Preparation method and device of SOD resistant to pepsin degradation

Abstract

The application belongs to the field of SOD preparation, and discloses a preparation method and device of SOD resistant to pepsin degradation, which comprises the following steps: S1 powder preparation: dissolving SOD fermentation pure liquid in a buffer solution with pH of 5.2-7.8, adding protective agent and tea yellow in sequence, stirring, filtering, and placing in a freeze dryer to prepare freeze-dried powder; S2 drying; S3 tabletting; S4, coating liquid preparation: dissolving wheat gliadin and soybean protein in a mixed solution prepared from water and ethanol with a volume ratio of 1:1, wherein the mass ratio of the wheat gliadin and the soybean protein is 0.5-1:1, adding glycerol, stirring for 20 min by using a magnetic stirrer, and ultrasonicating for 40 s; S5, coating: placing the tablets in a coating machine, setting air inlet volume, air inlet temperature, pan rotating speed, atomization rate, fan face pressure, and mortar flow, until the coating weight increases to 3%-10% in mass fraction and the coating thickness is 20-50 μm, and then drying and cooling. The prepared SOD is not easy to be photolyzed and can resist gastric acid degradation to ensure the complete activity of the SOD.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of SOD preparation, and particularly relates to a preparation method and device of SOD resistant to pepsin degradation. BACKGROUND

[0002] SOD (superoxide dismutase) is an important free radical scavenger in the body, and has important application value in antioxidant and anti-aging, etc. Since SOD was discovered, it has been favored by scholars at home and abroad, and the research on the properties of SOD has become more and more in-depth. It is found that SOD can scavenge free radicals, improve the oxidation-reduction environment in the intestinal tract, inhibit the growth and reproduction of harmful bacteria, reduce their adhesion and invasion to the intestinal mucosa, and thus maintain the stability of the intestinal flora. Meanwhile, SOD can also adjust the oxidation-reduction potential in the intestinal tract to create a suitable growth environment for beneficial bacteria such as bifidobacterium and lactobacillus, promote the growth and reproduction of the beneficial bacteria, and the beneficial bacteria can produce substances such as short-chain fatty acids to provide energy for intestinal epithelial cells and enhance the barrier function of the intestinal mucosa, thereby further maintaining intestinal health.

[0003] SOD is essentially a protein, and its light and thermal stability is poor, and it is easy to be inactivated under acid and alkali conditions. Therefore, in the gastric acid environment, the spatial structure of SOD may be denatured, resulting in a decrease or even loss of activity. In addition, pepsin in the stomach can decompose the protein into polypeptides and amino acids, so that SOD is difficult to maintain an intact active structure to reach the intestine to play a role. Meanwhile, the tablet is easy to be affected by light and temperature during preparation, resulting in photodegradation or inactivation, and poor stability.

[0004] When preparing SOD tablets, the existing rotary tablet press is used. When the powder is fed, the powder is discharged to the outside of the die groove due to the uninterrupted discharging and the interval between the die grooves, and the powder is accumulated in a triangular shape in the die groove during discharging. During tabletting, too much powder is squeezed onto the workbench, resulting in serious waste of powder and low tabletting efficiency. In addition, the powder accumulation also causes uneven density and inconsistent strength of the prepared tablets. SUMMARY

[0005] The application aims to provide a preparation method and device of SOD resistant to pepsin degradation, which has the effects of not being easily photolyzed, being resistant to gastric acid degradation, and ensuring the integrity of the activity of SOD.

[0006] The above technical purpose of the application is achieved by the following technical scheme:

[0007] A preparation method of SOD resistant to pepsin degradation, comprising the following steps:

[0008] S1, powdering: dissolve SOD fermentation pure liquid with a purity greater than 95% in a buffer solution with a pH of 5.2-7.8, add protective agents and tea yellow in turn, stir for 30 min, filter, and then put into a freeze dryer, first reduce the temperature to 40-60°C at a rate of 1-3°C / min, and keep for 2-4 h, then start the freeze dryer, freeze at-50-30°C and under high vacuum of 10-50 Pa for 12-48 h to produce freeze-dried powder;

[0009] S2, drying: after S1 is completed, gradually increase the temperature to 0-25°C, keep the vacuum degree at 10-30 Pa for 2-10 h until the water content of the freeze-dried powder is reduced to below 5%;

[0010] S3, tabletting: mix the SOD freeze-dried powder with a binder, and the mass ratio of the binder to the SOD freeze-dried powder is 13-20:20, then use a rotary tablet press to press into tablets with a diameter of 3-8 mm;

[0011] S4, coating liquid preparation: dissolve wheat gliadin and soybean protein in a mixed solution prepared from water and ethanol with a volume ratio of 1:1, wherein the mass ratio of the wheat gliadin to the soybean protein is 0.5-1:1, add glycerol, stir at room temperature and a speed of 500 rpm for 20 min using a magnetic stirrer, and ultrasonically treat for 40 s using an ultrasonic device;

[0012] S5, coating: place the tablets in a coating machine, set the air inlet volume to 1500-1800 m3 / h, the air inlet temperature to 35-40°C, the pot rotation speed to 2-10 rpm, the atomization rate to 2-5 mL / min, the fan face pressure to 1.0-3.0 bar, and the mortar flow to 60-400 g / min, until the coating weight increases to a mass fraction of 3-10% and the coating thickness is 20-50 μm, then slowly dry at 40°C for 1 h, and cool to obtain the coated tablets.

