In-situ intermediate detection mass spectrometry device

Abstract

The utility model discloses an in-situ intermediate detection mass spectrometry device, which comprises a high-resolution time-of-flight mass spectrometer, an automatic shunting dilution transmission device and an in-situ reaction mechanism, and the in-situ reaction mechanism comprises a reactor, a liquid injection mechanism and a heating magnetic stirrer. A six-way valve of the automatic shunting, diluting and conveying device is respectively communicated with a high-resolution time-of-flight mass spectrometer and a reactor, and the reactor is arranged at the top of a heating magnetic stirrer; the L-shaped plate can be unlocked by rotating the positioning block by a certain angle, and at the moment, the L-shaped plate can be rotated downwards to realize synchronous unlocking operation of the two injectors, so that the two injectors can be conveniently disassembled at the same time; when the injectors are fixed again, the L-shaped plate is rotated upwards to the maximum limit, and the L-shaped plate is positioned by using the connecting piece, so that the synchronous positioning operation of the two injectors can be completed, the disassembly and assembly steps of the injectors can be reduced, and the detection efficiency of the in-situ intermediate can be improved.

Description

Technical Field

[0001] The utility model relates to the technical field of in-situ mass spectrometry analysis, in particular to an in-situ intermediate detection mass spectrometry analysis device. Background Art

[0002] High-resolution time-of-flight mass spectrometers are mainly used to determine the precise relative molecular mass of compounds, and then the molecular formula of the compounds can be inferred by combining the abundance ratio information. The types of compounds that can be analyzed by this instrument are very large, and it has become an indispensable detection tool in research fields such as synthetic chemistry, coordination chemistry, metal organic, bioinorganic, natural products, drug development, pharmacokinetics, combinatorial chemistry, and biomacromolecule (peptide, protein) chemistry. In recent years, the use of high-resolution time-of-flight mass spectrometers for chemical reaction mechanism research has become a new direction for the application of this instrument. The research content of chemical reaction mechanism includes the detection of reactants, intermediates and products and their changes over time, the detection and structural analysis of intermediates, and the connection between intermediates and reaction mechanisms. Among them, the capture of chemical reaction intermediates and unstable intermediates can provide key hints for the expansion of research ideas.

[0003] The existing patent document with announcement number CN210401314U discloses a quasi-in-situ reaction monitoring system of a high-resolution time-of-flight mass spectrometer. The reactor, constant flow pump, stop valve, six-way valve, diverter and high-resolution time-of-flight mass spectrometer are connected by PEEK tubes, so that the reaction liquid to be tested in the in-situ reactor can be quickly diverted, diluted and transmitted to the mass spectrometer without contact with air, thereby completing the quasi-in-situ reaction monitoring of the chemical reaction, completely solving the problem that chemical reaction intermediates and unstable intermediates are difficult to detect under conventional chemical detection methods of high-resolution time-of-flight mass spectrometers, and further expanding the function of high-resolution time-of-flight mass spectrometers in reaction mechanism research.

[0004] Although the above-mentioned high-resolution time-of-flight mass spectrometer quasi-in-situ reaction monitoring system can solve the corresponding technical problems, it uses two injection pumps to control two syringes to inject catalyst and reaction substrate solutions into the reactor respectively, resulting in the need to fix and disassemble the two syringes separately for each detection, which is cumbersome to operate. Therefore, we propose an in-situ intermediate detection mass spectrometry analysis device. Utility Model Content

[0005] The utility model aims to provide an in-situ intermediate detection mass spectrometry analysis device, which is used to solve the problems raised by the above-mentioned background technology.

