Preparation method of cicada slough cough-relieving granules
Through the combined spray granulation method of ethanol and water extraction, the problems of unstable and low yield of baicalin in the preparation of cicada cough granules were solved, and efficient and stable granule preparation was achieved, which was suitable for industrial production.
Patent Information
- Application Number
- CN202411967933.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-30
- Publication Date
- 2025-08-29
- Estimated Expiration
- 2044-12-30
AI Technical Summary
The existing preparation process of cicada shell cough relieving granules has problems such as unstable thermal ingredient baicalin, complicated operation steps, difficult microbial control, and low yield of finished products.
The spray granulation process is adopted by combining ethanol and water extraction with spray granulation method. By adjusting parameters such as inlet air temperature, fan frequency, peristaltic pump speed and compressed air pressure, the spray granulation process is controlled, combined with the use of dextrin and steviol glycoside, a one-step granulation method is realized, reducing the viscosity of the extract and improving the yield of finished products.
It improves the transfer rate of the thermally sensitive component baicalin, shortens the preparation time, reduces energy consumption, improves the yield of finished products, and ensures the uniformity and stability of particles, which is suitable for industrial production.
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Figure CN119656116B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the field of traditional Chinese medicine pharmacy, in particular to a method for preparing cicada slough cough-relieving granules. Background Art
[0002] Based on the fundamental theories of Traditional Chinese Medicine (TCM), namely, "wind is the root of all diseases" and "wind is a yang evil, and coughs occur when wind and fire collide." Chantui Zhike Granules break the traditional practice of clearing heat and detoxifying, instead focusing on dispelling wind pathogens, clearing the lung meridians, and promoting cough relief. By carefully selecting and rationally combining herbs, they achieve the effects of promoting both purgation and purging, dispersing and restraining, combining movement and stillness, and promoting both ascending and descending. This new TCM medicine is safe, effective, convenient, and simple. Chinese patent CN101181561A discloses the active ingredients of Chantui Zhike Granules, including Chantui, Scutellaria baicalensis, Earthworm, Aster tataricus, Stemona tuber, Terminalia chebula, Schizonepeta tenuifolia, and Bombyx batryticatus. However, its preparation process has many shortcomings: 1. Because its extract contains a large number of polysaccharides and macromolecular components and is highly viscous, the reduced pressure drying time is about 50 hours, which consumes high energy and is time-consuming; 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 index ingredient baicalin in the original granules, and the transfer rate of baicalin compared to the input medicinal materials is low.
[0003] Therefore, it is urgent to modify the above preparation method to overcome the problems in the preparation process of cicada shell cough granules, such as the heat-sensitive component baicalin is unstable when heated and suffers high loss, the operation steps are cumbersome, the microorganisms are difficult to control, and the yield of the finished product is low. Summary of the Invention
[0004] The purpose of the present invention is to provide a new preparation method of cicada slough cough relieving granules to solve the above technical problems.
[0005] To achieve the purpose of the present invention, the technical solutions are as follows:
[0006] A method for preparing cicada slough cough-relieving granules comprises the following steps:
[0007] S1. Prepare cicada slough, scutellaria baicalensis, earthworm, aster root, stemona root, terminalia chebula, schizonepeta tenuifolia, and bombyx batryticatus according to the formula ratio;
[0008] S2, after soaking Nepeta in water, extracting volatile oil, Nepeta slag I and the residual liquid set aside;
[0009] S3. Take cicada slough, scutellaria baicalensis, earthworm, aster, stemona and terminalia chebula, add ethanol and reflux extract 2-4 times, filter, concentrate the filtrate, and combine the concentrates to obtain an alcohol extract and medicinal residue II; combine medicinal residue II with medicinal residue I and the residual liquid of Schizonepeta tenuifolia and Bombyx batryticatus, add water and decoct, filter, concentrate the filtrate under reduced pressure, and combine the concentrates to obtain a water extract;
[0010] S4. Mixing the alcohol extract and the water extract to concentrate the extract to obtain the cicada shell cough relieving granule extract;
[0011] S5. Add the cicada slough cough-relieving granule extract to hot water and stir, and heat and keep warm to 40~60°C; add dextrin and steviol glycoside to a boiling drying granulator, set the inlet air temperature to 80~120°C and the fan frequency to 20~50HZ, heat the material to a temperature of 55°C, turn on the peristaltic pump, maintain 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.
