Preparation process of Zhenwu soup granules

Abstract

The invention provides a preparation technology of Zhenwu decoction granules, and relates to the technical field of traditional Chinese medicine, and the preparation technology comprises the following steps: S1, preparing raw materials: poria cocos, radix paeoniae alba, ginger, bighead atractylodes rhizome and radix aconiti carmichaeli; s2, condensation reflux extraction is adopted, water is added into the prepared raw materials for common reflux decoction extraction for 1-3 times, the water adding amount is 6-8 times of that of the prepared raw materials each time, extraction lasts for 0.5-2 hours each time, and the temperature is reduced to 60-70 DEG C; s3, merging the filtrates, concentrating under reduced pressure to obtain an extract with the relative density of 1.10-1.15 (50 DEG C), and performing spray drying to obtain dry extract powder; s4, mixing an excipient with the dry paste powder, and pressing the mixture into granules in a dry granulator; in the extraction process, condensation reflux extraction is adopted, it is ensured that volatile components are reserved in an extracting solution, the extracting solution is rapidly cooled to 60-70 DEG C after extraction is finished, the temperature is controlled to be 60-70 DEG C in the closed storage and vacuum concentration process, and the volatile components and thermosensitive components are reserved to the maximum extent.

Description

Technical Field

[0001] The invention relates to the technical field of traditional Chinese medicines, and in particular to a preparation process of Zhenwu decoction granules. Background Art

[0002] Zhenwu Decoction is a famous ancient Chinese classic prescription, first recorded in Zhang Zhongjing's Treatise on Febrile Diseases. It has the effect of warming the yang and promoting diuresis, and is mainly used to treat yang deficiency and water retention syndrome. Its ingredients mainly include Poria cocos, white peony root, ginger, aconite root, Atractylodes macrocephala and other medicinal materials. The function of Zhenwu Decoction is to warm the yang and promote diuresis, and is mainly used to treat yang deficiency and water retention syndrome. Symptoms may include chills and limb coldness, difficulty urinating, palpitations and restlessness under the heart, dizziness, muscle twitching, unsteady standing, heavy and painful limbs, edema (especially below the waist), abdominal pain, diarrhea, cough, asthma, vomiting, etc. The tongue is pale and fat with teeth marks on the edges, the tongue coating is white and slippery, and the pulse is deep and thin, which are also typical manifestations of this syndrome. In medical theory, Zhenwu Decoction is suitable for patients with spleen and kidney yang deficiency and internal retention of dampness. The meaning of the prescription is to warm the spleen and kidney to help yang qi, and to facilitate urination to remove water evil. Aconite is the main drug in the prescription, which is pungent, sweet and hot in nature. It is used to warm the kidney and help yang to transform qi and promote water circulation, and warm the spleen and earth to warm and transport dampness. Poria promotes water and penetrates dampness, so that the water evil is removed through urination; Atractylodes macrocephala strengthens the spleen and dries dampness, and ginger warms and disperses water qi, which not only helps Aconite warm yang and dispel cold, but also combines with Poria and Atractylodes to disperse dampness. White peony root is used as an adjuvant, which has the effects of facilitating urination to promote water qi, softening the liver and relieving urgency to stop abdominal pain, and astringing yin and relaxing muscles to relieve muscle spasms. At the same time, it can prevent Aconite from damaging yin due to dryness and heat, so as to facilitate long-term use and slow treatment.

[0003] Chinese medicine granules are granules made under the theoretical guidance of traditional Chinese medicine hospitals, using standardized processed Chinese medicine pieces as raw materials and modern pharmaceutical technology. They overcome the problems of decocting first, adding later, wrapping and decocting in the traditional decoction process, and the non-standard decoction containers. They have obvious advantages in ensuring and stabilizing clinical efficacy. Chinese medicine granules can be used for flexible clinical prescription and preparation and can also be used as industrial raw materials for Chinese medicine preparations. As raw materials for tablets and capsules, Chinese medicine formula granules are packaged in aluminum foil bags or other convenient packages with accurate dosage, avoiding the common problems of oil loss, discoloration, insect infestation and mildew in the storage of traditional Chinese medicine pieces. They are convenient for drug storage and patient carrying. Patients save the trouble of decocting when using them. Even if they are on business trips or traveling, they will not interrupt treatment, which is conducive to expanding overseas markets. The standard for particle size of granules in General Chapter 0104 of Part IV of the Chinese Pharmacopoeia is: Unless otherwise specified, the double sieve method is used for determination. The sum of the particles that cannot pass through the No. 1 sieve (10 mesh) and the particles that can pass through the No. 5 sieve (80 mesh) shall not exceed 15%. Granules that meet this particle size standard have good fluidity, are evenly distributed, and are not easy to absorb moisture, which is conducive to bagging in large-scale industrial production processes;

