buffalo horn formula granules and a preparation method thereof.
Background
The traditional Chinese medicine formula particle is derived from decoction of traditional Chinese medicine decoction pieces and is a deep-processed product of the traditional Chinese medicine decoction pieces. The traditional Chinese medicine formula granule is a granule prepared by carrying out water extraction, separation, concentration, drying and granulation on single traditional Chinese medicine decoction pieces, and is prepared according to a traditional Chinese medicine clinical prescription under the guidance of the traditional Chinese medicine theory and is taken by patients. Has the advantages of convenient use and carrying, etc.
At present, no report and research is found on the formulation and particle method of the cattle horns in the animal traditional Chinese medicine in China. The buffalo horn is mostly used by grinding and concentrating powder instead of water decoction, and has the problems of weak compliance and difficult control of metering. The preparation technology of the buffalo horn formula particles has the technical problems of low spray drying yield, poor dissolubility, difficult dry granulation and the like.
Therefore, the technical scheme of the invention is provided.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides buffalo horn formula particles and a preparation method thereof. According to the preparation method, the obtained buffalo horn formula particles can completely meet the requirements through water extraction, concentration, spray drying and dry granulation processes, the dissolubility of the product is effectively improved, and the production efficiency and the product quality are also ensured.
The invention provides a preparation method of buffalo horn formula particles, which comprises the following steps:
(1) extracting cornu Bubali decoction pieces with water, and filtering to obtain extractive solution;
(2) concentrating the extracting solution obtained in the step (1) to obtain a concentrated solution;
(3) stirring and heating the concentrated solution obtained in the step (2), adding auxiliary materials, and performing spray drying to obtain dry powder;
(4) and (4) mixing the dry powder obtained in the step (3) with auxiliary materials, performing dry granulation, and sieving to obtain the buffalo horn formula granules.
Preferably, in step (1), the water extraction method comprises:
(i) mixing cornu Bubali decoction pieces with drinking water, heating to boil, extracting for the first time, and filtering to obtain primary residue and primary extractive solution;
(ii) mixing the primary filter residue with drinking water, heating to boil for secondary extraction, and filtering to obtain secondary filter residue and secondary extract;
(iii) mixing the secondary filter residue with drinking water, heating to boil for three times of extraction, and filtering to obtain tertiary filter residue and tertiary extract;
(iv) and mixing the primary extract, the secondary extract and the tertiary extract to obtain the extract.
Adopts a water extraction process, and accords with the basic property that the traditional Chinese medicine formula granules are from decoction.
Preferably, in the step (i), the drinking water is added in an amount of 8-10L/kg based on the weight of the buffalo horn decoction pieces; the time for primary extraction is 2-3 h.
Preferably, in the step (ii), the addition amount of the drinking water is 6-8L/kg based on the weight of the primary filter residue; the time of the secondary extraction is 1-2 h.
Preferably, in the step (iii), the addition amount of the drinking water is 4-6L/kg based on the weight of the secondary filter residue; the time for the three times of extraction is 0.5-1 h.
Preferably, in the step (2), the concentration temperature is 60-80 ℃, and the vacuum degree of concentration is-0.06-0.09 MPa; the relative density of the concentrated solution at 60 ℃ is 1.04-1.10.
Preferably, in the step (3), the heating temperature is 70-80 ℃, and the weight ratio of the auxiliary materials to the buffalo horn decoction pieces is 5-10: 100; the air inlet temperature of spray drying is 165-185 ℃, and the air outlet temperature is 70-95 ℃. After the auxiliary materials with a certain proportion are added into the concentrated solution, the fog drops can be promoted to form small particles and naturally fall off from the tower wall, and the phenomena of wall adhesion and gelatinization of dry paste in the spray drying process can be improved, so that the dissolubility and the yield are improved.
Preferably, in step (4), the parameters of the dry granulation are as follows: the vertical feeding rotating speed is 10-15 r/min, the horizontal feeding rotating speed is 35-45 r/min, the pressure of a compression roller is 5-10 Mpa, the rotating speed of the compression roller is 5-10 r/min, the whole grain rotating speed is 60-90 r/min, and the temperature of circulating water is 10-20 ℃. By adopting the dry granulation process, the granulation can be carried out without granules and the efficiency is high.
