Shenhuning granules as well as preparation method and identification method thereof

Abstract

The invention relates to the technical field of identification of traditional Chinese medicine preparations, and particularly discloses a preparation method of sphenhuning granules, which comprises the following steps: taking poria cocos and hawthorn, adding water, decocting twice, combining decoction, filtering, taking filtrate, concentrating the filtrate, adding ethanol until the ethanol content is 50-60%, standing to precipitate, taking supernate, and recovering the ethanol to obtain extract; adding cane sugar into the extract, uniformly stirring, then adding soybean protein isolate, stirring, then adding silicon dioxide, and continuously stirring to obtain a mixture; and granulating the mixture, and drying to obtain the Shenhuning granules. The soybean protein isolate and the silicon dioxide are sequentially added into the extract, so that the viscosity of the materials can be integrally reduced, and the wall sticking phenomenon in the granulation process is reduced; after drying, a film or a gel network with certain density can be formed, permeation of moisture in the environment can be blocked to a certain extent, and the prepared particles are relatively uniform in particle size and high in particle quality; meanwhile, the moisture resistance of the granules is improved, and the shelf life of the granules is prolonged.

Description

Technical Field

[0001] This invention relates to the field of traditional Chinese medicine preparation technology, and in particular to a spleen-soothing granule and its preparation and identification methods. Background Technology

[0002] Pishu Ning granules are mainly composed of hawthorn and poria cocos, and have the effects of strengthening the spleen and promoting digestion, calming the mind and soothing the nerves. They are primarily used for spleen deficiency with dampness retention, loss of appetite, irritability, and insomnia. This is a pharmaceutical preparation that the applicant has already put into production. Currently, the preparation method for Pishu Ning granules is as follows: Poria cocos and hawthorn are decocted to prepare a thick paste, then an appropriate amount of sucrose powder is added, mixed well, and granulated. Currently, there is a problem with Pishu Ning granules during the preparation process: if the material adhering to the machine wall cannot be removed in time, it will be charred or deteriorated. At the same time, the granules have uneven particle size distribution, poor forming rate, irregular shape, and are prone to moisture absorption, which will shorten the product's shelf life and affect product quality.

[0003] Furthermore, the standard for the use of Pishu Ning granules is the national drug standard. In the national drug standard, identification is based on a chemical colorimetric reaction, which, compared to the complex systems of multiple components in traditional Chinese medicines like hawthorn and poria, lacks strong specificity.

[0004] Hawthorn is the dried, ripe fruit of the hawthorn plant (Crataegus pinnatifida), belonging to the Rosaceae family. Hawthorn products have long been widely used clinically, possessing properties such as inhibiting thyroid peroxidase, anti-cancer effects, lowering blood pressure, anti-inflammation, promoting blood circulation, reducing blood lipids, and relieving spasms. Hawthorn contains various flavonoids and triterpenoids, saponins, vitamin C, digestive enzymes, chlorogenic acid, citric acid, and other fruit acids, as well as choline and tannic acid. Its organic acids are considered effective components for promoting digestion and strengthening the spleen. Thin-layer chromatography experiments were conducted on hawthorn using organic acids as the determining indicator. The method for identifying hawthorn in the Chinese Pharmacopoeia is as follows: Take 1g of the powder, add 4ml of ethyl acetate, sonicate for 15 minutes, filter, and use the filtrate as the test solution. Separately, prepare a reference solution by dissolving a fruit acid standard in methanol to a concentration of 1mg per ml. According to the thin-layer chromatography method (General Rule 0502), apply 4 μl of each of the two solutions to the same silica gel G thin-layer plate. Develop the plate using toluene-ethyl acetate-formic acid (20:4:0.5) as the developing solvent. Remove the plate, air dry, spray with sulfuric acid ethanol solution (3→10), and heat at 80℃ until the spots are clearly visible. In the chromatogram of the test sample, the same purplish-red spots appear at the corresponding positions as in the chromatogram of the reference sample; under ultraviolet light (365nm), the same orange-yellow fluorescent spots appear. Pishu Ning granules are prepared by water extraction, while the pharmacopoeia uses ethyl acetate extraction. The components extracted using different solvents are not entirely the same, and the hawthorn identification method in the pharmacopoeia is not applicable to the identification of hawthorn in Pishu Ning granules. Summary of the Invention

