Equisetum formula granules, preparation method and optimization method

Abstract

The invention relates to the technical field of traditional Chinese medicine formula granules, in particular to a horsetail formula granule, a preparation method and an optimization method. The preparation method comprises the following steps: sequentially processing, decocting and extracting, concentrating, drying and granulating raw medicinal materials of equisetum hiemale, so as to obtain the equisetum hiemale formula granules. Wherein the decocting and extracting step comprises the following steps: putting processed equisetum hiemale decoction pieces into an extracting tank, and soaking at the soaking temperature of 40 to 80 DEG C for 0.5 to 1.5 hours; sequentially carrying out extraction for three times, and merging the extracting solutions obtained by each extraction to obtain a horsetail filtrate; wherein during each extraction, the water adding amount in the extraction tank is 8-15 times of the weight of the raw medicinal material of the equisetum hiemale, and the time of each extraction is 0.5-1.5 h. The quality of the equisetum formula granule product can be improved.

Description

Technical Field

[0001] The present invention relates to the technical field of traditional Chinese medicine formula granules, in particular to horsetail formula granules, a preparation method and an optimization method. Background Art

[0002] Equisetum equisetum is derived from the dried aerial parts of Equisetum hyemale L., a plant of the Equisetaceae family. Equisetum equisetum formula granules are made from the dried aerial parts of Equisetum equisetum, processed according to the key quality standards of standard decoctions. It has a sweet, bitter, and neutral nature and enters the Lung and Liver meridians. It has the effects of dispersing wind-heat, removing eye opacities, and stopping bleeding. It is used for symptoms such as red eyes caused by wind-heat and tearing in response to wind.

[0003] Currently, horsetail granules are made from the raw horsetail herb, processed, extracted, concentrated, dried, and granulated. The standard for horsetail granules (YBZ-PFKL-2022041) only briefly describes the preparation process under the "method of preparation," which is of little use in guiding production. Therefore, research and optimization of the preparation process for horsetail granules is needed to ensure that they meet quality standards and to control the stability of their quality. Summary of the Invention

[0004] In view of the above problems, the present invention is proposed to provide an horsetail formula granule, a preparation method and an optimization method that overcome the above problems or at least partially solve the above problems, and can improve the quality of the horsetail formula granule product.

[0005] Specifically, the present invention provides a method for preparing horsetail formula granules, comprising: sequentially processing horsetail raw medicinal materials, decocting and extracting, concentrating, drying and granulating to obtain horsetail formula granules;

[0006] Wherein, the decoction and extraction step comprises:

[0007] The processed Equisetum arvense slices are placed in an extraction tank for soaking, wherein the soaking temperature is 40 to 80° C. and the soaking time is 0.5 to 1.5 h;

[0008] The extractions are performed three times in sequence, and the extracts obtained from each extraction are combined and filtered to obtain horsetail filtrate; wherein, during each extraction, the amount of water added to the extraction tank is 8 to 15 times the weight of the horsetail slices, and the time for each extraction is 0.5 to 1.5 hours.

[0009] Optionally, in the decoction extraction step:

[0010] The soaking temperature is 60°C and the soaking time is 1.5 hours; and / or

[0011] Each extraction time is 0.5h; and / or

[0012] During the first extraction, the amount of water added to the extraction tank is 15 times the weight of the Equisetum arvense slices; and / or

[0013] During the second extraction, the amount of water added to the extraction tank is 12 times the weight of the Equisetum arvense slices; and / or

[0014] During the third extraction, the amount of water added to the extraction tank is 12 times the weight of the horsetail slices.