Based on the same technical concept, the invention also provides buffalo horn formula particles prepared by the method.
The invention has the beneficial effects that:
according to the preparation method disclosed by the invention, the obtained buffalo horn formula particles can completely meet the requirements through water extraction, concentration, spray drying and dry granulation processes, the dissolubility of the product is effectively improved, and the production efficiency and the product quality are also ensured.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Example 1
The embodiment provides a preparation method of buffalo horn formula particles, which comprises the following steps:
(1) taking 100kg of cornu Bubali decoction pieces, adding 8L/kg of drinking water (based on the weight of cornu Bubali decoction pieces), heating to boil, extracting for 2 hr, and filtering to obtain primary residue and primary extractive solution; mixing the primary filter residue with 6L/kg drinking water (added based on the weight of the primary filter residue), heating to boil for extraction for 1h, and filtering to obtain secondary filter residue and secondary extract; mixing the secondary filter residue with 4L/kg drinking water (added based on the weight of the secondary filter residue), heating to boil for extraction for 0.5h, and filtering to obtain tertiary filter residue and tertiary extract; mixing the primary extract, the secondary extract and the tertiary extract to obtain an extract;
(2) concentrating the extracting solution in the step (1) under the conditions of vacuum degree of-0.06 MPa and 60 ℃ until the relative density is 1.04(60 ℃) to obtain concentrated solution; the solid content of the concentrated solution is 0.95 kg;
(3) stirring the concentrated solution obtained in the step (2), heating to 70 ℃, adding maltodextrin (the weight ratio of the maltodextrin to the buffalo horn decoction pieces is 5:100) for spray drying, and obtaining dry powder after completion; wherein the air inlet temperature of spray drying is 165 ℃, the air outlet temperature is 70 ℃, 5.62kg of dry extract powder is prepared, and the spray drying yield is 94.0%; (Note: weight of theoretical spray-dried powder is concentrated solution weight. times. solid content percentage; spray-drying yield:actualspray-dried powder weight/theoretical spray-dried powder weight. times.100%)
(4) Mixing the dry powder obtained in the step (3) with a proper amount of maltodextrin, carrying out dry granulation, and adjusting the parameters of a dry granulator to be as follows: the vertical feeding speed is 10r/min, the horizontal feeding speed is 35r/min, the pressure of a compression roller is 5Mpa, the rotation speed of the compression roller is 5r/min, the whole grain rotation speed is 60r/min, and the water temperature of circulating water is 10 ℃; and (4) screening the mixture by using a 16-mesh screen to obtain the buffalo horn formula particles. It is also emphasized that maltodextrin acts as an excipient to enhance the solubility and anti-hygroscopicity of the granules (the same applies below).
Example 2
The embodiment provides a preparation method of buffalo horn formula particles, which comprises the following steps:
(1) taking 100kg of cornu Bubali decoction pieces, adding 10L/kg of drinking water (based on the weight of cornu Bubali decoction pieces), heating to boil, extracting for 3 hr, and filtering to obtain primary residue and primary extractive solution; mixing the primary filter residue with 8L/kg drinking water (added based on the weight of the primary filter residue), heating to boil for extraction for 2h, and filtering to obtain secondary filter residue and secondary extract; mixing the secondary filter residue with 6L/kg of drinking water (added based on the weight of the secondary filter residue), heating to boil for extraction for 1h, and filtering to obtain tertiary filter residue and tertiary extract; mixing the primary extract, the secondary extract and the tertiary extract to obtain an extract;
(2) concentrating the extracting solution in the step (1) under the conditions of vacuum degree of-0.09 MPa and 80 ℃ until the relative density is 1.10(60 ℃), and obtaining a concentrated solution; the solid content of the concentrated solution is 0.93 kg;
(3) stirring the concentrated solution obtained in the step (2), heating to 80 ℃, adding maltodextrin (the weight ratio of the maltodextrin to the buffalo horn decoction pieces is 10:100) for spray drying, and obtaining dry powder after completion; wherein the air inlet temperature of spray drying is 185 ℃, the air outlet temperature is 95 ℃, 9.83kg of dry extract powder is prepared, and the spray drying yield is 89.8%; (Note: weight of theoretical spray-dried powder is concentrated solution weight. times. solid content percentage; spray-drying yield:actualspray-dried powder weight/theoretical spray-dried powder weight. times.100%)
(4) Mixing the dry powder obtained in the step (3) with a proper amount of maltodextrin, carrying out dry granulation, and adjusting the parameters of a dry granulator to be as follows: the vertical feeding speed is 15r/min, the horizontal feeding speed is 45r/min, the pressure of a compression roller is 10Mpa, the rotation speed of the compression roller is 10r/min, the whole grain rotation speed is 90r/min, and the water temperature of circulating water is 20 ℃; and (4) screening the mixture by a 40-mesh screen to obtain the buffalo horn formula particles.