[0004] The general preparation method of Chinese medicine preparation is to add Chinese medicine pieces according to proportion, add water and boil together, and concentrate into extract. The preparation process is as follows: ① The extract is oven-dried. The oven drying obtains a large sample, which needs to be crushed and sieved to obtain the granules required by the Chinese Pharmacopoeia (the sum of the samples that cannot pass through the No. 1 sieve and the samples that can pass through the No. 5 sieve shall not exceed 15%). There will be material loss during the crushing and sieving process. This method is cumbersome and has a low yield; ② The extract is directly added with auxiliary materials for wet granulation, and then the wet granules are dried, sorted and sieved to obtain qualified granules. Although this method is simple to operate, it is limited to the fact that the extract yield of classic prescription products is relatively high, and a large amount of auxiliary materials need to be added to carry the extract; ③ The extract is directly granulated and dried in a fluidized bed. Although this method is better than ①②, for heat-sensitive components, the granulation time is longer, and the loss of heat-sensitive volatile components is relatively large during the process. The extract auxiliary material ratio limit is about 1:1, and the auxiliary material dosage cannot reach the optimal amount. Therefore, the present invention proposes a preparation process of Zhenwu Decoction granules to solve the problems existing in the prior art. Summary of the invention

[0005] In view of the above problems, the present invention proposes a preparation process of Zhenwu Decoction granules. In the preparation process of Zhenwu Decoction granules, Poria cocos, white peony root, ginger, aconite root, and Atractylodes macrocephala are decocted together with water, concentrated at low temperature, spray-dried, dry granulated, and sifted to obtain granules, thereby retaining volatile components and heat-sensitive components to the greatest extent and having uniform and stable quality.

[0006] To achieve the purpose of the present invention, the present invention is implemented by the following technical scheme: a preparation process of Zhenwu Decoction granules, comprising the following steps:

[0007] S1: Prepare raw materials: Poria cocos, white peony root, ginger, Atractylodes macrocephala and Aconitum;

[0008] S2: using condensation reflux extraction, adding water to the prepared raw materials and reflux boiling and extracting 1-3 times, adding 6-8 times of water each time, extracting for 0.5-2 hours each time, and cooling to 60-70°C;

[0009] S3: The filtrates are combined and concentrated under reduced pressure to obtain an extract with a relative density of 1.10-1.15 (50°C), which is spray-dried into a dry extract powder;

[0010] S4: Mix the excipients with the dry paste powder and compress into granules in a dry granulator.

[0011] A further improvement is that in S1, the ratio of Poria cocos, white peony root, ginger, Atractylodes macrocephala and Aconitum carmichaelii is 2.76:2.76:2.76:1.84:1.

[0012] A further improvement is that in S2, after the extraction is completed, the extract is immediately cooled to 60-70°C and stored in a sealed container.

[0013] A further improvement is that in said S3, during the process of reduced pressure concentration, the temperature is maintained at 60-70°C.

[0014] A further improvement is that in S4, the excipient is a mixture of one or more of dextrin, maltodextrin, lactose and sucrose.

[0015] A further improvement is that in S4, granulation comprises the following steps:

[0016] S41: Add the dry paste powder and excipients into a mixing granulator and mix with a stirring and granulating knife for 2-10 minutes;

[0017] S42: placing the mixed dry powder in a clean container barrel, adding the premixed material into the feed port of the dry granulator, and performing dry granulation;

[0018] S43: Collect the obtained particles, sieve them through a rotary vibrating sieve, and collect qualified particles.

[0019] A further improvement is that in S41, the stirring speed is 120 rpm and the granulating knife speed is 1500 rpm.

[0020] Further improvement is that in the S42, during dry granulation, the stirring speed is controlled to 20-40 rpm, the feeding speed is controlled to 120-160 rpm, the pressing wheel speed is controlled to 12-25 rpm, the screen mesh is 10 mesh, the hydraulic pressure is controlled to 3-10Mpa, the upper pressing wheel water temperature is controlled to 22-30°C, the lower pressing wheel water temperature is controlled to 22-30°C, the granulation speed is controlled to 120-160 rpm, and the crushing speed is controlled to 100-160 rpm.