[0013] Further provided in the application is that in step S1, the protective agent is one or more of trehalose, cyclodextrin, and mannitol, the volume ratio of the protective agent to the fermentation pure liquid is 1:1, and the volume ratio of the tea yellow to the fermentation pure liquid is 1-3:1.

[0014] Further provided in the application is that in step S3, the binder is one or more of sorbitol and malt dextrin.

[0015] Further provided in the application is that in step S4, the wheat gliadin is replaced by corn gliadin.

[0016] Further provided in the application is that in step S4, the glycerol accounts for 10-15% of the mass of the wheat gliadin.

[0017] The application discloses a preparation device of SOD resistant to pepsin degradation, and applies the preparation method of the SOD resistant to pepsin degradation.

[0018] The auxiliary discharging assembly comprises a supporting horizontal rod fixed on the rotating shaft, and a scraper fixed on one end of the supporting horizontal rod away from the rotating shaft, and the bottom of the scraper is in abutment with the inner wall of the conical cylinder for scraping.

[0019] The leveling assembly comprises an L-shaped fixing frame fixed on the workbench, and a leveling plate is arranged on the L-shaped fixing frame, the leveling plate is arc-shaped, and the opening of the leveling plate is arranged towards the feeding assembly.

[0020] The bottom circumferential wall of the rotating disc is provided with a gear rack, and a gear is fixedly arranged on the output end of the driving motor and engaged with the gear rack.

[0021] The further setting of the application is that the demolding assembly comprises a feeding channel arranged below the discharging through slot and rotationally connected with the rotating disc, the feeding channel is arranged in an S shape, gas holes are uniformly arranged on the bottom of the feeding channel, and impact baffles are arranged on the two sides of the feeding channel.

[0022] The further setting of the application is that the pressing assembly comprises a pressing cylinder fixed on the workbench, a pressing plate is fixed on the piston rod of the pressing cylinder, and a pressing block is arranged on the bottom of the pressing plate.

[0023] The further setting of the application is that the feeding assembly comprises a support, a bidirectional motor, a mixing box is arranged on the support, a stirring motor is arranged on the top of the mixing box, a rotating rod is arranged in the mixing box, the stirring motor is used for driving the rotating rod to rotate, a mixing rod is arranged on the rotating rod, a discharging port is arranged on the bottom of the mixing box, a bidirectional screw rod is rotationally arranged on the support, and a guide rod is fixedly arranged on the support.

[0024] The further setting of the application is that the excess material groove is in a trapezoidal structure, and the two waist edges are tangent to the mold grooves.

[0025] The application has the beneficial effects that:

[0026] 1. In this application, theaflavins are mixed with pure fermentation broth in a buffer solution to prepare a lyophilized powder containing SOD, which is then compressed into tablets. The phenolic hydroxyl and ketone groups of theaflavins can form hydrogen bonds with the polar amino acid residues on the surface of SOD. The active center of Cu / Zn-SOD contains copper ions, whose empty orbitals can form coordinate bonds with the ortho-phenolic hydroxyl or ketone groups of theaflavins. The hydrogen bonds and coordination effects work together to stabilize the complex structure. In the intestine, the two work synergistically. Theaflavins can compensate for the limitations of SOD against non-superoxide free radicals (such as hydroxyl free radicals) and broaden the antioxidant spectrum. SOD can enhance the free radical scavenging efficiency of theaflavins and prolong the antioxidant effect time. At the same time, theaflavins can also protect SOD during the tableting process. On the one hand, they actively absorb light energy to form a physical barrier to protect SOD. On the other hand, they scavenge free radicals generated by photolysis, inhibit metal-catalyzed oxidation reactions, and form a chemical defense against SOD, reducing the photolysis loss of SOD during tableting.

[0027] 2. This application uses a mixture of soy protein and wheat gliadin as the coating layer for tablets. Soy protein is rich in disulfide bonds and polar groups, and has strong hydrophilicity. Coating with a mixture of soy protein and wheat gliadin can improve the hydrophilicity of the coating layer, thereby increasing the SOD carrying capacity and efficiency. Wheat gliadin contains a large number of nonpolar amino acids and has strong hydrophobicity. The polar groups of soy protein can also combine with the hydrophobic regions of gliadin through hydrogen bonds and hydrophobic interactions to form a more stable network structure, ensuring the stability of the coating layer. This allows SOD to be stably isolated inside the coating layer, achieving effective and stable physical isolation from gastric acid. Experiments conducted in a simulated gastric acid environment show that after prolonged immersion in gastric acid, the SOD activity inside the coating layer is almost unaffected (activity remains above 95%), while the activity of uncoated SOD is lost by more than 95% within the same time period.

