Eriocaulon buergerianum formula granules and preparation method thereof
By adding corn starch to the flocculation process during the preparation of the herbaceous granules, the problem of unqualified solubility was solved, and good solubility performance and maintenance of the active ingredient content were achieved.
Patent Information
- Application Number
- CN202511198690.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-26
- Publication Date
- 2025-10-17
AI Technical Summary
The existing production of celery granules has the problem of unqualified solubility, which affects its performance and quality.
The Herba Corydalis slices were decocted with water as the extraction solvent, concentrated, and then corn starch was added for flocculation, followed by centrifugation, spray drying and dry granulation to prepare the Herba Corydalis formula granules.
The prepared Herba Corydalis formula granules have better solubility performance, while the content of the active ingredient vanillic acid is not affected, thus solving the problem of unqualified solubility.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of processing of traditional Chinese medicinal materials, in particular to a formula granule of Desmodium caudatum and a preparation method thereof. BACKGROUND
[0002] In the Quality Control and Standard Formulation Technical Requirements of Traditional Chinese Medicine Formula Granules (Draft for Comments), it is stipulated that, in addition to the forming process, the preparation of traditional Chinese medicine formula granules should be basically consistent with traditional decoction, that is, water is used as the solvent for extraction, and physical methods are used for solid-liquid separation, concentration, drying, granulation and other processes. Based on the above-mentioned standard that the medicinal material of traditional Chinese medicine formula granules should be basically consistent with the water decoction of traditional Chinese medicine decoction pieces, the preparation of traditional Chinese medicine formula granules by water extraction is required by the industry standard.
[0003] The formula granule of Desmodium caudatum is a formula granule prepared by processing the dried flowered stems of the capitula of Desmodium caudatum and processing it according to the main quality indicators of standard decoction. The existing preparation method of the formula granule of Desmodium caudatum is as follows: 10,000 g of Desmodium caudatum decoction pieces are added with water for decoction, filtered, and the filtrate is concentrated into a clear paste (the dry extract paste has an extract paste rate of 6%~10%), and then appropriate amount of auxiliary materials are added, dried (or dried and crushed), and then appropriate amount of auxiliary materials are added, mixed, granulated, and 1,000 g of the granules are prepared.
[0004] The present application is obtained through research in daily production. The existing production process of the formula granule of Desmodium caudatum is adopted, and the prepared formula granule of Desmodium caudatum has unqualified solubility, which seriously affects the performance and quality of the formula granule of Desmodium caudatum.
[0005] Therefore, it is necessary and urgent to develop a preparation method of the formula granule of Desmodium caudatum to solve the problem of unqualified solubility of the existing formula granule of Desmodium caudatum while ensuring stable quality indicators.
[0006] Therefore, the present application is proposed. SUMMARY
[0007] The present application aims to provide a formula granule of Desmodium caudatum and a preparation method thereof. It has been verified that the formula granule of Desmodium caudatum prepared by the preparation method of the present application not only has better solubility, but also does not affect the content of the effective component (vanillic acid), thereby effectively alleviating the problem of unqualified solubility of the existing formula granule of Desmodium caudatum prepared by water extraction.
[0008] In order to achieve the above-mentioned purpose of the present application, the following technical solutions are adopted: The present application provides a preparation method of a formula granule of Desmodium caudatum, which comprises the following steps: S1: decocting and water extracting Desmodium caudatum decoction pieces with water as the extraction solvent, and concentrating the water-extracted product to obtain a concentrated solution; S2: adding corn starch in the concentrated liquid and mixing uniformly, then sequentially performing centrifugation and spray drying to obtain spray-dried powder, mixing the spray-dried powder after screening to obtain dry paste powder, and performing dry granulation on the dry paste powder to obtain the Guchengcao formula granules.
[0009] Further, the adding amount of the corn starch in the step S2 is 0.25-0.50% of the mass of the Guchengcao decoction pieces.
