Earthworm extract concentrated solution pre-drying process and radix astragali and dragon capsule preparation process

Abstract

The invention provides an earthworm extract concentrated solution pre-drying process and a Qilong capsule preparation process thereof, and relates to the technical field of Qilong capsule production and preparation. Comprising the following steps: S1, stirring and foaming an earthworm microfiltration concentrated solution with a certain relative density to obtain a concentrated solution with a certain foam density; s2, carrying out gradient vacuum drying on the concentrated solution with a certain foam density at the temperature of 40-48 DEG C to obtain a pre-dried material; by controlling the relative density and the foam density of the earthworm microfiltration concentrated solution, the relative density and the foam density are controlled within a certain range, so that the problem that the earthworm microfiltration concentrated solution is stuck to a machine in the pre-drying process is solved.

Description

Technical Field

[0001] The invention relates to the technical field of Qilong capsule production and preparation, and in particular to a pre-drying process for a concentrated earthworm extract and a Qilong capsule preparation process thereof. Background Art

[0002] During the production process of Qilong Capsules, the raw materials such as astragalus and earthworm need to be pre-processed. There is a problem of sticking to the machine during the extraction of earthworm extract. If the sticky material cannot be removed in time, on the one hand, it will cause the material to burn or deteriorate, affecting the product quality; on the other hand, when the sticking phenomenon is serious, in order to remove the sticky material, the preparation has to be stopped midway, which prolongs the operation cycle and reduces production efficiency.

[0003] The Chinese invention patent with patent publication number CN1541683A discloses an anti-thrombotic Qilong capsule. Although the main formula of Qilong capsule is disclosed, the application does not focus on the problem of sticking to the machine during the pre-drying and concentration process of earthworm extract. In order to improve the product quality of Qilong capsule and reduce the production cost, it is necessary to further optimize the production process of Qilong capsule. Summary of the invention

[0004] In order to solve the above problems, the inventors have found that the density of the earthworm microfiltration concentrate affects the degree of pre-drying. If the density of the concentrate is greater than 1.22g / cm3, the concentrate is very viscous and cannot be directly placed on the belt dryer by the feed pump, and will adhere to the feed pump. The foaming degree of the earthworm microfiltration concentrate affects the sticking machine problem. If the foaming process is not stirred before entering the belt dryer, the dried material will be adhered to the belt dryer. On the one hand, it is difficult to clean and affect the continued drying of subsequent materials, and on the other hand, it affects the quality of the earthworm concentrate product. The present application controls the relative density and foam density of the earthworm microfiltration concentrate within a certain range, thereby solving the problem of sticking machine during the pre-drying process of the earthworm microfiltration concentrate.

[0005] A first aspect of the present invention provides a pre-drying process for a concentrated solution of an earthworm extract, the pre-drying process for a concentrated solution of an earthworm extract comprising the following steps:

[0006] S1: stirring and foaming the earthworm microfiltration concentrate with a certain relative density to obtain a concentrate with a certain foam density.

[0007] S2: The concentrated liquid with a certain foam density is subjected to gradient vacuum drying at a temperature of 40-48°C to obtain pre-dried material. Figure 1 shown.

[0008] Among them, the relative density is not higher than 1.22g / cm 3 , foam density 120-180 quantity / mm 2; The moisture content in the pre-dried material is not higher than 15%.

[0009] Optionally, the gradient drying temperature in step S2 includes sequentially passing through the temperature of zone 1 at 45-48°C, the temperature of zone 2 at 45-48°C, the temperature of zone 3 at 44-46°C, and the temperature of zone 4 at 25-28°C. In the pre-drying process, the pre-dried material can be driven by a transmission motor on the belt dryer to first pass through the temperature of zone 1 and zone 2 for preliminary and long-term drying, and then pass through the temperature of zone 3, and the temperature drops slightly to prevent the continuous high temperature from causing the temperature of the material to be dried to exceed 50°C, affecting the activity of active ingredients such as autolytic enzymes, thereby affecting the quality of the product. On the other hand, it provides a transition for the subsequent temperature drop to further dry the material. Finally, the temperature is lowered so that the material is easy to desorb from the belt dryer at low temperatures.

[0010] Optionally, the pre-drying process of the concentrated earthworm extract solution further comprises the following steps:

[0011] S01: autolyzing and centrifuging the earthworm in sequence to obtain a centrifuge solution;

[0012] S02: subjecting the centrifuge to microfiltration and ultrafiltration treatments in sequence to obtain a microfiltrate;

[0013] S03: Concentrating the microfiltrate at a temperature not higher than 45° C. to obtain a microfiltrate concentrate of earthworms;

[0014] Among them, the temperature of autolysis in step S01 is 42-48°C, and the autolysis time is 16-19h. Furthermore, earthworms themselves have autolytic enzymes that play a role in dissolution. If the temperature is higher than 50°C, it will affect the activity of the autolytic enzymes, thereby affecting the quality of the product.

[0015] In step S02, the molecular weight cut-off is above 6,000 during the ultrafiltration process. The earthworm extract with a molecular weight below 6,000 can be made into an oral liquid, but the present invention is not limited thereto.

[0016] Optionally, the ultrafiltration membrane in the ultrafiltration process is a hollow fiber ultrafiltration membrane, which includes, by weight, 10-20 parts of polyethersulfone, 10-20 parts of modified polyacrylonitrile, 5-10 parts of carboxylated polyethyleneimine, 5-10 parts of polyethylene glycol, 2-7 parts of functional filler, and 2-10 parts of glutaraldehyde.

[0017] Optionally, the preparation method of the modified polyacrylonitrile comprises the following steps:

[0018] S1: mixing polyacrylonitrile and N,N-dimethylformamide to react to obtain a first mixture;

[0019] S2: mixing the first mixture with hydroxylamine hydrochloride, adjusting the pH to 6, reacting at a temperature of 60-70° C., and then washing and drying to obtain modified polyacrylonitrile;

[0020] The mass ratio of polyacrylonitrile to N,N-dimethylformamide is 1:(4-7).

[0021] Optionally, the method for preparing the functional filler comprises the following steps:

[0022] (1) mixing the nanoparticles with dopamine hydrochloride and tris(hydroxymethyl)aminomethane solution, reacting at room temperature, washing, and drying to obtain an intermediate;

[0023] (2) adding the intermediate obtained in step (1) to a tris(hydroxymethyl)aminomethane solution, and then adding potassium salt of 3-sulfonate propyl methacrylate, reacting at room temperature, and washing and drying the product in sequence to obtain a functional filler;

[0024] Among them, the nanoparticles are nano-silicon dioxide and nano-titanium dioxide;

[0025] The mass ratio of nanoparticles, dopamine hydrochloride and 3-sulfonate propyl methacrylate potassium salt is (1-3):1:(15-20).

