CN115177665A - Preparation method of madder formula granules - Google Patents
Preparation method of madder formula granules Download PDFInfo
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Abstract
The invention discloses a preparation method of madder formula particles, which comprises the following steps: (1) water extraction; (2) inclusion of the extracting solution; (3) concentrating under reduced pressure; (4) spray drying; (5) sieving and mixing; and (6) dry granulation. The preparation method solves the problem that the insoluble components in madder, such as anthraquinone and naphthoquinone medicinal components, such as madder, rubiadin and the like, are easy to lose in the concentration process, and improves the transfer rate of the medicinal components in the concentration process, so that the content of effective substances in the final product formula particles is improved, and the final product formula particles can achieve better curative effect; meanwhile, the treatment capacity of spray drying is reduced, the production energy consumption is reduced, and more energy is saved.
Description
Technical Field
The invention relates to a preparation method of formula granules, in particular to a preparation method of madder formula granules.
Background
Madder is a common Chinese medicine, which is a dried root and rhizome of madder belonging to the family rubiaceae, also called Huoxue grass, chenopodium hybridum and the like, and has a long history of use. It is bitter in taste and cold in nature, enters liver and heart channels, has effects of cooling blood, stopping bleeding, promoting blood circulation and removing blood stasis, and can be used for treating hematemesis, epistaxis, traumatic injury swelling and pain, rheumatalgia, amenorrhea and blood stasis. The chemical components of Rubia cordifolia mainly comprise anthraquinone and its glycosides (such as alizarin and hydroxyalizarin), and also comprise naphthoquinones (such as rubiadin), terpenes, capropeptides, polysaccharides, and other chemical components.
The traditional Chinese medicine formula particle is a new form of traditional Chinese medicine decoction piece innovation, maintains the characteristics of traditional Chinese medicine decoction pieces, has special characteristics, and has the characteristics of three effects (high efficiency, quick effect and long effect), three small effects (small dosage, small toxicity and small side effect), five convenience (convenient taking, carrying, storage, composing and transportation) and the like. In recent years, the traditional Chinese medicine formula granule industry is rapidly developed, but the traditional Chinese medicine formula granule industry is still imperfect in various aspects such as standard establishment, process control, quality control and the like.
Researches prove that the madder root has stronger effects of inhibiting the self-activation of the hyaluronic acid binding protein and resisting fungi, and the madder root has good effects of resisting platelet aggregation, resisting inflammation and tumors, inhibiting the surface antigen secretion of hepatitis B, protecting nerves and the like. In the '2020 edition of Chinese pharmacopoeia', madder and madder macrophylla are listed as index components of madder, and the madder macrophylla are also controlled as content measurement indexes in the madder formula particle standard (the standard of the traditional Chinese medicine formula particle of the drug supervision and administration of Jiangsu province, no. JS-YBZ-2021094). The quality evaluation of 6 madder formula particle samples of manufacturers by Chua le and the like shows that the content difference of the rubiadin is obvious and can be related to the difference between the production processes adopted by different manufacturers, which can greatly influence the clinical curative effect of the product.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a preparation method of madder formula particles with high retention rate of active ingredients in a concentration process and low yield of concentrated solution.
The technical scheme is as follows: the preparation method of the madder prescription granule comprises the following steps:
(1) Water extraction
Adding materials (madder decoction pieces), adding 10-14 times of water by weight, heating to slightly boil, and filtering; then adding 6-10 times of water by weight, heating to slight boiling, and filtering; mixing the filtrates to obtain extractive solution; recording the amount of the extract liquid, and sampling to determine the content of the madder root and the madder leaf;
(2) The extract is included
Adding beta-cyclodextrin with the feeding amount of 3-5% by mass of the decoction pieces into the madder root extracting solution while the solution is hot, dissolving the mixture evenly, and stirring the mixture for inclusion to obtain an inclusion solution;
(3) Concentrating under reduced pressure
Concentrating the madder inclusion solution under reduced pressure, filtering to obtain a concentrated solution, recording the amount of the concentrated solution, sampling and measuring the content of the madder element and the madder element, and calculating the retention rate of the madder element and the madder element in a concentration process (from an extracting solution to the concentrated solution);
(4) Spray drying the concentrated solution to obtain spray dried powder of radix Rubiae;
(5) Sieving and mixing
Adding maltodextrin, silicon dioxide and magnesium stearate into the madder spray-dried powder, sieving and mixing to obtain a madder extract;
(6) And (4) dry granulating.
