Preparation and separation process of donkey-hide gelatin peptide capable of tonifying qi and blood

Abstract

The invention discloses a preparation and separation process of a donkey-hide gelatin peptide for tonifying qi and blood, comprising: a housing in which a plurality of filter cartridges are uniformly arranged along the circumferential direction; a horizontal partition plate is fixed in the middle of the interior of each filter cartridge, a filter membrane roll is vertically arranged in the center of the partition plate, and a discharging barrel penetrating to the outer side of the bottom of the filter cartridge is fixedly connected to the lower portion of the filter membrane roll; a liquid inlet is formed in the side wall of the filter cartridge above the partition plate, and a liquid outlet is formed in the bottom of the filter cartridge; compared with the prior art, the device has the characteristics of multi-stage continuous screening, automatic film scraping and discharging and an anti-deformation structure, and has remarkable advantages in the aspects of separation efficiency, product purity and production cost control.

Description

Technical Field

[0001] The invention relates to the technical field of membrane separation, in particular to a preparation and separation process of donkey-hide gelatin peptide for replenishing qi and blood. Background Art

[0002] As an important component of traditional Chinese medicine, donkey-hide gelatin is made from donkey skin as the main raw material. It has the effects of replenishing qi and blood, nourishing yin and moistening dryness. However, the macromolecular collagen in traditional donkey-hide gelatin is difficult to be directly absorbed by the human body and has a low bioavailability. Decomposing macromolecular collagen into small molecular active peptides (i.e. donkey-hide gelatin peptides) through enzymatic or chemical hydrolysis can significantly improve its absorption rate and biological activity. Studies have shown that donkey-hide gelatin peptides not only retain the blood-tonifying effect of traditional donkey-hide gelatin, but also have new functions such as anti-oxidation and immune regulation. They are widely used in the fields of health products, functional foods and drug development.

[0003] At present, the separation and purification of donkey-hide gelatin peptides mainly rely on the following methods: centrifugal separation, which separates different molecular weight components through centrifugal force, but can only roughly separate large particle impurities and cannot achieve accurate molecular weight classification; multiple centrifugation operations are time-consuming and energy-consuming, and active peptides are easily denatured and inactivated due to mechanical shear force. Single-stage membrane filtration technology uses a single pore size filter membrane to intercept specific molecular weight peptides, but can only separate 1-2 target components. Multi-stage screening requires multiple devices in series, and the system is complex; the filter membrane is easy to clog and requires frequent shutdown for cleaning or replacement, resulting in low production efficiency; the residual peptides on the membrane surface are difficult to completely recover, resulting in a waste of resources. The retained materials on the surface of the filter membrane can be removed by a mechanical scraper, but because the filter membrane is elastic, the scraper and the filter membrane are not tightly attached, resulting in incomplete scraping; the filter membrane support structure is weak and is prone to deformation after long-term use, affecting the separation accuracy.

[0004] Therefore, it is necessary to provide a preparation and separation process of donkey-hide gelatin peptide for replenishing qi and blood to solve the problems raised in the above background technology. Summary of the invention

[0005] To achieve the above object, the present invention provides the following technical solutions:

[0006] A preparation and separation process of donkey-hide gelatin peptide for replenishing qi and blood, comprising the following steps:

[0007] S1. Raw material pretreatment: crush the donkey-hide gelatin raw material to a particle size of ≤1 mm, add deionized water at a material-liquid ratio of 1:10-1:15, stir to dissolve, adjust the pH to 6.5-7.5, heat to 50-60°C and keep warm for 30-40 minutes, centrifuge to remove insoluble matter, and obtain a crude donkey-hide gelatin extract;

[0008] S2. Enzymatic hydrolysis reaction: Add compound protease to the crude donkey-hide gelatin extract. The compound protease is a compound of trypsin and neutral protease in a mass ratio of 1:2 - 1:3. The enzymatic hydrolysis temperature is 45 - 55 °C, and the enzymatic hydrolysis time is 4 - 6 hours. After enzymatic hydrolysis, inactivate to obtain an enzymatic hydrolysate;

