Preparation method and product of Jinzhi detoxification granules

Abstract

The invention discloses a preparation method of herba artemisiae scopariae and fructus gardeniae detoxification granules and a product thereof. The herba artemisiae scopariae and fructus gardeniae detoxification granules are prepared from the following raw materials in parts by weight: 340-380 parts of herba artemisiae scopariae, 160-200 parts of fructus gardeniae, 180-220 parts of rhizoma polygoni cuspidati, 260-300 parts of radix scutellariae and 180-220 parts of ramulus uncariae cum uncis. Separately extracting polygonum cuspidatum into a polygonum cuspidatum alcohol extract, and concentrating the polygonum cuspidatum alcohol extract and the decoction to obtain an extract; and then crushing with other raw material extracts, mixing with cane sugar and dextrin, and carrying out dry granulation. The problem that the thin-layer identification of polygonum cuspidatum is interfered by co-extraction of oriental wormwood and polygonum cuspidatum is solved; according to the invention, through the processes of respectively preparing the extracts, mixing and then carrying out dry granulation, the contact of the oriental wormwood and the polygonum cuspidatum in a liquid state can be avoided, and the problem that the co-extraction of the oriental wormwood and the polygonum cuspidatum disturbs the thin-layer identification of the polygonum cuspidatum is solved; the preparation method is improved on the basis of the national standard, it is guaranteed that thin-layer identification of the polygonum cuspidatum is qualified, other detection items of the product all meet the requirements, and the actual large-scale production requirement can be met.

Description

Technical Field

[0001] The present invention relates to the technical field of traditional Chinese veterinary medicine preparations, and in particular to a preparation method of Yinzhi Jiedu granules and a product thereof. Background Art

[0002] Yinzhi Jiedu Granules are composed of Artemisia capillaris, Gardenia jasminoides, Polygonum cuspidatum, Scutellaria baicalensis, and Uncaria rhynchophylla. They have the effects of clearing heat and detoxifying, soothing the liver and relieving spasms, and are used to treat viral hepatitis in ducklings. This product is included in the Traditional Chinese Medicine Volume of the "Quality Standards for Veterinary Drugs." The following problems exist in the production and inspection of the product: After Yinzhi Jiedu Granules are prepared according to the [Preparation Method] in the Traditional Chinese Medicine Volume of the "Quality Standards for Veterinary Drugs," when the [Identification 4] test is performed, the Polygonum cuspidatum thin layer identification test fails, and the spots of emodin and emodin methyl ether are light in color or not displayed; the Polygonum cuspidatum medicinal material used in the product meets the quality standard requirements of Part II of the 2020 edition of the "Chinese Veterinary Pharmacopoeia." However, with the continuous improvement of the country's requirements for pharmaceutical quality, there are currently few relevant research reports on the product process in the field of veterinary preparations.

[0003] Therefore, it is urgent to design a product preparation method to improve the thin layer identification of Polygonum cuspidatum in Yinzhi Jiedu Granules. Summary of the Invention

[0004] The purpose of the present invention is to provide a method for preparing Yinzhi Jiedu granules to solve the problems existing in the above-mentioned prior art.

[0005] To achieve the above object, the present invention provides the following solution: The present invention provides a method for preparing Yinzhi Jiedu Granules, which are prepared from the following raw materials in parts by weight: 340-380 parts of Artemisia capillaris, 160-200 parts of Gardenia jasminoides, 180-220 parts of Polygonum cuspidatum, 260-300 parts of Scutellaria baicalensis, and 180-220 parts of Uncaria rhynchophylla; Putting Polygonum cuspidatum and 360-440 parts of 95% ethanol into an extraction tank, completely soaking the Polygonum cuspidatum to obtain a Polygonum cuspidatum alcohol extract; transferring the Polygonum cuspidatum alcohol extract to a storage tank; Add 1600L of water into the extraction tank and soak the knotweed for 2.5 hours to obtain a knotweed soaking liquid; transfer the knotweed soaking liquid to another storage tank; 2000L of water was added to the extraction tank to decoct the knotweed, and the first stock solution was obtained after sieving; 1600L of water was added again to decoct the knotweed for the second time, and the second stock solution was obtained after sieving; the second stock solution was mixed with the first stock solution and concentrated to obtain a decoction concentrate; The alcohol extract of Polygonum cuspidatum, the soaking liquid of Polygonum cuspidatum and the decoction concentrate are combined and filtered, and concentrated to a relative density of 1.08 using a double-effect concentrator, and then transferred to a scraper concentrator and concentrated to a relative density of 1.30; after obtaining a clear paste, it is crushed to obtain a Polygonum cuspidatum extract; Put Artemisia capillaris, Gardenia jasminoides, Scutellaria baicalensis and Uncaria rhynchophylla into an extraction tank, add 9200L of water to soak for 2 hours, and then decoct for 1 hour; after the decoction is completed, sieve to obtain a first medicinal liquid; add 7360L of water again and decoct for 1 hour; after the decoction is completed, sieve to obtain a second medicinal liquid; mix the second medicinal liquid with the first medicinal liquid and concentrate to obtain a decoction medicinal liquid; The decoction was concentrated under negative pressure, and when the relative density reached 1.20, 95% ethanol in an amount twice the volume of the concentrate was added, and the solution was allowed to stand to obtain an alcohol precipitate. The supernatant of the alcohol precipitation liquid is filtered and then evaporated, and concentrated to a relative density of 1.08 using a double-effect concentrator, transferred to a scraper concentrator, and concentrated to a relative density of 1.30, and filtered to obtain a clear paste; The medicinal liquid paste is vacuum dried and crushed to obtain the Yinzhi detoxification extract; The Yinzhi detoxification extract, polygonum cuspidatum extract, sucrose and dextrin are mixed and dry granulated in a certain proportion to prepare Yinzhi detoxification granules.