Preferably, the preparation method further comprises a pretreatment step before water extraction, specifically, impurity removal, cleaning, moistening and cutting into 5-10 mm short sections.
Preferably, the first micro-boiling retention time in the step (1) is 1 to 3 hours; the micro-boiling retention time is 0.5 to 1.5 hours again.
Preferably, the stirring time in the step (2) is 0.5 to 1.5 hours, and the stirring speed is 100 to 500 revolutions per minute.
Preferably, the concentration temperature in the step (3) is 50-70 ℃, and the relative density of the concentrated solution is 1.10-1.12; the filtration is performed by a 120-260 mesh filter.
Preferably, the spray drying in the step (4) is to input the concentrated solution into a spray dryer for drying, wherein the air inlet temperature is 165-175 ℃, the air outlet temperature is 105-110 ℃, and the frequency of an atomizing disc is 80-100%.
Preferably, in the step (5), the mass parts of the maltodextrin, the silicon dioxide and the magnesium stearate are respectively 0.5-3%, 0.1-0.3% and 0.1-0.2% of the feeding amount of the decoction pieces, 0.1-0.3% of the spray-dried powder of the madder; the screening and mixing steps are as follows: sieving with a sieve of 80-100 meshes, and placing in a fixed hopper mixer for total mixing, wherein the rotating speed of the mixer is 6-7 r/min, and the total mixing time is 15-45 min.
Preferably, the dry granulation parameters in step (6) are: vertical feeding: 15-20 r/min, horizontal feeding: 100-130 rpm, roll rotation speed: 12-15 rpm, pressure of press roll: 10-15 MPa, whole grain rotating speed: 100-140 r/min, mesh number of whole grain sieve: 12 to 40 meshes.
Aiming at the characteristics that anthraquinone compounds (such as madder, hydroxyrubicin) and naphthoquinone compounds (such as madder, zoxamine) are not easy to dissolve in water, dissolve in ether and ethanol and are easy to dissolve in chloroform and ethyl acetate, before an extracting solution is concentrated, beta-cyclodextrin is adopted for inclusion and solubilization, and then the extracting solution is concentrated to thick paste with certain relative density under reduced pressure, so that precipitation loss of effective substances such as the hydroxyrubicin and the madder in the concentration process due to reduction of solubility can be reduced, the content of the effective substances in final product formula particles is increased, a better curative effect can be achieved, the relative density of a concentrated solution can be increased, the spray drying treatment amount is reduced, and the effects of saving energy and reducing consumption are achieved.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: the invention solves the problem that the indissolvable components in the madder such as anthraquinone and naphthoquinone medicinal components such as hydroxyalizarin and rubiadin are easy to lose in the concentration process, improves the transfer rate of the medicinal components in the concentration process, thereby improving the content of effective substances in the final product formula particles and enabling the final product formula particles to achieve better curative effect; meanwhile, the treatment capacity of spray drying is reduced, the production energy consumption is reduced, and more energy is saved.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
Example 1
Rubia cordifolia formula particle
1. Pretreatment
Removing impurities, cleaning, moistening, and cutting into 5-10 mm short segments by a speed-regulating slicing and cutting machine.
