Preparation method of radix angelicae formula granules

Abstract

The invention relates to a preparation method of traditional Chinese medicine formula granules, in particular to a preparation method of angelica dahurica formula granules, which comprises the steps of water extraction, concentration, drying and preparation, the preparation method of the angelica dahurica formula granules comprises the steps of selecting and summarizing results for multiple times and multiple groups of experimental data, and determining the content of the angelica dahurica formula granules by repeatedly extracting and measuring the experimental data results for multiple times. After an optimal result is obtained, the influence of different dosages of beta cyclodextrin on the imperatorin extraction amount is measured, an optimal comparison test result is imported into different proportion data experiments, and an optimal proportion result is obtained by adopting a mode of selecting optimal from multiple components, so that the extraction efficiency of imperatorin is improved to the greatest extent, and the cost in the production process is reduced.

Description

Technical Field

[0001] The invention relates to a method for preparing Chinese medicine formula granules, and particularly to a method for preparing angelica root formula granules. Background Art

[0002] The process of Chinese medicine formula granules is water extraction, concentration, drying and preparation. The preparation mainly considers the powder forming. The steps that have a greater impact on the main ingredients in the formula granules are extraction, concentration and drying. Many ingredients in Chinese medicine are difficult to dissolve in water, or are unstable and easy to decompose, resulting in the content of the main ingredients of the prepared Chinese medicine formula granules not meeting the national standards.

[0003] For some components, the ordinary water reflux extraction method cannot meet the sample quality requirements, so a more flexible method can be used to protect the unstable components. Conventional experimental ideas usually consider adding excipients during the concentration and drying process after extraction. In order to maintain the full extraction process, the addition of new solutes to affect the dissolution is avoided. Adding excipients or other components during the extraction of traditional Chinese medicine may have an impact on it. Specifically: excipients may affect the stability of traditional Chinese medicine preparations. For example, some excipients can interact with traditional Chinese medicine raw materials, affecting the bioavailability of traditional Chinese medicine preparations (dissolution of active ingredients), and thus affecting their efficacy. The selection and addition of excipients may also affect the quality and efficacy of traditional Chinese medicine preparations. For example, adhesives and lubricants are indispensable excipients in traditional Chinese medicine preparations, but excessive addition may affect the release rate of traditional Chinese medicine ingredients, thereby affecting the efficacy of traditional Chinese medicine preparations. Therefore, in the process of traditional Chinese medicine extraction, it is very important to select appropriate excipients and control their addition amount.

[0004] β-cyclodextrin is used as a pharmaceutical excipient to increase the stability of drugs, prevent drug oxidation and decomposition, and can be used to improve the solubility and bioavailability of drugs. It is a good stabilizer. It can also be prepared into inclusion complexes with some drug molecules that are not biocompatible, which not only increases the biocompatibility of drugs, but also plays a role in sustained release. It can protect the ingredients in the drug preparation process. [1] Liang Mingjin, Yang Guangde, He Langchong. Study on the extraction method of imperatorin from Angelica dahurica [J]. Chinese Patent Medicine, 2000(012):022.

[0005] Patent No. 202211440060.6 provides a method for preparing Angelica dahurica formula granules, the main feature of which is that the extraction is carried out in three steps, 2% of β-cyclodextrin is added during the drying process, and up to 38% of β-cyclodextrin is added during the granulation process.

[0006] Different dosages and times of use of β-cyclodextrin can produce different experimental results under the same experimental environment. The technology of the above patent is achievable, but it is not optimal in an industrial environment. In an industrial environment, any improvement in efficiency or reduction in input is a major breakthrough. Only efficiency close to the optimal one is suitable for industrial production. Summary of the invention

[0007] The purpose of the present invention is to provide a preparation method of Angelica dahurica formula granules, which can use an extraction process that maximizes the results in the actual production process to reduce industrial production costs and achieve the highest output with the lowest loss.

