A multi-stage sinopicroside purification device containing an ion liquid modified chromatographic medium

Abstract

The application belongs to the technical field of medicine multistage purification, and discloses a tetrandrine multistage purification device containing ion liquid modified chromatography medium, which comprises chromatography columns, the chromatography columns are provided with three, upper and lower sealing plates are respectively fixedly connected to the top and bottom of the three chromatography columns, the cooperation of the structures of the horizontal plate, ring block, movable ring plate, vertical rod, upper rotary disc and lower rotary disc in the rotary switching mechanism is provided, double holes are formed in the upper rotary disc, three circular holes are formed in the lower rotary disc, when the horizontal plate rotates, the upper rotary disc and the lower rotary disc are synchronously rotated by the vertical rod, the double holes are aligned with the inlet of the next chromatography column, and the three circular holes are aligned with the outlet of the corresponding chromatography column, so that the seamless station switching between the multiple chromatography columns is facilitated, the operator only needs to rotate the horizontal plate to complete the synchronous switching of the inlet and outlet of the chromatography column, the chromatography column does not need to be stopped and balanced, the purification process is continuous and uninterrupted, and the production efficiency is greatly improved.

Description

Technical Field

[0001] This invention belongs to the field of tetrandrine preparation technology, specifically a multi-stage purification device for tetrandrine containing ionic liquid modified chromatography medium. Background Technology

[0002] Tetrandrine A is a dibenzylisoquinoline alkaloid extracted from the tuberous root of *Stephania tetrandra*, a plant in the Menispermaceae family. In the industrial production of tetrandrine A, a multi-stage purification device is used. Through multi-stage separation and purification methods, it mainly involves five steps: crude extract preparation, macroporous adsorption resin enrichment, silica gel column chromatography separation, ceramic membrane ultrafiltration decolorization, and ethanol recrystallization purification. This effectively separates tetrandrine A from tetrandrine B and other impurities, ultimately obtaining a high-purity tetrandrine product. In the purification device, the ionic liquid-modified chromatography medium has better selectivity and separation efficiency, which can further improve the separation degree of tetrandrine A from tetrandrine B.

[0003] A chromatographic separation device for tetrandrine, disclosed in prior art document CN219272213U, belongs to the field of chromatographic separation. This device includes a main support with a base fixedly connected to its bottom. A rotating shaft is rotatably connected to the main support, and a secondary support is fixedly connected to the end of the rotating shaft away from the main support. Fixed sleeves are fixedly connected to both ends of the secondary support, and separation tanks are fitted inside each of the two fixed sleeves. A separation tube connects the two separation tanks, and a pull ring is fixedly connected between the two fixed sleeves. The advantages of this device compared to existing technologies are: during the separation process, the two separation tanks are relatively sealed; separation is performed at the separation tube by controlling the separation valve; before separation, the liquid level can be adjusted by a one-way airbag on the separation tank; after separation, the liquid can be discharged from both separation tanks by rotating the pull ring to open the valve; and the device is easy to operate. Although the aforementioned patent achieves the chromatography and separation operation of tetrandrine by setting up a main support, a rotating shaft, a secondary support, and two separation tanks, it cannot effectively solve the problem of the inability to switch chromatography columns online and the discontinuous production during multi-stage purification. The separation tanks of this device are only connected by separation tubes. During the separation process, the two separation tanks are relatively sealed. When one separation tank completes the separation, it is necessary to stop the machine to unload the material and refill the separation medium, which makes it impossible to achieve continuous production. Summary of the Invention

[0004] The purpose of this invention is to provide a multi-stage purification device for tetrandrine using ion-modified chromatographic media with delayed switching and high efficiency, in order to solve the problems mentioned in the background art.