[0006] In order to achieve the above-mentioned purpose, the main technical solutions adopted by the utility model include:

[0007] An in-situ intermediate detection mass spectrometry analysis device, comprising:

[0008] A high-resolution time-of-flight mass spectrometer, an automatic diversion dilution and transmission device, and an in-situ reaction mechanism, wherein the in-situ reaction mechanism comprises a reactor, a liquid injection mechanism, and a heated magnetic stirrer, wherein the high-resolution time-of-flight mass spectrometer and the reactor are respectively connected to a six-way valve of the automatic diversion dilution and transmission device, and the reactor is arranged on the top of the heated magnetic stirrer;

[0009] The injection mechanism comprises a syringe pump body, a syringe connected to the reactor is provided at the lower part of one side of the syringe pump body, a pusher for clamping the syringe piston handle and driving the piston to move in the liquid discharge direction is mounted on the syringe pump body, two syringes are arranged on the syringe pump body in an upper and lower manner, and the two syringes are used to contain the catalyst solution and the reaction substrate solution respectively, and a fixing assembly for fixing the syringe barrel is provided on the syringe pump body;

[0010] Wherein, the fixing assembly comprises a clamping member which is arranged on the injection pump body and is used for synchronously positioning the two syringes, and the clamping member is provided with an adjusting member which is used for respectively positioning the two syringes.

[0011] Furthermore, the clamp comprises a boss and a convex plate integrally formed on the injection pump body, a gap is formed between the boss and the convex plate for limiting the movement of the convex edge of the syringe barrel, the bottom of the boss away from the injection pump body is rotatably connected with an L-shaped plate, a connecting piece is provided between the L-shaped plate and the injection pump body, and the adjusting piece is provided on the L-shaped plate.

[0012] Furthermore, the convex seat and the convex plate are both provided with an arc-shaped groove for placing the syringe on one side away from the injection pump body.

[0013] Furthermore, the connecting member includes a baffle integrally formed on the injection pump body, a side of the baffle away from the boss is rotatably connected to a positioning block, and an upper portion of the L-shaped plate surface is provided with a through hole for the positioning block to pass through.

[0014] Furthermore, the side of the positioning block facing the baffle is rotationally connected to the surface of the baffle via a damping shaft.

[0015] Furthermore, the positioning block and the through hole are both rectangular structures.

[0016] Furthermore, the adjusting member includes a screw sleeve fixedly passed through the L-shaped plate, the inner cavity of the screw sleeve is threadedly connected with a stud, one end of the stud passes through the inner cavity of the L-shaped plate and is rotatably connected to a clamp for cooperating with the arc groove to clamp the syringe, and the clamp has an arc-shaped structure.

[0017] Furthermore, one end of the stud away from the clamping plate is fixedly connected with a knob.

[0018] Furthermore, one side of the two clamping plates facing each other is integrally formed with an L-shaped block, the inner wall surface of the L-shaped plate is fixedly connected with a guide block, and the inner wall surface of the L-shaped block is slidably connected to the surface of the guide block.

[0019] Furthermore, the clamping plate and the inner wall surface of the arc-shaped groove are both glued with rubber pads, and the inner wall surface of the rubber pad is in contact with the outer surface of the syringe barrel.

[0020] The utility model has at least the following beneficial effects:

[0021] The beneficial effect of the utility model of the present application is that the L-shaped plate can be unlocked by rotating the positioning block at a certain angle, and the L-shaped plate can be rotated downward at this time to achieve the synchronous unlocking operation of the two syringes, thereby facilitating the simultaneous removal of the two syringes; when fixing the syringes again, it is only necessary to rotate the L-shaped plate upward to the maximum limit, and use the connecting piece to position the L-shaped plate to complete the synchronous positioning operation of the two syringes, thereby helping to reduce the steps of disassembly and assembly of the syringes, and helping to improve the detection efficiency of in-situ intermediates; by turning the knob, the clamping plate can be driven to move in the direction of the protruding seat, and syringes of different sizes can be clamped, thereby helping to improve the scope of application of the in-situ intermediate detection mass spectrometry analysis device. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is a schematic structural diagram of an in-situ intermediate detection mass spectrometry analysis device of the utility model;

[0023] Figure 2 A three-dimensional schematic diagram of the structure of the liquid injection mechanism of an in-situ intermediate detection mass spectrometry analysis device of the utility model Figure 1 ;

[0024] Figure 3 A three-dimensional schematic diagram of the structure of the liquid injection mechanism of an in-situ intermediate detection mass spectrometry analysis device of the utility model Figure 2 ;

[0025] Figure 4 It is a three-dimensional schematic diagram of the connection structure between an L-shaped plate and an adjusting member of an in-situ intermediate detection mass spectrometry analysis device of the utility model.

