Circulating device
By introducing a circulating device of buffer bottle and replenishing pump in the circulation preparation liquid chromatograph, the problems of solvent diffusion and pressure fluctuations of liquid phase pump are solved, and the stable operation of the liquid phase pump and the smooth baseline of the detector are achieved, which improves the separation and purification effect and collection efficiency.
Patent Information
- Application Number
- CN202422550451.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-22
- Publication Date
- 2025-07-22
- Estimated Expiration
- 2034-10-22
AI Technical Summary
During the circulation process, the existing cyclic liquid chromatographs have problems such as solvent diffusion, difficulty in liquid pumping, and high baseline noise of the detector, which affects the separation and purification effect.
A circulation device including a three-way valve, a buffer bottle, a replenishing pump and a controller is adopted to provide fresh solvents, absorb pressure pulsation of the liquid phase pump, capture gas, realize collection and cleaning within the circulation, and keep the liquid phase pump running normally.
Solvent diffusion and liquid phase pump pressure fluctuations are solved, the detector baseline is stable, the separation and purification effect and collection efficiency are improved, and the system residue is reduced.
Smart Images
Figure CN223137639U_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to a circulation device, belonging to the fields of medicine and food, and in particular to a circulation device for a preparative liquid phase capable of performing cyclic preparation. Background Art
[0002] A preparative liquid phase is an analytical instrument used for separating and purifying a single component in a sample. It separates by dissolving the sample in a mobile phase and pumping it through a chromatographic column filled with a stationary phase. Different components are separated based on their different interactions with the stationary phase. A preparative liquid chromatography instrument mainly consists of a pump, an injector, a chromatographic column, a detector, and a data system.
[0003] The technical characteristics of a preparative liquid chromatography instrument lie in its high-efficiency separation ability and the preparation of high-purity samples. Compared with traditional distillation, crystallization, or extraction methods, a preparative liquid chromatography instrument can separate and purify compounds more precisely and is suitable for the preparation of rare or precious products.
[0004] For the separation and purification of compounds with relatively small differences in molecular structure, theoretically, separation can be achieved by lengthening the chromatographic column. However, in practical applications, as the length of the chromatographic column increases, the column pressure rises, the cost increases, and the difficulty of packing also increases. Therefore, simply increasing the length of the chromatographic column cannot completely separate and purify structurally similar compounds. A cyclic preparative liquid chromatography instrument is based on a conventional preparative chromatograph. By means of a switching device, the separated substances flowing out of the detector are injected into the chromatographic column again for multiple separations. This is equivalent to lengthening the chromatographic column and avoids the increase in column pressure.
[0005] As Figure 1 shown, by adopting the cyclic preparation method, when the cycle is repeated 3 times, the components can be completely separated, greatly improving the separation and purification effect and also saving the solvent.
[0006] As Figure 2 shown, if the tee (101) is an open tee during cyclic preparation, when the liquid phase pump (102) pushes out, the liquid in the circulation system is pushed towards the solvent bottle (106). When the liquid phase pump (102) sucks, the liquid in the pipeline leading to the solvent bottle (106) is sucked into the liquid phase pump (102). Repeating this process multiple times, the liquid in the circulation system will diffuse into the solvent bottle (106), causing contamination of the solvent bottle and diffusion of the sample.
[0007] As Figure 3 shown, if the end of the tee (101) leading to the solvent bottle (106) is closed during cyclic preparation, since there is no pulsation space when the liquid phase pump (102) sucks and pushes, it is difficult for the liquid phase pump (102) to pump liquid. At the same time, due to the pressure fluctuation being superimposed on the detector (105), the baseline noise of the detector (105) is very large, affecting the collection of fractions. Summary of the Invention
[0008] In view of the above defects of the existing treatment methods, the object of the present invention is to provide a circulation device, which can provide fresh solvent when not in circulation. After the circulation is started, the liquid in the circulation system will not spread to the solvent bottle. At the same time, it also provides a pulsation space for the liquid phase pump, and can absorb the pressure pulsation generated by the liquid phase pump to make the detector baseline stable. In addition, the circulation device of the present invention can also perform in-circulation collection, can perform early collection on the well-separated partial peaks during circulation to reduce the diffusion of the peaks, while still maintaining the internal circulation, and then perform collection on the difficult-to-separate peaks after multiple circulations, improving the collection effect.
