Preparation method of cough and asthma relieving granules

Abstract

The application discloses a preparation method of Xia'e Chuan granules, and belongs to the field of traditional Chinese medicine preparation, and comprises the following steps: S1, closed extraction to obtain a mixed solution: first, pulse ultrasonic treatment of full mountain red in an ethanol aqueous solution for 1 min to 3 min, and then, extraction for 66 h to 78 h at a temperature of 30 DEG C to 40 DEG C with intermittent stirring; S2, filtration and squeezing to obtain an extraction liquid; S3, concentration of the extraction liquid to a clear extract with a relative density of 1.10 to 1.2 at 70 DEG C to 80 DEG C; S4, adjustment of pH to 3.5 to 5.5 to remove astringency; S5, ultrafiltration membrane filtration and concentration to obtain a clear extract with a relative density of 1.10 to 1.2 at 70 DEG C to 80 DEG C, and spray drying of the clear extract to obtain extract powder; and S6, mixing of the extract powder with auxiliary materials, preparation of granules, drying, whole granulation, screening, total mixing, and sub-packaging to obtain the Xia'e Chuan granules. The application shortens the extraction time and improves the stability of the product.

Description

TECHNICAL FIELD

[0001] The present application relates to the preparation of traditional Chinese medicine, in particular to a preparation method of Xiaokechuan granules. BACKGROUND

[0002] Xiaokechuan granules play an important role in the treatment of acute and chronic bronchitis, cold and cough, etc. respiratory diseases. It integrates the functions of "promoting lung, resolving phlegm, relieving cough and asthma" in one, and can effectively relieve the core symptoms such as cough, sputum and asthma. Its importance not only lies in the exact clinical efficacy and extensive mass application basis, but also lies in the fact that it represents the overall treatment advantage of "multiple components and multiple targets" of traditional Chinese medicine in the respiratory field, and provides a relatively small side effect and effective treatment scheme for patients.

[0003] CN115177592A discloses a preparation method and product of Xiaokechuan granules. In the preparation method, the extraction solvent of fuling red is a 40% ethanol aqueous solution, and the extraction temperature is 30~50℃ (compared with the pharmacopoeia, the upper limit temperature is increased by 10℃).

[0004] Although the Xiaokechuan granules disclosed in CN115177592A have good efficacy, there are still some deficiencies: (1) the soaking time is long, which needs 7 days, affecting the production efficiency; (2) the stability is poor.

[0005] The above background technology is for the convenience of understanding the present application, and is not the known technology which has been publicly disclosed to the public before the present application. SUMMARY

[0006] In view of the above defects, the present application provides a preparation method of Xiaokechuan granules, which aims to improve at least one problem mentioned in the background technology.

[0007] The technical scheme is: a preparation method of Xiaokechuan granules, comprising the following steps:

[0008] S1. Obtaining a mixed solution by closed extraction: fuling red is first pulsed ultrasonic in an ethanol aqueous solution for 1 min ~3min, and then extracted for 66 h~78h at a temperature of 30℃~40℃, and in the extraction, intermittent stirring is carried out;

[0009] S2. Filtering the mixed solution obtained in S1 to obtain filtrate and residue, squeezing the residue and filtering the squeezed liquid to obtain a squeezed filtrate, and combining the filtrate and the squeezed filtrate to obtain an extraction liquid;

[0010] S3. Concentrating the extraction liquid to a clear paste with a relative density of 1.10~1.2 at 70℃~80℃;

[0011] S4. Adding a pH adjusting agent to the clear paste to adjust the pH to 3.5~5.5, and adding astringency-removing aqueous solution to remove astringency under stirring;

[0012] S5. Ultrafiltration membrane filtration, concentrating the ultrafiltration filtrate, 70~80 DEG C under the relative density of 1.10~1.2 clear paste, and the clear paste spray drying extract powder;

[0013] S6. The extract powder is mixed with accessories, prepared granules, dried, whole grain, screening, total mixing, and packaging to obtain the Xiaokechuan granules.

[0014] Further, in S1, the pulsed ultrasound is 20 kHz~40 kHz, 90 W / cm²~110 W / cm², 45~55%, the pulse cycle is 2 seconds of work, 3 seconds of stop.