[0005] To achieve the above objectives, the present invention provides the following technical solution: a multi-stage purification device for tetrandrine containing ionic liquid-modified chromatography medium, comprising chromatography columns, wherein three chromatography columns are provided, and upper sealing plates and lower sealing plates are fixedly connected to the top and bottom of the three chromatography columns, respectively. Three regeneration tubes and three pairs of double feed tubes are fixedly connected to the top of the upper sealing plate, and each regeneration tube and each pair of double feed tubes corresponds to the lower chromatography column. Several discharge tubes are adapted and fixedly connected to the bottom of the lower sealing plate. The device also includes: A rotary switching mechanism, which is located on the upper sealing plate; A delay switching mechanism, which is connected to a rotary switching mechanism; The rotary switching mechanism includes an upper rotating disk rotatably connected to the lower side of the upper sealing plate, and a lower rotating disk rotatably connected to the middle of the lower sealing plate.

[0006] Preferably, the rotary switching mechanism further includes three sets of horizontal plates fixed to the upper rotating disk and the side wall of the three circular holes. Vertical rods are fixed to the inner sides of the upper and lower horizontal plates, and a ring block is fixed to the middle of the three vertical rods.

[0007] Preferably, each of the upper horizontal plates has a slot in the middle, and each horizontal plate is connected to an outer locking post through the slot.

[0008] Preferably, a movable ring plate is fixedly connected to the top of the multiple outer pins, and the inner side of the movable ring plate is slidably sleeved on the outer wall of the upper sealing plate.

[0009] Preferably, the outer side of the upper rotating disk is provided with an outer mesh hole, and the inner side of the upper rotating disk is provided with two holes side by side. Three inner locking posts are fixedly connected to the top of the upper rotating disk at equal intervals around the circumference.

[0010] Preferably, the lower rotating disk has three circular holes at the position corresponding to the double holes, and an indicator block is fixedly connected to the horizontal plate near the double holes.

[0011] Preferably, the delay switching mechanism includes a distribution plate rotatably connected to the inner cavity of the upper sealing plate, the inner side of the distribution plate having an inner mesh hole, and the outer side of the inner mesh hole having three liquid inlet holes equidistantly arranged around the circumference.

[0012] Preferably, six N-shaped plates are fixedly connected at equal intervals to the top of the movable ring plate, and the inner sides of the N-shaped plates are slidably connected to the edge of the upper sealing plate.

[0013] Preferably, the ends of the plurality of N-shaped plates are abutted against a retaining sleeve, and a sliding plate is fixedly attached to the top of each retaining sleeve.

[0014] Preferably, the distribution plate has six equidistant openings around its circumference on its lower side, and the sliding plate is elastically connected to the inner wall of the openings. The inner side of the sleeve is engaged with the inner locking post.

[0015] Compared with the prior art, the beneficial effects of the present invention are as follows: (1) The present invention sets up a rotating switching mechanism with the cooperation of a horizontal plate, a ring block, a movable ring plate, a vertical rod, an upper rotating disk and a lower rotating disk. The upper rotating disk has two holes and the lower rotating disk has three circular holes. When the horizontal plate rotates, the upper rotating disk and the lower rotating disk are driven to rotate synchronously through the vertical rod, so that the two holes are aligned with the inlet of the next chromatography column and the three circular holes are aligned with the outlet of the corresponding chromatography column. This facilitates seamless switching between multiple chromatography columns. The operator only needs to rotate the horizontal plate to complete the synchronous switching of the chromatography column inlet and outlet. There is no need to stop the machine to load columns or balance. The purification process is continuous and uninterrupted, which greatly improves the production efficiency.

[0016] (2) By setting up the N-shaped plate, distribution plate, ferrule and slide plate in the delayed switching mechanism, when the horizontal plate rotates, the ring block drives the upper and lower rotating plates to rotate synchronously through the vertical rod. The inner ferrule rotates synchronously with the upper rotating plate. When the rotation is close to 60 degrees, it abuts against the surface of the adjacent ferrule, pushing the distribution plate to rotate synchronously until the horizontal plate abuts against the surface of the outer ferrule. The ring plate is lifted and moved to make the outer ferrule and ferrule move upward synchronously. The upper and lower rotating plates are rotated into place, so that the distribution plate rotates 60 degrees later. The liquid inlet hole just reaches the position of the upper chromatography column to connect the regeneration tube, which facilitates the orderly switching between chromatography and regeneration states. The delayed switching ensures that the eluent flow direction is switched before the chromatography column enters the regeneration station, avoiding backflow, crossflow and cross-contamination of eluent at the moment of switching, ensuring the purity of each fraction collected, and making the separation degree of tetrandrine A and tetrandrine B stable.

