Preparation method of cicada slough cough-relieving granules

Through new preparation methods, including ethanol reflux extraction, multiple decoction and spray granulation, the problems of baicalin loss and complex operation in the preparation of cicada sulphur cough granules are solved, and a more efficient and stable granulation process and higher finished product yield are achieved.

CN119656116AActive Publication Date: 2025-03-21JINLING PHARMA
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Patent Information

Application Number
CN202411967933.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-30
Publication Date
2025-03-21
Estimated Expiration
2044-12-30

AI Technical Summary

Technical Problem

In the preparation process of cicada cough-relieving granules, the heat-sensitive ingredient baicalin is unstable due to heat and loses a lot, the operation steps are complicated, microbial control is difficult, and the finished product yield is low.

Method used

A new preparation method is adopted, including ethanol reflux extraction of volatile oils and cicada shells of medicinal materials such as schizonepeta, multiple decoctions of medicine residues, mixed concentration of alcohol extraction and water extraction extract, and spray granulation after adding dextrin and steviol glycoside. One-step granulation is achieved by adjusting process parameters such as air inlet temperature, fan frequency, material temperature, peristaltic pump speed and extract temperature during the injection process.

Benefits of technology

It significantly reduces the relative density of extract concentration, shortens the preparation time, improves the transfer rate of the thermally sensitive ingredient baicalin, improves the stability and finished product yield, simplifies the process flow, and reduces the risk of microbial contamination.

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Abstract

The invention relates to a novel preparation method of cicada slough cough-relieving granules, which comprises the following steps: taking cicada slough, scutellaria baicalensis, lumbricus, aster tataricus, stemona and myrobalan, adding ethanol, performing reflux extraction, filtering, concentrating filtrate, and merging concentrated solutions to obtain an alcohol extract and decoction dregs II; combining the medicine residue II with the medicine residue I of schizonepeta, residual liquid and stiff silkworm, adding water, decocting, filtering, concentrating filtrate under reduced pressure, and combining concentrated solutions to obtain a water extract; and mixing the alcohol extract and the water extract, and concentrating to obtain the cicada slough cough-relieving granule extract. And carrying out one-step granulation and drying on the cicada slough cough-relieving granule extract, sieving and finishing granules, and totally mixing to obtain the cicada slough cough-relieving granules. According to the method, multiple processes of mixing, spraying, forming, drying and the like are completed in one device, circulation of products among different devices is reduced, the risk of introducing microorganisms is reduced, the preparation time is shortened, the transfer rate of the index component baicalin is obviously increased, operation is easy, the yield of finished products is increased, and the method is suitable for industrial production.
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Description

Technical Field

[0001] The invention relates to the field of traditional Chinese medicine pharmacy, in particular to a method for preparing cicada shell cough relieving granules. Background Art

[0002] Chantui Anti-cough Granules are based on the basic theories of traditional Chinese medicine, "wind is the root of all diseases" and "wind is a yang evil, and coughing occurs when wind and fire collide". They break the habit of continuing to use heat-clearing and detoxifying drugs, establish the path of dispelling wind evil, clearing lung collaterals, and clearing and clearing cough as the main method, select drugs, and reasonably match them to achieve the effects of clearing and clearing, dispersing and collecting, combining movement and stillness, and rising and falling. It is a safe, efficient, convenient, and simple new Chinese medicine. Chinese patent CN101181561A discloses the active ingredients of Chantui Anti-cough Granules, including Chantui, Scutellaria, Pheretima, Aster, Stemona, Terminalia chebula, Schizonepeta, and Bombyx batryticatus. However, its preparation process has many shortcomings: 1. Because its extract contains more polysaccharides and macromolecular components and has high viscosity, the reduced pressure drying time is about 50 hours, which consumes high energy and time; 2. The extract accounts for a high proportion, and the traditional wet granulation process is difficult to granulate and has a low yield; 3. The heat-sensitive ingredient baicalin is easily decomposed by heat. If the extract drying and granulation drying time are long, it will lead to a large loss of the indicator ingredient baicalin in the original granules, and the transfer rate of baicalin compared to the input medicinal materials is lower.