[0005] To address the above shortcomings, this invention provides a method for preparing Spleen-Soothing Granules, reducing the problem of granules sticking to the wall during preparation and improving the moisture-proof performance of the resulting granules. The specific technical solution is as follows: A method for preparing Pishuning granules includes the following steps: S1. Take Poria cocos and hawthorn, decoct them twice with water, combine the decoctions, filter and take the filtrate, concentrate the filtrate, add ethanol to the alcohol content to 50-60%, let it stand to precipitate, take the supernatant to recover the ethanol and make an extract. S2. Add sucrose and soy protein isolate to the extract obtained in step S1, stir and disperse, heat to 40~50℃ and stir and disperse for 30~45 minutes, then add silica and continue stirring for 10~30 minutes to obtain a mixture; S3. The mixture is wet-granulated and dried to obtain Pishuning granules.

[0006] In the preparation method of the Pishuning granules of the present invention, soy protein isolate is first added to the extract. Soy protein isolate has certain adsorption and gelling properties, which can adsorb and fix the viscous components (such as polysaccharides and organic acids) in the Chinese medicine extract into the structure. At the same time, it can also adsorb moisture, thereby reducing the overall viscosity of the material and reducing the wall sticking phenomenon during the granulation process. On the other hand, after drying, it can form a film or gel network with a certain density, which can block the penetration of moisture in the environment to a certain extent. Silica has a lubricating and flow-aiding effect. Adding silica can further reduce adhesion and wall sticking, and the prepared granules have a relatively uniform particle size, improving the quality of Pishuning granules. The present invention can also improve the moisture resistance of the granules and extend their shelf life.

[0007] Preferably, in the above-mentioned method for preparing spleen-soothing granules, in step S1, the filtrate is concentrated to a relative density of 1.15~1.2.

[0008] Preferably, in the above-mentioned method for preparing Pishuning granules, in step S2, the amount of soy protein isolate is 1-5% of the extract mass, and the amount of silica is 2-6% of the extract mass.

[0009] Preferably, in the above-mentioned method for preparing spleen-soothing granules, in step S2, the stirring speed is 300~400 rpm.

[0010] Preferably, in the above-mentioned method for preparing Pishuning granules, the drying temperature in step S3 is 60~75℃.

[0011] On the other hand, the present invention also provides a spleen-soothing granule, which is prepared by the above-described preparation method.

[0012] On the other hand, the present invention also provides a method for identifying the above-mentioned Pishuning granules, comprising the following steps: (1) Preparation of test solution: Take the fine powder of the spleen-soothing granules to be tested, put it into ethanol and sonicate it to prepare the test solution; (2) Preparation of control medicinal material solution: Take hawthorn control medicinal material, add water, heat and reflux, filter, concentrate the filtrate, add ethanol and sonicate to prepare control medicinal material solution; (3) Preparation of negative solution: Take hawthorn negative sample powder, add ethanol and sonicate to prepare negative solution; (4) Thin-layer chromatography identification: Take the reference herb solution, the test solution, and the negative solution, and spot them separately on the same silica gel G thin-layer plate. Use chloroform-butanone-methanol-formic acid volume ratio of 3~7:3~7:1~3:0.5~2 as the developing solvent. Remove the plate, air dry it, and bake it at 105~110℃ for 1~2 hours. Spray it with bromophenol blue ethanol solution and develop the color under sunlight. In the chromatogram of the test sample, spots appear at the same positions as in the chromatogram of the reference sample.

