Preparation method for traditional chinese medicine pills for treating allergic rhinitis

Abstract

Provided is a preparation method for traditional Chinese medicine pills for treating allergic rhinitis, which comprises the following steps: uniformly mixing dry extract powder of traditional Chinese medicine pills and a volatile oil cyclodextrin inclusion complex with microcrystalline cellulose, magnesium stearate, silicon dioxide, and corn starch, and then subjecting the mixture to pelletizing. The pills are prepared by a compression method instead of the traditional plastic forming method. The preparation process is simple. The pill preparation process only involves three procedures: mixing, granulation, and pill compression, resulting in high production efficiency. The use of a pill compression mold enables precise control of the pill weight, so the difference in the pill weight is small. In addition, the compressed pill has a round and smooth appearance, thereby improving the aesthetic quality of the pills. In this method, the excipients are adjusted, so that the pill weight is stable during pill compression, and the hardness and friability both meet requirements, thereby meeting the requirements for the pill compression process. The method solves the problems of insufficient hardness and unqualified friability of small pills prepared by pill compression and can significantly improve the appearance quality and stability of pills. After being compressed, uncoated pills are wetted with 95% ethanol by means of pressurized direct spray atomization and then polished with 0.2% Chinese insect wax, making the pill surface brighter and improving moisture resistance.

Description

A method for preparing a traditional Chinese medicine pill for treating allergic rhinitis Technical Field

[0001] This invention belongs to the field of traditional Chinese medicine, specifically relating to a new method for preparing a traditional Chinese medicine pill for treating allergic rhinitis. Background Technology

[0002] A traditional Chinese medicine pill formula for treating allergic rhinitis consists of 14 herbs, including Astragalus membranaceus, Saposhnikovia divaricata, and Ephedra sinica (processed with honey). It has the effects of tonifying Qi and strengthening the exterior, dispelling wind and clearing the nasal passages, and is used to treat seasonal allergic rhinitis diagnosed as having a deficiency of lung and spleen Qi according to traditional Chinese medicine. Currently, the preparation method for this traditional Chinese medicine pill is a plastic forming process, which requires multiple steps including material mixing, adding binders, forming pill blocks, forming pill strips, shaping into round pills, drying the pills, and selecting the pills to obtain concentrated pills.

[0003] The preparation method has the following problems: ① The pelleting process is cumbersome and has poor controllability. Even with existing process parameters, the amount of binder added during pelleting still requires multiple adjustments based on manual experience to meet the requirements for soft material preparation. ② The pellet weight varies significantly, resulting in an unattractive appearance and low yield. After pelleting, the wet pellets are affected by the hardness of the soft material, leading to unstable shape, significant weight variations, and noticeable surface scars. This results in a low yield of qualified formulations after pellet selection, affecting the overall product quality. ③ The polishing effect is poor. The polishing process only involves placing the pellets in the coating pan and rotating them to improve roundness, which cannot guarantee the brightness and uniformity of the pellet's appearance.

[0004] Chinese patent CN101904948B discloses a new method for preparing Zhong Sheng Wan (a traditional Chinese medicine), with a pill weight of 0.27-0.42 g / pill and a spherical die size of 7.0-8.0 mm. Specifically, the traditional Zhong Sheng Wan preparation is extracted and concentrated twice to make an extract. The material temperature is controlled at 40-80℃, and the extract is dried into a dry powder using a vacuum belt dryer. The dry powder, Arisaema cum Bile powder, artificial bezoar, and excipients are mixed evenly, and then the mixture is pressed into pills using a pressing process. This replaces the traditional plasticizing method for pill making and solves the problems of the original pill making process, such as multiple steps, long production cycle, high cost, low efficiency, long drying time which is not conducive to the stability of Chinese medicine components, uneven surface, and large differences in pill weight.

[0005] The pills of this invention have a small weight, only 0.15g / pill. In practical applications, it has been found that it is difficult to control the stability of the process and the quality of the pills when directly using the existing pressing method to make pills. Summary of the Invention

[0006] The purpose of this invention is to provide a preparation process for a lightweight and small-sized traditional Chinese medicine pill for treating allergic rhinitis, based on existing technology.

[0007] The objective of this invention can be achieved through the following measures:

[0008] A method for preparing a traditional Chinese medicine pill for treating allergic rhinitis includes the following steps:

[0009] (1) Crush the magnolia flower, peony bark, saposhnikovia root, angelica root, and atractylodes macrocephala into small pieces, add water to extract the volatile oil, filter the oil, and store the water extract and the residue separately for later use.

[0010] (2) The volatile oil was encapsulated with β-cyclodextrin to obtain a volatile oil cyclodextrin inclusion complex. The volume-to-mass ratio of the volatile oil to β-cyclodextrin was 1 ml: 6-10 g.

[0011] (3) Take Poria cocos, dried plum, honey ephedra, Scutellaria baicalensis, licorice and the dregs after oil extraction in step (1) and decoct them with water once or multiple times. Combine them with the water extract after oil extraction in step (1) to obtain a concentrated liquid for later use.