[0008] To achieve the above purpose, the present invention provides a method for preparing angelica root formula granules, which comprises weighing angelica root slices, crushing them, putting them into an extraction tank, adding appropriate amount of auxiliary materials, adding 80 degrees Celsius drinking water for warm soaking and extraction for 2 times; adding 3% beta-cyclodextrin of the slice feeding amount, adding 8 times of water, and extracting for 0.5 hours for the first time; adding 2% beta-cyclodextrin of the slice feeding amount, adding 6 times of water, and extracting for 0.5 hours for the second time. The medicinal liquid is filtered through 200 mesh, and the filtrate is reserved for use, the filtrate is taken, and the relative density is 1.06-1.11 under reduced pressure at a temperature below 70 degrees Celsius to obtain a clear paste for use, the clear paste is taken, vacuum dried, crushed, and a dry paste powder is obtained for use, the dry paste powder and an appropriate amount of dextrin are taken, mixed evenly, dry granulated, and granulated to obtain granules.

[0009] Beneficial effects: The preparation method of the angelica root formula granules of the present invention is the result of the optimization summary of multiple experimental data. We pre-add β-cyclodextrin during the extraction process to improve the dissolution of the effective ingredient and reduce the impact of high temperature on the content of the effective ingredient imperatorin during the extraction process. In addition, our extraction time is shorter and the amount of water added is less, which can greatly save production costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0010] The present invention is further described below in conjunction with the accompanying drawings and embodiments;

[0011] Figure 1 It is a schematic diagram of the preparation process structure of the patent of the present invention;

[0012] Figure 2 This is the characteristic spectrum of the Angelica dahurica formula granules in Example 1 of the present invention;

[0013] Figure 3 It is a comparison of different β-cyclodextrin input amounts and imperatorin extraction results in the experimental group 1 of the present invention;

[0014] Figure 4 It is the comparison of different water addition multiples and the extraction results of imperatorin in the experimental group 2 of the present invention;

[0015] Figure 5 It is a comparison of the extraction results of imperatorin with different extraction times in the experimental group 3 of the present invention. DETAILED DESCRIPTION

[0016] This section will describe in detail the specific embodiments of the present invention. The preferred embodiments of the present invention are shown in the accompanying drawings. The purpose of the accompanying drawings is to supplement the description of the text part of the specification with graphics, so that people can intuitively and vividly understand each technical feature and the overall technical solution of the present invention, but it cannot be understood as a limitation on the scope of protection of the present invention.

[0017] Weigh the Angelica dahurica slices from different origins, crush them, put them into the extraction tank, extract them using different extraction methods, and divide them into several groups according to the table below for extraction process research.

[0018] Table 1: Extraction process research, where the amount of β-cyclodextrin added is the percentage of the amount of medicinal pieces.

[0019]

[0020]

[0021] Table 2: Concentration process research, where the amount of β-cyclodextrin added is a percentage of the amount of medicinal pieces.

[0022]

[0023] Table 3: Process research content detection data.

[0024]

[0025]

[0026] Table 3.1: Comparison table of different β-cyclodextrin input amounts and imperatorin extraction results in experimental group 1.

[0027]

[0028] Table 3.2: Comparison of different water addition multiples and the extraction results of imperatorin in experimental group 2.

[0029]

[0030] Table 3.3 Comparison of different extraction times and extraction results of imperatorin in experimental group 3

[0031]

[0032]

[0033] Among the three control experimental groups in Tables 3.1 to 3.3 above, control groups 1 to 3 are the effects of the amount of β-cyclodextrin added before extraction from 100 grams of herbal medicine, the multiple of water added and the extraction time on the extraction results of imperatorin. The experimental results show that the extraction time of 1 hour is the best, and the imperatorin content shows a decreasing trend after more than 1.2 hours; the water content is 14 to 15 times the best; and the amount of β-cyclodextrin added before concentration is 5% The best.

