Natural tremella polysaccharide and application thereof

Abstract

The present application belongs to the technical field of food technology, especially the field of extraction of tremella polysaccharide, and can be applied to the field of food and cosmetics as raw material. The preparation method of natural tremella polysaccharide comprises the following steps: S1. primary extraction: after the tremella is crushed, a certain amount of NaOH is added to adjust the pH to a certain range, and heating and incubation are performed; S2. solid-liquid separation: the pH of the extracted liquid is adjusted to neutral, and the extraction liquid and the precipitate are separated; S3. secondary extraction: the precipitate of step S2 is added with NaOH, and steps S1 and S2 are repeated, and the extraction liquids obtained twice are combined; S4. desalination: a membrane separation system with a suitable pore size is selected for desalination; S5. decolorization: the desalted extraction liquid is selected for decolorization by a suitable resin; S6. membrane concentration: the liquid is separated by a high molecular weight membrane separation system with a specific molecular weight cut-off, and the permeate and the retentate are collected respectively; S7. drying: the retentate is dried in a spray drying tower, and the dry powder is collected. The natural tremella polysaccharide has high extraction rate and high purity.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of food technology, especially the field of extraction of tremella polysaccharide, which can be used as raw material in the field of food and cosmetics. BACKGROUND

[0002] Tremella is a widely cultivated edible fungus in China, which has high nutritional value and high medicinal value. Tremella polysaccharide is the main active substance of tremella, accounting for 70-75% of the dry weight of tremella. A large number of studies have proved that tremella polysaccharide has the effects of immune regulation, hypoglycemic and hypolipidemic, anti-radiation, anti-oxidation, anti-aging, etc. In addition, tremella polysaccharide can increase the solution viscosity and emulsion stability, and has good moisturizing and lubricating effect, so tremella polysaccharide has a very high application prospect in the field of food and cosmetics.

[0003] Tremella polysaccharide is soluble in water, but difficult to dissolve in high-concentration organic solvents. At present, the methods commonly used for extracting tremella polysaccharide are hot water extraction, alkali extraction, enzyme extraction, ultrasonic extraction, etc. In addition, the crude polysaccharide contains a lot of impurities, and it is difficult to remove all the impurities by the existing technology, so the color of the crude polysaccharide is yellow. Patent CN112010993A uses enzyme method combined with ultrasonic-assisted extraction of tremella polysaccharide, and purifies the polysaccharide with ethanol / inorganic salt aqueous two-phase solution. The extraction conditions of this patent are mild, but the extraction rate of the prepared tremella polysaccharide is only 30%-45%, and the operation of this method is difficult, especially the preparation of ethanol / inorganic salt aqueous two-phase solution system, which is difficult to operate in industry. Patent CN112442135A uses freeze-drying technology to prepare tremella residues, and then repeatedly freeze-thaw the tremella residues to extract tremella polysaccharide. After microfiltration, alcohol precipitation and other steps, the refined tremella polysaccharide content can reach about 95%, but the yield is only 17.1%. In addition, the vacuum freeze-drying technology consumes a lot of energy, which is difficult to realize in industrial production. Patent CN104926953A uses ultrasonic-assisted treatment and then heat extraction to extract tremella polysaccharide, and then obtains a light yellow powder after ethanol precipitation and hydrogen peroxide decolorization. This method is relatively simple in process and saves energy, and the yield of tremella polysaccharide is about 20%.

[0004] At present, the extraction process of tremella polysaccharide is complex, the extraction rate is low and the cost is high, the purity of tremella polysaccharide is not enough, the color is yellow, and it cannot meet the market demand, which greatly limits the application of tremella polysaccharide. SUMMARY

[0005] The first technical purpose of the present application is to provide a natural tremella polysaccharide with high extraction rate and high purity.

[0006] The second technical purpose of the present application is to provide an application of a natural tremella polysaccharide with high extraction rate and high purity.

[0007] The first technical purpose of the present application is achieved by the following technical scheme:

[0008] A natural tremella polysaccharide, and a preparation method thereof, the preparation method comprising the following steps:

[0009] S1. Primary extraction: after the tremella is crushed, a certain proportion of pure water is added, a certain amount of NaOH is added to adjust the pH to a certain range, and heating and holding are performed;

[0010] S2. Solid-liquid separation: the extracted material liquid is adjusted to neutral pH, and is introduced into a separation device to obtain an extraction liquid and a precipitate;

[0011] S3. Secondary extraction: the precipitate of step S2 is added to a certain proportion of water and NaOH, and is extracted again under appropriate conditions, and steps S1 and S2 are repeated, and the extraction liquids obtained twice are combined;

[0012] S4. Desalination: a membrane separation system with a suitable pore size is selected for desalination;

[0013] S5. Decolorization: the desalted extraction liquid is selected to pass through a suitable resin for decolorization;

[0014] S6. Membrane concentration: the material liquid passes through a high molecular membrane separation system with a specific molecular weight cut-off to directionally cut off target substances in a certain molecular weight range, and the permeate and the cut-off liquid are collected respectively;

[0015] S7. Drying: the cut-off liquid is introduced into a spray drying tower for drying, and dry powder is collected.

[0016] The present application uses dry tremella fruiting bodies as raw materials, and prepares high-purity (≥90%) tremella polysaccharide products through extraction, desalination, decolorization, membrane separation, drying and other processes. The product prepared by the process has the advantages of high content and light color, greatly improves the product quality, reduces the application difficulty, has high yield, and is very suitable for industrial production.