[0015] Further, in S1, the intermittent stirring is once a day in the evening, the stirring time is 8min~12 min, and the stirring speed is 170rpm~190rpm.

[0016] Further, in S1, the amount of ethanol aqueous solution is 4500ml~5500 ml of ethanol aqueous solution per 1000g of full mountain red, and the ethanol aqueous solution is 30%v / v~50%v / v ethanol aqueous solution.

[0017] Further, in S1, the size of the full mountain red is 2mm~5mm.

[0018] Further, in S4, the pH regulator is lactic acid, and the astringent water solution is a chitosan aqueous solution.

[0019] Further, the chitosan aqueous solution is 1.5 wt%~2.5 wt% chitosan aqueous solution, and the amount of chitosan aqueous solution is 2.8~3.3 times the amount of the clear paste obtained in S3.

[0020] Further, in S4, the pH is 4.5.

[0021] Compared with the prior art, the beneficial effects of the present application are:

[0022] The present application shortens the extraction time and improves the stability of the product by the combination of short pulse + extraction + intermittent stirring, and the product stability is better. The present application also selects the full mountain red material, and uses 2mm~5mm full mountain red, which further improves the stability of the product while maintaining the efficacy of the newly prepared Xiaokechuan granules.

[0023] The present application also combines chitosan + lactic acid + specific pH range, which basically eliminates the astringent taste of the product, and the palatability is better. DETAILED DESCRIPTION

[0024] As used herein the terms "about" and "substantially" mean approximately or nearly, as in "about 90%," "substantially similar," or "substantially identical."

[0025] "Made by" is synonymous with "comprising." The terms "comprising," "including," "having," "with," or any other variation thereof, are intended to cover a non-exclusive inclusion. For example, a composition, a step, a method, an article, or an apparatus that comprises a list of elements is not necessarily limited to only those elements but can include other elements not expressly listed or inherent to such composition, step, method, article, or apparatus.

[0026] When equivalent, concentration, or other values or parameters are expressed in ranges, preferred ranges, or a series of upper preferred values and lower preferred values, it is to be understood that all ranges formed by any pair of any upper or lower preferred value, whether or not the range is expressly disclosed, are specifically disclosed. For example, when a range "1-5" is disclosed, the described range should be interpreted to include the ranges "1-4," "1-3," "1-2," "1-2 and 4-5," "1-3 and 5," etc. When numerical ranges are described herein, unless the context clearly dictates otherwise, the range is intended to include all integers and fractions within the range.

[0027] The technical solutions of the present application will be clearly and completely described below in combination with the embodiments. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative work are within the scope of protection of the present application.

[0028] Those skilled in the art will understand that the following examples are used to illustrate the present application and should not be considered limiting the scope of the present application. The specific conditions are not specified in the examples, and the conventional conditions or the conditions recommended by the manufacturer are used. The reagents or instruments used are not specified by the manufacturer, and are conventional products that can be purchased on the market.

[0029] In these examples, the parts and percentages are by mass unless otherwise indicated.

[0030] "Mass parts" refers to a basic unit of measurement representing the mass ratio relationship of multiple components. One part can represent any unit mass, such as 1 g, 2.689 g, etc. If we say that the mass parts of component A is a parts and the mass parts of component B is b parts, it means that the mass ratio of component A to component B is a:b. Alternatively, it means that the mass of component A is aK and the mass of component B is bK (K is an arbitrary number representing a multiple factor). It should not be misunderstood that unlike the mass parts, the sum of the mass parts of all components is not limited to 100 parts.

[0031] "And / or" is used to indicate that one or both of the described situations may occur, for example, A and / or B includes (A and B) and (A or B).

[0032] A method for preparing cough and asthma granules includes the following steps:

[0033] S1. Closed extraction to obtain a mixture: Rhododendron molle was first subjected to pulsed sonication in an ethanol-water solution for 1 min to 3 min, and then extracted for 66 h to 78 h at a temperature of 30℃ to 40℃, with intermittent stirring during the extraction process;

[0034] S2. Filter the mixture obtained in S1 to obtain filtrate and filter residue. Press the filter residue and filter the extract to obtain pressed filtrate. Combine the filtrate and pressed filtrate to obtain extract.