[0028] 3. This application is equipped with an arc-shaped leveling plate. The bottom of the arc-shaped leveling plate abuts against the turntable. As the turntable rotates, the leveling plate scrapes the SOD-containing powder in the mold slot, ensuring that the powder in the mold slot is evenly distributed. During pressing, there is no need for excessive pressure to level it. Only compaction is needed to make the density of each part of the tablet uniform and the strength consistent. This can effectively prevent the SOD in the tablet from being deactivated due to excessive pressure. There is a material trough between the mold slots, and the bottom of the material trough is inclined downward. The opening of the leveling plate is set towards the feeding component. The material trough can not only collect the material falling during the rotation of the turntable, but also scrape and collect the excess powder scraped off by the leveling plate. The powder falls into the conical cylinder through the material trough. The scraper inside the conical cylinder scrapes off and collects the excess material, avoiding powder waste.

[0029] 4. The application realizes automatic and continuous feeding, leveling, pressing and demolding collection of SOD tablets by setting the feeding assembly to feed the SOD-containing powder into the mold groove, moving the mold groove filled with powder to the bottom of the leveling assembly with the rotation of the rotating disc, scraping the powder flat by the leveling assembly, then rotating the rotating disc to transport the leveled mold groove to the pressing assembly for pressing, rotating the rotating disc again to drive the pressed tablet into the feeding channel for demolding by the demolding assembly, and collecting the demolding tablet, thereby realizing high processing efficiency. BRIEF DESCRIPTION OF DRAWINGS

[0030] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed in the embodiment description will be briefly introduced. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative labor.

[0031] Figure 1 is the overall structure diagram of the preparation device of the SOD resistant to pepsin degradation.

[0032] Figure 2 is the pressing assembly diagram of the preparation device of the SOD resistant to pepsin degradation.

[0033] Figure 3 is the preparation device of the SOD resistant to pepsin degradation. Figure 2

[0034] Figure 4 is the feeding assembly diagram of the preparation device of the SOD resistant to pepsin degradation.

[0035] Figure 5 is the preparation device of the SOD resistant to pepsin degradation. Figure 4

[0036] Figure 6 is the demolding assembly diagram of the preparation device of the SOD resistant to pepsin degradation.

[0037] ​​In the figure, 1, rotary tablet press; 2, workbench; 3, material guide groove; 4, bottom disc; 5, rotating disc; 6, mold groove; 7, excess material groove; 8, feeding assembly; 80, support; 81, bidirectional motor; 82, mixing box; 83, stirring motor; 84, rotating rod; 85, mixing rod; 86, discharge port; 87, bidirectional screw rod; 88, guide rod; 89, blocking plate; 9, leveling assembly; 90, L-shaped fixing frame; 91, leveling plate; 10, pressing assembly; 100, pressing cylinder; 101, pressing plate; 102, pressing block; 11, demolding assembly; 110, material conveying channel; 111, air hole; 112, collision baffle; 12, discharging channel; 13, conical cylinder; 14, rotating shaft; 15, auxiliary discharging assembly; 150, support cross rod; 151, scraper; 16, driving motor; 17, rack; 18, gear. DETAILED DESCRIPTION

[0038] The technical solutions of the present application will be described clearly and completely below in combination with specific embodiments. Obviously, the described embodiments are only some of the embodiments of the present application, rather than all the embodiments. Based on the embodiments of the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application. EMBODIMENT

[0039] The following steps are adopted to prepare the SOD-containing coated tablet 1:

[0040] S1, powder preparation: dissolve SOD fermentation pure liquid with a purity greater than 95% in a phosphate buffer with a pH of 5.2-7.8, add a mixture of trehalose and cyclodextrin with a volume ratio of 1:1 to the fermentation pure liquid, then add tea yellow with a volume ratio of 1:1 to the fermentation pure liquid, stir for 30 min, filter, and then put into a freeze dryer, first reduce the temperature at a rate of 1-3 ℃ / min to 40 ℃ to -60 ℃, and maintain for 2-4 h, then start the freeze dryer, freeze at -50 ℃ to -30 ℃ and high vacuum 10-50 Pa for 12-48 h to prepare freeze-dried powder;

[0041] S2, drying: after S1 is completed, gradually increase the temperature to 0 ℃-25 ℃, maintain the vacuum degree at 10-30 Pa for 2-10 h, until the water content of the freeze-dried powder is reduced to below 5%;

