Flow component collecting device
By designing a multifunctional fraction collection device, using automatic purge, cleaning and blow-drying functions, the problem of sample residue and automatic cleaning in existing fraction collectors is solved, and high-purity sample collection and equipment are realized Run efficiently.
Patent Information
- Application Number
- CN202420483392.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-03-13
- Publication Date
- 2025-02-14
- Estimated Expiration
- 2034-03-13
AI Technical Summary
The existing flow fraction collector has residual samples at the collection end, resulting in a decrease in the sample purity and the inability to automatically clean and blow-dry, affecting the collection of the next sample.
A flow-separation collection device is designed, including multiple three-way solenoid valves, XYZ movement mechanisms, peristaltic pumps, check valves and controllers, which can automatically purge, clean and blow dry the collection end to ensure that before each sample is collected. The pipes are clean and dry.
It effectively reduces sample residues, improves sample purity and collection efficiency, ensures the pure state of each sample collection, and completes the cleaning and blow-drying operation without affecting the mobile phase of high performance liquid chromatography.
Smart Images
Figure CN222482181U_ABST
Abstract
Description
Technical Field
[0001] The invention relates to a fraction collecting device, belonging to the fields of medicine, biology and chemistry, and in particular to a fraction collecting device for liquid chromatography. Background Art
[0002] Liquid chromatography is a type of separation and analysis technology, which is characterized by using liquid as the mobile phase. The high performance liquid chromatography (HPLC) system is mainly composed of a mobile phase storage bottle, an infusion pump, an injector, a chromatographic column, a detector and a recorder. High performance liquid chromatography is widely used in almost all fields of quantitative and qualitative analysis. Liquid chromatography can effectively separate the target main component from various impurity components, and quantify each component by integrating the detector signal.
[0003] In the fields of medicine and biosynthesis, crude macromolecular products need to be purified. Usually, the synthesized compounds are injected into a high-performance liquid chromatography instrument, separated by a chromatographic column, and the corresponding fractions of the main peak are collected to purify the synthesized compounds. The fraction collectors on the market install a three-way valve (liquid inlet, liquid outlet, and collection end) on the motion module to make the pipeline at the collection end thinner and shorter, thereby reducing the residue at the collection end. Even so, there will still be about a dozen microliters to tens of microliters of residual samples at the collection end that cannot be discharged and will remain in the next collected sample. This results in the inability to use the fraction collector when a high-purity target compound is required, and manual liquid collection is often used to complete it. Summary of the invention
[0004] In view of the above-mentioned defects of the existing processing methods, the purpose of the present invention is to provide a fraction collection device, which can purge the residual sample at the collection end, and can automatically clean and dry the pipeline after a sample is collected, so as to keep the pipeline clean and dry before each sample is collected, so as to prepare for the purification of the next sample, thereby greatly reducing the sample residue. At the same time, the device of the present invention has no effect on the normal operation and flow of the mobile phase of the high-performance liquid chromatography during the purge and cleaning. In addition, the present invention provides semiconductor refrigeration temperature control at the sample position, which is conducive to improving the stability of relatively unstable biological samples during preparation.
[0005] In order to achieve the above object, the present invention adopts the following technical solutions:
[0006] A fraction collection device comprises a first three-way solenoid valve (1), a second three-way solenoid valve (2), a third three-way solenoid valve (3), an XYZ motion mechanism (4), a fourth three-way solenoid valve (5), a peristaltic pump (6), a one-way valve (7), a collection end (8), a waste liquid discharge port (9), a physical three-way valve (10) and a controller (11), wherein the first three-way solenoid valve (1) is connected to a liquid chromatography detector (18), the second three-way solenoid valve (2) and the one-way valve (7), the second three-way solenoid valve (2) is connected to the first three-way solenoid valve (1), the peristaltic pump (6) and the third three-way solenoid valve (3), the third three-way solenoid valve (3) is installed on the XYZ motion mechanism (4), and is connected to the second three-way solenoid valve (2), the collection end (8) and the physical three-way valve (10), the XYZ motion mechanism (4) The third three-way solenoid valve (3) is carried and positioned above the fraction collection bottle (15) or the waste liquid discharge port (9); the fourth three-way solenoid valve (5) is connected to the peristaltic pump (6), the cleaning liquid interface and the air interface for switching to cleaning liquid or air; the peristaltic pump (6) is connected to the fourth three-way solenoid valve (5) and the second three-way solenoid valve (2) for extracting cleaning liquid or air to purge, clean or empty the pipeline; the one-way valve (7) is connected to the first three-way solenoid valve (1) and the physical three-way valve (10) to prevent the liquid flow or air flow generated by the peristaltic pump from affecting the liquid chromatography; the physical three-way valve (10) is connected to the one-way valve (7), the third three-way solenoid valve (3) and the waste liquid; and the controller (11) performs motion positioning, fraction collection, post-collection purge, post-collection cleaning and post-collection drying operations according to the user-set program.
