An automated high performance liquid chromatography column regeneration device and methods of use thereof
By automatically switching solvent and rinsing direction, the design solves the problems of complex operation and high labor costs of existing column regeneration devices, and realizes efficient and economical column regeneration.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- NOMI (DALIAN) ROBOT INTELLIGENT TECH CO LTD
- Filing Date
- 2023-11-10
- Publication Date
- 2026-05-05
AI Technical Summary
Existing column rinsing devices require manual operation to switch solvents and rinsing directions, resulting in complex operation, high labor costs, and low economic efficiency.
An automated high-performance liquid chromatography column regeneration device is designed, which adopts a multi-port selector valve and a two-position four-port switching valve to automatically switch the flushing solvent, flow direction and flow rate, simplifying the operation process.
It enables automatic switching of rinsing solvent and rinsing direction, eliminating the need for manual operation, thereby improving regeneration efficiency, reducing labor costs, and enhancing economic benefits.
Smart Images

Figure CN117531243B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of column regeneration technology, and specifically relates to an automatic high-performance liquid chromatography column regeneration device and its usage method. Background Technology
[0002] High-performance liquid chromatography (HPLC) is a novel analytical separation technique developed in the late 1960s and early 1970s. It is widely used in biochemistry, pharmaceutical analysis and production, environmental monitoring, chemical engineering, food hygiene, and commodity testing due to its high separation efficiency, fast analysis speed, and good detection sensitivity. The core of an HPLC instrument is the chromatographic column, and its performance directly affects the accuracy of measurements. After prolonged use or improper application, the column efficiency may decrease or even completely fail. Regenerating a poorly performing column to restore its performance as much as possible is an economical and effective method.
[0003] Conventional column regeneration methods involve rinsing the column inside the chromatograph or using a column rinsing device. However, rinsing the column inside the chromatograph occupies a detection position, reducing instrument efficiency. Furthermore, existing column rinsing devices have the following drawbacks:
[0004] 1. Multiple solvents are often required during the rinsing process. Existing column rinsing devices can only install one column and one rinsing solvent, requiring frequent solvent switching. Solvent switching requires manual operation, which is complicated and the accuracy is not easy to control.
[0005] 2. The rinsing process often requires forward rinsing followed by reverse rinsing, and then forward rinsing again, with alternating forward and reverse rinsing. Existing column rinsing devices generally only have one rinsing direction. Switching the rinsing direction requires disassembling, flipping, and reinstalling the column, which also requires manual switching. The operation is complicated, labor costs are high, and economic efficiency is low. Summary of the Invention
[0006] The purpose of this invention is to provide an automatic high-performance liquid chromatography column regeneration device and its usage method, which can automatically switch the rinsing solvent, flow direction and flow rate, solving the problems of existing column rinsing devices that require manual operation, are complicated to operate, have high labor costs and low economic benefits.
[0007] To achieve the above objectives, the solution of the present invention is as follows: An automatic high-performance liquid chromatography column regeneration device is provided, comprising a column temperature chamber and a power chamber. The column temperature chamber is equipped with a temperature control module, on which multiple chromatographic columns are mounted. The power chamber is equipped with switching valve A, switching valve B, switching valve C, switching valve D, and a pump. Switching valve A, switching valve B, and switching valve C are multi-port selector valves, each having a common interface and multiple branch interfaces. Switching valve D is a two-position four-way switching valve, having port 1, port 2, port 3, and port 4.
[0008] The multiple branch interfaces of the switching valve A are connected to multiple solvent bottles containing rinsing solvent through pipelines. The common interface of the switching valve A is connected to the inlet of the infusion pump. The outlet of the infusion pump is connected to port 1 of the switching valve D. The common interface of the switching valve B is connected to port 2 of the switching valve D. The multiple branch interfaces of the switching valve B are connected to one end of multiple chromatographic columns. The other end of the multiple chromatographic columns is connected to multiple branch interfaces of the switching valve C. The common interface of the switching valve C is connected to port 4 of the switching valve D. Port 3 of the switching valve D is connected to a waste liquid bottle or a chromatographic detector through pipelines.
[0009] Furthermore, the multiple branch interfaces of the switching valve C are respectively connected to the top of multiple chromatographic columns, and the multiple branch interfaces of the switching valve B are respectively connected to the bottom of multiple chromatographic columns. The flushing solvent flows into the top of the chromatographic column through the switching valve C and then flows out from the bottom of the chromatographic column to the switching valve B, which is a forward flushing, and the reverse is a reverse flushing.
