CN115429858A - Method for preparing powdered Chinese medicinal formula granules by water extraction - Google Patents
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Abstract
The invention provides a method for preparing powdered Chinese medicinal formula granules by water extraction. The method comprises the following steps: (1) Carrying out water extraction and decoction on the raw medicinal materials to obtain an extracting solution; (2) Concentrating the extracting solution obtained in the step (1) under reduced pressure to obtain clear paste; (3) Stirring and heating the clear paste obtained in the step (2), and then carrying out spray drying to obtain dry extract powder; (4) And (4) mixing the dry extract powder obtained in the step (3) with optional auxiliary materials, and performing dry granulation to obtain the traditional Chinese medicine formula granules. The method for preparing the powdered Chinese medicinal formula granules by using water extraction improves the paste yield of the powdered decoction pieces, and the prepared Chinese medicinal formula granules have high content of effective components; and the finished product of the granules has excellent quality: uniform particle size, high paste yield, high content of alcohol-soluble extract, low impurity content and high stability of finished products.
Description
Technical Field
The invention belongs to the field of traditional Chinese medicine extraction and preparation, and particularly relates to a method for preparing a powdering variety of traditional Chinese medicine formula granules by using water extraction.
Background
The traditional Chinese medicine formula granule is prepared by carrying out water extraction, concentration, drying and granulation on single traditional Chinese medicine decoction pieces under the guidance of the traditional Chinese medicine theory, and is taken by patients after the traditional Chinese medicine clinical formula. Wherein, a plurality of varieties are directly powdered or directly made into formula granules for taking.
According to the notice of technical guidance principle of revision of processing standard of Chinese-medicine decoction pieces by the State drug administration, stopping the 'decoction piece powdering' cannon rule, sending out the collective text in 10 provinces of 1 month in 2020, stopping the execution of the 'decoction piece powdering' cannon rule, and stopping the execution (or modification) of 288 local processing standard varieties. In order to ensure that the powder variety can be continuously used, the invention needs to carry out particle preparation by extracting the powder variety with water. The powder-making variety is generally taken by directly making powder or granulating, the research on standard decoction of the powder-making variety is not found in the prior art, and the research on the aspect of the water extraction process is less. Therefore, the water extraction state, extraction mode, drying mode and the like of the ground powder variety are urgently needed to be researched.
CN103638049A discloses a method for preparing clamshell formula granules. The preparation method comprises the following steps: weighing clamshell medicinal materials, and dividing into two parts, wherein the first part accounts for 20% of the total weight, and the second part accounts for 80% of the total weight; adopting an ultrafine grinding technology to grind the first part of clam shells into ultrafine powder for later use; and then putting the clamshell ultrafine powder and a second part of clamshell medicinal materials into the same decocting container, adding water and decocting for 2 times to obtain a decoction, filtering the decoction, concentrating into an extract, spray-drying, adding a proper amount of auxiliary materials, uniformly mixing, preparing into clamshell formula granules, and subpackaging to obtain the traditional Chinese medicine composition.
CN114288252A discloses a buffalo horn formula particle and a preparation method thereof. The preparation method of the buffalo horn formula particles 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; and stirring and heating the concentrated solution, adding auxiliary materials, and performing spray drying to obtain dry powder.
CN103405477A discloses a ootheca Mantidis formula granule, its preparation method and quality control method, the formula granule is prepared from ootheca Mantidis decoction pieces by the process flows of twice water extraction, reduced pressure concentration, spray drying, dry granulation, etc. The method specifically comprises the following steps: (1) Putting the ootheca Mantidis decoction pieces into an extraction tank, adding water 15-20 times the amount of the decoction pieces, heating and decocting for 2-3 hours, filtering liquid medicine, combining filtrates, pumping the filtrate into a concentration tank, concentrating to obtain extract with the relative density of 1.03-1.05, and sieving with a 150-200-mesh sieve for later use while the extract is hot; (2) Taking the extract obtained in the step (1), adding maltodextrin with the amount of 1-2% of that of the mantis egg-case decoction pieces, uniformly mixing, heating to 70-80 ℃, carrying out spray drying, and collecting dry extract powder for later use; (3) Crushing the dry paste powder obtained in the step (2), and sieving the crushed dry paste powder by a sieve of 80 to 120 meshes; granulating by dry method, packaging with medicinal composite film, and bagging to obtain the final product.
