Liquid-phase tandem mass spectrometry online solid-phase extraction and purification device for detecting vitamin K2

Abstract

The utility model relates to a liquid phase tandem mass spectrum on-line solid phase extraction and purification device for detecting vitamin K2, which comprises a bottom plate, a rotary table and a solid phase extraction column, and is technically characterized in that a horizontal support plate is suspended above the rotary table; a sample injection pipe, a first pressurization structure, an elution solvent injection pipe, a second pressurization structure, a cleaning liquid injection pipe and a third pressurization structure are arranged on the horizontal supporting plate, an output pipeline extending to the outer side of the rotary table is arranged on the side face of the bottom of the solid-phase extraction column, and a waste liquid collecting tank and a cleaning collecting tank are arranged at the positions, outside the rotary table, of the bottom plate. A horizontal conveying belt is arranged on the side of the rotary table, an eluent collecting bottle is arranged on the horizontal conveying belt, a cantilever support is arranged on the side of the horizontal conveying belt, a purging pipe assembly is arranged on the cantilever support, and the lower end of a purging pipe of the purging pipe assembly points to the upper surface of the horizontal conveying belt. The device solves the problems of low working efficiency, easy pollution and sample loss caused by manual participation, and remarkably improves the working efficiency and the detection accuracy compared with the prior art.

Description

TECHNICAL FIELD

[0001] The utility model relates to medical detection device technical field, concretely relates to a vitamin K2 detects with liquid phase tandem mass spectrum online solid phase extraction purification device. BACKGROUND

[0002] Vitamin K2 is a kind of fat-soluble vitamin containing methylnaphthoquinone structure, mainly distributes in extrahepatic tissue, such as kidney, pancreas, bone, reproductive organ and blood vessel wall etc.Vitamin K2 is an important, essential vitamin of human body, and research shows that, in addition to basic coagulation function, vitamin K2 participates in the metabolism and regulation of bone and calcium in body, and has indispensable basic role in promoting and maintaining the health of human bone.Therefore, quantitative detection of the concentration of vitamin K2 in human serum has important clinical significance.

[0003] At present, liquid phase tandem mass spectrometer can be used to detect the content of vitamin K2 in human blood, and human blood sample needs to be pretreated before detection, to obtain liquid phase tandem mass spectrometry sample.Sample extraction usually needs to be subjected to organic solvent protein precipitation, liquid-liquid extraction or solid phase extraction, wherein, solid phase extraction refers to that different components in sample matrix are different in distribution system, so that target analyte is retained and eluted, while interfering substances in sample are selectively removed, to obtain target analyte suitable for mass spectrometry.When solid phase extraction technology is used, target substance is usually adsorbed by solid phase extraction column, and then eluted by elution solvent, and finally concentrated and sent to liquid phase tandem mass spectrometer, and the more manual operation steps required in the whole process, the lower the working efficiency of automatic online equipment is, and meanwhile, sample is easily contaminated and lost in manual transfer process. UTILITARY MODEL CONTENT

[0004] The utility model aims at providing a vitamin K2 detection liquid phase tandem mass spectrum online solid phase extraction purification device with reasonable structure and reliable use, to solve the problems of low working efficiency, easy contamination and sample loss caused by manual participation, compared with prior art, significantly improve working efficiency and detection accuracy.

[0005] The technical scheme of the utility model is:

[0006] The application discloses a liquid chromatography tandem mass spectrometry online solid phase extraction purification device for vitamin K2 detection, which comprises a base plate, a rotary table and six solid phase extraction columns uniformly arranged on the upper surface of the rotary table, and has the following technical points: a horizontal support plate is suspended above the rotary table, the horizontal support plate is provided with a sample injection tube corresponding to the first solid phase extraction column, a first pressurizing structure corresponding to the second solid phase extraction column, an elution solvent injection tube corresponding to the third solid phase extraction column, a second pressurizing structure corresponding to the fourth solid phase extraction column, a cleaning liquid injection tube corresponding to the fifth solid phase extraction column and a third pressurizing structure corresponding to the sixth solid phase extraction column, the bottom side of the solid phase extraction column is provided with an output pipeline extending to the outside of the rotary table, the base plate is provided with a waste liquid collecting groove and a cleaning collecting groove at the position outside the rotary table, a horizontal conveying belt is arranged on the side of the rotary table, a plurality of elution liquid collecting bottles are arranged on the horizontal conveying belt at intervals, the second pressurizing structure is adjacent to the horizontal conveying belt in the horizontal direction, a cantilever frame is arranged on the side of the horizontal conveying belt, a blowing pipe assembly is arranged on the cantilever frame, and the lower end of the blowing pipe of the blowing pipe assembly points to the upper surface of the horizontal conveying belt.