[0026] Optionally, the preparation process of the hollow fiber ultrafiltration membrane comprises the following steps: (1) reacting polyethersulfone, modified polyacrylonitrile, carboxylated polyethyleneimine, polyethylene glycol and functional filler in proportion at 40-70° C. to obtain a membrane casting solution;

[0027] (2) pouring the casting solution into a spinning machine for spinning, soaking the obtained membrane fibers in a glutaraldehyde solution, cross-linking at a temperature of 50-60° C., and then washing to obtain a hollow fiber earthworm ultrafiltration membrane.

[0028] The hollow fiber earthworm ultrafiltration membrane prepared by the present invention improves the hydrophilicity of the ultrafiltration membrane, reduces the adsorption of earthworm extract on its surface during the filtration process, and ensures the membrane flux. In addition, it also reduces the adhesion and deposition of microorganisms on the membrane surface, improves the anti-pollution performance of the ultrafiltration membrane, further ensures the retention rate of the effective ingredients in the earthworm extract, lays a foundation for subsequent guarantee of the effective interception molecular weight, and also lays a foundation for subsequent obtaining of earthworm microfiltration concentrate with a certain relative density.

[0029] The second aspect of the present invention provides a preparation process of Qilong capsules, which comprises the above-mentioned pre-drying process of the concentrated earthworm extract and the extraction process of astragalus, salvia miltiorrhiza, peach kernel, safflower, chuanxiong, red peony root and angelica; the preparation process of Qilong capsules comprises the following steps:

[0030] (1) crushing and collecting the dried material obtained by the pre-drying process of the concentrated earthworm extract to obtain a first dried powder;

[0031] (2) performing vacuum freeze drying on the first dry powder at a temperature of -28°C to -23°C to obtain a second dry powder;

[0032] (3) mixing the second dry powder with the third dry powder obtained by the extraction process of astragalus, salvia miltiorrhiza, peach kernel, safflower, ligusticum chuanxiong, red peony root and angelica sinensis, and then filling the mixture into capsules to obtain Qilong capsules;

[0033] The moisture content of the second dried powder is not higher than 8%, and the moisture content of the third dried powder is not higher than 4.5%.

[0034] Optionally, the extraction process of Astragalus, Salvia miltiorrhiza, Peach Kernel, Carthamus tinctorius, Ligusticum chuanxiong, Paeonia lactiflora and Angelica sinensis comprises the following steps:

[0035] a. Take peach kernel, safflower, Chuanxiong, red peony root, astragalus, salvia miltiorrhiza and angelica and process them into 2.0±1.5cm clean medicinal materials, dry the processed Chuanxiong and red peony root at 75±5℃, and dry the processed angelica at 55±5℃;

[0036] b. Add 4 times the amount of water to Astragalus, Salvia miltiorrhiza, and Angelica sinensis and heat to boiling at a pressure of 0.15MPa-0.30MPa, adjust to 0.03MPa-0.08MPa, keep it at a slight boiling state, decoct 2-3 times, each time for 2-3h, combine the decoctions for primary concentration, and obtain a water extract concentrate and dregs;

[0037] c. Mix the residue with Chuanxiong, peach kernel, safflower, and red peony root, add 4 times the amount of 60% ethanol, heat to boiling at a pressure of 0.10MPa-0.25MPa, adjust to 0.02MPa-0.07MPa, keep it in a slightly boiling state, decoct 2-3 times, each time for 2-3h to obtain an alcohol extract, combine the alcohol extract and the water extract concentrate for secondary concentration to obtain a secondary mixed concentrate of Astragalus, Salvia miltiorrhiza, peach kernel, safflower, Chuanxiong, red peony root and Angelica sinensis;

[0038] d. The mixed concentrate is concentrated in three stages to obtain a three-stage mixed concentrate, the three-stage mixed concentrate is partitioned and dried, and then crushed and collected to obtain extracts such as Astragalus;

[0039] Among them, the relative density of the water-extracted concentrate is 1.05-1.15g / cm 3 (65-85℃), the relative density of the secondary mixed concentrate is 1.180-1.220g / cm 3 (70-80℃), the relative density of the three-stage mixed concentrate is 1.240-1.300g / cm 3 (40-50℃).

[0040] Optionally, the primary concentration is sequentially followed by a first-effect concentration and a second-effect concentration.

[0041] The primary concentration temperature is 65℃-85℃, and the vacuum degree is -0.05MPa~-0.08MPa;

[0042] The second-effect concentration temperature is 45℃-65℃, and the vacuum degree is -0.06MPa~-0.09MPa;

[0043] Optionally, the secondary concentration is sequentially followed by a triple-effect concentration and a quadruple-effect concentration.

[0044] The triple-effect concentration temperature is 65℃-80℃, and the vacuum degree is -0.04MPa~-0.07MPa;

[0045] The temperature of the fourth-effect concentration is 45℃-65℃, and the vacuum degree is -0.07MPa~-0.09MPa;

[0046] Optionally, the temperature of the third-stage concentration is 40-50°C and the vacuum degree is controlled above -0.08MPa.

[0047] Optionally, the zone drying temperatures in step D include, in sequence, a first stage temperature of 125±5°C, a second stage temperature of 100-105°C, a third stage temperature of 80-83°C, and a fourth stage temperature of 40-43°C.

[0048] Compared with the prior art, the present invention achieves at least one of the following beneficial effects:

[0049] (1) In the pre-drying process of the earthworm extract concentrate of the present invention, the relative density and foam density of the earthworm microfiltration concentrate are controlled to be within a certain range, thereby solving the problem of sticking to the machine during the pre-drying process of the earthworm microfiltration concentrate.

[0050] (2) Gradient drying is used in the pre-drying process of the concentrated earthworm extract of the present invention to prevent the continuous high temperature from causing the temperature of the material to be dried to exceed 50°C, which affects the activity of active ingredients such as autolytic enzymes. On the other hand, it provides a transition for the subsequent temperature drop to further dry the material. Finally, the temperature is lowered so that the material can be easily desorbed from the belt dryer at a low temperature.