[0026] In the figure: 1. high-resolution time-of-flight mass spectrometer; 2. automatic diversion dilution transmission device; 3. reactor; 4. injection mechanism; 41. injection pump body; 42. syringe; 43. pusher; 44. fixing assembly; 441. clamp; 4411. convex seat; 4412. convex plate; 4413. L-shaped plate; 4414. baffle; 4415. positioning block; 4416. through hole; 442. adjusting member; 4421. screw sleeve; 4422. stud; 4423. clamp; 4424. knob; 4425. U-shaped block; 4426. guide block; 45. rubber pad; 5. heating magnetic stirrer. DETAILED DESCRIPTION

[0027] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0028] See also Figure 1-Figure 4 The embodiment of the utility model provides an in-situ intermediate detection mass spectrometry analysis device, comprising: a high-resolution time-of-flight mass spectrometer 1, an automatic diversion dilution transmission device 2 and an in-situ reaction mechanism, the in-situ reaction mechanism comprising a reactor 3, an injection mechanism 4 and a heating magnetic stirrer 5, the high-resolution time-of-flight mass spectrometer 1 and the reactor 3 are respectively connected to the six-way valve of the automatic diversion dilution transmission device 2, the reactor 3 is arranged on the top of the heating magnetic stirrer 5; the injection mechanism 4 comprises an injection pump body 41, and a syringe 42 connected to the reactor 3 is provided at the lower part of one side of the injection pump body 41, and the injection pump body 41 is provided with a syringe 42 connected to the reactor 3. The pump body 41 is equipped with a pusher 43 for clamping the piston handle of the syringe 42 and driving the piston to move in the liquid discharge direction. Two syringes 42 are arranged on the injection pump body 41 in an upper and lower position, and the two syringes 42 are respectively used to contain the catalyst solution and the reaction substrate solution. The injection pump body 41 is provided with a fixing component 44 for fixing the barrel of the syringe 42; the fixing component 44 includes a clamping component 441 arranged on the injection pump body 41 and used for synchronously positioning the two syringes 42, and the clamping component 441 is provided with an adjusting component 442 for separately positioning the two syringes 42.

[0029] Among them, the clamp 441 includes a boss 4411 and a convex plate 4412 integrally formed on the injection pump body 41, and a gap is formed between the boss 4411 and the convex plate 4412 for limiting the movement of the convex edge of the syringe 42 barrel. The bottom of the boss 4411 away from the injection pump body 41 is rotatably connected with an L-shaped plate 4413, and a connecting piece is provided between the L-shaped plate 4413 and the injection pump body 41. The adjusting piece 442 is provided on the L-shaped plate 4413. By rotating the L-shaped plate 4413, the two adjusting pieces 442 can be driven to rotate synchronously, so as to realize the synchronous positioning and unlocking operations of the two syringes 42.

[0030] The sides of the convex seat 4411 and the convex plate 4412 away from the injection pump body 41 are both provided with arc grooves for placing the syringe 42 , so that the convex seat 4411 and the convex plate 4412 can fit the barrel of the syringe 42 more closely.

[0031] Among them, the connecting piece includes a baffle 4414 integrally formed on the injection pump body 41, and the baffle 4414 is rotatably connected with a positioning block 4415 on the side away from the protrusion 4411. A through hole 4416 is provided on the upper part of the surface of the L-shaped plate 4413 for the positioning block 4415 to pass through. The connecting piece can realize the quick connection operation of the L-shaped plate 4413 and the injection pump body 41, which facilitates the locking and unlocking operations of the L-shaped plate 4413.

[0032] Among them, the side of the positioning block 4415 facing the baffle 4414 is rotatably connected to the surface of the baffle 4414 through the damping shaft. The damping shaft can maintain the torsion angle fixing function to ensure that the positioning block 4415 does not loosen after rotation, thereby ensuring the stability of the positioning block 4415 when locking the L-shaped plate 4413.