[0007] Preferably, the first three-way solenoid valve (1) and the second three-way solenoid valve (2) are connected to the same solenoid valve drive interface, and a high or low level signal of the controller (11) is used to realize simultaneous switching of situation one (the first three-way solenoid valve (1) is connected to the one-way valve (7), and the second three-way solenoid valve (2) is connected to the peristaltic pump (6)) and situation two (the first three-way solenoid valve (1) is connected to the second three-way solenoid valve (2), and the second three-way solenoid valve (2) is connected to the first three-way solenoid valve (1)), thereby improving the simultaneity of valve switching and further reducing the influence of the start of the peristaltic pump on the liquid chromatography.
[0008] Preferably, the fraction collection device further comprises a semiconductor refrigeration plate (16), and the controller (11) controls the semiconductor refrigeration plate (16) to maintain the target set temperature through a proportional integral differential (PID) algorithm according to a user set temperature.
[0009] Preferably, the fraction collecting device further comprises an air filter (13), wherein the air filter (13) is located before the air interface of the fourth three-way solenoid valve (5) and filters the inhaled air to prevent dust particles from entering the system.
[0010] Preferably, the fraction collection device further comprises a detector, which is connected to the waste liquid port of the third three-way solenoid valve (3). Through the chromatographic peak retention time difference between the detector and the liquid chromatography detector (18), the dead volume from the liquid chromatography detector (18) to the collection end (8) can be accurately calculated, thereby enabling accurate delayed switching. Beneficial Effects
[0011] (1) There is no residue at the collection end of the present invention, thereby improving the purity of the collected sample.
[0012] (2) The present invention can purge the tail liquid at the collection end to improve the sample yield.
[0013] (3) The present invention can perform automatic cleaning and drying after collecting a sample, ensuring that each collected sample does not interfere with each other.
[0014] (4) The present invention can cool the sample, which is beneficial to improving the stability of the sample during collection.
[0015] (5) After the equipment is used, it can be cleaned and emptied online without the aid of a high-performance liquid chromatography (HPLC). The equipment does not need to be disconnected from the HPLC and can be normally connected to the HPLC and started when collection is required. BRIEF DESCRIPTION OF THE DRAWINGS
[0016] Figure 1 Schematic diagram of the flow fraction collection device embodiment 1 of the present invention
[0017] In the figure: 1. first three-way solenoid valve, 2. second three-way solenoid valve, 3. third three-way solenoid valve, 4. XYZ axis motion mechanism, 5. fourth three-way solenoid valve, 6. peristaltic pump, 7. one-way valve, 8. collecting end, 9. waste liquid discharge port, 10. physical three-way, 11. controller, 12. air, 13. air filter, 14. cleaning liquid bottle, 15. fraction collecting bottle, 16. semiconductor refrigeration plate, 17. waste liquid receiving bottle, 18. liquid chromatography detector.
[0018] Figure 2 This is a structural diagram of the flow fraction collection device of the present invention. DETAILED DESCRIPTION
[0019] The preferred embodiments of the present invention are described in detail below in conjunction with the accompanying drawings. Example
[0020] like Figure 1As shown, a flow fraction collection device includes a first three-way solenoid valve, a second three-way solenoid valve, a third three-way solenoid valve, an XYZ motion mechanism, a fourth three-way solenoid valve, a peristaltic pump, a one-way valve, a collection end, a waste liquid discharge port, a physical three-way valve, an air filter, a controller, and a semiconductor refrigeration plate.
[0021] The working procedure of the fraction collection device is as follows:
[0022] Temperature control: The user sets the temperature to be controlled in the UI. After clicking Set, the controller uses a separate thread to perform temperature control according to the set temperature.
[0023] Sequence collection and run: The user selects the sample rack type, the starting sample number and the ending sample number, sets the trigger collection threshold, and automatically executes the run after clicking Run. For each sample run, the current run starts when the liquid chromatography injection trigger signal is received, and the next run automatically runs after the movement ends until the sequence run ends.
