Bear gall powder preparation method

Abstract

The invention discloses a bear gall powder preparation method, an instant high-temperature sterilization process and a vacuum freeze-drying process, and the bear gall powder preparation method has the beneficial effects that the traditional sterilization process can be replaced by the bear gall powder preparation method provided by the invention, and the instant high-temperature sterilization work is carried out by using an ultrahigh-temperature sterilizer; according to the method, the bear gall powder can be sterilized and dried on the premise that active ingredients are not damaged, the retention rate of the bezoar ursodesoxycholic acid is increased to be larger than or equal to 50% and the water content of the bezoar ursodesoxycholic acid is smaller than or equal to 2% under the condition that no additive is added, the original luster of the product can be reserved, and the food safety of the product can be improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of medicinal material processing, in particular to a preparation method of bear bile powder. BACKGROUND

[0002] Bear bile is rich in tauroursodeoxycholic acid, ursodeoxycholic acid, and taurine chenodeoxycholic acid, which can clear heat, calm the liver, and improve eyesight. It has good therapeutic effects on jaundice, costalgia, cough, laryngalgia, drunkenness, sores, hemorrhoids, hyperlipidemia, and hepatitis. However, due to the influence of microorganisms and bacteria in the production process of bear bile, electron beam sterilization, high-temperature drying, and microwave drying are usually used. However, these methods can cause the loss of effective components in bear bile, reduce its biological activity, and change the original color of the product, thereby reducing the content of some effective components such as tauroursodeoxycholic acid and chenodeoxycholic acid, and seriously affecting the medicinal properties. SUMMARY

[0003] To achieve the above-mentioned purpose, the technical solution of the present application is as follows: a preparation method of bear bile powder, a transient high-temperature sterilization process, and a vacuum freeze-drying process.

[0004] The transient high-temperature sterilization process includes: a first temperature setting, a second temperature setting, a temperature difference setting, a material pump pumping, and an outfeed temperature detection. Through this process, the bear bile powder manufacturing raw materials can be subjected to transient high-temperature sterilization.

[0005] Preferably, an ultra-high-temperature sterilization machine is used when performing the transient high-temperature sterilization process. The ultra-high-temperature sterilization machine can achieve the required temperature for transient high-temperature.

[0006] Preferably, the vacuum freeze-drying process includes: a first-stage sublimation, a first-stage desorption drying, and a second-stage desorption sublimation.

[0007] Preferably, the content of tauroursodeoxycholic acid in the bear bile powder manufactured by the method is ≥ 50%, and the moisture content is ≤ 2%.

[0008] Preferably, the bear bile powder manufactured by the vacuum freeze-drying process needs to be sieved through a 50-mesh sieve. BRIEF DESCRIPTION OF DRAWINGS

[0009] Figure 1 The process flow diagram of the preparation method of bear bile powder according to the present application is shown in the figure.

[0010] Advantages:

[0011] The bear bile powder preparation method described in this case can replace the traditional sterilization process by using an ultra-high temperature sterilizer for instantaneous high-temperature sterilization. This method can sterilize and dry the bear bile powder without destroying the effective components. Without adding any additives, it can increase the retention rate of ursodeoxycholic acid in bezoar to ≥50%, reduce the moisture content to ≤2%, preserve the original luster of the product, and improve the food safety of the product. Detailed Implementation

[0012] The present invention will now be described in detail with reference to the accompanying drawings, such as... Figure 1 As shown, a method for preparing bear bile powder.

[0013] Those skilled in the art should connect all electrical components in this case to their compatible power supplies via wires. Appropriate controllers should be selected based on the actual situation to meet control requirements. The specific connections and control sequence should refer to the working principle described below, which outlines the sequential operation of each electrical component. The detailed connection methods are well-known in the art. The following primarily describes the working principle and process, without further explanation of electrical control. (Those skilled in the art should connect the components in this case sequentially. The specific connections and operating sequence should refer to the working principle described below. The detailed connection methods are well-known in the art. The following primarily describes the working principle and process.)

[0014] Example:

[0015] The present invention will now be described in detail with reference to the accompanying drawings, such as... Figure 1 As shown, a method for preparing bear bile powder includes a flash high-temperature sterilization process and a vacuum freeze-drying process;

[0016] The instantaneous high-temperature sterilization process includes: first-layer temperature setting, second-layer temperature setting, temperature difference setting, material pump extraction, and discharge temperature detection. This process can be used to instantaneously sterilize the raw materials for manufacturing bear bile powder.

[0017] It should be noted that during the high-temperature sterilization process, 100 portions of frozen bear bile are taken. The material container containing the frozen bear bile is placed in a material basket, and purified water is added to the basket, covering approximately 2 / 3 of the container. The mixture is then completely thawed at room temperature. A 100-mesh stainless steel sieve is placed on a stainless steel drum to sieve the thawed bear bile before it is poured into the stainless steel drum. The filtered bear bile is then sterilized using an instantaneous ultra-high temperature sterilization method. The ultra-high temperature sterilization process is as follows: the first layer is set at 125℃, the second layer at 135℃, the temperature difference is set at 35℃, the sterilization temperature of the ultra-high temperature sterilizer is not lower than 130℃, the feed pump frequency is 28Hz, and the discharge temperature is below 40℃. The sterilized bear bile is then loaded into trays, with each tray weighing no more than 1.5kg. The trays are then placed on the shelves of a vacuum freeze dryer. After loading, the vacuum freeze dryer door is closed.

[0018] An ultra-high temperature sterilizer is required when performing the instantaneous high-temperature sterilization process.

