Gentian formula granule, preparation method and optimization method
By optimizing the decoction and drying process of gentian formula granules, the problem of unstable quality of gentian formula granules is solved, high-quality and efficient preparation is achieved, the process flow is simplified and the cost is reduced.
Patent Information
- Application Number
- CN202411278468.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-12
- Publication Date
- 2024-12-20
AI Technical Summary
The gentian formula particles have uneven quality and are difficult to meet quality standards, resulting in the need to optimize the preparation process to ensure stability.
The gentian raw materials are cut into sections and soaked and decocted. Through multiple decoctions and water ratio adjustment, combined with the process flow of spray drying and dry pressing granulation, the extraction and drying process is optimized to improve the extraction rate and particle quality of the active ingredients.
It improves the quality and stability of gentian formula particles, simplifies the preparation process, reduces costs, facilitates large-scale production, and optimizes process conditions through orthogonal experiments to ensure compliance with national drug standards.
Smart Images
Figure CN119157925A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of traditional Chinese medicine formula granules, and in particular to gentian formula granules, a preparation method and an optimization method. Background Art
[0002] Gentiana is the dried root and rhizome of Gentiana scabra, a plant of the Gentianaceae family. It has the effects of clearing away heat and dampness, purging liver and gallbladder fire, strengthening the stomach, and lowering blood pressure. Modern pharmacological studies have shown that gentiopicroside, as the main active ingredient in Gentiana scabra, is basically consistent with the clinical application of traditional Chinese medicine.
[0003] Formula granules effectively avoid the situation that Chinese patent medicines are difficult to add or subtract according to symptoms, are easy to store and carry, and make taking medicine more convenient. The quality of gentian formula granules prepared under different process conditions varies. It is necessary to study and optimize the preparation process of gentian formula granules so that the gentian formula granules meet the quality standards and then control the stability of the quality of the gentian formula granules. Summary of the invention
[0004] In view of the above problems, the present invention is proposed to provide a gentian formula granule, preparation method and optimization method that overcome the above problems or at least partially solve the above problems, which can solve the problem of uneven quality of gentian formula granules and achieve the effect that the gentian formula granules meet the quality standards.
[0005] Specifically, the present invention provides a method for preparing gentian formula granules, comprising the following steps: Cut the gentian raw material into sections, and soak them in water at a first preset temperature for a first preset time; Decoction and extraction to obtain gentian filtrate; The gentian filtrate is concentrated to obtain a clear paste; Taking the clear paste and spray drying it to obtain dry paste powder; The dry paste powder is taken and dry-pressed into granules to prepare gentian formula granules.
[0006] Optionally, the decoction extraction to obtain the gentian filtrate comprises: For the first extraction, water is added in a first preset ratio, and the mixture is boiled and extracted for a second preset time, and the first extract is collected and stored in another container; For the second extraction, add water in a second preset ratio, decoct and extract for a third preset time, and collect the second extract and store it in another container; The first extract and the second extract are combined to obtain a gentian filtrate.
[0007] Optionally, the first preset ratio is a weight ratio of water to the gentian raw material during the first extraction, and the first preset ratio is 8:1 to 12:1; The second preset ratio is the weight ratio of water to the gentian raw material during the second extraction, and the second preset ratio is 6:1 to 10:1; The second preset time is 0.5h to 1.5h; The third preset time is 0.5h to 1h.
[0008] Optionally, the gentian raw material is cut into sections and immersed in water at a first preset temperature for a first preset time. The first preset temperature is 80°C to 100°C; The first preset time is 0h to 1h.
[0009] The present invention also provides a gentian formula granule, which is a gentian formula granule prepared by any of the preparation methods described above.
[0010] The present invention also provides an optimization method for the preparation method of the above-mentioned gentian formula granules, comprising: Conducting a preliminary test on the preparation of the gentian formula granules according to the preparation method to obtain multiple influencing factors affecting the preparation of the gentian formula granules and the value range of each influencing factor; Design and analyze orthogonal experiments based on the influencing factors and the value ranges of the influencing factors, and record the analysis data; The comprehensive score of each group of tests is calculated according to the analysis data, and the preparation method of the gentian formula granules is determined according to the comprehensive score.