[0015] Optionally, the concentration step comprises: concentrating the horsetail filtrate to obtain a concentrated ointment; wherein the steam pressure does not exceed 0.12 MPa, the vacuum degree is -0.03 to -0.09 MPa, the concentration temperature is 50 to 85° C., and the relative density of the concentrated ointment at 60 to 70° C. is 1.01 to 1.10; and / or

[0016] The drying step comprises: spray drying the concentrated ointment to obtain a dry ointment powder; wherein the air inlet temperature is 160 to 170°C, the air outlet temperature is 90 to 105°C, and the liquid inlet frequency is 10.0 to 25.0 Hz; and / or

[0017] The granulation step comprises: taking the dry paste powder and dry-pressing granules to obtain horsetail formula granules; wherein the granulation adopts a dry pressing granulation method, the mesh number of the granulator screen is 12 mesh, the mesh number of the granulation screen is 10 mesh and 40 mesh, the feeding speed is 20 to 230 r / min, the pressing wheel speed is 3 to 40 r / min, and the granulation speed is 20 to 230 r / min; during the granulation process, the weight ratio of the dry paste powder to dextrin is 1:0 to 1:0.8, and the amount of dextrin used is ≤8% of the input amount of the original medicinal material of horsetail.

[0018] Another aspect of the present invention provides an Equisetum formula granule, which is prepared by any one of the preparation methods described above.

[0019] Another aspect of the present invention also provides a process optimization method for horsetail formula granules, comprising: taking the comprehensive weighted score of kaempferol content, kaempferol-3-O-β-D-sophoroside content, and paste yield as evaluation indicators, using L9(3 4 ) Orthogonal experiment was conducted to optimize the process of horsetail formula granules and conduct process verification by taking the soaking time, soaking temperature, extraction time and water addition ratio in the decoction extraction process as the investigation factors.

[0020] Optionally, the calculation formula of the comprehensive weighted score is: comprehensive score = (cream yield / maximum cream yield) × 20% + (kaempferol content / maximum kaempferol content) × 40% + (kaempferol-3-O-β-D-sophoroside content) / maximum kaempferol-3-O-β-D-sophoroside content) × 40%;

[0021] Among them, the maximum value of the paste yield, the maximum value of the kaempferol content, and the maximum value of the kaempferol-3-O-β-D-sophoroside content in the orthogonal test results are taken as the maximum paste yield, the maximum kaempferol content, and the maximum kaempferol-3-O-β-D-sophoroside content, respectively.

[0022] Optionally, the optimal extraction process parameters obtained through process verification include:

[0023] The soaking temperature is 60℃ and the soaking time is 1.5h;

[0024] Add water and boil and extract three times, the extraction time for each extraction is 0.5h;

[0025] During the first extraction, the amount of water added to the extraction tank is 15 times the weight of the horsetail slices;

[0026] During the second and third extractions, the amount of water added to the extraction tank is 12 times the weight of the horsetail slices.

[0027] Beneficial effects of the present invention:

[0028] In the method for preparing horsetail formula granules of the present invention, the raw horsetail medicinal material is sequentially processed, decocted, extracted, concentrated, dried, and granulated to obtain the horsetail formula granules. The decoction extraction process involves soaking the raw material first, followed by three extractions, and reasonable process parameters are selected. This method can fully extract the kaempferol content and kaempferol-3-O-β-D-sophoroside components from the raw horsetail medicinal material, while also achieving a high paste yield, thereby resulting in high-quality horsetail formula granules.

[0029] Furthermore, the optimization method of the present invention can be used to optimize the extraction process parameters, thereby better guiding the production of horsetail formula granules, so that the horsetail formula granule products have higher quality.

[0030] Based on the following detailed description of specific embodiments of the present invention in conjunction with the accompanying drawings, those skilled in the art will become more aware of the above and other objects, advantages and features of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Hereinafter, some specific embodiments of the present invention will be described in detail in an exemplary and non-limiting manner with reference to the accompanying drawings. The same reference numerals in the accompanying drawings indicate the same or similar components or parts. It should be understood by those skilled in the art that these drawings are not necessarily drawn to scale. In the accompanying drawings:

[0032] Figure 1 1 is a schematic flow chart of a method for preparing horsetail formula granules according to one embodiment of the present invention. DETAILED DESCRIPTION

[0033] Refer to the following Figure 1 To describe an horsetail formula granule, preparation method and optimization method of an embodiment of the present invention. In the description of this embodiment, it should be understood that the terms "first" and "second" are used for descriptive purposes only, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, the features defined as "first" and "second" may explicitly or implicitly include at least one of the features, that is, include one or more of the features. In the description of the present invention, the meaning of "plurality" is at least two, such as two, three, etc., unless otherwise clearly and specifically defined. When a feature "includes or contains" one or some of the features it covers, unless otherwise specifically described, this indicates that other features are not excluded and may further include other features.