Example 3
The embodiment provides a preparation method of buffalo horn formula particles, which comprises the following steps:
(1) taking 100kg of cornu Bubali decoction pieces, adding 9L/kg of drinking water (based on the weight of cornu Bubali decoction pieces), heating to boil, extracting for 2.5 hr, and filtering to obtain primary residue and primary extractive solution; mixing the primary filter residue with 7L/kg drinking water (added based on the weight of the primary filter residue), heating to boil for extraction for 1.5h, and filtering to obtain secondary filter residue and secondary extract; mixing the secondary filter residue with 5L/kg drinking water (added based on the weight of the secondary filter residue), heating to boil and extracting for 0.75h, and filtering to obtain tertiary filter residue and tertiary extract; mixing the primary extract, the secondary extract and the tertiary extract to obtain an extract;
(2) concentrating the extracting solution in the step (1) under the conditions of vacuum degree of-0.07 MPa and 70 ℃ until the relative density is 1.07(60 ℃), and obtaining a concentrated solution; the solid content of the concentrated solution is 0.90 kg;
(3) stirring the concentrated solution obtained in the step (2), heating to 75 ℃, adding maltodextrin (the weight ratio of the maltodextrin to the buffalo horn decoction pieces is 7.5:100) and carrying out spray drying to obtain dry powder; wherein the air inlet temperature of spray drying is 175 ℃, the air outlet temperature is 82 ℃, 4.06kg of dry extract powder is prepared, and the spray drying yield is 91.2%; (Note: weight of theoretical spray-dried powder is concentrated solution weight. times. solid content percentage; spray-drying yield:actualspray-dried powder weight/theoretical spray-dried powder weight. times.100%)
(4) Mixing the dry powder obtained in the step (3) with a proper amount of maltodextrin, carrying out dry granulation, and adjusting the parameters of a dry granulator to be as follows: the vertical feeding speed is 12r/min, the horizontal feeding speed is 40r/min, the pressure of a compression roller is 7.5Mpa, the rotation speed of the compression roller is 7.5r/min, the whole grain rotation speed is 75r/min, and the water temperature of circulating water is 15 ℃; and (4) screening the mixture by a 40-mesh screen to obtain the buffalo horn formula particles.
Comparative example
The comparative example provides a preparation method of a buffalo horn standard decoction, which specifically comprises the following steps:
putting 1000g of water buffalo horn decoction pieces into a round-bottom flask, adding 20mL/g of drinking water for the first time, heating to boil and decocting for 3 hours, filtering, adding 20mL/g of drinking water for the second time of decoction pieces, heating to boil and decocting for 2 hours, filtering, combining the two filtrates, and concentrating under reduced pressure and low temperature to obtain thick paste; drying under reduced pressure at low temperature, and pulverizing to obtain 0.91 g. The dry extract rates of the buffalo horn formula granules and the buffalo horn standard decoction in the comparative example are shown in Table 1.
TABLE 1
Item Example 1 Example 2 Example 3 Comparative example
Dry extract rate 0.95% 0.93% 0.90% 0.91%
Note: the dry paste rate is solid content of concentrated solution/feeding amount of decoction pieces multiplied by 100 percent
As is clear from Table 1, the dry paste rate values of examples 1 to 3 are close to the standard values of the comparative examples.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.