[0012] (4) Extract Angelica dahurica, Schisandra chinensis, Astragalus membranaceus and Bupleurum chinense once or multiple times with ethanol or a mixture of ethanol and water, combine the ethanol liquids, recover the ethanol until there is no ethanol smell, concentrate and mix with the concentrated liquid obtained by water decoction in step (3), concentrate to a thick paste, dry and process into powder, i.e. dry paste powder.

[0013] (5) Add the volatile oil cyclodextrin inclusion complex, dry extract powder, microcrystalline cellulose and corn starch together into a mixer for premixing to obtain the initial mixture;

[0014] (6) After granulating the initial mixed material in step (5), add it to the mixer along with magnesium stearate and silicon dioxide for total mixing;

[0015] (7) The final mixture obtained in step (6) is shot-pressed, the shot weight is set and the weight difference is controlled to be ±8%.

[0016] (8) Place the vegetarian pills obtained in step (7) into a coating pan for polishing or coating.

[0017] In the traditional Chinese medicine pills of the present invention, the raw materials of each traditional Chinese medicine are as follows by weight: Astragalus membranaceus 5-20 parts, Saposhnikovia divaricata 5-15 parts, Ephedra sinica 2-6 parts, Magnolia biondii 2-10 parts, Angelica dahurica 2-10 parts, Atractylodes macrocephala 5-15 parts, Poria cocos 2-10 parts, Bupleurum chinense 2-10 parts, Angelica sinensis 2-10 parts, Paeonia suffruticosa 2-10 parts, Schisandra chinensis 2-10 parts, Prunus mume 2-10 parts, Scutellaria baicalensis 2-10 parts, and Glycyrrhiza uralensis 2-10 parts.

[0018] The volatile oil cyclodextrin inclusion complex of the traditional Chinese medicine pills in this invention is obtained by encapsulating volatile oils extracted from Magnolia biondii, Paeonia suffruticosa, Saposhnikovia divaricata, Angelica sinensis, and Atractylodes macrocephala with β-cyclodextrin. In one specific embodiment, the volume-to-mass ratio of volatile oil to β-cyclodextrin in the volatile oil cyclodextrin inclusion complex is 1 ml: 6-10 g, preferably 1 ml: 8 g.

[0019] In the method of this invention, the pressing method is used instead of the plasticizing method to make pellets, which can effectively solve the problems of complicated process, low production efficiency, high cost and low quality control.

[0020] The plasticizing method refers to a pelleting process in which drugs are mixed with suitable excipients, stirred evenly to form a soft material, extruded into pellets of a certain diameter by an extruder, and then cut by pelleting rollers to form uniformly sized spherical or near-spherical pellets. The plasticizing method is complex, requiring multiple steps such as material mixing, pelleting, pelleting strips, pellet forming, rounding, drying, and selection to produce concentrated pellets. This process results in low production efficiency, high production costs, and the amount of wetting agent added during pelleting relies heavily on manual experience, leading to numerous uncertainties and frequent problems such as poor pellet plasticity, inconsistent pellet size, surface hilum and depressions, and significant weight variations.

[0021] Compression molding is a pelleting process in which drugs are mixed with suitable excipients, then combined with binders and lubricants, or granulated and compressed into pellets. The compression molding process is simple, involving only three steps: mixing, granulation, and pelleting. It boasts high production efficiency and low production costs. The pellets, formed from powdered or granular drugs using molds, exhibit high hardness, minimal weight variation controlled by the mold, and are round, smooth, and free of dents or pits.

[0022] In the pelleting process in steps (5) and (6), the mass composition of each component includes: 40% to 80% dry powder, 1.0% to 3.0% volatile oil cyclodextrin inclusion complex, 20% to 30% microcrystalline cellulose, 0.4% to 0.6% magnesium stearate, 0.8% to 1.2% silicon dioxide, and an appropriate amount of corn starch.

[0023] In a preferred embodiment, during the pelleting process, the mass composition of each component includes: 50%–70% dry extract powder, 1.0%–2.5% volatile oil cyclodextrin inclusion complex, 21%–24% microcrystalline cellulose, 0.5% magnesium stearate, 1.0% silicon dioxide, and an appropriate amount of corn starch.

[0024] The original formulation of the herbal pills in this invention does not contain lubricants, resulting in poor flowability. When using a compression method to make the pills, the mixed powder is not fed smoothly during compression, easily clogging the hopper. Furthermore, the pills, after compression, lack hardness and crumble easily with light pressure, leading to breakage and loosening, failing to meet product quality requirements. This invention adds specific amounts of lubricants magnesium stearate and silicon dioxide to the original formulation and adjusts the amount of microcrystalline cellulose, increasing both the flowability and compressibility of the material.

[0025] In one specific embodiment, the formulation of the present invention is as follows:

[0026] Because this product has a pellet weight of 0.15g / pill, its small size makes it difficult to achieve the required hardness and brittleness of the pellets using conventional pelleting or tableting methods. To research and select a suitable pelleting process and parameters that achieves both lightweight and small size, the inventors conducted pelleting tests on multiple batches of materials. Through long-term experimentation, they adjusted parameters such as pelleting speed, powder filling thickness, and main pellet pressure. They determined that using a P3030 tablet press with a 6mm spherical mold, a pelleting speed controlled at 37-120 thousand pellets / hour, a powder filling thickness controlled at 5.0-6.0mm, and a main pellet pressure controlled at 7-12KN, could meet the requirement of a pellet weight of 0.15g / pill (with a weight difference within ±8%), a pellet hardness of 20-70N, and a brittleness within 0.5%. The key technical problems of insufficient hardness and unacceptable brittleness during the heavy compression of small pellets have been successfully solved.