[0003] Therefore, it is urgent to modify the above preparation method to overcome the problems in the preparation process of Chantui cough granules, such as the heat-sensitive component baicalin is unstable when heated and has a lot of losses, the operation steps are cumbersome, the microorganisms are difficult to control, and the finished product yield is low. Summary of the invention

[0004] The purpose of the present invention is to provide a new preparation method of cicada shell cough relieving granules to solve the above technical problems.

[0005] To achieve the purpose of the present invention, the technical solution is as follows: A method for preparing cicada shell cough relieving granules comprises the following steps: S1. Prepare the formula according to the ratio of cicada shell, scutellaria, earthworm, aster, radix stemonae, terminalia chebula, schizonepeta, and bombyx batryticatus; S2, Nepeta soaked in water, extract volatile oil, Nepeta residue I and the residual liquid set aside; S3, taking cicada slough, scutellaria, earthworm, aster, stemon and terminalia chebula, adding ethanol to extract 2-4 times, filtering, concentrating the filtrate, combining the concentrates to obtain an alcohol extract and a residue II; combining the residue II with the residue I and the residual liquid of schizonepeta tenuifolia and bombyx batryticatus, adding water to decoct, filtering, concentrating the filtrate under reduced pressure, combining the concentrates to obtain a water extract; S4, mixing the alcohol extract and the water extract to concentrate to obtain the cicada shell cough relieving granule extract; S5. Add the cicada slough cough relieving granule extract into hot water and stir, and heat and keep warm to 40-60°C; add dextrin and stevioside into a boiling drying granulator, set the inlet air temperature to 80-120°C and the fan frequency to 20-50HZ, heat the material to 55°C, turn on the peristaltic pump, keep the peristaltic pump speed at 200-600rpm, and perform spray granulation. During the spray granulation process, the material temperature in the furnace is 50-70°C, the temperature of the cicada slough cough relieving granule extract in the insulation barrel is maintained at 50-60°C, and the compressed air pressure is 0.35±0.05Mpa; after the cicada slough cough relieving granule thick extract is sprayed, the material temperature is controlled at 60-70°C and maintained for 15-60min to obtain one-step granulation granules.

[0006] Furthermore, after the step S5, the method further comprises the step S6 of sieving the one-step granulated particles; wherein the upper layer is sieved through a 14-mesh sieve and the lower layer is sieved through a 60-mesh sieve.

[0007] Further, in step S2, the volatile oil of Nepeta is obtained, which further includes adding beta-cyclodextrin and water, grinding and inclusion with a colloid mill, filtering, and drying the inclusion compound to prepare a volatile oil inclusion compound. Preferably, the amount of beta-cyclodextrin used is 4 times the amount of the volatile oil, and the amount of water is 40 times the amount of the volatile oil. The grinding and inclusion time is 10 minutes, and the mixture is dried at 70°C.

[0008] Furthermore, in step S2, the Nepeta tenuifolia is soaked in water, using 10 times the amount of water, for 2 hours, and the time for extracting volatile oil is 3 hours.

[0009] Further, in step S3, the ethanol used is 60-80% ethanol by mass concentration. Preferably, the ethanol by mass concentration is 70%. The ethanol reflux extraction time is 1-3h each time. Preferably, the ethanol reflux extraction is performed 3 times with a mass concentration of 70%, each time for 2 hours.

[0010] Further, in step S3, the residue II is combined with the residue I of Nepeta and the residual liquid, and Bombyx batryticatus, and boiled in water for 2-4 times, each time for 2-3 hours. Preferably, the residue II is combined with the residue I of Nepeta and the residual liquid, and Bombyx batryticatus, and boiled in water for 3 times, each time for 2.5 hours.

[0011] Furthermore, after step S6, the preparation method further comprises step S7, taking the whole sieved particles and adding the volatile oil inclusion compound. The mixing speed is 5 rpm and the operation time is 10 minutes.

[0012] Furthermore, the formula ratio described in step S1 is 400-450 parts by weight of cicada molt, 200-250 parts by weight of scutellaria baicalensis, 250-300 parts by weight of earthworm, 250-300 parts by weight of aster, 400-450 parts by weight of stemona, 200-250 parts by weight of terminalia chebula, 200-250 parts by weight of schizonepeta, and 200-250 parts by weight of bombyx batryticatus.