[0010] Furthermore, the No. 2 and No. 4 ports of the switching valve D are symmetrically arranged in the center and are adjacent to the No. 1 and No. 3 ports. Controlling the switching valve D to connect the No. 1 port with the No. 4 port and the No. 2 port with the No. 3 port achieves forward flushing, or connecting the No. 1 port with the No. 2 port and the No. 3 port with the No. 4 port achieves reverse flushing.
[0011] Furthermore, it also includes a housing, in which the column temperature chamber and the power chamber are arranged side by side. The housing has multiple through holes on one side wall of the power chamber. The pipe connected to the branch interface of the switching valve A passes through the through holes and connects to the solvent bottle outside the housing. The pipe connected to port 3 of the switching valve D passes through the through holes and connects to the waste liquid bottle or chromatography detector outside the housing.
[0012] Furthermore, switching valve A and switching valve B are arranged side by side above the infusion pump, and switching valve C and switching valve D are arranged side by side above switching valve A and switching valve B. Switching valve B and switching valve C are located on one side closer to the column temperature chamber.
[0013] Furthermore, the box body is equipped with a partition and a main frame. The partition divides the interior of the box body into a temperature chamber and a power chamber. The main frame is located on the rear side of the partition. The temperature control module, switching valve A, switching valve B, switching valve C, switching valve D and infusion pump are located on the main frame.
[0014] Furthermore, both the bottom of the temperature chamber and the power compartment are equipped with leakage channels, and leakage sensors are installed on the leakage channels. The bottom of the side wall of the box is equipped with a waste discharge port that communicates with the leakage channels.
[0015] Furthermore, the front of the enclosure is equipped with a switchable hatch, and the hatch is equipped with a control panel and buttons.
[0016] Furthermore, the valve heads of switching valves A, B, C, and D, as well as the pump head of the infusion pump, are made of SUS, PEEK, or Teflon.
[0017] The present invention also provides a method for using an automated high-performance liquid chromatography column regeneration device, comprising the following steps:
[0018] Step 1: Install the chromatographic column on the temperature control module and turn on the column temperature chamber to set the temperature;
[0019] Step 2: Control switching valves B and C to select the column that needs to be regenerated;
[0020] Step 3: Control switching valve A to select the rinsing solvent;
[0021] Step 4: Control the switching valve D to select either forward flushing or reverse flushing;
[0022] Step 5: Set the flow rate and flushing time of the infusion pump, and turn on the infusion pump to flush;
[0023] Step 6: After rinsing is complete, control switching valve A to switch the rinsing solvent, and repeat steps 4-5.
[0024] Step 7: After rinsing, control switching valves B and C to switch to the next column that needs to be cleaned. Repeat steps 3 to 6 to complete the rinsing of all columns.
[0025] After adopting the above solution, the beneficial effects of the present invention are as follows:
[0026] 1. The switching valve A of the present invention is a multi-port selector valve. The common interface of the switching valve A is connected to the inlet of the infusion pump, and the multiple branch interfaces of the switching valve A are respectively connected to multiple solvent bottles. By controlling the switching valve A, any flushing solvent can be selected for flushing, thereby automatically switching the flushing solvent without manual operation. The operation is simple and highly accurate.
[0027] 2. In this invention, switching valves B and C are multi-port selector valves, and switching valve D is a two-position four-port switching valve. Port 1 of switching valve D is connected to the outlet of the infusion pump, ports 2 and 4 are connected to the common interface of switching valves B and C respectively, and port 3 is connected to the waste bottle or chromatographic detector. Multiple branch interfaces of switching valves B and C are connected to the two ends of multiple chromatographic columns respectively. By controlling switching valves B and C, different chromatographic columns can be switched for cleaning, so that multiple chromatographic columns can be installed. Without frequent disassembly and assembly of chromatographic columns, different chromatographic columns can be automatically switched for cleaning, thereby improving the regeneration efficiency of chromatographic columns.