[0017] (3) By setting up a combination of structures such as a double feed tube, a regeneration tube and a moving ring plate, the feed channel of the double feed tube and the eluent channel of the regeneration tube are independent of each other. When the moving ring plate is lifted, it drives the outer clamping column and the clamping sleeve to move upward synchronously, so that the horizontal plate is disengaged and drives the upper and lower rotating disks to rotate. After the moving ring plate is reset, the outer clamping column and the clamping sleeve respectively clamp the horizontal plate and the inner clamping column. After the switch is completed, the regeneration tube introduces the regeneration liquid into the original chromatography column that has been cut off, thereby facilitating the online automatic regeneration of the chromatography column. The cut-off chromatography column automatically completes the washing, activation and balancing process in the standby station and can be put into use immediately when the next switch is completed. This realizes the regeneration of the chromatography column while working. The separation activity of the ion liquid modified chromatography medium is effectively restored under timely regeneration treatment, the medium replacement frequency is reduced, and the production cost and downtime are significantly reduced. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the overall structure of the present invention; Figure 2 This is a top view of the structure of the present invention; Figure 3This is a schematic diagram of the three-dimensional cross-sectional structure of the present invention; Figure 4 For the present invention Figure 3 A magnified view of the structure at point A in the middle; Figure 5 This is a schematic diagram showing the structural fit between the movable ring plate and the N-shaped plate of the present invention; Figure 6 This is a schematic diagram showing the structural fit between the rotating disk and the horizontal plate in this invention; Figure 7 This is a schematic diagram showing the structural fit between the rotating disk and the inner locking pin of the present invention; Figure 8 This is a schematic diagram illustrating the structural fit of the card sleeve and sliding plate of the present invention.

[0019] In the picture: 100. Chromatography column; 200. Regeneration tube; 300. Dual feed tubes; 400. Upper sealing plate; 500. Lower sealing plate; 600. Rotary switching mechanism; 610. Indicator block; 620. Horizontal plate; 630. Ring block; 640. Moving ring plate; 650. Vertical rod; 660. Upper rotating disk; 670. Lower rotating disk; 680. Inner clamping column; 690. Outer clamping column; 6100. Three circular holes; 6110. Double holes; 6120. Outer mesh; 700. Delay switching mechanism; 710. N-shaped plate; 720. Distribution disk; 730. Inner mesh; 740. Sleeve; 750. Slide plate; 760. Liquid inlet. Detailed Implementation

[0020] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0021] like Figures 1 to 8 As shown, this invention provides a multi-stage purification device for tetrandrine containing an ionic liquid-modified chromatography medium, comprising chromatography columns 100, of which three are arranged. An upper sealing plate 400 and a lower sealing plate 500 are fixedly connected to the top and bottom of each of the three chromatography columns 100, respectively. Three regeneration tubes 200 and three pairs of dual-feed tubes 300 are fixedly connected to the top of the upper sealing plate 400, and each regeneration tube 200 and each pair of dual-feed tubes 300 corresponds to the lower chromatography column 100. Several discharge tubes are adapted and fixedly connected to the bottom of the lower sealing plate 500. The device also includes: Rotary switching mechanism 600, which is located on upper sealing plate 400; The delay switching mechanism 700 is connected to the rotary switching mechanism 600; The rotary switching mechanism 600 includes an upper rotary disk 660 rotatably connected to the lower side of the upper sealing plate 400, and a lower rotary disk 670 rotatably connected to the middle of the lower sealing plate 500.

