Method for producing bear gall powder and freeze-drying device

Abstract

The present application belongs to the technical field of bear gall powder production, and provides a bear gall powder production method and a freeze-drying device. The method comprises the following steps: taking bear bile and filtering, obtaining a filtered bile solution after filtering; placing the filtered bile solution in a condition of-40 DEG C to-45 DEG C for pre-freezing treatment for 1.5 to 2.5 hours, keeping for 1.5 to 2.0 hours after pre-freezing; increasing the temperature to-10 DEG C to-15 DEG C, keeping for 1.5 to 2.5 hours; then controlling the temperature to increase in stages, keeping in stages, increasing the temperature to 37 DEG C to 40 DEG C and keeping, obtaining dry materials; sieving the dry materials, obtaining bear gall powder. The method can effectively reduce energy consumption, shorten processing time, and obtain bear gall powder with less impurities, low moisture, high purity and stable quality. The device has more uniform heat conduction, more sensitive temperature regulation, and can better meet the temperature increasing, temperature decreasing, keeping and other regulation and control requirements of the bear gall powder freeze-drying process.

Description

Technical Field

[0001] This invention belongs to the field of bear bile powder production technology, specifically relating to a method for producing bear bile powder and a freeze-drying apparatus. Background Technology

[0002] Bear bile powder is a processed product obtained from the bile of the black bear (Amur gudgeon), a traditional Chinese medicine with effects such as improving eyesight, clearing heat and detoxifying, and soothing the liver and promoting bile secretion. The main production methods for bear bile powder include oven drying, microwave drying, and freeze-drying. Oven drying and microwave drying involve high temperatures, which can lead to some loss of the effective components of bear bile and result in poor appearance, affecting the quality and appearance of the bear bile powder product. Freeze-drying involves drying by sublimation of water at low temperatures. This method has less impact on the effective components of bear bile, better preserves the active ingredients, and produces a better-looking product than oven-dried or microwave-dried bear bile powder. However, existing freeze-drying processes have problems such as long processing time and high energy consumption, resulting in high production costs. Summary of the Invention

[0003] To address the shortcomings of the existing technology, this invention provides a method for producing bear bile powder and a freeze-drying apparatus. This method effectively shortens the freeze-drying processing time and reduces energy consumption through pre-freezing treatment, holding, heating, holding, and staged heating and holding. The freeze-drying apparatus has more uniform heat conduction and more sensitive temperature regulation, which can better meet the control requirements of heating, cooling, and holding in the freeze-drying process of bear bile powder.

[0004] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0005] The method for producing bear bile powder includes the following steps:

[0006] S1, take bear bile and filter it to obtain filtered bile solution;

[0007] S2, the filtered bile solution is pre-frozen at -40℃ to -45℃ for 1.5 to 2.5 hours, and then kept at the pre-frozen temperature for 1.5 to 2.0 hours; the temperature is then raised to -10℃ to -15℃ and kept at the pre-frozen temperature for 1.5 to 2.5 hours; then the temperature is raised in stages and maintained in stages until the temperature reaches 37℃ to 40℃ and is maintained, thus obtaining the dried material;

[0008] S3. The dried material is sieved to obtain bear bile powder.

[0009] In one embodiment of this application, in step S1, the filtration includes two filtrations, the first filtration using a filter element with a pore size of 0.45 μm and the second filtration using a filter element with a pore size of 0.25 μm.

[0010] In one embodiment of this application, in step S2, the filtered bile solution is dispensed into a material tray for pre-freezing treatment, and the depth of the filtered bile solution in the material tray is controlled to be 1.8~2.2cm.

[0011] In one embodiment of this application, in step S2, when the temperature is raised to -10°C to -15°C and held, the vacuum degree is controlled to be 40 to 60 Pa; when the temperature is raised in stages and held in stages, the vacuum degree is controlled to be 15 to 25 Pa.

[0012] And / or, in step S2, during the pre-freezing treatment, the cooling rate is controlled at 0.45℃~0.6℃ / min; during the heating to -10℃~-15℃, the heating rate is controlled at 0.45℃~0.6℃ / min; during the staged heating, the heating rate is controlled at 0.4℃~0.5℃ / min.

[0013] In one embodiment of this application, in step S2, the temperature is controlled to rise in stages and maintained in stages, raising the temperature to 37°C~40°C and maintaining it, specifically including:

[0014] In the first stage, the temperature is controlled to rise to -8℃~-5℃, and the heating and holding time is 90~120min;

[0015] In the second stage, the temperature is controlled to rise to 2℃~5℃, and the heating and holding time is 90~120min;

[0016] In the third stage, the temperature is controlled to rise to 12℃~15℃, and the heating and holding time is 120~150min;

[0017] In the fourth stage, the temperature is controlled to rise to 22℃~25℃, and the heating and holding time is 120~150min;

[0018] In the fifth stage, the temperature is controlled to rise to 27℃~30℃, and the heating and holding time is 300~360 minutes.