[0027] Meanwhile, this invention further improves the polishing process. Pill polishing refers to the specific process applied to the pill after it has been formed, to achieve a smooth, glossy, and uniformly colored surface.

[0028] The current polishing process for this traditional Chinese medicine pill involves placing the pills into a water chestnut-shaped coating pan and rotating them for less than 5 minutes. This rotation and friction increases the roundness of the pills, but the gloss is relatively poor. To improve the appearance and gloss of the pills and increase their moisture resistance, the improved polishing process is as follows: Turn on the water chestnut-shaped coating pan and hot air. Place the concentrated pills in the pan and spray in 90%–96% ethanol to moisten them until the pills have a uniform color. Slowly add insect wax powder (0.1%–0.3% of the total weight of the concentrated pills) for polishing until the pill surface is glossy and the moisture content does not exceed 7.0%. Then stop heating and discharge the pills when the temperature of the pill bed is below 40℃.

[0029] In a preferred embodiment, the pellets are moistened in a 95% ethanol environment by pressurized direct spraying of ethanol, and polished with beeswax, wherein the amount of beeswax added is 0.2% of the total amount of the pellets.

[0030] The improved polishing process uses 95% ethanol as a wetting agent. 95% ethanol is highly volatile and evaporates rapidly, reducing residual liquid on the pill surface and shortening drying time. Simultaneously, the pressurized direct injection of 95% ethanol quickly and evenly wets the pill surface, avoiding the uneven wetting problem of traditional peristaltic pump injection methods. Furthermore, adding 0.2% beeswax to the wetted pills before polishing revealed that the beeswax partially dissolves in hot ethanol, resulting in a rapid and uniform gloss and color, improving the pills' moisture resistance, and preventing issues such as surface mottling and prolonged drying times after polishing. This significantly improves the appearance quality and stability of the pills.

[0031] In step (6), the preferred initial mixture is granulated using a dry granulator.

[0032] The method of the present invention may further include a coating process, that is, coating the pressed vegetarian pellets.

[0033] Coating is a process in which sugars or other film-forming materials are coated onto the outer surface of a solid pharmaceutical preparation using specific equipment and a specific process. After drying, it forms one or more multifunctional protective layers of varying thicknesses and elasticities that adhere tightly to the surface. Plain pills made by compression often exhibit uneven coloring and are prone to moisture absorption. Using a stomach-soluble film-coating premix, such as Opadry, to prepare a 20% coating solution, the pills are then coated. The weight gain after coating is within the range of 2.5% to 4.5%. Coated plain pills have a more uniform color and a smoother surface, reducing throat irritation during administration, facilitating swallowing, and effectively preventing moisture absorption and spoilage.

[0034] The present invention can use a film coating premix for coating.

[0035] A specific coating formula is as follows:

[0036] This invention includes a specific method for preparing traditional Chinese medicine pills, which includes the following steps:

[0037] (1) Crush the magnolia flower, peony bark, saposhnikovia root, angelica root, and atractylodes macrocephala into small pieces, add water to extract the volatile oil for 2-6 hours, filter, and store the water extract and the residue separately for later use.

[0038] (2) The volatile oil was encapsulated with β-cyclodextrin to obtain a volatile oil cyclodextrin inclusion complex. The volume-to-mass ratio of the volatile oil to β-cyclodextrin was 1 ml: 8 g.

[0039] (3) Take Poria cocos, dried plum, honey ephedra, Scutellaria baicalensis, licorice and the dregs after oil extraction in step (1) and add water to decoct once or several times for 1.5 hours each time. Combine it with the water extract after oil extraction in step (1) to prepare a concentrated solution for later use.

[0040] (4) Extract Angelica dahurica, Schisandra chinensis, Astragalus membranaceus and Bupleurum chinense three times with 70% ethanol for 2 hours each time. Combine the ethanol liquids, recover the ethanol until there is no ethanol smell, concentrate and mix with the concentrated liquid of the decoction in step (3), concentrate to a thick paste of 1.20-1.40 (55℃), dry and process into powder.

[0041] (5) Add the volatile oil cyclodextrin inclusion complex, dry extract powder, microcrystalline cellulose and corn starch together to a mixer and premix for 5-30 minutes to obtain the initial mixture.

[0042] (6) After granulating the initial mixed material in step (5), add it to the mixer along with magnesium stearate and silicon dioxide, and mix for 5-30 minutes.

[0043] (7) The final mixture from step (6) is compressed into pellets using a tablet press. The pellet weight is set and the pellets are compressed using a constant weight (0.15g / pellet). The weight difference limit is controlled to be ±8%.

[0044] (8) Place the vegetarian pills obtained in step (7) into a coating pan for polishing or coating.