[0009] To achieve the above object, the present invention adopts the following technical solutions:
[0010] A circulation device includes a first three-way joint (1), a first three-way valve (2), a second three-way joint (3), a second three-way valve (4), a buffer bottle (5), a replenishing pump (6), a third three-way valve (7) and a controller (8). The first three-way joint (1) is connected to the first three-way valve (2), the third three-way valve (7) and a solvent bottle (13). The first three-way valve (2) is connected to the first three-way joint (1), a liquid phase pump (9) and the second three-way joint (3). The second three-way joint (3) is connected to the first three-way valve (2), the buffer bottle (5) and the second three-way valve (4). The second three-way valve (4) is connected to a detector (12), the second three-way joint (3) and a collection end (17). The buffer bottle (5) is connected to the second three-way joint (3) and the replenishing pump (6), and is provided with a solvent overflow port (16) at the upper part. The replenishing pump (6) is located between the buffer bottle (5) and the third three-way valve (7). The third three-way valve (7) is connected to the first three-way joint (1), the replenishing pump (6) and a waste liquid port (15). The controller (8) performs non-circulation liquid supply, circulation preparation, circulation, in-circulation collection, cleaning and emptying operations according to the user-set program.
[0011] Preferably, a circulation device capable of trapping bubbles in the mobile phase includes a first three-way joint (1), a first three-way valve (2), a second three-way joint (3), a second three-way valve (4), a buffer bottle (5), a replenishing pump (6), a third three-way valve (7) and a controller (8). The first three-way joint (1) is connected to the first three-way valve (2), the third three-way valve (7) and a solvent bottle (13). The first three-way valve (2) is connected to the first three-way joint (1), a liquid phase pump (9) and the buffer bottle (5). The second three-way joint (3) is connected to the replenishing pump (6), the buffer bottle (5) and the second three-way valve (4). The second three-way valve (4) is connected to a detector (12), the second three-way joint (3) and a collection end (17). The buffer bottle (5) is connected to the second three-way joint (3) and the first three-way valve (2), and has a solvent overflow port (16) at the upper part. The replenishing pump (6) is located between the second three-way joint (3) and the third three-way valve (7). The third three-way valve (7) is connected to the first three-way joint (1), the replenishing pump (6) and a waste liquid port (15). The controller (8) performs non-circulating liquid supply, circulation preparation, circulation, in-circulation collection, cleaning and emptying operations according to the user-set program.
[0012] Preferably, the second three-way joint (3) is a Y-shaped three-way joint or a T-shaped three-way joint, which can well absorb the pressure pulsation when the liquid phase pump (9) is working.
[0013] Preferably, the replenishing pump (6) is a peristaltic pump, which can perform forward and reverse rotations. When rotating forward, it replenishes or cleans the buffer bottle (5), and when rotating backward, it empties the buffer bottle (5).
[0014] Preferably, the circulation device further includes a liquid level sensor (14). The liquid level sensor (14) is located on the buffer bottle (5), and can set an appropriate volume of the buffer solution in the buffer bottle (5) according to the volume of a single plunger movement of the liquid phase pump (9) during circulation preparation, so as to make the circulation state reach the best.
[0015] Preferably, when performing circulation, early collection can also be performed on some peaks with better separation. At this time, the third three-way valve (7) is connected to the first three-way joint (1), the replenishing pump (6) runs forward, and the replenishing operation is performed, and the liquid level in the buffer bottle (5) is always maintained, so as to achieve stable collection within the circulation. Beneficial effects
[0016] (1) When not in circulation, it provides fresh solvent for the liquid phase pump.