[0035] S3. Concentrate the extract to a clear paste with a relative density of 1.10 to 1.2 at 70℃ to 80℃;

[0036] S4. Add a pH adjuster to the ointment to adjust the pH to 3.5~5.5, and add the astringent solution while stirring to remove astringency;

[0037] S5. Ultrafiltration membrane filtration, concentrating the ultrafiltration filtrate to obtain a clear extract with a relative density of 1.10~1.2 at 70℃~80℃, and spray drying the clear extract to obtain an extract powder;

[0038] S6. Mix the extract powder with excipients, prepare granules, dry, granulate, sieve, mix, and package to obtain cough and asthma granules.

[0039] Preferably, in S1, the pulsed ultrasound has a frequency of 20kHz~40kHz, a power of 90 W / cm²~110 W / cm², an amplitude of 45~55%, and a pulse period of 2 seconds on and 3 seconds off.

[0040] As a preferred embodiment, in S1, the intermittent stirring is started once on the evening of the first day, with a stirring time of 8 to 12 minutes. From the second day onwards, the stirring is started once each in the morning and evening, with a stirring time of 8 to 12 minutes. The stirring speed for each stirring is 170 to 190 rpm.

[0041] Preferably, in S1, the amount of ethanol-water solution is 4500ml~5500ml of ethanol-water solution per 1000g of *Rhododendron molle*, and the ethanol-water solution is 30%v / v~50%v / v ethanol-water solution.

[0042] As a preferred option, in S1, the size of the rhododendron is 2mm~5mm.

[0043] As a preference, in S4, the pH regulator is lactic acid, and the astringent water solution is a chitosan water solution.

[0044] As a preference, the chitosan water solution is a 1.5 wt%~2.5 wt% chitosan water solution, and the amount of the chitosan water solution is 2.8~3.3 times the amount of the clear extract obtained in S3.

[0045] As a preference, in S4, the pH is 4.5.

[0046] In the following examples and comparative examples, the following methods are used to prepare Hongshan Hong I, Hongshan Hong II and Hongshan Hong III (the methods are conventional methods for preparing raw materials in the field of traditional Chinese medicine)

[0047] Hongshan Hong I preparation: After washing, selecting and drying Hongshan Hong purchased from the market, the Hongshan Hong is ground and sieved to obtain particles (or primary powder) of about 1 mm.

[0048] Hongshan Hong II preparation: After washing, selecting and drying Hongshan Hong purchased from the market, the Hongshan Hong is ground and sieved to obtain particles of about 2 mm~5 mm.

[0049] Hongshan Hong III preparation: After washing, selecting and drying Hongshan Hong purchased from the market, the Hongshan Hong is cut into segments to obtain segments of about 10 mm.

[0050] Example 1

[0051] A preparation method of a cough and asthma relieving granule, comprising the following steps:

[0052] S1. Extracting to obtain a mixed solution, comprising the following steps:

[0053] S11. Put 1000g of Hongshan Hong II into an extraction tank, add 5000ml of 40% v / v ethanol water solution, and then close the extraction tank.

[0054] S12. Turn on the ultrasonic wave, the time is 2min, the ultrasonic wave mode is pulse, the frequency is 30kHz, the power is 100 W / cm², the amplitude is 50%, the pulse cycle is 2 seconds of work and 3 seconds of stop, and then turn off the ultrasonic wave.

[0055] S13. Extracting, the time is 72h, during the extracting, stirring is started once in the evening of the first day, the stirring time is 10min, stirring is started once in the morning and in the evening of the second day and the third day respectively, the stirring time is 10min, and the stirring speed of each stirring is 180rpm.

[0056] In S12 and S13, the temperature of the liquid in the extraction tank is controlled at about 35°C.

[0057] S2. Filtering the mixed solution obtained in S1 to obtain a filtrate and a residue, squeezing the residue and filtering the squeezed liquid to obtain a squeezed filtrate, and combining the filtrate and the squeezed filtrate to obtain an extract.

[0058] S3. Concentrating the extract to a clear paste with a relative density of 1.15 at 75°C.