[0017] As preferred, the solid-liquid ratio of step S1 extraction is 1:30-80 (tremella W: water V), the pH is adjusted to 11-13, the extraction temperature is controlled at 60-100 DEG C, and the extraction time is 1-5 hours.

[0018] As preferred, the pH of the extraction liquid is adjusted to 6-8 by hydrochloric acid before the solid-liquid separation of step S2, and the solid-liquid separation device is one of a plate and frame filter, a horizontal screw centrifuge, a disc centrifuge or other solid-liquid separation devices.

[0019] As preferred, a high molecular membrane filtration system with a pore size of 1-100 KDa is selected for step S4, the conductivity of the concentrated liquid is monitored to be reduced to 1-100 ms / cm or less, and if the conductivity does not reach this value, several more times of water can be added.

[0020] Preferably, in step S5, a certain amount of water is added to the extract to make the Brix value of the extract within the range of 0.1-1%. The decolorizing resin type is either anion exchange resin or cationic resin, and the column loading method is static adsorption or dynamic adsorption to decolorize the extract.

[0021] Preferably, in step S6, a polymer membrane filtration system with a pore size of 30-300 kDa is selected to concentrate the feed solution to 2-5% Brix.

[0022] Preferably, the inlet air temperature for spray drying in step S7 is 180-200℃, and the outlet air temperature is 90-100℃.

[0023] Preferably, the decolorization step S5 uses a specific chromatography column adsorption elution device, including a box and a holding bottle. The box has placement holes, and multiple sets of holding bottles pass through the corresponding placement holes and are slidably connected to the box. The device also includes a clamping mechanism, a mounting mechanism, an adjusting device, a driving device, and a sealing device. The box has multiple mounting seats, and multiple clamping mechanisms pass through the corresponding mounting seats and are rotatably connected to the box. The box has a hinge, and the mounting mechanism passes through the hinge and is rotatably connected to the box. The connecting end of the adjusting device is connected to the output end of the holding bottle. The adjusting device has a working chamber, and the driving device is evenly installed in the working chamber. The connecting end of the sealing device is connected to the output end of the adjusting device.

[0024] More preferably, the clamping mechanism further includes sliders, knobs, clamping blocks, and rubber pads. Multiple sets of clamping blocks pass through corresponding mounting bases and are rotatably connected to the housing. Multiple sets of sliding grooves are provided on the housing. Multiple sets of sliders pass through corresponding sliding grooves and are slidably connected to the housing. Multiple sets of sliders are provided with rotating holes. Multiple sets of knobs pass through corresponding rotating holes and are threadedly connected to corresponding sliders. Multiple sets of rubber pads are evenly installed on corresponding clamping blocks. The output ends of multiple sets of sliders are hinged to the connecting ends of corresponding clamping blocks.

[0025] More preferably, the clamping mechanism further includes clamping blocks, buckles, baffles, and springs. Multiple sets of buckles pass through the hinge base and are rotatably connected to the housing. The hinge base is provided with multiple sets of clamping holes. Multiple sets of clamping blocks pass through the corresponding clamping holes and are threadedly connected to the hinge base. The housing is provided with multiple sets of grooves. The connecting ends of multiple sets of baffles pass through the corresponding grooves and are slidably connected to the housing. Multiple sets of springs are evenly installed on the corresponding baffles.

[0026] More preferably, the adjusting device further comprises sealing rings, end covers, connecting pipes, infusion tanks and filter covers, the connecting ends of the plurality of end covers are respectively communicated with the output ends of the corresponding holding bottles, the plurality of sealing rings are uniformly installed on the corresponding end covers, the connecting ends of the plurality of connecting pipes are communicated with the output ends of the corresponding end covers, a plurality of through holes are provided in the working cavity, the output ends of the plurality of connecting pipes are respectively fixedly sleeved with the infusion tanks through the corresponding through holes, a plurality of water outlets are provided in the working cavity, and the connecting ends of the plurality of filter covers are respectively connected with the connecting ends of the corresponding water outlets.

[0027] More preferably, the driving device further comprises a motor, a driving wheel, a driven wheel, an auxiliary wheel and valve shafts, a plurality of through holes are provided in the plurality of water outlets, the plurality of valve shafts are uniformly installed in the corresponding water outlets and are rotationally connected with the corresponding water outlets, the output ends of the plurality of driven wheels are respectively connected with the connecting ends of the corresponding valve shafts through the corresponding through holes, an installation groove is provided in the infusion tank, a plurality of shaft holes are provided in the installation groove, the output ends of the plurality of driven wheels are rotationally connected with the infusion tank through the corresponding shaft holes, the connecting end of the motor is connected with the top end of the infusion tank, the output end of the motor is connected with the connecting end of the driving wheel through the corresponding shaft hole, the connecting end of the auxiliary wheel is connected with the bottom end of the installation groove, and the output ends of the plurality of driven wheels are engaged with the output ends of the driving wheel and the driven wheel.

[0028] More preferably, the sealing device further comprises connecting buckles and screw rods, the connecting ends of the plurality of connecting buckles are respectively communicated with the output ends of the corresponding water outlets, screw holes are provided on the plurality of connecting buckles, and the plurality of screw rods are respectively threadedly connected with the corresponding connecting buckles through the corresponding screw holes.