[0007] The first pressurizing structure, the second pressurizing structure and the third pressurizing structure of the liquid chromatography tandem mass spectrometry online solid phase extraction purification device for vitamin K2 detection are respectively formed by a longitudinal electric push rod, a gland arranged at the lower end of the telescopic part of the electric push rod, a groove arranged on the lower surface of the gland, a pressurizing passage communicated between the bottom surface of the groove and the side wall of the gland and a pressurizing pipeline arranged at the outer end of the pressurizing passage.

[0008] The bottom of the solid phase extraction column of the liquid chromatography tandem mass spectrometry online solid phase extraction purification device for vitamin K2 detection is provided with a metal positioning disc, the upper surface of the rotary table is provided with positioning grooves corresponding to the metal positioning discs, and the inner ring surface of the positioning grooves is provided with magnetic positioning rings matched with the metal positioning discs.

[0009] The bottom side of the elution liquid collecting bottle of the liquid chromatography tandem mass spectrometry online solid phase extraction purification device for vitamin K2 detection is fixed with a micro pump, and the outlet of the micro pump is provided with a liquid delivery pipe used for being connected with a liquid chromatography tandem mass spectrometer.

[0010] The waste liquid collecting groove of the liquid chromatography tandem mass spectrometry online solid phase extraction purification device for vitamin K2 detection is adjacent to the sample injection tube, the first pressurizing structure and the elution solvent injection tube in the horizontal direction, and the cleaning collecting groove is adjacent to the cleaning liquid injection tube and the third pressurizing structure in the horizontal direction.

[0011] The output pipeline of the bottom of the solid phase extraction column of the liquid chromatography tandem mass spectrometry online solid phase extraction purification device for vitamin K2 detection is sleeved with a wear-resistant ring in contact with the edge top surface of the waste liquid collecting groove and the cleaning collecting groove.

[0012] The above-mentioned online solid-phase extraction and purification device for vitamin K2 detection by liquid chromatography-tandem mass spectrometry has a support column between the center of the base plate and the horizontal support plate. The turntable is supported above the base plate by bearings, and the center of the turntable has a clearance hole corresponding to the support column. The outer circumferential surface of the turntable is provided with a gear ring structure, and the base plate is provided with a transmission gear that meshes with the gear ring structure.

[0013] The beneficial effects of this utility model are:

[0014] This invention integrates functions such as sample injection, target substance elution, eluent concentration and output, and cleaning of solid phase extraction column, enabling online sample purification before detection. It solves the problems of low work efficiency, easy contamination and sample loss caused by manual intervention, and significantly improves work efficiency and detection accuracy compared with existing technologies. Attached Figure Description

[0015] Figure 1 This is a schematic diagram of the structure of this utility model;

[0016] Figure 2 This is a top view of the present invention (excluding the horizontal support plate and its components).

[0017] In the diagram: 1. Horizontal support plate, 2. Sample injection tube, 3. Third pressurization structure, 4. Cleaning fluid injection tube, 5. Second pressurization structure, 6. Cap, 7. Solid phase extraction column, 8. Output pipeline, 9. Metal positioning plate, 10. Wear-resistant ring, 11. Waste liquid collection tank, 12. Base plate, 13. Magnetic positioning ring, 14. Turntable, 15. Support column, 16. Gear ring structure, 17. Horizontal conveyor belt, 18. Micro pump, 19. Eluent collection bottle, 20. Purge tube, 21. Cantilever frame, 22. Purge tube assembly, 23. Groove, 24. Transmission gear, 25. Cleaning collection tank. Detailed Implementation

[0018] The present invention will be described in detail with reference to the accompanying drawings.

[0019] like Figure 1 , Figure 2 As shown, the online solid-phase extraction purification device for vitamin K2 detection by liquid chromatography-tandem mass spectrometry includes a base plate 12, a turntable 14, and six solid-phase extraction columns 7 evenly arranged on the upper surface of the turntable 14, corresponding to six workstations.