The method discloses a preparation method of traditional Chinese medicine formula granules of powder-making varieties, however, the methods are only suitable for respective specific products, and the processes of the powder-making varieties including mineral medicines, animal medicines, plants and the like are not communicated; the method does not investigate the states of the powder-making varieties and the decoction pieces and the extraction states, and lacks the guiding significance for the varieties; the preparation methods have low extraction yield and low alcohol-soluble extract content, and are difficult to ensure the product quality of the traditional Chinese medicine formula granules of different powdering varieties.
Therefore, the development of a preparation method of the powdering variety traditional Chinese medicine formula granules is urgently needed, the standards of the powdering variety, the decoction and the subsequent process are researched by taking the cream yield and the alcohol-soluble extract as evaluation indexes, the research idea of the water extraction process of the powdering variety is established, the production process and the preparation of the formula granules are designed and optimized, and the product quality is ensured.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for preparing a powdering variety of traditional Chinese medicine formula granules by water extraction. The invention strictly controls the parameters of the process steps, improves the paste yield of the powder-making variety decoction pieces, and the prepared traditional Chinese medicine formula granules have high content of effective components; and the finished product of the granules has excellent quality: uniform particle size, high paste yield, high content of alcohol-soluble extract, low impurity content and high stability of finished products.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for preparing a powdering variety of traditional Chinese medicine formula granules by water extraction, which comprises the following steps:
(1) Carrying out water extraction and decoction on the raw medicinal materials to obtain an extracting solution;
the raw material medicines are any one or a combination of at least two of coarse powder, fine powder or superfine powder, and are subjected to water extraction and decoction after being filled into a medicine bag; the raw material medicinal materials are decoction pieces, and the raw material medicinal materials are directly subjected to water extraction and decoction;
(2) Concentrating the extracting solution obtained in the step (1) under reduced pressure to obtain clear paste;
(3) Stirring and heating the clear paste obtained in the step (2), and then carrying out spray drying to obtain dry extract powder;
(4) And (4) mixing the dry extract powder obtained in the step (3) with optional auxiliary materials, and performing dry granulation to obtain the traditional Chinese medicine formula granules.
In the invention, the preparation process is adopted to research the standards of the powdering varieties, the decoction and the subsequent processes by taking the cream yield and the alcohol-soluble extract as evaluation indexes, establish the research thought of the water extraction process of the powdering varieties, design and optimize various production processes and the preparation of formula granules, and ensure the product quality. The invention strictly controls the parameters of the process steps, improves the paste yield of the powder-making variety decoction pieces, and the prepared traditional Chinese medicine formula granules have high content of effective components; and the quality of the finished granular product is excellent: uniform particle size, high paste yield, high content of alcohol-soluble extract, low impurity content and high stability of finished products.
Preferably, in the step (1), the raw material medicine is selected from any one or a combination of at least two of calcined clam shell, concretio silicea bambusae, buffalo horn and mantis egg-case.
Wherein the coarse powder is powder which passes through the No. two sieve totally but is mixed with less than 40wt% (for example, 40wt%, 30wt%, 20wt%, 10wt%, 5wt% and the like) of powder which can pass through the No. four sieve.
Wherein the fine powder is a powder which passes through the sieve of No. five in total but is mixed with a powder which can pass through the sieve of No. six by more than 95wt% (for example, 95wt%, 96wt%, 97wt%, 98wt%, 99wt%, etc.).
Preferably, in step (1), the particle size of the ultrafine powder is 0.001 to 0.075mm (for example, 0.001mm, 0.005mm, 0.01mm, 0.015mm, 0.02mm, 0.025mm, 0.030mm, 0.035mm, 0.04mm, 0.045mm, 0.05mm, 0.055mm, 0.06mm, 0.065mm, 0.07mm, 0.075mm, etc.).
