An automated device for SABRE hyperpolarization

By designing an automated SABRE hyperpolarization device and utilizing automated sample preparation, bubbling, and solution transfer units, the problems of low efficiency and poor reproducibility of manual operation in existing technologies have been solved, achieving efficient and reliable NMR signal amplification.

CN119164996BActive Publication Date: 2025-11-14XIAMEN UNIV
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Patent Information

Application Number
CN202411334453.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-09-24
Publication Date
2025-11-14
Estimated Expiration
2044-09-24

AI Technical Summary

Technical Problem

Existing SABRE hyperpolarization experiments rely on manual operation, resulting in low efficiency, poor reproducibility, and experimental errors, and lack of automated devices.

Method used

Design a SABRE hyperpolarization automation device that includes an automatic sample preparation unit, an automatic bubbling unit, and a rapid solution transfer unit. Utilize components such as an injection pump, solenoid valve, back pressure valve, and solenoid to achieve automated control and efficient circulation of sample solutions.

Benefits of technology

It improves the repeatability and safety of experiments, reduces the risk of human error, increases work efficiency and reduces experimental error, and achieves efficient polarization transfer and signal amplification of sample solutions.

✦ Generated by Eureka AI based on patent content.

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Abstract

This invention provides an automated device for SABRE hyperpolarization, comprising an automated sample preparation unit, an automated bubbling unit, and a rapid solution transfer unit. The automated sample preparation unit includes multiple syringe pumps and a back pressure valve; each syringe pump includes a switching valve. The automated bubbling unit includes a secondary hydrogen flask, a magnetic shielding cylinder, and a second solenoid valve. The secondary hydrogen flask is connected to a mass flow controller. The magnetic shielding cylinder contains a solenoid and a pressure-resistant bottle; the solenoid encloses the pressure-resistant bottle. The rapid solution transfer unit consists of a pressure-resistant bottle, an NMR tube, an NMR tube adapter, a first solenoid valve, a second solenoid valve, a third solenoid valve, and a three-way valve. The NMR tube is placed inside an NMR spectrometer, and the lower part of the NMR tube adapter is connected to the NMR spectrometer. The NMR tube contains a glass capillary tube. This device enables automated screening and analysis of experimental conditions for rapid SABRE hyperpolarization, significantly reducing human intervention and improving operational safety and the reproducibility of SABRE experiments.
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Description

Technical Field

[0001] This invention belongs to the field of nuclear magnetic resonance hyperpolarization technology, and particularly relates to an automated device for SABRE hyperpolarization. Background Technology

[0002] Nuclear magnetic resonance (NMR) technology is a commonly used analytical tool in chemistry, physics, and modern medicine. It can provide important structural information such as atomic chemical environment, coupling, chemical bonding, atomic spatial distance, and molecular size. However, its low detection sensitivity limits its wider application. In recent decades, various hyperpolarization techniques have been developed, including dynamic nuclear polarization (DNP), secondary hydrogen-induced polarization (PHIP), and reversible exchange signal amplification (SABRE), which have significantly improved the sensitivity of NMR signals.

[0003] SABRE hyperpolarization is a promising hyperpolarization technique that enhances the NMR signal by transferring the spin sequence from secondary hydrogen (an isomer of hydrogen molecules in a singlet nuclear spin state) to the substrate molecule to be polarized. Hyperpolarization of the free substrate is achieved through continuous chemical exchange between the free substrate and the hydrogen molecules in the sample solution, as well as between the metal-bound substrate and the hydrogen molecules. One advantage of this method is that the substrate does not require chemical modification, and its polarization can be regenerated multiple times by bubbling secondary hydrogen through the sample solution. SABRE hyperpolarization provides a rapid, regenerable, and continuous hyperpolarization pathway, capable of amplifying the NMR signal by thousands to tens of thousands of times. In the SABRE hyperpolarization transfer experiment, after introducing secondary hydrogen into the NMR tube containing the sample solution, the sample solution is agitated in a polarization transfer field (PTF) to ensure the secondary hydrogen is fully dissolved, thus initiating polarization transfer. Immediately after agitation, the sample solution is transferred to the NMR spectrometer for a single NMR measurement. However, the experimental process relies heavily on manual operation, which is inefficient. Furthermore, manually shaking and transferring the NMR tube carries the risk of human error, inevitably leading to experimental errors and poor reproducibility.

