A preparation method of Qi-promoting and blood-activating granules

Abstract

The invention discloses a preparation method of qi-promoting and blood-activating granules, belonging to the technical field of preparation of Chinese patent medicines. The qi-promoting and blood-activating granules of the invention are as follows: after raw materials are subjected to water extraction of volatile oil, water decoction extraction, concentration, drying and pulverization to obtain dry paste powder, a feed speed of 10-25rpm, a feed speed of 20-50rpm, a roller speed of 20-26rpm, and a roller temperature of ≤40°C are set, and the dry paste powder is granulated together with starch and powdered sugar; through the dry granulation method of the invention, the drying link of the granular soft material is reduced, the process loss caused by the strong viscosity of the variety is reduced, the yield of the product is increased by more than 30%, the production cost of the product is saved, and the market competitiveness is significantly improved; no adhesive is added, thereby reducing the risk of exceeding the microbial limit; no ethanol is used, thereby effectively reducing the safety risk caused by environmental pressure; and based on the content of paeoniflorin in red peony root, the content is increased by more than 50%, the efficacy of the product is significantly improved, and it is more conducive to the auxiliary treatment of hyperlipidemia.

Description

Technical Field

[0001] The invention relates to the technical field of preparation of Chinese patent medicines, and in particular to a method for preparing qi-promoting and blood-activating granules. Background Art

[0002] Chinese medicine granules are a commonly used dosage form of Chinese patent medicine. They are usually prepared by extracting Chinese medicinal materials and adding appropriate excipients to form granular preparations. Chinese medicine granules are a supplement to traditional dosage forms. This dosage form has the advantages of easy storage, transportation, use, and rapid onset, and is particularly suitable for children, the elderly and other patients.

[0003] Xingqi Huoxue Granules is one of the granules, which has the effects of promoting qi and blood circulation, invigorating qi and resolving phlegm, and is particularly suitable for the auxiliary treatment of hyperlipidemia of qi deficiency and blood stasis type. This variety is now included in the national drug standard WS-5388-(B-0388)-2014Z. The preparation method is: 12 ingredients including Chuanxiong, Astragalus, Red Peony Root, Peach Kernel, Safflower, Green Peel, Angelica, Atractylodes, Seaweed, Achyranthes, Citrus Aurantium, Platycodon, etc. Among them, volatile oil is extracted from Chuanxiong, Angelica, Peach Kernel, Citrus Aurantium, Green Peel, Atractylodes, and Red Peony Root. The remaining six ingredients including Red Peony Root are decocted twice with 8 times the amount of water and concentrated into a clear paste, ethanol is added to precipitate, the supernatant is concentrated into a thick paste, vacuum dried, and the dry paste is crushed into fine powder. Take 1 part of the fine powder, add medicinal starch, 0.8 parts of powdered sugar and appropriate amount of ethanol to make granules.

[0004] Among them, granulation is a key step in the preparation of Chinese medicine granules. The quality of the granules has a certain influence on the efficacy. The commonly used granulation methods include wet granulation, rapid stirring granulation, etc.

[0005] At present, most of the Chinese medicine granules are granulated by wet method, because of the advantages of wet granulation such as simple preparation process, low equipment requirements, high production efficiency, low energy consumption and wide application. The equipment used includes trough mixer (high-speed mixer), swing granulator, dryer, etc. Among them, trough mixer is an earlier soft material equipment used in preparation production. It is mainly used for uniform mixing of dry or wet powders of different ratios. It is convenient to load materials and easy to operate and control.

[0006] Xingqi Huoxue granules are currently produced by wet granulation. However, this method has the following problems: when making wet soft materials in a trough mixer, it is easy to have dead corners in mixing, resulting in uneven mixing; when the wet soft materials are discharged, the dumping type is used, the discharge is not thorough, and the product transfer rate is low; after drying and whole granulation mixing, the product yield is only 70%-80%, and the content of paeoniflorin in red peony root is 3.11-3.80mg / g. The product yield is extremely low and the content is difficult to meet the standard.

[0007] Therefore, there is an urgent need in the art to improve the preparation method of Qi-activating and blood-activating granules. Summary of the invention

[0008] The purpose of the present invention is to provide a method for preparing Qi-promoting and blood-activating granules to solve the above problems.