[0028] 3. The flushing direction can be selected by controlling switching valve D. Taking switching valve C connected to the top of the column and switching valve B connected to the bottom of the column as an example, controlling switching valve D to connect ports 1 and 4, and ports 2 and 3, allows the flushing solvent to flow out from the outlet of the infusion pump, sequentially through ports 1 and 4 of switching valve D and switching valve C, flowing from the top of the column to flush the column, then out from the bottom, and then sequentially through switching valve B, ports 2 and 3 of switching valve D into the waste bottle or chromatographic detector, achieving forward cleaning; if switching valve D is controlled to connect ports 1 and 4, then ports 2 and 3, the flushing direction can be selected. The system connects to port 2, and ports 3 and 4. After the rinsing solvent flows out from the outlet of the infusion pump, it passes sequentially through ports 1 and 2 of switching valve D and switching valve B, flowing from the bottom of the chromatographic column to rinse the column. Then it flows out from the top of the column and passes sequentially through switching valve C, ports 4 and 3 of switching valve D into the waste bottle or chromatographic detector, thus achieving reverse cleaning. Therefore, this invention can automatically control the rinsing direction without manual switching, i.e., without removing, flipping and reinstalling the chromatographic column. The operation is simple and quick, reducing labor costs, improving work efficiency, and resulting in high economic benefits. Attached Figure Description
[0029] Figure 1 This is a schematic diagram of the structure of the present invention;
[0030] Figure 2 This is a schematic diagram of the structure of the present invention with the hatch open;
[0031] Figure 3 This is a schematic diagram of the hidden hatch structure of the present invention;
[0032] Figure 4 This is an exploded view of the present invention;
[0033] Figure 5 This is a schematic diagram of the system principle of forward rinsing column 1 with solvent 1 in this invention;
[0034] Figure 6 This is a schematic diagram of the system principle of using solvent 1 to backwash column 1 in this invention;
[0035] Figure 7This is a schematic diagram of the system principle of using solvent 2 to backwash column 1 in this invention;
[0036] Figure 8 This is a schematic diagram of the system principle of using solvent 3 to backwash column 1 in this invention;
[0037] Figure 9 This is a schematic diagram of the system principle of using solvent 1 to backwash column 2 in this invention.
[0038] Label Explanation:
[0039] 1. Column temperature chamber; 11. Temperature control module; 111. Snap-fit; 12. Chromatographic column; 2. Power chamber; 21. Switching valve A; 22. Switching valve B; 23. Switching valve C; 24. Switching valve D; 25. Infusion pump; 3. Solvent bottle; 4. Waste bottle; 5. Cabinet; 51. Through hole; 52. Partition; 53. Main frame; 54. Leakage tank; 55. Leakage sensor; 56. Waste outlet; 57. Door; 571. Left door; 572. Right door; 573. Control panel; 574. Buttons; 58. Waste discharge channel; 59. Rear panel. Detailed Implementation
[0040] The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
[0041] like Figure 1-9 As shown, this invention provides an automatic high-performance liquid chromatography (HPLC) column regeneration device, comprising a column temperature chamber 1 and a power chamber 2. The column temperature chamber 1 is equipped with a temperature control module 11, which has multiple mounting positions for installing a chromatographic column 12. These mounting positions are arranged side-by-side, and each mounting position has a clip 111 for securing the chromatographic column 12. When the chromatographic column 12 needs heating or cooling, the temperature control module 11 initiates heating or cooling via a program, transferring the temperature to the chromatographic column 12 to achieve column regeneration. Precise temperature control of column 12 ensures a stable rinsing environment and improves regeneration efficiency. The power chamber 2 is equipped with switching valves A21, B22, C23, and D24, and a pump 25 (preferably a high-pressure horizontal flow pump). Switching valves A21, B22, and C23 are multi-port selector valves, each with a common interface and multiple branch interfaces. Switching valve D24 is a two-position four-way switching valve with ports 1, 2, 3, and 4.
[0042] The multiple branch interfaces of the switching valve A21 are connected to multiple solvent bottles 3 containing rinsing solvents via pipelines. The types of rinsing solvents in each solvent bottle 3 can be different or the same, depending on the needs. The common interface of the switching valve A21 is connected to the inlet of the infusion pump 25 via pipeline. By controlling the switching valve A21, different rinsing solvents can be switched to be connected to the infusion pump 25. Specifically, the switching can be achieved by rotating the switching dial device on the switching valve A21. The common interface on the switching valve A21 is located in the center, and multiple branch interfaces are arranged in a circle around the common interface. The switching dial device has a strip-shaped hole extending radially outward from the center. This strip-shaped hole allows any branch interface to connect to the common interface. Rotating the switching dial device allows different branch interfaces to connect to the common interface, and the switching dial device can be controlled by a set program to achieve automatic switching of rinsing solvents.