[0011] Optionally, after calculating the comprehensive score of each group of tests according to the analysis data and determining the preparation method of the gentian formula granules according to the comprehensive score, the method further includes: The gentian formula granule samples were prepared by the preparation method and analyzed, and the optimization results were verified by comparing with the control samples.
[0012] Optionally, the test results include the gentiopicroside content transfer rate, the paste yield rate and the fourth characteristic peak area in the characteristic spectrum; The influencing factors include the feeding method, decoction time and water addition amount; wherein the decoction time includes the first decoction time and the second decoction time; the water addition amount includes the first water addition amount and the second water addition amount; In the method of calculating the comprehensive score of each group of tests according to the test results and determining the preparation method of the gentian formula granules according to the comprehensive score, the comprehensive score is calculated as follows: ; Among them, A1 is the transfer rate of gentiopicroside content, A0 is the maximum transfer rate of gentiopicroside content, ais the first coefficient; B1 is the peak area of the fourth characteristic peak, B0 is the maximum peak area of the fourth characteristic peak, b is the second coefficient; C1 is the paste yield rate, C0 is the maximum paste yield rate, c is the third coefficient.
[0013] Optionally, the first coefficient is 0.5; The second coefficient is 0.3; The third coefficient is 0.2.
[0014] Optionally, the method for preparing the gentian formula granules comprises: Cut the gentian raw material into sections, put them into boiling water for the first decoction extraction, decoction extraction for 0.5 hours, collect the first extract and store it in another container; wherein the weight of the water is 12 times the weight of the gentian raw material; Add water to perform a second decoction extraction, decoct and extract for 0.5h, collect the second extract and store it in another container; wherein the weight of the water is 10 times the weight of the gentian raw material; combining the first extract and the second extract to obtain a gentian filtrate; The gentian filtrate is concentrated to obtain a clear paste with a specific gravity of 1.02; The clear paste is spray dried under the conditions of an inlet air temperature of 170° C., an outlet air temperature of 95° C., and a liquid inlet frequency of 13 Hz to obtain a dry paste powder; The dry paste powder is taken and dry-pressed into granules to prepare gentian formula granules.
[0015] In the gentian formula granules, preparation method and optimization method of the present invention, when preparing the gentian formula granules, the gentian raw material is cut into sections and soaked in water. After soaking, the water is heated to boiling and decocted to obtain a gentian filtrate. The gentian filtrate is concentrated and dried to obtain a dry paste powder. The dry paste powder is mixed with dextrin and then dry pressed to obtain the gentian formula granules. After the gentian raw material is soaked, water enters the tissue cells through osmosis, the gentian raw material softens, and the cells swell, which is more conducive to the dissolution of the active ingredients in the gentian raw material. Moreover, the active ingredients in the gentian raw material are more easily extracted by water in the subsequent decoction process, thereby improving the extraction rate of the active ingredients. The decoction process temperature is high, which can destroy the cell wall, so that the active ingredients wrapped in the cell wall and the cell membrane are released, so that the active ingredients in the gentian raw material are dissolved in water faster and more completely, thereby improving the extraction effect of the gentian and improving the quality of the gentian formula granules.
[0016] Furthermore, the gentian formula granules are prepared after the gentian raw materials are cut into sections, without the need for processing of gentian decoction pieces. The preparation method is simple, the preparation steps are reduced, and the preparation efficiency is improved, thereby reducing the preparation cost of the gentian formula granules and facilitating the production and processing of the gentian formula granules.
[0017] 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
[0018] 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: Figure 1 is a schematic flow chart of a method for preparing gentian formula granules according to one embodiment of the present invention; Figure 2 is a schematic flow chart of decocting and extracting gentian raw materials according to one embodiment of the present invention; Figure 3 is a schematic flow chart of an optimization method for preparing a gentian formula granule according to an embodiment of the present invention; Figure 4 It is the characteristic spectrum of the gentian reference herb; Figure 5 This is the characteristic spectrum of the gentian formula granules prepared according to Example 3. DETAILED DESCRIPTION
[0019] Refer to the following Figures 1 to 5 To describe the gentian formula granules, preparation method and optimization method of the 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 "multiple" 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.