[0029] As a preferred, the step S7 uses a spray drying device for spray drying the tremella polysaccharide concentrated solution, which comprises a spray drying device body, a storage cylinder body is arranged at the middle of the top end of the spray drying device body, a working cavity is arranged in the storage cylinder body, a lifting mechanism, a driving mechanism and a cleaning mechanism are arranged at the top end of the cleaning machine;

[0030] The cleaning mechanism further comprises a cleaning cover plate, a driving shaft, a mounting frame and cleaning brushes, the bottom end of the cleaning cover plate is provided with a clamping groove, the top end of the storage cylinder body is sealingly clamped with the clamping groove arranged at the bottom end of the cleaning cover plate, the top end of the cleaning cover plate is provided with a first through hole in the middle, the top end of the driving shaft is tightly sleeved with the first through hole arranged in the middle of the top end of the cleaning cover plate, the mounting frame is connected with the driving shaft, a plurality of cleaning brushes are arranged at the outer end of the mounting frame, the outer ends of the plurality of cleaning brushes are tightly attached to the side wall of the working cavity, the top end of the driving shaft is provided with the driving mechanism, the left and right ends of the cleaning cover plate are provided with the lifting mechanism, and the front and rear ends of the cleaning cover plate are provided with the limiting mechanism.

[0031] Preferably, the driving mechanism further comprises a servo motor and a controller, the bottom end of the servo motor is connected with the middle part of the top end of the cleaning cover plate, the output end of the servo motor is connected with the top end of the driving shaft, the front end of the spray drying device body is provided with the controller, the controller is electrically connected with the servo motor, and the outer end of the servo motor is provided with a protection mechanism.

[0032] Preferably, the lifting mechanism further comprises two groups of electric telescopic rods and a lifting plate, the two groups of electric telescopic rods are electrically connected with the controller, the outer end of the cleaning cover plate is provided with the lifting plate, the bottom ends of the two groups of electric telescopic rods are respectively connected with the left and right ends of the top end of the spray drying device body, and the output ends of the two groups of electric telescopic rods are respectively connected with the left and right ends of the bottom end of the lifting plate.

[0033] Preferably, the limiting mechanism further comprises two groups of limiting rods and two groups of blocking plates, the front and rear ends of the spray drying device body are provided with the two groups of limiting rods, the front and rear ends of the lifting plate are provided with second through holes, the two groups of limiting rods are respectively and slidably sleeved with the second through holes arranged at the front and rear ends of the lifting plate, and the top ends of the two groups of limiting rods are provided with the two groups of blocking plates.

[0034] In conclusion, the present application has the following advantages:

[0035] 1. The present application uses dry tremella fruiting body as raw material, and through extraction, desalination, decolorization, membrane separation and drying processes, a high-purity (≥90%) tremella polysaccharide product is prepared. The product prepared by the process has the advantages of high content and light color, greatly improving the product quality and reducing the application difficulty, and has a high yield, which is very suitable for industrial production.

[0036] 2. In the process of column chromatography, the eluent and adsorbent are extracted by the equipment, the containing bottle in the box is fixed by the sliding clamping mechanism, the containing bottle is stabilized by rotating the clamping mechanism, the containing bottle of the eluent and the adsorbent is switched by starting the driving device, and the containing bottle is discharged through the adjusting device, and the sealing device is communicated with the equipment, so that the convenience of the equipment is improved, the working efficiency of the column chromatography is improved, and the yield of natural tremella polysaccharide is improved.

[0037] 3. The use of the spray drying device body, storage cylinder, working cavity, cleaning cover plate, drive shaft, mounting bracket, cleaning brush, servo motor, controller, two sets of electric telescopic rods, lifting plate, two sets of limit rods and two sets of blocking plates, when the storage cylinder needs to be cleaned, first open the lid of the storage cylinder by the worker, then make the two sets of electric telescopic rods slide downward along the direction of the two sets of limit rods by the controller, so that the cleaning cover plate is sleeved with the storage cylinder, then start the servo motor, the servo motor drives the drive shaft to reciprocate in the forward and reverse directions, the drive shaft drives the mounting bracket and multiple cleaning brushes to rotate, thereby cleaning the inside of the storage cylinder, and resetting after cleaning, through a kind of convenient storage agar polysaccharide concentrate cylinder cleaning mechanism, the degree of automation is higher, thus the use efficiency and effect of the spray drying device are enhanced, thereby the production efficiency of natural agar polysaccharide is improved. BRIEF DESCRIPTION OF DRAWINGS

[0038] Fig. 1 is a structure schematic view of a chromatography column adsorption elution device used in the preparation of natural agar polysaccharide of the present application;

[0039] Fig. 2 is a partial enlarged structure schematic view of A of the chromatography column adsorption elution device of the present application;

[0040] Fig. 3 is a partial enlarged structure schematic view of B of the chromatography column adsorption elution device of the present application;

[0041] Fig. 4 is a structure schematic view of a spray drying device of the present application;

[0042] Fig. 5 is a structure schematic view of a top view of the spray drying device of the present application;

[0043] Markings in the drawings: 1, box; 2, holding bottle; 3, placing hole; 4, clamping mechanism; 5, clamping mechanism; 6, adjusting device; 7, driving device; 8, sealing device; 9, mounting seat; 10, binding seat; 11, working cavity; 401, sliding block; 402, knob; 403, clamping block; 404, rubber pad; 405, sliding groove; 406, rotating hole; 501, tight block; 502, buckle; 503, baffle; 504, spring; 505, tight hole; 506, groove; 601, sealing ring; 602, end cover; 603, connecting pipe; 604, infusion tank; 605, filter cover; 606, through hole; 607, water outlet; 701, motor; 702, driving wheel; 703, driven wheel; 704, auxiliary wheel; 705, valve shaft; 706, penetration hole; 707, mounting groove; 708, shaft hole; 801, connecting buckle; 802, screw; 803, screw hole;