2. Water extraction
60kg of materials are firstly put into a multifunctional tank, 12 times of water by weight is added, the mixture is heated to boil, the micro-boiling is kept for 2 hours, and the mixture is filtered by a 200-mesh duplex filter; adding 8 times of water by weight, heating to boil, keeping slightly boiling for 1 hour, and filtering with a 200-mesh duplex filter; mixing the filtrates to obtain extractive solution. Recording the amount of the extract liquid, sampling and determining the content of the madder and the rubiadin (the content of the madder is 27.40 mu g.mL) -1 17.09. Mu.g/mL of rubiadin -1 ) The determination method refers to the madder prescription granule standard (the standard of the traditional Chinese medicine prescription granule of the drug administration of Jiangsu province, the number is: JS-YBZ-2021094).
3. The extract is included
Adding betacyclodextrin with the mass percent of 5% of the feeding amount of the decoction pieces into the madder extracting solution while the solution is hot, dissolving the mixture evenly, stirring and including the mixture for 1 hour, and stirring the mixture at the speed of 107 r/min to obtain the inclusion solution.
4. Concentrating under reduced pressure
And (3) carrying out reduced pressure concentration on the madder seed coating solution, wherein the concentration temperature is 50-70 ℃, the relative density of the concentrated solution is 1.10 (measured at 40 ℃), filtering the concentrated solution by using a 200-mesh filter to obtain a concentrated solution, and recording the amount of the concentrated solution, wherein the paste recovery rate is 68%. Sampling to determine the content of madder and rubiadin (the content of madder is 478.27 mu g) -1 The rubiadin is 416.23 mu g -1 ) The determination method refers to the madder formula particle standard (the standard of traditional Chinese medicine formula particles of the drug administration of Jiangsu province, and the number is as follows: JS-YBZ-2021094), calculating the retention rates of the madder hydroxy-alizarin and the madder macrophyll in the concentration process (from the extract to the concentrated solution).
5. Spray drying
And (3) conveying the concentrated solution into a spray dryer for drying, wherein the air inlet temperature is 170 ℃, the air outlet temperature is 105 ℃, the frequency of an atomizing disc is 93%, and collecting powder timely to obtain the madder spray-dried powder.
6. Sieving and mixing
Adding maltodextrin (model MD20, 100 meshes) accounting for 3% of the material amount of the decoction pieces, silicon dioxide accounting for 0.3% of the material amount of the madder spray-dried powder and magnesium stearate accounting for 0.2% of the material amount of the madder spray-dried powder into the madder spray-dried powder, sieving the powder by a 80-mesh sieve, and placing the powder into a fixed hopper mixer for total mixing, wherein the rotating speed of the mixer is 7 r/min, and the total mixing time is 30 min to obtain the madder extract.
7. Dry granulation
Carrying out dry granulation on the madder extract, wherein the dry granulation parameters are as follows: vertical feeding: 15-20 r/min, horizontal feeding: 100-130 rpm, roll rotation speed: 12-15 rpm, pressure of press roll: 10-15 MPa, whole grain rotating speed: 100-140 r/min, mesh number of whole grain sieve: 12 to 40 meshes.
And packaging to obtain finished madder formula particles (each 1 g of formula particles is equivalent to 5 g of decoction pieces).
Comparative example 1
Rubia cordifolia formula particle
1. Pretreatment
Removing impurities, cleaning, moistening, and cutting into 5-10 mm short segments by a speed-regulating slicing and cutting machine.
2. Water extraction
60kg of materials are firstly put into a multifunctional tank, 12 times of water by weight is added, the mixture is heated to boil, the micro-boiling is kept for 2 hours, and the mixture is filtered by a 200-mesh duplex filter; adding 8 times of water by weight, heating to boil, keeping slightly boiling for 1 hour, and filtering with a 200-mesh duplex filter; mixing the filtrates to obtain extractive solution. Recording the amount of the extract liquid, sampling and determining the content of the madder element and the rubiadin (the content of the madder element is 29.64 mu g.mL) -1 15.82 mug. ML of rubiadin -1 ) The determination method refers to the madder prescription granule standard (the standard of the traditional Chinese medicine prescription granule of the drug administration of Jiangsu province, the number is: JS-YBZ-2021094).