[0009] S3. Multi-stage membrane separation: Pump the enzymatic hydrolysate into a multi-stage membrane separation device, and sequentially perform fractional retention through filter membranes with molecular weights of 10 kDa, 7 kDa, 4 kDa, and 1 kDa. Control the operating pressure at 0.2 - 0.5 MPa and the flow rate at 3 - 5 L / min, and collect each level of active peptide components respectively;

[0010] S4. Drying and purification: Vacuum-concentrate each level of active peptide components to a solid content of ≥ 30%, and perform spray drying with an inlet air temperature of 160 - 180 °C and an outlet air temperature of 70 - 90 °C to obtain donkey-hide gelatin peptide powder with a purity of ≥ 90%;

[0011] The multi-stage membrane separation device in S3 includes:

[0012] A housing, inside which there are a plurality of filter cylinders arranged evenly in the circumferential direction;

[0013] In the middle of each filter cylinder, a horizontal partition is fixed. At the central position of the partition, a filter membrane roll is vertically arranged. Below the filter membrane roll, a discharge cylinder is fixedly connected and penetrates to the outside of the bottom of the filter cylinder;

[0014] On the side wall of the filter cylinder above the partition, a liquid inlet is provided, and at the bottom of the filter cylinder, a liquid outlet is provided;

[0015] Below each discharge cylinder, a collection cylinder is placed.

[0016] Further, as a preference, at the upper end of each discharge cylinder, a baffle is provided, and at the center of the baffle, a rotating shaft is fixed, and the rotating shaft is rotatably connected to the side wall of the discharge cylinder.

[0017] Further, as a preference, one end of the rotating shaft rotatably penetrates the side walls of the discharge cylinder and the filter cylinder, and a driven bevel gear is fixed. A driving bevel gear is arranged inside the housing, and the driving bevel gear meshes with each driven bevel gear.

[0018] Further, as a preference, a piston is slidably arranged in each filter cylinder, and a one-way valve that only allows liquid to enter and not exit is provided in the liquid inlet.

[0019] Further, as a preference, a rotating block is rotatably arranged at the center of each piston, and a plurality of vertically arranged scraping blades are fixed below the rotating block.

[0020] Further, as a preference, a connecting shaft is fixed above each of the rotating blocks, the connecting shaft penetrates above the filter cartridge, a connecting disk is arranged above the filter cartridge, and each of the connecting shafts is rotatably connected to the connecting disk;

[0021] A driven gear is fixed to the upper end of each connecting shaft, and a driving gear is arranged at the center of the connecting disk, and the driving gear is meshed with each driven gear.

[0022] Further, as a preference, a top lifting cylinder is provided on the top of the outer shell, and a piston rod of the top lifting cylinder is fixed to the connecting plate.

[0023] Further, as a preference, a plurality of reinforcing ribs are fixedly attached to the outer wall of the filter membrane roll, and the upper ends of the reinforcing ribs are fixed to the partition;

[0024] Furthermore, preferably, a plurality of bonding plates are distributed along the gaps of the reinforcing ribs on the outer wall of the discharge barrel, and a slip ring is also slidably provided on the outer wall of the discharge barrel, and the bottom of the bonding plate is fixed to the slip ring.

[0025] Further, as a preference, a lifting plate is provided at the lower part of the shell, and a bottom lifting cylinder is provided between the lifting plate and the bottom of the shell;

[0026] A guide shaft is fixed under each of the slip rings, and each of the guide shafts passes through the lower end of the filter cartridge and is fixed to the lifting plate.

[0027] Compared with the prior art, the present invention has the following beneficial effects:

[0028] In the present invention, a plurality of filter cartridges connected in series and filter membrane pore sizes decreasing step by step are used to achieve continuous multi-stage screening of the molecular weight of donkey-hide gelatin peptide solution, and a plurality of active peptide segments with different molecular weights can be separated.

[0029] In the present invention, all scrapers are rotated synchronously by meshing the driving gear with the driven gear, and the peptides retained on the surface of the filter membrane are quickly stripped off. The filter membrane roll is ensured to be taut during the operation of the scraper under the action of the laminating plate, so that the scraper can be fully separated from the filter membrane roll to avoid the aperture deviation caused by deformation. The driving bevel gear is linked to control the opening and closing of the baffle, and the discharge process does not require manual intervention, avoiding the time-consuming problem of traditional filter membrane cleaning.