[0010] Further, the water extraction and decoction method in the step S1 comprises the following steps: weighing the Guchengcao decoction pieces and placing the Guchengcao decoction pieces in a container, adding 24-36 times the amount of water, decocting and extracting for 1-1.5 h, and filtering; adding 20-30 times the amount of water to the residue, decocting and extracting for 0.4-0.6 h, and filtering; and combining the two extraction liquids to obtain the water extraction liquid.
[0011] Still further, the temperature of the decocting and extracting is 95-100 DEG C.
[0012] Further, the water extraction liquid in the step S1 is concentrated by using a double-effect concentrator. Further, the relative density of the concentrated liquid is 1.02-1.06 g / mL.
[0013] Further, the particle size of the spray-dried powder after the spray drying in the step S2 is a powder that passes through an 80-mesh screen.
[0014] Further, the dry granulation method in the step S2 comprises the following steps: mixing the spray-dried powder with magnesium stearate and malt dextrin to obtain dry paste powder, and preparing the Guchengcao formula granules by using a dry granulator.
[0015] Further, the rotating speed of the mixing is 8-15 rpm, and the mixing time is 20-30 min.
[0016] The Guchengcao formula granules prepared by the preparation method of the Guchengcao formula granules provided in the application.
[0017] Compared with the prior art, the application has the following beneficial effects: The preparation method of the Guchengcao formula granules provided in the application can effectively alleviate the problem of unqualified solubility of the existing Guchengcao formula granules by adding corn starch in the concentrated liquid for flocculation treatment on the basis of preparing the Guchengcao formula granules by water extraction and decoction. DETAILED DESCRIPTION
[0018] The technical solutions of the present application will be clearly and completely described below with examples. Obviously, the described examples are part of the examples of the present application, rather than all the examples. Based on the examples in the present application, all the other examples obtained by those skilled in the art without creative labor fall within the protection scope of the present application.
[0019] According to an aspect of the present application, a preparation method of a formula granule of Desmodium caudatum is provided, and the preparation method comprises the following steps: S1: decocting and water extracting Desmodium caudatum decoction pieces with water as an extraction solvent, and concentrating the water extract to obtain a concentrated solution; S2: adding corn starch into the concentrated solution and uniformly mixing, and then sequentially performing centrifugation and spray drying to obtain a spray-dried powder, and mixing the spray-dried powder through a sieve to obtain a dry paste powder, and performing dry granulation on the dry paste powder to obtain the formula granule of Desmodium caudatum.
[0020] The preparation method of the formula granule of Desmodium caudatum provided by the present application can effectively alleviate the problem of unqualified solubility of the existing formula granule of Desmodium caudatum by adding corn starch into the concentrated solution for flocculation treatment on the basis of preparing the formula granule of Desmodium caudatum through water extraction and decoction. It has been verified that the formula granule of Desmodium caudatum prepared by the method of the present application not only has better solubility, but also does not affect the content of the effective component (vanillic acid).
[0021] In a preferred embodiment of the present application, the addition amount of corn starch in step S2 is 0.25-0.50% of the mass of Desmodium caudatum decoction pieces.
[0022] As a preferred embodiment, it has been verified that the addition amount of corn starch in the present application is in the range of 0.25-0.50%, which can effectively reduce the phenomena of precipitation and caking, and also does not excessively affect the clarity of the solution, so as to achieve the best preparation performance and quality control standard.
[0023] In a preferred embodiment of the present application, the method of decocting and water extracting in step S1 comprises the following steps: weighing Desmodium caudatum decoction pieces and placing them in a container, adding 24-36 times the amount of water, decocting and extracting for 1-1.5 h, and filtering; adding 20-30 times the amount of water to the residue, decocting and extracting for 0.4-0.6 h, filtering, and combining the two extraction solutions to obtain a water extract.
[0024] In the above preferred embodiment, the temperature of decocting and extracting is 95-100℃.