[0019] In the sixth stage, the temperature is controlled to rise to 32℃~35℃, and the heating and holding time is 300~360min;

[0020] In the seventh stage, the temperature is controlled to rise to 37℃~40℃, and the heating and holding time is 60~90 minutes.

[0021] In one embodiment of this application, the step S1 is further included:

[0022] S01, collect fresh bear bile, quick-freeze and transport it at -18℃~-22℃ for storage and use as raw material for bear bile cryopreservation;

[0023] S02, take the frozen bear bile raw material and thaw it in a water bath at 10℃~15℃ to obtain bear bile raw material.

[0024] In one embodiment of this application, in step S1, the bear bile is a mixture of a first bear bile raw material and a second bear bile raw material. The first bear bile raw material is bear bile collected from November to March of the following year, and the second bear bile raw material is bear bile collected from April to October. The volume ratio of the first bear bile raw material to the second bear bile raw material is 1:1.8~2.3.

[0025] In one embodiment of this application, the bear bile powder has a moisture content of less than 2% and a tauroursodeoxycholic acid content of 40.5% to 43.5%.

[0026] A freeze-drying apparatus for producing bear bile powder includes a freeze-drying chamber, wherein several freeze-drying shelves are installed vertically at intervals within the freeze-drying chamber, and the freeze-drying shelves include:

[0027] The top panel has a smooth heat-conducting surface on one side and a groove on the other side. Several spacers are arranged parallel to each other in the groove, and the spacers divide the groove into a continuous serpentine flow channel.

[0028] The bottom plate is adapted to fit into the groove of the top plate, and the bottom plate is provided with a slot corresponding to the spacer strip;

[0029] The upper panel is integrally formed with the partition strip; the lower panel is welded to the partition strip through the groove, and the edge of the lower panel is welded to the edge of the groove.

[0030] In one embodiment of this application, the top of the partition strip is provided with a large V-shaped groove along the length direction, the width of the groove opening is the same as the width of the large V-shaped groove, and the angles α of the bottom of the large V-shaped groove and β of the side wall of the large V-shaped groove and the side wall of the groove opening are both 110°~140°.

[0031] The upper panel has a first bevel on the outer edge of the groove, and the lower panel has a second bevel corresponding to the first bevel on the edge. The first bevel and the second bevel form a large V-shaped welding groove.

[0032] The groove opens at one end of the edge of the lower panel, and the large V-shaped groove and the large V-shaped welding groove are connected.

[0033] Compared with the prior art, the beneficial effects of the present invention are:

[0034] 1. The bear bile powder production method of the present invention includes pre-freezing treatment, post-pre-freezing holding, heating (-10℃ to -15℃), and holding treatment during the freeze-drying process. The pre-freezing treatment freezes the solution, changing it from a liquid to a solid state. Holding after freezing further develops the freezing process, increasing the gaps between the columnar ice crystals within the ice layer, which facilitates the direct sublimation of the solvent from solid to gas, accelerating the freeze-drying process. Then, the temperature is raised to a relatively high level (-10℃ to -15℃) for holding, ensuring sufficient sublimation drying while reducing cold energy consumption. Finally, through staged heating and temperature control holding, the drying time and energy consumption are shortened, allowing the bear bile powder to be dried at a relatively low temperature. The resulting bear bile powder has low moisture content, good retention of active ingredients, uniform crystals, a bright golden color, rapid dissolution, and no insoluble matter. This production method is particularly suitable for producing bear bile powder from bear bile in summer and autumn with relatively lower concentrations, as well as for producing bear bile powder with concentrations between those of bear bile in summer / autumn and winter.

[0035] 2. The bear bile powder production method of the present invention uses two filter cartridges with different pore sizes for filtration. The first filtration uses a filter cartridge with a pore size of 0.45μm, which has a fast filtration speed and can effectively remove large particles, fat and other impurities. The second filtration uses a filter cartridge with a pore size of 0.25μm, which is conducive to effectively filtering out bacteria and other microorganisms. The use of filter cartridges with different pore sizes for the two filtrations can effectively shorten the filtration time, reduce the loss of effective ingredients, and improve the filtration effect of impurities and microorganisms, resulting in a product with a reduced fishy smell.