[0045] The method for preparing traditional Chinese medicine pills provided by this invention has the following advantages:

[0046] ① The molding process of pelleting by compression replaces the traditional plastic pelleting process. The preparation process is simple, the production process is highly controllable, the production efficiency is high, the pellet weight difference is small, and the pellets are round and smooth.

[0047] ② The amount of microcrystalline cellulose in the formulation was adjusted from 8% to 21%–24%, and the amount of magnesium stearate (a lubricant) and silica (1.0%) was increased. Precise control of the amount of excipients in the formulation can improve the flowability and compressibility of the powder, reduce the breakage and loosening of the pills, ensure the quality stability of the pills, and improve product quality.

[0048] ③ Using a P3030 tablet press with a 6mm spherical mold for pellet compression, the pelleting speed is controlled at 37-120 thousand pellets / hour, the powder filling thickness is controlled at 5.0-6.0mm, and the main pressure of the pellet is controlled at 7-12KN. This meets the requirement of 0.15g / pill (pill weight difference within ±8%), the pellet hardness can reach 20-70N, and the friability is within 0.5%. This solves the problems of insufficient hardness and unacceptable friability when compressing small pellets.

[0049] ④ The polishing process uses 95% ethanol sprayed under pressure to quickly and evenly wet the surface of the pills. 95% ethanol is highly volatile and can evaporate quickly in a short time, reducing the drying time of the pill surface. After the pills are wetted with 95% ethanol, 0.2% beeswax is added for polishing, making the surface of the pills shinier and improving their moisture resistance. Attached Figure Description

[0050] Figure 1 is a picture of the product obtained in Embodiment 1 of the present invention;

[0051] Figure 2 is a picture of the product obtained in Embodiment 2 of the present invention;

[0052] Figure 3 is a picture of the product obtained in Embodiment 3 of the present invention;

[0053] Figure 4 is a picture of the dried pills moistened with different wetting agents in Experimental Example 5 of the present invention;

[0054] Figure 5 is a picture of the dried pills moistened with different concentrations of ethanol in Experimental Example 6 of the present invention;

[0055] Figure 6 is a picture of the dried pill after being moistened with 95% ethanol by different spraying methods in Experimental Example 7 of the present invention;

[0056] Figure 7 is a picture of the pills after being illuminated by different types of light-emitting agents in Experimental Example 8 of the present invention;

[0057] Figure 8 is a picture of the pills after polishing with different amounts of insect wax in Experimental Example 9 of the present invention;

[0058] Figure 9 is a picture of pills with different proportions of dry powder after being polished in Experimental Example 10 of the present invention. Detailed Implementation

[0059] The technical solution of the present invention will be further described below with reference to specific embodiments, but the scope of protection is not limited to the description.

[0060] The traditional Chinese medicine pills referred to in this invention contain the following raw materials in parts by weight: Astragalus membranaceus 5-20 parts, Saposhnikovia divaricata 5-15 parts, Ephedra sinica (honey-processed) 2-6 parts, Magnolia biondii 2-10 parts, Angelica dahurica 2-10 parts, Atractylodes macrocephala 5-15 parts, Poria cocos 2-10 parts, Bupleurum chinense 2-10 parts, Angelica sinensis 2-10 parts, Paeonia suffruticosa 2-10 parts, Schisandra chinensis 2-10 parts, Prunus mume 2-10 parts, Scutellaria baicalensis 2-10 parts, and Glycyrrhiza uralensis 2-10 parts.

[0061] Example 1

[0062] The raw materials for a traditional Chinese medicine pill are as follows: Astragalus membranaceus 400g, Saposhnikovia divaricata 300g, Ephedra sinica (honey-processed) 120g, Magnolia biondii 200g, Angelica dahurica 200g, Atractylodes macrocephala 300g, Poria cocos 200g, Bupleurum chinense 200g, Angelica sinensis 200g, Paeonia suffruticosa 200g, Schisandra chinensis 200g, Prunus mume 200g, Scutellaria baicalensis 200g, and Glycyrrhiza uralensis 120g.

[0063] The formulation is as follows:

[0064] The preparation method of the traditional Chinese medicine pills in this example includes the following steps:

[0065] (1) Crush the magnolia flower, peony bark, saposhnikovia root, angelica root, and atractylodes macrocephala into small pieces, add water to extract the volatile oil for 6 hours, filter, and store the water extract and the residue separately for later use.

[0066] (2) The volatile oil was encapsulated with β-cyclodextrin to obtain a volatile oil cyclodextrin inclusion complex. The ratio of the volatile oil to β-cyclodextrin was 1 ml: 8 g.

[0067] (3) Take Poria cocos, dried plum, honey ephedra, Scutellaria baicalensis, licorice and the dregs after oil extraction in step (1) and decoct them twice with water for 1.5 hours each time. Combine them with the water extract after oil extraction in step (1) to prepare a concentrated solution for later use.

[0068] (4) Extract Angelica dahurica, Schisandra chinensis, Astragalus membranaceus and Bupleurum chinense three times with 70% ethanol for 2 hours each time. Combine the ethanol liquids, recover the ethanol until there is no ethanol smell, concentrate and mix with the concentrated liquid of the decoction in step (3), concentrate to a thick paste of 1.20-1.40 (55℃), dry and process into powder.