[0006] The Yinzhi Detoxification Granules are prepared from the following raw materials in parts by weight: 360 parts of Artemisia capillaris, 180 parts of Gardenia jasminoides, 200 parts of Polygonum cuspidatum, 280 parts of Scutellaria baicalensis, and 200 parts of Uncaria rhynchophylla.

[0007] The polygonum cuspidatum is immersed in 95% ethanol for no less than 12 hours.

[0008] A Yinzhi detoxification product, comprising Yinzhi detoxification granules obtained according to a preparation method of Yinzhi detoxification granules.

[0009] The present invention discloses the following technical effects: In the present invention, the polygonum cuspidatum extract is obtained by vacuum drying after decoction and concentration of polygonum cuspidatum alcohol extract, polygonum cuspidatum soaking liquid; the extract is then crushed with other raw material extracts, mixed with sucrose and dextrin, and dry granulated. By preparing the extracts separately and mixing them before dry granulation, the contact between Artemisia capillaris and polygonum cuspidatum in liquid state can be avoided, thus solving the problem of interference of co-extraction of Artemisia capillaris and polygonum cuspidatum medicinal materials with thin-layer identification of polygonum cuspidatum; this preparation method is improved on the basis of the national standard formula, ensuring that the thin-layer identification of polygonum cuspidatum is qualified, and other test items of the product meet the requirements, which can meet the needs of actual large-scale production. BRIEF DESCRIPTION OF THE DRAWINGS

[0010] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0011] Figure 1 This is a schematic diagram of the comparison results of the test of Comparative Example 1 and Comparative Example 2 according to the veterinary drug quality standards; Figure 2Schematic diagram of the comparison results of the thin layer chromatography method between Comparative Example 1 and Comparative Example 2; in, Figure 1 Sample 1 is comparative example 1, sample 2 is comparative example 2, sample 3 is emodin, sample 4 is emodin methyl ether, sample 5 is polygonum cuspidatum reference medicinal material, and sample 6 is polygonum cuspidatum extract; Figure 2 Sample 1 is a 2.5 μL sample of the example, sample 2 is a 5 μL sample of the example, sample 3 is emodin, sample 4 is a control medicinal material of polygonum cuspidatum, sample 5 is a 2.5 μL sample of the example, and sample 6 is 5 μL of the example. DETAILED DESCRIPTION