[0004] Currently, there are relatively few SABRE hyperpolarization devices in China capable of conducting automated magnetic field circulation experiments. Therefore, it is essential to propose an automated SABRE hyperpolarization device for screening and analyzing automated experimental conditions for SABRE hyperpolarization. Summary of the Invention

[0005] The purpose of this invention is to address the above-mentioned problems by providing an automated device for SABRE hyperpolarization that is highly efficient and reproducible.

[0006] To achieve the above objectives, the technical solution adopted by this invention is as follows:

[0007] An automated device for SABRE hyperpolarization includes an automated sample preparation unit, an automated bubbling unit, and a rapid solution transfer unit;

[0008] The automatic sample preparation unit includes multiple injection pumps and a back pressure valve. The injection pump includes a switching valve, and a PEEK tube is connected to the switching valve.

[0009] The automatic bubbling unit includes a secondary hydrogen cylinder, a magnetic shielding cylinder, and a second solenoid valve. The secondary hydrogen cylinder is connected to a mass flow controller. The magnetic shielding cylinder contains a solenoid and a pressure-resistant bottle. The solenoid encloses the pressure-resistant bottle.

[0010] The rapid solution transfer unit consists of a pressure-resistant bottle, an NMR tube, an NMR tube adapter, a first solenoid valve, a second solenoid valve, a third solenoid valve, and a three-way valve; the NMR tube is placed inside the NMR instrument, and the lower part of the NMR tube adapter is connected to the NMR instrument; the NMR tube contains a glass capillary tube.

[0011] The pressure-resistant bottle is connected to the switching valve, the first solenoid valve, the three-way valve, and the back pressure valve respectively; the three-way valve includes a left port, a right port, and a lower port, the left port is connected to the pressure-resistant bottle, the right port is connected to the nuclear magnetic tube adapter, and the lower port is connected to a waste liquid bottle;

[0012] The back pressure valve includes an air inlet and an air outlet. The air inlet is connected to a pressure-resistant bottle, and the air outlet is connected to an outlet end. The nuclear magnetic tube adapter has three connecting ports on its top, which are a left port, a middle port, and a right port. The left port is connected to a second solenoid valve, the middle port is connected to a three-way valve, and the right port is connected to a third solenoid valve.

[0013] In a preferred embodiment, the injection pump and the switching valve are integrated into one unit.

[0014] In a preferred embodiment, the switching valve is provided with multiple valve ports, one of which is connected to the pressure-resistant bottle, and the remaining valve ports are used to connect to different sample bottles respectively.

[0015] The sample solutions contained in the different sample vials are substrate, catalyst, and washing solution, respectively.

[0016] In a preferred embodiment, the solenoid is externally connected to a magnetic shielding device, and the solenoid is controlled by the magnetic shielding device.

[0017] In a preferred embodiment, the automation device further includes an integrated control system, which includes a PCB board and a PC host computer; the PCB board and the PC host computer communicate via a serial port.

[0018] The PCB board is electrically connected to the first solenoid valve, the second solenoid valve, the third solenoid valve, and the three-way valve, respectively. The PC host computer is electrically connected to the injection pump, the MRI machine, the mass flow controller, the back pressure valve, and the magnetic shielding device, respectively.

[0019] In a preferred embodiment, the mass flow controller is connected to a first solenoid valve and a second solenoid valve, and the mass flow controller is used to control the flow rate of the secondary hydrogen cylinder, which outputs secondary hydrogen.

[0020] In a preferred embodiment, the back pressure valve is used to control the pressure inside the pressure-resistant bottle.