[0034] Example 1: Preparation of Angelica dahurica Formula Granules (1)

[0035] Weigh the Angelica dahurica slices, crush them, put them into the extraction tank, add appropriate amount of auxiliary materials, add 80 degrees Celsius drinking water for warm soaking and extraction twice; add 3% beta-cyclodextrin of the slice feed amount, add 8 times the amount of water, and extract for 0.5 hours for the first time; add 2% beta-cyclodextrin of the slice feed amount, add 6 times the amount of water, and extract for 0.5 hours for the second time. Filter the liquid with 200 mesh, and use the filtrate for later use.

[0036] Take the filtrate and concentrate it under reduced pressure at a temperature below 70 degrees Celsius to a relative density of 1.06-1.11 to obtain a clear paste for later use.

[0037] Take the clear paste, vacuum dry it, crush it to get dry paste powder, and set aside.

[0038] Take the dry paste powder and appropriate amount of dextrin, mix them evenly, granulate them by dry method, and granulate them to obtain granules.

[0039] The test data are as follows: Table 4 Decoction content test data

[0040] batch number Moisture (%) Imperatorin content (%) BZ-YP210702 11.0 0.242 BZ-YP210704 10.9 0.303 BZ-YP210706 8.8 0.217 BZ-YP210708 10.6 0.262 BZ-YP210709 11.1 0.257

[0041] Table 5 Process research content test data

[0042]

[0043] The national standard for Angelica dahurica formula granules stipulates: 1. Specification: Each 1g of formula granules is equivalent to 3g of decoction pieces; 2. Content: Each 1g of granules of this product contains imperatorin (C 16 H 14 O4) should be 0.25mg~1.20mg.

[0044] It can be seen from Tables 4 and 5 that the imperatorin transfer rate is good and the content of the granule sample meets the standard. This example is the final method.

[0045] Example 2: Preparation of Angelica Dahurica Formula Granules (2)

[0046] Weigh the Angelica dahurica slices, crush them, put them into the extraction tank, add appropriate amount of auxiliary materials, add 75 degrees Celsius drinking water for warm soaking and extraction twice; add 2% beta-cyclodextrin of the slice feed amount, add 8 times the amount of water, and extract for 0.5 hours for the first time; add 2% beta-cyclodextrin of the slice feed amount, add 6 times the amount of water, and extract for 0.5 hours for the second time. Filter the liquid with 200 mesh, and use the filtrate for later use.

[0047] Take the filtrate and concentrate it under reduced pressure at a temperature below 70 degrees Celsius to a relative density of 1.06-1.11 to obtain a clear paste for later use.

[0048] Take the clear paste, vacuum dry it, crush it to get dry paste powder, and set aside.

[0049] Take the dry paste powder and appropriate amount of dextrin, mix them evenly, granulate them by dry method, and granulate them to obtain granules.

[0050] The test data are as follows: Table 6 Process research content test data

[0051]

[0052]

[0053] As shown in Table 6, the transfer rate of imperatorin is good and the content of the granule sample meets the standard.

[0054] Example 3: Preparation of Angelica Dahurica Formula Granules (3)

[0055] Weigh the slices of Angelica dahurica, crush them, put them into an extraction tank, add appropriate amount of auxiliary materials, add 85 degrees Celsius drinking water for warm soaking and extraction twice; add 2% beta-cyclodextrin of the slice feed amount, add 8 times the amount of water, and extract for 0.5 hours for the first time; add 2% beta-cyclodextrin of the slice feed amount, add 6 times the amount of water, and extract for 0.5 hours for the second time. Filter the liquid with 200 mesh, and use the filtrate for later use.

[0056] Take the filtrate and concentrate it under reduced pressure at a temperature below 70 degrees Celsius to a relative density of 1.06-1.11 to obtain a clear paste for later use.

[0057] Take the clear paste, vacuum dry it, crush it to get dry paste powder, and set aside.

[0058] Take the dry paste powder and appropriate amount of dextrin, mix them evenly, granulate them by dry method, and granulate them to obtain granules.

