Preparation method of Cinnamomum camphora red tangerine peel formula granules

Abstract

The preparation method comprises the following steps: taking Cinnamomum camphora red dried orange peel decoction pieces, adding water, decocting, filtering to obtain a Cinnamomum camphora red dried orange peel extracting solution, concentrating the extracting solution to obtain clear paste, adding a proper amount of auxiliary materials into the clear paste, drying to obtain Cinnamomum camphora red dried orange peel dry paste powder, uniformly mixing the dry paste powder with a proper amount of auxiliary materials, performing dry granulation, and packaging to obtain the Cinnamomum camphora red dried orange peel formula granules. The cinnamomum camphora red tangerine peel formula granules are obtained. The invention establishes a preparation process of the Cinnamomum camphora red dried orange peel formula granules, and by mixing beta-cyclodextrin and silicon dioxide with the Cinnamomum camphora red dried orange peel clear paste before drying, the powder yield of the Cinnamomum camphora red dried orange peel dry paste powder is remarkably improved. The prepared Cinnamomum camphora red dried tangerine peel formula granules have low hygroscopicity and good formability and fluidity.

Description

Technical Field

[0001] This invention relates to the field of traditional Chinese medicine preparation technology, and in particular to a method for preparing a formula granule of camphor red tangerine peel. Background Technology

[0002] Traditional Chinese medicine (TCM) granules are granules made from single-herb medicinal slices through water extraction, concentration, drying, granulation, and quantitative packaging. As a modern dosage form of traditional decoctions, compared to traditional decoctions, they can maintain the quality and efficacy of the original medicinal slices, meet the needs of clinical diagnosis and treatment, allow for adjustments based on symptoms, and are easier to store, take, and carry, bringing many conveniences to doctors and patients and showing good development prospects. However, currently, TCM granules are mainly manufactured using traditional techniques such as extraction, concentration, drying, granulation, and packaging. This can lead to the loss of effective components and unstable quality in some medicinal materials containing volatile substances or high levels of starch and mucilage during the preparation process.

[0003] Camphor Red Citrus reticulate cv. Zhangshuensis Citrus aurantium, a plant of the Rutaceae family Citrus reticulata Blanco A cultivated variety, it is a perennial woody plant. Zhangtouhong is a citrus variety characteristic of Jiangxi Province and a local species endemic to Zhangshu City. It is mainly planted in the alluvial plains of the Yuanhe and Ganjiang Rivers, including Zhoushang Township and Linjiang Town, and has a long history of cultivation. In 2020, it was included in the "Ten Delicacies of Jiangxi" list. It is a traditional Chinese medicine that is both food and medicine, and can be used in medicine and as a tea. It has the effects of regulating qi, strengthening the spleen, drying dampness, and resolving phlegm, and has a huge market prospect.

[0004] As a specialty variety of Jiangxi Province, Zhangtou Red Tangerine Peel has broad market prospects. However, there are currently no clear reports on the preparation method of its formula granules. Due to its properties, when preparing formula granules using conventional processes, the dry powder is highly viscous and easily absorbs moisture, leading to increased production costs and reduced powder collection efficiency. Summary of the Invention

[0005] The purpose of this invention is to provide a method for preparing camphor red tangerine peel formula granules, which can maximize the drying process in actual production, reduce the amount of process components, and achieve the highest output with the lowest loss.

[0006] To achieve this objective, the present invention adopts the following technical solution: In a first aspect, the present invention provides a method for preparing camphor-root red tangerine peel formula granules, comprising the following steps: S1: Take the red tangerine peel of camphor tree, add water and decoct to obtain the extract; S2: Concentrate the extract to obtain a clear paste; S3: Add the clear paste to the first excipient, mix well, and dry to obtain a dry paste powder; the first excipient includes beta-cyclodextrin and silicon dioxide; S4: mixing the dry powder with the second excipient, granulating to obtain the Zangtouhongchenpi formula granules.

[0007] Further, in step S3, the betadex added amount is 5.0-15.0wt% of Zangtouhongchenpi, and the silicon dioxide added amount is 0.5-5.0wt% of Zangtouhongchenpi.

[0008] Further, in step S4, the second excipient includes one or at least two of malt dextrin, starch, magnesium stearate, silicon dioxide, lactose, and betadex; and the second excipient added amount is 0.0-15.0wt% of Zangtouhongchenpi.