[0021] The beneficial effects of the present invention are:

[0022] 1. In the extraction process of the present invention, condensation reflux extraction is adopted to ensure that the volatile components are retained in the extract. After the extraction is completed, the extract is quickly cooled to 60-70°C and sealed for storage. The temperature of the reduced pressure concentration process is controlled at 60-70°C to retain the volatile components and heat-sensitive components to the greatest extent.

[0023] 2. The present invention obtains an extract with a relative density of 1.10-1.15 (50°C) by reduced pressure concentration, spray drying into a dry paste powder, and dry granulating and pressing into granules with an excipient. It has been verified that the amount of excipients is optimal, meets the standard of the particle size of the Chinese Pharmacopoeia, has uniform and stable quality, and the key quality attributes are consistent with the key quality attributes of the Zhenwu Decoction material benchmark. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 It is a flow chart of the present invention. DETAILED DESCRIPTION

[0025] In order to deepen the understanding of the present invention, the present invention will be further described in detail below in conjunction with examples. The examples are only used to explain the present invention and do not constitute a limitation on the protection scope of the present invention.

[0026] Embodiment 1

[0027] according to Figure 1 As shown, this embodiment proposes a preparation process of Zhenwu Decoction granules, comprising the following steps:

[0028] Prepare the raw materials: Poria cocos, white peony root, ginger, Atractylodes macrocephala and Aconite root; the ratio of Poria cocos, white peony root, ginger, Atractylodes macrocephala and Aconite root is 2.76:2.76:2.76:1.84:1;

[0029] Using condensation reflux extraction, add water to the prepared raw materials and reflux and decoct them once, add 6 times the amount of water each time, and extract for 0.5 hours each time. After the extraction is completed, the extract is immediately cooled to 60°C and sealed for storage;

[0030] The filtrates were combined, the temperature was maintained at 60°C, and the extracts were concentrated under reduced pressure to obtain an extract with a relative density of 1.10-1.15 (50°C), and the extracts were spray-dried into dry extract powder;

[0031] The excipient is mixed with the dry paste powder and pressed into granules in a dry granulator, wherein the excipient is a mixture of one or more of dextrin, maltodextrin, lactose and sucrose as an auxiliary material; the granulation comprises the following steps:

[0032] Add the dry paste powder and excipients into a mixing granulator and mix with a granulator for 2 minutes at a stirring speed of 120 rpm and a granulator speed of 1500 rpm;

[0033] Place the mixed dry powder in a clean container barrel, add the premixed material into the feed port of the dry granulator for dry granulation, control the stirring speed to 20 rpm, the feeding speed to 120 rpm, the pressing wheel speed to 12 rpm, the screen mesh to 10 mesh, the hydraulic pressure to 3 MPa, the upper pressing wheel water temperature to 22°C, the lower pressing wheel water temperature to 22°C, the granulation speed to 120 rpm, and the crushing speed to 100 rpm;

[0034] The obtained granules are collected, and the whole granules are screened with a rotary vibrating sieve to collect qualified granules; the particle size of the prepared granules meets the particle size standard of the Chinese Pharmacopoeia, the quality is uniform and stable, and the key quality attributes are consistent with the key quality attributes of the Zhenwu Decoction material benchmark. The Zhenwu Decoction material benchmark refers to a traditional Chinese medicine prepared based on the preparation method of ancient classic prescriptions recorded in ancient medical books. Except for the molding process, the other preparation methods should be basically consistent with the records in ancient medical books.

[0035] Embodiment 2

[0036] according to Figure 1 As shown, this embodiment proposes a preparation process of Zhenwu Decoction granules, comprising the following steps:

[0037] Prepare the raw materials: Poria cocos, white peony root, ginger, Atractylodes macrocephala and Aconite root; the ratio of Poria cocos, white peony root, ginger, Atractylodes macrocephala and Aconite root is 2.76:2.76:2.76:1.84:1;

[0038] Using condensation reflux extraction, the prepared raw materials are added with water and refluxed and boiled for extraction twice, with 7 times the amount of water added each time, and each extraction lasts for 1 hour. After the extraction is completed, the extract is immediately cooled to 65°C and sealed for storage;