[0025] In a preferred embodiment of the present application, the water extract in step S1 is concentrated by using a double-effect concentrator. As a preferred embodiment, the concentration is performed by a double-effect concentrator, wherein the temperature is: 75-85 DEG C for the first effect and 65-75 DEG C for the second effect; and the vacuum degree is: -0.07 to -0.03 MPa for the first effect and -0.08 to -0.06 MPa for the second effect. The double-effect concentrator can effectively reduce the boiling point and reduce the influence of temperature-sensitive components.
[0026] In a preferred embodiment of the present application, the relative density of the concentrated solution is 1.02-1.06 g / mL.
[0027] In a preferred embodiment of the present application, the temperature of the flocculation treatment is 75-95 DEG C and the time is 30-40 min. In a preferred embodiment of the present application, the particle size of the spray-dried powder after the spray drying in step S2 is a powder passing through an 80-mesh sieve.
[0028] Preferably, the process parameters of the spray drying are: steam post-temperature 140-170 DEG C, air inlet temperature 175-185 DEG C, material feeding temperature 45-60 DEG C, air blowing frequency 35-45 Hz, air induction frequency 40-50 Hz, and atomization frequency 30-45 Hz.
[0029] In a preferred embodiment of the present application, the dry granulation method in step S2 is: the spray-dried powder is mixed with magnesium stearate and malt dextrin to obtain a dry paste powder, and the dry granulation machine is used to prepare the Yu Jing Cao formula granules.
[0030] As a preferred embodiment, the dry granulation method comprises: the spray-dried powder after sieving is mixed with 0.02% of the amount of magnesium stearate and the corresponding amount of malt dextrin to obtain a dry paste powder, and the mixing speed is set to 10 rpm and the mixing time is 30 min. In the formula, the amount of malt dextrin added = total amount of the medicinal material × 10.0% - amount of the spray-dried powder after crushing and sieving - amount of corn starch - amount of magnesium stearate.
[0031] In a preferred embodiment of the present application, the mixing speed is 8-15 rpm and the mixing time is 20-30 min.
[0032] Preferably, the oil cylinder pressure of the dry granulation machine is 5-20 MPa, the feeding speed is 25-150 rpm, the tabletting speed is 8-40 rpm, and the granulating speed is 80-120 rpm; and the whole-granule screen mesh size of the dry granulation machine is 12 mesh or 30 mesh.
[0033] According to an aspect of the present application, the Yu Jing Cao formula granules are prepared by the preparation method of the Yu Jing Cao formula granules.
[0034] The prepared Guchuancao formula granules can effectively alleviate the problem of unqualified solubility of the existing Guchuancao formula granules under the condition of ensuring stable quality indexes.
[0035] The technical solutions of the present application will be further described below in combination with examples.
[0036] Example 1 A Guchuancao formula granule preparation process, comprising the following steps: 1. Weigh Guchuancao decoction pieces and place them in a container, add 30 times the amount of water of the decoction pieces, boil and decoct for 1.0 h, control the decocting temperature at 100℃, and filter; then add 25 times the amount of water of the decoction pieces to the residue, boil and decoct at 100℃ for 0.5 h; combine the two extraction liquids to obtain Guchuancao water decoction extraction liquid; 2. Filter the extraction liquid through a double filter with a mesh size of 100 to an extraction liquid storage tank; use a double-effect concentrator to concentrate the Guchuancao water decoction extraction liquid, control the temperature at 80℃ for the first effect and 70℃ for the second effect; control the vacuum degree at -0.05 MPa for the first effect and -0.07 MPa for the second effect; Concentrate the Guchuancao extraction liquid to a test density of 1.04 to obtain a concentrated liquid; 3. Add 0.5% of the amount of corn starch of the decoction pieces to the concentrated liquid for flocculation treatment, control the temperature of the batching tank at 85℃ and keep the stirring always on, maintain stirring for 30 minutes, and use a centrifuge to centrifugal filter (7000 rpm, 15 min, centrifugal liquid passes through a 350 mesh screen) to obtain a filtered liquid; 4. Spray dry the filtered liquid to obtain a powder that passes through an 80 mesh screen, then dry granulate the powder that passes through a 12 mesh screen to obtain Guchuancao formula granules; The spray drying process parameters are: steam after temperature 150℃, air inlet temperature 180℃, material conveying temperature 55℃, air blowing frequency 40Hz, air induction frequency 45Hz, atomization frequency 35Hz; The dry granulation method comprises: after sieving, mix the spray dried powder with 0.02% of the amount of magnesium stearate of the decoction pieces and the corresponding amount of malt dextrin to obtain a dry paste powder, set the mixing speed to 10 rpm and the mixing time to 30 min; install a 12 mesh screen on the dry granulator, adjust the main oil cylinder pressure, roller speed and feeding screw speed parameters for granulation.