[0034] In the description of the present embodiment, reference to the terms "one embodiment," "some embodiments," "illustrative embodiments," "example," "specific example," or "some examples" means that the specific features, structures, materials, or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the exemplary expressions of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials, or characteristics described may be combined in any appropriate manner in any one or more embodiments or examples.

[0035] An embodiment of the present invention provides a method for preparing horsetail formula granules, which comprises sequentially processing, decocting and extracting, concentrating, drying and granulating horsetail raw medicinal materials to obtain horsetail formula granules.

[0036] Wherein, the decoction and extraction step comprises:

[0037] The processed Equisetum arvense slices are placed in an extraction tank for soaking, wherein the soaking temperature is 40 to 80° C. and the soaking time is 0.5 to 1.5 h;

[0038] The extractions are performed three times in sequence, and the extracts obtained from each extraction are combined and filtered to obtain an horsetail filtrate; wherein, during each extraction, the amount of water added to the extraction tank is 8 to 15 times (for example, 8 times, 9 times, 10 times, 11 times, 12 times, 13 times, 14 times or 15 times) the weight of the horsetail slices, and the time for each extraction is 0.5 to 1.5 hours (for example, 0.5 hours, 0.8 hours, 1.0 hours, 1.2 hours, 1.4 hours or 1.5 hours).

[0039] In this example, the raw material of horsetail was subjected to the steps of processing, decoction extraction, concentration, drying, and granulation to produce horsetail formula granules. The decoction extraction process involved soaking first, followed by three extractions, and reasonable process parameters were selected. This method allows for the full extraction of the active ingredients from the raw material of horsetail, resulting in a high paste yield and, consequently, a high-quality horsetail formula granule product.

[0040] In some optional embodiments of the present invention, in the decoction extraction step: the soaking temperature is 60° C., and the soaking time is 1.5 h.

[0041] In some optional embodiments of the present invention, in the decoction extraction step: the time for each extraction is 0.5 h.

[0042] In some optional embodiments of the present invention, in the decoction extraction step: during the first extraction, the amount of water added to the extraction tank is 15 times the weight of the Equisetum arvense slices.

[0043] In some optional embodiments of the present invention, in the decoction extraction step: during the second extraction, the amount of water added to the extraction tank is 12 times the weight of the Equisetum arvense slices.

[0044] In some optional embodiments of the present invention, in the decoction extraction step: during the third extraction, the amount of water added to the extraction tank is 12 times the weight of the Equisetum arvense slices.

[0045] In some optional embodiments of the present invention, the concentration step includes: concentrating the horsetail filtrate to obtain a concentrated ointment; wherein, the steam pressure of the concentration process is controlled to be no more than 0.12 MPa, the vacuum degree is -0.03 to -0.09 MPa (for example: -0.03 MPa, -0.05 MPa, -0.06 MPa, -0.07 MPa, -0.08 MPa, -0.09 MPa), the concentration temperature is 50 to 85°C (for example: 50°C, 60°C, 70°C, 80°C or 85°C), and the relative density of the concentrated ointment at 60 to 70°C is 1.01 to 1.10 (for example: 1.01, 1.03, 1.05, 1.07, 1.09 or 1.10).

[0046] In this embodiment, the concentrated ointment can also be called an extract. In the process of preparing the extract, steam pressure, concentration temperature and relative density (specific gravity) are three core parameters that have an important impact on the quality and production efficiency of the extract.