[0013] Furthermore, in step S5, the peristaltic pump speed is 200-600 rpm, which means that the speed is 200 rpm when the peristaltic pump is turned on, and the speed of the peristaltic pump is gradually adjusted to 600 rpm. Preferably, the peristaltic pump speed is 230-500 rpm; more preferably, 230-400 rpm.

[0014] Furthermore, in step S5, the amount of dextrin added is 15% to 40% of the theoretical total amount; the amount of stevioside added is 0.3% to 1.0% of the theoretical total amount. Preferably, the amount of dextrin added is 20 to 30% of the theoretical amount; the amount of stevioside added is 0.5% of the theoretical amount.

[0015] Furthermore, in step S3, the cicada slough, scutellaria baicalensis, earthworm, aster, stemon and terminalia chebula are extracted with ethanol by reflux, filtered, and the filtrate is concentrated to a relative density of 1.15-1.30; the medicinal residue II is combined with the medicinal residue I of schizonepeta tenuifolia and the residual liquid, and bombyx batryticatus, boiled with water, filtered, and the filtrate is concentrated under reduced pressure to a relative density of 1.15-1.30.

[0016] Furthermore, in step S4, the alcohol extract and the water extract are mixed and concentrated to 70° C., with a relative density of 1.15 to 1.30, preferably 1.20.

[0017] Furthermore, in step S5, the cicada shell cough relieving granule extract is added to hot water and stirred, and heated and kept warm to 40-60° C., with a relative density of 1.16-1.20. Preferably, heated and kept warm to 50-60° C., with a relative density of 1.18.

[0018] It should be noted that in step S5, the materials in the furnace during the spray granulation process include dextrin, steviol glycoside, and when the granulation starts, the dextrin and steviol glycoside that wrap the cicada shell cough relieving granule extract.

[0019] Compared with the prior art, the present invention has the following significant advantages: (1) Compared with the original process (Example 1 of CN101181561A), the present invention reduces the relative density of the concentrated extract, shortens the preparation time, and significantly improves the transfer rate of the heat-sensitive component baicalin; (2) In the 0, 1, 2, 3, 6 accelerated and 3, 6 month long-term stability tests, there was no significant change in moisture, particle size and baicalin content, indicating good stability; (3) The one-step granulation method reduces the flow of products between different equipment, reduces the risk of introducing microorganisms, and reduces the loss of extracts; (4) The preparation process is simple and suitable for industrial production; (5) The extract of Chan Tuo Antitussive Granules accounts for a very high proportion. The general one-step granulation process parameters are easy to cause "bed collapse" and make granulation impossible. By adjusting relevant process parameters, such as air inlet temperature, fan frequency, material temperature, peristaltic pump speed, extract temperature during spraying, compressed air pressure, and the synergistic effect of materials after spraying, the final granules are more uniform and have a high yield rate. At the same time, by adding hot water to stir the Chan Tuo Antitussive Granule extract, keeping it warm, and controlling its density, it is conducive to atomization and makes the spraying smoother. The drying efficiency is guaranteed by controlling the air inlet temperature. The spraying speed is controlled by the peristaltic pump speed to ensure the size of the particles. The extract temperature during the spraying process is conducive to atomization and makes the spraying smoother. Finally, the particle size and uniformity of the particles are guaranteed by screening and total mixing. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 It is a flow chart of the preparation process of Example 1 of the present invention.

[0021] Figure 2 This is a graph showing the variation trend of baicalin content in Example 3 of the present invention. DETAILED DESCRIPTION

[0022] The embodiments of the present invention are described in detail below with reference to the accompanying drawings.

[0023] Example 1 Preparation of cicada shell cough relieving granules The formula of cicada shell cough-relieving granules includes: cicada shell 41.4kg, scutellaria baicalensis 23.0kg, earthworm 27.6kg, bombyx batryticatus 23.0kg, schizonepeta tenuifolia 23.0kg, aster tataricus 27.6kg, stemona 41.4kg, and terminalia chebula 23.0kg.