Inspecting and extracting by adopting a pack-frying mode according to standard frying parameters, and finally determining that the crushing degree of the medicinal materials is not suitable for being too fine according to result analysis.
Preferably, in the step (1), the material of the medicine bag is any one of corn fiber, non-woven fabric pp material or non-woven fabric pet material, and is preferably the non-woven fabric pp material.
Preferably, in step (1), the loading amount of the drug substance is less than 50% of the total volume of the drug package, and may be, for example, 50%, 45%, 40%, 35%, 30%, 25%, 20%, etc.
Preferably, in step (1), the water extraction and decoction is extraction by heating to boiling.
Preferably, the number of times of water extraction and decoction is 1 to 3, for example, 1, 2, 3, preferably 2.
Preferably, the total time of the water extraction and decoction is 0.5 to 3 hours, such as 0.5 hour, 0.6 hour, 0.8 hour, 1 hour, 1.2 hour, 1.4 hour, 1.6 hour, 1.8 hour, 2 hours, 3 hours and the like, and preferably 0.5 to 2 hours.
Preferably, the amount of the solvent for water extraction and decoction is 6 to 20 times, for example, 6 times, 8 times, 10 times, 12 times, 14 times, 16 times, 18 times, 20 times, etc., preferably 8 to 14 times.
Preferably, the water extraction and decoction comprises the following specific steps:
(a) Adding water into the medicine bag filled with the raw medicinal materials, decocting for the first time, filtering, and collecting dregs and a first extracting solution;
(b) Adding water into the dregs obtained in the step (a), carrying out second decoction to obtain a second extracting solution, and combining the first extracting solution and the second extracting solution to obtain an extracting solution.
Preferably, in the step (2), the temperature of the concentration under reduced pressure is 50 to 80 ℃, for example, 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃ and the like, and the pressure of the concentration under reduced pressure is 0.07 to 0.09MPa, for example, 0.07MPa, 0.075MPa, 0.08MPa, 0.085MPa, 0.09MPa and the like.
Preferably, in the step (2), the relative density of the clear paste is 1.05-1.20, for example, 1.05, 1.1, 1.15, 1.20, etc.
Preferably, in the step (3), the stirring is carried out at 55 to 65 ℃ and the temperature may be 55 ℃, 58 ℃, 60 ℃, 62 ℃, 65 ℃ or the like.
Preferably, in the step (3), in the spray drying, the inlet air temperature of the spray tower is 160-180 ℃, such as 160 ℃, 165 ℃, 170 ℃, 175 ℃, 180 ℃ and the like, the outlet air temperature of the spray tower is 60-85 ℃, such as 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃, 85 ℃ and the like, and the feeding pump frequency is 20-30 Hz, such as 20Hz, 22Hz, 24Hz, 26Hz, 28Hz, 30Hz and the like.
Preferably, in the step (4), the auxiliary material is selected from any one of maltodextrin, dextrin, corn starch or potato starch, and is preferably maltodextrin.
Preferably, in the step (4), the mass ratio of the dry extract powder to the auxiliary materials is 1 (0-1) (wherein, 0-1 can be 0, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1, etc.).
Preferably, in step (4), the mixing speed is 80-180 rpm (for example, 80rpm, 90rpm, 100rpm, 110rpm, 120rpm, 130rpm, 140rpm, 150rpm, 160rpm, 170rpm, 180rpm, etc.), and the mixing time is 20-60 min, for example, 20min, 25min, 30min, 35min, 40min, 45min, 50min, 55min, 60min, etc.
Preferably, in step (4), in the dry granulation, the roll gap is 0.6-2.5 mm, such as 0.6mm, 0.8mm, 1mm, 1.5mm, 2mm, 2.2mm, 2.5mm, etc., the roll rotation speed is 20-50 rpm, such as 20rpm, 30rpm, 40rpm, 50rpm, etc., and the pressure is 80-100 bar, such as 80bar, 85bar, 90bar, 95bar, 100bar, etc.