[0059] The test data are as follows: Table 7 Process research content test data

[0060]

[0061] As shown in Table 7, the transfer rate of imperatorin is good and the content of the granule sample meets the standard.

[0062] Example 4: Preparation of Angelica Dahurica Formula Granules (4)

[0063] Weigh the Angelica dahurica slices, crush them, put them into the extraction tank, add appropriate amount of auxiliary materials, add 80 degrees Celsius drinking water for warm soaking and extraction twice; add 3% beta-cyclodextrin of the slice feed amount, add 8 times the amount of water, extract for 1 hour; add 2% beta-cyclodextrin of the slice feed amount, add 6 times the amount of water, extract for 1 hour. Filter the liquid through 200 mesh, and use the filtrate for later use.

[0064] Take the filtrate and concentrate it under reduced pressure at a temperature below 70 degrees Celsius to a relative density of 1.06-1.11 to obtain a clear paste for later use.

[0065] Take the clear paste, vacuum dry it, crush it to get dry paste powder, and set aside.

[0066] Take the dry paste powder and appropriate amount of dextrin, mix them evenly, granulate them by dry method, and granulate them to obtain granules.

[0067] The test data are as follows: Table 8 Process research content test data

[0068]

[0069] As can be seen from the above table, the transfer rate of imperatorin is good and the content of the granule sample meets the standard.

[0070] Example 5: Preparation of Angelica Dahurica Formula Granules (5)

[0071] Weigh the Angelica dahurica slices, crush them, put them into the extraction tank, add appropriate amount of auxiliary materials, add 80 degrees Celsius drinking water for warm soaking and extraction twice; add 3% beta-cyclodextrin of the slice feed amount, add 10 times the amount of water, and extract for 0.5 hours; add 2% beta-cyclodextrin of the slice feed amount, add 8 times the amount of water, and extract for 0.5 hours. Filter the liquid through 200 mesh, and use the filtrate for later use.

[0072] Take the filtrate and concentrate it under reduced pressure at a temperature below 70 degrees Celsius to a relative density of 1.06-1.11 to obtain a clear paste for later use.

[0073] Take the clear paste, vacuum dry it, crush it to get dry paste powder, and set aside.

[0074] Take the dry paste powder and appropriate amount of dextrin, mix them evenly, granulate them by dry method, and granulate them to obtain granules.

[0075] The test data are as follows: Table 9 Process research content test data

[0076]

[0077]

[0078] As shown in Table 9, the imperatorin transfer rate is good and the content of the granule sample meets the standard. Comparative Example 1: Preparation method of Angelica dahurica formula granules (1)

[0079] Weigh the Angelica dahurica slices, put them into an extraction tank, add drinking water and extract twice at normal pressure and slightly boil; add 8 times the amount of water for the first time and extract for 1.5 hours; add 6 times the amount of water for the second time and extract for 1 hour. Filter the liquid through 200 mesh and keep the filtrate for later use.

[0080] Take the filtrate and concentrate it under reduced pressure at a temperature below 70 degrees Celsius to a relative density of 1.06-1.11 to obtain a clear paste for later use.

[0081] Take the clear paste, spray dry it to get dry paste powder, and set aside.

[0082] Take the dry paste powder and appropriate amount of dextrin, mix them evenly, granulate them by dry method, and granulate them to obtain granules.

[0083] The test data are as follows: Table 10 Process research content test data

[0084]

[0085] As shown in Table 10, the imperatorin transfer rate is low and the content of the granule sample does not meet the standard. Comparative Example 2: Preparation method of angelica root formula granules (2)

[0086] Weigh the Angelica dahurica slices, crush them, put them into an extraction tank, add appropriate amount of auxiliary materials, add drinking water and extract twice at normal pressure and slightly boil; add 5% beta-cyclodextrin of the slices for the first time, add 9 times the amount of water, extract for 1 hour; add 7 times the amount of water for the second time, extract for 0.5 hour. Filter the liquid through 200 mesh, and keep the filtrate for later use.