[0042] S3, tabletting: mix the SOD freeze-dried powder with the binder xylitol uniformly, the mass ratio of the binder to the SOD freeze-dried powder is 13-20:20, then adopt a rotary tablet press to press into tablets with a diameter of 3-8 mm;

[0043] S4, coating liquid preparation: dissolve the wheat prolamin and soybean protein in a mixed solution prepared from water: ethanol with a volume ratio of 1:1, wherein the mass ratio of the wheat prolamin to the soybean protein is 0.5:1, add 10%~15% of glycerol based on the mass of the wheat prolamin, stir at room temperature at a speed of 500 rpm for 20 min with a magnetic stirrer, and ultrasonic for 40 s with an ultrasonic device;

[0044] S5, coating: place the tablets in a coating machine, set the air inlet volume at 1500~1800m3 / h, the air inlet temperature at 35~40℃, the pot rotation speed at 2~10rpm, set the atomization rate at 2~5 mL / min, the fan face pressure at 1.0~3.0bar, and the mortar flow at 60~400g / min, until the coating weight increases to a mass fraction of 3%~10% and the coating thickness is 20-50μm, and then slowly dry at 40℃ for 1h, and then cool to obtain the coated tablets. Example

[0045] The following steps are used to prepare the SOD-containing coated tablets 2:

[0046] S1, powder preparation: dissolve the SOD fermentation pure liquid with a purity of more than 95% in a phosphate buffer with a pH of 5.2~7.8, add a mixture of trehalose and cyclodextrin with a volume ratio of 1:1 to the fermentation pure liquid, and then add tea yellow with a volume ratio of 3:1 to the fermentation pure liquid, stir for 30 min, filter, and then put into a freeze dryer, first reduce the temperature to 40℃ to -60℃ at a cooling rate of 1 ~3℃ / min and maintain for 2~4h, and then start the freeze dryer, freeze at -50℃ to -30℃ and under high vacuum of 10~50Pa for 12~48h to prepare the freeze-dried powder;

[0047] S2, drying: after S1 is completed, gradually increase the temperature to 0℃~25℃, maintain the vacuum degree at 10~30 Pa for 2~10h, until the water content of the freeze-dried powder is reduced to below 5%;

[0048] S3, tabletting: mix the SOD freeze-dried powder with the binder erythritol uniformly, and the mass ratio of the binder to the SOD freeze-dried powder is 13~20:20, and then use a rotary tablet press to press into tablets with a diameter of 3~8mm;

[0049] S4, coating liquid preparation: dissolve the wheat prolamin and soybean protein in a mixed solution prepared from water: ethanol with a volume ratio of 1:1, wherein the mass ratio of the wheat prolamin to the soybean protein is 1:1, add 10%~15% of glycerol based on the mass of the wheat prolamin, stir at room temperature at a speed of 500 rpm for 20 min with a magnetic stirrer, and ultrasonic for 40 s with an ultrasonic device;

[0050] S5, coating: the tablets are placed in a coating machine, the air inlet is set to 1500-1800 m3 / h, the air inlet temperature is set to 35-40°C, the pot rotation speed is set to 2-10 rpm, the atomization rate is set to 2-5 mL / min, the fan face pressure is set to 1.0-3.0 bar, and the mortar flow is set to 60-400 g / min, until the coating weight increases to 3%-10% by mass fraction and the coating thickness is 20-50 μm, 40°C slow drying for 1 h, and cooling to obtain the coated tablets. Example

[0051] The following steps are used to prepare the SOD-containing coated tablets 3:

[0052] S1, powdering: dissolve the SOD fermentation pure liquid with a purity of more than 95% in a phosphate buffer with a pH of 5.2-7.8, add a mixture of trehalose and cyclodextrin with a volume ratio of 1:1 to the fermentation pure liquid, then add tea yellow with a volume ratio of 1:1 to the fermentation pure liquid, stir for 30 min, filter, and then put into a freeze dryer, first reduce the temperature to 40°C to -60°C at a rate of 1-3°C / min, and maintain for 2-4 h, then start the freeze dryer, freeze at -50°C to -30°C and high vacuum of 10-50 Pa for 12-48 h to prepare the freeze-dried powder;

[0053] S2, drying: after S1 is completed, gradually increase the temperature to 0°C-25°C, maintain the vacuum degree at 10-30 Pa for 2-10 h, until the water content of the freeze-dried powder is reduced to below 5%;

[0054] S3, tabletting: mix the SOD freeze-dried powder with the binder erythritol uniformly, the mass ratio of the binder to the SOD freeze-dried powder is 13-20:20, then use a rotary tablet press to press into tablets with a diameter of 3-8 mm;

[0055] S4, coating liquid preparation: dissolve the wheat gliadin and soybean protein in a mixed solution prepared by mixing water and ethanol with a volume ratio of 1:1, wherein the mass ratio of the wheat gliadin to the soybean protein is 0.5:1, add 10%-15% of glycerol based on the mass of the wheat gliadin, stir at room temperature with a magnetic stirrer at a speed of 500 rpm for 20 min, and ultrasonic for 40 s with an ultrasonic device;