[0021] In a preferred embodiment, a lower connection port is provided below the nuclear magnetic tube adapter, and the lower connection port is bonded to the glass capillary tube by epoxy resin.

[0022] In a preferred embodiment, the first solenoid valve, the second solenoid valve, the third solenoid valve, the three-way valve, the PCB board, and the back pressure valve are all powered by a regulated power supply.

[0023] In a preferred embodiment, the sample vial, syringe pump, magnetic shielding cylinder, first solenoid valve, second solenoid valve, third solenoid valve, three-way valve, NMR spectrometer, back pressure valve, PCB board, PC host computer, magnetic shielding instrument, and regulated power supply are all placed in an anti-static cabinet.

[0024] Compared with the prior art, the technical solution of the present invention has the following beneficial effects:

[0025] 1. An NMR tube adapter is set up. A glass capillary tube is installed inside the NMR tube connected to the NMR tube adapter, so that the sample solution in the NMR tube can flow back to the pressure bottle through the glass capillary tube and undergo polarization transfer again, realizing the SABRE hyperpolarized magnetic field cycle experiment, which greatly improves the polarization transfer efficiency.

[0026] 2. A back pressure valve is installed for pressure control. The pressure difference allows the secondary hydrogen to continuously bubble in the pressure-resistant bottle containing the sample solution, fully dissolving the secondary hydrogen into the sample solution and causing polarization transfer. A PCB board is installed to precisely control the bubbling time, greatly improving the repeatability and reliability of the experiment. A first, second, and third solenoid valve are installed to control the gas pressure by controlling the gas path opening and closing, allowing the sample solution to be quickly transferred from the pressure-resistant bottle to the NMR tube, which greatly solves the problem of NMR signal attenuation caused by slow manual solution transfer.

[0027] 3. By designing a highly integrated and compact PCB circuit, the reliability, stability, and scalability of the entire system are improved; by setting up a regulated power supply, the entire device has a stable voltage and current, ensuring normal operation of the equipment; by setting up an anti-static cabinet, the entire device is protected from static electricity damage; by setting up a three-way valve, the sample solution can flow back from the NMR tube to the pressure-resistant bottle, and also flow from the NMR tube into the waste bottle; by setting up multiple injection pumps, and integrating the injection pumps with the switching valve, the pipeline design is optimized, the operating efficiency is improved, and the maintenance cost is reduced.

[0028] 4. The experimental process of this device is fully automated, which greatly reduces human intervention, lowers the risk of human error, improves operational safety, and allows researchers to devote more time to more creative work.

[0029] 5. The device has a reasonable and compact structure, is easy to replicate, and has high reliability. The entire device does not exchange gases with the outside world, allowing for completely inert conditions and preventing the sample solution from oxidizing and deteriorating upon contact with air. Attached Figure Description

[0030] Figure 1 This is a schematic diagram of the main structure of the automation device in a preferred embodiment of the present invention;

[0031] Figure 2 This is a side view of the automated device in a preferred embodiment of the present invention;

[0032] Figure 3 This is a top view of the automated device in a preferred embodiment of the present invention;

[0033] Figure 4 This is a schematic cross-sectional view of the shielding cylinder in a preferred embodiment of the present invention;

[0034] Figure 5 This is a schematic diagram of the exploded disassembly structure of the shielding cylinder in a preferred embodiment of the present invention;

[0035] Figure 6 This is a schematic cross-sectional view of the nuclear magnetic resonance spectrometer in a preferred embodiment of the present invention;

[0036] Figure 7 This is a schematic diagram of the syringe pump structure in a preferred embodiment of the present invention.