[0037] The malt dextrin addition amount = total amount of decoction pieces × 10.0% - amount of spray dried powder after crushing and sieving - amount of corn starch - amount of magnesium stearate. The control oil cylinder pressure is 15 MPa, the feeding speed is 80 rpm, the tabletting speed is 35 rpm, and the granulation speed is 100 rpm. The prepared granules are sieved with a 12 mesh screen.
[0038] Example 2 A preparation process of a formula granule of Desmodium caudatum, comprising the following steps: 1. Put the Desmodium caudatum decoction pieces into a container, add 24 times the amount of water of the decoction pieces, boil and decoct for 1.0 h, control the decocting temperature at 95℃, and filter; then add 20 times the amount of water of the decoction pieces to the residue, boil and decoct for 0.5 h at 95℃, and combine the two extraction solutions to obtain a water decoction extraction solution of Desmodium caudatum; 2. Filter the extraction solution through a double filter with a mesh size of 100 to an extraction solution storage tank; use a double-effect concentrator to concentrate the water decoction extraction solution of Desmodium caudatum, control the temperature at 75℃ for the first effect and 65℃ for the second effect, and control the vacuum degree at -0.07 MPa for the first effect and -0.08 MPa for the second effect; Concentrate the Desmodium caudatum extraction solution to a test density of 1.02 to obtain a concentrated solution; 3. Add 0.5% of the amount of corn starch of the decoction pieces to the concentrated solution for flocculation treatment, control the temperature of the batching tank at 75℃ and keep the stirring on, maintain the stirring for 30 min, and use a centrifuge to centrifugal filter (7000 r / min, 15 min, centrifugal liquid passes through a 350-mesh screen) to obtain a filtered solution; 4. Spray dry the filtered solution to obtain a powder passing through an 80-mesh screen, and then dry granulate the powder passing through a 12-mesh screen to obtain a formula granule of Desmodium caudatum; The spray drying process parameters are as follows: steam post-temperature 140℃, air inlet temperature 175℃, material conveying temperature 45℃, air blowing frequency 35 Hz, air induction frequency 40 Hz, and atomization frequency 30 Hz; The dry granulation method comprises the following steps: mix the sieved and spray-dried powder with 0.02% of the amount of magnesium stearate of the decoction pieces and the corresponding amount of malt dextrin to obtain a dry paste powder, set the mixing speed at 10 rpm, and mix for 30 min; wherein: the amount of malt dextrin added = total amount of decoction pieces × 10.0% - amount of sieved and spray-dried powder - amount of corn starch - amount of magnesium stearate.
[0039] Install a 12-mesh screen on the dry granulator, adjust the main oil cylinder pressure, roller speed and feeding screw speed parameters, and perform granulation. Control the oil cylinder pressure at 5 MPa, the feeding speed at 25 rpm, the tabletting speed at 8 rpm, and the granulation speed at 80 rpm. The prepared granules are sieved with a 12-mesh screen.