[0039] The filtrates were combined, the temperature was maintained at 65°C, and the extracts were concentrated under reduced pressure to obtain an extract with a relative density of 1.10-1.15 (50°C), and the extracts were spray-dried into dry extract powder;

[0040] The excipient is mixed with the dry paste powder and pressed into granules in a dry granulator, wherein the excipient is a mixture of one or more of dextrin, maltodextrin, lactose and sucrose as an auxiliary material; the granulation comprises the following steps:

[0041] Add the dry paste powder and excipients into a mixing granulator and mix with a granulator for 5 minutes at a stirring speed of 120 rpm and a granulator speed of 1500 rpm;

[0042] Place the mixed dry powder in a clean container barrel, add the premixed material into the feed port of the dry granulator for dry granulation, control the stirring speed to 30 rpm, the feeding speed to 140 rpm, the pressing wheel speed to 20 rpm, the screen mesh to 10 mesh, the hydraulic pressure to 7 MPa, the upper pressing wheel water temperature to 25°C, the lower pressing wheel water temperature to 25°C, the granulation speed to 140 rpm, and the crushing speed to 130 rpm;

[0043] The obtained granules are collected, and the whole granules are screened with a rotary vibrating sieve to collect qualified granules; the particle size of the prepared granules meets the particle size standard of the Chinese Pharmacopoeia, the quality is uniform and stable, and the key quality attributes are consistent with the key quality attributes of the Zhenwu Decoction material benchmark. The Zhenwu Decoction material benchmark refers to a traditional Chinese medicine prepared based on the preparation method of ancient classic prescriptions recorded in ancient medical books. Except for the molding process, the other preparation methods should be basically consistent with the records in ancient medical books.

[0044] Embodiment 3

[0045] according to Figure 1 As shown, this embodiment proposes a preparation process of Zhenwu Decoction granules, comprising the following steps:

[0046] Prepare the raw materials: Poria cocos, white peony root, ginger, Atractylodes macrocephala and Aconite root; the ratio of Poria cocos, white peony root, ginger, Atractylodes macrocephala and Aconite root is 2.76:2.76:2.76:1.84:1;

[0047] The condensation reflux extraction was adopted. The prepared raw materials were added with water and refluxed and boiled for extraction 3 times. Each time, 8 times of water was added. Each extraction lasted for 2 hours. After the extraction was completed, the extract was immediately cooled to 70°C and sealed for storage.

[0048] The filtrates were combined, the temperature was maintained at 70°C, and the extracts were concentrated under reduced pressure to obtain an extract with a relative density of 1.10-1.15 (50°C), and the extracts were spray-dried into dry extract powder;

[0049] The excipient is mixed with the dry paste powder and pressed into granules in a dry granulator, wherein the excipient is a mixture of one or more of dextrin, maltodextrin, lactose and sucrose as an auxiliary material; the granulation comprises the following steps:

[0050] Add the dry paste powder and excipients into a mixing granulator and mix with a granulator for 10 minutes at a stirring speed of 120 rpm and a granulator speed of 1500 rpm;

[0051] Place the mixed dry powder in a clean container barrel, add the premixed material into the feed port of the dry granulator for dry granulation, control the stirring speed to 40 rpm, the feeding speed to 160 rpm, the pressing wheel speed to 25 rpm, the screen mesh to 10 mesh, the hydraulic pressure to 10 MPa, the upper pressing wheel water temperature to 30°C, the lower pressing wheel water temperature to 30°C, the granulation speed to 160 rpm, and the crushing speed to 160 rpm;

[0052] The obtained granules are collected, and the whole granules are screened with a rotary vibrating sieve to collect qualified granules; the particle size of the prepared granules meets the particle size standard of the Chinese Pharmacopoeia, the quality is uniform and stable, and the key quality attributes are consistent with the key quality attributes of the Zhenwu Decoction material benchmark. The Zhenwu Decoction material benchmark refers to a traditional Chinese medicine prepared based on the preparation method of ancient classic prescriptions recorded in ancient medical books. Except for the molding process, the other preparation methods should be basically consistent with the records in ancient medical books.

[0053] Spray drying is a drying method that uses an atomizer to disperse the raw material liquid into droplets and uses hot gas (air, nitrogen or superheated steam) to dry the droplets to obtain a product. This method obtains a powder with very small particles, more than 90% of which can pass through the No. 5 sieve and do not meet the particle size standards of the Chinese Pharmacopoeia. Therefore, in order to obtain granule size standards that meet the Chinese Pharmacopoeia, the powder needs to be wet granulated or dry granulated; extract refers to the concentrated liquid obtained by decocting, filtering and concentrating the Chinese herbal medicine slices in the prescribed proportion.