[0024] like Figure 1 , 2, the preparation method comprises the following steps: S1 Take the raw materials according to the above formula, wherein Nepeta add 10 times the amount of water soaked for 2 hours, extract the volatile oil for 3 hours, the residue I and the residual liquid set aside; S2 step S1 extracted volatile oil plus 40 times the amount of water, 4 times the amount of his cyclodextrin, with a colloid mill inclusion for 10 minutes, filtered, the inclusion complex 70 ℃ drying, set aside; S3: add 1472L of 70% ethanol to Periostracum Cicadae, Radix Scutellariae, Pheretima, Radix Asteris, Radix Stemonae, and Fructus Terminaliae Terminaliae, extract by reflux for 3 times, each time for 2 hours, filter, concentrate the filtrate to 70°C, relative density 1.15-1.30, combine the three extracts to obtain alcohol extract and residue II; combine the residue II obtained above with the residue I and the residual liquid in step S1, add Bombyx Batryticatus, add 1840L of water, decoct for 3 times, each time for 2.5 hours, filter, reduce the pressure on the filtrate and concentrate it to 70°C with relative density 1.15-1.30, combine the three extracts to obtain water extract; S4. Mix the alcohol extract and the water extract, and concentrate to a relative density of 1.20 at 70°C to obtain the cicada shell cough relieving granule extract; S5 Add appropriate amount of hot water to the cicada shell cough relieving granule extract in a mixing bucket and stir evenly. Heat and keep warm to 50℃~60℃, with a relative density of 1.18. Add dextrin (the amount added is 23% of the total amount theoretically obtained) and stevioside (the amount added is 0.5% of the total amount theoretically obtained) into the boiling drying granulator, set the inlet air temperature to 90-110°C and the fan frequency to 20-50HZ, heat the material to 55°C, set the peristaltic pump to maintain the speed at 230-360rpm (i.e., the speed is 230 rpm when the peristaltic pump is turned on, and the speed of the peristaltic pump is gradually adjusted to 360rpm), and start spray granulation. During the spray granulation process, the inlet air temperature is controlled at 90-105°C, the material temperature in the furnace is 60-70°C, the temperature of the cicada shell cough relieving granule extract in the barrel is maintained at 50-60°C, and the compressed air pressure is 0.35±0.05Mpa; after the cicada shell cough relieving granule extract is sprayed, the material temperature is controlled at 60-70°C for 40 minutes; S6. The granules obtained in step S5 are sieved through a sieve with a mesh size of 14 mesh on the upper layer and 60 mesh on the lower layer; S7 Total mixing: Add the qualified granules after sieving to the volatile oil inclusion compound obtained in step S2, rotate at 5 rpm, mix for 10 minutes, and mix evenly to obtain Chantui cough-relieving granules.

[0025] Comparative Example 1: Changes in one-step granulation process parameters The same formula and preparation method as in Example 1 are the same, except that in step S5: the cicada shell cough relieving granule extract is at room temperature and has a relative density of 1.35. Dextrin (the amount added is 23% of the total amount theoretically obtained) and stevioside (the amount added is 0.5% of the total amount theoretically obtained) are added to the boiling drying granulator. The parameters of the boiling drying granulator are set as follows: inlet air temperature 50~79℃; fan frequency 25~28HZ; material temperature in the furnace 40~50℃; peristaltic pump speed is maintained at a constant 230rpm; compressed air pressure 0.35±0.05Mpa.

[0026] Result: The extract was viscous, precipitation occurred and blocked the spray gun and pipeline, and granulation could not be successfully performed in one step.

[0027] Comparative Example 2: Changes in one-step granulation process parameters The same formula and preparation method as in Example 1 are the same, except that in step S5: add appropriate amount of hot water to the cicada shell cough granule extract and stir evenly in a stirring barrel, heat and keep warm to 50-60°C, the relative density of the extract is 1.18, and dextrin (the amount added is 23% of the total amount theoretically obtained) and stevioside (the amount added is 0.5% of the total amount theoretically obtained) are added to the boiling drying granulator. The parameters of the boiling drying granulator are set as follows: inlet air temperature 50-79°C; fan frequency 25-28HZ; material temperature in the furnace 40-49°C; peristaltic pump speed is maintained at a constant 230rpm; compressed air pressure 0.35±0.05Mpa. The extract is kept warm at 50-60°C during the granulation process.

[0028] Results: By adjusting the relative density and temperature of the Chantui Antitussive Granules extract, the initial stage of granulation was normal, but as the granulation progressed, the material in the pot collapsed.