[0012] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0013] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0014] In Example 1 of the present invention, a Yinzhi Jiedu granule is prepared from 360 kg of Artemisia capillaris, 180 kg of Gardenia jasminoides, 200 kg of Polygonum cuspidatum, 280 kg of Scutellaria baicalensis, and 200 kg of Uncaria rhynchophylla; the specific preparation steps are as follows: Putting Polygonum cuspidatum and 360-440 parts of 95% ethanol into an extraction tank, completely soaking the Polygonum cuspidatum to obtain a Polygonum cuspidatum alcohol extract; transferring the Polygonum cuspidatum alcohol extract to a storage tank; Add 1600L of water into the extraction tank and soak the knotweed for 2.5 hours to obtain a knotweed soaking liquid; transfer the knotweed soaking liquid to another storage tank; 2000L of water was added to the extraction tank to decoct the knotweed, and the first stock solution was obtained after sieving; 1600L of water was added again to decoct the knotweed for the second time, and the second stock solution was obtained after sieving; the second stock solution was mixed with the first stock solution and concentrated to obtain a decoction concentrate; The alcohol extract of Polygonum cuspidatum, the soaking liquid of Polygonum cuspidatum and the decoction concentrate were combined and filtered, and concentrated to a relative density of 1.08 (80°C) using a double-effect concentrator, and then transferred to a scraper concentrator and concentrated to a relative density of 1.30 (80°C); after obtaining a clear paste, it was vacuum-dried and crushed to obtain a Polygonum cuspidatum extract; Put Artemisia capillaris, Gardenia jasminoides, Scutellaria baicalensis and Uncaria rhynchophylla into an extraction tank, add 9200L of water to soak for 2 hours, and then decoct for 1 hour; after the decoction is completed, sieve to obtain a first medicinal liquid; add 7360L of water again and decoct for 1 hour; after the decoction is completed, sieve to obtain a second medicinal liquid; mix the second medicinal liquid with the first medicinal liquid and concentrate to obtain a decoction medicinal liquid; The decoction was concentrated under negative pressure, and when the relative density reached 1.20 (80°C), 95% ethanol (2 times the volume of the concentrate) was added, and the solution was allowed to stand to obtain an alcohol precipitate. The supernatant of the alcohol precipitation liquid is filtered and then evaporated, and concentrated to a relative density of 1.08 using a double-effect concentrator, transferred to a scraper concentrator, and concentrated to a relative density of 1.30 (80°C), and filtered to obtain a clear paste; The medicinal liquid paste is vacuum dried and crushed to obtain the Gardenia odorifera detoxification extract (Polygonum cuspidatum negative); The Yinzhi detoxification extract (Polygonum cuspidatum negative), Polygonum cuspidatum extract, sucrose and dextrin were mixed and dry granulated in a certain proportion to prepare 700 kg of Yinzhi detoxification granules.

[0015] In this embodiment, the Polygonum cuspidatum extract is prepared by using Polygonum cuspidatum alcohol extract, Polygonum cuspidatum soaking liquid and decoction concentrate, and is combined with dry granulation to solve the problem of co-extraction of Artemisia capillaris and Polygonum cuspidatum interfering with the thin layer identification of Polygonum cuspidatum; this preparation method is improved on the basis of the national standard formula, ensuring that the thin layer identification of Polygonum cuspidatum is qualified, and other test items of the product meet the requirements, which can meet the actual large-scale production needs.

[0016] In this embodiment, the principle of using ethanol infiltration is that the anthraquinone components in the medicinal material Polygonum cuspidatum are almost insoluble in water but easily soluble in organic solvents.

[0017] Ethanol is often widely used as an extraction solvent, so this property can be used for alcohol extraction using ethanol. Considering the extraction cost of the solvent, this scheme adopts a combination of ethanol infiltration, water soaking and water extraction of Polygonum cuspidatum, which can meet the requirements of thin layer identification of Polygonum cuspidatum, while reducing the use of ethanol and reducing production costs.

[0018] Furthermore, through research and experiments, it was found that in the conventional production process of Yinzhi Detoxification Granules, Artemisia capillaris and Polygonum cuspidatum are in contact in liquid state, which interferes with the thin layer identification of Polygonum cuspidatum. The mixed extraction production process brings the two into direct contact. At the same time, wet granulation requires extract mixing and granulation, which cannot avoid the extract contact in liquid state, thereby causing Artemisia capillaris to affect the thin layer identification of Polygonum cuspidatum. Furthermore, by preparing the extracts separately and mixing them and then dry granulating them, the contact between Artemisia capillaris and Polygonum cuspidatum in liquid state can be avoided.

[0019] Comparative Example 1 The national standard for Yinzhi Jiedu Granules is prepared according to the preparation method of Yinzhi Jiedu Granules in the 2017 edition of the Chinese medicine volume of the "Quality Standards for Veterinary Drugs", which includes the following steps: Put 360kg of Artemisia capillaris, 180kg of Gardenia jasminoides, 180kg of Scutellaria baicalensis, 200kg of Polygonum cuspidatum and 200kg of Uncaria rhynchophylla in the prescription into the extraction tank, add 8960L of water for decoction, and decoct for 1 hour after boiling.

[0020] The decocted medicinal liquid is pumped into the storage tank, and then 7360L of water is added to the extraction tank. After boiling and decocting for 1 hour, the medicinal liquid is pumped into the storage tank.

[0021] Combine the two decoctions and pump them into a negative pressure concentrator. When the liquid is concentrated to about 1000 L under negative pressure, add ethanol twice the volume of the liquid and let it stand (4°C) for 24 hours.