[0047] Steam pressure refers to the pressure of steam generated by a steam generator or steam boiler during the concentration process. Steam pressure directly affects steam temperature and heat transfer efficiency. Generally speaking, higher steam pressure leads to higher steam temperature and greater heat transfer efficiency, which accelerates the concentration of the extract. However, excessively high steam pressure may also destroy or volatilize certain components in the extract. This embodiment selects an appropriate steam pressure based on the extract's composition, properties, and concentration requirements, thereby ensuring the safe operation of the steam generator and steam piping and avoiding safety hazards such as overpressure.

[0048] Concentration temperature refers to the temperature environment in which the extract is exposed during the concentration process. The concentration temperature directly affects the evaporation rate of water in the extract and the viscosity of the extract. Generally speaking, the higher the concentration temperature, the faster the evaporation rate and the higher the viscosity of the extract. However, excessively high concentration temperatures may destroy certain components in the extract or cause adverse reactions. This embodiment sets an appropriate concentration temperature based on the extract's composition, properties, and concentration requirements. This ensures the accuracy and stability of the heating equipment and temperature control system, and prevents temperature fluctuations from affecting the quality of the ointment.

[0049] Relative density refers to the ratio of the density of an extract to the density of water and is commonly used to measure the viscosity and concentration of an extract. Generally speaking, the higher the relative density, the higher the viscosity and better the stability of the extract. However, excessively high relative density may make the extract difficult to apply or absorb. This embodiment, by setting a reasonable relative density, can ensure the texture, stability, and performance of the extract.

[0050] Therefore, by setting reasonable concentration process parameters, this embodiment can not only obtain high-quality extracts, but also have high production efficiency, and can also ensure the accuracy, stability and safety of production equipment.

[0051] In some optional embodiments of the present invention, the drying step includes: taking the concentrated ointment and spray drying it to obtain a dry ointment powder; wherein, the drying is carried out using a spray drying tower, and the inlet air temperature is controlled to be 160 to 170°C (for example: 160°C, 163°C, 165°C, 168°C or 160°C), the outlet air temperature is 90 to 105°C (for example: 90°C, 95°C, 98°C, 100°C, 103°C or 105°C), and the liquid inlet frequency is 10.0 to 25.0Hz (for example: 10.0Hz, 15.0Hz, 18.0Hz, 10.0Hz, 13.0Hz or 25.0Hz).

[0052] In this embodiment, the inlet air temperature refers to the temperature of the hot air flow entering the drying tower, which directly affects the heat absorbed by the droplets and the rate of water evaporation. Setting the inlet air temperature to 160 to 170°C achieves a higher water evaporation rate without damaging the active ingredients in the product. The outlet air temperature determines the final state of the dried paste powder. Excessively high outlet air temperatures may cause the product to char, melt, or decompose, while excessively low outlet air temperatures may leave the product semi-dry, causing it to stick or aggregate at the bottom of the drying chamber. To avoid the effects of excessively high or low outlet air temperatures on the dried paste powder, this embodiment sets the outlet air temperature to 90 to 105°C, resulting in higher-quality dried paste powder. The liquid inlet frequency refers to the rate at which the liquid is delivered to the spray drying tower, which determines the number and size of the droplets. Excessively fast liquid inlet rates may result in overly large droplets and incomplete drying; excessively slow liquid inlet rates may reduce production efficiency. In this embodiment, the liquid inlet frequency is set to 10.0 to 25.0 Hz to ensure uniform droplet size and effective drying.

[0053] Therefore, this embodiment is beneficial to controlling the preparation efficiency and quality of dry paste powder by setting reasonable drying process parameters.