3. Concentrating under reduced pressure
And (3) carrying out reduced pressure concentration on the madder extract, wherein the concentration temperature is 50-70 ℃, the relative density of the concentrated solution is 1.06 (measured at 40 ℃), filtering the concentrated solution by using a 200-mesh filter to obtain the concentrated solution, and recording the amount of the concentrated solution, wherein the paste recovery rate is 121%. Sampling and measuring the contents of the madder and the rubiadin (the content of the madder is 142.11 mu g.g.g) -1 157.44 micrograg/g of rubiadin -1 ) The determination method refers to the madder prescription granule standard (the standard of the traditional Chinese medicine prescription granule of the drug administration of Jiangsu province, the number is: JS-YBZ-2021094), calculating the retention rates of the madder hydroxy-alizarin and the madder macrophyll in the concentration process (from the extract to the concentrated solution).
4. Spray drying
And (3) conveying the concentrated solution into a spray dryer for drying, wherein the air inlet temperature is 170 ℃, the air outlet temperature is 105 ℃, the frequency of an atomizing disc is 90%, and collecting powder timely to obtain the madder spray-dried powder.
5. Sieving and mixing
Adding maltodextrin (model MD20, 100 meshes) with the amount of 7% by mass of the decoction pieces, silicon dioxide with the amount of 0.3% by mass of the madder spray-dried powder and magnesium stearate with the amount of 0.2% by mass of the madder spray-dried powder into the madder spray-dried powder, sieving by a 80-mesh sieve, and placing the mixture into a fixed hopper mixer for total mixing, wherein the rotating speed of the mixer is 7 revolutions per minute, and the total mixing time is 30 minutes to obtain the madder extract.
6. Dry granulation
Carrying out dry granulation on the madder extract, wherein the dry granulation parameters are as follows: vertical feeding: 15-20 r/min, horizontal feeding: 100-130 rpm, roll rotation speed: 12-15 rpm, compression roller pressure: 10-15 MPa, whole grain rotating speed: 100-140 r/min, mesh number of whole grain sieve: 12 to 40 meshes.
And packaging to obtain finished madder prescription granules (each 1 g of prescription granules is equivalent to 5 g of decoction pieces).
Comparative example 2
Rubia cordifolia formula particle
1. Pretreatment
Removing impurities, cleaning, moistening, and cutting into 5-10 mm short sections by a speed-regulating slicing and cutting machine.
2. Water extraction
60kg of materials are firstly put into a multifunctional tank, 12 times of water by weight is added, the mixture is heated to boil, the micro-boiling is kept for 2 hours, and the mixture is filtered by a 200-mesh duplex filter; adding 8 times of water by weight, heating to boil, keeping slightly boiling for 1 hour, and filtering by a 200-mesh duplex filter; mixing the filtrates to obtain extractive solution. Recording the amount of the extract liquid, sampling and determining the content of the madder and the rubiadin (the content of the madder is 28.76 mu g.mL) -1 The rubiadin is 18.13 mu g/mL -1 ) The determination method refers to the madder prescription granule standard (the standard of the traditional Chinese medicine prescription granule of the drug administration of Jiangsu province, the number is: JS-YBZ-2021094).
3. Concentrating under reduced pressure
And (3) carrying out reduced pressure concentration on the madder extract, wherein the concentration temperature is 50-70 ℃, the relative density of the concentrated solution is 1.08 (measured at 40 ℃), filtering the concentrated solution by using a 200-mesh filter to obtain the concentrated solution, and recording the amount of the concentrated solution, wherein the paste recovery rate is 89%. Sampling to determine the content of madder and rubiadin (the content of madder is 145.87 mug. G) -1 The rubiadin accounts for 219.08 mu g/g -1 ) The determination method refers to the madder formula particle standard (the standard of traditional Chinese medicine formula particles of the drug administration of Jiangsu province, and the number is as follows: JS-YBZ-2021094), calculating the retention rates of the madder hydroxy-alizarin and the madder macrophyll in the concentration process (from the extract to the concentrated solution).