[0033] The positioning block 4415 and the through hole 4416 are both rectangular structures, so that the positioning block 4415 can be staggered with the through hole 4416 after the damping shaft rotates a certain angle to achieve the locking operation of the L-shaped plate 4413.

[0034] Among them, the adjusting member 442 includes a screw sleeve 4421 fixedly passed through the L-shaped plate 4413, the inner cavity of the screw sleeve 4421 is threadedly connected with a stud 4422, one end of the stud 4422 passes through the inner cavity of the L-shaped plate 4413 and is rotatably connected through a bearing to a clamp 4423 for clamping the syringe 42 in cooperation with the arc groove, the clamp 4423 has an arc-shaped structure, and by rotating the stud 4422, the clamp 4423 can be driven to move horizontally along the axial direction of the stud 4422 under the action of the thread, and then the distance between the clamp 4423 and the boss 4411 can be adjusted according to the outer diameter of the barrel of the syringe 42, so as to realize the positioning of syringes 42 of different sizes.

[0035] Among them, one end of the stud 4422 away from the clamping plate 4423 is fixedly connected with a knob 4424, which can increase the force area between the hand and the stud 4422 and facilitate the rotation of the stud 4422.

[0036] Among them, the two opposite sides of the two splints 4423 are integrally formed with a L-shaped block 4425, and the inner wall surface of the L-shaped plate 4413 is horizontally fixedly connected with a guide block 4426. The inner wall surface of the L-shaped block 4425 is slidably connected to the surface of the guide block 4426. When the stud 4422 drives the splint 4423 to move horizontally, the L-shaped block 4425 and the guide block 4426 can limit the splint 4423, thereby enabling the splint 4423 to stably move horizontally along the axis direction of the stud 4422.

[0037] Among them, the clamping plate 4423 and the inner wall surface of the arc groove are glued with rubber pads 45, and the inner wall surface of the rubber pads 45 is in contact with the outer surface of the barrel of the syringe 42. The rubber pads 45 can increase the friction between the syringe 42 and the clamping plate 4423, and the syringe 42 and the arc groove, which helps to improve the stability of the syringe 42 when it is fixed, and can also avoid the phenomenon that the clamping force applied by the clamping plate 4423 is too large and causes wear on the surface of the syringe 42.

[0038] The working principle of the utility model is as follows: two syringes 42 respectively filled with catalyst solution and reaction substrate solution are placed in the arc groove, and the piston handle of the syringe 42 is clamped on the pusher 43, and the convex edge of the syringe 42 barrel is clamped in the gap between the convex seat 4411 and the convex plate 4412, and then the L-shaped plate 4413 is rotated upward, so that the L-shaped plate 4413 drives the adjustment member 442 to rotate synchronously, until the upper part of the inner wall surface of the L-shaped plate 4413 contacts one side of the baffle 4414, at this time, the positioning block 4415 passes through one side of the L-shaped plate 4413 through the through hole 4416, and the positioning block 4415 is rotated so that the positioning block 4415 and the through hole 4416 are staggered. , the L-shaped plate 4413 can be positioned, thereby completing the synchronous positioning operation of the two syringes 42; on the contrary, the above steps can be reversed to complete the synchronous unlocking operation of the two syringes 42; by turning the knob 4424, the knob 4424 drives the stud 4422 to rotate in the inner cavity of the screw sleeve 4421, and under the action of the thread, the stud 4422 drives the clamping plate 4423 to move along the axial direction of the stud 4422, and the clamping plate 4423 drives the U-shaped block 4425 to slide on the surface of the guide block 4426 until the rubber pad 45 on the inner wall of the clamping plate 4423 is tightly against the barrel of the syringe 42, so that syringes 42 of different sizes can be fixed.

[0039] Parts not involved in the present invention are the same as the prior art or can be implemented by the prior art. Although the embodiments of the present invention have been shown and described, it is understood by those skilled in the art that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of the present invention, and the scope of the present invention is defined by the attached claims and their equivalents.