[0056] S5, coating: the tablets are placed in a coating machine, the air inlet is set to 1500-1800 m3 / h, the air inlet temperature is set to 35-40°C, the pot rotation speed is set to 2-10 rpm, the atomization rate is set to 2-5 mL / min, the fan face pressure is set to 1.0-3.0 bar, and the mortar flow is set to 60-400 g / min, until the coating weight increases to 3%-10% by mass fraction and the coating thickness is 20-50 μm, 40°C slow drying for 1 h, and cooling to obtain the coated tablets. Example

[0057] SOD-containing coated tablets 4 were prepared by the following steps:

[0058] The wheat prolamin in step S4 was replaced by corn prolamin, and other steps were the same as in Example 1.

[0059] Comparative Example 1

[0060] SOD-containing coated tablets 5 were prepared by the following steps:

[0061] S1, powdering: dissolve SOD fermentation pure liquid with a purity of more than 95% in a phosphate buffer with a pH of 5.2-7.8, add a mixture of trehalose and cyclodextrin at a volume ratio of 1:1 to the fermentation pure liquid, then add a pure water solution at a volume ratio of 1:1 to the fermentation pure liquid, stir for 30 min, filter, and then put into a freeze dryer, first reduce the temperature to 40-60°C at a rate of 1-3°C / min, and maintain for 2-4 h, then start the freeze dryer, and freeze at -50-30°C and under high vacuum of 10-50 Pa for 12-48 h to prepare a freeze-dried powder;

[0062] S2, drying: after S1 is completed, gradually increase the temperature to 0-25°C, maintain the vacuum degree at 10-30 Pa for 2-10 h, until the water content of the freeze-dried powder is reduced to below 5%;

[0063] S3, tabletting: mix the SOD freeze-dried powder with the binder xylitol uniformly, the mass ratio of the binder to the SOD freeze-dried powder is 13-20:20, then use a rotary tablet press to press into tablets with a diameter of 3-8 mm;

[0064] S4, preparation of coating solution: dissolve wheat prolamin and soybean protein in a mixed solution prepared by mixing water and ethanol at a volume ratio of 1:1, wherein the mass ratio of wheat prolamin to soybean protein is 0.5:1, add 10-15% glycerol based on the mass of the wheat prolamin, stir at room temperature at a speed of 500 rpm for 20 min using a magnetic stirrer, and ultrasonic for 40 s using an ultrasonic device;

[0065] S5, coating: place the tablets in a coating machine, set the air inlet volume at 1500-1800 m3 / h, the air inlet temperature at 35-40°C, the pan rotation speed at 2-10 rpm, set the atomization rate at 2-5 mL / min, the fan face pressure at 1.0-3.0 bar, and the mortar flow rate at 60-400 g / min, until the coating weight increases to a mass fraction of 3-10% and the coating thickness is 20-50 μm, then slowly dry at 40°C for 1 h, and cool to obtain the coated tablets.

[0066] Comparative Example 2

[0067] The following steps are used to prepare SOD-containing tablet 6:

[0068] S1, powdering: Dissolve SOD fermentation pure liquid with a purity greater than 95% in a phosphate buffer with a pH of 5.2-7.8, add a mixture of trehalose and cyclodextrin at a volume ratio of 1:1 to the fermentation pure liquid, then add tea polyphenol at a volume ratio of 1-3:1 to the fermentation pure liquid, stir for 30 min, filter, and then place in a freeze dryer, first reduce the temperature to 40-60°C at a rate of 1-3°C / min, and maintain for 2-4 h, then start the freeze dryer, and freeze at -50-30°C and a high vacuum of 10-50 Pa for 12-48 h to produce freeze-dried powder;

[0069] S2, drying: After S1 is complete, gradually increase the temperature to 0-25°C, maintain a vacuum of 10-30 Pa for 2-10 h, until the water content of the freeze-dried powder is reduced to less than 5%;

[0070] S3, tabletting: Mix the SOD freeze-dried powder with the binder, xylitol, uniformly, the mass ratio of the binder to the SOD freeze-dried powder is 13-20:20, then use a rotary tablet press to press into tablets with a diameter of 3-8 mm, to produce uncoated tablets 6.

[0071] Test method: Test the gastric acid resistance of coated tablets 1-5 and tablet 6

[0072] Simulated gastric acid environment: Prepare a hydrochloric acid solution with a pH of 1.2, containing 0.3% (w / v) pepsin, as a simulated gastric acid environment.

[0073] Sample processing: Take coated tablets 1-5 and tablet 6 and add to the simulated gastric acid solution, and incubate in a constant-temperature shaking incubator at 37°C with shaking at 100 rpm for 4 h.

[0074] Activity detection: After incubation, determine the activity of SOD in the solution by a specific SOD activity detection kit, and compare with the activity of untreated SOD.