In the invention, the drying mode which takes short time, has high powder collecting rate and has less influence on indexes is selected by taking the cream yield and the alcohol-soluble extract as evaluation indexes and combining the drying powder collecting rate to compare the reduced pressure drying with the spray drying.
Preferably, in step (4), the dry granulation is further followed by sieving.
Preferably, in step (4), the particle size of the traditional Chinese medicine formula particle is 16-40 meshes, for example, 16 meshes, 18 meshes, 20 meshes, 22 meshes, 24 meshes, 26 meshes, 28 meshes, 30 meshes, 32 meshes, 35 meshes, 38 meshes, 40 meshes, and the like.
As a preferred technical scheme of the invention, the method comprises the following steps:
(1) Adding 8-14 times of water by mass into a medicine package filled with the raw medicinal materials, heating to boil, decocting for 0.5-2 h, filtering, and collecting dregs and a first extracting solution; adding water with the mass of 8-14 times of that of the obtained dregs of a decoction into the obtained dregs of a decoction, heating the obtained dregs of a decoction to boil, decocting the dregs of a decoction for 0.5-2 hours to obtain a second extracting solution, and combining the first extracting solution and the second extracting solution to obtain an extracting solution;
the raw material medicines are any one of coarse powder, fine powder or superfine powder or a combination of at least two of the coarse powder, the fine powder and the superfine powder, and the raw material medicines are subjected to water extraction and decoction after being packed into a medicine bag; the raw material medicinal materials are decoction pieces, and the raw material medicinal materials are directly subjected to water extraction and decoction;
(2) Concentrating the extracting solution obtained in the step (1) under reduced pressure at the temperature of 50-80 ℃ and under the pressure of 0.07-0.09 Mpa until clear paste with the relative density of 1.05-1.20 is obtained;
(3) Stirring and heating the clear paste obtained in the step (2) to 55-65 ℃, and then carrying out spray drying, wherein the air inlet temperature of a spray tower is 160-180 ℃, the air outlet temperature of the spray tower is 60-85 ℃, and the frequency of a feeding pump is 20-30 Hz, so as to obtain dry extract powder;
(4) Mixing the dry extract powder obtained in the step (3) with the mass ratio of 1 (0-1) with auxiliary materials, and performing dry granulation, wherein the gap between compression rollers is 0.6-2.5 mm, the rotation speed of the compression rollers is 20-50 rpm, and the pressure is 80-100 bar to obtain the traditional Chinese medicine formula granules.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the method, the standard frying parameters of the powder variety are investigated, the research idea of the standard frying water extraction process of the powder variety is constructed, and reference is provided for the subsequent powder variety research;
(2) The invention researches and researches the preparation of the formula granules of the powder-making variety, and ensures that the powder-making variety can be normally used under the policy of forbidding decoction piece powder-making;
(3) The invention strictly controls the parameters of the process steps, improves the paste yield of the powder-making variety decoction pieces, and the prepared traditional Chinese medicine formula granules have high content of effective components; and the finished product of the granules has excellent quality: uniform particle size, high paste yield, high content of alcohol-soluble extract, low impurity content and high stability of finished products.
Detailed Description
The technical solution of the present invention is further described below by way of specific embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
The sources of the raw materials in the following examples and comparative examples are as follows:
| name(s) | Manufacturer of the product | Branding/batch number |
| Clam shell decoction pieces | ANHUI XIEHECHENG CHINESE HERBAL MEDICINE Co.,Ltd. | 20200205、20200206、20200207 |
| Concretio silicea Bambusae seu Schizostachyi | ANHUI XIEHECHENG CHINESE HERBAL MEDICINE Co.,Ltd. | 20200107、20200108、20200109 |
| Buffalo horn medicinal material | ANHUI XIEHECHENG CHINESE HERBAL MEDICINE Co.,Ltd. | 20200303、20200304、20200305 |
| Agilawood decoction pieces | ANHUI XIEHECHENG CHINESE HERBAL MEDICINE Co.,Ltd. | 20200914、20200915、20200916 |
| Auxiliary materials | Changling Jilong biopharmaceutical industries Ltd | A200601 |
In examples 1-3, the material of the medicated bag is non-woven pp.