[0051] (3) The hollow fiber earthworm ultrafiltration membrane prepared by the present invention improves the hydrophilicity of the ultrafiltration membrane, reduces the adsorption of earthworm extract on its surface during filtration, and ensures the membrane flux. In addition, it also reduces the adhesion and deposition of microorganisms on the membrane surface, improves the anti-pollution performance of the ultrafiltration membrane, and further ensures the retention rate of the effective ingredients in the earthworm extract, laying a foundation for the subsequent guarantee of the effective interception molecular weight, and also laying a foundation for the subsequent acquisition of earthworm microfiltration concentrate with a certain relative density.

[0052] (4) In the preparation process of the Qilong capsule of the present invention, the effective ingredients can be retained by effectively controlling the pre-drying process of the earthworm extract concentrate and the extraction process of astragalus, salvia miltiorrhiza, peach kernel, safflower, chuanxiong, red peony root and angelica. BRIEF DESCRIPTION OF THE DRAWINGS

[0053] The drawings described herein are used to provide a further understanding of the present invention and constitute a part of the present invention. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. In the drawings:

[0054] Figure 1 The flowchart of the pre-drying process of the concentrated liquid of earthworm extract of the present invention is shown. DETAILED DESCRIPTION

[0055] In order to more clearly illustrate the overall concept of the present invention, a detailed description is given below in an exemplary manner in conjunction with the accompanying drawings.

[0056] In the following description, many specific details are set forth to facilitate a full understanding of the present invention. However, the present invention may also be implemented in other ways different from those described herein. Therefore, the protection scope of the present invention is not limited to the specific embodiments disclosed below.

[0057] Example 1

[0058] The preparation process of Qilong Capsules includes the pre-drying process of the concentrated earthworm extract and the extraction process of astragalus, salvia miltiorrhiza, peach kernel, safflower, ligusticum chuanxiong, red peony root and angelica.

[0059] The pre-drying process of the earthworm extract concentrate comprises the following steps:

[0060] S01a: Autolyze the earthworms in sequence: add earthworms to each dispensing tank and extract them in 6 tanks. After the feeding is completed, add 6 times the amount of water as the earthworms to the dispensing tank. After the water is added, soak for 3 hours to allow the earthworms to completely soften and swell. After the soaking is completed, add 18 times the amount of water as the earthworms to the dispensing tank again. After the water is added, set the stirring frequency to 15Hz (speed 30%), the heating temperature to 45℃, start stirring and heat to increase the temperature. When the temperature of the dispensing tank reaches 45℃, set the timed stirring, stir for 5 minutes, stop for 25 minutes, and control the temperature of the dispensing tank at 45±3℃ at the same time, record the dissolution temperature, and do it once every hour. After 16 hours of constant temperature (45±3℃) dissolution, use a diaphragm pump to pump the supernatant in the dispensing tank into the high-level tank, and the slag is discharged through the drain valve.

[0061] S01b: Centrifugation: Set the centrifugal slag discharge time to 150±30s and the partial discharge time to 2±1s. After the parameters are confirmed, check that the liquid level in the centrifuge water tank meets the requirements, click "System Start", start the booster pump, wait for the centrifuge frequency to stabilize at 50Hz, and after the feed prompt appears on the operation interface, open the feed valve to obtain the centrifuge liquid.

[0062] S02a: Microfilter the centrifuge liquid in sequence: open the inlet and outlet valves and start the motor. The centrifuge liquid enters the six-stage filter element of the microfilter in sequence for graded filtration, and its inlet pressure is maintained at ≤0.1MPa. Open the drain valve of each filter element to release the air in the filter element. The filtrate is directly pumped into the microfiltration tank in the clean area to obtain microfiltrate.

[0063] S02b: Ultrafiltration: The microfiltrate is filtered twice with an ultrafiltration machine. Before the equipment is operated, click "dual system emptying" to drain the liquid in the ultrafiltration component. Select dual system operation, start the equipment, and start ultrafiltration. The concentrated water pressure is maintained at ≤0.1MPa, and the microfiltrate is concentrated to 1 / 4 of the original solution, with a cut-off molecular weight of more than 6,000 active ingredients.

[0064] S03: Concentration: The ultrafiltrate is concentrated in a low-temperature vacuum concentrator to obtain the earthworm microfiltration concentrate, wherein the material concentration temperature is less than 45°C, the vacuum degree is between -95.0 and -100 KPa, and the paste density is 1.200 g / cm 3 .

[0065] S1: The density of the collected paste is 1.200g / cm 3 The micro-filtered concentrated solution of earthworms is stirred and foamed to obtain a concentrated solution with a foam density of 120.

[0066] S2: Pre-drying: Set the PLC parameters of the belt dryer: set the feed pump frequency to 15±3Hz, the crawler frequency to 5Hz-7Hz. When the material level reaches the minimum value, turn off the feed pump after 300S, and the other values ​​remain unchanged. Set the temperature of zone 1 to 45℃, the temperature of zone 2 to 45℃, the temperature of zone 3 to 44℃, and the upper and lower limits of cooling water in zone 4 to 25℃; turn on the crawler drive motor, heating water pump, cooling water pump, and temperature control of each zone; turn on the main machine vacuum, the vacuum degree requirement is -100KPa, and after reaching the limit vacuum, turn on the feed pump, gate device and automatic material collection for about 20 minutes. When the material liquid is discharged from the discharge port, observe whether the material distribution is uniform, check the material temperature of the equipment at any time <50℃, ensure that the equipment is within the normal range, observe the material drying at any time, and directly put the dry material obtained by the pre-drying process of the earthworm extract concentrate into the grinder equipped with a 40-mesh screen of the dryer for crushing, and collect the powder to obtain the first dry powder. After all materials are dried, stop the machine and clear the site, and test the moisture content of the first dry powder.

[0067] S3: Freeze drying: The first dried powder is dried at a temperature of -25°C, the vacuum pressure is set to 100ubar, and the drying time is about 3 hours to obtain the second dried powder. The second dried powder is tested for moisture content.