[0020] In the description of the present embodiment, the description with reference to the terms "one embodiment", "some embodiments", "illustrative embodiments", "examples", "specific examples", 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 schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials, or characteristics described may be combined in any one or more embodiments or examples in a suitable manner.
[0021] Figure 1 is a schematic flow chart of a method for preparing gentian formula granules according to an embodiment of the present invention, such as Figure 1 As shown, and refer to Figures 2 to 5 The present invention provides a method for preparing gentian formula granules, comprising the following steps: Step S100, cutting gentian raw material into sections, and soaking them in water at a first preset temperature for a first preset time.
[0022] Step S200, decoction and extraction to obtain gentian filtrate.
[0023] Step S300, concentrating the gentian filtrate to obtain a clear paste.
[0024] Step S400, taking the clear paste and spray drying it to obtain dry paste powder.
[0025] Step S500, taking the dry paste powder and dry-pressing it into granules to obtain gentian formula granules.
[0026] In the present embodiment, when preparing the gentian formula granules, the gentian raw material is cut into sections and soaked in water. After soaking, the water is heated to boiling and decocted to obtain the gentian filtrate. The gentian filtrate is concentrated and dried to obtain a dry paste powder. The dry paste powder is mixed with dextrin and then dry pressed to obtain the gentian formula granules. After the gentian raw material is soaked, water enters the tissue cells through osmosis, the gentian raw material softens, and the cells swell, which is more conducive to the dissolution of the active ingredients in the gentian raw material. Moreover, the active ingredients in the gentian raw material are more easily extracted by water in the subsequent decoction process, thereby improving the extraction rate of the active ingredients. The decoction process temperature is high, which can destroy the cell wall, so that the active ingredients wrapped in the cell wall and the cell membrane are released, so that the active ingredients in the gentian raw material are dissolved in water faster and more completely, thereby improving the extraction effect of the gentian and improving the quality of the gentian formula granules.
[0027] Furthermore, the gentian formula granules are prepared after the gentian raw materials are cut into sections, without the need for processing of gentian decoction pieces, and the preparation method is simple, the preparation steps are reduced, and the preparation efficiency is improved, thereby reducing the preparation cost of the gentian formula granules and facilitating the production and processing of the gentian formula granules.
[0028] In some embodiments of the present invention, Figure 2 As shown, step S200, decoction and extraction to obtain gentian filtrate, comprises: Step S210, the first extraction, adding water in a first preset ratio, boiling and extracting for a second preset time, collecting the first extract and storing it in another container.
[0029] Step S220, extracting for the second time, adding water in a second preset ratio, boiling and extracting for a third preset time, collecting the second extract and storing it in another container.
[0030] Step S230, combining the first extract and the second extract to obtain gentian filtrate.
[0031] In this embodiment, water is used to extract gentiopicroside, the main component of gentian. The water extraction and decoction method is simple. When extracting the active ingredients in gentian, the concentration difference of the active ingredients inside and outside the cells of the gentian slices is used to diffuse the active ingredients in the cells into the water. As the active ingredients in the water increase, the diffusion rate of the active ingredients decreases. By replacing new water, the diffusion rate of the active ingredients increases, the diffusion rate of the active ingredients is improved, thereby reducing the extraction time of the active ingredients, and then improving the quality of the gentian formula granules.
[0032] In some embodiments of the present invention, the first preset ratio is the weight ratio of water to gentian raw material during the first extraction, and the first preset ratio is 8:1 to 12:1. For example, the first preset ratio is 8:1, 9:1, 10:1, 11:1 or 12:1.
[0033] In this embodiment, the larger the first preset ratio is, the larger the amount of water is, the greater the concentration difference between the gentiopicroside content in the water and the gentian raw material is, and the more conducive to the dissolution of gentiopicroside. During the first decoction extraction, the gentian raw material is put into 8 to 12 times the amount of water for extraction, so that the gentiopicroside in the gentian raw material is fully dissolved.
[0034] In some embodiments of the present invention, the second preset ratio is the weight ratio of water to gentian raw material during the second extraction, and the second preset ratio is 6:1 to 10:1. For example, the first preset ratio is 6:1, 7:1, 8:1, 9:1 or 10:1.