[0012] Furthermore, after step S5, the method further includes 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.
[0013] Furthermore, in step S2, the volatile oil of Schizonepeta tenuifolia is obtained, and the method further comprises adding beta-cyclodextrin and water, grinding and including the inclusion compound in 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 used is 40 times the amount of the volatile oil. The grinding and including compounding time is 10 minutes, and the inclusion compound is dried at 70°C.
[0014] Furthermore, in step S2, the herb is soaked in water, using 10 times the amount of water, for 2 hours, and the volatile oil is extracted for 3 hours.
[0015] Furthermore, in step S3, the ethanol used is 60-80% by mass. Preferably, the ethanol is 70% by mass. The ethanol reflux extraction time is 1-3 hours each time. Preferably, the 70% by mass ethanol reflux extraction is performed three times, each time for 2 hours.
[0016] Furthermore, in step S3, the residue II is combined with the residue I of Schizonepeta tenuifolia and the residual liquid, and Bombyx batryticatus, and decocted with water for 2-4 times, each time for 2-3 hours. Preferably, the residue II is combined with the residue I of Schizonepeta tenuifolia and the residual liquid, and Bombyx batryticatus, and decocted with water for 3 times, each time for 2.5 hours.
[0017] Furthermore, after step S6, the preparation method further comprises step S7, wherein the sieved whole granules are added to the volatile oil inclusion compound. The mixing speed is 5 rpm and the operation time is 10 minutes.
[0018] Furthermore, the formula ratio described in step S1 is 400-450 parts by weight of cicada slough, 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 tenuifolia, and 200-250 parts by weight of bombyx batryticatus.
[0019] Furthermore, in step S5, the peristaltic pump speed is 200-600 rpm, which means that the peristaltic pump speed is 200 rpm when it is turned on, and the peristaltic pump speed is gradually adjusted to 600 rpm. Preferably, the peristaltic pump speed is 230-500 rpm; more preferably, 230-400 rpm.
[0020] Furthermore, in step S5, the amount of dextrin added is 15% to 40% of the theoretical total amount; the amount of steviol glycoside 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; and the amount of steviol glycoside added is 0.5% of the theoretical amount.
[0021] Furthermore, in step S3, the cicada slough, scutellaria baicalensis, earthworm, aster root, stemona radix and terminalia chebula are refluxed and extracted with ethanol, 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 the silkworm pupa, decocted with water, filtered, and the filtrate is concentrated under reduced pressure to a relative density of 1.15-1.30.
[0022] 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.
[0023] Furthermore, in step S5, the cicada slough cough-relieving granule extract is added to hot water with stirring, and heated to 40-60° C. with a relative density of 1.16-1.20. Preferably, the extract is heated to 50-60° C. with a relative density of 1.18.
[0024] 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.
[0025] Compared with the prior art, the present invention has the following significant advantages:
[0026] (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;
[0027] (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;
[0028] (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 extract;
[0029] (4) The preparation process is simple and suitable for industrial production;
[0030] (5) The extract of cicada shell cough relieving granules accounts for a very high proportion. The general one-step granulation process parameters are easy to cause "bed collapse" and granulation failure. By adjusting the relevant process parameters, such as the inlet air temperature, fan frequency, material temperature, peristaltic pump speed, extract temperature during spraying, compressed air pressure, and the synergistic effect of the material after spraying, the final granules are more uniform and have a high yield rate. At the same time, by adding hot water to the cicada shell cough relieving granules, stirring, keeping warm, and controlling its density, it is conducive to atomization and makes the spraying smoother. The drying efficiency is guaranteed by controlling the inlet air temperature. The spraying speed is controlled by the peristaltic pump speed to ensure the size of the particles formed. 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 mixing. BRIEF DESCRIPTION OF THE DRAWINGS
[0031] Figure 1 It is a flow chart of the preparation process of Example 1 of the present invention.