[0019] It should be noted that ultra-high temperature sterilizers can provide the temperature required for instantaneous high temperatures.

[0020] Preferably, and further still, the vacuum freeze-drying process includes: a first-stage sublimation, a first-stage desorption drying, and a second-stage desorption sublimation state.

[0021] It should be noted that this process is a pre-frozen state. The first stage of sublimation is when the frozen product is heated in a vacuum state through heat transfer oil, and its ice crystals will sublimate into water vapor and escape, thus dehydrating and drying the product.

[0022] The first stage of drying involves moving from the outer surface inwards. After the ice crystals sublimate, the remaining voids become the escape of sublimated water vapor. At this point, the material appears as a solid powder with a honeycomb-like surface, but ice crystals still exist inside, making it impossible to obtain a completely dried product.

[0023] The second stage of desorption drying is then employed because the first stage removes water as ice crystals. Therefore, the temperature and pressure must be controlled below the product's eutectic point to prevent the ice crystals from melting. For adsorbed water, due to its high adsorption energy, sufficient energy is required for water to desorb. To ensure the desorbed water vapor has sufficient driving force to escape the product, a significant vapor pressure difference must be created inside and outside the product. Therefore, a high vacuum must be maintained inside the drying chamber. After desorption drying, the product is completely free of ice crystals and remains a honeycomb-like solid. At this point, the product moisture content is ≤2%.

[0024] Preferably, and further still, the bear bile powder produced by this method contains ≥50% taurine deoxycholic acid and ≤2% moisture.

[0025] It should be noted that the preparation method in this case can ensure that the moisture content of the bear bile powder can be further reduced compared to the preparation methods on the market, and the content of taurine deoxycholic acid can be increased.

[0026] Preferably, and further still, the bear bile powder produced by the vacuum freeze-drying process needs to be sieved through a 50-mesh sieve.

[0027] It should be noted that a uniform 50-mesh bear bile powder product can be obtained through the sieving process.

[0028] The entire freeze-drying process includes:

[0029] I. Pre-freezing procedure during the freezing stage: The material is rapidly cooled to a core temperature of -40℃ within 0.5 hours using a linear cooling method;

[0030] 2. Maintain constant temperature: Keep the -40℃ cryogenic environment for 6 hours to ensure that the material is completely solidified and crystallized;

[0031] III. System state: The macroscopic phase transformation of the material is a homogeneous frozen body;

[0032] IV. Primary drying stage (sublimation drying);

[0033] V. Vacuum Establishment: Start the vacuum system and precisely control the chamber pressure at a gradient of 0.2 mbar (absolute pressure) with increasing temperature.

[0034] VI. First stage: Raise the shelf temperature to 0℃ at a rate of 0.25℃ / min (total time 8 hours). Insulation stage: Maintain 0℃ for ice crystal sublimation for 11.5-20 hours (adjust according to material thickness).

[0035] VII. Secondary drying stage (analytical drying) temperature increase:

[0036] 8. Second stage: Increase to 15℃ at a rate of 0.083℃ / min (total time 3 hours) to achieve equilibrium: Maintain 15℃ for bound water removal for 12-20 hours;

[0037] IX. Third stage: Increase to 30℃ at a rate of 0.083℃ / min (total time 3 hours) for final drying stage: maintain 30℃ to ensure residual moisture ≤2% for 20-68 hours;

[0038] 10. Post-processing step: Emptying and material removal: The chamber is restored to normal pressure in a clean environment;

[0039] XI. Crushing Process: The bear bile powder is scooped off the rotating tray by a shovel and collected into a stainless steel drum. It is then classified into particles through a 50-mesh (300μm aperture) pharmaceutical-grade stainless steel sieve.

[0040] 12. Quality Inspection:

[0041] 1. Moisture content ≤ 2%; biological activity.

[0042] 2. The retention rate of ursodeoxycholic acid from oxorubicin is ≥50%;

[0043] 3. Microbiological indicators: Compliant with the Liaoning Province Traditional Chinese Medicine Processing Specifications and the 2020 edition of the Pharmacopoeia of the People's Republic of China, Volume IV;

[0044] 4. Control of key process parameters: Vacuum accuracy: ±0.02mbar;

[0045] 5. Plate temperature uniformity: ±1.5℃;

[0046] 6. Heating / cooling rate error: ≤5%;

[0047] 7. Inter-batch repeatability RSD < 3%;

[0048] The above technical solutions only embody the preferred technical solutions of the present invention. Any modifications that may be made by those skilled in the art to certain parts thereof embody the principles of the present invention and fall within the protection scope of the present invention.

Claims

1. A method for preparing bear bile powder, characterized in that, Instantaneous high-temperature sterilization process and vacuum freeze-drying process; The instantaneous high-temperature sterilization process includes: setting the temperature of the first layer, setting the temperature of the second layer, setting the temperature difference, pumping material, and detecting the discharge temperature.

2. The method for preparing bear bile powder according to claim 1, characterized in that, An ultra-high temperature sterilizer is required when performing the instantaneous high-temperature sterilization process.

3. The method for preparing bear bile powder according to claim 1, characterized in that, The vacuum freeze-drying process includes: a first-stage sublimation, a first-stage desorption drying, and a second-stage desorption sublimation.

4. The method for preparing bear bile powder according to claim 1, characterized in that, The bear bile powder produced by this method contains ≥50% taurine deoxycholic acid and ≤2% moisture.

5. The method for preparing bear bile powder according to claim 2, characterized in that, The bear bile powder produced by the vacuum freeze-drying process needs to be sieved through a 50-mesh sieve.

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