[0054] In some optional embodiments of the present invention, the granulation step includes: taking the dry paste powder and dry-pressing granules to obtain horsetail formula granules; wherein the granulation adopts a dry pressing granulation method, the granulator screen mesh number is 12 mesh, the granulation screen mesh number is 10 mesh and 40 mesh, the feeding speed is 20 to 230 r / min (for example: 20 r / min, 50 r / min, 80 r / min, 100 r / min, 150 r / min, 200 r / min, 230 r / min), and the pressing wheel speed is 3 to 40 r / min. min (for example: 3 r / min, 10 r / min, 20 r / min, 30 r / min or 40 r / min), the granulation speed is 20 to 230 r / min (20 r / min, 50 r / min, 80 r / min, 100 r / min, 150 r / min, 200 r / min or 230 r / min); the weight ratio of dry paste powder to dextrin during the granulation process is 1:0 to 1:0.8, and the amount of dextrin is ≤8% of the feeding amount of the original medicinal material of Equisetum arvense.

[0055] In this embodiment, the granulation step is specifically as follows: the dry paste powder and dextrin are mixed evenly in a certain proportion, and the mixed material is added to the dry pressing granulator; the material is pressed into thin slices by adjusting the parameters such as the pressing wheel speed and the pressing wheel pressure; the thin slices are cut into particles through a crushing chamber; the particles are granulated by screens of different sizes to obtain formula particles that meet the requirements. The mesh size of the screen directly affects the size of the particles; the lower the mesh size, the larger the particles; the higher the mesh size, the finer the particles; this embodiment can obtain particles of reasonable size by setting a reasonable screen mesh size. The feed speed affects the rate at which the material enters the dry pressing granulator; the pressing wheel speed affects the pressure time and pressure distribution of the material in the roller bite area; this embodiment can ensure that the material can enter the pressing wheel area for pressing evenly and stably by setting a reasonable feed speed and pressing wheel speed. The ratio of dry paste powder to dextrin affects the formability, stability and solubility of the particles; this embodiment can ensure that the particles have good fluidity and disintegration by setting an appropriate ratio.

[0056] Therefore, this embodiment is beneficial to controlling the quality and yield of horsetail formula granules by setting reasonable granulation working parameters.

[0057] like Figure 1 As shown, a preferred embodiment of a method for preparing horsetail formula granules

[0058] The preparation method of the horsetail formula granules may comprise the following steps:

[0059] Preparation: Take the original medicinal material of Equisetum arvense, remove impurities, cut into 10-15mm segments, and obtain Equisetum arvense slices.

[0060] Decoction Extraction: Place the Equisetum slices in an extraction tank and soak at 60°C for 0.5 hours. Three extractions are then performed sequentially, and the resulting Equisetum extracts are combined and filtered to obtain the Equisetum filtrate. Each extraction lasts 0.5 hours. For the first extraction, add 15 times the weight of the Equisetum raw material to the extraction tank; for the second extraction, add 12 times the weight of the Equisetum raw material; and for the third extraction, add 12 times the weight of the Equisetum raw material.

[0061] Concentration: Concentrating the horsetail filtrate to produce a concentrated ointment; wherein the steam pressure does not exceed 0.12 MPa, the vacuum degree is -0.03 to -0.09 MPa, the concentration temperature is 50 to 85°C, and the relative density of the concentrated ointment at 60 to 70°C is 1.01 to 1.10;

[0062] Drying: spray drying the concentrated ointment to obtain dry ointment powder; wherein the air inlet temperature is 160 to 170°C, the air outlet temperature is 90 to 105°C, and the liquid feeding frequency is 10.0 to 25.0 Hz;

[0063] Granulation: The dry paste powder is dry-pressed and granulated to obtain horsetail formula granules; wherein, the granulation adopts a dry pressing granulation method, the granulator screen has a mesh size of 12 mesh, the granulation screen has a mesh size of 10 mesh and 40 mesh, the feeding speed is 20 to 230 r / min, the pressing wheel speed is 3 to 40 r / min, and the granulation speed is 20 to 230 r / min; during the granulation process, the weight ratio of the dry paste powder to dextrin is 1:0 to 1:0.8, and the amount of dextrin used is ≤8% of the feed amount of the original horsetail medicinal material.

[0064] The preparation method of this embodiment, by setting reasonable process parameters and process routes, can ensure that the prepared horsetail formula granule product has high quality and stability and meets national standards.

[0065] Another aspect of the embodiments of the present invention further provides an Equisetum formula granule, which is prepared by the preparation method described in any one of the above embodiments.