[0044] 91, spray drying device body; 92, storage cylinder; 93, working cavity; 94, cleaning cover plate; 95, drive shaft; 96, mounting frame; 97, cleaning brush; 98, servo motor; 99, controller; 910, electric telescopic rod; 911, lifting plate; 912, limiting rod; 913, blocking plate; 914, motor shock pad; 915, motor protection cover; 916, hand-held handle; 917, anti-skid handle cover. DETAILED DESCRIPTION Example 1

[0045] Take 50g silver fungus, add 3L pure water, add NaOH to adjust pH to 12.5, heat the material liquid to 90℃±2℃, keep warm and stir for 3 hours, cool to below 40℃, adjust pH to 7.5 with hydrochloric acid, centrifuge to obtain extract and precipitate; add 30 times water to the precipitate, adjust pH to 12.5, 90℃±2℃, keep warm and stir for 1 hour, cool to below 40℃, adjust pH to 7.5 with hydrochloric acid, centrifuge to obtain extract and precipitate; combine the two times of silver fungus extract and perform desalting treatment, select 30KDa membrane filtration system, continuously add water to the system, monitor the conductivity of the concentrated liquid, stop adding water when the conductivity is ≤3ms / cm; dilute the desalted silver fungus extract with water to Brix 0.4, decolorize the diluted extract with cation resin, flow rate 200mL / h, collect the cation resin effluent; concentrate the decolorized silver fungus extract with membrane, select 300KDa membrane filtration system, stop concentrating when the concentration of the concentrated liquid reaches Brix 2%±0.1%; spray dry the concentrated silver fungus extract, inlet air temperature 180℃, outlet air temperature 90-100℃, collect silver fungus polysaccharide powder.

[0046] A specific chromatography column adsorption elution device is used for decolorization, such as Figs. 1-3The chromatography column adsorption elution device of the present application is shown, which comprises a box body 1 and a containing bottle 2. The box body 1 is provided with a placing hole 3. A plurality of containing bottles 2 are respectively connected with the box body 1 through the corresponding placing holes 3. The device further comprises clamping mechanisms 4, clamping mechanisms 5, adjusting devices 6, driving devices 7 and sealing devices 8. A plurality of mounting seats 9 are provided on the box body 1. A plurality of clamping mechanisms 4 are respectively connected with the box body 1 through the corresponding mounting seats 9. A wrench seat 10 is provided on the box body 1. The clamping mechanisms 5 are connected with the box body 1 through the wrench seat 10. The output end of the containing bottle 2 is connected with the connecting end of the adjusting device 6. The adjusting device 6 is provided with a working cavity 11. The driving devices 7 are uniformly arranged in the working cavity 11. The connecting end of the sealing device 8 is connected with the output end of the adjusting device 6. During column chromatography, the eluent and the adsorbent are extracted by the device. The containing bottles in the box body are fixed by the sliding clamping mechanism. During this process, the containing bottles are stabilized by rotating the clamping mechanism. The driving device is started to switch the closing of the containing bottles of the eluent and the adsorbent, so that they are discharged through the adjusting device. The sealing device is connected with the equipment to improve the convenience of the equipment, thereby improving the working efficiency of the equipment.

[0047] The clamping mechanism of the chromatography column adsorption elution device of the present application further comprises a sliding block 401, a knob 402, a clamping block 403 and a rubber pad 404. A plurality of clamping blocks 403 are respectively connected with the box body 1 through the corresponding mounting seats 9. A plurality of sliding grooves 405 are provided on the box body 1. A plurality of sliding blocks 401 are respectively connected with the box body 1 through the corresponding sliding grooves 405. A plurality of rotating holes 406 are provided on the sliding blocks 401. A plurality of knobs 402 are respectively connected with the corresponding sliding blocks 401 through the corresponding rotating holes 406. A plurality of rubber pads 404 are uniformly arranged on the corresponding clamping blocks 403. The output end of the sliding block 401 is hingedly connected with the connecting end of the corresponding clamping block 403. During clamping of the containing bottles, the containing bottles are placed into the box body through the placing hole. The clamping blocks connected with the sliding blocks are rotated on the mounting seat. A plurality of containing bottles are clamped and fixed by rotating the knobs. The rubber pads protect the containing bottles to improve the clamping convenience of the equipment, thereby improving the working efficiency of the equipment.

[0048] The chromatography column adsorption elution device of the application, the clamping mechanism further comprises a tight block 501, a buckle 502, a baffle 503 and a spring 504, a plurality of buckles 502 are all connected with the box 1 in rotation through the binding seat 10, a plurality of tight holes 505 are arranged on the binding seat 10, a plurality of tight blocks 501 are all connected with the binding seat 10 in screw thread respectively by penetrating the corresponding tight holes 505, a plurality of recesses 506 are arranged on the box 1, the connecting ends of a plurality of baffles 503 are all connected with the box 1 in sliding respectively by penetrating the corresponding recesses 506, and a plurality of springs 504 are evenly installed on the corresponding baffles 503; in the process of stabilizing the containing bottle, the buckle is rotated to be matched with the outer wall of the containing bottle, and the tight block is rotated to be fixed, in the process, the baffle is slid in the recess, and the spring is supported to improve the stability of the equipment clamping, and therefore the working efficiency of the equipment is improved.