Example 1
This example provides a method of preparing a calcined clamshell formula using aqueous extraction, comprising the steps of:
(1) Taking 150kg of calcined clamshell decoction pieces, pulverizing into fine powder, packaging into a medicinal bag (the loading amount of the fine powder accounts for 1/3 of the volume of the medicinal bag), putting into an extraction tank, adding drinking water with the amount of 8L/kg of the decoction pieces, heating to boil and extracting for 0.5h, and filtering; adding drinking water of 6L/kg, boiling for 0.5 hr, filtering, mixing the extractive solutions, and storing in a storage tank;
(2) Concentrating under reduced pressure at 70 deg.C under vacuum degree of 0.08Mpa to obtain fluid extract with relative density of 1.05 (60 deg.C);
(3) Stirring and heating the fluid extract to 60 deg.C, and spray drying (inlet air temperature of spray tower is 165 deg.C, outlet air temperature of spray tower is 60 deg.C, and frequency of feeding pump is 20 Hz) to obtain dry extract powder;
(4) Mixing adjuvants accounting for 0% of the raw materials with dry extract powder at 120rpm for 30min, performing dry granulation (with a roller gap of 1.5mm, a roller rotation speed of 30rpm and a pressure of 90 bar), and sieving to obtain final product of formula granule of Concha Meretricis Seu Cyclinae, wherein each gram of formula granule of Concha Meretricis Seu Cyclinae is equivalent to 6 g of crude drug.
Example 2
This example provides a method for preparing a concretio silicea bambusae formula granule using water extraction, comprising the steps of:
(1) Taking 150kg of concretio silicea Bambusae seu Schizostachyi, pulverizing into superfine powder, packaging into medicinal bag (the loading amount of the superfine powder is 1/2 of the medicinal bag volume), putting into extraction tank, adding drinking water of 10L/kg of decoction pieces, heating to boil and extracting for 1 hr, and filtering; adding drinking water with the amount of 8L/kg of the decoction pieces, boiling and extracting for 1h, filtering, combining the two extracting solutions, and storing in a storage tank;
(2) Concentrating under reduced pressure at 60 deg.C under 0.07Mpa to obtain fluid extract with relative density of 1.10 (60 deg.C);
(3) Stirring and heating the clear paste to 60 ℃, and spray drying (the air inlet temperature of a spray tower is 170 ℃, the air outlet temperature of the spray tower is 70 ℃, and the frequency of a feeding pump is 30 Hz) to obtain dry extract powder;
(4) Mixing adjuvants (maltodextrin) 2% of the raw materials with dry extract powder at 150rpm for 30min, granulating by dry method (with a compression roller gap of 0.6mm, a compression roller rotation speed of 30rpm, and a pressure of 80 bar), and sieving to obtain concretio silicea Bambusae seu Schizostachyi formula granule product, wherein each gram of concretio silicea Bambusae seu Schizostachyi formula granule is equivalent to 7.5 g of crude drug.
Example 3
This example provides a method for preparing a buffalo horn formula granule using water extraction, comprising the steps of:
(1) Taking 150kg of water cattle horn medicinal material, crushing into superfine powder, filling into a medicine bag (the loading amount of the superfine powder accounts for 1/2 of the volume of the medicine bag), putting into an extraction tank, adding drinking water with the amount of 12L/kg of the decoction pieces, heating to boil and extracting for 1.5h, and filtering; adding 10L/kg drinking water, boiling for 1.5 hr, filtering, mixing the extractive solutions, and storing in a storage tank;
(2) Concentrating under reduced pressure at 70 deg.C under vacuum degree of 0.09Mpa to obtain fluid extract with relative density of 1.15 (60 deg.C);
(3) Stirring and heating the fluid extract to 60 deg.C, and spray drying (inlet air temperature of spray tower is 175 deg.C, outlet air temperature of spray tower is 75 deg.C, and frequency of feeding pump is 25 Hz) to obtain dry extract powder;
(4) Mixing adjuvants (maltodextrin) 1% of the raw materials with dry extract powder at 150rpm for 30min, dry granulating (press roller gap is 2.5mm, press roller rotation speed is 30rpm, pressure is 100 bar), and sieving to obtain cornu Bubali formula granule product, wherein each gram of cornu Bubali formula granule is equal to 33 g of crude drug.