[0024] Each needle is operated: under normal conditions, the first three-way solenoid valve (1) is connected to the second three-way solenoid valve (2), the second three-way solenoid valve (2) is connected to the third three-way solenoid valve (3), and the third three-way solenoid valve (3) is connected to the physical three-way valve (10). After the liquid chromatograph injector injects the sample, the external interrupt of the controller (11) is triggered, and the controller (11) controls the XYZ motion mechanism to move to the top of the corresponding sample position. At the same time, the controller (11) starts to monitor the liquid chromatograph detector signal. When the signal intensity exceeds the set threshold, the collection timing is started and the cumulative delay volume is calculated. When the cumulative delay volume reaches the system dead volume, the third three-way solenoid valve (3) is connected to the collection end (4) to perform fraction collection. When the liquid chromatograph detector signal is detected to be lower than the set threshold, the collection timing is started and the cumulative delay volume is calculated. When the cumulative delay volume reaches the system dead volume, the third three-way solenoid valve (3) is connected to the physical three-way valve (10) to end the collection.
[0025] Purging after collection: When the collection of this needle is completed, the first three-way solenoid valve (1) is connected to the one-way valve (7), the fourth three-way solenoid valve (5) is connected to the air filter (13), the second three-way solenoid valve (2) is connected to the peristaltic pump (6), the third three-way solenoid valve (3) is connected to the physical three-way valve (10), the peristaltic pump (6) is turned on, air is pumped in, the pipeline is emptied, and the peristaltic pump (6) is stopped. The third three-way solenoid valve (3) is connected to the collection end (8), the peristaltic pump (6) is turned on, air is pumped in, the residual sample at the collection end is purged, and the peristaltic pump (6) is stopped.
[0026] Cleaning after collection: The controller (11) controls the XYZ motion mechanism to move to the top of the waste liquid discharge port (9), the first three-way solenoid valve (1) is connected to the one-way valve (7), the fourth three-way solenoid valve (5) is connected to the cleaning liquid (14), the second three-way solenoid valve (2) is connected to the peristaltic pump (6), the third three-way solenoid valve (3) is connected to the collection end (8), the peristaltic pump (6) is turned on, the cleaning liquid is pumped in, the pipeline is cleaned, and the peristaltic pump (6) is stopped.
[0027] Blow dry after collection: The XYZ motion mechanism moves and remains above the waste liquid discharge port (9), the first three-way solenoid valve (1) is connected to the one-way valve (7), the fourth three-way solenoid valve (5) is connected to the air filter (13), the second three-way solenoid valve (2) is connected to the peristaltic pump (6), the third three-way solenoid valve (3) is connected to the collection end (8), the peristaltic pump (6) is turned on, air is pumped in, the pipeline is blown dry, and the peristaltic pump (6) is stopped.
Claims
1. A fraction collection device, characterized in that: The invention comprises a first three-way solenoid valve (1), a second three-way solenoid valve (2), a third three-way solenoid valve (3), an XYZ motion mechanism (4), a fourth three-way solenoid valve (5), a peristaltic pump (6), a one-way valve (7), a collecting end (8), a waste liquid discharge port (9), a physical three-way valve (10) and a controller (11), wherein the first three-way solenoid valve (1) is connected to a liquid chromatography detector (18), the second three-way solenoid valve (2) and the one-way valve (7), the second three-way solenoid valve (2) is connected to the first three-way solenoid valve (1), the peristaltic pump (6) and the third three-way solenoid valve (3), and the third three-way solenoid valve (3) is installed on the XYZ motion mechanism (4) and connected to the second three-way solenoid valve (2), the collecting end (8) and the physical three-way valve (10). The XYZ motion mechanism (4) carries a third three-way solenoid valve (3) positioned above the fraction collection bottle (15) or the waste liquid outlet (9); the fourth three-way solenoid valve (5) is connected to the peristaltic pump (6), the cleaning liquid interface and the air interface for switching to cleaning liquid or air; the peristaltic pump (6) is connected to the fourth three-way solenoid valve (5) and the second three-way solenoid valve (2) for extracting cleaning liquid or air to purge, clean or empty the pipeline; the one-way valve (7) is connected to the first three-way solenoid valve (1) and the physical three-way valve (10) to prevent the liquid flow or air flow generated by the peristaltic pump from affecting the liquid chromatography; the physical three-way valve (10) is connected to the one-way valve (7), the third three-way solenoid valve (3) and the waste liquid.
2. A fraction collection device according to claim 1, characterized in that: The fraction collection device also includes a semiconductor refrigeration plate (16) for maintaining the sample at a target set temperature.
3. A fraction collection device according to claim 1 or 2, characterized in that: The flow fraction collection device further comprises an air filter (13), wherein the air filter (13) is located before the air interface of the fourth three-way solenoid valve (5) and filters the inhaled air to prevent dust particles from entering the system.