[0040] Example 3 A preparation process of a formula granule of Desmodium caudatum, comprising the following steps: 1. Put the Desmodium caudatum decoction pieces into a container, add 24 times the amount of water of the decoction pieces, boil and decoct for 1.0 h, control the decocting temperature at 95℃, and filter; then add 20 times the amount of water of the decoction pieces to the residue, boil and decoct for 0.5 h at 95℃, and combine the two extraction solutions to obtain a water decoction extraction solution of Desmodium caudatum; 2, the extract liquid is filtered by double filter to 100 mesh to the extract liquid storage tank; the double-effect concentrator is used to concentrate the decoction extract of the herba setariae viridis, the temperature is controlled to 85 DEG C in the first effect and 75 DEG C in the second effect, the vacuum degree is controlled to-0.03 MPa in the first effect and-0.06 MPa in the second effect; The herba setariae viridis extract liquid is concentrated to the measuring density 1.06, and the concentrated liquid is obtained; 3, the concentrated liquid is added to the corn starch of 0.5% of the decoction piece for flocculation treatment, the temperature of the batching tank is controlled to 95 DEG C, and the stirring is kept open, the stirring is maintained for 30 minutes, and the centrifugal filter (7000 r / min, 15 min, the centrifugal liquid is filtered through 350 mesh screen) is used, and the filtrate is obtained; 4, the filtrate is spray dried to obtain the powder through 80 mesh screen, and then the dry granulation is carried out to obtain the granules through 12 mesh screen, and the herba setariae viridis formula granules are obtained; The spray drying process parameters are: steam after temperature 170 DEG C, air inlet temperature 185 DEG C, material conveying temperature 60 DEG C, air blowing frequency 45 Hz, air induction frequency 50 Hz, atomization frequency 45 Hz; The dry granulation method comprises the following steps: after screening, the spray dry powder is mixed with 0.02% magnesium stearate and the corresponding amount of malt dextrin to obtain dry paste powder, the mixing speed is set to 10 rpm, and the mixing time is 30 min; wherein: the amount of malt dextrin added = total amount of decoction piece feed × 10.0%-spray dry powder after crushing and screening amount-corn starch amount-magnesium stearate amount.
[0041] The 12 mesh screen is installed on the dry granulator, and the parameters of the main oil cylinder pressure, the roller speed and the feeding screw speed are adjusted for granulation. The oil cylinder pressure is controlled to be 20 MPa, the feeding speed is controlled to be 150 rpm, the tabletting speed is controlled to be 40 rpm, and the granulating speed is controlled to be 120 rpm. The prepared granules are sieved with 12 mesh screen.
[0042] Examples 4-9 Examples 4-9 of the present application are different from example 1 in that the amount of corn starch added in step 3 is different, and the rest is the same as example 1, as shown in table 1.
[0043] Table 1:
[0044] Comparative example 1 The comparative example is the same as example 1 except that no "corn starch" is added in step 3.
[0045] Comparative example 2 The comparative example is the same as example 1 except that the "corn starch" in step 3 is replaced by an equal amount of malt dextrin.
[0046] Comparative example 3 This comparative example is the same as Example 1 except that the "corn starch" in step 3 is replaced by an equal amount of beta-cyclodextrin.
[0047] Comparative Example 4 This comparative example is the same as Example 1 except that the "corn starch" in step 3 is replaced by an equal amount of gelatin.
[0048] Comparative Example 5 This comparative example is the same as Example 1 except that the "corn starch" in step 3 is replaced by an equal amount of chitosan.
[0049] Experimental Example 1 In order to demonstrate that the Herba Corydalis glutinosa granules prepared by the preparation method of the present invention not only have better solubility but also have the technical effect of not affecting the content of the active ingredient (vanillic acid), the Herba Corydalis glutinosa granules prepared in Examples 1 to 9 of the present invention and Comparative Examples 1 to 5 are subjected to performance testing.