4. Spray drying
And (3) conveying the concentrated solution into a spray dryer for drying, wherein the air inlet temperature is 170 ℃, the air outlet temperature is 105 ℃, the frequency of an atomizing disc is 95%, and collecting powder timely to obtain the madder spray-dried powder.
5. Sieving and mixing
Adding 8 mass percent of maltodextrin (model MD20, 100 meshes) into the madder spray-dried powder, 0.3 mass percent of silicon dioxide into the madder spray-dried powder, and 0.2 mass percent of magnesium stearate into the madder spray-dried powder, sieving by a 80-mesh sieve, and placing the mixture into a fixed hopper mixer for total mixing, wherein the rotating speed of the mixer is 7 revolutions per minute, and the total mixing time is 30 minutes, so as to obtain the madder extract.
6. Dry granulation
Carrying out dry granulation on the madder extract, wherein the dry granulation parameters are as follows: vertical feeding: 15-20 r/min, horizontal feeding: 100-130 rpm, roll rotation speed: 12-15 rpm, compression roller pressure: 10-15 MPa, whole grain rotating speed: 100-140 r/min, mesh number of whole grain sieve: 12 to 40 meshes.
And packaging to obtain finished madder prescription granules (each 1 g of prescription granules is equivalent to 5 g of decoction pieces).
TABLE 1 recovery rate of Rubia cordifolia concentrate and retention rate of madder element and rubiadin in concentration process
| Yield (%) of concentrate | Concentration step Hydroxyalizarin Retention ratio (%) | Concentration procedure madder leaf retention (%) | |
| Example 1 | 68 | 69.82 | 97.42 |
| Comparative example 1 | 121 | 33.15 | 68.81 |
| Comparative example 2 | 89 | 25.36 | 60.42 |
As can be seen from table 1, in the preparation method provided in embodiment 1 of the present invention, the retention rates of madder in the concentration step and madder in the big leaf can reach 69.82% and 97.42%, respectively, both of which are at a higher level, and the loss of the active ingredients is less.
Compared with the comparative example 1, the concentration procedure of the example 1 has the advantages that the retention rates of the madder in the hydroxy group and the madder in the greater leaf are higher than those of the comparative example 1. The paste yield of the concentrated solution in the example 1 is far lower than that of the comparative example 1, namely the amount of the material to be spray-dried in the example 1 is far lower than that in the comparative example I, so that the energy consumption of a spray-drying process can be greatly reduced.
Compared with the comparative example 2, the concentration procedure of the example 1 has the rubiadin and rubiadin retention rates which are much higher than those of the comparative example 1. The yield of the concentrated solution in the example 1 is lower than that in the comparative example 2, namely the amount of the material to be spray-dried in the example 1 is lower than that in the comparative example 2, so that the energy consumption of a spray-drying process can be reduced.
The filter residue of the concentrated solution of the comparative example 1 and the concentrated solution of the comparative example 2 are obviously more than that of the concentrated solution of the example 1, so that the retention rate of the active ingredients of the comparative example 1 and the comparative example 2 is lower.