[0037] Explanation of reference numerals in the attached diagram: 1. Sample vial; 2. Syringe pump; 3. PEEK tube; 4. Diverter valve; 5. Magnetic shielding cylinder; 6. Three-way valve; 7. NMR tube; 7a. NMR tube adapter; 8. NMR instrument; 9. Gas outlet; 10. Anti-static cabinet; 11. Regulated power supply; 12. Magnetic shielding instrument; 13. PC host computer; 14. PCB board; 15. Hydrogen cylinder; 16. Pneumatic hose; 17. Mass flow controller; 18. First solenoid valve; 18a. Second solenoid valve; 18b. Third solenoid valve; 19. Back pressure valve; 20. Waste liquid bottle; 21. Solenoid; 22. Pressure-resistant bottle; 22a. Pressure-resistant bottle stopper; 23. Glass capillary tube. Detailed Implementation

[0038] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0039] In the description of this invention, it should be noted that the terms "upper," "lower," "inner," "outer," "top / bottom," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing the invention and for simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0040] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installed", "equipped", "sleeved / connected", "connected", etc., should be interpreted broadly. For example, "connection" can be a wall-mounted connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium; it can be a connection within two components. For those skilled in the art, the specific meaning of the above terms in this invention can be understood according to the specific circumstances.

[0041] refer to Figures 1-7 This embodiment provides an automated apparatus for SABRE hyperpolarization, enabling rapid automated screening and analysis of experimental conditions for SABRE hyperpolarization. By significantly reducing human intervention, it not only improves operational safety but also enhances the reproducibility of SABRE experiments. This automated apparatus, with its automated design, provides a more convenient experimental tool for the field of nuclear magnetic resonance hyperpolarization.

[0042] The SABRE hyperpolarization automation device has the following specific structure: it includes an automatic sample preparation unit, an automatic bubbling unit, and a rapid solution transfer unit. The total equipment of each unit includes a sample bottle 1, an injection pump 2, a PEEK tube 3, a switching valve 4, a magnetic shielding cylinder 5, a three-way valve 6, an NMR tube 7, an NMR tube adapter 7a, an NMR instrument 8, an outlet 9, a cabinet, a regulated power supply 11, a magnetic shielding instrument 12, a PC host computer 13, a PCB board 14, a secondary hydrogen cylinder 15, a pneumatic hose 16, a mass flow controller 17, a first solenoid valve 18, a second solenoid valve 18a, a third solenoid valve 18b, a back pressure valve 19, a waste liquid bottle 20, a solenoid 21, a pressure-resistant bottle 22, a pressure-resistant bottle stopper 22a, and a glass capillary tube 23.

[0043] The automatic sample preparation unit consists of multiple injection pumps 2 and a back pressure valve 19. The injection pump 2 is equipped with a switching valve 4, and the injection pump 2 and the switching valve 4 are integrated into one unit. A PEEK pipe 3 is connected to the switching valve 4, and the switching valve 4 can be connected to the pressure bottle 22 through the PEEK pipe 3.

[0044] The automatic bubbling unit consists of a secondary hydrogen cylinder 15, a magnetic shielding cylinder 5, a second solenoid valve 18a, and a mass flow controller 17. The secondary hydrogen cylinder 15 is connected to the mass flow controller 17 via a pneumatic hose 16. The magnetic shielding cylinder 5 contains a solenoid tube 21 and a pressure-resistant bottle 22, with the solenoid tube 21 enclosing the pressure-resistant bottle 22. The pressure-resistant bottle 22 is connected to a switching valve 4, a first solenoid valve 18, a three-way valve 6, and a back pressure valve 19. The switching valve 4 is connected to the pressure-resistant bottle 22 via a PEEK pipe 3, and the first solenoid valve 18 is connected to the pressure-resistant bottle 22 via the pneumatic hose 16.

[0045] The three-way valve 6 is provided with a left port, a right port, and a lower port. The lower port of the three-way valve 6 is connected to the waste liquid bottle 20 through a PEEK tube 3, the left port of the three-way valve 6 is connected to the pressure-resistant bottle 22 through a PEEK tube 3, and the right port of the three-way valve 6 is connected to the nuclear magnetic resonance tube adapter 7a through a PEEK tube 3.

[0046] The back pressure valve 19 is provided with an air inlet and an air outlet. The air inlet of the back pressure valve 19 is connected to the pressure-resistant bottle 22 via a pneumatic hose 16, and the air outlet of the back pressure valve 19 is connected to the air outlet 9 via a pneumatic hose 16.