[0036] 3. Bear bile is low in yield and thick in winter (approximately November to March of the following year), and high in yield and thin in summer and autumn (approximately April to October). When bear bile from different seasons is freeze-dried separately, the quality of the resulting bear bile powder varies greatly. Furthermore, the freeze-drying process using a universal method maintains a relatively low temperature range, leading to energy waste when freeze-drying bear bile from summer and autumn. This invention mixes bear bile from winter and summer / autumn in a specific ratio to obtain a mixed bear bile raw material with a suitable concentration. The freezing point / eutectic point of this mixed bear bile raw material is higher than that of the winter bear bile (thick), allowing for freeze-drying at a relatively high temperature (-10℃ to -15℃). This achieves the freeze-drying effect while reducing energy consumption, and the resulting bear bile powder product has good quality stability.

[0037] 4. The freeze-drying apparatus of this application features a groove and spacer on the upper panel of the freeze-drying layer. The spacer and the upper panel are integrally formed without welding (in traditional freeze-drying layers, the spacer, upper panel, and lower panel are separate structures, connected by welding, i.e., the spacer is welded to both the upper and lower panels). This design makes heat conduction between the heat transfer medium and the heat transfer surface more uniform and temperature adjustment more sensitive, resulting in a more uniform temperature distribution of the material in contact with the heat transfer surface. When used for freeze-drying process control in the bear bile powder production method of this invention, it can effectively meet the control requirements for cooling / heating, making the freeze-drying process control more precise. Furthermore, the freeze-drying layer of this application has grooves on the lower panel corresponding to the spacer, through which the spacer is welded to the lower panel, as well as the edges. This reduces the number of welding points on the freeze-drying layer, lowers the welding difficulty, simplifies operation, effectively reduces manufacturing costs, and eliminates welding deformation on the heat transfer surface of the upper panel, making quality control easier.

[0038] 5. Setting up large V-grooves and large V-shaped welding grooves (first bevel and second bevel), and connecting the large V-grooves and large V-shaped welding grooves, can effectively ensure the welding quality of the weld, avoid incomplete fusion and penetration, and further ensure the quality of the freeze-dried layer. Attached Figure Description

[0039] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0040] Figure 1 This is a flowchart of the bear bile powder production method in this invention.

[0041] Figure 2 These are comparative photographs of the bear bile powder prepared in Example 1 and Comparative Example 1.

[0042] Figure 3 The images show a comparison between the bear bile powder of Example 1 and bear bile powder prepared by a commercially available drying process.

[0043] Figure 4 This is a schematic diagram of the structure of the freeze-drying chamber and freeze-drying layer in the freeze-drying device for producing bear bile powder in this invention.

[0044] Figure 5 This is a three-dimensional structural diagram of the freeze-dried layer in this invention.

[0045] Figure 6 This is a schematic diagram of the structure of the upper panel with the groove side in this invention.

[0046] Figure 7 This is a schematic diagram of the structure of the lower panel and the upper panel mating side in this invention.

[0047] Figure 8 for Figure 6 A schematic diagram of the cross-sectional structure of the BB section.

[0048] Figure 9 for Figure 5 A schematic diagram of the cross-sectional structure of the AA section.

[0049] Figure 10 for Figure 9 Enlarged structural diagram of part C in the middle.

[0050] Figure 11 for Figure 10 Enlarged structural diagram of part D in the middle.

[0051] Figure label:

[0052] 1. Freeze-drying chamber;

[0053] 2. Freeze-dried shelves;

[0054] 3. Top panel; 31. Heat conduction surface; 32. Groove; 33. Spacer; 331. Large V-groove; 34. First bevel;

[0055] 4. Bottom panel; 41. Groove; 42. Second bevel. Detailed Implementation

[0056] In the following description, only certain exemplary embodiments are briefly described. As those skilled in the art will recognize, the described embodiments can be modified in various ways without departing from the spirit or scope of the invention. Therefore, the drawings and description are considered to be exemplary in nature and not restrictive.

[0057] The embodiments of the present invention will now be described in detail with reference to the accompanying drawings.

[0058] This invention provides a method for producing bear bile powder, which involves freeze-drying bear bile to produce bear bile powder. Figure 1 As shown, the method for producing bear bile powder includes the following steps:

[0059] S1, take bear bile and filter it to obtain a filtered bile solution.

[0060] Preferably, a two-stage filtration process is employed. The first filtration uses a filter element with a pore size of 0.45 μm to quickly remove large particulate impurities from the bear bile, such as tissue fragments and fat. The second filtration uses a filter element with a pore size of 0.25 μm to ensure effective removal of fine microbial impurities from the bile solution, minimize the loss of active ingredients, and shorten the filtration time.