[0032] Figure 2 3 is a graph showing the changing trend of baicalin content in Example 3 of the present invention. DETAILED DESCRIPTION
[0033] The embodiments of the present invention are described in detail below with reference to the accompanying drawings.
[0034] Example 1 Preparation of cicada shell cough-relieving granules
[0035] The formula of cicada slough cough-relieving granules includes: cicada slough 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.
[0036] like Figure 1 , 2 shown, the preparation method comprises the following steps:
[0037] S1 Take the raw medicinal materials according to the above formula, wherein Schizonepeta 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;
[0038] S2 step S1 extracted volatile oil plus 40 times the amount of water, 4 times the amount of his cyclodextrin, colloid mill inclusion for 10 minutes, filtered, the inclusion complex 70 ℃ drying, set aside;
[0039] S3: Add 1472 L of 70% ethanol to the cicada slough, scutellaria baicalensis, earthworm, aster root, stemona root, and terminalia chebula, and extract them three times with reflux, each time for 2 hours. Filter and concentrate the filtrate to 70°C, with a relative density of 1.15-1.30. Combine the three extracts to obtain an alcohol extract and a medicinal residue II. Combine the medicinal residue II obtained above with the medicinal residue I and the residual liquid from step S1, add Bombyx batryticatus, add 1840 L of water, and boil three times, each time for 2.5 hours. Filter and concentrate the filtrate under reduced pressure, with a relative density of 1.15-1.30 at 70°C. Combine the three extracts to obtain a water extract.
[0040] 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;
[0041] 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℃. The relative density is 1.18. Dextrin (added amount is 23% of the total theoretical amount) and stevioside (added amount is 0.5% of the total theoretical amount) are added to the boiling drying granulator, and the inlet air temperature is set to 90-110°C and the fan frequency is 20-50HZ. After the material is heated to a temperature of 55°C, the peristaltic pump is set to maintain a speed of 230-360rpm (i.e., the speed is 230 rpm when the peristaltic pump is turned on, and the peristaltic pump speed is gradually adjusted to 360rpm). Spray granulation is started. 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.
[0042] S6. The granules obtained in step S5 are sieved through a 14-mesh sieve on the upper layer and a 60-mesh sieve on the lower layer;
[0043] S7 Total mixing: Add the qualified granules after sieving to the volatile oil inclusion compound obtained in step S2, rotate at 5 rpm, and mix for 10 minutes until evenly mixed to obtain the Chan Tuo Zhi Ke granules.
[0044] Comparative Example 1: Changes in one-step granulation process parameters
[0045] The same formulation and preparation method as in Example 1 were used, except that in step S5: Chan Tuo Zhi Ke Granule Extract was prepared at room temperature with a relative density of 1.35. Dextrin (23% of the theoretical total amount) and steviol glycoside (0.5% of the theoretical total amount) were added to a fluidized bed drying granulator. The fluidized bed drying granulator parameters were as follows: inlet air temperature 50-79°C; fan frequency 25-28 Hz; furnace material temperature 40-50°C; peristaltic pump speed maintained at a constant 230 rpm; and compressed air pressure 0.35±0.05 MPa.
[0046] Result: The extract was viscous, precipitation occurred and blocked the spray gun and pipeline, and granulation could not be successfully performed in one step.
[0047] Comparative Example 2: Changes in one-step granulation process parameters
[0048] The formula and preparation method are the same as in Example 1, except that in step S5, an appropriate amount of hot water is added to the cicada shell cough-relieving granule extract in a mixing bucket and stirred evenly. The extract is heated to 50-60°C, with a relative density of 1.18. Dextrin (23% of the theoretical total) and steviol glycoside (0.5% of the theoretical total) are then added to a fluidized bed drying granulator. The fluidized bed drying granulator parameters are: inlet air temperature 50-79°C; fan frequency 25-28 Hz; furnace material temperature 40-49°C; peristaltic pump speed maintained at a constant 230 rpm; compressed air pressure 0.35±0.05 MPa. The extract is kept at 50-60°C during granulation.