[0049] The chromatography column adsorption elution device of the application, the adjusting device further comprises a sealing ring 601, an end cover 602, a connecting pipe 603, a liquid delivery tank 604 and a filter cover 605, the connecting ends of a plurality of end covers 602 are communicated with the output ends of the corresponding containing bottles 2 respectively, a plurality of sealing rings 601 are evenly installed on the corresponding end covers 602, the connecting ends of a plurality of connecting pipes 603 are communicated with the output ends of the corresponding end covers 602, a plurality of through holes 606 are arranged in the working cavity 11 in penetration, the output ends of a plurality of connecting pipes 603 are all fixedly sleeved with the liquid delivery tank 604 respectively by penetrating the corresponding through holes 606, a plurality of water outlets 607 are arranged in the working cavity 11 in penetration, and the connecting ends of a plurality of filter covers 605 are connected with the connecting ends of the corresponding water outlets 607 respectively; in the process of delivering the liquid, the equipment sucks the liquid in a plurality of containing bottles, the end cover is buckled with the containing bottle, the sealing ring is sealed, the liquid flows into the working cavity through the connecting pipe and is isolated respectively, the filter cover is filtered and absorbed, the convenience of switching of the equipment is improved, and therefore the working efficiency of the equipment is improved.

[0050] The chromatography column adsorption elution device of the application, the driving device further comprises a motor 701, a driving wheel 702, a driven wheel 703, an auxiliary wheel 704 and a valve shaft 705, a plurality of groups of through holes 706 are arranged in the water outlets 607, a plurality of groups of valve shafts 705 are uniformly arranged in the corresponding water outlets 607 and are rotationally connected with the corresponding water outlets 607, the output ends of a plurality of groups of driven wheels 703 are connected through the corresponding through holes 706 and the connecting ends of the corresponding valve shafts 705, a mounting groove 707 is arranged in the infusion tank 604, a plurality of groups of shaft holes 708 are arranged in the mounting groove 707, a plurality of groups of driven wheels 703 are rotationally connected through the corresponding shaft holes 708 and the infusion tank 604, the connecting end of the motor 701 is connected with the top end of the infusion tank 604, the output end of the motor 701 is connected through the corresponding shaft hole 708 and the connecting end of the driving wheel 702, the connecting end of the auxiliary wheel 704 is connected with the bottom end of the mounting groove 707, and the output ends of the plurality of groups of driven wheels 703 are engaged with the output ends of the driving wheel 702 and the driven wheel 703; in the process of switching and absorbing the liquid, the motor is started to drive the driving wheel connected therewith to rotate, a plurality of groups of driven wheels are driven by the driving wheel to rotate in the opposite direction, the valve shafts at different opening positions are rotated by rotating, the water outlet position of the water outlet is switched, the use of the eluent and the inhalant is switched, the convenience of the equipment is improved, and therefore the working efficiency of the equipment is improved, thereby increasing the practicability.

[0051] The chromatography column adsorption elution device of the application, the sealing device further comprises a connecting buckle 801 and a screw rod 802, the connecting ends of a plurality of groups of connecting buckles 801 are respectively communicated with the output ends of the corresponding water outlets 607, a plurality of groups of screw holes 803 are arranged on the connecting buckles 801, and a plurality of groups of screw rods 802 are respectively screwed through the corresponding screw holes 803 and the corresponding connecting buckles 801; in the process of connecting the equipment, after the pipe body of the equipment is sealed and engaged through the connecting buckle, the screw rod is rotated to clamp and fix the pipe body, so as to improve the convenience of clamping the equipment, and therefore the working efficiency of the equipment is improved.

[0052] The application discloses a chromatographic column adsorption and elution device. When working, the device extracts eluent and adsorbent, fixes the containing bottles in the box through the sliding clamping mechanism, stabilizes the containing bottles through the rotating clamping mechanism, switches the closing of the containing bottles of the eluent and the adsorbent through the starting driving device, discharges the eluent and the adsorbent through the adjusting device, communicates with the device through the sealing device, places the containing bottles into the box through the placing hole, rotates the clamping blocks connected with the sliding blocks on the mounting seat, buckles and clamps the containing bottles, fixes the containing bottles through the rotating knob, protects the containing bottles through the rubber pad, makes the containing bottles and the outer wall of the containing bottles fit through the rotating buckle, fixes the containing bottles through the rotating fast block, slides the baffle in the groove, supports the baffle through the spring, sucks the liquid in the containing bottles through the device, buckles the end cover and the containing bottles, seals the end cover through the sealing ring, makes the liquid flow into the working cavities through the connecting pipes, filters and absorbs the liquid through the filter cover, rotates the driving wheels connected with the motor through the starting motor, rotates the driven wheels in the opposite direction through the driving wheels, rotates the valve shafts at different opening positions through the rotating, switches the water outlet position of the water outlet, and rotates the screw rod to clamp and fix the pipe body after the pipe body of the device is sealed and fitted with the connecting buckle.

[0053] During spray drying, a spray drying device for a tremella polysaccharide concentrate is used. Figs. 4 to 5 As shown, the spray drying device body 91 is provided with a storage cylinder 92 at the top middle part, the storage cylinder 92 is provided with a working cavity 93, the top of the device is provided with a lifting mechanism, a driving mechanism and a cleaning mechanism.