[0061] S2, the filtered bile solution obtained in step S1 is dispensed and placed in a freeze-drying device for freeze-drying. First, it is pre-frozen at -40℃ to -45℃ for 1.5 to 2.5 hours. After the pre-freezing time is reached, the temperature is maintained for 1.5 to 2.0 hours. After the maintenance time is reached, the temperature is raised at a relatively uniform rate until it reaches -10℃ to -15℃, and then the temperature is maintained for 1.5 to 2.5 hours. Then, the temperature is raised in stages and maintained in stages until the temperature finally reaches 37℃ to 40℃ and is maintained to obtain the dried material.

[0062] The process involves dispensing the filtered bile solution into a material tray for pre-freezing, with the depth of the filtered bile solution in the material tray preferably controlled to be 1.8~2.2cm.

[0063] Pre-freezing and subsequent holding are performed at atmospheric pressure without vacuum treatment. However, when controlling the temperature to rise at a relatively uniform rate to -10℃ to -15℃ and maintaining the temperature, vacuum treatment is required, with the vacuum level controlled at 40~60 Pa. When controlling the temperature rise in stages and maintaining it in stages, controlling the vacuum level within the range of 15~25 Pa can effectively remove bound moisture.

[0064] During pre-freezing, the cooling rate is preferably controlled at approximately 0.45℃~0.6℃ / min; during the heating process from -40℃~-45℃ to -10℃~-15℃, the heating rate is controlled at 0.45℃~0.6℃ / min; during the staged heating, the heating rate is controlled at 0.4℃~0.5℃ / min. By controlling the cooling rate of the pre-freezing treatment, the size of the crystals formed during the freezing process can be controlled to a certain extent. Combined with the holding treatment after pre-freezing, a faster sublimation drying rate and bound water removal rate can be obtained, thereby shortening the freeze-drying time.

[0065] The process involves controlling the temperature rise in stages and maintaining it in phases to ultimately reach 37℃~40℃, and includes the following seven stages:

[0066] In the first stage, the temperature is controlled to rise from -10℃ to -15℃ to -8℃ to -5℃, the heating rate is controlled, and the total holding time after the temperature rises to -8℃ to -5℃ is controlled to be 90 to 120 minutes.

[0067] In the second stage, the temperature is controlled to rise from -8℃ to -5℃ to 2℃ to 5℃, the heating rate is controlled, and the total duration of the heating process and holding at 2℃ to 5℃ is controlled to be 90 to 120 minutes.

[0068] In the third stage, the temperature is controlled to rise from 2℃~5℃ to 12℃~15℃, the heating rate is controlled, and the total holding time after heating to 12℃~15℃ is controlled to be 120~150min.

[0069] In the fourth stage, the temperature is controlled to rise from 12℃~15℃ to 22℃~25℃, the heating rate is controlled, and the total holding time after the temperature rises to 22℃~25℃ is controlled to be 120~150min.

[0070] In the fifth stage, the temperature is controlled to rise from 22℃~25℃ to 27℃~30℃, the heating rate is controlled, and the total holding time after the temperature rises to 27℃~30℃ is controlled to be 300~360min.

[0071] In the sixth stage, the temperature is controlled to rise from 27℃~30℃ to 32℃~35℃, the heating rate is controlled, and the total holding time after the temperature reaches 32℃~35℃ is controlled to be 300~360min.

[0072] In the seventh stage, the temperature is controlled to rise from 32℃~35℃ to 37℃~40℃, the heating rate is controlled, and the total holding time after the temperature reaches 37℃~40℃ is controlled to be 60~90 minutes.

[0073] By controlling the temperature rise in stages and maintaining the temperature in stages, the bound moisture in the material can be effectively removed, saving energy and reducing the impact on the effective components in the material.

[0074] In step S2, a pre-freezing treatment is performed to rapidly freeze the solution from a liquid to a solid state. After freezing, the temperature is maintained constant to further develop the freezing process during sublimation drying. This increases the gaps between the columnar ice crystals within the ice layer, making it easier for the solvent to sublimate directly from the solid to the gaseous state, thus accelerating the freeze-drying process. Then, the temperature is raised to -10℃ to -15℃, a temperature range close to but lower than the eutectic point / freezing point of the filtered bile solution. Maintaining this temperature for continuous sublimation drying effectively ensures the sublimation drying effect while reducing cold energy consumption. Finally, by using a phased heating and temperature control method, strongly bound adsorbed moisture is better removed, and the drying temperature is reduced, shortening the drying time.

[0075] S3. The dried material obtained in step S2 is a loose, lumpy material. It needs to be sieved through a sterilized sieve in a clean environment to obtain a bear bile powder product with uniform particles.

[0076] Preferably, the bear bile powder is sieved through a 60-mesh vibrating screen. After sieving, the bear bile powder can be further sterilized by ozone or ultraviolet light.