[0069] (5) Add the volatile oil cyclodextrin inclusion complex, dry extract powder, microcrystalline cellulose and corn starch together into a mixer for premixing to obtain the initial mixture;

[0070] (6) The mixture initially mixed in step (5) is granulated by a dry granulator;

[0071] (7) Add the dry granulation particles from step (6) to a mixer along with magnesium stearate and silica and mix them together.

[0072] (8) The final mixture from step (7) is compressed into pellets using a P3030 tablet press. The pellet weight is set and the pellets are compressed using a constant weight (0.15g / pellet). The weight difference limit is controlled to be ±8%.

[0073] (9) Place the vegetarian pills obtained in step (8) in a coating pan for preheating, spray in 95% ethanol to moisten until the pills are uniform in color, slowly add insect wax powder for polishing, the amount of insect wax is 0.2% of the total weight of the vegetarian pills, until the surface of the pills is bright and the moisture content is not more than 7.0%, then stop heating and discharge the material when the temperature of the pill bed is less than 40°C.

[0074] Example 2

[0075] The raw materials for a traditional Chinese medicine pill are as follows: Astragalus membranaceus 500g, Saposhnikovia divaricata 500g, Ephedra sinica (honey-processed) 200g, Magnolia biondii 200g, Angelica dahurica 200g, Atractylodes macrocephala 500g, Poria cocos 200g, Bupleurum chinense 200g, Angelica sinensis 200g, Paeonia suffruticosa 200g, Schisandra chinensis 200g, Prunus mume 200g, Scutellaria baicalensis 200g, and Glycyrrhiza uralensis 200g.

[0076] The formulation is as follows:

[0077] The coating prescription is as follows:

[0078] The preparation method of the traditional Chinese medicine pills of this invention includes the following steps:

[0079] (1) Crush the magnolia flower, peony bark, saposhnikovia root, angelica root, and atractylodes macrocephala into small pieces, add water to extract the volatile oil for 6 hours, filter, and store the water extract and the residue separately for later use.

[0080] (2) The volatile oil was encapsulated with β-cyclodextrin to obtain a volatile oil cyclodextrin inclusion complex. The ratio of the volatile oil to β-cyclodextrin was 1 ml: 8 g.

[0081] (3) Take Poria cocos, dried plum, honey ephedra, Scutellaria baicalensis, licorice and the dregs after oil extraction in step (1) and decoct them twice with water for 1.5 hours each time. Combine them with the water extract after oil extraction in step (1) to prepare a concentrated solution for later use.

[0082] (4) Extract Angelica dahurica, Schisandra chinensis, Astragalus membranaceus and Bupleurum chinense three times with 70% ethanol for 2 hours each time. Combine the ethanol liquids, recover the ethanol until there is no ethanol smell, concentrate and mix with the concentrated liquid of the decoction in step (3), concentrate to a thick paste of 1.20-1.40 (55℃), dry and process into powder.

[0083] (5) Add the volatile oil cyclodextrin inclusion complex, dry extract powder, microcrystalline cellulose and corn starch together into a mixer for premixing to obtain the initial mixture;

[0084] (6) The mixture initially mixed in step (5) is granulated by a dry granulator;

[0085] (7) Add the dry granulation particles from step (6) to a mixer along with magnesium stearate and silica and mix them together.

[0086] (8) The final mixture from step (7) is compressed into pellets using a P3030 tablet press. The pellet weight is set and the pellets are compressed using a constant weight (0.15g / pellet). The weight difference limit is controlled to be ±8%.

[0087] (9) Place the vegetarian pills obtained in step (8) into a coating pan for preheating. After the preheating temperature is reached, adjust the position of the spray gun and use 20% of the stomach-soluble film coating premix Opadry aqueous solution for coating. The coating weight gain rate is 2.5-4.5%.

[0088] Example 3

[0089] The raw materials for a traditional Chinese medicine pill are as follows: Astragalus membranaceus 750g, Saposhnikovia divaricata 500g, Ephedra sinica 200g, Magnolia biondii 250g, Angelica dahurica 250g, Atractylodes macrocephala 500g, Poria cocos 250g, Bupleurum chinense 250g, Angelica sinensis 250g, Paeonia suffruticosa 250g, Schisandra chinensis 250g, Prunus mume 250g, Scutellaria baicalensis 250g, and Glycyrrhiza uralensis 250g.

[0090] The formulation is as follows:

[0091] The coating prescription is as follows:

[0092] The preparation method of the traditional Chinese medicine pills in this example includes the following steps:

[0093] (1) Crush the magnolia flower, peony bark, saposhnikovia root, angelica root, and atractylodes macrocephala into small pieces, add water to extract the volatile oil for 6 hours, filter, and store the water extract and the residue separately for later use.

[0094] (2) The volatile oil was encapsulated with β-cyclodextrin to obtain a cyclodextrin inclusion complex. The ratio of the volatile oil to β-cyclodextrin was 1 ml: 8 g.

[0095] (3) Take Poria cocos, dried plum, honey ephedra, Scutellaria baicalensis, licorice and the dregs after oil extraction in step (1) and decoct them twice with water for 1.5 hours each time. Combine them with the water extract after oil extraction in step (1) to prepare a concentrated solution for later use.