Example 4
This example provides a method for preparing agilawood formulation granules by water extraction, comprising the following steps:
(1) Taking 150kg of agilawood decoction pieces, removing impurities, putting into an extraction tank, adding drinking water with the amount of 9L/kg of decoction pieces, heating to boil, extracting for 0.5h, and simultaneously extracting volatile oil; adding drinking water with the amount of decoction pieces of 9L/kg, boiling and extracting for 0.5h, and simultaneously extracting volatile oil; combining the two filtrates, and storing in a storage tank;
(2) Concentrating under reduced pressure at 50 deg.C under vacuum degree of 0.08Mpa to obtain fluid extract with relative density of 1.20 (60 deg.C);
(3) Collecting 100mL of volatile oil, performing inclusion (including beta-cyclodextrin, volatile oil and aromatic water), adding the concentrated solution (the concentrated solution is obtained after mixing and concentrating the two filtrates), uniformly stirring, heating to 60 ℃, and performing spray drying (the air inlet temperature of a spray tower is 180 ℃, the air outlet temperature of the spray tower is 85 ℃, and the frequency of a feeding pump is 25 Hz) to obtain dry extract powder;
(4) Mixing 0% adjuvant (maltodextrin) and dry extract powder at 180rpm for 30min, granulating by dry method (compression roller gap is 2.0mm, compression roller rotation speed is 30rpm, pressure is 95 bar), and sieving to obtain lignum Aquilariae Resinatum granule product, wherein each gram of lignum Aquilariae Resinatum granule is equivalent to crude drug amount of 1.1.
Example 5
This example provides a process for the preparation of granules of a calcined clamshell formula using aqueous extraction, differing from example 1 only in that the grinding to a particle size of 500 mesh, is carried out in the same manner as in example 1.
Example 6
This example provides a process for the preparation of granules of a calcined clamshell formula using aqueous extraction, differing from example 1 only in that the grinding to a particle size of 10 mesh, is carried out in the same manner as in example 1.
Example 7
This example provides a method for preparing a granule of a calcined clamshell formula using water extraction, which differs from example 1 only in that only one decoction is performed, specifically: adding drinking water of 15L/kg, boiling and extracting for 1 hr to obtain extractive solution, storing in storage tank, and the other steps are the same as example 1.
Example 8
This example provides a process for the preparation of a granulate of a formula of calcined clamshell by means of water extraction, which differs from example 1 only in that 3 times of decoction are carried out, in particular: adding drinking water of 6L/kg, heating to boil, extracting for 0.4 hr, and filtering; adding drinking water of 4L/kg, boiling for 0.3 hr, and filtering; and finally adding drinking water with the amount of 4L/kg of the decoction pieces, boiling and extracting for 0.3h, filtering, combining the two extracting solutions, and storing in a storage tank, wherein the other steps are the same as the example 1.
Example 9
This example provides a process for the preparation of granules of a calcined clamshell formulation using aqueous extraction, differing from example 1 only in that the loading of fines is 2/3 of the volume of the pack, the other steps being the same as in example 1.
Example 10
This example provides a process for preparing a calcined clamshell formula using aqueous extraction, differing from example 1 only in that the specific parameters of spray drying are: the inlet air temperature of the spray tower is 150 ℃, the outlet air temperature of the spray tower is 55 ℃, and other steps are the same as those in the embodiment 1.
Example 11
This example provides a process for the preparation of a calcined clamshell formula using aqueous extraction, differing from example 1 only in that the specific parameters of spray drying are: the inlet air temperature of the spray tower is 185 ℃, the outlet air temperature of the spray tower is 90 ℃, and other steps are the same as example 1.