[0054] The cleaning mechanism further comprises a cleaning cover plate 94, a driving shaft 95, a mounting frame 96 and a plurality of cleaning brushes 97, the bottom end of the cleaning cover plate 94 is provided with a clamping groove, the top end of the storage cylinder 92 is sealingly clamped with the clamping groove provided at the bottom end of the cleaning cover plate 94, the middle of the top end of the cleaning cover plate 94 is provided with a first through hole, the top end of the driving shaft 95 is tightly sleeved with a bearing sleeve of the first through hole provided at the middle of the top end of the cleaning cover plate 94, the mounting frame 96 is connected with the driving shaft 95, the outer end of the mounting frame 96 is provided with a plurality of cleaning brushes 97, the outer ends of the plurality of cleaning brushes 97 are tightly attached to the side wall of the working cavity 93, the top end of the driving shaft 95 is provided with a driving mechanism, the left and right ends of the cleaning cover plate 94 are provided with lifting mechanisms, and the front and rear ends of the cleaning cover plate 94 are provided with limiting mechanisms; through the use of the spray drying device body, the storage cylinder, the working cavity, the cleaning cover plate, the driving shaft, the mounting frame, the cleaning brush, the servo motor, the controller, the two groups of electric telescopic rods, the lifting plate, the two groups of limiting rods and the two groups of blocking plates, when it is necessary to clean the storage cylinder, the worker first opens the lid of the storage cylinder, and then controls the two groups of electric telescopic rods to slide downward along the direction of the two groups of limiting rods, so that the cleaning cover plate is sleeved with the storage cylinder, and then the servo motor is started, the servo motor drives the driving shaft to rotate forward and reversely, the driving shaft drives the mounting frame and the plurality of cleaning brushes to rotate, so that the inside of the storage cylinder is cleaned, and the cleaning is reset after completion. Through the mechanism for conveniently cleaning the cylinder for storing tremella polysaccharide concentrate, the use efficiency and effect of the spray drying device are enhanced.

[0055] As a preferred embodiment of the above, the driving mechanism further comprises a servo motor 98 and a controller 99, the bottom end of the servo motor 98 is connected with the middle of the top end of the cleaning cover plate 94, the output end of the servo motor 98 is connected with the top end of the driving shaft 95, the front end of the spray drying device body 91 is provided with the controller 99, the controller 99 is electrically connected with the servo motor 98, and the outer end of the servo motor 98 is provided with a protection mechanism; through the use of the driving mechanism, the cleaning mechanism is conveniently driven, thereby enhancing the practicality.

[0056] As a preferred embodiment of the above, the lifting mechanism further comprises two groups of electric telescopic rods 910 and a lifting plate 911, the two groups of electric telescopic rods 910 are electrically connected with the controller 99, the outer end of the cleaning cover plate 94 is provided with the lifting plate 911, the bottom ends of the two groups of electric telescopic rods 910 are respectively connected with the left and right ends of the top end of the spray drying device body 91, and the output ends of the two groups of electric telescopic rods 910 are respectively connected with the left and right ends of the bottom end of the lifting plate 911; through the use of the lifting mechanism, the height of the cleaning cover plate is conveniently controlled, thereby enhancing the practicality.

[0057] As the preferred of the above embodiment, the limiting mechanism further comprises two sets of limiting rods 912 and two sets of blocking plates 913, two sets of limiting rods 912 are arranged at the front and rear ends of the spray drying device body 91, the front and rear ends of the lifting plate 911 are provided with second through holes, the two sets of limiting rods 912 are respectively sleeved with the second through holes arranged at the front and rear ends of the lifting plate 911, and the top ends of the two sets of limiting rods 912 are provided with two sets of blocking plates 913; through the use of the limiting mechanism, the cleaning cover plate can slide up and down along the direction of the limiting rod, thereby enhancing the practicability.

[0058] As the preferred of the above embodiment, the protection mechanism further comprises a motor damping pad 914, the bottom end of the servo motor 98 is provided with the motor damping pad 914, and the bottom end of the motor damping pad 914 is connected with the middle part of the top end of the cleaning cover plate 94; the vibration of the servo motor is reduced through the motor damping pad, thereby prolonging the service life and enhancing the practicability.

[0059] As the preferred of the above embodiment, the protection mechanism further comprises a motor protection cover 915, the outer end of the servo motor 98 is provided with the motor protection cover 915, and the bottom end of the motor protection cover 915 is connected with the middle part of the top end of the cleaning cover plate 94; the motor protection cover prevents the damage of sundries to the servo motor, thereby enhancing the practicability.

[0060] As the preferred of the above embodiment, a hand-held handle 916 is further arranged, and the bottom end of the hand-held handle 916 is connected with the middle part of the top end of the motor protection cover 915; the hand-held handle can be used to conveniently and quickly move the protection cover, thereby enhancing the practicability.

[0061] As the preferred of the above embodiment, an anti-skid handle sleeve 917 is further arranged, and the anti-skid handle sleeve 917 is tightly sleeved with the middle part of the top end of the hand-held handle 916; the anti-skid handle sleeve can increase the friction force between the handle and the palm, thereby preventing slipping and enhancing the practicability.

[0062] The working principle of the spray drying device for tremella polysaccharide concentrate liquid is that, when the storage cylinder needs to be cleaned, the worker first opens the lid of the storage cylinder, then controls the two sets of electric telescopic rods to slide downward along the direction of the two sets of limiting rods, so that the cleaning cover plate is sleeved with the storage cylinder, then the servo motor is started, the servo motor drives the driving shaft to reciprocate in the forward direction and the reverse direction, the driving shaft drives the mounting frame and the plurality of cleaning brushes to rotate, so that the inside of the storage cylinder is cleaned, and the cleaning is reset after completion, thereby saving manpower and material resources and having high automation degree.