[0087] Take the filtrate and concentrate it under reduced pressure at a temperature below 70 degrees Celsius to a relative density of 1.06-1.11 to obtain a clear paste for later use.

[0088] Take the clear paste, spray dry it to get dry paste powder, and set aside.

[0089] Take the dry paste powder and appropriate amount of dextrin, mix them evenly, granulate them by dry method, and granulate them to obtain granules.

[0090] The test data are as follows: Table 11 Process research content test data

[0091]

[0092] From the above table, we can see that the imperatorin transfer rate is low and the content of the granule sample does not meet the standard.

[0093] Weigh the Angelica dahurica slices, crush them, put them into the extraction tank, and divide them into several groups according to the table below for extraction process research.

[0094] The conditions and relevant data of each group are as follows: Table 12 Extraction process research

[0095]

[0096]

[0097] Note: The total amount of β-cyclodextrin added for one extraction is 5g. The total amount of β-cyclodextrin added for two extractions is 3g for the first extraction, accounting for 3% of the total amount of the raw materials, and 2g for the second extraction, accounting for 2% of the total amount of the raw materials.

[0098] As shown in Table 12, the imperatorin transfer rate in Group 4 was higher, while the imperatorin transfer rates in the other four groups were lower.

[0099] It can be seen from the test data of Tables 1 to 12 and control experimental groups 1 to 3 that the optimal embodiment of the present invention is: 80 degrees Celsius warm immersion extraction twice, 3% β-cyclodextrin is added to the slices before the first extraction, and the extraction is performed for 0.5 hour; 2% β-cyclodextrin is added to the slices before the second extraction, and the extraction is performed for 0.5 hour. The transfer rate of imperatorin content is higher than that of continuous countercurrent extraction for 1 hour in the comparative document, 7% β-cyclodextrin is added to the slices before concentration.

[0100] The embodiments of the present invention are described in detail above in conjunction with the accompanying drawings and the appended tables. Compared with the preparation method of the Angelica dahurica formula granules provided by Patent No. 202211440060.6, the usage and dosage of cyclodextrin in the patent of the present invention are essentially different. The experimental data from Tables 1 to 12 can prove that in the implementation mode of the patent of the present invention, the extraction amount of imperatorin is essentially improved compared with the prior art and the technology in the comparative patent.

[0101] However, the present invention is not limited to the above embodiments, and various changes can be made within the knowledge scope of ordinary technicians in the technical field without departing from the purpose of the present invention.

Claims

1. A method for preparing angelica root granules, characterized in that The preparation method is divided into the following steps: 1) Water extraction, weigh the Angelica dahurica slices, crush them, put them into an extraction tank, add appropriate amount of auxiliary materials, add 80 degrees Celsius drinking water for warm soaking extraction twice, the auxiliary material is β-cyclodextrin, in the two warm soaking extraction processes, add 3% of the slice feed amount of β-cyclodextrin for the first time, add 8 times the amount of water, extract for 0.5 hours, add 2% of the slice feed amount of β-cyclodextrin for the second time, add 6 times the amount of water, extract for 0.5 hours, filter the liquid through 200 mesh, and use the filtrate for later use; 2) Concentrating, taking the filtrate, concentrating it under reduced pressure at a temperature below 70 degrees Celsius to a relative density of 1.06 to 1.11 to obtain a clear paste for later use; 3) Drying: taking the clear paste, vacuum drying, and crushing to obtain dry paste powder for later use; 4) Preparation: take the dry paste powder and an appropriate amount of dextrin, mix them evenly, dry granulate them, and granulate them to obtain granules.

2. The method for preparing the Angelica dahurica formula granules according to claim 1, characterized in that: During extraction, first add the medicinal materials, then add 5% of the decoction amount of β-cyclodextrin, and then add water at 70 to 80 degrees Celsius.

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