[0009] Further, in step S1, the decoction is performed twice, in the first decoction, the Zangtouhongchenpi is soaked with water, the water added amount is 6-15 times of the mass of Zangtouhongchenpi, after soaking for 10-60min, the decoction is performed for 10-90min and filtered; the filter residue is taken, water is added again, the second decoction is performed, and the filtrates are combined to obtain the extract.

[0010] Further, in step S1, the filtration uses a 100-300 mesh sieve.

[0011] Further, in step S2, the concentration conditions are: the concentration temperature is 40-80℃, and the concentration time is ≤12h. The relative density of the concentrated clear paste is 1.01-1.06, measured at 60℃.

[0012] Further, in step S3, the drying treatment includes at least one of reduced pressure drying, freeze drying, microwave drying, and spray drying. The dry paste powder obtained by drying can pass through an 80 mesh sieve.

[0013] In a second aspect, the application further provides a Zangtouhongchenpi formula granule prepared by the above preparation method.

[0014] Compared with the prior art, the application has the following beneficial effects: (1) The application provides a preparation method of Zangtouhongchenpi formula granules, which adds excipients betadex and silicon dioxide to the concentrated clear paste before drying. The two cooperate in the drying process, not only effectively improving the formability and fluidity of the formula granules, reducing the hygroscopicity, but also significantly improving the powder yield of the dry paste, thereby improving the overall product quality.

[0015] (2) The preparation method of camphor red tangerine peel formula granules provided by the present invention controls the amount of beta-cyclodextrin added to 5.0%~15.0% of the amount of medicinal slices added and the amount of silica added to 0.5%~5.0% during the drying process. This not only synergistically improves the powder yield of the dry extract, but also significantly improves the formability and flowability of the obtained formula granules.

[0016] (3) The preparation method of camphor red tangerine peel formula granules provided by the present invention is a method that was screened and confirmed after a large number of experiments and proposed for the first time for camphor red. Each process is simple and reasonable and can be effectively applied to large-scale production. Attached Figure Description

[0017] Figure 1 This is a schematic diagram of the preparation process structure of this invention patent. Detailed Implementation

[0018] The following embodiments are provided to better understand the present invention and are not intended to limit the preferred embodiments. They do not constitute a limitation on the content and scope of protection of the present invention. Any product that is the same as or similar to the present invention, derived by any person under the guidance of the present invention or by combining the features of the present invention with other prior art, falls within the scope of protection of the present invention. Where specific experimental steps or conditions are not specified in the embodiments, they can be performed according to the conventional experimental steps or conditions described in the literature in the art. Reagents or instruments used, unless otherwise specified, are all commercially available conventional reagent products.

[0019] The following examples are combined Figure 1 The solution of the present invention will be further described.

[0020] Example 1: Preparation of Camphor Red Tangerine Peel Formula Granules Step 1: Take 1 part by weight of camphor red tangerine peel slices, add 10 parts by weight of water to the camphor red tangerine peel slices, soak for 30 minutes, decoct and extract for 60 minutes, filter, and reserve the filtrate; add 8 parts by weight of water to the dregs after the first decoction, decoct and extract for 30 minutes, filter, and reserve the filtrate; combine the two filtrates, mix well, and obtain the extract, which is filtered through a 300-mesh sieve; Step 2: Concentrate under reduced pressure at a vacuum of -0.04 to -0.08 MPa and a concentration temperature of 40 to 80°C to obtain a clear extract with a relative density of 1.04 (measured at 60°C); Step 3: Add 10.4 wt% beta-cyclodextrin and 1.6 wt% silica to the clear extract, mix well, preheat and stir the clear extract to 70°C, and spray dry (inlet air temperature is 160~190°C, outlet air temperature is 80~110°C) to obtain dry extract powder. Step 4: Add 5 wt% of maltodextrin to the dry extract powder, place it in a mixer, mix for 20 minutes, and granulate using a dry granulation machine to obtain 14-40 mesh camphor red tangerine peel formula granules.