[0009] In order to achieve the above object, the technical solution adopted by the present invention is as follows: a method for preparing Qi-promoting and blood-activating granules, comprising the following steps:

[0010] (1) According to the formula, weigh out the original medicinal materials Chuanxiong, Astragalus, Red Peony Root, Peach Kernel, Carthamus tinctorius, Citrus aurantium, Angelica sinensis, Atractylodes lancea, Sargassum, Achyranthes bidentata, Citrus aurantium, and Platycodon grandiflorum, a total of twelve ingredients, of which Chuanxiong, Angelica sinensis, Peach Kernel, Citrus aurantium, Citrus aurantium, and Atractylodes lancea are added with 6-10 times the weight of water to extract volatile oil; the remaining six ingredients are decocted with 6-10 times the weight of water at least once, each time for 0.5-2 hours, and concentrated into a clear paste;

[0011] (2) Add ethanol to the clear paste and stir while adding. Let it stand and take the supernatant to concentrate it into a thick paste.

[0012] (3) Drying the thick paste: The thick paste of step (2) is placed in a pan, the drying temperature is controlled within the range of 60°C to 80°C, and the vacuum degree is -0.04 to -0.06 MPa; and the thick paste is dried to a dry paste, and the moisture content of the dry paste is controlled to be below 3.0%;

[0013] (4) crushing the dry paste into dry paste powder;

[0014] (5) Install the screen, start the dry granulator, set the feed speed to 10-25 rpm, the feeding speed to 20-50 rpm, the roller speed to 20-26 rpm, and the roller temperature to ≤40°C, granulate the dry paste powder with starch and powdered sugar, and add the volatile oil of step (1) to the obtained granules.

[0015] In order to solve the problems existing in the prior art, the inventors of the present application conducted a large number of experiments and analyses: the prescription of Xingqi Huoxue Granules contains 12 ingredients in total. The composition of the prescription was analyzed, among which the main ingredient of Astragalus is the dried root of Astragalusmembranaceus (Fisch.) Bge.var.mongholicus (Bge.) Hsiao or Astragalusmembranaceus (Fisch.) Bge. of the Leguminosae family, and the main ingredients are calycosin glucoside and astragaloside I, and the glycosides will be converted into sugar after hydrolysis; the main ingredient of seaweed is the dried algae of Sargassum pallidum (Turn.) C.Ag. or Sargassum fusiforme (Harv.) Setch. of the Sargassumaceae family, and the main ingredient is fucose. Angelica sinensis is the dried root of Angelica sinensis (Oliv.) Diels, a plant of the Umbelliferae family. Polysaccharides, volatile oils, flavonoids, organic acids, various amino acids, vitamins and trace elements are found in Angelica sinensis, among which Angelica sinensis polysaccharide is one of the main active ingredients. The above three herbs account for nearly 40% of the content in the prescription, and polysaccharides are their main components. After being soaked in water, polysaccharides swell and become sticky, resulting in extremely strong viscosity of the extract after extraction, concentration and heating. The strong viscosity of the variety causes large process losses, resulting in low particle yield and low paeoniflorin content.

[0016] The Qi-activating and Blood-activating Granules of the present invention innovatively adopt a dry granulation preparation method. Dry granulation generally involves uniformly mixing drug powder and auxiliary materials, first pressing them into blocks of a certain size, and then crushing them to form particles of the desired size. Dry granulation usually does not require the addition of any liquid, and relies on the strong pressure generated by the machine to press the drug and auxiliary materials into blocks. In order to ensure that a series of test items such as moisture, properties, particle size, solubility, and content of the particles meet the standards, dry granulation is used. Since dry granulation does not require the addition of any liquid, the moisture content of the extract powder needs to be strictly controlled to ensure that the moisture content of the particles meets the standards during granulation; if the particles are too loose, the particle size will be unqualified; if the particles are too compact, the solubility of the particles will be unqualified.

[0017] In the dry granulation process of the present invention, while ensuring the moisture content of the extract powder (i.e., controlling the moisture content within 3.0% in the drying step of step (3)), the process parameters such as the feed speed, the feeding speed, the roller speed and the roller temperature on the dry granulator are adjusted and optimized to form the particles, ensure that the particle size meets the requirements, and improve the particle yield.