[0047] The NMR tube adapter 7a has three connection ports on its upper part: a left port, a middle port, and a right port. The left port of the NMR tube adapter 7a is connected to the second solenoid valve 18a via a pneumatic hose 16; the middle port is connected to the three-way valve 6 via a PEEK tube 3; and the right port is connected to the third solenoid valve 18b via a pneumatic hose 16. The lower part of the NMR tube adapter 7a is connected to the NMR tube 7, which is placed inside the NMR spectrometer 8 and contains a glass capillary tube 23.

[0048] The switching valve 4 is equipped with 6 valve ports. One valve port is connected to the pressure-resistant bottle 22 through the PEEK tube 3, and the remaining 5 valve ports are connected to different sample bottles 1 through the PEEK tube 3 respectively. This allows the syringe pump 2 to draw sample solutions from multiple sample bottles 1 and inject them into the pressure-resistant bottle 22 for mixing and sample preparation, thereby improving the efficiency of the syringe pump 2. The sample solutions contained in the different sample bottles 1 are substrate, catalyst and washing solution, respectively.

[0049] The solenoid 21 is controlled by the magnetic shielding device 12. The magnetic shielding device 12 controls the current of the solenoid 21, thereby generating a low magnetic field from nanotesla to millitalas in the solenoid 21, which in turn provides polarization transfer field conditions for the pressure-resistant bottle 22.

[0050] The syringe pump 2, first solenoid valve 18, second solenoid valve 18a, third solenoid valve 18b, three-way valve 6, magnetic shielding device 12, and NMR device 8 are all controlled by an integrated control system. This allows the system units to work collaboratively, improving operational efficiency, eliminating system redundancy, reducing maintenance costs, and minimizing damage caused by external interference. The integrated control system includes a PCB board 14 and a PC host computer 13, which communicate via a serial port. The PCB board 14 is electrically connected to the first solenoid valve 18, second solenoid valve 18a, third solenoid valve 18b, and three-way valve 6, respectively. The PC host computer 13 is electrically connected to the syringe pump 2, NMR device 8, mass flow controller 17, back pressure valve 19, and magnetic shielding device 12, respectively.

[0051] Sample vial 1 and pressure-resistant bottle stopper 22a are both sealed, so that the device does not exchange gases with the outside world, allowing for completely inert conditions and preventing the sample solution from oxidizing and deteriorating upon contact with air.

[0052] The mass flow controller 17 is connected to the first solenoid valve 18 and the second solenoid valve 18a. The mass flow controller 17 is used to control the flow rate of the secondary hydrogen bottle 15, which outputs secondary hydrogen. The back pressure valve 19 is used to control the pressure inside the pressure-resistant bottle 22. By setting the flow rate of the mass flow controller 17 and the pressure of the back pressure valve 19, the secondary hydrogen can be continuously bubbled in the pressure-resistant bottle 22 containing the sample solution, fully dissolving the secondary hydrogen into the sample solution and causing polarization transfer.

[0053] The glass capillary 23 can function as a foreign object without affecting the detection of the NMR instrument 8. A lower connection port is provided below the NMR tube adapter 7a. The glass capillary 23 and the lower connection port of the NMR tube adapter 7a are bonded together with epoxy resin, so that the sample solution in the NMR tube 7 can flow back to the pressure bottle 22 through the glass capillary 23, and polarization transfer occurs again. This realizes the SABRE hyperpolarization magnetic field cycle experiment, which greatly improves the polarization transfer efficiency.

[0054] The syringe pump 2, the first solenoid valve 18, the second solenoid valve 18a, the third solenoid valve 18b, the three-way valve 6, the PCB board 14, and the back pressure valve 19 are all powered by the regulated power supply 11, which ensures that the entire device has a stable voltage and current, guaranteeing the normal operation of the equipment.