Example 12
This example provides a process for the preparation of a calcined clamshell formula using aqueous extraction, differing from example 1 only in that the specific parameters of dry granulation are: the nip was 1.5mm, the speed of the rolls was 30rpm, the pressure was 75bar, and the other steps were the same as in example 1.
Example 13
This example provides a process for the preparation of a granulate of a calcined clamshell formulation using aqueous extraction, differing from example 1 only in that the specific parameters of dry granulation are: the nip was 1.5mm, the roll speed was 30rpm, the pressure was 110bar, and the other steps were the same as in example 1.
Comparative example 1
This comparative example provides a process for the preparation of a granulate of a formula of calcined clamshell by means of water extraction, which differs from example 1 only in that the fine powder is not packed in a cartridge, but is directly put into an extraction tank, and the other steps are the same as in example 1.
Comparative example 2
This comparative example provides a process for preparing concretio silicea bambusae formula granules using water extraction, which differs from example 2 only in that the ultra-fine powder is not packed in a cartridge, but is directly put into an extraction tank, and the other steps are the same as example 2.
Comparative example 3
This comparative example provides a process for the preparation of buffalo horn formulation granules using water extraction, differing from example 3 only in that the ultra fine powder is not packed in a cartridge, but is directly put into an extraction tank, and the other steps are the same as example 3.
Test example
Test samples: finished products of the traditional Chinese medicine formula granules provided in examples 1-13 and comparative examples 1-3;
the test method comprises the following steps:
(1) The paste yield is as follows: the total yield of the dry extract is calculated by weighing the total liquid medicine amount and the yield of the dry extract of part of the liquid medicine, thereby calculating the yield. The process is as follows: weighing an empty beaker (M0); after the two decoctions are combined into a beaker and cooled to room temperature, weighing the total weight (M1) of the beaker and the liquid medicine; uniformly stirring the liquid medicine, weighing one tenth (M sample) of the liquid medicine by mass, and putting the liquid medicine on a constant weight evaporating dish (M dish) to be evaporated to dryness on a water bath kettle; the evaporation dish was dried in an oven at 105 ℃ for 5-6h (M2).
Wherein M is Medicine = amount of the fed decoction pieces.
(2) Alcohol-soluble extract content: two samples (2 g, M) are precisely weighed and respectively placed in a 100ml conical flask, 50ml of diluted ethanol is precisely added, and the sample is tightly plugged to be used as a test sample.
The test samples were weighed to mass (m 1) and allowed to stand for 1 hour. Reflux for another 1h, let to room temperature, make up the lost weight with water and weigh (m 2). The mixture is rapidly filtered through a drying filter, 25ml of the subsequent filtrate is taken precisely and placed in an evaporating dish (W) which is dried to a constant weight. Drying the sample solution in water bath, drying at 105 deg.C for 3 hr, transferring to a drier, cooling for 30min, and quickly and precisely weighing.
(3) Drying and powder collecting rate:
the test results are specifically shown in table 1 below:
TABLE 1
Wherein the content of the first and second substances,
as can be seen from the test data in Table 1, the invention further improves the paste yield of the powder-making variety decoction pieces by strictly controlling the parameters of the process steps, and the prepared traditional Chinese medicine formula granules have high content of effective components; and the finished product of the granules has excellent quality: uniform particle size, high paste yield, high content of alcohol-soluble extract, low impurity content and high stability of finished products.
As is clear from the comparison between examples 1 to 3 and comparative examples 1 to 3, the yield of the paste obtained by direct feeding without casing was higher than that obtained by casing, but casing was selected in consideration of the production facilities, such as clogging of piping, filtration of the extract, and the like.