[0035] In this embodiment, the larger the second preset ratio is, the larger the amount of water is, the greater the concentration difference between the gentiopicroside content in the water and the gentian raw material is, and the more conducive to the dissolution of gentiopicroside. During the second decoction extraction, the gentian raw material is put into 6 to 10 times the amount of water for extraction, so that the gentiopicroside in the gentian raw material is fully dissolved.
[0036] In some embodiments of the present invention, the second preset time is 0.5h to 1.5h. For example, the second preset time is 0.5h, 1h or 1.5h.
[0037] In this embodiment, the first decoction and extraction time is 0.5h to 1h. Through long-term high-temperature decoction, the gentiopicroside in the gentian raw material is fully dissolved in water, thereby improving the transfer rate of gentianpicroside and improving the quality of the gentian formula granules.
[0038] In some embodiments of the present invention, the third preset time is 0.5h to 1h. For example, the third preset time is 0.5h, 0.6h, 0.7h, 0.8h, 0.9h or 1h.
[0039] In this embodiment, after the first decoction and extraction, part of gentiopicroside is extracted, and part of it is still present in the gentian raw material. Gentiopicroside is subjected to a second decoction and extraction, and the second decoction and extraction time is 0.5h to 1h, so that the gentiopicroside in the gentian raw material is fully dissolved in water, thereby improving the transfer rate of gentiopicroside and improving the quality of the gentian formula granules.
[0040] In some embodiments of the present invention, in step S100, the gentian raw material is cut into segments and immersed in water at a first preset temperature for a first preset time, wherein the first preset temperature is 80° C. to 100° C. For example, the first preset temperature is 80° C., 85° C., 90° C., 95° C. or 100° C. The first preset time is 0 h to 1 h. The first preset time is 0 h, 0.5 h or 1 h.
[0041] In this embodiment, when preparing the gentian formula granules, the gentian raw material is first soaked in water at 80° C. to 100° C. for 0 h to 1 h. When the gentian is soaked at high temperature, water enters the tissue cells through osmosis, the gentian raw material softens, and the cells swell, which is more conducive to the dissolution of the active ingredients in the gentian raw material.
[0042] An embodiment of the present invention further provides a gentian formula granule, which is a gentian formula granule prepared by the preparation method in any one of the above embodiments.
[0043] In this embodiment, the preparation method of the gentian formula granules is simple and convenient, with simple steps and easy operation, which is conducive to the mass production of the gentian formula granules.
[0044] like Figure 3 As shown, the present invention also provides an optimization method for the preparation method of the gentian formula granules in the above embodiments, comprising: Step S600, conducting a preliminary test on the preparation of the gentian formula granules according to the preparation method, and obtaining a plurality of influencing factors affecting the preparation of the gentian formula granules and a value range of each influencing factor.
[0045] Step S700, designing and analyzing an orthogonal experiment according to the influencing factors and the value ranges of the influencing factors, and recording the analysis data.
[0046] Step S800, calculating the comprehensive score of each group of experiments according to the analysis data, and determining the preparation method of the gentian formula granules according to the comprehensive score.
[0047] In this embodiment, a preliminary experiment of gentian formula granules is first carried out, and multiple influencing factors of the preparation of gentian formula granules are obtained through the preliminary experiment, and an orthogonal experiment is carried out according to the multiple influencing factors. The experimental data during the experiment is measured. The comprehensive score of each group of test results is calculated according to the obtained experimental data, and the preparation method of the gentian formula granules is determined according to the comprehensive score. The process conditions corresponding to the test group with the highest comprehensive score are the optimal preparation conditions of the gentian formula granules.
[0048] In some embodiments of the present invention, when conducting a preliminary experiment, the gentian raw material is placed in water 10 times the weight of the gentian raw material, and the water is heated to 80°C and soaked for 1 hour. The water is heated to boiling and decocted for 1 hour, and the gentian filtrate after decoction is poured out and collected. Water 10 times the weight of the gentian raw material is added again, the water is heated to boiling and decocted for 0.5 hours, and the gentian filtrate after decoction is poured out and collected. The filtrates after the two decoctions are mixed together. The transfer rate of gentiopicroside content and the cream yield are measured. The test shows that the transfer rate of gentiopicroside content is 53.7%, and the cream yield is 29.4%.