[0049] Results: By adjusting the relative density and temperature of the Chantuo Zhike Granule extract, the initial stage of granulation was normal, but as the granulation progressed, the material in the pot collapsed.
[0050] Comparative Example 3: Changes in one-step granulation process parameters
[0051] The formula and preparation method are the same as in Example 1, except that in step S5, an appropriate amount of hot water is added to the cicada shell cough-relieving granule extract in a mixing bucket and stirred evenly. The extract is heated to 50-60°C, with a relative density of 1.18. Dextrin (23% of the theoretical total) and steviol glycoside (0.5% of the theoretical total) are then added to a fluidized bed drying granulator. The fluidized bed drying granulator parameters are: inlet air temperature 80-100°C; fan frequency 25-30 Hz; furnace material temperature 60-70°C; peristaltic pump speed maintained at a constant 230 rpm; compressed air pressure 0.35±0.05 MPa. The extract is kept at 50-60°C during granulation.
[0052] Results: The drying efficiency can be improved by adjusting the inlet air temperature and the material temperature in the furnace. However, the amount of fine powder produced is large, which does not meet the production requirements. In addition, the spraying preparation time is long and the efficiency is low.
[0053] Example 2: Changes in one-step granulation process parameters
[0054] The formula and preparation method are the same as in Example 1, except that in step S5: an appropriate amount of hot water is added to the cicada shell cough-relieving granule extract in a mixing bucket and stirred evenly. The extract is heated to 50-60°C, with a relative density of 1.18. Dextrin (23% of the theoretical total amount) and steviol glycoside (0.5% of the theoretical total amount) are then added to a fluidized bed drying granulator. The fluidized bed drying granulator parameters are: inlet air temperature 90-105°C; fan frequency 25-30 Hz; furnace material temperature 60-70°C; peristaltic pump speed 230-400 rpm (i.e., starting at 230 rpm and gradually adjusting to 400 rpm); and compressed air pressure 0.35±0.05 MPa. The extract is kept at 50-60°C during granulation.
[0055] Results: During the preparation process, the peristaltic pump speed was adjusted to reduce the amount of fine powder and improve the yield.
[0056] Example 3
[0057] The specific process steps in CN101181561A are as follows:
[0058] The recipe is the same as that of Example 1.
[0059] The preparation method is as follows:
[0060] a. Take the raw materials according to the above formula, wherein Schizonepeta soaked in water for 2 hours, extract the volatile oil for 3 hours, the residue 1 and the residual liquid set aside;
[0061] b. Volatile oil plus 40 times the amount of water, 4 times the amount of β-cyclodextrin, colloid mill inclusion for 10 minutes, filtered, the inclusion complex 70 ℃ drying, set aside;
[0062] c. cicada slough, scutellaria, earthworm, aster, stemona, terminalia chebula plus 1472L, mass concentration of 70% ethanol reflux extraction three times, each for 2 hours, filtered to obtain the residue II and the filtrate, the filtrates were combined, ethanol was recovered until there was no alcohol taste, the liquid was ready;
[0063] d. The residue II and the residue of step a 1 were combined with the residual liquid, added silkworm, added water 1840L, decocted 3 times, each time for 2.5 hours, the combined filtrates were filtered, and the filtrate was concentrated under reduced pressure to a relative density of about 1.3 at 70 ° C, and the resulting solution in step c was combined, vacuum dried, and pulverized into a fine powder;
[0064] e. Add 45kg 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. Dispense and prepare granules.
[0065] The cicada shell cough-relieving granules of Example 1 are compared with the original process CN101181561A. The specific key process parameters are shown in Table 1.