Claims (9)

1. A preparation method of buffalo horn formula particles is characterized by comprising the following steps:
(1) extracting cornu Bubali decoction pieces with water, and filtering to obtain extractive solution;
(2) concentrating the extracting solution obtained in the step (1) to obtain a concentrated solution;
(3) stirring and heating the concentrated solution obtained in the step (2), adding auxiliary materials, and performing spray drying to obtain dry powder;
(4) and (4) mixing the dry powder obtained in the step (3) with auxiliary materials, performing dry granulation, and sieving to obtain the buffalo horn formula granules.
2. The method for preparing the buffalo horn formula particle according to claim 1, wherein in the step (1), the water extraction method comprises the following steps:
(i) mixing cornu Bubali decoction pieces with drinking water, heating to boil, extracting for the first time, and filtering to obtain primary residue and primary extractive solution;
(ii) mixing the primary filter residue with drinking water, heating to boil for secondary extraction, and filtering to obtain secondary filter residue and secondary extract;
(iii) mixing the secondary filter residue with drinking water, heating to boil for three times of extraction, and filtering to obtain tertiary filter residue and tertiary extract;
(iv) and mixing the primary extract, the secondary extract and the tertiary extract to obtain the extract.
3. The preparation method of the buffalo horn formula particle as claimed in claim 2, wherein in the step (i), the weight of the buffalo horn decoction pieces is taken as a reference, and the addition amount of drinking water is 8-10L/kg; the time for primary extraction is 2-3 h.
4. The preparation method of the buffalo horn formula particle according to claim 2, wherein in the step (ii), the addition amount of drinking water is 6-8L/kg based on the weight of the primary filter residue; the time of the secondary extraction is 1-2 h.
5. The preparation method of the buffalo horn formula particle according to claim 2, wherein in the step (iii), the addition amount of drinking water is 4-6L/kg based on the weight of the secondary filter residue; the time for the three times of extraction is 0.5-1 h.
6. The method for preparing the buffalo horn formula particle according to claim 1, wherein in the step (2), the concentration temperature is 60-80 ℃, and the vacuum degree of the concentration is-0.06-0.09 MPa; the relative density of the concentrated solution at 60 ℃ is 1.04-1.10.
7. The preparation method of the cornu bubali formula particle according to claim 1, wherein in the step (3), the heating temperature is 70-80 ℃, and the weight ratio of the auxiliary material to the cornu bubali decoction pieces is 5-10: 100; the air inlet temperature of spray drying is 165-185 ℃, and the air outlet temperature is 70-95 ℃.
8. The method for preparing cornu bubali formula granules according to claim 1, wherein in the step (4), the parameters of the dry granulation are as follows: the vertical feeding rotating speed is 10-15 r/min, the horizontal feeding rotating speed is 35-45 r/min, the pressure of a compression roller is 5-10 Mpa, the rotating speed of the compression roller is 5-10 r/min, the whole grain rotating speed is 60-90 r/min, and the temperature of circulating water is 10-20 ℃.
9. A buffalo horn formulation prepared by the method of any one of claims 1 to 8.
CN202210187031.7A 2022-02-28 2022-02-28 Buffalo horn formula particle and preparation method thereof Pending CN114288252A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115429858A (en) * 2022-09-23 2022-12-06 北京康仁堂药业有限公司 Method for preparing powdered Chinese medicinal formula granules by water extraction

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106727349A (en) * 2016-12-22 2017-05-31 江西济民可信药业有限公司 A kind of preparation method for concentrating cornu bubali particle
CN109464507A (en) * 2018-09-30 2019-03-15 康美药业股份有限公司 A kind of preparation method of hawthorn granule

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106727349A (en) * 2016-12-22 2017-05-31 江西济民可信药业有限公司 A kind of preparation method for concentrating cornu bubali particle
CN109464507A (en) * 2018-09-30 2019-03-15 康美药业股份有限公司 A kind of preparation method of hawthorn granule

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115429858A (en) * 2022-09-23 2022-12-06 北京康仁堂药业有限公司 Method for preparing powdered Chinese medicinal formula granules by water extraction

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