[0075] The results show that after 4 h of simulated gastric acid treatment, SOD in coated tablets 1-4 still retains more than 95% of the activity, among which coated tablet 2 has the best effect, retaining 99.3% of the activity of SOD, while the activity of SOD in coated tablet 5 is maintained at 85%, and the activity of SOD in tablet 6 is lost by more than 98%, indicating that the addition of tea polyphenol can increase the activity of the prepared SOD coated tablets, and the coating layer formed by the mixture of soybean protein and wheat prolamin is more stable, which can protect SOD from pepsin degradation. Example

[0076] The application discloses a preparation device of SOD resistant to pepsin degradation, and applies the preparation method of the SOD resistant to pepsin degradation. Figures 1-6 As shown in the figure, the device comprises a rotary tablet press 1, the rotary tablet press 1 comprises a workbench 2, a guide groove 3 is formed in the workbench 2, a bottom disc 4 is fixedly arranged in the guide groove 3, a rotating disc 5 is rotatably connected to the upper portion of the bottom disc 4, die grooves 6 are uniformly formed along the circumference of the rotating disc 5, at least four die grooves 6 are arranged and excess material grooves 7 are arranged between the die grooves 6, the die grooves 6 and the bottom disc 4 form a material storage space, an upper feeding assembly 8, a leveling assembly 9, a pressing assembly 10 and a demolding assembly 11 are sequentially arranged along the outer circumference of the rotating disc 5, a discharging through groove 12 is formed in the bottom disc 4 at the demolding assembly 11, the excess material grooves 7 are arranged in a downwardly inclined manner and a conical cylinder 13 is arranged below the excess material grooves 7, the top of the conical cylinder 13 is open, a rotating shaft 14 is fixedly arranged at the center of the rotating disc 5, the rotating shaft 14 penetrates through the conical cylinder 13 and an auxiliary discharging assembly 15 is arranged at the portion of the rotating shaft 14 in the conical cylinder 13, wherein the excess material grooves 7 are in a trapezoidal structure and the two waist sides are tangent to the die grooves 6.

[0077] As shown in the figure, Figure 6 The auxiliary discharging assembly 15 comprises a supporting cross rod 150 fixedly arranged on the rotating shaft 14, a scraper 151 is fixedly arranged at the end of the supporting cross rod 150 away from the rotating shaft 14, and the bottom of the scraper 151 is in abutment with the inner wall of the conical cylinder 13 for scraping material.

[0078] As shown in the figure, Figure 6 The leveling assembly 9 comprises an L-shaped fixing frame 90 fixedly arranged on the workbench 2, the L-shaped fixing frame 90 is provided with a leveling plate 91, the leveling plate 91 is in an arc shape and the opening of the leveling plate 91 is arranged towards the upper feeding assembly 8, and the bottom of the leveling plate 91 is in sliding connection with the rotating disc 5.

[0079] As shown in the figure, Figure 3 , Figure 6 The device further comprises a driving motor 16 for driving the rotating disc 5 to rotate, the bottom of the rotating disc 5 is provided with a rack 17, a gear 18 is fixedly arranged at the output end of the driving motor 16, and the gear 18 is in meshing connection with the rack 17.

[0080] As shown in the figure, Figure 6 The demolding assembly 11 comprises a material conveying passage 110 arranged below the discharging through groove 12 and in rotatable connection with the rotating disc 5, the material conveying passage 110 is in an S shape and is uniformly provided with air holes 111 at the bottom, and impact baffles 112 are arranged at the two sides of the material conveying passage 110.

[0081] As shown in the figure, Figure 2 , Figure 3 The pressing assembly 10 comprises a pressing air cylinder 100 fixedly arranged on the workbench 2, a pressing plate 101 is fixedly arranged on the piston rod of the pressing air cylinder 100, a pressing block 102 is arranged at the bottom of the pressing plate 101, and the size of the pressing block 102 is matched with the size of the die grooves 6.

[0082] AsFigure 4 、 Figure 5 、 Figure 6 As shown in FIGS. 8 to 10, the feeding assembly 8 comprises a support 80, a bidirectional motor 81, the support 80 is provided with a mixing box 82, the top of the mixing box 82 is provided with a stirring motor 83, the inside of the mixing box 82 is provided with a rotating rod 84, the stirring motor 83 is used to drive the rotating rod 84 to rotate, the rotating rod 84 is provided with a mixing rod 85, the bottom of the mixing box 82 is provided with a discharging port 86, the support 80 is rotatably provided with a bidirectional screw rod 87, and a guide rod 88 is fixedly arranged on the support 80, the bidirectional motor 81 is used to drive the bidirectional screw rod 87 to rotate, the discharging port 86 is slidably connected with a blocking plate 89, one end of the blocking plate 89 is threadedly connected with the bidirectional screw rod 87, and the other end of the blocking plate 89 is slidably connected with the guide rod 88.