[0068] The extraction process of astragalus, salvia miltiorrhiza, peach kernel, safflower, chuanxiong, red peony root and angelica comprises the following steps:

[0069] A. Pretreatment: Take peach kernel, safflower, Chuanxiong, red peony root, astragalus, salvia miltiorrhiza and angelica and process them into 2.0±1.5cm clean medicinal materials, dry the Chuanxiong and red peony root at 75±5℃, and dry the angelica at 55±5℃;

[0070] B. Water extraction and concentration: First, add 4 times the amount of water to the pre-treated Astragalus, Salvia miltiorrhiza, and Angelica sinensis, open the steam valve for heating, adjust the steam valve to 0.15MPa-0.30MPa, and after the liquid medicine boils, adjust the steam valve to 0.03MPa-0.08MPa and keep it in a slightly boiling state. Decoction twice, each time for 2 hours, control the temperature and pressure, and record every 30 minutes. Filter the two water extracts, combine them, and pull them into the double-effect concentrator for concentration. The steam regulating valve controls the first-effect concentration temperature at 65℃℃, the second-effect concentration temperature at 45℃℃, the first-effect vacuum degree at -0.05MPa, and the second-effect vacuum degree at -0.06MPa. Obtain water-extracted concentrate and medicinal residues, the relative density of the water-extracted concentrate is 1.05g / cm 3 .

[0071] C. Add the drug residue, Chuanxiong, peach kernel, safflower, and red peony root into a multifunctional extraction tank, add 4 times the amount of 60% ethanol, open the steam valve for heating, adjust the steam valve to 0.10MPa-0.25MPa, and after the drug liquid boils, adjust the steam valve to 0.02MPa-0.07MPa and keep it in a slightly boiling state. Decoction twice, 2 hours each time, control the temperature and pressure, and record every 30 minutes. Filter the alcohol extract, combine it with the water extract concentrate, and recover the ethanol. Control the concentration temperature of the first effect to 65℃, the concentration temperature of the second effect to 45℃, the vacuum degree of the first effect to -0.04MPa, and the vacuum degree of the second effect to -0.07MPa. Concentrate to a relative density of 1.180g / cm 3 , and obtain a secondary mixed concentrated solution.

[0072] D. Transfer the secondary mixed concentrate into the scraper concentrator for further concentration. The vacuum degree of the scraper concentrator is controlled at above -0.08MPa and concentrated to a relative density of 1.240g / cm 3 (40-50°C) to obtain a three-stage mixed concentrated solution.

[0073] E. Belt drying of three-stage mixed concentrate: Set the PLC parameters of the equipment: feed pump frequency is set to 25-30Hz, crawler frequency is set to 6Hz-8Hz, when the material level reaches the lowest value, turn off the feed pump after 200 seconds, and the other values ​​remain unchanged. Set the temperature control system, heating in zone 1 is set to 120℃, heating in zone 2 is set to 100℃, heating upper and lower limits in zone 3 are set to 80℃, and cooling water upper and lower limits in zone 4 are set to 40℃; turn on the crawler drive motor, heating water pump, cooling water pump, and temperature control in each zone; turn on the main machine vacuum, and after reaching the limit vacuum, six feed pumps, gate device and automatic material collection, about 5 minutes, observe whether the material is evenly distributed when the material liquid is discharged from the discharge port. During the operation of the equipment, check at any time that the material temperature is ≤95℃ and the vacuum requirement is -100KPa. Ensure that the equipment is within the normal range, set the predetermined drying temperature according to the material temperature, observe the material drying situation at any time, and the dry material directly enters the dryer's built-in crusher equipped with a 30-mesh screen for crushing and collecting powder to obtain the third dry powder, and the third dry powder is tested for moisture.

[0074] The second dry powder is mixed with the third dry powder obtained by the extraction process of astragalus, salvia miltiorrhiza, peach kernel, safflower, chuanxiong, red peony root and angelica, and then capsules are filled to obtain Qilong capsules.

[0075] Example 2

[0076] The preparation process of Qilong Capsules includes the pre-drying process of the concentrated earthworm extract and the extraction process of astragalus, salvia miltiorrhiza, peach kernel, safflower, ligusticum chuanxiong, red peony root and angelica.

[0077] The pre-drying process of the earthworm extract concentrate comprises the following steps:

[0078] S01a: Autolyze the earthworms in sequence: add earthworms to each dispensing tank and extract them in 6 tanks. After the feeding is completed, add 6 times the amount of water as the earthworms to the dispensing tank. After the water is added, soak for 3 hours to allow the earthworms to completely soften and swell. After the soaking is completed, add 18 times the amount of water as the earthworms to the dispensing tank again. After the water is added, set the stirring frequency to 15Hz (speed 30%), the heating temperature to 45℃, start stirring and heat to increase the temperature. When the temperature of the dispensing tank reaches 45℃, set the timed stirring, stir for 5 minutes, stop for 25 minutes, and control the temperature of the dispensing tank at 45±3℃ at the same time, record the dissolution temperature, and do it once every hour. After 16 hours of constant temperature (45±3℃) dissolution, use a diaphragm pump to pump the supernatant in the dispensing tank into the high-level tank, and the slag is discharged through the drain valve.

[0079] S01b: Centrifugation: Set the centrifugal slag discharge time to 150±30s and the partial discharge time to 2±1s. After the parameters are confirmed, check that the liquid level in the centrifuge water tank meets the requirements, click "System Start", start the booster pump, wait for the centrifuge frequency to stabilize at 50Hz, and after the feed prompt appears on the operation interface, open the feed valve to obtain the centrifuge liquid.

[0080] S02a: Microfilter the centrifuge liquid in sequence: open the inlet and outlet valves and start the motor. The centrifuge liquid enters the six-stage filter element of the microfilter in sequence for graded filtration, and its inlet pressure is maintained at ≤0.1MPa. Open the drain valve of each filter element to release the air in the filter element. The filtrate is directly pumped into the microfiltration tank in the clean area to obtain microfiltrate.

[0081] S02b: Ultrafiltration: The microfiltrate is filtered twice with an ultrafiltration machine. Before the equipment is operated, click "dual system emptying" to drain the liquid in the ultrafiltration component. Select dual system operation, start the equipment, and start ultrafiltration. The concentrated water pressure is maintained at ≤0.1MPa, and the microfiltrate is concentrated to 1 / 4 of the original solution, with a cut-off molecular weight of more than 6,000 active ingredients.

[0082] S03: Concentration: The ultrafiltrate is concentrated in a low-temperature vacuum concentrator to obtain the earthworm microfiltration concentrate, wherein the material concentration temperature is less than 45°C, the vacuum degree is between -95.0 and -100 KPa, and the paste density is 1.220 g / cm 3 .

[0083] S1: The density of the collected paste is 1.220g / cm 3 The micro-filtered concentrated solution of earthworms is stirred and foamed to obtain a concentrated solution with a foam density of 180.