[0077] Steps S1 to S3 are all performed in a clean environment, and all equipment used is disinfected. Environmental and equipment disinfection can be carried out using ultraviolet light, ozone, alcohol, high temperature and humidity, etc.

[0078] In one embodiment, a pretreatment step of bear bile is included before performing step S1, specifically including the following steps:

[0079] S01. Bear bile is collected from healthy black bears aged 4-6 years at the breeding farm using a drainage tube. After collection, the bile is packaged and quickly frozen at -18℃ to -22℃. It is then stored and transported at -18℃ to -22℃. The quick-frozen fresh bear bile is used as raw material for bear bile cryopreservation. The preferred cryopreservation time for bear bile raw material is controlled within 24 months.

[0080] S02, before performing step S1, take the above-mentioned frozen bear bile raw material and place it in a water bath at 10℃~15℃ for rapid thawing. After thawing, the required bear bile raw material is obtained.

[0081] Quick-freezing and transporting fresh bear bile effectively solves the problem of unstable and fluctuating bile collection volumes from farms. Multiple collections can be conducted before transportation and subsequent freeze-drying, facilitating transportation, preserving the active components of bear bile, and controlling batch production in the freeze-drying process, thus ensuring consistent product quality across batches. Before freeze-drying, a suitable amount of frozen bear bile is thawed according to the batch production volume using a rapid thawing method in a 10℃~15℃ water bath. This effectively avoids the problems of temperature instability and damage to active components associated with natural thawing, as well as the leaching of insoluble substances from effective components during natural thawing, thus better guaranteeing the quality of the obtained bear bile.

[0082] Preferably, in step S1, the bear bile used is a mixture of a first bear bile raw material and a second bear bile raw material. The first bear bile raw material is bear bile collected from November to March of the following year, i.e., winter bear bile; the second bear bile raw material is bear bile collected from April to October of the year, i.e., summer and autumn bear bile. When mixing the bear bile, it is preferable to control the volume ratio of the first bear bile raw material to the second bear bile raw material to be 1:1.8~2.3.

[0083] Black bear bile has a low yield and is viscous in winter (approximately November to March of the following year), while it is high yield and thin in summer and autumn (approximately April to October). When bear bile from different seasons is freeze-dried separately, the quality of the resulting bear bile powder varies significantly. Furthermore, using a universal freeze-drying process for summer and autumn bear bile results in energy waste. Mixing winter and summer / autumn bear bile in a specific ratio yields a mixed bear bile raw material with a suitable concentration. This mixed bear bile raw material has a higher freezing point / eutectic point than the winter bear bile (which is viscous), allowing the freeze-drying process to be conducted at a relatively high temperature (-10℃ to -15℃). This achieves the freeze-drying effect while reducing energy consumption, and the resulting bear bile powder product exhibits good quality stability.

[0084] The bear bile powder prepared by the above method has a moisture content of less than 2% and a tauroursodeoxycholic acid content of 40.5% to 43.5%.

[0085] For the same purpose, the present invention also provides a freeze-drying apparatus for producing bear bile powder.

[0086] like Figure 4-11 As shown, the freeze-drying device for producing bear bile powder includes a freeze-drying chamber 1, and several freeze-drying plates 2 are installed vertically and vertically inside the freeze-drying chamber 1, with equal spacing between adjacent freeze-drying plates 2.

[0087] The freeze-drying shelf 2 has a heat transfer medium flowing through it for heat transfer between the heat transfer medium and the freeze-dried material. The freeze-drying shelf 2 includes an upper panel 3 and a lower panel 4, which are welded together.

[0088] Specifically, such as Figure 5 , Figure 6 , Figure 8 and Figure 9 As shown, one side of the upper panel 3 is a smooth heat conduction surface 31, which is used to contact the material tray or material; the other side of the upper panel 3 has a concave groove 32, the groove wall of which is at the edge of the upper panel 3, and several spacers 33 are arranged parallel to each other in the groove 32. The spacers 33 are staggered and connected to the two opposite sides of the groove 32, and the spacers 33 divide the groove 32 into a continuous serpentine flow channel. One end of the serpentine flow channel has an inlet and the other end has an outlet for the heat conduction medium to flow.

[0089] like Figure 7 , Figure 9 , Figure 10 and Figure 11As shown, the lower panel 4 is sized to fit the upper panel 3 and fits onto one side of the groove 32 in the upper panel 3, sealing the opening of the groove 32. The lower panel 4 is provided with several slots 41 corresponding to the inner spacers 33 in the upper panel 3. One end of each slot 41 is open and the other end is blind. The slots 41 are parallel to each other and their openings are staggered and face the two opposite sides of the lower panel 4.