[0043] The outlet of the infusion pump 25 is connected to port 1 of the switching valve D24. The common interface of the switching valve B22 is connected to port 2 of the switching valve D24. Multiple branch interfaces of the switching valve B22 are connected to one end of multiple chromatographic columns 12, and the other end of the multiple chromatographic columns 12 are connected to multiple branch interfaces of the switching valve C23. The common interface of the switching valve C23 is connected to port 4 of the switching valve D24. Port 3 of the switching valve D24 is connected to the waste liquid bottle 4 or the chromatographic detector via a pipeline. All the above connections use pipeline connections, which is existing technology and will not be described in detail here.
[0044] Different chromatographic columns 12 can be switched by controlling switching valves B22 and C23. The arrangement of the branch interfaces of switching valves B22 and C23 and the switching method are the same as those of switching valve A21, that is, switching different branch interfaces to connect with the common interface to realize automatic switching of different chromatographic columns 12. Thus, this invention can install multiple chromatographic columns 12 at one time. After the previous chromatographic column 12 is flushed, the next chromatographic column 12 can be replaced without interruption, eliminating the need for frequent replacement of chromatographic columns 12 and greatly improving the regeneration efficiency of chromatographic columns 12. In addition, it should be noted that the branch interfaces of switching valves B22 and C23 connected to the common interface are connected to one chromatographic column 12; otherwise, the flushing wastewater cannot be discharged.
[0045] The flushing direction can be selected by controlling the switching valve D24. Specifically, this is achieved by rotating the switching disc on the switching valve D24. Ports 1, 2, 3, and 4 are arranged in a circle. The switching disc of the switching valve D24 has two arc-shaped holes. Rotating this switching disc allows the two arc-shaped holes to connect port 1 with port 2, port 3, and port 4 respectively, or to connect port 1 with port 4 and port 2 with port 3. This is existing technology and will not be described in detail here. (Refer to...) Figure 5 and Figure 6Taking the example of multiple branch interfaces of switching valve C23 connected to the top of multiple chromatographic columns 12 respectively, and multiple branch interfaces of switching valve B22 connected to the bottom of multiple chromatographic columns 12 respectively, the switching valve D24 is controlled to connect ports 1 and 4, and ports 2 and 3 respectively. After the flushing solvent flows out from the outlet of the infusion pump 25, it flows into the flushing column 12 from the top of the column 12 through ports 1 and 4 of switching valve D24 and switching valve C23 in sequence, and then flows out from the bottom of the column 12, and then flows into the switching valve B22 and switching valve D2 in sequence. Ports 2 and 3 of column 4 enter waste bottle 4 or the chromatographic detector for forward cleaning. If switching valve D24 is controlled to connect ports 1 and 2, and ports 3 and 4, the rinsing solvent, after flowing from the outlet of pump 25, will sequentially pass through ports 1 and 2 of switching valve D24 and switching valve B22, flowing from the bottom of column 12 to rinse column 12, then flowing out from the top of column 12, and then sequentially passing through switching valve C23, ports 4 and 3 of switching valve D24 into waste bottle 4 or the chromatographic detector for reverse cleaning. The switching disc device of switching valve D24 can also be controlled by a set program, thus automatically selecting the rinsing direction without manual switching. This simplifies operation, greatly reduces labor costs, and is highly economical.
[0046] The chromatographic column 12 generally needs to be rinsed multiple times. The waste liquid from the first few rinses is usually discharged into the waste liquid bottle 4, while the waste liquid from the later rinses can be discharged into the chromatographic detector (not shown in the figure) to detect the regeneration status of the chromatographic column 12. If the detection is qualified, the regeneration is complete.
[0047] Key references Figure 5 The switching valve D24 has ports 2 and 4 symmetrically arranged, both adjacent to ports 1 and 3. That is, ports 2 and 4, and ports 1 and 3 are not adjacent. Rotating the rotating disc of the switching valve D24 can only connect ports 1 and 4, or ports 2 and 3 to achieve forward flushing, or connect ports 1 and 2, or ports 3 and 4 to achieve reverse flushing, to prevent ports 2 and 4, or ports 1 and 3 from being connected and thus failing to achieve the flushing effect.