[0084] S2: Pre-drying: Set the PLC parameters of the belt dryer: set the feed pump frequency to 15±3Hz, the crawler frequency to 5Hz-7Hz. When the material level reaches the minimum value, turn off the feed pump after 300S, and the other values ​​remain unchanged. Set the temperature of zone 1 to 48℃, the temperature of zone 2 to 48℃, the temperature of zone 3 to 46℃, and the upper and lower limits of cooling water in zone 4 to 28℃; turn on the crawler drive motor, heating water pump, cooling water pump, and temperature control of each zone; turn on the main machine vacuum, the vacuum degree requirement is -100KPa, and after reaching the limit vacuum, turn on the feed pump, gate device and automatic material collection for about 20 minutes. When the material liquid is discharged from the discharge port, observe whether the material distribution is uniform, check the material temperature of the equipment at any time <50℃, ensure that the equipment is within the normal range, observe the drying of the material at any time, and directly put the dry material obtained by the pre-drying process of the earthworm extract concentrate into the grinder equipped with a 40-mesh screen of the dryer for crushing, and collect the powder to obtain the first dry powder. After all materials are dried, stop the machine and clear the site, and test the moisture content of the first dry powder.

[0085] S3: Freeze drying: The first dried powder is dried at a temperature of -25°C, the vacuum pressure is set to 100ubar, and the drying time is about 3 hours to obtain the second dried powder. The second dried powder is tested for moisture content.

[0086] The extraction process of astragalus, salvia miltiorrhiza, peach kernel, safflower, chuanxiong, red peony root and angelica comprises the following steps:

[0087] A. Pretreatment: Take peach kernel, safflower, Chuanxiong, red peony root, astragalus, salvia miltiorrhiza and angelica and process them into 2.0±1.5cm clean medicinal materials, dry the Chuanxiong and red peony root at 75±5℃, and dry the angelica at 55±5℃;

[0088] B. Water extraction and concentration: First, add 4 times the amount of water to the pre-treated Astragalus, Salvia miltiorrhiza, and Angelica sinensis, open the steam valve for heating, adjust the steam valve to 0.15MPa-0.30MPa, and after the liquid medicine boils, adjust the steam valve to 0.03MPa-0.08MPa and keep it in a slightly boiling state. Decoction twice, each time for 2 hours, control the temperature and pressure, and record every 30 minutes. Filter the two water extracts, combine them, and pull them into the double-effect concentrator for concentration. The steam regulating valve controls the first-effect concentration temperature to 85°C, the second-effect concentration temperature to 65°C, the first-effect vacuum degree to -0.08MPa, and the second-effect vacuum degree to -0.09MPa. Get the water extract concentrate and medicinal residues, the relative density of the water extract concentrate is 1.15g / cm 3 .

[0089] C. Add the drug residue, Chuanxiong, peach kernel, safflower, and red peony root into a multifunctional extraction tank, add 4 times the amount of 60% ethanol, open the steam valve for heating, adjust the steam valve to 0.10MPa-0.25MPa, and after the drug liquid boils, adjust the steam valve to 0.02MPa-0.07MPa and keep it in a slightly boiling state. Decoction twice, 2 hours each time, control the temperature and pressure, and record every 30 minutes. Filter the alcohol extract, combine it with the water extract concentrate, and recover the ethanol. Control the concentration temperature of the first effect to 80℃, the concentration temperature of the second effect to 65℃, the vacuum degree of the first effect to -0.07MPa, and the vacuum degree of the second effect to -0.09MPa. Concentrate to a relative density of 1.220g / cm 3 , and obtain a secondary mixed concentrated solution.

[0090] D. The secondary mixed concentrate is transferred to the scraper concentrator for further concentration. The vacuum degree of the scraper concentrator is controlled at above -0.08MPa and concentrated to a relative density of 1.300g / cm 3 (40-50°C) to obtain a three-stage mixed concentrated solution.

[0091] E. Belt drying of three-stage mixed concentrate: Set the PLC parameters of the equipment: feed pump frequency is set to 25-30Hz, crawler frequency is set to 6Hz-8Hz, when the material level reaches the lowest value, turn off the feed pump after 200 seconds, and the other values ​​remain unchanged. Set the temperature control system, heating in zone 1 is set to 130℃, heating in zone 2 is set to 105℃, heating upper and lower limits in zone 3 are set to 83℃, and cooling water upper and lower limits in zone 4 are set to 43℃; turn on the crawler drive motor, heating water pump, cooling water pump, and temperature control in each zone; turn on the main machine vacuum, and after reaching the limit vacuum, six feed pumps, gate device and automatic material collection, about 5 minutes, observe whether the material is evenly distributed when the material liquid is discharged from the discharge port. During the operation of the equipment, check at any time that the material temperature is ≤95℃ and the vacuum requirement is -100KPa. Ensure that the equipment is within the normal range, set the predetermined drying temperature according to the material temperature, observe the material drying situation at any time, and the dry material directly enters the dryer's built-in crusher equipped with a 30-mesh screen for crushing and collecting powder to obtain the third dry powder, and the third dry powder is tested for moisture.

[0092] The second dry powder is mixed with the third dry powder obtained by the extraction process of astragalus, salvia miltiorrhiza, peach kernel, safflower, chuanxiong, red peony root and angelica, and then capsules are filled to obtain Qilong capsules.

[0093] Example 3

[0094] The preparation process of Qilong Capsules includes the pre-drying process of the concentrated earthworm extract and the extraction process of astragalus, salvia miltiorrhiza, peach kernel, safflower, ligusticum chuanxiong, red peony root and angelica.

[0095] The pre-drying process of the earthworm extract concentrate comprises the following steps:

[0096] S01a: Autolyze the earthworms in sequence: add earthworms to each dispensing tank and extract them in 6 tanks. After the feeding is completed, add 6 times the amount of water as the earthworms to the dispensing tank. After the water is added, soak for 3 hours to allow the earthworms to completely soften and swell. After the soaking is completed, add 18 times the amount of water as the earthworms to the dispensing tank again. After the water is added, set the stirring frequency to 15Hz (speed 30%), the heating temperature to 45℃, start stirring and heat to increase the temperature. When the temperature of the dispensing tank reaches 45℃, set the timed stirring, stir for 5 minutes, stop for 25 minutes, and control the temperature of the dispensing tank at 45±3℃ at the same time, record the dissolution temperature, and do it once every hour. After 16 hours of constant temperature (45±3℃) dissolution, use a diaphragm pump to pump the supernatant in the dispensing tank into the high-level tank, and the slag is discharged through the drain valve.