[0013] Prior to this, in the above-mentioned identification method for Pishuning granules, step (1) specifically involves: taking fine powder of Pishuning granules, adding ethanol, with the ratio of fine powder of Pishuning granules to ethanol being 1g:2~4ml, sonicating for 20~60min, filtering, evaporating the filtrate to dryness, adding ethanol to dissolve it, and using it as the test solution. The extraction process of this preparation (Pishuning granules) is water extraction and alcohol precipitation. The water-soluble organic acids in hawthorn mainly include water-soluble fatty acids such as malic acid, citric acid, succinic acid, and tartaric acid. These fatty acids can dissolve or have a certain degree of solubility in ethanol. Therefore, using ethanol as a solvent can not only extract these organic acids but also avoid or reduce the influence of sucrose on the experiment.

[0014] Prior to this, in the above-mentioned identification method of Pishu Ning granules, step (1) is as follows: take hawthorn reference material, add water and heat under reflux for 1-2 hours, the ratio of hawthorn reference material to water is 0.2g: 50-150ml, filter, concentrate the filtrate to near dryness, add ethanol, sonicate for 20-60 minutes, filter, evaporate the filtrate to dryness, add ethanol to dissolve, and use as reference material solution.

[0015] Preferred, in the above-mentioned identification method of Pishu Ning granules, step (3) specifically involves: taking hawthorn negative sample fine powder, adding ethanol, the ratio of hawthorn negative sample fine powder to ethanol being 1g:2~4ml, sonicating for 20~60min; filtering, evaporating the filtrate to dryness, adding ethanol to dissolve, and preparing a negative solution.

[0016] Preferably, in the above-mentioned method for identifying Pishuning granules, the volume ratio of chloroform-butanone-methanol-formic acid is 4~6:4~6:1.5~2.5:0.8~1.5.

[0017] Preferably, in the above-mentioned method for identifying Pishuning granules, the volume ratio of chloroform-butanone-methanol-formic acid is 5:5:2:1.

[0018] Preferredly, in the above-mentioned identification method for Pishu Ning granules, step (4) specifically involves: taking 10 μL each of the reference herb solution, the test sample solution, and the negative solution, and spotting them separately onto the same silica gel G thin-layer plate. Develop the plate using a chloroform-butanone-methanol-formic acid volume ratio of 5:5:2:1 as the developing solvent. Remove the plate, air dry it, bake it at 105°C for 2 hours, and spray it with 0.1% bromophenol blue ethanol solution. Because the colorimetric reagent used (0.1% bromophenol blue ethanol solution) is an acid-base indicator, the presence of formic acid in the developing solvent will seriously affect the observation of the test results. Since the boiling point of formic acid is 100.5°C, baking it at 105°C for 2 hours is necessary to remove the formic acid.

[0019] Compared with the prior art, the beneficial effects of the present invention are: 1. In the preparation method of the spleen-soothing granules of the present invention, soybean protein isolate and silica are added to the extract in sequence, which can reduce the viscosity of the material as a whole and reduce the phenomenon of sticking to the wall during the granulation process; after drying, a thin film or gel network with a certain density can be formed, which can block the penetration of moisture in the environment to a certain extent; the addition of silica can further reduce adhesion and reduce wall sticking, and the prepared granules have relatively uniform particle size and high granule quality; at the same time, it can improve the moisture resistance of the granules and extend the shelf life of the granules.

[0020] 2. The identification method of the present invention for Pishu Ning granules is used for identification. The test solution shows spots of the same color at the corresponding positions of the chromatogram of the reference medicinal material, with good separation. The negative solution chromatogram does not show spots, and the negative sample does not interfere. The operation is simple and has good specificity. It can be used as a reference for the control of hawthorn index of Pishu Ning granules, which is beneficial to the quality control and testing of Pishu Ning granules and improves reliability. Attached Figure Description