Claims (9)
1. The preparation method of the madder prescription granule is characterized by comprising the following steps:
(1) Water extraction
Feeding, adding 10-14 times of water by weight, heating to slightly boil, and filtering; then adding 6 to 10 times of water by weight, heating to slightly boiling, and filtering; mixing the filtrates to obtain extractive solution; recording the amount of the extract liquid, and sampling to determine the content of the madder root and the madder leaf;
(2) The extract liquid is included
Adding beta-cyclodextrin with the feeding amount of 3-5% by mass of decoction pieces into the madder extracting solution while the solution is hot, uniformly dissolving, and carrying out stirring inclusion to obtain an inclusion solution;
(3) Concentrating under reduced pressure
Concentrating the madder wrapped liquid under reduced pressure, filtering to obtain a concentrated solution, recording the amount of the concentrated solution, sampling and determining the content of madder element and madder element, and calculating the retention rate of the madder element and the madder element in the concentration process;
(4) Spray drying the concentrated solution to obtain spray dried powder of radix Rubiae;
(5) Sieving and mixing
Adding maltodextrin, silicon dioxide and magnesium stearate into the madder spray-dried powder, sieving and mixing to obtain a madder extract;
(6) And (4) dry granulating.
2. The method for preparing Rubia cordifolia formulation granule according to claim 1, further comprising a pretreatment step before water extraction, specifically removing impurities, washing, moistening, and cutting into 5-10 mm short segments.
3. The method for preparing madder formula particles according to claim 1, wherein the first micro-boiling retention time in step (1) is 1 to 3 hours; the retention time for the secondary slight boiling is 0.5 to 1.5 hours.
4. The method for preparing Rubia cordifolia granules according to claim 1, wherein the stirring time in step (2) is 0.5 to 1.5 hours, and the stirring rate is 100 to 500 rpm.
5. The method for preparing the madder formula particle according to claim 1, wherein the concentration temperature in the step (3) is 50 to 70 ℃, and the relative density of the concentrated solution is 1.10 to 1.12; the filtration is carried out by a filter of 120 to 260 meshes.
6. The preparation method of madder formula particles according to claim 1, wherein the spray drying in step (4) is to dry the concentrated solution in a spray dryer at air inlet temperature of 165-175 ℃, air outlet temperature of 105-110 ℃ and atomizing disc frequency of 80-100%.
7. The preparation method of the madder dispensing granule according to claim 1, characterized in that in the step (5), the mass parts of the maltodextrin, the silicon dioxide and the magnesium stearate are respectively 0.5-3%, 0.1-0.3% and 0.1-0.2% of the feeding amount of the decoction pieces, 0.1-0.3% of the spray-dried powder of the madder and 0.1-0.2% of the spray-dried powder of the madder.
8. The method for preparing Rubia cordifolia formulation according to claim 1, wherein the sieving and mixing in step (5) comprises the following steps: sieving the mixture by a sieve with 80-100 meshes, and placing the mixture into a fixed hopper mixer for total mixing, wherein the rotating speed of the mixer is 6-7 rpm, and the total mixing time is 15-45 minutes.
9. The method for preparing the madder formula according to claim 1, wherein the dry granulation parameters in step (6) are: vertical feeding: 15 to 20 rpm, horizontal feeding: 100 to 130 revolutions per minute, the rotation speed of a compression roller: 12 to 15 revolutions per minute, compression roller pressure: 10 to 15MPa, granulation speed: 100 to 140 revolutions per minute, and the mesh number of the whole grain sieve: 12 to 40 meshes.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110201120A (en) * | 2019-06-21 | 2019-09-06 | 广东一方制药有限公司 | A kind of Chinese medicinal granule and preparation method thereof containing sesquiterpenoids |
| CN112336757A (en) * | 2020-10-20 | 2021-02-09 | 广东一方制药有限公司 | Traditional Chinese medicine formula granule containing coumarin compound and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110201120A (en) * | 2019-06-21 | 2019-09-06 | 广东一方制药有限公司 | A kind of Chinese medicinal granule and preparation method thereof containing sesquiterpenoids |
| CN112336757A (en) * | 2020-10-20 | 2021-02-09 | 广东一方制药有限公司 | Traditional Chinese medicine formula granule containing coumarin compound and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 朱丽红;贺文娟;王梅;唐俊琪;: "茜草配方颗粒的制备工艺及质量评价研究" * |
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