[0022] The above alcohol precipitation supernatant is filtered and the alcohol is evaporated. When the relative density is 1.08 (80°C) using a double-effect concentrator, it is transferred to a scraper concentrator and concentrated to a relative density of 1.30 (80°C). After filtering, a clear medicinal liquid paste is obtained.

[0023] In the granulation workshop, the clear paste, sucrose and dextrin are granulated and dried in a certain proportion to make 700kg of Yinzhi Detoxification Granules.

[0024] Comparative Example 2 The preparation method of Yinzhi Jiedu Granules (Polygonum cuspidatum alcohol extract) comprises the following steps: 1. Pour 200kg of Polygonum cuspidatum medicinal materials into the extraction tank, add ethanol twice the amount of the medicinal materials to soak the Polygonum cuspidatum medicinal materials for more than 12 hours, until they are completely soaked, and obtain the Polygonum cuspidatum alcohol extract, which is then pumped into the storage tank for later use.

[0025] 2. Add 1600L to the above extraction tank and soak for 2.5 hours. The obtained knotweed soaking liquid is transferred to another storage tank.

[0026] 3. Add 2000L of water to the above-mentioned extraction tank and decoct once for 1 hour. After decoction, filter the first decoction through a 200-mesh sieve and transfer it to a storage tank for standby use. After decoction, add 1600L of water again and decoct for 1 hour. After decoction, filter the second decoction through a 200-mesh sieve and mix it with the first decoction. The decoction is concentrated to a density of 1.07 for standby use.

[0027] 4. Combine the alcohol extract of Polygonum cuspidatum, the soaking liquid of Polygonum cuspidatum and the decoction concentrate, filter them, and use a double-effect concentrator to concentrate them to a relative density of 1.08 (80°C). Then transfer them to a scraper concentrator and concentrate them to a relative density of 1.30 (80°C). After filtering, a clear paste of the medicinal liquid is obtained.

[0028] 5. Add 360 kg of Herba Artemisiae Scopariae, 180 kg of Gardenia Fructus, 180 kg of Radix Scutellariae, and 200 kg of Rhizoma Uncariae to an extraction tank, add 9200 L of water, soak for 2 hours, and then decoct for 1 hour. After decoction, filter the first decoction through a 200-mesh sieve and transfer it to a storage tank for later use. After decoction, add 7360 L of water and decoct again for 1 hour. After decoction, filter the second decoction through a 200-mesh sieve, mix with the first decoction, and concentrate.

[0029] 6. Concentrate the above decoction under negative pressure. When the relative density reaches 1.20 (80°C), add ethanol twice the volume of the concentrate and let it stand at 4°C for 24 hours.

[0030] 7. Filter the above alcohol precipitation supernatant and evaporate the alcohol. Use a double-effect concentrator to concentrate to a relative density of 1.08 (80°C), transfer it to a scraper concentrator, and concentrate it to a relative density of 1.30 (80°C). After filtering, obtain a clear medicinal liquid paste.

[0031] 8. In the granulation workshop, mix the clear pastes from step 4 and step 7 evenly, add a certain proportion of sucrose and dextrin, granulate and dry, and make 700 kg of Yinzhi Jiedu granules.

[0032] The samples in comparative example 1 and comparative example 2 were tested according to the method [Identification 4] of Yinzhi Jiedu Granules in the Chinese medicine volume of the "Quality Standards for Veterinary Drugs": Take 4g of the finely ground powder of this product, add 25mL of chloroform, and ultrasonicate for 20 minutes. Filter, evaporate the filtrate to dryness, and dissolve the residue in 0.5mL of methanol to prepare the test solution. Take 0.6g of Polygonum cuspidatum as a control medicinal material and prepare the control medicinal material solution in the same way.

[0033] Next, take the emodin reference substance and add methanol to create a solution containing 1 mg per 1 mL. For thin-layer chromatography, apply 5 μL of each of the three solutions to the same silica gel G thin-layer plate using toluene-ethyl acetate-formic acid (15:2:1) as the developing solvent. Develop the plate, remove the plate, air-dry it, and examine it under a UV lamp (365 nm). The test sample's chromatogram will display a fluorescent spot of the same color at the corresponding position in the reference sample and reference herbal chromatograms. After exposure to ammonia, the spot turns red.

[0034] Furthermore, by attaching Figure 1 As can be seen, the Polygonum cuspidatum TLC identification in Comparative Examples 1 and 2 failed. These two comparative examples demonstrate that contact between Artemisia capillaris and Polygonum cuspidatum in the liquid phase during the extraction and granulation stages interferes with the TLC identification of Polygonum cuspidatum. Polygonum cuspidatum extract was sampled based on the TLC identification sampling volume of Polygonum cuspidatum and tested according to the [Identification 4] method in the 2017 edition of the Veterinary Drug Quality Standards for Chinese Medicine. The Polygonum cuspidatum extract passed the test and can be used for the next step of dry granulation.