[0054] Verification Example: Comparison of Examples 1, 2, and 3 with the prior art, the prior art is the actual situation of fluidized bed spray granulation

[0055]

[0056] During the extraction process, the Zhenwu Decoction granule preparation process adopts condensation reflux extraction to ensure that the volatile components are retained in the extract. After the extraction, the extract is quickly cooled to 60-70°C and stored in a sealed manner. The temperature of the vacuum concentration process is controlled at 60-70°C to retain the volatile components and heat-sensitive components to the greatest extent. The vacuum concentration produces an extract with a relative density of 1.10-1.15 (50°C), which is spray-dried into a dry paste powder, and dry-granulated and pressed into granules with excipients. It has been verified that the amount of excipients is optimal and meets the particle size standard of the Chinese Pharmacopoeia. The quality is uniform and stable, and the key quality attributes are consistent with the key quality attributes of the Zhenwu Decoction material benchmark.

[0057] The above shows and describes the basic principles, main features and advantages of the present invention. It should be understood by those skilled in the art that the present invention is not limited to the above embodiments. The above embodiments and descriptions are only for explaining the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, which fall within the scope of the present invention. The scope of protection of the present invention is defined by the attached claims and their equivalents.

Claims

1. A process for preparing Zhenwu Decoction granules, characterized in that: The following steps are involved: S1: Prepare raw materials: Poria cocos, white peony root, ginger, Atractylodes macrocephala and Aconitum; S2: using condensation reflux extraction, adding water to the prepared raw materials and reflux boiling and extracting 1-3 times, adding 6-8 times of water each time, extracting for 0.5-2 hours each time, and cooling to 60-70°C; S3: The filtrates are combined and concentrated under reduced pressure to obtain an extract with a relative density of 1.10-1.15 (50°C), which is spray-dried into a dry extract powder; S4: Mix the excipients with the dry paste powder and compress into granules in a dry granulator.

2. The process for preparing Zhenwu Decoction granules according to claim 1, characterized in that: In S1, the ratio of Poria cocos, white peony root, ginger, Atractylodes macrocephala and Aconitum carmichaelii is 2.76:2.76:2.76:1.84:

1.

3. The process for preparing Zhenwu Decoction granules according to claim 1, characterized in that: The ginger is fresh ginger, and the aconite root is Heishunpian.

4. The process for preparing Zhenwu Decoction granules according to claim 1, characterized in that: In S2, after the extraction is completed, the extract is immediately cooled to 60-70°C and stored in a sealed container.

5. The process for preparing Zhenwu Decoction granules according to claim 1, characterized in that: In S3, during the process of reduced pressure concentration, the temperature is maintained at 60-70°C.

6. The process for preparing Zhenwu Decoction granules according to claim 1, characterized in that: In S4, the excipient is a mixture of one or more of dextrin, maltodextrin, lactose and sucrose.

7. The process for preparing Zhenwu Decoction granules according to claim 6, characterized in that: In S4, granulation comprises the following steps: S41: Add the dry paste powder and excipients into a mixing granulator and mix with a stirring and granulating knife for 2-10 minutes; S42: placing the mixed dry powder in a clean container barrel, adding the premixed material into the feed port of the dry granulator, and performing dry granulation; S43: Collect the obtained particles, sieve them through a rotary vibrating sieve, and collect qualified particles.

8. The process for preparing Zhenwu Decoction granules according to claim 7, characterized in that: In the S41, the stirring speed is 120 rpm, and the granulating knife speed is 1500 rpm.

9. The process for preparing Zhenwu Decoction granules according to claim 7, characterized in that: In the S42, during dry granulation, the stirring speed is controlled at 20-40 rpm, the feeding speed is controlled at 120-160 rpm, the pressing wheel speed is controlled at 12-25 rpm, the screen mesh is 10 mesh, the hydraulic pressure is controlled at 3-10 MPa, the upper pressing wheel water temperature is controlled at 22-30°C, the lower pressing wheel water temperature is controlled at 22-30°C, the granulation speed is controlled at 120-160 rpm, and the crushing speed is controlled at 100-160 rpm.

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