[0017] (2) During circulation preparation, there is no need to stop the pump, and the preparation of the buffer bottle can be carried out synchronously.
[0018] (3) During circulation, the solution within the circulation will not diffuse into the solvent bottle.
[0019] During circulation, sufficient pulsation space is provided for the liquid-phase pump to ensure the normal operation of the liquid-phase pump.
[0020] During circulation, the pressure pulsation during the operation of the liquid-phase pump is absorbed, making the detector baseline stable.
[0021] During circulation, the gas in the mobile phase will be trapped by the buffer bottle, greatly reducing the influence of the gas in the flow path on the detector.
[0022] During circulation, in-cycle collection can be performed. While maintaining the circulation state, early collection can be carried out for some well-separated peaks, improving the collection efficiency.
[0023] The appropriate buffer capacity can be set according to the plunger volume of the liquid-phase pump to optimize the circulation state.
[0024] The system can be easily cleaned and emptied, with little system residue. Description of the Drawings
[0025] Figure 1 is the cyclic preparative chromatogram
[0026] In the figure: 0, first chromatographic separation; 1, one-time cyclic preparation; 2, two-time cyclic preparation; 3, three-time cyclic preparation.
[0027] Figure 2 is the schematic diagram of open three-way cyclic preparation
[0028] In the figure: 101, three-way; 102, liquid-phase pump; 103, injector; 104, chromatographic column; 105, detector; 106, solvent bottle.
[0029] Figure 3 is the schematic diagram of closed three-way cyclic preparation
[0030] In the figure: 101, three-way; 102, liquid-phase pump; 103, injector; 104, chromatographic column; 105, detector; 106, solvent bottle.
[0031] Figure 4 is the schematic diagram of Embodiment 1 of the cyclic device of the present invention
[0032] In the figure: 1, the first three-way; 2, the first three-way valve; 3, the second three-way; 4, the second three-way valve; 5, buffer bottle; 6, make-up pump; 7, the third three-way valve; 8, controller; 9, liquid-phase pump; 10, injector; 11, chromatographic column; 12, detector; 13, solvent bottle; 14, liquid level sensor; 15, waste liquid port; 16, solvent overflow port; 17, collection end.
[0033] Figure 5 is the schematic diagram of Embodiment 2 of the cyclic device of the present invention
[0034] In the figure: 1. The first three-way joint, 2. The first three-way valve, 3. The second three-way joint, 4. The second three-way valve, 5. The buffer bottle, 6. The liquid replenishing pump, 7. The third three-way valve, 8. The controller, 9. The liquid phase pump, 10. The injector, 11. The chromatographic column, / 2. The detector, 13. The solvent bottle, 14. The liquid level sensor, 15. The waste liquid port, 16. The solvent overflow port, 17. The collection end. Specific Embodiment
[0035] The following describes in detail the preferred embodiments of the present invention with reference to the accompanying drawings. Embodiment 1
[0036] As Figure 4 shown, a circulation device includes the first three-way joint, the first three-way valve, the second three-way joint, the second three-way valve, the buffer bottle, the liquid replenishing pump, the third three-way valve, the controller, the liquid phase pump, the injector, the chromatographic column, the detector, the solvent bottle, and the liquid level sensor.
[0037] The working procedure of the circulation device is as follows:
[0038] Non-circulating liquid supply: The first three-way valve (2) is connected to the first three-way joint (1), the second three-way valve (4) is connected to the collection end (17), the liquid phase pump (9) operates, sucks the solvent from the solvent bottle (13), passes through the chromatographic column (11) and the detector (12), and flows out from the collection end.
[0039] Preparation before circulation: The third three-way valve (7) is connected to the first three-way joint (1), the liquid replenishing pump (6) runs forward, sucks the solvent from the solvent bottle (13) into the buffer bottle (5), and when the liquid level sensor (14) shows that the set liquid level is reached, the liquid replenishing pump (6) stops running.