[0090] The upper panel 3 and the spacer 33 are integrally formed, ensuring uniform heat conduction. The lower panel 4 is welded to the spacer 33 via a welding rod / welding bar inserted through the groove 41, preferably with the weld surface flush with the side of the lower panel 4 away from the groove 32. The edge of the lower panel 4 is welded to the edge of the groove 32, which means the edge of the lower panel 4 is welded to the edge of the other side of the upper panel 3.

[0091] In a preferred embodiment, such as Figure 6 , Figure 7 , Figure 9 , Figure 10 and Figure 11 As shown, the top of the partition strip 33 has a large V-shaped groove 331 along its length, and the bottom of the large V-shaped groove 331 has an included angle α. The width of the groove opening 41 is the same as the width of the large V-shaped groove 331. When the upper panel 3 and the lower panel 4 are correspondingly closed, the groove opening 41 and the large V-shaped groove 331 are appropriately matched, and the side wall of the groove opening 41 and the side wall opening of the large V-shaped groove 331 are joined to form an included angle β. The included angle α at the bottom of the large V-shaped groove 331 and the included angle β between the side wall of the large V-shaped groove 331 and the side wall of the groove opening 41 are both 110°~140°, preferably both included angle α and included angle β are 120°.

[0092] Correspondingly, the outer edge of the groove 32 of the upper panel 3 is provided with a first bevel 34. The edge of the lower panel 4 is provided with a second bevel 42 corresponding to the first bevel 34. When the upper panel 3 and the lower panel 4 are closed, the first bevel 34 and the second bevel 42 are joined to form a large V-shaped weld groove. Preferably, the included angle of the large V-shaped weld groove is 110°~140°.

[0093] The large V-groove 331 extends from one end of the spacer 33 to the opening at the first bevel 34, and the other end is a blind end; the groove 41 of the lower panel 4 is open on one side edge; the large V-groove 331, the groove 41 and the large V-shaped welding groove are connected during welding, which can effectively avoid leakage points.

[0094] The freeze-drying device features a groove 32 and a spacer 33 on the upper panel 3 of the freeze-drying plate 2. The spacer 33 and the upper panel 3 are integrally formed without welding (in traditional freeze-drying plates, the spacer, upper panel, and lower panel are separate structures, connected by welding, i.e., the spacer is welded to both the upper and lower panels). This makes the heat conduction between the heat transfer medium and the heat transfer surface 31 more uniform and the temperature adjustment more sensitive, resulting in a more uniform temperature distribution of the material in contact with the heat transfer surface 31. When used for freeze-drying process control in the bear bile powder production method of this invention, it can effectively meet the control requirements for cooling / heating, making the freeze-drying process control more precise. The lower panel 4 of the freeze-drying plate 2 has a groove 41 corresponding to the spacer 33. The spacer 33 is welded to the lower panel 3 through the groove 41, and the edges are also welded. This reduces the number of welding parts in the freeze-drying plate 2, lowers the welding difficulty, simplifies operation, and effectively reduces manufacturing costs. Furthermore, there is no welding deformation on the heat transfer surface 31 of the upper panel 3, making quality easier to control. Setting up a large V-groove 331, a large V-shaped welding groove (first bevel 34, second bevel 42), and connecting the large V-groove 331 and the large V-shaped welding groove can effectively ensure the welding quality of the weld, avoid incomplete fusion and penetration, and further ensure the quality of the freeze-dried layer 2.

[0095] Experimental Example 1

[0096] A method for producing bear bile powder includes the following steps:

[0097] S01. Bear bile is collected from healthy black bears aged 4-6 years at the breeding farm, packaged, and quickly frozen at approximately -20°C. It is then transported at -18°C to -22°C and sent to the freeze-drying workshop as raw material for bear bile cryopreservation. Bear bile collected between November and March of the following year is used as the first type of bear bile raw material, and bear bile collected between April and October is used as the second type of bear bile raw material; both are stored and labeled separately.

[0098] S02, take the frozen bear bile raw material and place it in a water bath at about 15°C to thaw quickly. After thawing, the desired bear bile raw material is obtained.

[0099] S1, take the first bear bile raw material and the second bear bile raw material and mix them in a volume ratio of 1:2. Then, filter the mixed bear bile through a filter element with a pore size of 0.45μm for the first time and through a filter element with a pore size of 0.25μm for the second time. After the second filtration, the filtered bile solution is obtained.