[0059] S4. Adding lactic acid to the clear paste to adjust the pH to 4.5, adding a chitosan aqueous solution (with a concentration of 2 wt%, the temperature of the chitosan aqueous solution being 70°C, and the amount of the chitosan aqueous solution being 3 times the amount of the clear paste) while stirring, and starting cooling to 40°C.

[0060] S5. Filtering with an ultrafiltration membrane to obtain an ultrafiltration filtrate, concentrating the ultrafiltration filtrate to a clear paste with a relative density of 1.15 at 75°C, and spray drying the clear paste to obtain a powder extract.

[0061] S6. Mixing and adjusting half of the powder extract of S5 with dextrin, preparing granules, drying, sizing, screening, total mixing, and packaging to obtain the Xiaokechuan granules.

[0062] In S6, the total amount of the powder extract and dextrin is 500 g, and the amount of dextrin added is adjusted according to the amount of the powder extract.

[0063] Example 2

[0064] Compared with Example 1, the difference is that in S11, the Hongshan Hong No. 3 is replaced by Hongshan Hong No. 2.

[0065] Example 3

[0066] Compared with Example 1, the difference is that in S11, the Hongshan Hong No. 1 is replaced by Hongshan Hong No. 2.

[0067] Example 4

[0068] A preparation method of Xiaokechuan granules, comprising the following steps:

[0069] S1. Extracting to obtain a mixed solution, comprising the following steps:

[0070] S11. Placing 1000 g of Hongshan Hong No. 2 into an extraction tank, adding 5000 ml of a 40% v / v ethanol aqueous solution, and then closing the extraction tank.

[0071] S12. Starting ultrasonic waves, with a time of 2 min, an ultrasonic wave mode of pulse, a frequency of 30 kHz, a power of 100 W / cm², an amplitude of 50%, a pulse cycle of working for 2 seconds and stopping for 3 seconds, and then stopping the ultrasonic waves.

[0072] S13. The extraction time is 72 h. The stirring is started once at the end of the first day, and the stirring time is 10 min. The stirring is started once at the morning and evening of the second and third days, and the stirring time is 10 min. The stirring speed is 180 rpm.

[0073] In S12 and S13, the temperature of the liquid in the extraction tank is controlled at about 35°C.

[0074] S2. The filtrate and residue are obtained by filtering the mixed solution obtained in S1. The residue is squeezed and the squeezed filtrate is obtained by filtering the squeezed liquid. The filtrate and the squeezed filtrate are combined to obtain the extraction liquid.

[0075] S3. The extraction liquid is concentrated to a clear extract with a relative density of 1.15 at 75°C.

[0076] S4. Lactic acid is added to the clear extract to adjust the pH to 5.5. The chitosan aqueous solution (the concentration is 2 wt%, the temperature of the chitosan aqueous solution is 70°C, and the amount of the chitosan aqueous solution is 3 times the amount of the clear extract) is added while stirring. The cooling is started, and the temperature is cooled to 40°C.

[0077] S5. The ultrafiltration membrane filtration is performed to obtain the ultrafiltration filtrate. The ultrafiltration filtrate is concentrated to a clear extract with a relative density of 1.15 at 75°C. The clear extract is spray dried to obtain the extract powder.

[0078] S6. The extract powder of S5 is mixed with dextrin to adjust the particle size, dried, granulated, sieved, mixed, and packaged to obtain the Xiaokechuan granules.

[0079] In S6, the total amount of the extract powder and dextrin is 1000 g. The amount of dextrin is adjusted according to the amount of the extract powder.

[0080] Example 5

[0081] Compared with Example 4, the difference is that in S4, the lactic acid is adjusted to pH 3.5.

[0082] Example 6

[0083] Compared with Example 4, the difference is that in S4, the lactic acid is replaced by citric acid, and the citric acid is adjusted to pH 4.5.

[0084] Example 7

[0085] Compared with Example 4, the difference is that in S4, the lactic acid is adjusted to pH 4.5, and the chitosan is replaced by gelatin.

[0086] Example 8

[0087] Compared with Example 4, the difference is that in S4, the lactic acid is replaced by citric acid, the citric acid is adjusted to pH 4.5, and the chitosan is replaced by gelatin.