[0096] (4) Extract Angelica dahurica, Schisandra chinensis, Astragalus membranaceus and Bupleurum chinense three times with 70% ethanol for 2 hours each time. Combine the ethanol liquids, recover the ethanol until there is no ethanol smell, concentrate and mix with the concentrated liquid of the decoction in step (3), concentrate to a thick paste of 1.20-1.40 (55℃), dry and process into powder.

[0097] (5) Add the volatile oil cyclodextrin inclusion complex, dry extract powder, microcrystalline cellulose and corn starch together into a mixer for premixing to obtain the initial mixture;

[0098] (6) The mixture initially mixed in step (5) is granulated by a dry granulator;

[0099] (7) Add the dry granulation particles from step (6) to a mixer along with magnesium stearate and silica and mix them together.

[0100] (8) The final mixture from step (7) is compressed into pellets using a P3030 tablet press. The pellet weight is set and the pellets are compressed using a constant weight (0.15g / pellet). The weight difference limit is controlled to be ±8%.

[0101] (9) Place the vegetarian pills obtained in step (8) into a coating pan for preheating. After the preheating temperature is reached, adjust the position of the spray gun and use 20% of the stomach-soluble film coating premix Opadry aqueous solution for coating. The coating weight gain rate is 2.5-4.5%.

[0102] Experimental Example 1

[0103] The original formulation of the Chinese herbal pills in this invention does not contain lubricant and has poor fluidity. When the pills are pressed using the compression method, problems such as pills not forming properly and easily dispersing may occur.

[0104] The shot-forming method was used to investigate the effects of different types and amounts of lubricants on the shot-forming effect. The results are shown in Table 1 below.

[0105] Table 1. Investigation of Lubricant Types and Dosage Note: Beta-cyclodextrin was used instead of volatile oil cyclodextrin inclusion complex.

[0106] The results above show that a good pelletizing effect is achieved only when magnesium stearate and silica at specific concentrations are present and work synergistically. The pelleting effect was best with a formulation containing 0.5% magnesium stearate and 1.0% silica lubricant; no breakage occurred during the pressing process, and the hardness and brittleness tests all met the requirements.

[0107] Experimental Example 2

[0108] In the original formulation of the traditional Chinese medicine pills of this invention, microcrystalline cellulose accounts for 8%. Given the strong compressibility of microcrystalline cellulose, the compressibility of microcrystalline cellulose materials with different proportions in the formulation was investigated. The specific test results are shown in Table 2 below.

[0109] Table 2. Investigation on the dosage of microcrystalline cellulose Note: Beta-cyclodextrin was used instead of volatile oil cyclodextrin inclusion complex.

[0110] The results above show that increasing the amount of microcrystalline cellulose significantly improves the dry granulation effect and compressibility of the pills; as its proportion increases, the pill hardness also increases accordingly. When the proportion of microcrystalline cellulose is above 20%, the pills exhibit good hardness and granulation performance, maintaining a low principal pressure while meeting the brittleness requirements. Considering the proportion of dry extract powder and volatile oil cyclodextrin inclusion complex in the pill-making process of this invention, the proportion of microcrystalline cellulose is preferably determined to be between 20% and 30%.

[0111] Experimental Example 3

[0112] According to the traditional Chinese medicine pill formulation of this invention, the proportion of dry extract powder is between 40% and 80%. The pelleting method was used to confirm the pelleting effect of different proportions (50%, 60%, 70%) of dry extract powder, 1.5% beta-cyclodextrin, 21% or 24% microcrystalline cellulose, 0.5% magnesium stearate, 1.0% silica, and appropriate amounts of corn starch. The results are shown in Table 3.

[0113] Table 3. Formulations of dry ointment powder preparations with different proportions. Note: Beta-cyclodextrin was used instead of volatile oil cyclodextrin inclusion complex.

[0114] The test results show that: with a formulation containing 50%–70% dry extract powder, 1.5% beta-cyclodextrin, 21%–24% microcrystalline cellulose, 0.5% magnesium stearate, 1.0% silica, and 3%–26% corn starch, the pills are round and smooth, the weight is precisely controlled with minimal fluctuation, the brittleness test is qualified, the average hardness is above 30N, and the pelleting process is stable.

[0115] Experiment Example 4

[0116] The traditional Chinese medicine pills of this invention weigh 0.15g / pill. Due to their small weight, a spherical mold is used for pressing. During the pressing process, the contact area between the powder and the mold is small. It is difficult to achieve the required hardness and brittleness of the pressed pills using conventional pressing or tableting methods.

[0117] The formulation of Example 1 was used, and the pelleting process was adjusted. Multiple batches of materials were subjected to pelleting tests, and the results of parameters such as pelleting speed, powder filling thickness, and main pellet pressure were compared. Specific experimental results are shown in Table 4.

[0118] Table 4. Statistical table of pelleting process parameters for different formulation batches

[0119] The test results show that when using a P3030 tablet press with a 6mm spherical mold for pelleting, the pelleting speed is controlled at 37-120 thousand pellets / hour, the powder filling thickness is controlled at 5.0-6.0mm, and the main pressure of the pellet is controlled at 7-12KN. This can meet the requirement of 0.15g / pill (pill weight difference within ±8%), the pellet hardness can reach 20-70N, the brittleness is within 0.5%, and the pelleting yield is above 95%.