[0063] The total sugar content of the tremella polysaccharide prepared by the method is 93.75%, the ash content is 0.3%, the polysaccharide yield is 53.45%, and the white powder is obtained. Example 2

[0064] Take 50g tremella, add 3L purified water, adjust pH to 12.5 with NaOH, heat the material liquid to 90℃±2℃, keep stirring for 3 hours, cool down to below 40℃, adjust pH to 7.5 with hydrochloric acid, centrifugal to get the extract and precipitate; add 30 times water to the precipitate, adjust pH to 12.5, 90℃±2℃, keep stirring for 1 hour, cool down to below 40℃, adjust pH to 7.5 with hydrochloric acid, centrifugal to get the extract and precipitate; combine the two times of tremella extract, and desalt treatment, select 30KDa membrane filtration system, constantly add water to the system, monitor the conductivity of the concentrated liquid, stop adding water when the conductivity is less than or equal to 3ms / cm; dilute the desalted tremella extract to Brix 0.4 with water, decolorize the diluted extract with anion resin at a flow rate of 200mL / h, collect the anion resin effluent; concentrate the decolorized tremella extract with a membrane, select 300KDa membrane filtration system, stop concentrating when the concentration of the concentrated liquid reaches Brix 2%±0.1%; spray dry the concentrated tremella extract, the inlet air temperature is 180℃, the outlet air temperature is 90-100℃, and collect the tremella polysaccharide powder.

[0065] The total sugar content of the tremella polysaccharide prepared by the method is 92.23%, the ash content is 0.4%, the polysaccharide yield is 51.76%, and the white powder is obtained. Comparative Example 1

[0066] Take 50g tremella, add 3L purified water, adjust pH to 12.5 with NaOH, heat the material liquid to 90℃±2℃, keep stirring for 3 hours, centrifugal to get the extract and precipitate; add 30 times water to the precipitate, adjust pH to 12.5, 90℃±2℃, keep stirring for 1 hour, centrifugal to get the extract and precipitate; combine the two times of tremella extract, adjust pH to 7.5 with hydrochloric acid, concentrate with a membrane, select 30KDa membrane filtration system, constantly add water to the system, monitor the conductivity of the concentrated liquid, stop adding water when the conductivity is less than or equal to 3ms / cm, stop concentrating when the concentration of the concentrated liquid reaches Brix 2%±0.1%; spray dry the concentrated tremella extract, the inlet air temperature is 180℃, the outlet air temperature is 90-100℃, and collect the tremella polysaccharide powder.

[0067] The total sugar content of the tremella polysaccharide prepared by the method is 76.76%, the ash content is 0.4%, the polysaccharide yield is 43.55%, and the gray powder is obtained. Comparative Example 2

[0068] Take 50g silver fungus, add 3L pure water, add NaOH to adjust pH to 12.5, the liquid is heated to 90℃±2℃, keep warm stirring for 3 hours, cooling to below 40℃, hydrochloric acid to adjust pH to 7.5, centrifugal get extract and precipitate; to the precipitate added 30 times water, adjust pH to 12.5, 90℃±2℃, keep warm stirring for 1 hour, cooling to below 40℃, hydrochloric acid to adjust pH to 7.5, centrifugal get extract and precipitate; the two times of extraction of silver fungus extract combined, add water to dilute to Brix 0.4; dilution of the extract on anion resin decolorization and desalination, flow rate 200mL / h, collect anion resin effluent; anion resin effluent on cation resin decolorization again, flow rate 200mL / h, collect cation resin effluent; the decolorized silver fungus extract is concentrated under reduced pressure, the concentration of the concentrated liquid reaches Brix 2%±0.1% to stop concentration; the concentrated silver fungus extract is spray dried, the inlet air temperature is 180℃, the outlet air temperature is 90-100℃, and the silver fungus polysaccharide powder is collected by spraying.

[0069] The silver fungus polysaccharide prepared by this method has a total sugar content of 79.64%, an ash content of 5.6%, a polysaccharide yield of 24.67%, and a light yellow powder. Comparative Example 3

[0070] Take 50g silver fungus, add 3L pure water, add NaOH to adjust pH to 12.5, the liquid is heated to 90℃±2℃, keep warm stirring for 3 hours, centrifugal get extract and precipitate; to the precipitate added 30 times water, adjust pH to 12.5, 90℃±2℃, keep warm stirring for 1 hour, centrifugal get extract and precipitate; the two times of extraction of silver fungus extract combined, add water to dilute to Brix 0.4; dilution of the extract on anion resin decolorization and desalination, flow rate 200mL / h, collect anion resin effluent; anion resin effluent on cation resin decolorization again, flow rate 200mL / h, collect cation resin effluent; the decolorized silver fungus extract is concentrated under reduced pressure, the concentration of the concentrated liquid reaches Brix 2%±0.1% to stop concentration; the concentrated silver fungus extract is spray dried, the inlet air temperature is 180℃, the outlet air temperature is 90-100℃, and the silver fungus polysaccharide powder is collected by spraying.

[0071] The silver fungus polysaccharide prepared by this method has a total sugar content of 79.64%, an ash content of 5.6%, a polysaccharide yield of 24.67%, and a light yellow powder.

[0072]

[0073] The embodiments are only used for explaining the present application, and are not used for limiting the present application, and the person skilled in the art can make the modification of the embodiments without the creative contribution according to the need after reading the description, and as long as the modification is within the scope of the claims of the present application, it is protected by the patent law.