[0066] Table 1: Summary of key parameters of new and old processes
[0067]
[0068] Note: * Granulation process time includes extract drying time and granulation time
[0069] **Amount per bag: 10g
[0070] The total extract, in the preparation method of CN101181561A, refers to the extract obtained by combining the medicinal solution obtained in step d with the medicinal solution obtained in step c. In Example 1, it refers to the extract obtained in step S4.
[0071] The method for determining the content of baicalin is as follows: determined according to high performance liquid chromatography (High Performance Liquid Chromatography, General Chapter 0512 of Part IV of the 2020 edition of the Chinese Pharmacopoeia).
[0072] Chromatographic conditions and system suitability testing were performed using octadecylsilane bonded silica gel as the filler, methanol as mobile phase A, and 0.6% phosphoric acid solution as mobile phase B. Gradient elution was performed according to the specifications in Table 2 below. The column temperature was 25°C, the flow rate was 1 ml / min, and the detection wavelength was 280 nm. The number of theoretical plates calculated based on the baicalin peak should be no less than 2500.
[0073] Table 2: Gradient elution program
[0074]
[0075] Preparation of reference solution: Accurately weigh an appropriate amount of baicalin reference substance and add methanol to make a solution containing 30 μg per 1 ml.
[0076] Preparation of test solution: Take the product, grind it into powder, take about 0.5g, accurately weigh it, put it into a 100ml volumetric flask, slowly add 90ml of 75% methanol, shake while adding, ultrasonically treat (power 500W, frequency 40kHz) for 1 hour, let it cool, add 75% methanol to dilute to the scale, shake well, let it stand, centrifuge (5000rpm, 5 minutes), accurately measure 2ml of the supernatant, put it into a 10ml volumetric flask, add methanol to dilute to the scale, shake well, filter through a 0.45μm microporous filter membrane, and take the filtrate to obtain.
[0077] Determination method: Accurately aspirate 10μl of reference solution and test solution respectively, inject into liquid chromatograph, and determine.
[0078] As can be seen from Table 1: 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 is shorter in the new process, and the content of the heat-sensitive component baicalin is increased by about 40% compared with the old process; 3. The new process reduces the flow of products between different equipment, greatly reduces losses, and the granule yield of the new process is also significantly improved.
[0079] Example 4 Investigation of baicalin transfer rate during one-step granulation
[0080] Add an appropriate amount of hot water to the cicada slough cough relieving granule extract and stir evenly in a mixing barrel. Heat and keep warm to 50-60°C, with a relative density of 1.18. Add 23% of the theoretical amount of dextrin and 0.5% of the theoretical amount of stevioside to a boiling drying granulator. Set the inlet air temperature to 90-110°C and the fan frequency to 20-50 Hz. After heating the material to 55°C, set the peristaltic pump and maintain the speed at 230 rpm to start spray granulation. During the spray granulation process, control the material temperature in the furnace at 60-70°C, the temperature of the cicada slough cough relieving granule extract in the barrel at 50-60°C, the compressed air pressure at 0.35±0.05 MPa, and gradually adjust the peristaltic pump speed to 400 rpm. After the cicada slough cough relieving granule extract is sprayed, control the material temperature below 60-70°C for 15-60 minutes. As the extract was continuously sprayed into the boiling dry granulator, samples were taken to test the baicalin content in the sprayed Chantui Zhike granules (i.e., the amount of baicalin input) and the baicalin content in the material in the furnace (i.e., the amount of baicalin measured). The results are shown in Table 3.
[0081] Table 3 Change trend of baicalin during the new process
[0082]
[0083] The results in Table 3 show that during the granulation process of the new process provided by the present application, the loss of the heat-sensitive component baicalin is relatively small.
[0084] Example 5 Stability Study
[0085] Samples of the granules prepared in Example 1 were placed in a stability test chamber for accelerated and long-term stability testing. Accelerated stability testing conditions were set at (40°C ± 2°C, RH 75% ± 5%), with samples collected at 0, 1, 2, 3, and 6 months. Long-term stability testing conditions were set at (25°C ± 2°C, RH 60% ± 10%), with samples collected at 0, 3, and 6 months. The results are shown in Tables 4 and 5.