[0018] In dry granulation, the increase in feeding speed and feeding speed will increase the pressure accordingly, thereby improving the yield of particles. However, excessive feeding speed can easily cause blockage, causing the material to adhere to the equipment and cause material loss. If the roller speed is too slow, the hardness and particle size of the dry granules will be too large. The faster the roller speed, the less time the material stays between the two rollers, the plastic deformation of the powder particles decreases, and the particle structure is loose, making some powder-pressed embryos loose. The powder leaks as the roller rolls, causing a sharp drop in the particle yield. Due to the high viscosity of this variety, if the feeding speed and feeding speed are too slow during the dry granulation process, the pressing time will be too long, and too much material will accumulate between the upper and lower rollers. Long-term operation of the equipment will cause the equipment to heat up, affecting the content of paeoniflorin.

[0019] As a preferred technical solution, in step (1), the amount of water added is 8 times the weight of the medicinal material, and the water is decocted twice, each time for 1 hour.

[0020] As a preferred technical solution, in step (5), the feed speed is set to 15 rpm, the delivery speed is set to 35 rpm, and the roller speed is set to 24 rpm. The best particle yield and the highest paeoniflorin content can be obtained.

[0021] Compared with the prior art, the advantages of the present invention are:

[0022] (1) The dry granulation method of the present invention reduces the process loss caused by the strong viscosity of the product, increases the product yield by more than 30%, reduces the drying process of the granular soft material, saves the production cost of the product, and significantly improves the market competitiveness;

[0023] (2) The dry granulation of the present invention does not add a binder, thereby reducing the risk of exceeding the microbial limit;

[0024] (3) The dry granulation process does not use ethanol, which effectively reduces the safety risks caused by environmental pressure;

[0025] (4) Compared with wet granulation (the content of paeoniflorin in the finished product prepared by wet granulation is 3.11-3.8 mg / g, as shown in Table 1 and Figure 9-10 As shown), by adopting the method of the present invention, the content of paeoniflorin in red peony root is increased by more than 50%, which significantly improves the efficacy of the product and is more conducive to the auxiliary treatment of hyperlipidemia.

[0026] Table 1 Comparison of products obtained by different methods

[0027] BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1This is the HPLC chart of the standard product when detecting the content of paeoniflorin in Example 1 of the present invention;

[0029] Figure 2 This is the HPLC graph of the sample when the paeoniflorin content is detected in Example 1 of the present invention;

[0030] Figure 3 This is the HPLC chart of the standard product when detecting the content of paeoniflorin in Example 2 of the present invention;

[0031] Figure 4 HPLC diagram of the sample when detecting the content of paeoniflorin in Example 2 of the present invention

[0032] Figure 5 This is the HPLC chart of the standard product when detecting the content of paeoniflorin in Example 3 of the present invention;

[0033] Figure 6 This is the HPLC graph of the sample when the paeoniflorin content is detected in Example 3 of the present invention;

[0034] Figure 7 This is the HPLC chart of the standard product when detecting the content of paeoniflorin in the comparative example of the present invention;

[0035] Figure 8 The HPLC diagram of the sample when the paeoniflorin content is detected in the comparative example of the present invention;

[0036] Fig. 9 This is the HPLC chart of the standard product when the content of paeoniflorin was detected by wet granulation;

[0037] Fig.10 This is the HPLC chart of the sample when the paeoniflorin content was detected by wet granulation. DETAILED DESCRIPTION

[0038] The present invention will be further described below in conjunction with the accompanying drawings.

[0039] Embodiment 1: The present invention will be further described below in conjunction with embodiment.

[0040] Embodiment 1:

[0041] A method for preparing Qi-promoting and blood-activating granules comprises the following steps:

[0042] (1) 12 ingredients including Chuanxiong, Astragalus, Red Peony Root, Peach Kernel, Safflower, Citrus Aurantii, Angelica Sinensis, Atractylodes, Seaweed, Achyranthes Bidentata, Citrus Aurantium, and Platycodon grandiflorum. Among them, volatile oils are extracted from Chuanxiong, Angelica Sinensis, Peach Kernel, Citrus Aurantium, Citrus Aurantii, and Atractylodes with 8 times the amount of water. The remaining six ingredients including Red Peony Root are decocted twice with 8 times the amount of water for one hour each time, and then concentrated into a clear paste.