[0021] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0022] Figure 1 Photograph of the spleen-soothing granules prepared in Example 1 of this invention; Figure 2 Photograph of the spleen-soothing granules prepared in Comparative Example 1 of this invention; Figure 3This is a thin-layer chromatography chromatogram of Example 4 of the present invention, wherein 1 is hawthorn reference material, 2 is the test sample, and 3 is the negative control. Detailed Implementation

[0023] The specific embodiments of the present invention are described in detail below, but it should be understood that the scope of protection of the present invention is not limited to the specific embodiments. Unless otherwise defined, all technical terms used below have the same meaning as commonly understood by those skilled in the art. The technical terms used herein are for the purpose of describing specific embodiments only and are not intended to limit the scope of protection of the present invention. Unless otherwise specifically stated, all raw materials, reagents, instruments, and equipment used in the present invention are commercially available or can be prepared by existing methods.

[0024] Sources of raw materials and consumables: Hawthorn reference material: Source: National Institutes for Food and Drug Control, Batch: 201206.

[0025] Spleen-Soothing Granules: Homemade.

[0026] Thin-layer plates: self-made, glass plates with dimensions of 20cm*10cm, silica gel G produced by Qingdao Ocean Chemical Plant, prepared according to the method and conditions for self-made thin-layer plates in Part IV, 0502 of the 2020 edition of the Chinese Pharmacopoeia.

[0027] Example 1 A method for preparing Pishuning granules includes the following steps: S1. Take Poria cocos and hawthorn and add 8 times the amount of water to decoct twice. The weight ratio of hawthorn to Poria cocos is 2:1. The first decoction is 2 hours and the second decoction is 1 hour. Combine the decoctions, filter and collect the filtrate. Concentrate the filtrate to a relative density of 1.2 (80℃), cool, add ethanol to a concentration of 60%, let stand to allow precipitation, collect the supernatant and recover the ethanol to obtain the extract. S2. Add 6 times the weight of sucrose to the extract obtained in step S1 and stir until homogeneous. Add 3% soy protein isolate and stir at 300 rpm for 15 min. Heat to 45°C and stir to disperse for 30 min. Then add 4% silica by weight of the extract and continue stirring for 15 min to obtain the mixture. S3. The mixture is wet-granulated and dried at 70℃ to obtain Pishuning granules.

[0028] The spleen-soothing granules prepared in this embodiment are shown below. Figure 1 The particles are uniform in size and color.

[0029] Example 2 A method for preparing Pishuning granules includes the following steps: S1. Take Poria cocos and hawthorn, add 8 times the amount of water and decoct twice. The weight ratio of hawthorn to Poria cocos is 2:1. The first decoction is 2 hours and the second decoction is 1 hour. Combine the decoctions, filter and collect the filtrate. Concentrate the filtrate to a relative density of 1.2 (80℃). Add ethanol to a concentration of 60% alcohol. Let it stand to precipitate. Take the supernatant, recover the ethanol, and concentrate it to an extract with a relative density of 1.2. S2. Add 6 times the weight of sucrose and 5% soy protein isolate to the extract obtained in step (1), stir at 300 rpm for 15 min to disperse, heat to 45℃ and stir to disperse for 35 min, then add 5% silica by weight of the extract and continue stirring for 15 min to obtain the mixture; S3. The mixture is wet-granulated and dried at 70°C to obtain Spleen-Soothing Granules. The Spleen-Soothing Granules prepared in this embodiment are uniform in size and color.

[0030] Example 3 A method for preparing Pishuning granules includes the following steps: S1. Take Poria cocos and hawthorn, add 8 times the amount of water and decoct twice. The weight ratio of hawthorn to Poria cocos is 2:1. The first decoction is 2 hours and the second decoction is 1 hour. Combine the decoctions, filter and collect the filtrate. Concentrate the filtrate to a relative density of 1.2 (80℃). Add ethanol to a concentration of 60% alcohol. Let it stand to precipitate. Take the supernatant, recover the ethanol, and concentrate it to an extract with a relative density of 1.2. S2. Add 6 times the weight of sucrose and 1% soy protein isolate to the extract obtained in step (1), stir at 300 rpm for 15 min to disperse, heat to 40℃ and stir to disperse for 45 min, then add 2% silica by weight of the extract and continue stirring for 15 min to obtain the mixture; S3. The mixture is wet-granulated and dried at 65℃ to obtain Pishuning granules.