[0088] Comparative Example 1

[0089] A preparation method of Xiaoechuan granules, comprising the following steps:

[0090] S1. Extracting to obtain a mixed solution, comprising the following steps:

[0091] S11. Put 1000 g of Rhododendron simsii into an extraction tank, add 5000 ml of 40% v / v ethanol aqueous solution, and then close the extraction tank.

[0092] S12. Turn on the ultrasonic wave, the time is 35 min, the ultrasonic wave mode is pulse, the frequency is 30 kHz, the power is 100 W / cm2, the amplitude is 50%, and the pulse cycle is working for 2 seconds and stopping for 3 seconds.

[0093] In S12, the temperature of the liquid in the extraction tank is controlled at about 35°C.

[0094] S2. Filter the mixed solution obtained in S1 to obtain filtrate and residue, squeeze the residue, filter the squeezed liquid to obtain a squeezed filtrate, and combine the filtrate and the squeezed filtrate to obtain an extract.

[0095] S3. Concentrate the extract to a clear paste with a relative density of 1.15 at 75°C.

[0096] S4. Add lactic acid to the clear paste to adjust the pH to 4.5, add a chitosan aqueous solution (concentration of 2 wt%, temperature of the chitosan aqueous solution is 70°C, and the amount of the chitosan aqueous solution is 3 times the amount of the clear paste) while stirring, and open the cooling to cool to 40°C.

[0097] S5. Filter with an ultrafiltration membrane to obtain an ultrafiltration filtrate, concentrate the ultrafiltration filtrate to a clear paste with a relative density of 1.15 at 75°C, and spray dry the clear paste to obtain an extract powder.

[0098] S6. Mix half of the extract powder of S5 with dextrin, adjust, prepare granules, dry, size, screen, mix, and package to obtain Xiaoechuan granules.

[0099] In S6, the total amount of the extract powder and dextrin is 500 g, and the amount of dextrin added is adjusted according to the amount of the extract powder.

[0100] Comparative Example 2

[0101] Compared with Comparative Example 1, the difference is that in S12, the ultrasonic wave mode is continuous instead of pulse.

[0102] Comparative Example 3

[0103] A preparation method of Xiaoechuan granules, comprising the following steps:

[0104] S1. Extraction to obtain a mixture solution, comprising the following steps:

[0105] S11. Put 1000g of Rhododendron simsii leaves into an extraction tank, add 5000ml of 40% v / v ethanol aqueous solution, and then seal the extraction tank.

[0106] S13. Stirring extraction, the stirring time is 72h, and the stirring speed is 180rpm.

[0107] In S13, the temperature of the liquid in the extraction tank is controlled at about 35℃.

[0108] S2. Filter the mixture solution obtained in S1 to obtain a filtrate and a residue, squeeze the residue, filter the squeezed liquid to obtain a squeezed filtrate, and combine the filtrate and the squeezed filtrate to obtain an extraction solution.

[0109] S3. Concentrate the extraction solution to a clear extract with a relative density of 1.15 at 75℃.

[0110] S4. Add lactic acid to the clear extract to adjust the pH to 4.5, add a chitosan aqueous solution (with a concentration of 2wt%, the temperature of the chitosan aqueous solution is 70℃, and the amount of the chitosan aqueous solution is 3 times the amount of the clear extract) while stirring, and start cooling to 40℃.

[0111] S5. Ultrafiltration membrane filtration to obtain an ultrafiltration filtrate, concentrate the ultrafiltration filtrate to a clear extract with a relative density of 1.15 at 75℃, and spray dry the clear extract to obtain a extract powder.

[0112] S6. Mix half of the extract powder of S5 with dextrin, adjust, prepare granules, dry, size, screen, mix, and package to obtain the Xiaokechuan granules.

[0113] In S6, the total amount of the extract powder and dextrin is 500g, and the amount of dextrin added is adjusted according to the amount of the extract powder.