[0043] (2) Add ethanol to the clear paste while stirring, let it stand for 24 hours, and take the supernatant to concentrate it into a thick paste;

[0044] (3) Drying the thick paste: put the thick paste into the drying tray at an average weight of 2 kg / tray, control the drying temperature within 60°C, and the vacuum degree of -0.04 to -0.06 MPa; dry it into a dry paste, and control the moisture content of the dry paste to be below 3.0%;

[0045] (4) crushing the dry paste into dry paste powder;

[0046] (5) Install the screen, start the dry granulator, set the feed speed to 10 rpm, the feeding speed to 20 rpm, the roller speed to 20 rpm, and the roller temperature to ≤ 40°C, granulate the dry paste powder together with starch and powdered sugar, add the same amount of auxiliary materials (i.e. starch and powdered sugar) as the amount of dry paste powder, mix the volatile oil in step (1) into the obtained granules, and obtain;

[0047] (6) The granule yield was 96.5% (granule yield = qualified granule quantity / theoretical batch, qualified granules 394 kg, theoretical batch 408 kg). The content of paeoniflorin in the finished product was tested by HPLC. The test conditions were as follows: Figure 1-2 As shown, its content is 4.76 mg / g.

[0048] Example 2

[0049] A method for preparing Qi-promoting and blood-activating granules comprises the following steps:

[0050] (1) 12 ingredients including Chuanxiong, Astragalus, Red Peony Root, Peach Kernel, Safflower, Citrus Aurantii, Angelica Sinensis, Atractylodes, Seaweed, Achyranthes Bidentata, Citrus Aurantium, and Platycodon grandiflorum. Among them, volatile oils are extracted from Chuanxiong, Angelica Sinensis, Peach Kernel, Citrus Aurantium, Citrus Aurantii, and Atractylodes with 8 times the amount of water. The remaining six ingredients including Red Peony Root are decocted twice with 8 times the amount of water for one hour each time, and then concentrated into a clear paste.

[0051] (2) Add ethanol to the clear paste while stirring, let it stand for 24 hours, and take the supernatant to concentrate it into a thick paste;

[0052] (3) Drying the thick paste: put the thick paste into the drying tray at an average weight of 2 kg / tray, control the drying temperature within 80°C, and the vacuum degree at -0.04 to -0.06 MPa; dry it into a dry paste;

[0053] (4) crushing the dry paste into dry paste powder;

[0054] (5) Install the screen, start the dry granulator, set the feed speed to 25 rpm, the feeding speed to 50 rpm, the roller speed to 26 rpm, and the roller temperature to ≤40°C, granulate the dry paste powder, starch, and powdered sugar together, and add the same amount of auxiliary materials as the dry paste powder. Add the volatile oil in step (1) to the obtained granules to obtain the product;

[0055] (6) The granule yield was 90.5%. The content of paeoniflorin in the finished product was detected using the same HPLC method as in Example 1. The results were as follows: Figure 3-4 As shown, its content is 4.83 mg / g.

[0056] Example 3

[0057] A method for preparing Qi-promoting and blood-activating granules comprises the following steps:

[0058] (1) 12 ingredients including Chuanxiong, Astragalus, Red Peony Root, Peach Kernel, Safflower, Citrus Aurantii, Angelica Sinensis, Atractylodes, Seaweed, Achyranthes Bidentata, Citrus Aurantium, and Platycodon grandiflorum. Among them, volatile oils are extracted from Chuanxiong, Angelica Sinensis, Peach Kernel, Citrus Aurantium, Citrus Aurantii, and Atractylodes with 8 times the amount of water. The remaining six ingredients including Red Peony Root are decocted twice with 8 times the amount of water for one hour each time, and then concentrated into a clear paste.

[0059] (2) Add ethanol to the clear paste while stirring, let it stand for 24 hours, and take the supernatant to concentrate it into a thick paste;

[0060] (3) Drying the thick paste: put the thick paste into the drying tray at an average weight of 2 kg / tray, control the drying temperature within 80°C, and the vacuum degree at -0.04 to -0.06 MPa; dry it into a dry paste;

[0061] (4) crushing the dry paste into dry paste powder;

[0062] (5) Install the screen, start the dry granulator, set the feed speed to 15 rpm, the feeding speed to 35 rpm, the roller speed to 24 rpm, and the roller temperature to ≤40°C, granulate the dry paste powder, starch, and powdered sugar together, add the same amount of auxiliary materials as the dry paste powder, mix the volatile oil in step (1) into the obtained granules, and obtain;

[0063] (6) The granule yield was 105.6%. The content of paeoniflorin in the finished product was detected using the same HPLC method as in Example 1. The results were as follows: Figure 5-6 As shown, its content is 5.42 mg / g.