[0021] Example 2: Preparation of Camphor Red Tangerine Peel Formula Granules Step 1: Take 1 part by weight of camphor red tangerine peel slices, add 10 parts by weight of water to the camphor red tangerine peel slices, soak for 30 minutes, decoct and extract for 60 minutes, filter, and reserve the filtrate; add 8 parts by weight of water to the dregs after the first decoction, decoct and extract for 30 minutes, filter, and reserve the filtrate; combine the two filtrates, mix well, and obtain the extract, which is filtered through a 300-mesh sieve; Step 2: Concentrate under reduced pressure at a vacuum of -0.04 to -0.08 MPa and a concentration temperature of 40 to 80°C to obtain a clear extract with a relative density of 1.04 (measured at 60°C); Step 3: Add 7.8 wt% betacyclodextrin and 1.2 wt% silica to the clear extract, mix well, preheat and stir the clear extract to 70°C, and spray dry (inlet air temperature is 160~190°C, outlet air temperature is 80~110°C) to obtain dry extract powder. Step 4: Add 4 wt% of maltodextrin to the dry extract powder, place it in a mixer, mix for 20 minutes, and granulate using a dry granulation machine to obtain 14-40 mesh camphor red tangerine peel formula granules.

[0022] Example 3: Preparation of Camphor Red Tangerine Peel Formula Granules Step 1: Take 1 part by weight of camphor red tangerine peel slices, add 10 parts by weight of water to camphor red tangerine peel slices, soak for 30 minutes, decoct and extract for 60 minutes, filter, and reserve the filtrate; after the first decoction, add 8 parts by weight of water to the dregs of camphor red tangerine peel slices, decoct and extract for 30 minutes, filter, and reserve the filtrate; combine the two filtrates, mix well, and obtain the extract, which is filtered through a 300-mesh sieve; Step 2: Concentrate under reduced pressure at a vacuum of -0.04 to -0.08 MPa and a concentration temperature of 40 to 80°C to obtain a clear extract with a relative density of 1.04 (measured at 60°C); Step 3: Add 13wt% betacyclodextrin and 2wt% silica to the clear extract, mix well, preheat and stir the clear extract to 70℃, and spray dry (inlet air temperature 160~190℃, outlet air temperature 80~110℃) to obtain dry extract powder. Step 4: Add 11% of the amount of maltodextrin added to the dry extract powder, place it in a mixer, mix for 20 minutes, and granulate using a dry granulation machine to obtain 14-40 mesh camphor red tangerine peel formula granules.

[0023] Comparative Example 1 This comparative example provides a method for preparing camphor red tangerine peel formula granules, which is basically the same as that in Example 1. The only difference is that in step 3, no excipients are added to the clear paste before spray drying. All other processes are the same as in Example 1.

[0024] Comparative Example 2 This comparative example provides a method for preparing camphor red tangerine peel formula granules, which is basically the same as that in Example 1, except that in step 3, 12wt% betacyclodextrin is added to the clear paste before spray drying. The rest of the process is the same as in Example 1.

[0025] Experimental Example 1: Investigation of Spray Drying Performance In Examples 1-3 and Comparative Examples 1-2 above, the process conditions during spray drying were examined, and the powder recovery rate (%) after spray drying was calculated according to the following formula: Powder recovery rate = weight of dry powder (g) / (weight of solids in the clear paste (g) + weight of excipients added before drying (g)) × 100%. Results: The dry powder obtained in Examples 1-3 showed no obvious wall adhesion phenomenon, and all could be collected as loose dry powder with a recovery rate greater than 95%, and all could pass through an 80-mesh sieve. The dry powder obtained in Comparative Example 1 showed severe wall adhesion, and the collected dry powder was relatively compact, with a recovery rate of less than 40%. The dry powder obtained in Comparative Example 2 showed wall adhesion phenomenon, and the collected dry powder was relatively loose, with a recovery rate of less than 80%. This indicates that the spray drying process of the present invention has excellent process performance for drying the materials of the present invention.

[0026] Experimental Example 2: Investigation of Granulation Process In Examples 1-3 above, the process conditions during granulation were examined. The results showed that all batches of granules had moderate hardness, uniform size, and no color difference. The material formed strips and did not stick to the rollers during granulation, indicating that the granulation process of the present invention has good performance when used to granulate the material of the present invention.

[0027] Experimental Example 3: Flowability Test of Formulation Particles The flowability of solid materials, especially granules, is usually characterized by the angle of repose. An angle of repose less than 40°, especially less than 35°, indicates excellent flowability, while an angle of repose greater than 40°, especially greater than 45°, indicates poor flowability. Good flowability of granules is generally beneficial for subsequent processing, such as repackaging.

[0028] The method for determining the angle of repose is as follows: Using the fixed funnel method, three funnels are connected in series and fixed, ensuring that the distance between the lower end of each funnel and the horizontally placed coordinate paper is 1 cm (H value). The sample is carefully poured along the funnel wall into the uppermost funnel until the tip of the sample cone formed on the coordinate paper touches the funnel opening. The diameter of the bottom of the cone (2R) is measured from the coordinate paper, and the radius (R) is calculated. This is performed five times, and the average value is calculated. The angle of repose tanα = H / R.