[0035] Furthermore, by attaching Figure 2 It can be seen that the results of the thin layer identification of Polygonum cuspidatum are qualified when the samples are prepared according to the new process of the embodiment and the sample volume is 2.5μL and 5μL; this shows that the preparation method can ensure that the thin layer identification of Polygonum cuspidatum complies with the regulations and meets the judgment requirements of the national standard test of Yinzhi Jiedu Granules.

[0036] In the description of the present invention, it should be understood that the terms "longitudinal", "transverse", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", etc., indicating the orientation or position relationship, are based on the orientation or position relationship shown in the accompanying drawings, and are only for the convenience of describing the present invention, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention.

[0037] The embodiments described above are merely descriptions of preferred embodiments of the present invention and are not intended to limit the scope of the present invention. Without departing from the spirit of the present invention, various modifications and improvements made to the technical solutions of the present invention by persons skilled in the art should fall within the scope of protection defined by the claims of the present invention.

Claims

1. A method for preparing Yinzhi Jiedu granules, characterized in that It is prepared from the following raw materials in parts by weight: 340-380 parts of Artemisia capillaris, 160-200 parts of Gardenia jasminoides, 180-220 parts of Polygonum cuspidatum, 260-300 parts of Scutellaria baicalensis, and 180-220 parts of Uncaria rhynchophylla; Putting Polygonum cuspidatum and 360-440 parts of 95% ethanol into an extraction tank, completely soaking the Polygonum cuspidatum to obtain a Polygonum cuspidatum alcohol extract; transferring the Polygonum cuspidatum alcohol extract to a storage tank; 1600L of water is added to the extraction tank to soak the knotweed to obtain a knotweed soaking liquid; the knotweed soaking liquid is transferred to another storage tank; 2000L of water was added to the extraction tank to decoct the knotweed, and the first stock solution was obtained after sieving; 1600L of water was added again to decoct the knotweed for the second time, and the second stock solution was obtained after sieving; the second stock solution was mixed with the first stock solution and concentrated to obtain a decoction concentrate; The alcohol extract of Polygonum cuspidatum, the soaking liquid of Polygonum cuspidatum and the decoction concentrate are combined and filtered, and concentrated to a relative density of 1.08 using a double-effect concentrator, and then transferred to a scraper concentrator and concentrated to a relative density of 1.30; after obtaining a clear paste, it is crushed to obtain a Polygonum cuspidatum extract; Put Artemisia capillaris, Gardenia jasminoides, Scutellaria baicalensis and Uncaria rhynchophylla into an extraction tank, add 9200L of water to soak for 2 hours, and then decoct for 1 hour; after the decoction is completed, sieve to obtain a first medicinal liquid; add 7360L of water again and decoct for 1 hour; after the decoction is completed, sieve to obtain a second medicinal liquid; mix the second medicinal liquid with the first medicinal liquid and concentrate to obtain a decoction medicinal liquid; The decoction was concentrated under negative pressure, and when the relative density reached 1.20, 95% ethanol in an amount twice the volume of the concentrate was added, and the solution was allowed to stand to obtain an alcohol precipitate. The supernatant of the alcohol precipitation liquid is filtered and then evaporated, and concentrated to a relative density of 1.08 using a double-effect concentrator, transferred to a scraper concentrator, and concentrated to a relative density of 1.30, and filtered to obtain a clear paste; The medicinal liquid paste is vacuum dried and crushed to obtain the Yinzhi detoxification extract; The Yinzhi detoxification extract, the knotweed extract, sucrose and dextrin are mixed and dry granulated in a certain proportion to prepare the Yinzhi detoxification granules.

2. The method for preparing Yinzhi Jiedu Granules according to claim 1, wherein: The Yinzhi Jiedu granules are prepared from the following raw materials in parts by weight: 360 parts of Artemisia capillaris, 180 parts of Gardenia jasminoides, 200 parts of Polygonum cuspidatum, 280 parts of Scutellaria baicalensis, and 200 parts of Uncaria rhynchophylla.

3. The method for preparing Yinzhi Jiedu Granules according to claim 1, wherein: The polygonum cuspidatum is immersed in 95% ethanol for no less than 12 hours.

4. A Yinzhi Jiedu Granule product, which is the Yinzhi Jiedu Granule prepared according to the Yinzhi Jiedu Granule preparation method according to any one of claims 1 to 3.

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