[0086] Table 4 Accelerated stability results
[0087]
[0088] Table 5 Long-term stability results
[0089]
[0090] 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 the stability was good.
Claims
1. A method for preparing cicada slough cough-relieving granules, characterized by: The preparation method comprises the following steps: S1. Prepare cicada slough, scutellaria baicalensis, earthworm, aster root, stemona root, terminalia chebula, schizonepeta tenuifolia, and bombyx batryticatus according to the formula ratio; After S2 and Herba Schizonepetae are soaked in water, volatile oil is extracted, and the slag I and residual liquid of Herba Schizonepetae are separately set aside; S3. Take cicada slough, scutellaria baicalensis, earthworm, aster, stemona and terminalia chebula, add ethanol and reflux extract 2 to 4 times, filter, concentrate the filtrate, and combine the concentrates to obtain an alcohol extract and medicinal residue II; combine medicinal residue II with medicinal residue I and the residual liquid of Schizonepeta tenuifolia and Bombyx batryticatus, add water and decoct, filter, concentrate the filtrate under reduced pressure, and combine the concentrates to obtain a water extract; S4. Mixing the alcohol extract and the water extract, and concentrating them to obtain the cicada shell cough-relieving granule extract; S5, add the cicada slough cough relieving granule extract to hot water and stir, heat and keep warm to 40-60 ℃; add dextrin and steviol glycoside to the boiling drying granulator, set the air inlet temperature to 80-120 ℃, the fan frequency to 20-50HZ, heat the material to a temperature of 55 ℃, turn on the peristaltic pump, keep the peristaltic pump speed at 200-600rpm, and spray granulate. During the spray granulation process, the material temperature in the furnace is 50-70 ℃, and the temperature of the cicada slough cough relieving granule extract in the insulation barrel is kept at 50-60 ℃. 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 15-60 minutes to obtain one-step granulation granules; in step S5, the cicada slough cough-relieving granule extract is added to hot water and stirred, heated and kept warm to 40-60°C, and the relative density is 1.16-1.20; in step S5, the amount of dextrin added is 15%-40% of the theoretical total amount; the amount of stevioside added is 0.3%-1.0% of the theoretical total amount.
2. The method for preparing the cicada slough cough-relieving granules according to claim 1, wherein: After step S5, the method further includes 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 slough cough-relieving granules according to claim 2, wherein: The step S2 of obtaining the volatile oil of Schizonepeta tenuifolia also includes adding cyclodextrin and water, grinding and inclusion by a colloid mill, filtering, and drying the inclusion compound to prepare the volatile oil inclusion compound.
4. The method for preparing the cicada slough cough-relieving granules according to claim 3, wherein: After step S6, the preparation method further includes step S7, taking the sieved whole particles and adding the volatile oil inclusion compound.
5. The method for preparing the cicada slough cough-relieving granules according to claim 4, wherein: The rotation speed of the volatile oil inclusion compound is 5 rpm, and the operation time is 10 minutes.
6. The method for preparing the cicada slough cough-relieving granules according to claim 1, wherein: The formula ratio described in step S1 is 400-450 parts by weight of cicada slough, 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 tenuifolia, and 200-250 parts by weight of bombyx batryticatus.
7. The method for preparing the cicada slough 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 of the peristaltic pump is 200 rpm when it is turned on, and the speed of the peristaltic pump is gradually adjusted to 600 rpm.
8. The method for preparing the cicada slough cough-relieving granules according to claim 1, characterized in that: In step S3, the cicada slough, scutellaria baicalensis, earthworm, aster root, stemona root and terminalia chebula are refluxed and extracted with ethanol 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 the silkworm is decocted with water, filtered, and the filtrate is concentrated under reduced pressure to a relative density of 1.15 to 1.
30.
9. The method for preparing the cicada slough 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.
Citation Information
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Chinese medicine as well as preparation method and application thereof
CN101181561A
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