[0114] Comparative Example 4

[0115] A preparation method of Xiaokechuan granules, comprising the following steps:

[0116] S1. Extraction to obtain a mixture solution, comprising the following steps:

[0117] S11. Put 1000g of Rhododendron simsii leaves into an extraction tank, add 5000ml of 40% v / v ethanol aqueous solution, and then seal the extraction tank.

[0118] S13. Extraction, the extraction time is 168h, in the extraction, stirring is started once a day in the morning and in the evening respectively, the stirring time is 10min, and the stirring speed is 180rpm.

[0119] In S13, the temperature of the liquid in the extraction tank is controlled at about 35°C.

[0120] S2. The mixture obtained in S1 is filtered to obtain a filtrate and a residue, the residue is squeezed and the squeezed liquid is filtered to obtain a squeezed filtrate, and the filtrate and the squeezed filtrate are combined to obtain an extract.

[0121] S3. The extract is concentrated to a clear paste with a relative density of 1.15 at 75°C.

[0122] S4. Lactic acid is added to the clear paste to adjust the pH to 4.5, and a chitosan aqueous solution (concentration of 2 wt%, temperature of the chitosan aqueous solution is 70°C, and the amount of the chitosan aqueous solution is 3 times the amount of the clear paste) is added while stirring, and cooling is started and the temperature is cooled to 40°C.

[0123] S5. The extract is filtered by an ultrafiltration membrane to obtain an ultrafiltration filtrate, the ultrafiltration filtrate is concentrated to a clear paste with a relative density of 1.15 at 75°C, and the clear paste is spray-dried to obtain a extract powder.

[0124] S6. Half of the extract powder of S5 is mixed with dextrin to adjust the particle size, dried, granulated, sieved, mixed, and packaged to obtain the Xiaohetan granules.

[0125] In S6, the total amount of the extract powder and dextrin is 500 g, and the amount of dextrin added is adjusted according to the amount of the extract powder.

[0126] The Xiaohetan granules of Examples 1-3 and Comparative Examples 1-4 are subjected to total flavonoid detection and rhodotoxin detection, and the results are shown in Table 1 below.

[0127] Table 1: Results of total flavonoid (calculated as rutin) and rhodotoxin detection

[0128]

[0129] In Table 1, the values are the contents in one bag of Xiaohetan granules (weight of 2 g).

[0130] The extract powders of Examples 1-3 and Comparative Examples 1-4 are subjected to accelerated stability tests (0 months, 3 months, and 12 months, respectively), and the test conditions are: temperature of 40°C ± 2°C and relative humidity of 75% ± 5%. The extract powders after the accelerated tests are subjected to solubility detection, and the solubility solvent is 40% v / v ethanol aqueous solution, the amount of the ethanol aqueous solution is 200 ml, the amount of the solubility sample is 2 g, and the detection equipment is a turbidimeter. The results are shown in Table 2 below.

[0131] Table 2: Results of solubility detection

[0132] In Table 2, the turbidity change value is based on the turbidity value of the sample at 0 months, and the turbidity value of the sample at 3 months / 9 months minus the turbidity value of the sample at 0 months.

[0133] From Table 1, it can be seen that, although the extraction time is shortened, the target component content of Example 1-Example 3 is not much different from that of Comparative Example 4, and the extraction effect of Comparative Example 1-Comparative Example 3 is better than that of Example 1. However, from Table 2, it can be seen that, although the turbidity of Example 1-Example 3 increases after the 3-month and 12-month accelerated tests, the change is not large, and the change of Example 2 is the smallest, and the turbidity of Comparative Example 1-Comparative Example 4 changes greatly, and the change value of Comparative Example 1 is as high as 12.55 NTU after 3 months and 17.55 NTU after 12 months. In combination of Table 1 and Table 2, Example 1-Example 3 not only shortens the extraction time while maintaining the efficacy of the newly prepared Xiaogan Granules, but also improves the stability of the product, so that the shelf life of the product is better.

[0134] The Xiaogan Granules of Example 1, Example 4-Example 8 were taken for astringency comparison, and the results are shown in Table 3.

[0135] The astringency evaluators were selected from personnel who had never contacted traditional Chinese medicinal materials for extraction and production, and the evaluators were personnel sensitive to astringency. At least 6 evaluators were selected.