[0066] Another aspect of the present invention provides a process optimization method for horsetail formula granules, the process optimization method comprising: taking the comprehensive weighted score of kaempferol content, kaempferol-3-O-β-D-sophoroside content, and paste yield as evaluation indicators, using L9(3 4 ) Orthogonal experiment was conducted to optimize the process of horsetail formula granules and conduct process verification by taking the soaking time, soaking temperature, extraction time and water addition ratio in the decoction extraction process as the investigation factors.

[0067] The extraction process plays a crucial role in the preparation of horsetail granules. It directly impacts product quality and efficacy. Furthermore, preliminary experiments have determined that the primary factors influencing the yield and content of kaempferol and kaempferol-3-O-β-D-sophoroside are soaking time, soaking temperature, extraction time, and water addition ratio. Therefore, this example uses horsetail granules as the research subject, examining water extraction methods using different soaking times, soaking temperatures, extraction times, and water addition ratios, ultimately selecting the optimal extraction process suitable for industrial production. This not only ensures that horsetail granules meet national standards but also provides valuable guidance for the production process.

[0068] In some optional embodiments of the present invention, the calculation formula of the comprehensive weighted score is: comprehensive score = (cream yield / maximum cream yield) × 20% + (kaempferol content / maximum kaempferol content) × 40% + (kaempferol-3-O-β-D-sophoroside content) / maximum kaempferol-3-O-β-D-sophoroside content) × 40%.

[0069] Among them, the maximum value of the paste yield, the maximum value of the kaempferol content, and the maximum value of the kaempferol-3-O-β-D-sophoroside content in the orthogonal test results are taken as the maximum paste yield, the maximum kaempferol content, and the maximum kaempferol-3-O-β-D-sophoroside content, respectively.

[0070] The calculation formula of this embodiment can be used to quickly and accurately calculate the comprehensive weighted score. Moreover, the above calculation formula is reasonably set, which is conducive to obtaining the most preferred process parameters.

[0071] In some optional embodiments of the present invention, the optimal extraction process parameters obtained through process verification include: soaking temperature of 60°C, soaking time of 1.5h; decocting and extracting three times with each extraction time of 0.5h; during the first extraction, the amount of water added to the extraction tank is 15 times the weight of the horsetail slices; during the second and third extractions, the amount of water added to the extraction tank is 12 times the weight of the horsetail slices.

[0072] The process optimization method of the horsetail formula granules of the present invention is further described in detail below with reference to specific examples. Unless otherwise specified, the raw materials used in the following examples are all commercially available products.

[0073] Example 1

[0074] 1. Instruments and test drugs

[0075] 1.1 Instruments: Agilent 1260Ⅱ high performance liquid chromatograph; JA1203N analytical balance.

[0076] 1.2 Drug testing

[0077] Equisetum arvense (origin: Fusong, Jilin) ​​was authenticated as authentic by the Quality Control Department of Zhongjing Wanxi Pharmaceutical. Equisetum arvense reference material (Batch No. 320027-202311), kaempferol reference material (Batch No. 110861-202214), and kaempferol-3-O-β-D-sophoroside reference material (Batch No. 190183-202207) were purchased from the China Food and Drug Administration. Acetonitrile was chromatographic grade, and all other reagents were analytical grade.

[0078] 2. Methods and Results

[0079] 2.1 Experimental design

[0080] Through preliminary experiments, it was determined that the main factors affecting the paste yield and the contents of kaempferol and kaempferol-3-O-β-D-sophoroside were soaking time (factor A), soaking temperature (factor B), extraction time (factor C), and water addition ratio (factor D). The comprehensive index of the contents of kaempferol and kaempferol-3-O-β-D-sophoroside and paste yield under the [Content Determination] item of the standard for Chinese medicine formula granules of Equisetum arvense (YBZ-PFKL-2022041) [(paste yield / maximum paste yield) × 20% + (kaempferol content / maximum kaempferol content) × 40% + (kaempferol-3-O-β-D-sophoroside content) / maximum kaempferol-3-O-β-D-sophoroside content) × 40%] was used as the evaluation index for the extraction effect. The orthogonal test was carried out according to the L9 (34) orthogonal table. The factors and levels of the investigation are shown in Table 1.