[0030] In the present invention, the hydrolyzed donkey-hide gelatin solution can be passed through the filter membrane roll under pressure through the piston, thereby improving the filtration efficiency. The piston rises and cooperates with the sealing effect of the laminating plate to form a stable negative pressure, ensuring that the solution is efficiently absorbed and evenly distributed. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 The present invention is a flow chart of the preparation and separation process of donkey-hide gelatin peptide for replenishing qi and blood;

[0032] Figure 2 It is a schematic diagram of the internal structure of a multi-stage membrane separation device;

[0033] Figure 3 It is a schematic diagram of the sectional structure of a multi-stage membrane separation device;

[0034] Figure 4 It is a top view schematic diagram of a multi-stage membrane separation device;

[0035] Figure 5 It is a schematic diagram of the internal structure of a filter cartridge;

[0036] Figure 6 It is a schematic diagram of the sectional structure of a filter cartridge;

[0037] In the figure: 1. Outer shell; 2. Filter cartridge; 201. Partition board; 202. Filter membrane roll; 203. Discharge cylinder; 204. Baffle; 205. Piston; 206. Rotating block; 207. Scraper; 208. Liquid inlet; 209. Liquid outlet; 210. Rotating shaft; 211. Reinforcing rib; 212. Fitting plate; 213. Slip ring; 214. Guide shaft; 215. Driven bevel gear; 216. Driving bevel gear; 3. Collection cylinder; 4. Connecting pipe; 5. Connecting shaft; 6. Connecting disc; 7. Driven gear; 8. Driving gear; 9. Top lifting cylinder; 10. Lifting disc; 11. Bottom lifting cylinder. Specific implementation manner

[0038] Please refer to Figures 1-6 , in the embodiment of the present invention, a preparation and separation process of donkey-hide gelatin peptides for tonifying qi and blood is characterized by comprising the following steps:

[0039] S1. Raw material pretreatment: Crush the donkey-hide gelatin raw material to a particle size ≤ 1 mm, add deionized water according to a solid-liquid ratio of 1:10 - 1:15, stir and dissolve, then adjust the pH to 6.5 - 7.5, heat up to 50 - 60 °C and keep warm for 30 - 40 minutes, and centrifuge to remove insoluble substances to obtain a crude donkey-hide gelatin extract;

[0040] S2. Enzymatic hydrolysis reaction: Add a compound protease to the crude donkey-hide gelatin extract, the compound protease is a compound of trypsin and neutral protease in a mass ratio of 1:2 - 1:3, the enzymatic hydrolysis temperature is 45 - 55 °C, the enzymatic hydrolysis time is 4 - 6 hours, and inactivate after enzymatic hydrolysis to obtain an enzymatic hydrolysate;

[0041] S3. Multi-stage membrane separation: Pump the enzymatic hydrolysate into a multi-stage membrane separation device, and sequentially perform fractional retention through filter membranes of 10 kDa, 7 kDa, 4 kDa, and 1 kDa, control the operating pressure at 0.2 - 0.5 MPa, the flow rate at 3 - 5 L / min, and collect each level of active peptide components respectively;

[0042] S4. Drying and purification: Concentrate each level of active peptide components to a solid content of ≥30% under vacuum, and perform spray drying with an inlet air temperature of 160 - 180°C and an outlet air temperature of 70 - 90°C to obtain donkey-hide gelatin peptide powder with a purity of ≥90%.

[0043] The multi-stage membrane separation device in S3 includes:

[0044] A housing 1, inside which there are a plurality of filter cylinders 2 arranged evenly along the circumferential direction;

[0045] In the middle of each filter cylinder 2, a horizontal partition 201 is fixed. At the central position of the partition 201, a filter membrane roll 202 is vertically arranged. Below the filter membrane roll 202, a discharge cylinder 203 is fixedly connected and penetrates to the outside of the bottom of the filter cylinder 2;

[0046] On the side wall of the filter cylinder 2 above the partition 201, a liquid inlet 208 is provided, and at the bottom of the filter cylinder 2, a liquid outlet 209 is provided;

[0047] Below each discharge cylinder 203, a collection cylinder 3 is placed.