[0097] S01b: Centrifugation: Set the centrifugal slag discharge time to 150±30s and the partial discharge time to 2±1s. After the parameters are confirmed, check that the liquid level in the centrifuge water tank meets the requirements, click "System Start", start the booster pump, wait for the centrifuge frequency to stabilize at 50Hz, and after the feed prompt appears on the operation interface, open the feed valve to obtain the centrifuge liquid.

[0098] S02a: Microfilter the centrifuge liquid in sequence: open the inlet and outlet valves and start the motor. The centrifuge liquid enters the six-stage filter element of the microfilter in sequence for graded filtration, and its inlet pressure is maintained at ≤0.1MPa. Open the drain valve of each filter element to release the air in the filter element. The filtrate is directly pumped into the microfiltration tank in the clean area to obtain microfiltrate.

[0099] S02b: Ultrafiltration: The microfiltrate is filtered twice with an ultrafiltration machine. Before the equipment is operated, click "dual system emptying" to drain the liquid in the ultrafiltration component. Select dual system operation, start the equipment, and start ultrafiltration. The concentrated water pressure is maintained at ≤0.1MPa, and the microfiltrate is concentrated to 1 / 4 of the original solution, with a cut-off molecular weight of more than 6,000 active ingredients.

[0100] S03: Concentration: The ultrafiltrate is concentrated in a low-temperature vacuum concentrator to obtain the earthworm microfiltration concentrate, wherein the material concentration temperature is less than 45°C, the vacuum degree is between -95.0 and -100 KPa, and the paste density is 1.200 g / cm 3 .

[0101] S1: The density of the collected paste is 1.200g / cm 3 The micro-filtered concentrated solution of earthworms is stirred and foamed to obtain a concentrated solution with a foam density of 150.

[0102] S2: Pre-drying: Set the PLC parameters of the belt dryer: set the feed pump frequency to 15±3Hz, the crawler frequency to 5Hz-7Hz. When the material level reaches the minimum value, turn off the feed pump after 300S, and the other values ​​remain unchanged. Set the temperature of zone 1 to 46℃, the temperature of zone 2 to 45℃, the temperature of zone 3 to 44℃, and the upper and lower limits of cooling water in zone 4 to 26℃; turn on the crawler drive motor, heating water pump, cooling water pump, and temperature control of each zone; turn on the main machine vacuum, the vacuum degree requirement is -100KPa, and after reaching the limit vacuum, turn on the feed pump, gate device and automatic material collection for about 20 minutes. When the material liquid is discharged from the discharge port, observe whether the material distribution is uniform, check the material temperature of the equipment at any time <50℃, ensure that the equipment is within the normal range, observe the material drying at any time, and directly put the dry material obtained by the pre-drying process of the earthworm extract concentrate into the grinder equipped with a 40-mesh screen of the dryer for crushing, and collect the powder to obtain the first dry powder. After all materials are dried, stop the machine and clear the site, and test the moisture content of the first dry powder.

[0103] S3: Freeze drying: The first dried powder is dried at a temperature of -25°C, the vacuum pressure is set to 100ubar, and the drying time is about 3 hours to obtain the second dried powder. The second dried powder is tested for moisture content.

[0104] The extraction process of astragalus, salvia miltiorrhiza, peach kernel, safflower, chuanxiong, red peony root and angelica comprises the following steps:

[0105] A. Pretreatment: Take peach kernel, safflower, Chuanxiong, red peony root, astragalus, salvia miltiorrhiza and angelica and process them into 2.0±1.5cm clean medicinal materials, dry the Chuanxiong and red peony root at 75±5℃, and dry the angelica at 55±5℃;

[0106] B. Water extraction and concentration: First, add 4 times the amount of water to the pre-treated Astragalus, Salvia miltiorrhiza, and Angelica sinensis, open the steam valve for heating, adjust the steam valve to 0.15MPa-0.30MPa, and after the liquid medicine boils, adjust the steam valve to 0.03MPa-0.08MPa and keep it in a slightly boiling state. Decoction twice, each time for 2 hours, control the temperature and pressure, and record every 30 minutes. Filter the two water extracts, combine them, and pull them into the double-effect concentrator for concentration. The steam regulating valve controls the first-effect concentration temperature to 75°C, the second-effect concentration temperature to 55°C, the first-effect vacuum degree to -0.06MPa, and the second-effect vacuum degree to -0.07MPa. Get the water-extracted concentrate and medicinal residues, the relative density of the water-extracted concentrate is 1.10g / cm 3 .

[0107] C. Add the drug residue, Chuanxiong, peach kernel, safflower, and red peony root into a multifunctional extraction tank, add 4 times the amount of 60% ethanol, open the steam valve for heating, adjust the steam valve to 0.10MPa-0.25MPa, and after the drug liquid boils, adjust the steam valve to 0.02MPa-0.07MPa and keep it in a slightly boiling state. Decoction twice, each time for 2 hours, control the temperature and pressure, and record every 30 minutes. Filter the alcohol extract, combine it with the water extract concentrate, and recover the ethanol. Control the concentration temperature of the first effect to 70℃, the concentration temperature of the second effect to 55℃, the vacuum degree of the first effect to -0.05MPa, and the vacuum degree of the second effect to -0.08MPa. Concentrate to a relative density of 1.20g / cm 3 , and obtain a secondary mixed concentrated solution.

[0108] D. Transfer the secondary mixed concentrate into the scraper concentrator for further concentration. The vacuum degree of the scraper concentrator is controlled at above -0.08MPa and concentrated to a relative density of 1.280g / cm 3 (40-50°C) to obtain a three-stage mixed concentrated solution.

[0109] E. Belt drying of three-stage mixed concentrate: Set the PLC parameters of the equipment: feed pump frequency is set to 25-30Hz, crawler frequency is set to 6Hz-8Hz, when the material level reaches the lowest value, turn off the feed pump after 200 seconds, and the other values ​​remain unchanged. Set the temperature control system, heating in zone 1 is set to 125℃, heating in zone 2 is set to 102℃, heating upper and lower limits in zone 3 are set to 82℃, and cooling water upper and lower limits in zone 4 are set to 42℃; turn on the crawler drive motor, heating water pump, cooling water pump, and temperature control in each zone; turn on the main machine vacuum, and after reaching the limit vacuum, six feed pumps, gate device and automatic material collection, about 5 minutes, observe whether the material is evenly distributed when the material liquid is discharged from the discharge port. During the operation of the equipment, check at any time that the material temperature is ≤95℃ and the vacuum requirement is -100KPa. Ensure that the equipment is within the normal range, set the predetermined drying temperature according to the material temperature, observe the material drying situation at any time, and the dry material directly enters the dryer's built-in crusher equipped with a 30-mesh screen for crushing and collecting powder to obtain the third dry powder, and the third dry powder is tested for moisture.