[0048] Key references Figure 1-4This invention separates the temperature control module 11, the chromatographic column 12, and all switching valves and infusion pumps 25, ensuring that the heating or cooling of the chromatographic column 12 is unaffected by external factors and the switching valves and infusion pumps 25. This guarantees precise temperature control, stabilizes the rinsing environment of the chromatographic column 12, and improves regeneration efficiency. The switching valves and infusion pumps 25 are also unaffected by temperature, resulting in smoother operation. The invention also includes a housing 5, within which the column temperature chamber 1 and the power chamber 2 are arranged side-by-side. This adjacent arrangement facilitates the connection of switching valves B22 and C23 to the chromatographic column 12. Furthermore, the mounting positions on the temperature control module 11 can be arranged side-by-side, allowing multiple chromatographic columns 12 to be installed side-by-side. This rational layout allows for the installation of more chromatographic columns 12 while minimizing space requirements.
[0049] Key references Figure 1 and Figure 3 The housing 5 has multiple through holes 51 on one side wall of the power compartment 2. The pipe connected to the branch interface of the switching valve A21 can pass through the through holes 51 and connect to the solvent bottle 3 outside the housing 5. The pipe connected to port 3 of the switching valve D24 can also pass through one of the through holes 51 and connect to the waste liquid bottle 4 or the chromatography detector outside the housing 5. The left and right sides of the housing 5 are also provided with air inlets and outlets for ventilation.
[0050] Key references Figure 2 and Figure 3 Furthermore, switching valves A21 and B22 are preferably arranged side-by-side above the infusion pump 25, and switching valves C23 and D24 are preferably arranged side-by-side above switching valves A21 and B22. Switching valves B22 and C23 are preferably located on the side closer to the column temperature chamber 1 to facilitate their connection with the chromatographic column 12. Switching valves A21 and D24 are located on the other side, near the through hole 51 on the housing 5, to facilitate their connection with the solvent bottle 3 and the waste liquid bottle 4 or the chromatographic detector. Switching valve A21 is also close to the infusion pump 25 for easy connection. Switching valve D24 is adjacent to the other three switching valves for easy connection. In addition, all switching valves and infusion pumps 25 are arranged vertically in a regular pattern to reduce space occupation; and it should be added that the positions of all switching valves and infusion pumps 25 are not fixed and can be adjusted as needed.
[0051] In summary, the arrangement of all structures within the housing 5 of this invention is reasonable, which not only facilitates the connection between various components and reduces the space occupied, but also minimizes the mutual influence between the temperature chamber 1 and the power chamber 2, enabling the regeneration device to operate stably.
[0052] Key references Figure 4The enclosure 5 is equipped with a partition 52 and a main frame 53. The partition 52 divides the interior of the enclosure 5 into a column temperature chamber 1 and a power chamber 2. The main frame 53 is located behind the partition 52. The temperature control module 11, switching valve A21, switching valve B22, switching valve C23, switching valve D24 and infusion pump 25 are mounted on the main frame 53. The rear panel 59 of the enclosure 5 is detachable. The components in the column temperature chamber 1 and the power chamber 2 can be installed on the main frame 53 first, and then the rear panel 59 can be removed and the main frame 53 can be installed into the enclosure 5. This allows all the components in the column temperature chamber 1 and the power chamber 2 to be installed into the enclosure 5 at once, making the installation convenient and quick.
[0053] Key references Figure 3 Both the column temperature chamber 1 and the power chamber 2 are equipped with leakage channels 54 at their bottoms to receive leaked liquid. Each leakage channel 54 is equipped with a leakage sensor 55, which will trigger an alarm when the waste liquid level is higher than the sensor 55, alerting personnel for maintenance. The bottom side wall of the housing 5 has a waste discharge port 56 communicating with the leakage channels 54, through which waste liquid can be discharged from the housing 5. Specifically, two leakage channels 54 are preferably provided, respectively located at the bottom of the column temperature chamber 1 and the power chamber 2, with one channel 54 being higher than the other. A waste discharge channel 58 is opened at the bottom of the partition 52 to connect the two channels 54. Waste liquid in the higher channel is discharged into the lower channel, and waste liquid in the lower channel is discharged through the waste discharge port 56. In addition to the leakage sensor 55, the invention can also be equipped with a temperature alarm and a pressure detection alarm to monitor temperature and pressure, respectively, ensuring the safety and reliability of the regeneration device and enabling it to operate without manual supervision.