[0029] Comparative Example 3: Changes in one-step granulation process parameters The same formula and preparation method as in Example 1 are the same, except that in step S5: add appropriate amount of hot water to the cicada shell cough granule extract and stir evenly in a stirring barrel, heat and keep warm to 50-60°C, the extract relative density is 1.18, and dextrin (the amount added is 23% of the total amount theoretically obtained) and stevioside (the amount added is 0.5% of the total amount theoretically obtained) are added to the boiling drying granulator. The parameters of the boiling drying granulator are set as follows: inlet air temperature 80-100°C; fan frequency 25-30HZ; material temperature in the furnace 60-70°C; peristaltic pump speed is maintained at a constant 230rpm; compressed air pressure 0.35±0.05Mpa. The extract is kept warm at 50-60°C during the granulation process.

[0030] Results: The drying efficiency can be improved by adjusting the air inlet temperature and the material temperature in the furnace, but the amount of fine powder produced is relatively large, which does not meet the production requirements, and the spraying preparation time is long and the efficiency is low.

[0031] Example 2: Changes in one-step granulation process parameters The same formula and preparation method as in Example 1 are the same, except that in step S5: add appropriate amount of hot water to the cicada shell cough granule extract and stir evenly in a stirring barrel, heat and keep warm to 50-60°C, the relative density of the extract is 1.18, and dextrin (the amount added is 23% of the total amount theoretically obtained) and stevioside (the amount added is 0.5% of the total amount theoretically obtained) are added to the boiling drying granulator. The parameters of the boiling drying granulator are set as follows: inlet air temperature 90-105°C; fan frequency 25-30HZ; material temperature in the furnace 60-70°C; peristaltic pump speed 230-400rpm (i.e., the speed is 230 rpm when the peristaltic pump is turned on, and the peristaltic pump speed is gradually adjusted to 400rpm); compressed air pressure 0.35±0.05Mpa. The extract is kept warm at 50-60°C during the granulation process.

[0032] Results: During the preparation process, the rotation speed of the peristaltic pump was adjusted to reduce the amount of fine powder and improve the yield.

[0033] Example 3 The specific process steps in CN101181561A are as follows: The recipe is the same as in Example 1.

[0034] The preparation method is as follows: a. Take the raw materials according to the above recipe, where Nepeta soaked in water for 2 hours, extract the volatile oil for 3 hours, 1 residue and the residual liquid set aside; b. Add 40 times the amount of water and 4 times the amount of β-cyclodextrin to the volatile oil, grind it with a colloid mill for 10 minutes, filter it, dry the inclusion complex at 70°C, and set aside for later use; c. cicada slough, scutellaria, earthworm, aster, stemon, terminalia chebula plus 1472L, mass concentration of 70% ethanol reflux extraction 3 times, each 2 hours, filtered to obtain the residue II and the filtrate, the filtrate was combined, ethanol was recovered until there was no alcohol taste, the liquid was reserved; d. The residue II and the residue 1 of step a were combined with the residual liquid, added to silkworm, 1840L of water, decocted 3 times, each time for 2.5 hours, the filtrate was combined, filtered, and the filtrate was concentrated to a relative density of about 1.3 at 70 ° C under reduced pressure, combined with the liquid obtained in step c, vacuum dried, and crushed into a fine powder; e. Add 45 kg of dextrin to the fine powder and mix well. Prepare granules with 80% ethanol by mass concentration. Add the inclusion compound obtained in step b to the granules and mix well. Pack and prepare granules.

[0035] The cicada shell cough relieving granules of Example 1 are compared with the original process CN101181561A, and the specific key process parameters are shown in Table 1.

[0036] Table 1: Summary of key parameters of new and old processes

[0037] Note: * Granulation process time includes extract drying time and granulation time **Amount per bag: 10g Total extract, in the preparation method of CN101181561A, refers to the extract obtained by combining the drug solution obtained in step c in step d. In Example 1, it refers to the extract obtained in step S4.

[0038] The method for determining the content of baicalin is as follows: determined according to high performance liquid chromatography (High Performance Liquid Chromatography, General Rules 0512 of Part IV of the 2020 Edition of the Chinese Pharmacopoeia).

[0039] Chromatographic conditions and system suitability test: Octadecylsilane bonded silica gel was used as filler, methanol was used as mobile phase A, 0.6% phosphoric acid solution was used as mobile phase B, gradient elution was performed according to the provisions in Table 2, column temperature was 25°C, flow rate was 1ml / min, and detection wavelength was 280nm. The theoretical plate number calculated based on the baicalin peak should be no less than 2500.