[0083] The working principle is as follows: first, the stirring motor 83 is started to drive the rotating rod 84 and the mixing rod 85 to rotate, so that the powder in the mixing box 82 is uniformly mixed, the bidirectional motor 81 is controlled to drive the bidirectional screw rod 87 to rotate, so as to drive the blocking plate 89 to slide along the guide rod 88, when the blocking plate 89 moves away from the rotating disc 5, the discharging port 86 is gradually opened, the discharging speed becomes faster, when the blocking plate 89 moves towards the rotating disc 5, the discharging port 86 is gradually closed, the discharging speed becomes slower, the discharging speed can be flexibly adjusted, the tabletting efficiency is improved, and the powder falls from the falling port to the storage space formed by the mold groove 6 and the bottom disc 4 below;

[0084] When the storage space is filled to a certain amount, the driving motor 16 is started to drive the gear 18 to rotate, so as to drive the rotating disc 5 to rotate, the rotating disc 5 rotates by 90 degrees each time, drives the mold groove 6 full of powder to move to the leveling assembly 9, then the next mold groove 6 continues to feed, after the feeding is completed, the rotating disc 5 rotates by 90 degrees again, in the rotating process, the leveling plate 91 scrapes the powder accumulated in the mold groove 6 to be flat, and scrapes the excess powder and the powder falling on the rotating disc 5 in the rotating process into the excess material groove 7, after the scraping is completed, the mold groove 6 whose powder is leveled is located at the pressing assembly 10, at this time, the pressing cylinder 100 is started to drive the pressing plate 101 and the pressing block 102 to move downwards to press the leveled powder into a tablet shape, then the rotating disc 5 rotates by 90 degrees again, at this time, the powder in the next mold groove 6 is scraped to be flat, the tablet product is moved to the discharging groove 12 on the bottom disc 4, falls into the S-shaped conveying channel 110 through the discharging groove 12 automatically, and continuously collides with the collision baffle 112 in the process of falling along the S-shaped conveying channel 110, so as to vibrate the powder remaining on the tablet to fall off, the air hole 111 is larger than the size of the powder, the excess powder falls through the air hole 111 and is collected, the tablet is collected through the discharge port of the conveying channel 110, the empty mold groove 6 moves to the discharging port 86 again to discharge, and the feeding, scraping, pressing and demolding and collecting are circularly implemented, so that the automatic tabletting and high processing efficiency are realized;

[0085] When the rotary disc 5 rotates, the powder falling from the discharge port 86 is automatically dropped into the excess material groove 7, the excess powder generated by scraping is also scraped into the excess material groove 7, and the powder falling on the rotary disc 5 during rotation is also scraped into the excess material groove 7. The bottom of the excess material groove 7 is inclined downward, and the powder is automatically dropped into the opening of the conical cylinder 13. When the driving motor 16 is started to drive the rotary disc 5 to rotate, the rotating shaft 14 rotates, and then drives the supporting cross rod 150 and the scraper 151 to rotate. The scraper 151 abuts against the inner wall of the conical cylinder 13 to scrape off the powder falling on the inner wall of the conical cylinder 13, and finally falls from the discharge port 86 of the conical cylinder 13 to realize automatic collection and reuse, avoiding waste of powder.

Claims

1. A method for preparing SOD resistant to pepsin degradation, characterized in that: Includes the following steps: S1. Powdering: Dissolve SOD fermentation broth with a purity greater than 95% in a buffer solution with a pH of 5.2-7.8, add the protective agent and theaflavins sequentially, stir for 30 min, filter, and place in a freeze dryer. First, cool to 40℃ to -60℃ at a cooling rate of 1-3℃ / min and maintain for 2-4 h. Then start the freeze dryer and freeze at -50℃ to -30℃ and high vacuum of 10-50Pa for 12-48 h to produce freeze-dried powder. The protective agent is one or more of trehalose, cyclodextrin, and mannitol. The volume ratio of the protective agent to the fermentation broth is 1:1, and the volume ratio of theaflavins to the fermentation broth is 1-3:

1. S2. Drying: After S1 is completed, gradually reduce the temperature to 0℃~25℃ and maintain a vacuum of 10~30 Pa for 2~10 hours until the moisture content of the freeze-dried powder is reduced to below 5%. S3. Tableting: Mix the SOD lyophilized powder and binder evenly. The mass ratio of binder to SOD lyophilized powder is 13~20:

20. Then, use a rotary tablet press to compress the mixture into tablets with a diameter of 3~8mm. S4. Preparation of coating solution: Dissolve wheat gliadin and soy protein in a mixed solution with a water:ethanol volume ratio of 1:1, wherein the mass ratio of wheat gliadin to soy protein is 0.5~1:

1. Add glycerol, stir with a magnetic stirrer at room temperature and 500 rpm for 20 min, and sonicate with an ultrasonic device for 40 s. S5. Coating: Place the tablets in the coating machine and set the airflow to 1500~1800 m³ / h. 3 The process involves setting the following parameters: air inlet temperature at 35-40℃, drum rotation speed at 2-10 rpm, atomization rate at 2-5 mL / min, fan pressure at 1.0-3.0 bar, and spray flow rate at 60-400 g / min. The coating is dried slowly at 40℃ for 1 hour until the weight gain reaches 3%-10% by mass and the coating thickness is 20-50 μm. The coated sheets are then obtained by cooling.