[0022] The above scheme employs a system in which three chromatography columns 100 are arranged side-by-side and formed by upper sealing plates 400 and lower sealing plates 500 fixed to their top and bottom, respectively. Each column 100 has a regeneration tube 200 for introducing regeneration solution and a pair of dual feed tubes 300 for alternating sample loading and elution. Each column 100 has a discharge tube fixedly connected to the lower sealing plate 500 at its bottom. A rotary switching mechanism 600 is provided on the upper sealing plate 400. The rotary switching mechanism 600 includes an upper rotating disk 660 rotatably connected to the lower side of the upper sealing plate 400 and a lower rotating disk 670 rotatably connected to the middle of the lower sealing plate 500. The upper rotating disk 660 and the lower rotating disk 670 are fixedly connected by the vertical rod 650 and rotate synchronously. The upper rotating disk 660 is provided with a double hole 6110 for switching between different regeneration tubes 200 and dual feed tubes 300, and the lower rotating disk 670 is provided with a triple hole 6100 for switching between different discharge tubes. The delayed switching mechanism 700 is connected to the rotating switching mechanism 600. Its distribution disk 720 is connected to the upper rotating disk 660 through the sleeve 740 and the slide plate 750 to form a delayed linkage with the upper rotating disk 660, so that the rotation of the distribution disk 720 lags behind the upper rotating disk 660 by a predetermined angle, so as to realize the sequential and orderly execution of the working position switching and regeneration position access of the chromatography column 100.

[0023] like Figures 3 to 7 As shown, the rotary switching mechanism 600 also includes three sets of horizontal plates 620 fixed to the side walls of the upper rotating disk 660 and the three circular holes 6100. Vertical rods 650 are fixed to the inner sides of the upper and lower horizontal plates 620, and a ring block 630 is fixedly connected to the middle of the three vertical rods 650. A slot is provided in the middle of the upper horizontal plate 620, and an outer locking post 690 is engaged with each horizontal plate 620 through the slot. A movable ring plate 640 is fixedly connected to the top of the multiple outer locking posts 690, allowing for the movement of... The inner side of the ring plate 640 is slidably sleeved on the outer wall of the upper sealing plate 400; the outer side of the upper rotating disk 660 is provided with an outer mesh hole 6120, and the inner side of the upper rotating disk 660 is provided with double holes 6110 side by side; three inner locking posts 680 are fixedly connected to the top of the upper rotating disk 660 at equal intervals around the circumference; the lower rotating disk 670 is provided with three round holes 6100 corresponding to the position of the double holes 6110; an indicator block 610 is fixedly connected to the horizontal plate 620 in the direction close to the double holes 6110.

[0024] The above scheme employs an indicator block 610 fixed to the horizontal plate 620. The direction the indicator block points to different chromatography columns 100 indicates the current working position of the chromatography column 100, allowing operators to accurately grasp the system's operating status without needing to observe through the sealed housing. When switching positions, the operator first pushes the moving ring plate 640 upwards. At this time, the outer clamping column 690, the N-shaped plate 710, and the clamping sleeve 740 all move upwards along with the moving ring plate 640, disengaging the horizontal plate 620 from its clamping constraint. Then, rotating the horizontal plate 620 drives the ring block 630 to rotate, allowing the moving ring plate 640 to automatically fall back to its original position under gravity. Combined with the transmission action of the vertical rod 650, this drives the upper rotating disk 660 and the lower rotating disk 670 to rotate synchronously. When the upper rotating disk 660 rotates, its two orifices 6110 align with the inlet of the next chromatography column 100, switching the eluent input channel. When the lower rotating disk 670 rotates synchronously, its three circular orifices 6100 align with the outlet of the corresponding chromatography column 100, switching the effluent collection channel. Through this mechanical linkage, seamless switching between multiple chromatography columns 100 is achieved without stopping the machine for column loading and equilibration, ensuring continuous and uninterrupted purification and significantly improving production efficiency.

[0025] like Figures 3 to 5 , Figure 8 As shown, the delay switching mechanism 700 includes a distribution plate 720 rotatably connected to the inner cavity of the upper sealing plate 400. The inner side of the distribution plate 720 is provided with an inner mesh hole 730, and the outer side of the inner mesh hole 730 is provided with three liquid inlet holes 760 at equal intervals around the circumference. Six N-shaped plates 710 are fixedly connected at equal intervals to the top of the movable ring plate 640. The inner sides of the N-shaped plates 710 are slidably connected to the edge of the upper sealing plate 400. The ends of the multiple N-shaped plates 710 abut against the sleeves 740, and the top of the sleeves 740 is fixedly connected with the slide plates 750. Six opening slots are provided at equal intervals around the circumference on the lower side of the distribution plate 720. The slide plates 750 are elastically connected to the inner wall of the opening slots. The inner side of the sleeves 740 is engaged with the inner locking post 680.