[0031] The spleen-soothing granules prepared in this embodiment are uniform in size and color.

[0032] Comparative Example 1 A method for preparing Pishuning granules includes the following steps: S1. Take Poria cocos and hawthorn, add 8 times the amount of water and decoct twice. The weight ratio of hawthorn to Poria cocos is 2:1. The first decoction is 2 hours and the second decoction is 1 hour. Combine the decoctions, filter and collect the filtrate. Concentrate the filtrate to a relative density of 1.2 (80℃). Add ethanol to a concentration of 60% alcohol. Let it stand to precipitate. Take the supernatant, recover the ethanol, and concentrate it to an extract with a relative density of 1.2. S2. The extract obtained in step (1) is mixed with 6 times its weight of sucrose, wet granulation is performed, and the mixture is dried at 70°C to obtain Spleen-Soothing Granules (e.g., Spleen-Soothing Granules). Figure 2As shown in the figure, the particle size distribution of the comparative sample is not uniform.

[0033] Comparative Example 2 A method for preparing Pishuning granules includes the following steps: S1. Take Poria cocos and hawthorn, add 8 times the amount of water and decoct twice. The weight ratio of hawthorn to Poria cocos is 2:1. The first decoction is 2 hours and the second decoction is 1 hour. Combine the decoctions, filter and collect the filtrate. Concentrate the filtrate to a relative density of 1.2 (80℃). Add ethanol to a concentration of 60% alcohol. Let it stand to precipitate. Take the supernatant, recover the ethanol, and concentrate it to an extract with a relative density of 1.2. S2. Add 6 times the weight of sucrose to the extract obtained in step (1) and stir evenly. Then add 3% soy protein isolate, stir at 300 rpm for 15 min, heat to 45℃ and stir to disperse for 30 min to obtain the mixture. S3. The mixture is wet-granulated and dried at 70℃ to obtain Pishuning granules.

[0034] Comparative Example 3 A method for preparing Pishuning granules includes the following steps: S1. Take Poria cocos and hawthorn, add 8 times the amount of water and decoct twice. The weight ratio of hawthorn to Poria cocos is 2:1. The first decoction is 2 hours and the second decoction is 1 hour. Combine the decoctions, filter and collect the filtrate. Concentrate the filtrate to a relative density of 1.2 (80℃). Add ethanol to a concentration of 60% alcohol. Let it stand to precipitate. Take the supernatant, recover the ethanol, and concentrate it to an extract with a relative density of 1.2. S2. Add 6 times the weight of sucrose to the extract obtained in step (1) and stir until uniform. Add 4% silicon dioxide and stir at 300 rpm for 15 min to disperse. Heat to 50°C and stir to disperse for 45 min to obtain a mixture. S3. The mixture is wet-granulated and dried at 70℃ to obtain Pishuning granules.

[0035] Comparative Example 4 A method for preparing Pishuning granules includes the following steps: S1. Take Poria cocos and hawthorn and add 8 times the amount of water to decoct twice. The weight ratio of hawthorn to Poria cocos is 2:1. The first decoction is 2 hours and the second decoction is 1 hour. Combine the decoctions, filter and collect the filtrate. Concentrate the filtrate to a relative density of 1.2 (80℃), cool, add ethanol to a concentration of 60%, let stand to allow precipitation, collect the supernatant and recover the ethanol to obtain the extract. S2. Add 6 times the weight of sucrose to the extract obtained in step S1 and stir until homogeneous. Add 3% soy protein isolate and 4% silica by weight of the extract. Stir at 300 rpm for 15 min, then heat to 45°C and stir to disperse for 30 min to obtain the mixture. S3. The mixture is wet-granulated and dried at 70℃ to obtain Pishuning granules.