[0049] In some embodiments of the present invention, after preliminary experiments, the number of decoctions was selected to be two, and the feeding method, decoction time and water addition amount were selected as influencing factors for orthogonal experiments.
[0050] In some embodiments of the present invention, after calculating the comprehensive score of each group of experiments according to the analysis data in step S800 and determining the preparation method of the gentian formula granules according to the comprehensive score, the method further includes: Step S900, preparing a sample of the gentian formula granules using the preparation method and analyzing it, and verifying the optimization result by comparing it with a control sample.
[0051] In this example, the optimized preparation method was used to prepare gentian formula granule samples, and the samples were compared with control medicinal materials to verify the optimization effect and ensure the reliability of the optimized preparation method.
[0052] In some embodiments of the present invention, the test results include the gentiopicroside content transfer rate, the paste yield rate and the fourth characteristic peak area in the characteristic spectrum. The influencing factors include the feeding method, the decoction time and the amount of water added; wherein the decoction time includes the first decoction time and the second decoction time. The amount of water added includes the first water addition amount and the second water addition amount. The feeding method includes the feeding temperature and the soaking time.
[0053] In this embodiment, the number of decoctions of the gentian raw material, the decoction time, the first preset ratio, and the soaking time are optimized to study the best preparation method of the gentian formula granules, thereby improving the quality of the gentian formula granules. In addition, optimizing the preparation method of the gentian formula granules can save preparation time, reduce energy consumption, and thereby improve the preparation efficiency of the gentian formula granules.
[0054] In some embodiments of the present invention, in step S800, a comprehensive score of each group of tests is calculated according to the test results, and in determining the preparation method of the gentian formula granules according to the comprehensive score, the calculation method of the comprehensive score is: ; Among them, A1 is the transfer rate of gentiopicroside content, A0 is the maximum transfer rate of gentiopicroside content, a is the first coefficient. B1 is the peak area of the fourth characteristic peak, B0 is the maximum peak area of the fourth characteristic peak, b is the second coefficient. C1 is the paste output rate, C0 is the maximum paste output rate, c is the third coefficient.
[0055] Among them, the fourth characteristic peak is the fourth characteristic peak appearing in the characteristic spectrum measured for the gentian formula granules.
[0056] In some embodiments of the present invention, the first coefficient is 0.5, the second coefficient is 0.3, and the third coefficient is 0.2.
[0057] In some embodiments of the present invention, the calculation method of the gentiopicroside content transfer rate is:
[0058] In some embodiments of the present invention, when determining the content and characteristic spectrum of gentiopicroside, take the gentian formula granules, grind them into powder, take 0.1g, and put them into a conical flask. Add 50mL of methanol, weigh the weight, and ultrasonically treat for 15min at a power of 300W and a frequency of 40kHz. After cooling, weigh the weight again, make up the lost weight with methanol, shake well, filter, and take the filtrate to obtain the sample to be tested. Take 1μL and 10μL of the sample to be tested and inject them into the liquid chromatograph respectively to measure the content and characteristic spectrum of gentiopicroside. Obtain the peak area of the fourth characteristic peak according to the characteristic spectrum.
[0059] The calculation method of the paste yield is:
[0060] Among them, the determination of the dryness of the extract is based on the drying method in the moisture determination method in the "Pharmacopoeia of Chinese Medicine".
[0061] In some embodiments of the present invention, in step S300, the gentian filtrate is concentrated to obtain a clear paste, and the concentration is carried out in an environment with a vacuum degree of -0.03MPa to -0.09MPa, and the concentration temperature is 55°C to 85°C, and a clear paste with a specific gravity of 1.01 to 1.03 at a temperature of 60°C to 70°C is obtained. For example, the vacuum degree is -0.03MPa, -0.04MPa, -0.05MPa, -0.06MPa, -0.06MPa, -0.08MPa or -0.09MPa. The concentration temperature is 55°C, 65°C, 75°C or 85°C. The specific gravity of the clear paste is 1.01, 1.02 or 1.03.