[0026] Using the above scheme: when the horizontal plate 620 rotates, the ring block 630 drives the upper rotating disk 660 and the lower rotating disk 670 to rotate synchronously through the three vertical rods 650. At this time, the double hole 6110 and the three circular holes 6100 move synchronously to the position of the next chromatography column 100. During this process, since the moving ring plate 640 has been reset, the ferrule 740 is in the state of extending out of the bottom of the distribution plate 720, and the inner ferrule 680 rotates synchronously with the upper rotating plate 660. When the inner ferrule 680 rotates to nearly 60 degrees, it can abut against the surface of the adjacent ferrule 740, pushing the distribution plate 720 to rotate synchronously. When the rotation is close to 120 degrees, the horizontal plate 620 with the indicator block 610 fixed to it abuts against the surface of the outer ferrule 690. The operator lifts the moving ring plate 640 again, so that the outer ferrule 690 and the ferrule 740 move upward synchronously, and continues to rotate the upper rotating plate 660 and the lower rotating plate 670 into place until the moving ring plate 640 is lowered, so that the outer ferrule 690 and the ferrule 740 respectively engage with the horizontal plate 620 and the inner ferrule 680, completing the entire switching process. The upper rotating disk 660 rotates 120 degrees, and the distribution disk 720 rotates 60 degrees. At this point, the inlet port 760 is positioned exactly at the previous chromatography column 100, connecting the regeneration tube 200 to that column 100. The 60-degree delay in the rotation of the distribution disk 720 ensures that the switching of the working position and the connection of the regeneration position are performed sequentially. The new column is connected to the eluent first to start working, and the old column is connected to the regeneration solution to start regeneration. This avoids cross-flow and mixing of the eluent and regeneration solution due to simultaneous connection of pipelines during the switching process, ensuring the purity of each fraction collected. The dual feed tubes 300 continuously deliver eluent to the chromatography column 100 in the working position to continue the new purification process. The three chromatography columns 100 are in working, regeneration, and standby states respectively, which are rotated periodically by the rotating switching mechanism 600 without interference. Operators only need to rotate the horizontal plate 620 to simultaneously perform three actions: switching the inlet and outlet of the chromatography column 100, and distributing the regenerated solution flow direction. The operation is extremely simple and highly reliable. Simultaneously, with timely regeneration, the separation activity of the ion-liquid modified chromatography medium is effectively restored, reducing the frequency of medium replacement and significantly lowering production costs and downtime. This achieves continuous, automated, and intrinsically safe operation of the multi-stage purification process of tetrandrine.

[0027] Working principle and usage process of this invention: First, a chromatography system is constructed using three chromatography columns 100. The concentrated extract of tetrandrine crude extract, obtained by enrichment with macroporous adsorption resin, is then fed into column 100 through a dual feed tube 300, which consists of a sample loading tube and an elution tube. The feed channel of the dual feed tube 300 and the eluent channel of the regeneration tube 200 are independent, allowing for alternating sample loading and elution without disassembling the tubing. During sample loading, the concentrated extract enters column 100 through the dual feed tube 300. The ionic liquid-modified chromatography medium selectively adsorbs tetrandrine, while highly polar impurities are discharged with the effluent. After sample loading, the regeneration tube 200 is switched to introduce eluent with a composition of dichloromethane:ethyl acetate:triethylamine = 90:20:0.1, to elute and separate the target analyte adsorbed on the chromatography medium. During this process, the upper sealing plate 400 and the lower sealing plate 500 seal the upper and lower ends of the chromatography column 100 respectively to ensure that the elution process is carried out in a closed environment and to prevent the evaporation and leakage of organic solvents.