[0040] Circulation: The first three-way valve (2) is connected to the second three-way joint (3), the second three-way valve (4) is connected to the second three-way joint (3), the liquid phase pump (9) keeps operating. When the liquid phase pump (9) pushes out, the excess liquid enters the buffer bottle (5), and when the liquid phase pump (9) sucks, it sucks the liquid from the buffer bottle (5). At the same time, the pressure pulsation during the operation of the liquid phase pump (9) is absorbed by the second three-way joint (3) and the buffer bottle (5).
[0041] Collection within the loop: The first three-way valve (2) is connected to the second three-way (3), the second three-way valve (4) is connected to the collection end (17), the liquid phase pump (9) remains operational, and the solvent flows through the chromatographic column (11), the detector (12), and the second three-way valve (4) towards the collection end (17). Meanwhile, the controller (8) monitors the decrease in the liquid level in the buffer bottle (5), and the replenishing pump (6) starts to operate to replenish the solvent into the buffer bottle (5) until the target liquid level is reached. In this way, the liquid level in the buffer bottle is maintained at all times. After the collection is completed, the second three-way valve (4) is connected to the second three-way (3), and the loop continues to execute.
[0042] Cleaning: First, the first three-way valve (2) is connected to the first three-way (1), the second three-way valve (4) is connected to the second three-way (3), the liquid phase pump (9) operates to draw the solvent from the solvent bottle (13), passes through the chromatographic column (11), the detector (12), the second three-way valve (4), and the second three-way (3), enters the buffer bottle (5), and flows out through the overflow port (16) into the waste liquid collection container to clean the branch pipeline of the second three-way (3). Subsequently, the third three-way valve (7) is connected to the first three-way (1), the replenishing pump (6) runs forward, and the solvent enters the buffer bottle (5) and flows out through the overflow port (16) into the waste liquid collection container to clean the buffer bottle.
[0043] Emptying: The third three-way valve (7) is connected to the waste liquid port (15), the replenishing pump (6) runs in reverse, air enters from the overflow port (16) of the buffer bottle (5), and the liquid in the buffer bottle (5) is emptied. Example 2
[0044] As Figure 5 shown, a circulation device includes a first three-way, a first three-way valve, a second three-way, a second three-way valve, a buffer bottle, a replenishing pump, a third three-way valve, a controller, a liquid phase pump, an injector, a chromatographic column, a detector, a solvent bottle, and a liquid level sensor.
[0045] The working procedure of the circulation device is as follows:
[0046] Non-circulating liquid supply: The first three-way valve (2) is connected to the first three-way (1), the second three-way valve (4) is connected to the collection end (17), the liquid phase pump (9) operates to draw the solvent from the solvent bottle (13), passes through the chromatographic column (11) and the detector (12), and flows out at the collection end.
[0047] Preparation before circulation: The third three-way valve (7) is connected to the first three-way (1), the replenishing pump (6) runs forward to draw the solvent from the solvent bottle (13) into the buffer bottle (5). When the liquid level sensor (14) shows that the set liquid level is reached, the replenishing pump (6) stops operating.
[0048] Circulation: The first three-way valve (2) is connected to the buffer bottle (5), the second three-way valve (4) is connected to the second three-way (3), and the liquid phase pump (9) remains working. When the liquid phase pump (9) pushes out, the excess liquid enters the buffer bottle (5), and at the same time, the gas in the mobile phase is trapped by the buffer bottle. When the liquid phase pump (9) sucks, the liquid is drawn from the buffer bottle (5), and at the same time, the pressure pulsation during the operation of the liquid phase pump (9) is absorbed by the second three-way (3) and the buffer bottle (5).
[0049] Collection within the circulation: The first three-way valve (2) is connected to the buffer bottle (5), the second three-way valve (4) is connected to the collection end (17), and the liquid phase pump (9) remains working. The solvent flows through the chromatographic column (11), the detector (12), and the second three-way valve (4) to the collection end (17). At the same time, the controller (8) monitors that the liquid level in the buffer bottle (5) drops, and the replenishing pump (6) starts to work to replenish the solvent into the buffer bottle (5) until the target liquid level is reached. In this way, the liquid level in the buffer bottle is always maintained. After the collection is completed, the second three-way valve (4) is connected to the second three-way (3), and the circulation continues to be executed.