[0120] Experimental Example 5

[0121] The original polishing process for the pills in this invention only improved the roundness of the pills through rotation and friction, which could not guarantee the uniformity of the pills' properties. In order to improve the appearance of the pills and enhance the product's moisture resistance, the polishing process was optimized, and the effects of different types and amounts of polishing agents on the polishing effect were investigated.

[0122] The mixed powder of the traditional Chinese medicine pills prepared in Example 1 was dissolved in 95% ethanol, 75% ethanol, 35% ethanol and water. The results showed that the higher the ethanol concentration, the worse the solubility of the mixed powder, and it was easy to separate into layers after standing. Therefore, the mixed powder solution dissolved in 35% ethanol and the mixed powder solution dissolved in water were selected as wetting agents to wet the pills. The results are shown in Table 5 below.

[0123] Table 5. Investigation of Wetting Agent Types

[0124] The above test results show that neither 35% ethanol nor water can completely dissolve the mixed powder to form a homogeneous solution. Prolonged spraying is required to achieve a uniform color in the pills. Furthermore, since the pills are a whole extract preparation, prolonged contact with the aqueous solution causes partial dissolution, resulting in a rough surface and poor roundness after drying. Therefore, medicinal juices should not be used as wetting agents.

[0125] Experimental Example 6

[0126] Under otherwise unchanged conditions, the raw pills prepared in Example 1 were placed in a coating pan and moistened with 95% ethanol, 85% ethanol, and 75% ethanol. The effects of different wetting agents on the pills were observed. The specific experimental results are shown in Table 6 below.

[0127] Table 6 Ethanol Concentration Screening

[0128] The experimental results show that when the pills are moistened with 95% ethanol, 85% ethanol, and 75% ethanol before drying, the pills exhibit greater fluidity during the polishing process, shorter drying time, and more uniform color after drying as the ethanol concentration increases. Given the high volatility of 95% ethanol, which rapidly evaporates, reducing residual liquid on the pill surface and shortening drying time, 95% ethanol is the preferred choice for moistening the pills.

[0129] Experimental Example 7

[0130] Based on Experiment 6, the effects of different wetting methods of 95% ethanol on the pills were investigated, and the results are shown in Table 7 below.

[0131] Table 7 Investigation of Ethanol Wetting Methods

[0132] The test results show that when using a peristaltic pump or a handheld spray bottle to wet the pills, the limited amount sprayed at one time results in uneven color of the pills. In order to increase the instantaneous amount of ethanol sprayed, wetting the pills with 95% ethanol by pressurized direct spraying can rapidly increase the amount of ethanol sprayed, so that the pills can achieve the purpose of wetting and uniform color in a short time.

[0133] Experimental Example 8

[0134] With other conditions remaining unchanged, adjustments were made to Example 1. Talc and beeswax were used for polishing and testing, and the specific test results are shown in Table 8 below.

[0135] Table 8 Screening of Lighting Agent Types

[0136] The test results show that when talcum powder is used for polishing, the surface of the pills is covered with obvious talcum powder; when beeswax is used for polishing, a small amount of beeswax accumulates at the waistline of the pills, while there is almost no residue on the round surface, and the pills are shiny. Therefore, beeswax is the better polishing agent.

[0137] Experimental Example 9

[0138] Based on Experiment 8, the dosage of insect wax was investigated at 1.0%, 0.5%, 0.3%, 0.1%, 0.05%, and 0.02%, and the specific experimental results are shown in Table 9 below.

[0139] Table 9. Investigation of the Dosage of Polishing Agent

[0140] The experimental results show that polishing with insect beeswax enhances the overall gloss of the pills. Furthermore, the gloss level gradually increases with increasing beeswax content. However, when the beeswax content exceeds 0.3%, beeswax powder adheres to the surface and waistline of the pills, resulting in uneven color. To ensure the pills' gloss and moisture resistance, the recommended beeswax content is 0.1%-0.3% of the total pill weight.

[0141] Experimental Example 10

[0142] Based on the formulation of Example 1, the amount of dry powder was adjusted, and the polishing effect of the pellets after compression was verified for different proportions of 50%, 60%, and 70% dry powder formulations to ensure the stability and feasibility of the polishing process. The specific experimental process and results are shown in Table 10 below.

[0143] Table 10. Verification Test of Lighting Process

[0144] The experimental results show that after pressing the raw pills into pellets with different proportions of 50%, 60%, and 70% dry ointment powder, the pills have a bright surface and uniform color after polishing, indicating that the polishing process is feasible.

[0145] As seen in Experiments 5-10, using pressurized direct spraying of 95% ethanol to wet the pills can rapidly increase the amount of ethanol sprayed, enabling the pills to achieve wetting and uniform color in a short time. Using 0.2% beeswax as a polishing agent can ensure a smooth surface and uniform color of the pills. The polishing process is as follows: turn on the water chestnut-shaped coating pan and hot air, place the plain pills in the coating pan, spray in 95% ethanol to wet until the pills have a uniform color, slowly add beeswax powder for polishing, the amount of beeswax is 0.2% of the total weight of the plain pills, until the surface of the pills is shiny and the moisture content does not exceed 7.0%, then stop heating and discharge the material when the pill bed temperature is below 40℃.