Claims

1. An in-situ intermediate detection mass spectrometry analysis device, characterized in that: include: A high-resolution time-of-flight mass spectrometer (1), an automatic diversion dilution transmission device (2), and an in-situ reaction mechanism, wherein the in-situ reaction mechanism comprises a reactor (3), a liquid injection mechanism (4), and a heating magnetic stirrer (5), wherein the high-resolution time-of-flight mass spectrometer (1) and the reactor (3) are respectively connected to a six-way valve of the automatic diversion dilution transmission device (2), and the reactor (3) is arranged on the top of the heating magnetic stirrer (5); The injection mechanism (4) comprises a syringe pump body (41), a syringe (42) connected to the reactor (3) is provided at the lower part of one side of the syringe pump body (41), a pusher (43) for clamping the piston handle of the syringe (42) and driving the piston to move in the liquid discharge direction is mounted on the syringe pump body (41), two syringes (42) are arranged on the syringe pump body (41) in an upper and lower manner, and the two syringes (42) are used to contain a catalyst solution and a reaction substrate solution respectively, and a fixing component (44) for fixing the barrel of the syringe (42) is provided on the syringe pump body (41); The fixing assembly (44) comprises a clamp (441) provided on the injection pump body (41) and used for synchronously positioning the two syringes (42); the clamp (441) is provided with an adjusting member (442) for respectively positioning the two syringes (42).

2. The in-situ intermediate detection mass spectrometry analysis device according to claim 1, characterized in that: The clamp (441) includes a convex seat (4411) and a convex plate (4412) integrally formed on the injection pump body (41); a gap is formed between the convex seat (4411) and the convex plate (4412) for limiting the movement of the convex edge of the syringe (42) barrel; the bottom of the convex seat (4411) away from the injection pump body (41) is rotatably connected to an L-shaped plate (4413); a connecting piece is provided between the L-shaped plate (4413) and the injection pump body (41); and the adjusting piece (442) is provided on the L-shaped plate (4413).

3. The in-situ intermediate detection mass spectrometry analysis device according to claim 2, characterized in that: The convex seat (4411) and the convex plate (4412) are both provided with an arc-shaped groove for placing the syringe (42) on the side away from the injection pump body (41).

4. The in-situ intermediate detection mass spectrometry analysis device according to claim 2, characterized in that: The connecting member comprises a baffle (4414) integrally formed on the injection pump body (41), and a positioning block (4415) is rotatably connected to the side of the baffle (4414) away from the convex seat (4411), and a through hole (4416) for the positioning block (4415) to pass through is opened on the upper part of the surface of the L-shaped plate (4413).

5. The in-situ intermediate detection mass spectrometry analysis device according to claim 4, characterized in that: The side of the positioning block (4415) facing the baffle (4414) is rotationally connected to the surface of the baffle (4414) via a damping shaft.

6. The in-situ intermediate detection mass spectrometry analysis device according to claim 5, characterized in that: The positioning block (4415) and the through hole (4416) are both rectangular structures.

7. The in-situ intermediate detection mass spectrometry analysis device according to claim 3, characterized in that: The adjusting member (442) comprises a screw sleeve (4421) fixedly passed through the L-shaped plate (4413); the inner cavity of the screw sleeve (4421) is threadedly connected with a stud (4422); one end of the stud (4422) passes through the inner cavity of the L-shaped plate (4413) and is rotatably connected with a clamping plate (4423) for cooperating with the arc groove to clamp the syringe (42); the clamping plate (4423) is an arc-shaped structure.

8. The in-situ intermediate detection mass spectrometry analysis device according to claim 7, characterized in that: One end of the stud (4422) away from the clamping plate (4423) is fixedly connected to a knob (4424).

9. The in-situ intermediate detection mass spectrometry analysis device according to claim 7, characterized in that: A U-shaped block (4425) is integrally formed on one side opposite to the two clamping plates (4423); a guide block (4426) is fixedly connected to the inner wall surface of the L-shaped plate (4413); and the inner wall surface of the U-shaped block (4425) is slidably connected to the surface of the guide block (4426).

10. The in-situ intermediate detection mass spectrometry analysis device according to claim 7, characterized in that: The clamping plate (4423) and the inner wall surface of the arc-shaped groove are both glued with a rubber pad (45), and the inner wall surface of the rubber pad (45) is in contact with the outer surface of the barrel of the syringe (42).

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