[0062] In this embodiment, the clear paste is prepared by decompression concentration, and the gentian filtrate is concentrated in a vacuum environment. High temperature is not required during concentration to prevent high temperature from affecting the gentian filtrate. The specific gravity of the clear paste is the ratio of the density of the clear paste to the density of water at the same temperature. The specific gravity of the clear paste affects the effect of the spray. If the specific gravity of the clear paste is too large, it will cause difficulty in spraying, thereby affecting the drying of the clear paste.
[0063] Furthermore, when the gentian filtrate is concentrated, the steam pressure does not exceed 0.10 MPa.
[0064] In some embodiments of the present invention, in step S400, the clear paste is spray-dried to obtain a dry paste powder, in which the air inlet temperature is 140° C. to 180° C., the air outlet temperature is 80° C. to 100° C., and the liquid inlet frequency is 10 Hz to 25 Hz.
[0065] In this embodiment, the dry paste powder is obtained by drying using a spray drying method, so that the clear paste is dried instantly, the drying time of the clear paste is reduced, and the production cost of the gentian formula granules is reduced. In addition, most of the heat in the spray drying process is used to evaporate the water in the clear paste, and the heating time of the clear paste is extremely short, and the quality of the dry paste powder will not be affected by high temperature.
[0066] In some embodiments of the present invention, in step S500, the dry paste powder is taken and dry-pressed into granules to prepare gentian formula granules, comprising: The dry paste powder is added into the hopper of the dry pressing granulator, sent to the pressing wheel through the feeding, dry pressed into tablets, broken, granulated through a 12-mesh sieve, and the gentian formula granules are obtained.
[0067] The conveying rotation speed is 20 r / min to 230 r / min, for example, the conveying rotation speed is 20 r / min, 50 r / min, 100 r / min, 150 r / min, 200 r / min or 230 r / min.
[0068] The pressure roller speed is 3 r / min to 40 r / min, for example, the pressure roller speed is 3 r / min, 5 r / min, 10 r / min, 15 r / min, 20 r / min, 25 r / min, 30 r / min, 35 r / min or 40 r / min.
[0069] The granulation speed is 20 r / min to 200 r / min. For example, the granulation speed is 20 r / min, 50 r / min, 100 r / min, 150 r / min or 200 r / min.
[0070] In some embodiments of the present invention, the method for preparing the gentian formula granules comprises: Step S11, cut the gentian raw material into sections, put them into boiling water for the first decoction extraction, decoction extraction for 0.5h, collect the first extract and store it in another container; wherein the weight of water is 12 times the weight of the gentian raw material.
[0071] Step S12, adding water to perform a second decoction extraction, decoction extraction for 0.5h, collecting the second extract and storing it in another container; wherein the weight of the water is 10 times the weight of the gentian raw material.
[0072] Step S13, combining the first extract and the second extract to obtain gentian filtrate.
[0073] Step S14, concentrating the gentian filtrate to obtain a clear paste with a specific gravity of 1.02.
[0074] Step S15, spray drying the clear paste under the conditions of an inlet air temperature of 170° C., an outlet air temperature of 95° C., and a liquid inlet frequency of 13 Hz to obtain a dry paste powder.
[0075] Step S16, taking the dry paste powder and dry-pressing it into granules to obtain gentian formula granules.
[0076] In this embodiment, after optimization, the feeding method is boiling water feeding, decocting in water 12 times the amount of the gentian raw material for 0.5h, and then decocting in water 10 times the amount of the gentian raw material for 0.5h. The gentian filtrate is obtained, concentrated and dried, and then dry-pressed into granules. After optimization, no soaking is required, and the decoction time is short, which saves the preparation time of the gentian formula granules, improves the preparation efficiency of the gentian formula granules, and reduces the preparation cost of the gentian formula granules. Example
[0077] Step S21, take 250g of gentian raw material, cut it into sections, put it into boiling water for the first decoction extraction, decoction extraction for 0.5h, collect the first extract and store it in another container, wherein the weight of water is 12 times the weight of the gentian raw material.