[0054] Key references Figure 1 and Figure 2 The front of the housing 5 is equipped with a switchable hatch 57, specifically two hatches 57, one on the left and one on the right, for easy opening and closing. The two hatches 57 are designed with one larger than the other, with the left hatch 571 larger than the right hatch 572. A control panel 573 and buttons 574 can be installed on the left hatch 571. The control panel 573 can be an electronic touchscreen. On the control panel 573, the type of rinsing solvent, rinsing direction, rinsing time, column temperature chamber 1 temperature, and infusion pump 25 flow rate can be set. Pressing the button 574 will start the regeneration device to automatically rinse the chromatographic column 12. Furthermore, when the liquid level in the leakage tank 54 is higher than the leakage sensor 55, a warning will be displayed on the control panel 573.
[0055] As a preferred option, all pipelines in this device, as well as the valve heads of switching valves A21, B22, C23, and D24, and the pump head of infusion pump 25, can be made of SUS, PEEK, or Teflon, which have strong corrosion resistance and long service life.
[0056] The present invention also provides a method for using an automated high-performance liquid chromatography column 12 regeneration device, specifically including the following steps:
[0057] Step 1: Install the chromatographic column 12 in the forward direction on the temperature control module 11 and connect it in the forward direction. That is, the top of the chromatographic column 12 is connected to the branch interface of the switching valve C23 through a pipeline, and the bottom of the chromatographic column 12 is connected to the branch interface of the switching valve B22 through a pipeline. Turn on the column temperature chamber 1 and set the temperature.
[0058] Step 2: Control switching valves B22 and C23 to select the chromatographic column 12 that needs to be regenerated, that is, connect the common interface of switching valves B22 and C23 to the branch interface of the chromatographic column 12 that needs to be regenerated.
[0059] Step 3: Control the switching valve A21 to select the flushing solvent, that is, connect the common interface of the switching valve A21 to the branch interface of the selected flushing solvent.
[0060] Step 4: Control the switching valve D24 to select forward flushing or reverse flushing, that is, control the connection of port 1 and port 4, port 2 and port 3 of the switching valve D24, or the connection of port 1 and port 2, port 3 and port 4.
[0061] Step 5: Set the flow rate and flushing time of the infusion pump 25, and turn on the infusion pump 25 to flush;
[0062] Step 6: After rinsing is complete, control the switching valve A21 to switch the rinsing solvent and repeat steps 4-5.
[0063] Step 7: After rinsing is completed, control switching valves B22 and C23 to switch to the next column 12 that needs to be cleaned. Repeat steps 3 to 6 to complete the rinsing of all columns 12.
[0064] The above steps can be controlled manually or run automatically through programming. All parameters can be set in advance, and pressing button 574 will automatically run all the above steps. The operation is simple and greatly improves the regeneration efficiency.
[0065] The following specific embodiments further illustrate the method of using the regeneration device:
[0066] Example 1:
[0067] Referring specifically to points 5-8, in this embodiment: the switching valve A21 has eight branch interfaces, and the solvent bottle 3 has eight corresponding interfaces, allowing for the selection of up to eight rinsing solvents. Solvent 1 is pure water, solvent 2 is a protease reagent (0.5% trypsin reagent), solvent 3 is a surfactant (0.1% EDTA-2Na), solvent 4 is an ion group reactivator solution (0.1 mol / L sodium hydroxide solution), solvent 5 is whole blood perfusion fluid, and solvents 6-7 can be other solvents or the solvents mentioned above. The switching valves B22 and C have six branch interfaces, and the chromatographic columns 12 are correspondingly arranged in six positions, allowing for the simultaneous installation of six chromatographic columns 12. All chromatographic columns 12 can be of the same or different types. If the columns are of the same type but different sizes, only the rinsing time needs to be adjusted. If the columns are of different types, the regeneration steps will also differ and can be set according to specific circumstances. This embodiment takes the regeneration of six identical glycated hemoglobin analyzer high-performance liquid chromatography columns as an example, and the specific regeneration steps are as follows:
[0068] Step 1: Install the six chromatographic columns on the temperature control module and connect them in the forward direction. Turn on the column temperature chamber and set the temperature to 37°C.