[0055] Sample vial 1, syringe pump 2, magnetic shielding cylinder 5, first solenoid valve 18, second solenoid valve 18a, third solenoid valve 18b, three-way valve 6, nuclear magnetic resonance spectrometer 8, back pressure valve 19, PCB board 14, PC host computer 13, magnetic shielding device 12, and voltage regulator 11 are all placed in anti-static cabinet 10, thereby protecting the entire device from static electricity.

[0056] Working Principle: When using this SABRE hyperpolarization automated device, firstly, as shown in 1-7, open the first solenoid valve 18, the second solenoid valve 18a, and the third solenoid valve 18b to purge air from the device by introducing secondary hydrogen, preventing the sample solution from oxidizing and deteriorating upon contact with air. Then, close the first solenoid valve 18, the second solenoid valve 18a, and the third solenoid valve 18b. Multiple injection pumps 2 simultaneously draw sample solution from sample vials 1 and inject it into pressure-resistant bottles 22. The back pressure valve 19 automatically adjusts its parameters, and the three-way valve 6 is switched to connect the NMR tube 7 to the pressure-resistant bottle 22. Then, open the second solenoid valve 18a, the second solenoid valve 18b, and the third solenoid valve 18b. Solenoid valve 18a is used to introduce secondary hydrogen into pressure-resistant bottle 22 to bubble the sample solution, initiating polarization transfer. After bubbling for a certain period, the second solenoid valve 18a is closed, and the third solenoid valve 18b is opened. At this point, the pressure inside pressure-resistant bottle 22 is greater than the pressure inside NMR tube 7, and the sample solution is forced from pressure-resistant bottle 22 into NMR tube 7. The three-way valve 6 is switched to connect NMR tube 7 to waste bottle 20, and NMR instrument 8 automatically samples. After sampling, the third solenoid valve 18b is closed, the three-way valve 6 is switched to connect NMR tube 7 to pressure-resistant bottle 22, and the second solenoid valve 18a is opened to introduce secondary hydrogen to bubble the sample solution. The sample solution is pushed back into the pressure-resistant bottle 22, and secondary hydrogen is continuously introduced to bubble the sample solution, causing polarization transfer. After bubbling for a certain period of time, the second solenoid valve 18a is closed, and the third solenoid valve 18b is opened, allowing the sample solution to be pushed from the pressure-resistant bottle 22 into the NMR tube 7. The three-way valve 6 is switched to connect the NMR tube 7 to the waste liquid bottle 20, and the NMR instrument 8 automatically samples. The above steps are repeated to acquire multiple NMR spectra, realizing the SABRE hyperpolarization magnetic field cycle experiment. After the experiment, the three-way valve 6 is switched to connect the NMR tube 7 to the waste liquid bottle 20, and the second solenoid valve 18a is opened to introduce secondary hydrogen. The secondary hydrogen pump pressurizes the sample solution into the waste bottle 20. Then, the switching valve 4 is turned to the valve port connecting the cleaning solution. The syringe pump 2 draws the cleaning solution from the sample bottle 1 and injects it into the pressure-resistant bottle 22. The three-way valve 6 is turned to connect the NMR tube 7 to the pressure-resistant bottle 22. The first solenoid valve 18 is opened, and the secondary hydrogen pump is introduced to pressurize the cleaning solution into the NMR tube 7. The first solenoid valve 18 is closed, and the three-way valve 6 is turned to connect the NMR tube 7 to the waste bottle 20. The second solenoid valve 18a is opened, and the secondary hydrogen pump is introduced to pressurize the cleaning solution into the waste bottle 20. The automatic cleaning of the NMR tube 7 is completed, and the next sample solution can be tested.

[0057] The contents not described in detail in this invention are existing technologies known to those skilled in the art.

[0058] The above description is merely a preferred embodiment of the present invention, but the design concept of the present invention is not limited thereto. Any non-substantial modifications made to the present invention by those skilled in the art within the scope of the technology disclosed in the present invention using this concept shall be deemed as an infringement of the protection scope of the present invention.