[0050] The specific detection method refers to the Guangdong Provincial Quality Standard for Traditional Chinese Medicine Formula Granules: Codonopsis pilosula Formula Granules Guangdong PFKL20230042 (Trial).
[0051] The specific test results are shown in Table 2 and Table 3.
[0052] Table 2:
[0053] The above experimental results show that there are significant differences in the effects when using different doses of corn starch for treatment, that is, the addition amount of corn starch should be controlled in the range of 0.25%~0.50%, so as to ensure that it can effectively reduce precipitation and agglomeration without excessively affecting the clarity of the solution, thereby achieving the best formulation performance and quality control standards.
[0054] Table 3:
[0055] Note: The amount of auxiliary materials / flocculants added in Comparative Examples 2 to 5 is the same as the amount of corn starch added in Example 1, which is 0.5% of the amount of the decoction piece.
[0056] As can be seen from the above table, the content of active ingredients in the treatment of Herba Corydalis glutinosa concentrate with a variety of different flocculants did not have a significant impact. However, according to the results of the solubility test, corn starch as a flocculant only caused slight turbidity and no foreign matter or charred debris, and its effect was significantly better than other flocculant technical solutions.
[0057] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, and are not intended to limit the present application; although the present application has been described in detail with reference to the above embodiments, those skilled in the art should understand that the technical solutions recorded in the above embodiments can be modified, or some or all of the technical features can be replaced by equivalents; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present application.
Claims
1. A method for preparing Herba Codonopsis pilosulae granules, characterized in that: The preparation method comprises the following steps: S1: using water as an extraction solvent to decoct the Herba Glechomae glutinosae slices, and then concentrating the extracted pieces to obtain a concentrated solution; S2: Add corn starch to the concentrate and mix evenly, then centrifuge and spray dry to obtain spray-dried powder, sieve and mix to obtain dry paste powder, dry granulate the dry paste powder to obtain Coix glutinosa formula granules.
2. The method for preparing the Herba Codonopsis pilosulae formula granules according to claim 1, characterized in that: The amount of corn starch added in step S2 is 0.25-0.50% of the mass of the Herba Codonopsis pilosulae decoction pieces.
3. The method for preparing the Herba Codonopsis pilosulae formula granules according to claim 1, characterized in that: The decoction and water extraction method in step S1 comprises: Weigh the Herba Codonopsis pilosulae slices and place them in a container. Add 24-36 times the amount of water, decoct and extract for 1-1.5 hours, and filter. Add 20-30 times the amount of water to the residue, decoct and extract for 0.4-0.6 hours, filter, and combine the two extracts to obtain the water extract.
4. The method for preparing the Herba Codonopsis pilosulae formula granules according to claim 3, characterized in that: The decoction extraction temperature is 95-100°C.
5. The method for preparing the Herba Codonopsis pilosulae formula granules according to claim 1, characterized in that: In step S1, the water extract is concentrated using a double-effect concentrator.
6. The method for preparing the Herba Codonopsis pilosulae formula granules according to claim 5, characterized in that: The relative density of the concentrated solution is 1.02-1.06 g / mL.
7. The method for preparing the Herba Codonopsis pilosulae formula granules according to claim 1, characterized in that: The particle size of the spray-dried powder after spray drying in step S2 is powder that passes through an 80-mesh sieve.
8. The method for preparing the Herba Codonopsis pilosulae formula granules according to claim 1, characterized in that: The dry granulation method in step S2 is: mixing the spray-dried powder with magnesium stearate and maltodextrin to obtain a dry paste powder, and preparing the Herba Codonopsis pilosulae formula granules using a dry granulator.
9. The method for preparing the Herba Codonopsis pilosulae formula granules according to claim 8, characterized in that: The mixing speed is 8-15 rpm, and the mixing time is 20-30 min.
10. The Herba Codonopsis pilosulae granules prepared by the preparation method according to any one of claims 1 to 9.