The applicant states that the present invention is illustrated by the above examples, but the present invention is not limited to the above examples, i.e. the present invention is not limited to the above examples. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of the raw materials of the product of the present invention, and the addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A method for preparing a powdering variety of traditional Chinese medicine formula granules by water extraction is characterized by comprising the following steps:
(1) Carrying out water extraction and decoction on the raw medicinal materials to obtain an extracting solution;
the raw material medicines are any one of coarse powder, fine powder or superfine powder or a combination of at least two of the coarse powder, the fine powder and the superfine powder, and the raw material medicines are subjected to water extraction and decoction after being packed into a medicine bag; the raw material medicinal materials are decoction pieces, and the raw material medicinal materials are directly subjected to water extraction and decoction;
(2) Concentrating the extracting solution obtained in the step (1) under reduced pressure to obtain clear paste;
(3) Stirring and heating the clear paste obtained in the step (2), and then carrying out spray drying to obtain dry extract powder;
(4) And (4) mixing the dry extract powder obtained in the step (3) with optional auxiliary materials, and performing dry granulation to obtain the traditional Chinese medicine formula granules.
2. The method for preparing powdered Chinese medicinal formula granule with water extraction of claim 1, wherein in step (1), the raw material herbs are selected from one or a combination of at least two of calcined clamshell, concretio silicea bambusae, cornu bubali and ootheca mantidis.
3. The method for preparing powdered traditional Chinese medicine formula granules by water extraction as claimed in claim 1 or 2, wherein in step (1), the particle size of the ultra-fine powder is 0.001-0.075 mm.
4. The method for preparing powdered traditional Chinese medicine formula granule by water extraction according to any one of claims 1-3, wherein in step (1), the material of the pack is any one of corn fiber, non-woven pp material or non-woven pet material, preferably non-woven pp material;
preferably, in step (1), the loading amount of the drug substance is less than 50% of the total volume of the drug package.
5. The method for preparing powdered variety of Chinese medicinal formula granule with water extraction of any one of claims 1-4, wherein in step (1), the water extraction and decoction is heating to boiling extraction;
preferably, the number of times of water extraction and decoction is 1 to 3 times, preferably 2 times;
preferably, the total time of water extraction and decoction is 0.5 to 3 hours, preferably 0.5 to 2 hours;
preferably, the amount of the solvent for water extraction and decoction is 6 to 20 times, and preferably 8 to 14 times.
6. The method for preparing powdered variety of Chinese medicinal formula granule with water extraction according to any of claims 1-5, wherein the water extraction and decoction comprises the following steps:
(a) Adding water into the medicine bag filled with the raw medicinal materials, decocting for the first time, filtering, and collecting dregs and a first extracting solution;
(b) Adding water into the dregs obtained in the step (a), carrying out second decoction to obtain a second extracting solution, and combining the first extracting solution and the second extracting solution to obtain an extracting solution.
7. The method for preparing powdered Chinese medicinal formula particles by water extraction as claimed in any one of claims 1-6, wherein in step (2), the temperature of the vacuum concentration is 50-80 ℃, and the pressure of the vacuum concentration is 0.07-0.09 Mpa;
preferably, in the step (2), the relative density of the clear paste is 1.05-1.20.
8. The method for preparing powdered variety of Chinese medicinal formula particle with water extraction of any one of claims 1-7, wherein in step (3), the stirring is heated to 55-65 ℃;
preferably, in the step (3), in the spray drying, the inlet air temperature of the spray tower is 160-180 ℃, the outlet air temperature of the spray tower is 60-85 ℃, and the feeding pump frequency is 20-30 Hz.
9. The method for preparing powdered variety of Chinese medicinal formula granule with water extraction of any one of claims 1-8, wherein in step (4), the adjuvant is selected from any one of maltodextrin, dextrin, corn starch or potato starch, preferably maltodextrin;
preferably, in the step (4), the mass ratio of the dry extract powder to the auxiliary materials is 1 (0-1);
preferably, in the step (4), the rotation speed of the mixing is 80-180 rpm, and the mixing time is 20-60 min.
10. The method for preparing powdered Chinese medicine formulation granule with water extraction according to any one of claims 1-9, wherein in step (4), the dry granulation has a roller gap of 0.6-2.5 mm, a roller rotation speed of 20-50 rpm, and a pressure of 80-100 bar;
preferably, in step (4), the dry granulation is further screened
Preferably, in the step (4), the particle size of the traditional Chinese medicine formula particle is 16-40 meshes.
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