[0136] During the evaluation, before each sample was evaluated, the evaluators rinsed their mouths with normal temperature purified water, and then took about 3-5 mL of the sample liquid into the mouth with a special dropper or a small spoon, and through gentle sipping, the liquid was evenly distributed in the front part of the oral cavity, and swallowing was avoided. The liquid was allowed to contact the entire oral cavity for about 5-8 seconds, and the contraction feeling of the tongue, the upper palate and the inner side of the cheek was mainly felt.

[0137] The judgment rule was that the astringency of the sample liquid of Example 6 was taken as the benchmark and marked as 1, the astringency of Example 6 was marked as 1+, and the astringency of Example 6 was marked as 1-. The more +, the heavier the astringency, and the more -, the lighter the astringency.

[0138] Table 3 Astringency detection results

[0139]

[0140] From Table 3, it can be seen that the astringency degrees of Example 6-8 are basically the same, and the evaluators cannot distinguish Example 7 and Example 8 from Example 6, the astringency of Example 4 and Example 5 is 1- lighter than that of Example 6, and the astringency of Example 1 is 1- - lighter than that of Example 6.

[0141] The preferred embodiments of the application have been described above, but the application is not limited to the above. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the application shall be included in the protection scope of the application.

Claims

1. A method of preparing a cough and asthma relieving granule, characterized by, The method comprises the following steps: S1. Closed extraction to obtain a mixed solution: first pulse ultrasonic treatment of the Radix Isatidis in an ethanol aqueous solution for 1 min ~ 3 min, and then extraction for 66 h ~ 78 h at a temperature of 30 ℃ ~ 40 ℃, with intermittent stirring during the extraction; S2. Filtering the mixed solution obtained in S1 to obtain a filtrate and a residue, squeezing the residue, and filtering the squeezed liquid to obtain a squeezed filtrate, and combining the filtrate and the squeezed filtrate to obtain an extract; S3. Concentrating the extract to a clear extract with a relative density of 1.10 ~ 1.2 at 70 ℃ ~ 80 ℃; S4. Adding a pH adjuster to the clear extract to adjust the pH to 3.5 ~ 5.5, and adding an astringency-removing aqueous solution to remove astringency under stirring; S5. Ultrafiltration membrane filtration, concentrating the ultrafiltration filtrate to a clear extract with a relative density of 1.10 ~ 1.2 at 70 ℃ ~ 80 ℃, and spray drying the clear extract to obtain an extract powder; S6. Mixing and adjusting the extract powder with excipients, preparing granules, drying, sizing, screening, total mixing, and packaging to obtain the Cough and Asthma Relieving Granules; In S1, the pulse ultrasonic treatment has a frequency of 20 kHz ~ 40 kHz, a power of 90 W / cm² ~ 110 W / cm², and an amplitude of 45 ~ 55%, with a pulse cycle of 2 seconds of work and 3 seconds of stop; In S4, the pH adjuster is lactic acid, and the astringency-removing aqueous solution is a chitosan aqueous solution; The chitosan aqueous solution is a chitosan aqueous solution with a concentration of 1.5 wt% ~ 2.5 wt%, and the amount of the chitosan aqueous solution is 2.8 ~ 3.3 times the amount of the clear extract obtained in S3.

2. The method of preparing the Xiaona granules according to claim 1, characterized in that, In S1, the intermittent stirring is once in the evening on the first day, with a stirring time of 8 min ~ 12 min, and once in the morning and once in the evening on each of the following days, with a stirring time of 8 min ~ 12 min, and the stirring speed of each stirring is 170 rpm ~ 190 rpm.

3. The method of claim 1, wherein the preparation of the Xiaona granules is characterized by, In S1, the amount of the ethanol aqueous solution is 4500 ml ~ 5500 ml per 1000 g of the Radix Isatidis, and the ethanol aqueous solution is an ethanol aqueous solution with a concentration of 30% v / v ~ 50% v / v.

4. The preparation method of the Xiaona granules according to claim 1, characterized in that, In S1, the size of the Radix Isatidis is 2 mm ~ 5 mm.

5. The preparation method of the cough and asthma relieving granules according to claim 1, characterized by, In S4, the pH is 4.5.

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