[0040] Table 2: Gradient elution program

[0041] Preparation of reference solution: Accurately weigh an appropriate amount of baicalin reference substance, add methanol to make a solution containing 30 μg per 1 ml.

[0042] Preparation of test solution: Take the product, grind it into powder, take about 0.5g, accurately weigh it, put it in a 100ml volumetric flask, slowly add 90ml of 75% methanol, shake while adding, ultrasonically treat (power 500W, frequency 40kHz) for 1 hour, let cool, add 75% methanol to dilute to the scale, shake well, let stand, centrifuge (5000rpm, 5 minutes), accurately measure 2ml of the supernatant, put it in a 10ml volumetric flask, add methanol to dilute to the scale, shake well, filter through 0.45μm microporous filter membrane, and take the filtrate to obtain.

[0043] Determination method: Accurately pipette 10μl of reference solution and test solution respectively, inject into liquid chromatograph, and determine.

[0044] It can be seen from Table 1 that: 1. In the new process of Example 1, the alcohol extract or the water extract is concentrated separately and then combined, which reduces the requirement for extract concentration, shortens the heating time of the extract, and the extraction rate of the heat-sensitive component baicalin is higher than that of the original extraction process; 2. The granulation time in the new process is shorter, and the content of the heat-sensitive component baicalin is about 40% higher than that of the old process; 3. The new process reduces the flow of products between different equipment, the loss is greatly reduced, and the particle yield of the new process is also significantly improved.

[0045] Example 4 Investigation of baicalin transfer rate during one-step granulation Add appropriate amount of hot water to the cicada shell cough relieving granule extract and stir evenly in a mixing barrel, heat and keep warm to 50℃-60℃, relative density 1.18. Add 23% of the theoretical amount of dextrin and 0.5% of the theoretical amount of stevioside to the boiling drying granulator, set the air inlet temperature to 90-110℃, the fan frequency to 20-50HZ, heat the material to 55℃, set the peristaltic pump, keep the speed at 230rpm, start spray granulation, control the material temperature in the furnace to 60-70℃ during the spray granulation process, the temperature of the cicada shell cough relieving granule extract in the barrel is 50-60℃, the compressed air pressure is 0.35±0.05Mpa, and gradually adjust the peristaltic pump speed to 400rpm. After the cicada shell cough relieving granule extract is sprayed, the material temperature is controlled below 60-70℃ for 15-60min. As the extract was continuously sprayed into the boiling drying granulator, samples were taken to detect the baicalin content in the sprayed Chantui Antitussive Granule extract (i.e., the baicalin input amount) and the baicalin content in the material in the furnace (i.e., the baicalin measured amount). The results are shown in Table 3.

[0046] Table 3 Change trend of baicalin in the new process

[0047] The results in Table 3 show that during the new granulation process provided by the present application, the loss of the heat-sensitive component baicalin is relatively small.

[0048] Example 5 Stability Study The granule sample prepared in Example 1 was placed in a stability test chamber for accelerated and long-term stability tests. The accelerated stability test conditions were set to (40°C ± 2°C, RH 75% ± 5%), and samples were taken at 0, 1, 2, 3, and 6 months respectively; the long-term stability test conditions were set to (25°C ± 2°C, RH 60% ± 10%), and samples were taken at 0, 3, and 6 months respectively. The results are shown in Tables 4 and 5.

[0049] Table 4 Accelerated stability results

[0050] Table 5 Long-term stability results

[0051] The results showed that under long-term and accelerated test conditions, the samples prepared by the new process did not show significant changes in moisture, particle size, baicalin content and other indicators compared with the 0-day results, the microbial limits met the quality standards and had good stability.