[0020] Wherein: a horizontal support plate 1 is suspended above the turntable 14. In this embodiment, a support column 15 is provided between the center of the base plate 12 and the horizontal support plate 1. The turntable 14 is supported above the base plate 12 by bearings, and the center of the turntable 14 is provided with a clearance hole corresponding to the support column 15. A gear ring structure 16 is provided on the outer circumference of the turntable 14, and a transmission gear 24 that meshes with the gear ring structure 16 is provided on the base plate 12.

[0021] The horizontal support plate 1 is equipped with a sample injection tube 2 corresponding to the first solid-phase extraction column, a first pressurization structure corresponding to the second adjacent solid-phase extraction column, an elution solvent injection tube corresponding to the third adjacent solid-phase extraction column, a second pressurization structure 5 corresponding to the fourth adjacent solid-phase extraction column, a cleaning solution injection tube 4 corresponding to the fifth adjacent solid-phase extraction column, and a third pressurization structure 3 corresponding to the sixth adjacent solid-phase extraction column. In this embodiment, the first pressurization structure, the second pressurization structure 5, and the third pressurization structure 3 are respectively composed of a longitudinal electric push rod, a pressure cap 6 located at the lower end of the telescopic part of the electric push rod, a groove 23 located on the lower surface of the pressure cap 6, a pressurization passage connecting the bottom surface of the groove 23 and the side wall of the pressure cap 6, and a pressurization pipeline located at the outer end of the pressurization passage.

[0022] The solid-phase extraction column 7 has an output pipe 8 extending to the outside of the turntable 14 on its bottom side. The base plate 12 has a waste liquid collection tank 11 and a washing collection tank 25 located outside the turntable 14. In this embodiment, the waste liquid collection tank 11 is adjacent to the sample injection tube 2, the first pressurization structure, and the elution solvent injection tube in the horizontal direction. The washing collection tank 25 is adjacent to the washing liquid injection tube 4 and the third pressurization structure 3 in the horizontal direction. A horizontal conveyor belt 17 is provided on the side of the turntable 14. Multiple eluent collection bottles 19 are arranged at intervals on the horizontal conveyor belt 17. The second pressurization structure 5 is adjacent to the horizontal conveyor belt 17 in the horizontal direction. A cantilever frame 21 is provided on the side of the horizontal conveyor belt 17. A purge tube assembly 22 is provided on the cantilever frame 21. The lower end of the purge tube 20 of the purge tube assembly 22 points to the upper surface of the horizontal conveyor belt 17. In this embodiment, a micro pump 18 is fixed to the bottom side of the eluent collection bottle 19, and the outlet of the micro pump 18 is provided with a liquid delivery tube for connection to a liquid phase tandem mass spectrometer.

[0023] The solid-phase extraction column 7 is provided with a metal positioning disk 9 at its bottom. The upper surface of the turntable 14 is provided with positioning grooves that correspond one-to-one with the metal positioning disks 9. The inner ring surface of the positioning groove is provided with a magnetic positioning ring 13 that cooperates with the metal positioning disks 9. The output pipe 8 at the bottom of the solid-phase extraction column 7 is fitted with a wear-resistant ring 10 that contacts the top edge of the waste liquid collection tank 11 and the cleaning collection tank 25.

[0024] Working principle:

[0025] 1. The sample solution is quantitatively injected into the first solid-phase extraction column 7 through the sample injection tube 2. Driven by the turntable 14, it reaches the original position of the second solid-phase extraction column. The telescopic part of the electric push rod of the first pressurizing structure moves downward and drives the pressure cap to press against the upper end of the first solid-phase extraction column. The pressurizing device is activated, and pressure is applied to the solid-phase extraction column through the pressurizing pipeline and pressurizing passage. The sample solution moves downward, while the target substance is adsorbed in the packing of the solid-phase extraction column 7. Under the action of the first pressurizing structure, the rest of the sample solution, except for the target substance, is discharged into the waste liquid collection tank 11.

[0026] 2. Driven by the turntable 14, the first solid-phase extraction column 7 reaches the original position of the third solid-phase extraction column. The elution solvent injection tube injects the elution solvent into the solid-phase extraction column 7. Then, driven by the turntable 14, the first solid-phase extraction column 7 reaches the original position of the fourth solid-phase extraction column. The telescopic part of the electric push rod of the second pressurization structure 5 moves downward and drives the pressure cap 6 to press against the upper end of the first solid-phase extraction column 7. The pressurization device is activated, and pressure is applied to the solid-phase extraction column 7 through the pressurization pipeline and pressurization passage. The eluent carries the target substance out of the solid-phase extraction column 7 and falls into the eluent collection bottle 19 on the horizontal conveyor belt 17.