[0078] Step S22, adding water to perform a second decoction extraction, decoction extraction for 0.5h, collecting the second extract and storing it in another container; wherein the weight of the water is 10 times the weight of the gentian raw material.
[0079] Step S23, combining the first extract and the second extract to obtain gentian filtrate.
[0080] Step S24, concentrating the gentian filtrate to obtain a clear paste with a specific gravity of 1.02.
[0081] Step S25, spray drying the clear paste under the conditions of an inlet air temperature of 170° C., an outlet air temperature of 95° C., and a liquid inlet frequency of 13 Hz to obtain a dry paste powder.
[0082] The prepared gentian formula granules were tested, and the transfer rate of gentiopicroside content in the gentian formula granules was measured to be 95.8%, the paste yield was 31.7%, the peak area of the fourth characteristic peak in the characteristic spectrum was 67, and the calculated comprehensive score was 95.8. According to the measured data, the gentian formula granules meet the requirements of the national drug standards. Example
[0083] Step S31, taking 250g of gentian raw material, cutting into segments, putting into boiling water for the first decoction extraction, decoction extraction for 1 hour, collecting the first extract and storing in another container; wherein the weight of water is 8 times the weight of the gentian raw material.
[0084] Step S32, adding water to perform a second decoction extraction, decoction extraction for 0.5h, collecting the second extract and storing it in another container; wherein the weight of the water is 6 times the weight of the gentian raw material.
[0085] The subsequent steps are the same as in Example 1.
[0086] The prepared gentian formula granules were tested, and the transfer rate of gentiopicroside content in the gentian formula granules was measured to be 87.4%, the paste yield was 27.9%, the peak area of the fourth characteristic peak in the characteristic spectrum was 51, and the calculated comprehensive score was 82.3. According to the measured data, the gentian formula granules meet the requirements of the national drug standards. Example
[0087] Step S41, taking 25 kg of gentian raw material, cutting it into sections, putting it into boiling water for the first decoction extraction, decoction extraction for 0.5 h, collecting the first extract and storing it in another container; wherein the weight of water is 12 times the weight of the gentian raw material.
[0088] Step S42, adding water to perform a second decoction extraction, decoction extraction for 0.5h, collecting the second extract and storing it in another container; wherein the weight of the water is 10 times the weight of the gentian raw material.
[0089] The subsequent steps are the same as in Example 1.
[0090] Figure 4 This is the characteristic spectrum of the reference medicinal materials of Gentiana formula granules. Figure 5 is the characteristic spectrum of the gentian formula granules in this embodiment. Among them, M1, M2 and M3 are the characteristic spectrum results of multiple batches of gentian formula granules prepared under the same conditions. Peak 1 is the loganin peak, peak 2 is the swertiamarin peak, and peak 3 is the gentiopicroside peak. Figure 4 and Figure 5 It can be seen that the composition and retention time of the gentian formula granules prepared in this embodiment are consistent with those in the control medicinal materials. The prepared gentian formula granules were tested, and the gentiopicroside content transfer rate of the gentian formula granules was measured to be 94.2%, the paste rate was 33.6%, and the peak area of the fourth characteristic peak in the characteristic spectrum was 59. The moisture content in the gentian formula granules was 3.4%, and each 1g of the gentian formula granules contained 75.4mg of gentiopicroside, and the extract was 62.2%. In thin layer identification, the gentian formula granules showed the same color as the control medicinal materials and the reference substance at the corresponding positions.
[0091] According to the measured data, the gentian formula granules meet the requirements of the national drug standards, indicating that the optimized preparation method of the gentian formula granules can continuously and stably produce gentian formula granules products that meet the national drug standards and are suitable for large-scale production.
[0092] At this point, those skilled in the art should recognize that, although multiple exemplary embodiments of the present invention have been shown and described in detail herein, many other variations or modifications that conform to the principles of the present invention can still be directly determined or derived based on the content disclosed in 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 recognized as covering all these other variations or modifications.
Claims
1. A method for preparing gentian formula granules, characterized in that: The following steps are involved: Cut the gentian raw material into sections, and soak them in water at a first preset temperature for a first preset time; Decoction and extraction to obtain gentian filtrate; The gentian filtrate is concentrated to obtain a clear paste; Taking the clear paste and spray drying it to obtain dry paste powder; The dry paste powder is taken and dry-pressed into granules to prepare gentian formula granules.