Claims

1. A method for preparing cicada shell cough relieving granules, characterized in that: The preparation method comprises the following steps: S1. Prepare the formula according to the ratio of cicada shell, scutellaria, earthworm, aster, radix stemonae, terminalia chebula, schizonepeta, and bombyx batryticatus; S2, Nepeta soaked in water, extract volatile oil, Nepeta residue I and the residual liquid set aside; S3, taking cicada slough, scutellaria, earthworm, aster, stemon and terminalia chebula, adding ethanol to extract 2-4 times, filtering, concentrating the filtrate, combining the concentrates to obtain an alcohol extract and a residue II; combining the residue II with the residue I and the residual liquid of schizonepeta tenuifolia and bombyx batryticatus, adding water to decoct, filtering, concentrating the filtrate under reduced pressure, combining the concentrates to obtain a water extract; S4, mixing the alcohol extract and the water extract, concentrating, and obtaining the cicada shell cough relieving granule extract; S5. Add the cicada slough cough relieving granule extract into hot water and stir, and heat and keep warm to 40-60°C; add dextrin and stevioside into a boiling drying granulator, set the inlet air temperature to 80-120°C and the fan frequency to 20-50HZ, heat the material to 55°C, turn on the peristaltic pump, keep the peristaltic pump speed at 200-600rpm, and perform spray granulation. During the spray granulation process, the material temperature in the furnace is 50-70°C, the temperature of the cicada slough cough relieving granule extract in the insulation barrel is maintained at 50-60°C, and the compressed air pressure is 0.35±0.05Mpa; after the cicada slough cough relieving granule thick extract is sprayed, the material temperature is controlled at 60-70°C and maintained for 15-60min to obtain one-step granulation granules.

2. The method for preparing the cicada shell cough relieving granules according to claim 1, characterized in that: After step S5, the method further comprises step S6 of sieving the one-step granulated particles; wherein the upper layer is sieved through a 14-mesh sieve and the lower layer is sieved through a 60-mesh sieve.

3. The method for preparing the cicada shell cough relieving granules according to claim 2, characterized in that: The step S2 of obtaining schizonepeta volatile oil also includes adding cyclodextrin and water, grinding and inclusion by a colloid mill, filtering, and drying the inclusion compound to prepare a volatile oil inclusion compound.

4. The method for preparing the cicada shell cough relieving granules according to claim 3, characterized in that: After step S6, the preparation method further comprises step S7, taking the sieved whole grains and adding the volatile oil inclusion compound.

5. The method for preparing the cicada shell cough relieving granules according to claim 4, characterized in that: The rotation speed of adding the volatile oil inclusion compound and mixing is 5 rpm, and the operation time is 10 minutes.

6. The method for preparing the cicada shell cough relieving granules according to claim 1, characterized in that: The formula ratio in step S1 is 400-450 parts by weight of cicada molt, 200-250 parts by weight of scutellaria baicalensis, 250-300 parts by weight of earthworm, 250-300 parts by weight of aster, 400-450 parts by weight of stemona, 200-250 parts by weight of terminalia chebula, 200-250 parts by weight of schizonepeta, and 200-250 parts by weight of bombyx batryticatus.

7. The method for preparing the cicada shell cough relieving granules according to claim 1, characterized in that: In step S5, the peristaltic pump speed is 200-600 rpm, which means that the speed is 200 rpm when the peristaltic pump is turned on, and the speed of the peristaltic pump is gradually adjusted to 600 rpm.

8. The method for preparing the cicada shell cough relieving granules according to claim 1, characterized in that: In step S5, the amount of dextrin added is 15% to 40% of the total amount theoretically prepared; the amount of stevioside added is 0.3% to 1.0% of the total amount theoretically prepared.

9. The method for preparing the cicada shell cough relieving granules according to claim 1, characterized in that: In step S3, the cicada slough, scutellaria baicalensis, earthworm, aster, stemona and terminalia chebula are extracted with ethanol reflux for 2 to 4 times, filtered, and the filtrate is concentrated to a relative density of 1.15 to 1.30; the medicinal residue II is combined with the medicinal residue I of schizonepeta tenuifolia and the residual liquid, and bombyx batryticatus, boiled with water, filtered, and the filtrate is concentrated under reduced pressure to a relative density of 1.15 to 1.

30.

10. The method for preparing the cicada shell cough relieving granules according to claim 1, characterized in that: In step S4, the alcohol extract and the water extract are mixed and concentrated to 70° C. with a relative density of 1.15 to 1.

30.

11. The method for preparing the cicada shell cough relieving granules according to claim 1, characterized in that: In step S5, the cicada shell cough relieving granule extract is added into hot water and stirred, and heated to 40-60° C., with a relative density of 1.16-1.20.

Citation Information

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