[0146] Finally, it should be noted that the technical solutions of the present invention are not limited to the above embodiments. All modifications that can be directly derived or conceived by those skilled in the art from the content disclosed in the present invention should be considered to be within the scope of protection of the present invention.

Claims

1. A method for preparing a traditional Chinese medicine pill for treating allergic rhinitis, comprising the following steps: (1) Crush the magnolia flower, peony bark, saposhnikovia root, angelica root, and atractylodes macrocephala into small pieces, add water to extract the volatile oil, filter the oil, and store the water extract and the residue separately for later use. (2) The volatile oil was encapsulated with β-cyclodextrin to obtain a volatile oil cyclodextrin inclusion complex. The volume-to-mass ratio of the volatile oil to β-cyclodextrin was 1 ml: 6-10 g. (3) Take Poria cocos, dried plum, honey ephedra, Scutellaria baicalensis, licorice and the dregs after oil extraction in step (1) and decoct them with water once or multiple times. Combine them with the water extract after oil extraction in step (1) to obtain a concentrated liquid for later use. (4) Extract Angelica dahurica, Schisandra chinensis, Astragalus membranaceus and Bupleurum chinense once or multiple times with ethanol or a mixture of ethanol and water, combine the ethanol liquids, recover the ethanol until there is no ethanol smell, concentrate and mix with the concentrated liquid obtained by water decoction in step (3), concentrate to a thick paste, dry and process into powder, i.e. dry paste powder. (5) Add the volatile oil cyclodextrin inclusion complex, dry extract powder, microcrystalline cellulose and corn starch together into a mixer for premixing to obtain the initial mixture; (6) After granulating the initial mixed material in step (5), add it to the mixer along with magnesium stearate and silicon dioxide for total mixing; (7) The final mixture obtained in step (6) is pelletized with a set pellet weight, and the weight difference is controlled to be within ±8%. (8) Place the vegetarian pills obtained in step (7) into a coating pan for polishing or coating.

2. The method for preparing the traditional Chinese medicine pills for treating allergic rhinitis according to claim 1, characterized in that, In step (7), the pelleting speed is controlled at 37-120 thousand pellets / hour, the powder filling thickness is controlled at 5.0-6.0 mm, the pressure is controlled at 7-12 KN, and the pellet hardness is controlled at 20-70 N.

3. The method for preparing the traditional Chinese medicine pills for treating allergic rhinitis according to claim 1, characterized in that, In steps (5) and (6), the mass composition of each component includes: 40%–80% dry extract powder, 1%–3% volatile oil cyclodextrin inclusion complex, 20%–30% microcrystalline cellulose, 0.4%–0.6% magnesium stearate, 0.8%–1.2% silicon dioxide, and an appropriate amount of corn starch; the raw materials of each Chinese herbal medicine in the pills include, by weight: Astragalus membranaceus 5–20 parts, Saposhnikovia divaricata 5–15 parts, Ephedra sinica 2–6 parts, Magnolia biondii 2–10 parts, Angelica dahurica 2–10 parts, Atractylodes macrocephala 5–15 parts, Poria cocos 2–10 parts, Bupleurum chinense 2–10 parts, Angelica sinensis 2–10 parts, Paeonia suffruticosa 2–10 parts, Schisandra chinensis 2–10 parts, Prunus mume 2–10 parts, Scutellaria baicalensis 2–10 parts, and Glycyrrhiza uralensis 2–10 parts.

4. The method for preparing the traditional Chinese medicine pills for treating allergic rhinitis according to claim 1, characterized in that, In step (8), when polishing, the vegetarian pills obtained in step (7) are placed in a coating pan for preheating. They are moistened with 90% to 96% ethanol until the pills have a uniform color. Insect wax is slowly added for polishing. The amount of insect wax is 0.1% to 0.3% of the total weight of the vegetarian pills. The heating is stopped when the surface of the pills is shiny and the moisture content does not exceed 7.0%. The pills are discharged when the temperature of the pill bed is less than 40°C.

5. The method for preparing the traditional Chinese medicine pills for treating allergic rhinitis according to claim 4, characterized in that, During the polishing process, the ethanol concentration is 95%, and the amount of insect wax added is 0.2% of the total amount of the raw pills.

6. The method for preparing the traditional Chinese medicine pills for treating allergic rhinitis according to claim 4, characterized in that, During the polishing process, the concentrated pellets are moistened by pressurized direct spraying of ethanol.

7. The method for preparing the traditional Chinese medicine pills for treating allergic rhinitis according to claim 1, characterized in that, In step (8), when coating, the vegetarian pills obtained in step (7) are placed in a coating pan for preheating. After the preheating temperature is reached, the position of the spray gun is adjusted and 20% of the stomach-soluble film coating premix Opadry aqueous solution is used for coating. The coating weight gain rate is 2.5 to 4.5%.

8. The method for preparing the traditional Chinese medicine pills for treating allergic rhinitis according to claim 1, characterized in that, In step (6), the initial mixture is granulated using a dry granulator.

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