[0028] Secondly, when elution reaches the main peak of tetrandrine, the station of the chromatography column 100 is switched via a rotary switching mechanism 600. The rotary switching mechanism 600 includes an indicator block 610, a horizontal plate 620, an annular block 630, a movable annular plate 640, a vertical rod 650, an upper rotating disk 660, and a lower rotating disk 670. The upper rotating disk 660 and the lower rotating disk 670 are respectively provided with three circular holes 6100 and two holes 6110 for docking with the inlet and outlet of different chromatography columns 100. The operator determines the current working status by observing the position of the indicator block 610. First, the moving ring plate 640 is pushed upwards. At this time, the outer clamping column 690, N-shaped plate 710, and clamping sleeve 740 all move upwards with the moving ring plate 640, disengaging the horizontal plate 620. Then, the horizontal plate 620 is rotated, causing the ring block 630 to rotate, allowing the moving ring plate 640 to automatically fall. Together with the vertical rod 650, this drives the upper rotating disk 660 and the lower rotating disk 670 to rotate synchronously. When the upper rotating disk 660 rotates, its two holes 6110 align with the inlet of the next chromatography column 100, switching the eluent input channel. When the lower rotating disk 670 rotates synchronously, its three circular holes 6100 align with the outlet of the corresponding chromatography column 100, switching the effluent collection channel. This achieves seamless switching between multiple chromatography columns 100 without requiring shutdown for column loading and equilibration, ensuring continuous and uninterrupted purification and significantly improving production efficiency.

[0029] Furthermore, while the rotary switching mechanism 600 operates, the delayed switching mechanism 700 sequentially distributes the eluent flow direction. The delayed switching mechanism 700 includes an N-shaped plate 710, a distribution disk 720, a retainer 740, and a slide plate 750. The distribution disk 720 has an inner mesh hole 730 and a liquid inlet hole 760. The N-shaped plate 710 is linked to the horizontal plate 620 of the rotary switching mechanism 600. When the horizontal plate 620 rotates, the ring block 630 drives the upper rotating disk 660 and the lower rotating disk 670 to rotate synchronously through three vertical rods 650. At this time, the double hole 6110 and the three circular holes 6100 move to the position of the next chromatography column 100. During this process, since the moving ring plate 640 has been reset, the ferrule 740 is positioned at the bottom of the distribution plate 720. At this time, the inner ferrule 680 also rotates synchronously with the upper rotating plate 660. Therefore, when the inner ferrule 680 rotates to a position close to 60 degrees, it can abut against the surface of the adjacent ferrule 740, pushing the distribution plate 720 to rotate synchronously. When it is close to 120 degrees, the horizontal plate 620 of the fixed observation indicator block 610 abuts against the surface of the outer ferrule 690. The operator then lifts the moving ring plate 640 again, causing the outer ferrule 690 and the ferrule 740 to move upward synchronously. The upper rotating plate 660 and the lower rotating plate 670 are rotated into place until the moving ring plate 640 is lowered, so that the outer ferrule 690 and the ferrule 740 respectively engage with the horizontal plate 620 and the inner ferrule 680, completing the switching. That is, the upper rotating disk 660 rotates 120 degrees, and the distribution disk 720 rotates 60 degrees. At this time, the liquid inlet 760 is exactly at the position of the previous chromatography column 100, connecting the regeneration tube 200. The 60-degree delay in the rotation of the distribution disk 720 ensures that the chromatography state and the regeneration state proceed in sequence.

[0030] Finally, the cut-out original chromatography column 100 enters the regeneration station. The regeneration tube 200 is circulated with regeneration solution through the external mesh 6120, undergoing sequential washing with 50% ethanol, activation with 90% ethanol, and equilibration with 50% ethanol. After regeneration, it is ready for standby. During this process, the dual feed tubes 300 continuously supply eluent to the chromatography column 100 in the working station, continuing the new purification process. The operator only needs to rotate the horizontal plate 620 to simultaneously perform the three actions of switching the inlet and outlet of the chromatography column 100 and distributing the regeneration solution flow direction, making the operation extremely simple and highly reliable. Simultaneously, with timely regeneration, the separation activity of the ion liquid-modified chromatography medium is effectively restored, reducing the medium replacement frequency by more than 50%, significantly reducing production costs and downtime. This completes a full cycle of elution, switching, delayed distribution, and regeneration, achieving continuous, automated, and intrinsically safe operation of the tetrandrine multi-stage purification process.