[0048] The plurality of filter cylinders 2 are connected in series in sequence: The liquid inlet 208 of the first filter cylinder 2 is connected to the supply pipeline of the hydrolyzed donkey-hide gelatin peptide solution. The liquid inlets 208 of the remaining filter cylinders 2 are respectively connected to the liquid outlet 209 of the previous filter cylinder 2, and the liquid outlet 209 of the last filter cylinder 2 is connected to the waste liquid collection device;

[0049] The filter membrane pore diameters of each filter membrane roll 202 gradually decrease along the liquid flow direction, and are used for multi-stage screening of peptide segments in the donkey-hide gelatin peptide solution according to molecular weight.

[0050] In this embodiment, at the upper end of each discharge cylinder 203, a baffle 204 is provided. At the center of the baffle 204, a rotating shaft 210 is fixed, and the rotating shaft 210 is rotatably connected to the side wall of the discharge cylinder 203.

[0051] In this embodiment, one end of the rotating shaft 210 rotatably penetrates the side walls of the discharge cylinder 203 and the filter cylinder 2, and a driven bevel gear 215 is fixed. A driving bevel gear 216 is arranged inside the housing 1, and the driving bevel gear 216 meshes with each driven bevel gear 215.

[0052] Through the driving bevel gear 216, each driven bevel gear 215 can be driven to rotate, thereby controlling the opening and closing of each baffle 204. When the filter membrane roll 202 finishes filtering, by opening the baffle 204, the peptide segments filtered and left in the filter membrane roll 202 can be discharged from the discharge cylinder 203 into the collection cylinder 3.

[0053] In this embodiment, a piston 205 is slidably arranged in each filter cylinder 2, and a one-way valve that only allows liquid to enter but not exit is arranged in the liquid inlet 208.

[0054] When the piston 205 slides upward, it can suck the ejiao peptide solution from the supply pipeline or the connecting pipe 4 into the upper part of the partition plate 201 in the filter cartridge 2.

[0055] In this embodiment, a rotating block 206 is rotatably arranged at the center of each piston 205, and a plurality of vertically arranged scraping blades 207 are fixed below the rotating block 206.

[0056] When the piston 205 descends to fit with the partition plate 201, by rotating the rotating block 206, the scraping blades 207 can move circumferentially on the inner wall of the filter membrane roll 202, so that the peptide segments on the inner wall of the filter membrane roll 202 fall off and are discharged from the discharge cylinder 203.

[0057] In this embodiment, a connecting shaft 5 is fixed above each rotating block 206. The connecting shaft 5 penetrates above the filter cartridge 2. A connecting disc 6 is arranged above the filter cartridge 2, and each connecting shaft 5 is rotatably connected to the connecting disc 6;

[0058] A driven gear 7 is fixed at the upper end of each connecting shaft 5. A driving gear 8 is arranged at the center of the connecting disc 6, and the driving gear 8 meshes with each driven gear 7.

[0059] That is to say, by driving the driving gear 8, each driven gear 7 can be driven to rotate, so as to control the rotation of each rotating block 206.

[0060] In this embodiment, a top lifting cylinder 9 is arranged at the top of the housing 1, and the piston rod of the top lifting cylinder 9 is fixed to the connecting disc 6.

[0061] By the top lifting cylinder 9, the connecting disc 6 can be driven to lift and lower, so as to control the lifting and lowering of each piston 205.

[0062] In this embodiment, a plurality of reinforcing ribs 211 are fixedly attached to the outer wall of the filter membrane roll 202, and the upper ends of the reinforcing ribs 211 are fixed to the partition plate 201.

[0063] Through the reinforcing ribs 211, the tension of the filter membrane roll 202 can be maintained to ensure that it remains taut.

[0064] In this embodiment, a plurality of fitting plates 212 are distributed along the gaps between the reinforcing ribs 211 on the outer wall of the discharge cylinder 203. A sliding ring 213 is also slidably arranged on the outer wall of the discharge cylinder 203, and the bottoms of the fitting plates 212 are fixed to the sliding ring 213.