[0069] Step 2: Select column 1, that is, connect the common interface of control switching valve B and switching valve C to the branch interface connected to column 1.
[0070] Step 3: Select solvent 1 (pure water), that is, connect the common interface of control switching valve A to the branch interface of solvent 1;
[0071] Step 4: Select reverse flushing, that is, connect port 1 of control switching valve D to port 2, port 3 and port 4;
[0072] Step 5: Set the infusion pump flow rate to 1.5 ml / min and the flushing time to 17 min, then turn on the infusion pump to flush.
[0073] Step 6: After rinsing, connect the common interface of control switching valve A to the branch interface of solvent 2 (0.5% trypsin reagent), set the flow rate of the infusion pump to 0.5 ml / min, set the rinsing time to 30 min, and perform rinsing.
[0074] Step 7: After rinsing, connect the common interface of control switching valve A to the branch interface of solvent 3 (0.1% EDTA-2Na), set the flow rate of the infusion pump to 1.0 ml / min, set the rinsing time to 30 min, and perform rinsing.
[0075] Step 8: After rinsing, connect the common interface of control switching valve A to the branch interface of solvent 4 (ionic group reactivator solution), set the flow rate of the infusion pump to 1.0 ml / min, set the rinsing time to 50 min, and perform rinsing.
[0076] Step 9: After rinsing, connect the common interface of control switching valve A to the branch interface of solvent 5 (whole blood perfusion solution), and connect port 1 of control switching valve D to port 4, port 2 and port 3, i.e. select forward rinsing, set the flow rate of the infusion pump to 0.5 ml / min, set the rinsing time to 20 min, and perform rinsing.
[0077] Step 10: After rinsing, connect the common interface of switching valve B and switching valve C to the branch interface connected to column 2, and repeat steps 3 to 8 to rinse column 2. Repeat this cycle to complete the rinsing of all six columns.
[0078] Example 2:
[0079] This embodiment uses a standard C8 and C18 column with a regeneration size of 4.6 mm × 250 mm as an example. The number of common interfaces of each switching valve and the number of solvent bottles 3 are the same as in Example 1. The type of rinsing solvent is different, and the rinsing procedure can be as follows:
[0080] Step 1: Install the six chromatographic columns on the temperature control module and connect them in the forward direction. Turn on the column temperature chamber and set the temperature to 35°C.
[0081] Step 2: Select column 1, that is, connect the common interface of control switching valve B and switching valve C to the branch interface connected to column 1.
[0082] Step 3: Select solvent 1 (water-methanol = 90:10), that is, connect the common interface of control switching valve A to the branch interface of solvent 1;
[0083] Step 4: Select reverse flushing, that is, connect port 1 of control switching valve D to port 2, port 3 and port 4;
[0084] Step 5: Set the infusion pump flow rate to 0.5 ml / min and the flushing time to 30 min, then turn on the infusion pump to flush.
[0085] Step 6: After rinsing is completed, connect port 1 of the control switching valve D to port 4, port 2 and port 3, that is, select forward cleaning, set the rinsing time to 300 minutes, and perform rinsing.
[0086] Step 7: After rinsing is completed, connect the common interface of control switching valve A to the branch interface of solvent 2 (water-methanol = 10:90), set the rinsing time to 60 minutes, and perform rinsing.
[0087] Step 8: After rinsing is completed, connect the common interface of control switching valve A to the branch interface of solvent 3 (water-methanol = 5:95), set the rinsing time to 60 minutes, and perform rinsing.
[0088] Step 9: After rinsing is completed, connect the common interface of control switching valve A to the branch interface of solvent 4 (methanol), set the rinsing time to 60 minutes, and perform rinsing.
[0089] Step 10: After rinsing, set the infusion pump flow rate to 1.0 ml / min and the rinsing time to 60 min for rinsing.
[0090] Step 11: After rinsing, connect the common interface of switching valve B and switching valve C to the branch interface connected to column 2, and repeat steps 3 to 8 to rinse column 2. Repeat this cycle to complete the rinsing of all six columns.
[0091] The above description is only a preferred embodiment of the present invention and is not intended to limit the design of this case. All equivalent changes made based on the key design features of this case shall fall within the protection scope of this case.