[0110] The second dry powder is mixed with the third dry powder obtained by the extraction process of astragalus, salvia miltiorrhiza, peach kernel, safflower, chuanxiong, red peony root and angelica, and then capsules are filled to obtain Qilong capsules.

[0111] Example 4

[0112] Based on Example 3, the main difference is that the ultrafiltration membrane in the ultrafiltration process is a hollow fiber ultrafiltration membrane, and the hollow fiber earthworm ultrafiltration membrane comprises, by weight, 15 parts of polyether sulfone, 15 parts of modified polyacrylonitrile, 5 parts of carboxylated polyethyleneimine, 8 parts of polyethylene glycol, 5 parts of functional filler, with an average particle size of 40 nm, 5 parts of glutaraldehyde and 40 parts of N-methylpyrrolidone.

[0113] The preparation method of modified polyacrylonitrile comprises the following steps:

[0114] S1: mixing polyacrylonitrile and N,N-dimethylformamide at a mass ratio of 1:5 to obtain a first mixture;

[0115] S2: The first mixture is mixed with 40 g / L hydroxylamine hydrochloride, the pH is adjusted to 6, the mixture is reacted at 65° C., and then the mixture is washed and dried to obtain modified polyacrylonitrile.

[0116] The preparation process of hollow fiber earthworm ultrafiltration membrane for Qilong capsule comprises the following steps:

[0117] (1) reacting polyethersulfone, modified polyacrylonitrile, carboxylated polyethyleneimine, polyethylene glycol, nano-titanium dioxide and N,N-dimethylacetamide at 50° C. in proportion to obtain a casting solution;

[0118] (2) pouring the casting solution into a spinning machine for spinning, soaking the obtained membrane fibers in a 3% by mass glutaraldehyde solution, cross-linking at 55° C., and then washing to obtain a hollow fiber earthworm ultrafiltration membrane for Qilong capsule.

[0119] The preparation method of the functional filler comprises the following steps:

[0120] (1) 4 mg of the nanoparticles were mixed with 4 mg of dopamine hydrochloride and 80 ml of 0.1 mol / L tris(hydroxymethyl)aminomethane solution, reacted at room temperature, washed and dried to obtain an intermediate;

[0121] (2) adding the intermediate obtained in step (1) into 40 ml of tris(hydroxymethyl)aminomethane solution, and then adding 60 mg of 3-sulfonic acid propyl methacrylate potassium salt, reacting at room temperature (25° C.), and washing and drying the product in turn to obtain a functional filler;

[0122] The nanoparticles are nano-silicon dioxide and nano-titanium dioxide; the mass ratio of nano-silicon dioxide to nano-titanium dioxide is 1:1, and the average particle sizes of nano-silicon dioxide and nano-titanium dioxide are both 50nm.

[0123] Example 5

[0124] Based on Example 1, the main difference is that in step S2 pre-drying, the temperature of zone 1 is set to 45°C, the temperature of zone 2 is set to 45°C, the temperature of zone 3 is set to 44°C, and the upper and lower limits of cooling water in zone 4 are set to 45°C.

[0125] Comparative Example 1

[0126] Based on Example 1, the main difference is that the relative density of the earthworm microfiltration concentrate is 1.6 g / cm 3 , foam density 120.

[0127] Comparative Example 2

[0128] Based on Example 1, the main difference is that the relative density of the earthworm microfiltration concentrate is 1.2 g / cm 3 , foam density 90.

[0129] Comparative Example 3

[0130] Based on Example 1, the main difference is that the relative density of the earthworm microfiltration concentrate is 1.2 g / cm 3 , foam density 250.

[0131] Performance Testing

[0132] Test the viscosity of the pre-drying process of the earthworm extract concentrate:

[0133] Desorption rate (%) = (AS) / A*100, wherein A is the area of ​​the belt dryer when not adhered, and S is the area of ​​the earthworm extract concentrate adhered after drying. The test results are shown in Table 1.

[0134] Table 1

[0135]

[0136]

[0137] Referring to Table 1, it can be seen that the pre-drying process of the earthworm extract concentrate of the present application can make the desorption rate of the dried earthworm extract not less than 75%, thereby ensuring the product quality of the Qilong Capsule and improving the production cost.

[0138] Moisture test: The test results are shown in Table 2.

[0139] Table 2

[0140]

[0141] Active ingredient detection:

[0142] The effective ingredients in the earthworm extract (the second dry powder) and the third dry powder were detected, and the test results are shown in Table 3. Among them, in the embodiment of the present application, 400g of earthworm, 480g of astragalus, 24g of salvia miltiorrhiza, 24g of angelica, 24g of red peony root, 12g of chuanxiong, 12g of safflower and 2g of peach kernel.

[0143] Table 3

[0144]

[0145] Referring to Table 3, it can be seen that the earthworm extract extracted by the present invention can well ensure its biological activity, and the extracts extracted by the extraction process of Astragalus, Salvia miltiorrhiza, peach kernel, safflower, Chuanxiong, red peony root and Angelica sinensis can retain the content of the effective ingredients ferulic acid and astragaloside IV to the greatest extent. Comparative Examples 1-3 failed to produce the finished product due to sticking during the drying process.

[0146] The above description is only an embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent substitution, improvement, etc. made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.

Claims

1. A pre-drying process for a concentrated solution of earthworm extract, characterized in that: The pre-drying process of the concentrated solution of earthworm extract comprises the following steps: S1: stirring and foaming the earthworm microfiltration concentrate having a certain relative density to obtain a concentrate having a certain foam density; S2: drying the concentrated liquid with a certain foam density in a gradient vacuum at a temperature of 40-48°C to obtain a pre-dried material; Among them, the relative density is not higher than 1.22g / cm 3 , foam density 120-180; the moisture content in the pre-dried material is not higher than 15%.

2. The pre-drying process of the concentrated earthworm extract according to claim 1, characterized in that: The gradient drying temperatures include zone 1 temperature 45-48°C, zone 2 temperature 45-48°C, zone 3 temperature 44-46°C, and zone 4 temperature 25-28°C.