Claims

1. A method for preparing natural tremella polysaccharide, characterized in that, It comprises the following steps: S1. One extraction: after the silver fungus is broken, a certain proportion of pure water is added, the solid-liquid ratio is 1:30-80, the silver fungus W: water V, a certain amount of NaOH is added to adjust the pH to 11-13, heating and keeping warm, the extraction temperature is controlled at 60-100℃, the extraction time is 1-5 hours; S2. Solid-liquid separation: after the extraction, the pH is adjusted to 6-8 by hydrochloric acid, and the separation device is entered to obtain the extraction liquid and the precipitate, and the solid-liquid separation device is one of plate and frame filter, horizontal screw centrifuge and disc centrifuge; S3. Second extraction: the precipitate of step S2 is added to a certain proportion of water and NaOH, and extracted again under appropriate conditions, and steps S1 and S2 are repeated, and the extraction liquids obtained twice are combined; S4. Desalination: a high molecular membrane filtration system with a model of 1-100KDa is selected for desalination, and the conductivity of the concentrated liquid is monitored to be below 100ms / cm, and more water is added if the conductivity does not reach this value; S5. Decolorization: a certain amount of water is added to the desalted extraction liquid to make the Brix value of the extraction liquid in the range of 0.1-1%, and a suitable resin is selected for decolorization, and the type of decolorization resin is any one of anion resin and cation resin, and the column loading mode is static adsorption or dynamic adsorption; S6. Membrane concentration: the feed liquid passes through a high molecular membrane separation system with a pore size of 30-300KDa to selectively intercept target substances with a certain molecular weight range, and is concentrated to a Brix of 2-5%, and the permeate and the retentate are collected respectively; S7. Drying: the retentate enters the spray drying tower for drying, and the dry powder is collected, the inlet air temperature is 180-200℃, and the outlet air temperature is 90-100℃. The natural tremella polysaccharide is a white powder with a purity of not less than 90% and an ash content of not higher than 0.5%.

2. The method for preparing natural tremella polysaccharide according to claim 1, characterized in that: The step S5 decolorization adopts a chromatography column adsorption elution device, which comprises a box body (1) and a containing bottle (2). The box body (1) is provided with a plurality of placing holes (3). A plurality of containing bottles (2) are respectively arranged through the corresponding placing holes (3) and are slidably connected with the box body (1). The device is characterized in that it further comprises clamping mechanisms (4), clamping mechanisms (5), adjusting devices (6), driving devices (7) and sealing devices (8). A plurality of mounting seats (9) are arranged on the box body (1). A plurality of clamping mechanisms (4) are respectively arranged through the corresponding mounting seats (9) and are rotatably connected with the box body (1). A wrench (10) is arranged on the box body (1). The clamping mechanism (5) is rotatably connected through the wrench (10) and the box body (1). The output end of the containing bottle (2) is connected with the connecting end of the adjusting device (6). The adjusting device (6) is provided with a working cavity (11) in the inside. The driving devices (7) are uniformly arranged in the working cavity (11). The connecting end of the sealing device (8) is connected with the output end of the adjusting device (6). The clamping mechanism further comprises a clamping block (501), a buckle (502), a baffle (503) and a spring (504), a plurality of buckles (502) are rotatably connected to the box body (1) through the winding base (10), a plurality of clamping holes (505) are arranged on the winding base (10), a plurality of clamping blocks (501) are threadedly connected to the winding base (10) through the corresponding clamping holes (505), a plurality of recesses (506) are arranged on the box body (1), the connecting ends of a plurality of baffles (503) are slidably connected to the box body (1) through the corresponding recesses (506), and a plurality of springs (504) are uniformly arranged on the corresponding baffles (503).

3. The method for preparing natural tremella polysaccharide according to claim 1, characterized in that: The step S7 sprays the spray drying device for the silver ear polysaccharide concentrated solution, including spray drying device body (91), the top of spray drying device body (92) is provided with storage cylinder, the inside of storage cylinder (92) is provided with working cavity (93), the top of cleaning machine is provided with lifting mechanism, drive mechanism and cleaning mechanism; The cleaning mechanism further comprises a cleaning cover plate (94), a drive shaft (95), a mounting frame (96) and a cleaning brush (97), the bottom end of the cleaning cover plate (94) is provided with a clamping groove, the top end of the storage cylinder (92) is sealingly clamped with the clamping groove provided at the bottom end of the cleaning cover plate (94), the top end of the cleaning cover plate (94) is provided with a first through hole, the top end of the drive shaft (95) is fastened with a bearing sleeve through the first through hole provided at the top end of the cleaning cover plate (94), the mounting frame (96) is connected with the drive shaft (95), a plurality of cleaning brushes (97) are provided at the outer end of the mounting frame (96), the outer end of the plurality of cleaning brushes (97) is tightly attached to the side wall of the working cavity (93), the top end of the drive shaft (95) is provided with a drive mechanism, the left and right ends of the cleaning cover plate (94) are provided with a lifting mechanism, and the front and rear ends of the cleaning cover plate (94) are provided with a limiting mechanism; The drive mechanism further comprises a servo motor (98) and a controller (99), the bottom end of the servo motor (98) is connected with the top end of the cleaning cover plate (94), the output end of the servo motor (98) is connected with the top end of the drive shaft (95), the front end of the spray drying device body (91) is provided with a controller (99), the controller (99) is electrically connected with the servo motor (98), and the outer end of the servo motor (98) is provided with a protection mechanism; The lifting mechanism further comprises two groups of electric telescopic rods (910) and a lifting plate (911), the two groups of electric telescopic rods (910) are electrically connected with the controller (99), the outer end of the cleaning cover plate (94) is provided with a lifting plate (911), the bottom ends of the two groups of electric telescopic rods (910) are respectively connected with the left and right ends of the top end of the spray drying device body (91), and the output ends of the two groups of electric telescopic rods (910) are respectively connected with the left and right ends of the bottom end of the lifting plate (911).

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