[0100] S2, the filtered bile solution is dispensed into material trays, with a solution depth of approximately 2.0 cm and an area of ​​not less than 0.2 m². It is then placed in the freeze-drying chamber of the freeze-drying apparatus, with the temperature controlled at approximately -42°C. The cooling rate is controlled at approximately 0.5°C / min by adjusting the flow rate of the heat transfer medium, and the pre-freezing process is carried out for 2.2~2.5 h. The temperature is then maintained at approximately -42°C for 2.0 h. Next, the vacuum level is controlled at 40~60 Pa, and the temperature is increased at approximately 0.5°C / min to approximately -15°C, and this temperature is maintained for approximately 2.0 h. Afterwards, the vacuum level is controlled within the range of 15~25 Pa, and the temperature is increased in stages at approximately 0.4°C / min, with staged temperature control and maintenance. The specific stage control is as follows:

[0101] In the first stage, the temperature is controlled to rise from -15℃ to -5℃, and the total duration of the temperature rise and temperature holding is 100 minutes.

[0102] In the second stage, the temperature is controlled to rise from -5℃ to 5℃, and the total duration of the temperature rise and temperature holding is 100 minutes.

[0103] In the third stage, the temperature is controlled to rise from 5℃ to 15℃, and the total duration of the temperature rise and temperature holding is 145 minutes.

[0104] In the fourth stage, the temperature is controlled to rise from 15℃ to 25℃, and the total duration of the temperature rise and temperature holding is 145 minutes.

[0105] In the fifth stage, the temperature is controlled to rise from 25°C to 0°C, and the total duration of the temperature rise and temperature holding is 330 minutes.

[0106] In the sixth stage, the temperature is controlled to rise from 30℃ to 35℃, the heating rate is controlled, and the total duration of the heating process and temperature holding is controlled to be 330 minutes.

[0107] In the seventh stage, the temperature is controlled to rise from 35℃ to 40℃, and the total duration of the temperature rise and temperature holding is 80 minutes.

[0108] After the freeze-drying process in step S2, a fluffy dried material is obtained.

[0109] S3, the screening room is treated with ozone sterilization for 60 minutes to remove the freeze-dried material. The material is then vibrated and sieved through a sterilized 60-mesh sieve to obtain a golden-yellow, bright, and uniformly sized bear bile powder product. Figure 2 and Figure 3 As shown, the bear bile powder was tested and found to have a moisture content of 1.28% and a tauroursodeoxycholic acid content of 42.2%.

[0110] Depend on Figure 3It is evident that the bear bile powder prepared in this experiment has a more golden and lustrous color, higher crystal purity, and better appearance; while commercially available bear bile powder produced using a drying process contains black impurities and is brown in color.

[0111] Experiment Example 2

[0112] The difference between this experimental example and Experimental Example 1 is that the quick-freezing and preservation in step S01 and the thawing process in step S02 were not performed. The fresh bear bile used in summer and autumn in step S1 was filtered directly. The remaining operations in this experimental example are the same as in Experimental Example 1 and will not be described again.

[0113] The bear bile powder product obtained in this experiment is golden and bright in color, with uniform granules / crystals; the moisture content of the bear bile powder was 1.17%, and the tauroursodeoxycholic acid content was 40.9%.

[0114] Experimental Example 3

[0115] The difference between this experimental example and Experimental Example 1 is that in step S1, the bear bile is obtained by mixing the first bear bile raw material and the second bear bile raw material at a volume ratio of 1:1.8. The remaining operations in this experimental example are the same as in Experimental Example 1 and will not be repeated here.

[0116] The bear bile powder product obtained in this experiment is golden and bright in color, with uniform granules / crystals; the moisture content of the bear bile powder was tested to be 1.83%, and the tauroursodeoxycholic acid content was 43.4%.

[0117] Experiment Example 4

[0118] The difference between this experimental example and Experimental Example 1 is that in step S1, the bear bile is obtained by mixing the first bear bile raw material and the second bear bile raw material at a volume ratio of 1:2.3. The remaining operations in this experimental example are the same as in Experimental Example 1 and will not be repeated here.

[0119] The bear bile powder product obtained in this experiment is golden and bright in color, with uniform granules / crystals; the moisture content of the bear bile powder was tested to be 1.18%, and the tauroursodeoxycholic acid content was 41.2%.

[0120] Comparative Example 1

[0121] The difference between this comparative example and Experimental Example 1 is that the bear bile used in step S1 is the first bear bile raw material; both filtrations were performed using a filter cartridge with a pore size of 0.45 μm. The remaining operations are the same as in Experimental Example 1 and will not be described again.

[0122] The obtained bear bile powder products, such as Figure 2 As shown, the color is orange-yellow, and the particles / crystals are uniform. The test results showed that the moisture content of the bear bile powder was 4.69%, and the tauroursodeoxycholic acid content was 39.6%.