Claims

1. An automated device for SABRE hyperpolarization, characterized in that: Includes an automatic sample preparation unit, an automatic bubbling unit, and a rapid solution transfer unit; The automatic sample preparation unit includes multiple injection pumps and a back pressure valve. The injection pump includes a switching valve, and a PEEK tube is connected to the switching valve. The automatic bubbling unit includes a secondary hydrogen cylinder, a magnetic shielding cylinder, and a second solenoid valve. The secondary hydrogen cylinder is connected to a mass flow controller. The magnetic shielding cylinder contains a solenoid and a pressure-resistant bottle. The solenoid encloses the pressure-resistant bottle. The rapid solution transfer unit consists of a pressure-resistant bottle, an NMR tube, an NMR tube adapter, a first solenoid valve, a second solenoid valve, a third solenoid valve, and a three-way valve; the NMR tube is placed inside the NMR instrument, and the lower part of the NMR tube adapter is connected to the NMR instrument; the NMR tube contains a glass capillary tube. The pressure-resistant bottle is connected to the switching valve, the first solenoid valve, the three-way valve, and the back pressure valve respectively; the three-way valve includes a left port, a right port, and a lower port, the left port is connected to the pressure-resistant bottle, the right port is connected to the nuclear magnetic tube adapter, and the lower port is connected to a waste liquid bottle; The back pressure valve includes an air inlet and an air outlet. The air inlet is connected to a pressure-resistant bottle, and the air outlet is connected to an outlet end. The nuclear magnetic tube adapter has three connecting ports on its top, which are a left port, a middle port, and a right port. The left port is connected to a second solenoid valve, the middle port is connected to a three-way valve, and the right port is connected to a third solenoid valve.

2. The SABRE hyperpolarization automation device according to claim 1, characterized in that: The injection pump and the switching valve are integrated into one unit.

3. The automated device for SABRE hyperpolarization according to claim 2, characterized in that: The switching valve is provided with multiple valve ports, one of which is connected to the pressure-resistant bottle, and the remaining valve ports are used to connect to different sample bottles respectively. The sample solutions contained in the different sample vials are substrate, catalyst, and washing solution, respectively.

4. The SABRE hyperpolarization automation device according to claim 3, characterized in that: The solenoid is externally connected to a magnetic shielding device, and the solenoid is controlled by the magnetic shielding device.

5. The SABRE hyperpolarization automation device according to claim 4, characterized in that: The automation device also includes an integrated control system, which includes a PCB board and a PC host computer; the PCB board and the PC host computer communicate via a serial port. The PCB board is electrically connected to the first solenoid valve, the second solenoid valve, the third solenoid valve, and the three-way valve, respectively. The PC host computer is electrically connected to the injection pump, the MRI machine, the mass flow controller, the back pressure valve, and the magnetic shielding device, respectively.

6. The SABRE hyperpolarization automation device according to claim 1, characterized in that: The mass flow controller is connected to the first solenoid valve and the second solenoid valve. The mass flow controller is used to control the flow rate of the secondary hydrogen cylinder, and the secondary hydrogen cylinder outputs secondary hydrogen.

7. The SABRE hyperpolarization automation device according to claim 1, characterized in that: The back pressure valve is used to control the pressure inside the pressure-resistant bottle.

8. The SABRE hyperpolarization automation device according to claim 1, characterized in that: The NMR tube adapter has a lower connection port, which is bonded to the glass capillary tube with epoxy resin.

9. The SABRE hyperpolarization automation device according to claim 5, characterized in that: The first solenoid valve, the second solenoid valve, the third solenoid valve, the three-way valve, the PCB board, and the back pressure valve are all powered by a regulated power supply.

10. The SABRE hyperpolarization automation device according to claim 9, characterized in that: The sample vials, syringe pump, magnetic shielding cylinder, first solenoid valve, second solenoid valve, third solenoid valve, three-way valve, NMR spectrometer, back pressure valve, PCB board, PC host computer, magnetic shielding instrument, and regulated power supply are all placed in an anti-static cabinet.

Citation Information

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