[0050] Cleaning: First, the first three-way valve (2) is connected to the first three-way (1), the second three-way valve (4) is connected to the second three-way (3), and the liquid phase pump (9) works to suck the solvent from the solvent bottle (13), passes through the chromatographic column (11), the detector (12), the second three-way valve (4), and the second three-way (3), enters the buffer bottle (5), and flows out from the overflow port (16) into the waste liquid collection container to clean the branch pipeline of the second three-way (3). Subsequently, the third three-way valve (7) is connected to the first three-way (1), and the replenishing pump (6) runs forward, and the solvent enters the buffer bottle (5) and flows out from the overflow port (16) into the waste liquid collection container to clean the buffer bottle.
[0051] Emptying: The third three-way valve (7) is connected to the waste liquid port (15), and the replenishing pump (6) runs in reverse to introduce air from the overflow port (16) of the buffer bottle (5) to empty the liquid in the buffer bottle (5).
Claims
1. A circulation device, characterized in that: It includes a first three-way joint (1), a first three-way valve (2), a second three-way joint (3), a second three-way valve (4), a buffer bottle (5), a liquid replenishing pump (6), a third three-way valve (7) and a controller (8). The first three-way joint (1) is connected to the first three-way valve (2), the third three-way valve (7) and a solvent bottle (13). The first three-way valve (2) is connected to the first three-way joint (1), a liquid phase pump (9) and the second three-way joint (3). The second three-way joint (3) is connected to the first three-way valve (2), the buffer bottle (5) and the second three-way valve (4). The second three-way valve (4) is connected to a detector (12), the second three-way joint (3) and a collection end (17). The buffer bottle (5) is connected to the second three-way joint (3) and the liquid replenishing pump (6), and has a solvent overflow port (16) at the upper part. The liquid replenishing pump (6) is located between the buffer bottle (5) and the third three-way valve (7). The third three-way valve (7) is connected to the first three-way joint (1), the liquid replenishing pump (6) and a waste liquid port (15).
2. A circulation device, characterized in that: It includes a first three-way joint (1), a first three-way valve (2), a second three-way joint (3), a second three-way valve (4), a buffer bottle (5), a liquid replenishing pump (6), a third three-way valve (7) and a controller (8). The first three-way joint (1) is connected to the first three-way valve (2), the third three-way valve (7) and a solvent bottle (13). The first three-way valve (2) is connected to the first three-way joint (1), a liquid phase pump (9) and the buffer bottle (5). The second three-way joint (3) is connected to the liquid replenishing pump (6), the buffer bottle (5) and the second three-way valve (4). The second three-way valve (4) is connected to a detector (12), the second three-way joint (3) and a collection end (17). The buffer bottle (5) is connected to the second three-way joint (3) and the first three-way valve (2), and has a solvent overflow port (16) at the upper part. The liquid replenishing pump (6) is located between the second three-way joint (3) and the third three-way valve (7). The third three-way valve (7) is connected to the first three-way joint (1), the liquid replenishing pump (6) and a waste liquid port (15).
3. A recycling device according to claim 1 or 2, characterized in that: The second three-way joint (3) is a Y-shaped three-way joint or a T-shaped three-way joint, which can absorb the pressure pulsation when the liquid phase pump (9) is working.
4. A recycling device according to claim 1 or 2, characterized in that: The liquid replenishing pump (6) is a peristaltic pump, which can perform forward and reverse rotations. When rotating forward, it replenishes or cleans the buffer bottle (5), and when rotating reverse, it empties the buffer bottle (5).
5. A circulation device according to claim 1 or 2, characterized in that: The circulation device further includes a liquid level sensor (14). The liquid level sensor (14) is located on the buffer bottle (5) and can be used to maintain the liquid level in the buffer bottle at a certain level.