[0065] In this embodiment, a lifting disc 10 is arranged below the housing 1, and a bottom lifting cylinder 11 is arranged between the lifting disc 10 and the bottom of the housing 1;

[0066] A guiding shaft 214 is fixed below each of the slip rings 213, and each guiding shaft 214 penetrates through the lower end of the filter cartridge 2 and is fixed to the lifting disc 10.

[0067] The lifting disc 10 can be driven by the bottom lifting cylinder 11 to move up and down, thereby controlling the sliding of each slip ring 213, so that the fitting plate 212 can fit along the gap of the reinforcing rib 211 to the outer wall of the filter membrane roll 202. When the scraper 207 moves in a circular motion on the inner wall of the filter membrane roll 202 to scrape off the peptide segments, the filter membrane roll 202 is limited in position under the action of the fitting plate 212, so that it can be closely attached to the scraper 207. In addition, when the piston 205 moves upward, the fitting plate 212 can seal the filter membrane roll 202 to ensure that a negative pressure is generated at the liquid inlet 208.

[0068] Specifically, the multi-stage membrane separation process includes:

[0069] The top lifting cylinder 9 drives the connecting disc 6 to drive all the pistons 205 to rise synchronously. When the pistons rise, the one-way valves open, and the solution is sequentially sucked into the chambers above the partition plates 201 of each filter cartridge through the liquid inlet 208;

[0070] The top lifting cylinder 9 drives the connecting disc 6 to drive all the pistons 205 to descend synchronously until they fit with the partition plate 201. During the process, the solution penetrates through the filter membrane roll 202 under the action of gravity and pressure. The large molecular peptide segments are intercepted on the inner wall of the primary filter membrane, and the small molecules enter the next stage. Each stage of the filter membrane intercepts the peptide segments within the corresponding molecular weight range, and the final filtrate is discharged as waste liquid;

[0071] The bottom lifting cylinder 11 is used to drive the lifting disc 10 to rise, so that the fitting plate 212 rises along the gap of the reinforcing rib 211 to ensure close contact with the outer wall of the filter membrane roll;

[0072] The driving bevel gear 216 is rotated to drive the driven bevel gear 215 to open the baffle 204, and the driving gear 8 is started to drive all the rotating blocks 206 and the scraper 207 to rotate, and the peptide segments on the inner wall of the filter membrane are scraped into the discharge cylinder 203.

[0073] The above is only the preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art within the technical scope disclosed by the present invention, according to the technical solution and inventive concept of the present invention, makes equivalent substitutions or changes, and should be covered by the protection scope of the present invention.

Claims

1. A preparation and separation process of Ejiao peptides for supplementing qi and blood, characterized in that, It includes the following steps: S1. Raw material pretreatment: Crush the donkey-hide gelatin raw materials to a particle size ≤ 1 mm, add deionized water according to a solid-liquid ratio of 1:10 - 1:15, stir and dissolve, then adjust the pH to 6.5 - 7.5, raise the temperature to 50 - 60 °C and keep warm for 30 - 40 minutes, and centrifuge to remove insoluble substances to obtain a crude donkey-hide gelatin extract; S2. Enzymatic hydrolysis reaction: Add a compound protease to the crude donkey-hide gelatin extract. The compound protease is a compound of trypsin and neutral protease in a mass ratio of 1:2 - 1:

3. The enzymatic hydrolysis temperature is 45 - 55 °C, the enzymatic hydrolysis time is 4 - 6 hours, and inactivate after enzymatic hydrolysis to obtain an enzymatic hydrolysate; S3. Multi-stage membrane separation: Pump the enzymatic hydrolysate into a multi-stage membrane separation device, and sequentially perform fractional retention through filter membranes with cut-off molecular weights of 10 kDa, 7 kDa, 4 kDa, and 1 kDa. Control the operating pressure at 0.2 - 0.5 MPa and the flow rate at 3 - 5 L / min, and collect each level of active peptide components respectively; S4. Drying and purification: Vacuum concentrate each level of active peptide components to a solid content ≥ 30%, and perform spray drying with an inlet air temperature of 160 - 180 °C and an outlet air temperature of 70 - 90 °C to obtain donkey-hide gelatin peptide powder with a purity ≥ 90%; The multi-stage membrane separation device in S3 includes: A housing (1) with a plurality of filter cylinders (2) uniformly arranged along the circumferential direction inside; In the middle of each filter cylinder (2), a horizontal partition plate (201) is fixed. A filter membrane roll (202) is vertically arranged at the central position of the partition plate (201), and a discharge cylinder (203) that penetrates to the outside of the bottom of the filter cylinder (2) is fixedly connected below the filter membrane roll (202); An inlet (208) is opened on the side wall of the filter cylinder (2) above the partition plate (201), and an outlet (209) is opened at the bottom of the filter cylinder (2); A collection cylinder (3) is placed below each discharge cylinder (203).

2. The preparation and separation process of a donkey-hide gelatin peptide for supplementing qi and blood according to claim 1, characterized in that, A baffle (204) is provided at the upper end of each discharge cylinder (203), and a rotating shaft (210) is fixed at the center of the baffle (204). The rotating shaft (210) is rotatably connected to the side wall of the discharge cylinder (203).

3. The preparation and separation process of an ejiao peptide for supplementing qi and blood according to claim 2, characterized in that, One end of the rotating shaft (210) rotatably penetrates the side walls of the discharge cylinder (203) and the filter cylinder (2), and a driven bevel gear (215) is fixed. A driving bevel gear (216) is arranged inside the housing (1), and the driving bevel gear (216) meshes with each driven bevel gear (215).

4. The preparation and separation process of a donkey-hide gelatin peptide for supplementing qi and blood according to claim 1, characterized in that, A piston (205) is slidably arranged in each filter cylinder (2), and a check valve that only allows liquid to enter but not exit is arranged in the inlet (208).

5. The preparation and separation process of a donkey-hide gelatin peptide for supplementing qi and blood according to claim 4, characterized in that, A rotating block (206) is rotatably arranged at the center of each piston (205), and a plurality of vertically arranged scraping blades (207) are fixed below the rotating block (206).

6. The preparation and separation process of the donkey-hide gelatin peptide for supplementing qi and blood according to claim 5, characterized in that, A connecting shaft (5) is fixed above each rotating block (206). The connecting shaft (5) penetrates above the filter cylinder (2), and a connecting disc (6) is arranged above the filter cylinder (2). Each connecting shaft (5) is rotatably connected to the connecting disc (6); A driven gear (7) is fixed to the upper end of each connecting shaft (5), a driving gear (8) is arranged at the center of the connecting disc (6), and the driving gear (8) meshes with each driven gear (7).

7. The preparation and separation process of an Ejiao peptide for supplementing qi and blood according to claim 6, characterized in that, A top lifting cylinder (9) is arranged at the top of the housing (1), and the piston rod of the top lifting cylinder (9) is fixed into the connecting disc (6).

8. The preparation and separation process of a donkey-hide gelatin peptide for supplementing qi and blood according to claim 1, characterized in that, A plurality of reinforcing ribs (211) are fixedly attached to the outer wall of the filter membrane roll (202), and the upper ends of the reinforcing ribs (211) are fixed into the partition plate (201).

9. The preparation and separation process of a donkey-hide gelatin peptide for supplementing qi and blood according to claim 8, characterized in that, A plurality of attaching plates (212) are distributed along the gaps between the reinforcing ribs (211) on the outer wall of the discharge cylinder (203), a sliding ring (213) is further slidably arranged on the outer wall of the discharge cylinder (203), and the bottom of the attaching plate (212) is fixed into the sliding ring (213).

10. The preparation and separation process of a donkey-hide gelatin peptide for supplementing qi and blood according to claim 9, characterized in that, A lifting disc (10) is arranged below the inner part of the housing (1), and a bottom lifting cylinder (11) is arranged between the lifting disc (10) and the bottom of the housing (1); A guide shaft (214) is fixed below each sliding ring (213), and each guide shaft (214) penetrates through the lower end of the filter cylinder (2) and is fixed into the lifting disc (10).

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