3. The pre-drying process of the concentrated earthworm extract according to claim 1, characterized in that: The pre-drying process of the concentrated earthworm extract also includes the following steps: S01: autolyzing and centrifuging the earthworm in sequence to obtain a centrifuge solution; S02: subjecting the centrifuge to microfiltration and ultrafiltration treatments in sequence to obtain a microfiltrate; S03: Concentrating the microfiltrate at a temperature not higher than 45° C. to obtain a microfiltrate concentrate of earthworms; Among them, the autolysis temperature is 42-48°C, and the autolysis time is 16-19h; During the ultrafiltration process, the molecular weight cut-off is above six thousand.

4. The pre-drying process of the concentrated earthworm extract according to claim 3, characterized in that: The ultrafiltration membrane in the ultrafiltration process is a hollow fiber ultrafiltration membrane, which includes 10-20 parts of polyethersulfone, 10-20 parts of modified polyacrylonitrile, 5-10 parts of carboxylated polyethyleneimine, 5-10 parts of polyethylene glycol, 2-7 parts of functional filler and 2-10 parts of glutaraldehyde by weight.

5. The pre-drying process of the concentrated solution of earthworm extract according to claim 4, characterized in that: The preparation method of the modified polyacrylonitrile comprises the following steps: S1: mixing polyacrylonitrile and N,N-dimethylformamide to react to obtain a first mixture; S2: mixing the first mixture with hydroxylamine hydrochloride, adjusting the pH to 6, reacting at a temperature of 60-70° C., and then washing and drying to obtain modified polyacrylonitrile; The mass ratio of polyacrylonitrile to N,N-dimethylformamide is 1:(4-7).

6. The pre-drying process of the concentrated earthworm extract according to claim 4, characterized in that: The preparation method of the functional filler comprises the following steps: (1) mixing the nanoparticles with dopamine hydrochloride and tris(hydroxymethyl)aminomethane solution, reacting at room temperature, washing, and drying to obtain an intermediate; (2) adding the intermediate obtained in step (1) to a tris(hydroxymethyl)aminomethane solution, and then adding potassium salt of 3-sulfonyl methacrylate to react at room temperature, and washing and drying the product in turn to obtain a functional filler; Among them, the nanoparticles are nano-silicon dioxide and nano-titanium dioxide; The mass ratio of nanoparticles, dopamine hydrochloride and 3-sulfonate propyl methacrylate potassium salt is (1-3):1:(15-20).

7. A process for preparing Qilong capsules, characterized in that: The preparation process of the Qilong capsule comprises the pre-drying process of the concentrated earthworm extract according to any one of claims 1 to 6 and the extraction process of astragalus, salvia miltiorrhiza, peach kernel, safflower, chuanxiong, red peony root and angelica; the preparation process of the Qilong capsule comprises the following steps: (1) crushing and collecting the dried material obtained by the pre-drying process of the concentrated earthworm extract to obtain a first dried powder; (2) performing vacuum freeze drying on the first dry powder at a temperature of -28°C to -23°C to obtain a second dry powder; (3) mixing the second dry powder with the third dry powder obtained by the extraction process of astragalus, salvia miltiorrhiza, peach kernel, safflower, ligusticum chuanxiong, red peony root and angelica sinensis, and then filling the mixture into capsules to obtain Qilong capsules; The moisture content of the second dried powder is not higher than 8%, and the moisture content of the third dried powder is not higher than 4.5%.

8. The preparation process of Qilong Capsules according to claim 7, characterized in that: The extraction process of astragalus, salvia miltiorrhiza, peach kernel, safflower, chuanxiong, red peony root and angelica comprises the following steps: a. Take peach kernel, safflower, Chuanxiong, red peony root, astragalus, salvia miltiorrhiza and angelica and process them into 2.0±1.5cm clean medicinal materials, dry the processed Chuanxiong and red peony root at 75±5℃, and dry the processed angelica at 55±5℃; b. Add 4 times the amount of water to Astragalus, Salvia miltiorrhiza, and Angelica sinensis and heat to boiling at a pressure of 0.15MPa-0.30MPa, adjust to 0.03MPa-0.08MPa, keep it at a slight boiling state, decoct 2-3 times, each time for 2-3h, combine the decoctions for primary concentration, and obtain a water extract concentrate and dregs; C. Mix the residue with Chuanxiong, peach kernel, safflower, and red peony root, add 4 times the amount of 60% ethanol, heat to boiling at a pressure of 0.10MPa-0.25MPa, adjust to 0.02MPa-0.07MPa, keep it in a slightly boiling state, decoct 2-3 times, each time for 2-3h, to obtain an alcohol extract, combine the alcohol extract and the water extract concentrate for secondary concentration, and obtain a secondary mixed concentrate of astragalus, salvia miltiorrhiza, peach kernel, safflower, Chuanxiong, red peony root, and angelica; D. performing three-stage concentration on the mixed concentrate to obtain a three-stage mixed concentrate, performing zone drying on the three-stage mixed concentrate, and then crushing and collecting powder to obtain extracts such as astragalus; Among them, the relative density of the water-extracted concentrate is 1.05-1.15g / cm 3 The relative density of the secondary mixed concentrate is 1.180-1.220g / cm 3 The relative density of the three-stage mixed concentrate is 1.240-1.300g / cm 3 .

9. The preparation process of Qilong Capsules according to claim 8, characterized in that: The first-stage concentration is carried out through the first-effect concentration and the second-effect concentration in sequence. The primary concentration temperature is 65℃-85℃, and the vacuum degree is -0.05MPa~-0.08MPa; The second-effect concentration temperature is 45℃-65℃, and the vacuum degree is -0.06MPa~-0.09MPa; and / or secondary concentration, followed by triple-effect concentration and quadruple-effect concentration, The triple-effect concentration temperature is 65℃-80℃, and the vacuum degree is -0.04MPa~-0.07MPa; The temperature of the fourth-effect concentration is 45℃-65℃, and the vacuum degree is -0.07MPa~-0.09MPa; And / or the temperature of the third stage concentration is 40-50°C, and the vacuum degree is controlled above -0.08MPa.

10. The preparation process of Qilong Capsules according to claim 8, characterized in that: The zone drying temperatures in step D include a first stage temperature of 125±5°C, a second stage temperature of 100-105°C, a third stage temperature of 80-83°C, and a fourth stage temperature of 40-43°C.

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