[0064] Comparative Example

[0065] A method for preparing Qi-promoting and blood-activating granules comprises the following steps:

[0066] (1) 12 ingredients including Chuanxiong, Astragalus, Red Peony Root, Peach Kernel, Safflower, Citrus Aurantii, Angelica Sinensis, Atractylodes, Seaweed, Achyranthes Bidentata, Citrus Aurantium, and Platycodon grandiflorum. Among them, volatile oils are extracted from Chuanxiong, Angelica Sinensis, Peach Kernel, Citrus Aurantium, Citrus Aurantii, and Atractylodes with 8 times the amount of water. The remaining six ingredients including Red Peony Root are decocted twice with 8 times the amount of water for one hour each time, and then concentrated into a clear paste.

[0067] (2) Add ethanol to the clear paste while stirring, let it stand for 24 hours, and take the supernatant to concentrate it into a thick paste;

[0068] (3) Drying the thick paste: put the thick paste into the drying tray at an average weight of 2 kg / tray, control the drying temperature within 80°C, and the vacuum degree at -0.04 to -0.06 MPa; dry it into a dry paste;

[0069] (4) crushing the dry paste into dry paste powder;

[0070] (5) Install the screen, start the dry granulator, set the feed speed to 5rpm, the feeding speed to 20rpm, the roller speed to 5rpm, the roller temperature to ≤40℃, granulate the dry paste powder together with starch and powdered sugar, and the amount of auxiliary materials added should be equal to the amount of dry paste powder;

[0071] (6) The granule yield was 77.5%. The content of paeoniflorin in the finished product was detected using the same HPLC method as in Example 1. The results were as follows: Figure 7-8 As shown, its content is 3.33 mg / g.

[0072] This shows that the process parameters such as feeding speed, feeding speed, roller speed and roller temperature during granulation are relatively critical, and these process parameters will also affect the granule yield and paeoniflorin content of the finished product.

[0073] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing Qi-promoting and blood-activating granules, characterized in that: The steps include: (1) According to the formula, weigh out the original medicinal materials Chuanxiong, Astragalus, Red Peony Root, Peach Kernel, Carthamus tinctorius, Citrus aurantium, Angelica sinensis, Atractylodes lancea, Sargassum, Achyranthes bidentata, Citrus aurantium, and Platycodon grandiflorum, a total of twelve ingredients, of which Chuanxiong, Angelica sinensis, Peach Kernel, Citrus aurantium, Citrus aurantium, and Atractylodes lancea are added with 6-10 times the weight of water to extract volatile oil; the remaining six ingredients are decocted with 6-10 times the weight of water at least once, each time for 0.5-2 hours, and concentrated into a clear paste; (2) Add ethanol to the clear paste and precipitate it while stirring. Let it stand and take the supernatant to concentrate it into a thick paste. (3) Drying the thick paste: The thick paste obtained in step (2) is placed in a pan, the drying temperature is controlled within the range of 60°C to 80°C, and the vacuum degree is -0.04 to -0.06 MPa; and dried into a dry paste; (4) crushing the dry paste into dry paste powder; (5) Install the screen, start the dry granulator, set the feed speed to 10-25 rpm, the feeding speed to 20-50 rpm, the roller speed to 20-26 rpm, and the roller temperature to ≤40°C, granulate the dry paste powder with starch and powdered sugar, and then add the volatile oil of step (1) to the obtained granules.

2. The method for preparing the Qi-activating and blood-activating granules according to claim 1, characterized in that: In step (1), the amount of water added is 8 times the weight of the medicinal material, and the mixture is decocted in water twice, each time for 1 hour.

3. The method for preparing Qi-activating and blood-activating granules according to claim 1, characterized in that: In step (5), the feed speed is set to 15 rpm, the delivery speed is set to 35 rpm, and the pressure roller speed is set to 24 rpm.

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