[0081] Table 1 Factor level table

[0082]

[0083] Note: The temperature control range of the equipment is ±1°C.

[0084] Nine portions of horsetail were selected, each weighing 2 kg. The experimental arrangement and results are shown in Table 2.

[0085] Table 2 Orthogonal test results

[0086]

[0087] Among them, the preparation method of horsetail formula granules used in each group of experiments was the same except for the extraction step.

[0088] 2.2 Determination of paste yield

[0089] Take the horsetail extract and filter to obtain the horsetail filtrate. Accurately pipette 50 ml of the filtrate into an evaporating dish that has been dried to a constant weight. Evaporate to dryness at 105°C for 3 hours. Cool in a desiccator for 1 hour. Quickly weigh and calculate the weight.

[0090]

[0091] Wherein, W1 is the sum of the weight of the evaporating dish and the dry paste, W2 is the weight of the evaporating dish, M is the mass of the medicinal piece, and V is the total volume of the sample extract.

[0092] 2.3 Determination of Kaempferol-3-O-β-D-sophoroside and Kaempferol Content

[0093] The determination of kaempferol-3-O-β-D-sophoroside content and kaempferol content were carried out according to the methods under the national drug standard Equisetum formula granules (YBZ-PFKL-2022041).

[0094] 2.4 Results of the orthogonal test on Equisetum

[0095] With factors A, B, C, and D as variables, according to L9(3 4 ) orthogonal table, and the results are shown in Table 2. Based on the intuitive analysis results in Table 2, the optimal process was A3B2C1D3, using comprehensive evaluation as the indicator. A variance analysis, as shown in Table 3, showed that soaking temperature had a highly significant influence among the four factors examined. Considering factors such as ease of operation and cost savings during large-scale production, the optimal process for horsetail granules was A3B2C1D3.

[0096] Table 3 Results of variance analysis

[0097]

[0098] 2.5 Pilot Plant Process for Equisetum Granules

[0099] 2.5.1 Pilot Test Results Three batches (231201, 231202, and 231203) of horsetail granules were produced in pilot production using the preferred process described above. Each batch was fed 10 kg of material, yielding three batches of dry paste powders of horsetail granules. The dry paste powders were tested according to the national pharmaceutical standards for horsetail granules, and the test results for all three pilot samples met the national pharmaceutical standards for horsetail granules. The test results are shown in Table 4.

[0100] Table 4 Quality inspection results of 3 batches of pilot finished products

[0101]

[0102] The content indicators of the three batches of horsetail formula granules (batch numbers: 231201, 231202, and 231203) produced according to the preferred process all met the standards, indicating that the process can produce stable products and is suitable for large-scale production.

[0103] In this example, horsetail has the efficacy of dispelling wind-heat, improving eyesight and removing cataracts, and is relatively common in traditional Chinese medicine prescriptions. This example uses the yield of the paste and the content of kaempferol and kaempferol-3-O-β-D-sophoroside as evaluation indicators. Taking into account the influence of various factors, the final process is to soak at 60°C for 1.5 hours, then decoct and extract three times with water added in 15, 12, and 12 times the amount of water, respectively, for each extraction time of 0.5 hours. This method can both ensure the yield of the paste and increase the content, making it suitable for industrial production.

[0104] At this point, those skilled in the art will recognize that, although a number of exemplary embodiments of the present invention have been shown and described in detail herein, many other variations or modifications consistent with the principles of the present invention may be directly determined or derived from the disclosure of the present invention without departing from the spirit and scope of the present invention. Therefore, the scope of the present invention should be understood and deemed to cover all such other variations or modifications.