[0031] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.

[0032] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A multi-stage purification device for tetrandrine containing ionic liquid-modified chromatography medium, comprising chromatography columns (100), wherein three chromatography columns (100) are provided, and an upper sealing plate (400) and a lower sealing plate (500) are fixedly connected to the top and bottom of the three chromatography columns (100), respectively. The top of the upper sealing plate (400) is fixedly connected to three regeneration tubes (200) and three pairs of double feed tubes (300), and each regeneration tube (200) and each pair of double feed tubes (300) corresponds to the lower chromatography column (100). The bottom of the lower sealing plate (500) is adapted to be fixedly connected to several discharge tubes, characterized in that... Also includes: A rotary switching mechanism (600) is located on the upper sealing plate (400); A delay switching mechanism (700) is connected to a rotary switching mechanism (600); The rotary switching mechanism (600) includes an upper rotating disk (660) rotatably connected to the lower side of the upper sealing plate (400), and a lower rotating disk (670) rotatably connected to the middle of the lower sealing plate (500).

2. The multi-stage purification apparatus for tetrandrine containing ionic liquid-modified chromatography medium according to claim 1, characterized in that: The rotary switching mechanism (600) also includes three sets of horizontal plates (620) fixed to the side wall of the upper rotating disk (660) and the three circular holes (6100). The inner sides of the upper and lower horizontal plates (620) are fixed with vertical rods (650), and the three vertical rods (650) are fixed with a ring block (630) in the middle.

3. The multi-stage purification apparatus for tetrandrine containing ionic liquid-modified chromatography medium according to claim 2, characterized in that: Each of the upper horizontal plates (620) has a slot in the middle, and each horizontal plate (620) is connected to an outer locking post (690) through the slot.

4. The multi-stage purification apparatus for tetrandrine containing ionic liquid-modified chromatography medium according to claim 3, characterized in that: The top of the multiple outer pins (690) is fixedly connected to a movable ring plate (640), and the inner side of the movable ring plate (640) is slidably sleeved on the outer wall of the upper sealing plate (400).

5. The multi-stage purification apparatus for tetrandrine containing ionic liquid-modified chromatography medium according to claim 4, characterized in that: The upper rotating disk (660) has an outer mesh hole (6120) on its outer side and a double hole (6110) on its inner side. The top of the upper rotating disk (660) is fixed with three inner locking posts (680) at equal intervals around the circumference.

6. The multi-stage purification apparatus for tetrandrine containing ionic liquid-modified chromatography medium according to claim 5, characterized in that: The lower rotating disk (670) has three circular holes (6100) at the position corresponding to the double holes (6110), and the horizontal plate (620) has an indicator block (610) fixedly connected to it in the direction close to the double holes (6110).

7. The multi-stage purification apparatus for tetrandrine containing ionic liquid-modified chromatography medium according to claim 5, characterized in that: The delay switching mechanism (700) includes a distribution plate (720) rotatably connected to the inner cavity of the upper sealing plate (400). The inner side of the distribution plate (720) is provided with an inner mesh hole (730), and the outer side of the inner mesh hole (730) is provided with three liquid inlet holes (760) at equal intervals around the circumference.

8. The multi-stage purification apparatus for tetrandrine containing ionic liquid-modified chromatography medium according to claim 7, characterized in that: The top of the movable ring plate (640) is fixedly connected to six N-shaped plates (710) at equal intervals, and the inner sides of the N-shaped plates (710) are all slidably connected to the edge of the upper sealing plate (400).

9. The multi-stage purification apparatus for tetrandrine containing ionic liquid-modified chromatography medium according to claim 8, characterized in that: Each of the N-shaped plates (710) has a sleeve (740) at its end, and a slide plate (750) is fixed to the top of each sleeve (740).

10. The multi-stage purification apparatus for tetrandrine containing ionic liquid-modified chromatography medium according to claim 9, characterized in that: The distribution plate (720) has six opening slots equidistantly spaced around its lower circumference. The sliding plate (750) is elastically connected to the inner wall of the opening slot. The inner side of the sleeve (740) is engaged with the inner locking post (680).

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