2. The method for preparing SOD resistant to pepsin degradation according to claim 1, characterized in that: In step S3, the binder is one or more of sorbitol and maltodextrin.

3. The method for preparing SOD resistant to pepsin degradation according to claim 1, characterized in that: In step S4, wheat gliadin is replaced with zein.

4. The method for preparing SOD resistant to pepsin degradation according to claim 1, characterized in that: In step S4, glycerol accounts for 10% to 15% of the amount of wheat alcohol-soluble protein.

5. An apparatus for preparing SOD resistant to pepsin degradation, using the method for preparing SOD resistant to pepsin degradation as described in any one of claims 1-4, characterized in that: The rotary tablet press includes a worktable (2) with a guide groove (3) on it. A base plate (4) is fixed inside the guide groove (3). A turntable (5) is rotatably attached above the base plate (4). Mold slots (6) are evenly distributed along the circumference of the turntable (5). There are at least four mold slots (6), and a material storage slot (7) is provided between each mold slot (6). The mold slots (6) and the base plate (4) form a material storage space. Material is stored sequentially along the outer circumference of the turntable (5). The device is equipped with a feeding assembly (8), a leveling assembly (9), a pressing assembly (10), and a demolding assembly (11). The chassis (4) has a discharge channel (12) at the demolding assembly (11). The waste material groove (7) is inclined downward and has a conical cylinder (13) below it. The top of the conical cylinder (13) is open. The turntable (5) has a rotating shaft (14) fixed in the center. The rotating shaft (14) passes through the conical cylinder (13), and an auxiliary feeding assembly (15) is provided at the part of the rotating shaft (14) inside the conical cylinder (13). The auxiliary feeding assembly (15) includes a support crossbar (150) fixed on the rotating shaft (14). A scraper (151) is fixed at one end of the support crossbar (150) away from the rotating shaft (14). The bottom of the scraper (151) abuts against the inner wall of the conical cylinder (13) for scraping material. The leveling component (9) includes an L-shaped fixing frame (90) fixed on the workbench (2), and a leveling plate (91) is provided on the L-shaped fixing frame (90). The leveling plate (91) is arc-shaped and the opening faces the feeding component (8). The bottom of the leveling plate (91) is slidably connected to the turntable (5). It also includes a drive motor (16) for driving the turntable (5) to rotate. The bottom circumferential outer wall of the turntable (5) is provided with a rack (17). The output end of the drive motor (16) is fixed with a gear (18), which meshes with the rack (17).

6. The apparatus for preparing SOD resistant to pepsin degradation according to claim 5, characterized in that: The demolding assembly (11) includes a material conveying channel (110) located below the material feeding channel (12) and rotatably connected to the turntable (5). The material conveying channel (110) is S-shaped and has air holes (111) evenly opened at the bottom. Collision baffles (112) are provided on both sides of the material conveying channel (110).

7. The apparatus for preparing SOD resistant to pepsin degradation according to claim 6, characterized in that: The pressing assembly (10) includes a pressing cylinder (100) fixed on the workbench (2). A pressure plate (101) is fixed on the piston rod of the pressing cylinder (100). A pressing block (102) is provided at the bottom of the pressure plate (101). The size of the pressing block (102) is adapted to the size of the mold groove (6).

8. The apparatus for preparing SOD resistant to pepsin degradation according to claim 6, characterized in that: The feeding assembly (8) includes a bracket (80) and a bidirectional motor (81). The bracket (80) is provided with a mixing box (82). The mixing box (82) is provided with a stirring motor (83) at the top and a rotating rod (84) inside. The stirring motor (83) is used to drive the rotating rod (84) to rotate. The rotating rod (84) is provided with a mixing rod (85). The mixing box (82) is provided with a discharge port (86) at the bottom. The bracket (80) is rotatably provided with a bidirectional lead screw (87) and a guide rod (88) is fixedly provided. The bidirectional motor (81) is used to drive the bidirectional lead screw (87) to rotate. A sealing plate (89) is slidably connected at the discharge port (86). One end of the sealing plate (89) is threaded to the bidirectional lead screw (87), and the other end is slidably connected to the guide rod (88).

9. The apparatus for preparing SOD resistant to pepsin degradation according to claim 6, characterized in that: The waste material groove (7) has a trapezoidal structure, and its two waist sides are tangent to the mold groove (6).

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