Claims

1. A method for preparing horsetail formula granules, characterized in that: include: The raw material of horsetail is processed, decocted and extracted, concentrated, dried and granulated in sequence to obtain horsetail formula granules; Wherein, the decoction and extraction step comprises: The processed Equisetum arvense slices are placed in an extraction tank for soaking, wherein the soaking temperature is 40 to 80° C. and the soaking time is 0.5 to 1.5 h; The extractions are performed three times in sequence, and the extracts obtained from each extraction are combined and filtered to obtain horsetail filtrate; wherein, during each extraction, the amount of water added to the extraction tank is 8 to 15 times the weight of the horsetail slices, and the time for each extraction is 0.5 to 1.5 hours.

2. The preparation method according to claim 1, characterized in that In the decoction extraction step: The soaking temperature is 60°C and the soaking time is 1.5 hours; and / or Each extraction time is 0.5h; and / or During the first extraction, the amount of water added to the extraction tank is 15 times the weight of the Equisetum arvense slices; and / or During the second extraction, the amount of water added to the extraction tank is 12 times the weight of the Equisetum arvense slices; and / or During the third extraction, the amount of water added to the extraction tank is 12 times the weight of the horsetail slices.

3. The preparation method according to claim 1, wherein The concentration step comprises: concentrating the horsetail filtrate to obtain a concentrated ointment; wherein the steam pressure does not exceed 0.12 MPa, the vacuum degree is -0.03 to -0.09 MPa, the concentration temperature is 50 to 85° C., and the relative density of the concentrated ointment at 60 to 70° C. is 1.01 to 1.10; and / or The drying step comprises: spray drying the concentrated ointment to obtain a dry ointment powder; wherein the air inlet temperature is 160 to 170°C, the air outlet temperature is 90 to 105°C, and the liquid inlet frequency is 10.0 to 25.0 Hz; and / or The granulation step comprises: taking the dry paste powder and dry-pressing granules to obtain horsetail formula granules; wherein the granulation adopts a dry pressing granulation method, the mesh number of the granulator screen is 12 mesh, the mesh number of the granulation screen is 10 mesh and 40 mesh, the feeding speed is 20 to 230 r / min, the pressing wheel speed is 3 to 40 r / min, and the granulation speed is 20 to 230 r / min; during the granulation process, the weight ratio of the dry paste powder to dextrin is 1:0 to 1:0.8, and the amount of the dextrin is ≤8% of the feeding amount of the horsetail decoction pieces.

4. A formula granule of horsetail, characterized in that: The horsetail formula granules are prepared using the preparation method according to any one of claims 1 to 3.

5. A process optimization method for horsetail formula granules, characterized in that: include: The comprehensive weighted score of kaempferol content, kaempferol-3-O-β-D-sophoroside content and paste yield was used as the evaluation index. 4 ) Orthogonal experiment was conducted to optimize the process of horsetail formula granules and conduct process verification by taking the soaking time, soaking temperature, extraction time and water addition ratio in the decoction extraction process as the investigation factors.

6. The optimization method according to claim 5, characterized in that: The calculation formula of the comprehensive weighted score is: comprehensive score = (cream yield / maximum cream yield) × 20% + (kaempferol content / maximum kaempferol content) × 40% + (kaempferol-3-O-β-D-sophoroside content) / maximum kaempferol-3-O-β-D-sophoroside content) × 40%; Among them, the maximum value of the paste yield, the maximum value of the kaempferol content, and the maximum value of the kaempferol-3-O-β-D-sophoroside content in the orthogonal test results are taken as the maximum paste yield, the maximum kaempferol content, and the maximum kaempferol-3-O-β-D-sophoroside content, respectively.

7. The optimization method according to claim 5, characterized in that: Through process verification, the optimal extraction process parameters obtained include: The soaking temperature is 60℃ and the soaking time is 1.5h; Add water and boil for three times, each extraction time is 0.5h; During the first extraction, add 15 times the weight of the Equisetum arvense slices into the extraction tank; During the second and third extractions, the amount of water added to the extraction tank is 12 times the weight of the Equisetum arvense slices.

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