[0036] The particle size distribution, drying yield, and solubility of the spleen-soothing granules prepared in Examples 1-3 and Comparative Examples 1-4 were tested using the following methods: Drying yield (%) = Actual particle weight * 100 / Theoretical particle weight The actual particle weight is the actual weight of the dried spleen-soothing granules, while the theoretical particle weight is the sum of the weight of solids, sucrose, soy protein isolate, and silica in the extract.

[0037] Solubility: According to the 2020 edition of the Pharmacopoeia of the People's Republic of China, Part IV, 0104 Soluble Particle Test Method for Granules, take 10g of the test sample (one bag for single-dose packaging of traditional Chinese medicine), add 200ml of hot water, stir for 5 minutes, and observe immediately. The soluble particles should be completely dissolved or slightly turbid.

[0038] Particle size detection method: Manual double sieving method according to General Chapter 0982 of Part IV of the 2020 Pharmacopoeia of the People's Republic of China, with sieve mesh numbers of 20 mesh and 50 mesh.

[0039] The test results are shown in Table 1. The results indicate that the particle size distribution of the example was more uniform and the yield was higher than that of the comparative example. The addition of soy protein and silica synergistically improved the particle size uniformity of the spleen-soothing granules, reduced wall adhesion, and increased the yield. Comparing the results of Example 1 and Comparative Example 4, the order of adding soy protein and silica affected the effect; adding soy protein first, followed by silica, was beneficial for improving the uniformity of the prepared particles and the yield.

[0040] Table 1. Particle size, yield, solubility, and appearance of the particles prepared in Examples 1-3 and Comparative Examples 1-4. Example 4 A method for identifying Pishu Ning granules includes the following steps: (1) Preparation of the test solution: Take 10g of Pishu Ning granules powder, add 30ml of ethanol, sonicate for 30min, filter, evaporate the filtrate to dryness, add 1ml of ethanol to dissolve, and use as the test solution. (2) Preparation of control herbal solution: Take 0.2g of hawthorn reference material, add 100ml of water, heat under reflux for 1 hour, filter, concentrate the filtrate to near dryness, add 30ml of ethanol, sonicate for 30 minutes, filter, evaporate the filtrate to dryness, add 1ml of ethanol to dissolve, and use as the reference material solution. (3) Preparation of negative solution: Take 10g of hawthorn negative sample powder, add 30ml of ethanol, sonicate for 30 minutes, filter, evaporate the filtrate to dryness, add 1ml of ethanol to dissolve, and prepare a negative solution; (4) Thin-layer chromatography identification: Take 10 μL each of the reference herb solution, the test solution, and the negative solution, and spot them separately on the same silica gel G thin-layer plate. Develop the plate using chloroform-butanone-methanol-formic acid in a volume ratio of 5:5:2:1. Remove the plate, air dry it, bake it at 105℃ for 2 hours, and spray it with 0.1% bromophenol blue ethanol solution.

[0041] (5) Judgment indicators: When developed under sunlight, the test sample chromatogram shows spots of the same color at the corresponding positions as the reference medicinal material chromatogram, while the negative sample shows no spots.

[0042] The spleen-soothing granules prepared in Example 1 were identified using the identification method of this embodiment. The identification results are as follows: Figure 3 As shown.

[0043] from Figure 3 It can be seen that Pishuning granules and hawthorn control herbs show spots of the same color in the same position. No spots are found in the negative sample chromatogram at this position, indicating that this method has strong specificity and can effectively distinguish between Pishuning granules and negative samples lacking hawthorn. It can be used for thin-layer chromatography identification of hawthorn in Pishuning granules.

[0044] The foregoing description of specific exemplary embodiments of the invention is for illustrative and explanatory purposes. These descriptions are not intended to limit the invention to the precise forms disclosed, and it will be apparent that many changes and variations can be made in accordance with the foregoing teachings. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application, thereby enabling those skilled in the art to implement and utilize various different exemplary embodiments of the invention, as well as various different choices and variations. The scope of the invention is intended to be defined by the claims and their equivalents.