[0027] 3. The horizontal conveyor belt 17 carries the eluent collection bottle 19 forward to the purge tube 20 of the purge tube assembly 22. The purge tube 20 blows heated nitrogen into the eluent collection bottle 19 for concentration treatment, and finally pumps it to the liquid phase tandem mass spectrometer.

[0028] 4. The first solid-phase extraction column 7 is driven by the turntable 14 to the original position of the fifth solid-phase extraction column. The cleaning solution is injected into it by the cleaning solution injection tube 4. Then, driven by the turntable 14, it is driven to the original position of the sixth solid-phase extraction column. The telescopic part of the electric push rod of the third pressurizing structure 3 moves down and drives the pressure cap 6 to press against the upper end of the first solid-phase extraction column 7. The pressurizing device is started and pressure is applied to the solid-phase extraction column through the pressurizing pipeline and pressurizing passage. The cleaning liquid is pumped out of the solid-phase extraction column and falls into the cleaning collection tank 25.

[0029] The embodiments of this utility model have been described in detail above, but the content described is only a preferred embodiment of this utility model and should not be considered as limiting the scope of implementation of this utility model. All equivalent changes and improvements made within the scope of this utility model should still fall within the scope of this utility model.

Claims

1. A liquid chromatography tandem mass spectrometry online solid phase extraction purification device for vitamin K2 detection, comprising a base plate, a turntable, and six solid phase extraction columns uniformly arranged on the upper surface of the turntable, characterized in that: The horizontal support plate is provided above the rotating table, and the horizontal support plate is provided with a sample injection tube corresponding to the first solid-phase extraction column, a first pressurizing structure corresponding to the second adjacent solid-phase extraction column, an eluent injection tube corresponding to the third adjacent solid-phase extraction column, a second pressurizing structure corresponding to the fourth adjacent solid-phase extraction column, a cleaning liquid injection tube corresponding to the fifth adjacent solid-phase extraction column, and a third pressurizing structure corresponding to the sixth adjacent solid-phase extraction column.

2. The online solid phase extraction purification device for vitamin K2 detection by liquid chromatography tandem mass spectrometry according to claim 1, characterized in that: The first pressurizing structure, the second pressurizing structure and the third pressurizing structure are respectively provided with a longitudinal electric push rod, a gland provided at the lower end of the telescopic part of the electric push rod, a groove provided at the lower surface of the gland, a pressurizing passage communicated between the bottom surface of the groove and the side wall of the gland, and a pressurizing pipeline provided at the outer end of the pressurizing passage.

3. The online solid phase extraction purification device for vitamin K2 detection by liquid chromatography tandem mass spectrometry according to claim 1, characterized in that: The bottom of the solid-phase extraction column is provided with a metal positioning disc, and the upper surface of the rotating table is provided with a positioning groove corresponding to the metal positioning disc.

4. The online solid phase extraction purification device for vitamin K2 detection by liquid chromatography tandem mass spectrometry according to claim 1, characterized in that: The bottom side of the eluent collection bottle is fixed with a micro pump, and the outlet of the micro pump is provided with a liquid delivery pipe for connecting with a liquid chromatography tandem mass spectrometer.

5. The online solid phase extraction purification device for vitamin K2 detection by liquid chromatography tandem mass spectrometry according to claim 1, characterized in that: The waste liquid collection tank is adjacent to the sample injection tube, the first pressurizing structure and the eluent injection tube in the horizontal direction, and the cleaning collection tank is adjacent to the cleaning liquid injection tube and the third pressurizing structure in the horizontal direction.

6. The online solid phase extraction purification device for vitamin K2 detection by liquid chromatography tandem mass spectrometry according to claim 1, characterized in that: The output pipeline of the bottom of the solid-phase extraction column is sleeved with a wear-resistant ring in contact with the edge top surface of the waste liquid collection tank and the cleaning collection tank.

7. The online solid phase extraction purification device for vitamin K2 detection by liquid chromatography tandem mass spectrometry according to claim 1, characterized in that: The bottom plate and the horizontal support plate are provided with a support column between the centers, the rotating table is supported above the bottom plate by a bearing, and the center of the rotating table is provided with an avoiding hole corresponding to the support column, the outer peripheral surface of the rotating table is provided with a gear ring structure, and the bottom plate is provided with a transmission gear meshing with the gear ring structure.

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