2. The preparation method according to claim 1, characterized in that: The decoction and extraction to obtain the gentian filtrate comprises: For the first extraction, water is added in a first preset ratio, and the mixture is boiled and extracted for a second preset time, and the first extract is collected and stored in another container; For the second extraction, add water in a second preset ratio, decoct and extract for a third preset time, and collect the second extract and store it in another container; The first extract and the second extract are combined to obtain a gentian filtrate.
3. The preparation method according to claim 2, characterized in that: The first preset ratio is the weight ratio of water to the gentian raw material during the first extraction, and the first preset ratio is 8:1 to 12:1; The second preset ratio is the weight ratio of water to the gentian raw material during the second extraction, and the second preset ratio is 6:1 to 10:1; The second preset time is 0.5h to 1.5h; The third preset time is 0.5h to 1h.
4. The preparation method according to claim 1, characterized in that: In the step of cutting the gentian raw material into sections, soaking the sections in water at a first preset temperature for a first preset time, The first preset temperature is 80°C to 100°C; The first preset time is 0h to 1h.
5. A gentian formula granule, characterized in that: The gentian formula granules are prepared by the preparation method described in any one of claims 1 to 4.
6. A method for optimizing the preparation method of the gentian formula granules as claimed in claim 1, characterized in that: include: Conducting a preliminary test on the preparation of the gentian formula granules according to the preparation method to obtain multiple influencing factors affecting the preparation of the gentian formula granules and the value range of each of the influencing factors; Design and analyze orthogonal experiments based on the influencing factors and the value ranges of the influencing factors, and record the analysis data; The comprehensive score of each group of tests is calculated according to the analysis data, and the preparation method of the gentian formula granules is determined according to the comprehensive score.
7. The optimization method according to claim 6, characterized in that: After calculating the comprehensive score of each group of tests according to the analysis data and determining the preparation method of the gentian formula granules according to the comprehensive score, the method further includes: The gentian formula granule samples were prepared by the preparation method and analyzed, and the optimization results were verified by comparing with the control samples.
8. The optimization method according to claim 6, characterized in that: The test results include the gentiopicroside content transfer rate, the paste yield rate and the fourth characteristic peak area in the characteristic spectrum; The influencing factors include the feeding method, decoction time and water addition amount; wherein the decoction time includes the first decoction time and the second decoction time; the water addition amount includes the first water addition amount and the second water addition amount; In the method of calculating the comprehensive score of each group of tests according to the test results and determining the preparation method of the gentian formula granules according to the comprehensive score, the comprehensive score is calculated as follows: ; Among them, A1 is the transfer rate of gentiopicroside content, A0 is the maximum transfer rate of gentiopicroside content, a is the first coefficient; B1 is the peak area of the fourth characteristic peak, B0 is the maximum peak area of the fourth characteristic peak, b is the second coefficient; C1 is the paste yield rate, C0 is the maximum paste yield rate, c is the third coefficient.
9. The optimization method according to claim 8, characterized in that: The first coefficient is 0.5; The second coefficient is 0.3; The third coefficient is 0.
2.
10. The optimization method according to claim 9, characterized in that: The method for preparing the gentian formula granules comprises: Cut the gentian raw material into sections, put them into boiling water for the first decoction extraction, decoction extraction for 0.5h, collect the first extract and store it in another container; wherein the weight of the water is 12 times the weight of the gentian raw material; Add water to perform a second decoction extraction, decoct and extract for 0.5h, collect the second extract and store it in another container; wherein the weight of the water is 10 times the weight of the gentian raw material; combining the first extract and the second extract to obtain a gentian filtrate; The gentian filtrate is concentrated to obtain a clear paste with a specific gravity of 1.02; The clear paste is spray dried under the conditions of an inlet air temperature of 170° C., an outlet air temperature of 95° C., and a liquid inlet frequency of 13 Hz to obtain a dry paste powder; The dry paste powder is taken and dry-pressed into granules to prepare gentian formula granules.