[0029] The angle of repose of the granules prepared according to the present invention was measured. The results showed that the angles of repose for Examples 1-3 were 32.3°, 31.0°, and 31.7°, respectively; the angle of repose for Comparative Example 1 was 47.6°; and the angle of repose for Comparative Example 2 was 38.9°. The flowability results indicated that the simultaneous addition of beta-cyclodextrin and silica before drying significantly improved the flowability of the granules. When neither was added or only one was added, the flowability of the granules was significantly lower than when both were added.

[0030] Experimental Example 4: Investigation of the hygroscopicity of the formulation granules The method for testing hygroscopicity is as follows: Take a dry, stoppered glass weighing bottle (outer diameter 50 mm, height 15 mm), and place it in a suitable constant temperature desiccator (with a saturated solution of ammonium chloride or ammonium sulfate at the bottom) or artificial climate chamber (temperature set at 25℃±1℃, relative humidity at 80%±2%) one day before the test, and accurately weigh it (m1). Take an appropriate amount of the test sample, spread it evenly in the weighing bottle, the thickness of the test sample is generally about 1 mm, and accurately weigh it (m2). Leave the weighing bottle open and place it under the above constant temperature and humidity conditions for 24 hours, along with the cap. Close the cap of the weighing bottle and accurately weigh it (m3). Hygroscopic rate = (m3-m2) / (m2-m1)×100%.

[0031] The hygroscopicity of the granules prepared according to this invention was determined. The results showed that the hygroscopic rates of Examples 1-3 were 26.9%, 26.6%, and 27.0%, respectively, while the hygroscopic rate of Comparative Example 1 was 35.1%, and the hygroscopic rate of Comparative Example 2 was 29.7%. The hygroscopicity results indicate that the type and nature of the excipients added or not added before drying have a significant impact on the hygroscopicity of the camphor red tangerine peel granules.

[0032] Based on the above results, the three types of particles in Examples 1-3 are significantly better than the particles in Comparative Examples 1-2 in terms of both flowability and hygroscopicity.

[0033] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these modifications and improvements all fall within the scope of protection of the present invention. Therefore, the scope of protection of this patent should be determined by the appended claims.

Claims

1. A method for preparing camphor-root red tangerine peel granules, characterized in that, Includes the following steps: S1: Take the red tangerine peel of camphor tree, add water and decoct to obtain the extract; S2: Concentrate the extract to obtain a clear paste; S3: Add the clear paste to the first excipient, mix well, and dry to obtain a dry paste powder; the first excipient includes beta-cyclodextrin and silicon dioxide; S4: Mix the dry powder with the second excipient, granulate, and obtain camphor red tangerine peel formula granules.

2. The preparation method according to claim 1, characterized in that, In step S3, the amount of beta-cyclodextrin added is 5.0~15.0 wt% of the tangerine peel of camphor red, and the amount of silica added is 0.5~5.0 wt% of the tangerine peel of camphor red.

3. The preparation method according to claim 1, characterized in that, In step S4, the second excipient includes one or at least two of maltodextrin, starch, magnesium stearate, silicon dioxide, lactose, and betacyclodextrin; the amount of the second excipient added is 0.0~15.0 wt% of camphor red tangerine peel.

4. The preparation method according to claim 1, characterized in that, In step S1, the decoction is performed twice. During the first decoction, water is added to the camphor red tangerine peel for soaking. The amount of water added is 6-15 times the mass of the camphor red tangerine peel. After soaking for 10-60 minutes, the decoction is performed for 10-90 minutes and then filtered. The residue is collected, water is added again, and the decoction is performed a second time. The filtrates are combined to obtain the extract.

5. The preparation method according to claim 4, characterized in that, In step S1, a 100-300 mesh sieve is used for filtration.

6. The preparation method according to claim 1, characterized in that, In step S2, the concentration conditions are: concentration temperature 40-80℃, concentration time ≤12h; The relative density of the concentrated extract was 1.01~1.06, as determined at 60℃.

7. The preparation method according to claim 1, characterized in that, In step S3, the drying process includes at least one of vacuum drying, freeze drying, microwave drying, and spray drying. The dried powder obtained can pass through an 80-mesh sieve.

8. A formula granule containing camphor-headed red tangerine peel, characterized in that, It is prepared by any one of the preparation methods described in claims 1-7.

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