Claims
1. An automated high-performance liquid chromatography column regeneration device, characterized in that: It includes a column temperature chamber and a power chamber. The column temperature chamber is equipped with a temperature control module, on which multiple chromatographic columns are installed. The power chamber is equipped with switching valve A, switching valve B, switching valve C, switching valve D and an infusion pump. Switching valve A, switching valve B and switching valve C are multi-port selector valves, each with one common interface and multiple branch interfaces. Switching valve D is a two-position four-way switching valve with port 1, port 2, port 3 and port 4. The multiple branch interfaces of the switching valve A are connected to multiple solvent bottles containing rinsing solvent through pipelines. The common interface of the switching valve A is connected to the inlet of the infusion pump. The outlet of the infusion pump is connected to port 1 of the switching valve D. The common interface of the switching valve B is connected to port 2 of the switching valve D. The multiple branch interfaces of the switching valve B are connected to one end of multiple chromatographic columns. The other end of the multiple chromatographic columns is connected to multiple branch interfaces of the switching valve C. The common interface of the switching valve C is connected to port 4 of the switching valve D. Port 3 of the switching valve D is connected to a waste liquid bottle or a chromatographic detector through pipelines. In this system, multiple branch interfaces of switching valve C are connected to the tops of multiple chromatographic columns, and multiple branch interfaces of switching valve B are connected to the bottoms of multiple chromatographic columns. The flushing solvent flows from the top of the chromatographic column through switching valve C and then flows out from the bottom of the chromatographic column to switching valve B, which is forward flushing, and vice versa, which is reverse flushing. The No. 2 and No. 4 ports of switching valve D are symmetrically arranged and are adjacent to No. 1 and No.
3. Controlling switching valve D to connect No. 1 and No. 4 and No. 2 and No. 3 ports achieves forward flushing, or connecting No. 1 and No. 2 and No. 3 and No. 4 ports achieves reverse flushing.
2. An automated high-performance liquid chromatography column regeneration device as described in any one of claims 1, characterized in that: It also includes a housing, in which the column temperature chamber and the power chamber are arranged side by side. The housing has multiple through holes on one side wall of the power chamber. The pipe connected to the branch interface of the switching valve A passes through the through holes and connects to the solvent bottle outside the housing. The pipe connected to port 3 of the switching valve D passes through the through holes and connects to the waste liquid bottle or chromatography detector outside the housing.
3. The automated high-performance liquid chromatography column regeneration device as described in claim 2, characterized in that: The switching valves A and B are arranged side by side above the infusion pump, and the switching valves C and D are arranged side by side above the switching valves A and B. The switching valves B and C are located on one side closer to the column temperature chamber.
4. The automated high-performance liquid chromatography column regeneration device as described in claim 3, characterized in that: The box is equipped with a partition and a main frame. The partition divides the interior of the box into a temperature chamber and a power chamber. The main frame is located behind the partition. The temperature control module, switching valve A, switching valve B, switching valve C, switching valve D and infusion pump are located on the main frame.
5. An automated high-performance liquid chromatography column regeneration device as described in claim 2, characterized in that: Both the bottom of the temperature chamber and the power compartment are equipped with a leakage tank, and a leakage sensor is installed on the leakage tank. The bottom of the side wall of the box is equipped with a waste discharge port that communicates with the leakage tank.
6. An automated high-performance liquid chromatography column regeneration device as described in claim 2, characterized in that: The front of the enclosure is equipped with a switchable hatch, and the hatch is equipped with a control panel and buttons.
7. The automated high-performance liquid chromatography column regeneration device as described in claim 1, characterized in that: The valve heads of switching valves A, B, C, and D, as well as the pump head of the infusion pump, are made of SUS, PEEK, or Teflon.
8. The method of using the automated high-performance liquid chromatography column regeneration device as described in claim 1, characterized in that: Includes the following steps: Step 1: Install the chromatographic column on the temperature control module and turn on the column temperature chamber to set the temperature; Step 2: Control switching valves B and C to select the column that needs to be regenerated; Step 3: Control switching valve A to select the rinsing solvent; Step 4: Control the switching valve D to select either forward flushing or reverse flushing; Step 5: Set the flow rate and flushing time of the infusion pump, and turn on the infusion pump to flush; Step 6: After rinsing is complete, control switching valve A to switch the rinsing solvent and repeat steps 4-5. Step 7: After rinsing, control switching valves B and C to switch to the next column that needs to be cleaned. Repeat steps 3 to 6 to complete the rinsing of all columns.
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