[0123] Depend on Figure 2 It is evident that the bear bile powder prepared in Experiment Example 1 has a more golden and bright color and higher crystal purity.

[0124] Comparative Example 2

[0125] The difference between this comparative example and Experimental Example 1 is that both the first and second filtrations in step S1 use filter cartridges with a pore size of 0.25 μm. The remaining operations are the same as in Experimental Example 1 and will not be described again.

[0126] The obtained bear bile powder product has an orange-yellow color and uniform granules / crystals; the moisture content of the bear bile powder is 1.43%, and the tauroursodeoxycholic acid content is 36.3%.

[0127] Comparative Example 3

[0128] The difference between this comparative example and Experimental Example 1 is that in step S2, the filtered bile solution is dispensed into material trays and placed in the freeze-drying chamber of the freeze-drying apparatus, with the temperature controlled at around -42℃ for pre-freezing for 5-6 hours; then the temperature is raised and vacuum is applied, controlling the temperature to 40-50℃ and the vacuum degree to 20-30 Pa, for drying for 18-19 hours. The remaining operations are the same as in Experimental Example 1.

[0129] The obtained bear bile powder product is golden and bright in color, with uniform granules / crystals; the moisture content of the bear bile powder is 7.82%, and the tauroursodeoxycholic acid content is 38.4%.

Claims

1. A method for producing bear bile powder, characterized in that, Includes the following steps: S01, Fresh bear bile is quick-frozen and transported at -18℃ to -22℃ as raw material for bear bile cryopreservation; S02, take the frozen bear bile raw material and thaw it in a water bath at 10℃~15℃ to obtain bear bile raw material; S1, take bear bile and filter it to obtain filtered bile solution; In step S1, the bear bile is a mixture of a first bear bile raw material and a second bear bile raw material. The first bear bile raw material is bear bile from November to March of the following year, and the second bear bile raw material is bear bile from April to October. The volume ratio of the first bear bile raw material to the second bear bile raw material is 1:1.8~2.

3. S2, the filtered bile solution is pre-frozen at -40℃ to -45℃ for 1.5 to 2.5 hours, and then kept at the pre-frozen temperature for 1.5 to 2.0 hours; the temperature is then raised to -10℃ to -15℃ and kept at the pre-frozen temperature for 1.5 to 2.5 hours; then the temperature is raised in stages and maintained in stages until the temperature reaches 37℃ to 40℃ and is maintained, thus obtaining the dried material; S3. The dried material is sieved to obtain bear bile powder.

2. The method for producing bear bile powder according to claim 1, characterized in that, In step S1, the filtration includes two filtrations. The first filtration uses a filter element with a pore size of 0.45 μm, and the second filtration uses a filter element with a pore size of 0.25 μm.

3. The method for producing bear bile powder according to claim 1, characterized in that, In step S2, the filtered bile solution is dispensed into a material tray for pre-freezing, and the depth of the filtered bile solution in the material tray is controlled to be 1.8~2.2cm.

4. The method for producing bear bile powder according to claim 1 or 3, characterized in that, In step S2, when the temperature is raised to -10℃ to -15℃ and held, the vacuum degree is controlled at 40~60Pa; when the temperature is raised in stages and held in stages, the vacuum degree is controlled at 15~25Pa. And / or, in step S2, during the pre-freezing treatment, the cooling rate is controlled at 0.45℃~0.6℃ / min; during the heating to -10℃~-15℃, the heating rate is controlled at 0.45℃~0.6℃ / min; during the staged heating, the heating rate is controlled at 0.4℃~0.5℃ / min.

5. The method for producing bear bile powder according to claim 4, characterized in that, In step S2, the temperature is controlled to rise in stages and maintained in stages, raising the temperature to 37℃~40℃ and holding it thereafter. Specifically, this includes: In the first stage, the temperature is controlled to rise to -8℃~-5℃, and the heating and holding time is 90~120min; In the second stage, the temperature is controlled to rise to 2℃~5℃, and the heating and holding time is 90~120min; In the third stage, the temperature is controlled to rise to 12℃~15℃, and the heating and holding time is 120~150min; In the fourth stage, the temperature is controlled to rise to 22℃~25℃, and the heating and holding time is 120~150min; In the fifth stage, the temperature is controlled to rise to 27℃~30℃, and the heating and holding time is 300~360 minutes. In the sixth stage, the temperature is controlled to rise to 32℃~35℃, and the heating and holding time is 300~360min; In the seventh stage, the temperature is controlled to rise to 37℃~40℃, and the heating and holding time is 60~90 minutes.

6. The method for producing bear bile powder according to claim 1, characterized in that, The bear bile powder has a moisture content of less than 2% and a tauroursodeoxycholic acid content of 40.5% to 43.5%.

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