Claims

1. A method for preparing Pishuning granules, characterized in that, Includes the following steps: S1. Take Poria cocos and hawthorn, decoct them twice with water, combine the decoctions, filter and take the filtrate, concentrate the filtrate, add ethanol to the alcohol content to 50-60%, let it stand to precipitate, take the supernatant to recover the ethanol, and then obtain the extract. S2. Add sucrose to the extract obtained in step S1 and stir until homogeneous. Then add soy protein isolate, heat to 40-50°C and stir to disperse for 30-45 minutes. Then add silica and continue stirring for 10-30 minutes to obtain a mixture. S3. The mixture is wet-granulated and dried to obtain Pishuning granules.

2. The method for preparing Pishuning granules according to claim 1, characterized in that, In step S1, the filtrate is concentrated to a relative density of 1.15 to 1.

2.

3. The method for preparing Pishuning granules according to claim 1, characterized in that, In step S2, the amount of soy protein isolate used is 1-5% of the extract mass, and the amount of silica used is 2-6% of the extract mass; the stirring speed is 300-400 rpm.

4. The method for preparing Pishuning granules according to claim 1, characterized in that, In step S3, the drying temperature is 60~75℃.

5. A spleen-soothing granule, characterized in that, The spleen-soothing granules are prepared by the preparation method according to any one of claims 1 to 4.

6. A method for identifying the Pishu Ning granules as described in claim 5, characterized in that, Includes the following steps (1) Preparation of test solution: Take the fine powder of the spleen-soothing granules to be tested, put it into ethanol and sonicate it to prepare the test solution; (2) Preparation of control medicinal material solution: Take hawthorn control medicinal material, add water, heat and reflux, filter, concentrate the filtrate, add ethanol and sonicate to prepare control medicinal material solution; (3) Preparation of negative solution: Take hawthorn negative sample powder, add ethanol and sonicate to prepare negative solution; (4) Thin-layer chromatography identification: Take the reference herb solution, the test solution, and the negative solution, and spot them separately on the same silica gel G thin-layer plate. Use chloroform-butanone-methanol-formic acid in a volume ratio of 3~7:3~7:1~3:0.5~2 as the developing solvent. Remove the plate, air dry it, and bake it at 100~110℃ for 1~2 hours. Spray it with bromophenol blue ethanol solution and develop the color under sunlight. In the chromatogram of the test sample, spots appear at the same positions as in the chromatogram of the reference sample.

7. The method for identifying Pishuning granules according to claim 6, characterized in that, The specific steps (1) are as follows: take the fine powder of Pishuning granules, add ethanol, the ratio of fine powder of Pishuning granules to ethanol is 1g: 2~4ml, sonicate for 20~60min, filter, evaporate the filtrate to dryness, add ethanol to dissolve, and use it as the test solution.

8. The method for identifying Pishuning granules according to claim 6, characterized in that, The specific steps (2) are as follows: take hawthorn reference material, add water and heat under reflux for 1-2 hours. The ratio of hawthorn reference material to water is 0.2g: 50-150ml. Filter, concentrate the filtrate to near dryness, add ethanol, sonicate for 20-60 minutes, filter, evaporate the filtrate to dryness, add ethanol to dissolve, and use as the reference material solution.

9. The method for identifying Pishuning granules according to claim 6, characterized in that, The specific steps (3) are as follows: take hawthorn negative sample fine powder, add ethanol, the ratio of hawthorn negative sample fine powder to ethanol is 1g: 2~4ml, sonicate for 20~60min; filter, evaporate the filtrate to dryness, add ethanol to dissolve, and prepare a negative solution.

10. The method for identifying Pishuning granules according to claim 6, characterized in that, The volume ratio of chloroform-butanone-methanol-formic acid is 5:5:2:1.

Images