A pre-treatment device based on fluoxastrobin and a detection method thereof

Abstract

The application relates to the technical field of product detection, and discloses a flutriafol-based early-stage treatment device and a detection method thereof, which comprises a liquid chromatograph body, a solvent chamber is arranged on the liquid chromatograph body, a solvent bottle is arranged on the inner side of the solvent chamber, the bottom end of the inner side of the solvent chamber is provided with a liquid inlet matched with the solvent bottle, liquid can be fed into the inner side of the solvent bottle through the inner hole on the inner side of the liquid inlet, a threaded groove is arranged at the lower end of the inner side of the solvent bottle, the inner side of the threaded groove is provided with a sealing assembly for sealing, the liquid chromatograph body is provided with a sealing assembly, a threaded groove, a threaded block and a top rod, when the solvent bottle is installed on the inner side of the solvent chamber, no additional hose is needed, the stable flow of the solvent into the inner side of the liquid chromatograph body can be ensured, and the solvent bottle and the liquid inlet interface can be tightly sealed through two sealing processes, the risk of solvent leakage caused by the loosening of the interface can be avoided, and the liquid chromatograph body can be stably provided with the mobile phase.

Description

Technical Field

[0001] This invention relates to the field of product testing technology, specifically to a pretreatment device and testing method based on fluopyram. Background Technology

[0002] Fluopyram is an important active fungicide for agricultural use, and its residue detection in agricultural products typically employs liquid chromatography-mass spectrometry (LC-MS). During the detection process, a stable supply of the mobile phase is crucial for ensuring the accuracy and repeatability of the analytical results. Current LC instruments are usually equipped with a solvent chamber, where solvent bottles are placed to store solvents such as methanol, acetonitrile, and water. The solvent is then led out through a tubing to a pump inside the LC instrument, thus enabling the preparation and delivery of the mobile phase.

[0003] Existing chromatograph solvent bottles have a top-outlet structure, where one end of a flexible tube is inserted into the top of the solvent bottle and the other end is connected to the inlet. In actual use, a certain length of flexible tube needs to be reserved for easy access to the solvent bottle. However, during operation, the flexible tube is easily pulled, bent, or squeezed, leading to improper installation or even tube detachment, affecting the stable supply of solvent. Secondly, the sealing structure between the solvent bottle and the inlet is relatively simple, usually relying only on the bottle cap or the flexible tube interface for sealing. Long-term use or under instrument vibration can easily cause solvent leakage, which not only wastes solvent but may also contaminate the solvent chamber and the inside of the instrument. To address this, we propose a pretreatment device and its detection method based on fluopyram. Summary of the Invention

[0004] The purpose of this invention is to provide a pretreatment device and detection method based on fluopyram to solve the problems mentioned in the background art.

[0005] To achieve the above objectives, the present invention provides the following technical solution: a pretreatment device based on fluopyram, comprising:

[0006] A liquid chromatograph body, wherein a solvent chamber is provided on the liquid chromatograph body;

[0007] A solvent bottle is disposed inside the solvent chamber, and the bottom end of the solvent chamber has a liquid inlet that mates with the solvent bottle, so that liquid can enter the inside of the solvent bottle through the inner hole inside the liquid inlet;

[0008] A threaded groove is formed at the lower inner end of the solvent bottle, and a sealing component is provided inside the threaded groove to seal it.

[0009] A threaded block is fixed to the upper surface of the inlet to engage with a threaded groove, and the inner side of the inlet has a push rod that drives the sealing assembly to open so that the inlet communicates with the inside of the solvent bottle.

[0010] Preferably, the push rod is cylindrical and is fixed to the inside of the liquid inlet by a support rod.

[0011] Preferably, the sealing assembly includes a mounting block, a connecting port, a first sealing block, a second spring, and a second sealing block. The mounting block is fixed to the bottom inner side of the solvent bottle to correspond to the threaded groove, and the lower inner side of the mounting block has a connecting port that connects the threaded groove to the inside of the solvent bottle. The mounting block has an inner groove along its height direction. The second spring and the second sealing block are sequentially arranged inside the inner groove, and the second sealing block corresponds to the connecting port to seal the connecting port. The first sealing block is connected to the lower inner side of the mounting block through an elastic guide structure to seal the threaded groove. When the first sealing block is pushed by the push rod, it drives the second sealing block to move and open the connecting port.

[0012] Preferably, the elastic guide structure includes a first spring, a guide cylinder, a protrusion, and a guide groove. The guide cylinder is fixed to the middle of the inner side of the mounting block, and the first sealing block is provided with a guide groove that cooperates with the guide cylinder. The first spring is disposed inside the guide groove. The outer surface of the first sealing block extends outward to form a protrusion, and the inner wall of the mounting block has a stop block that cooperates with the protrusion to form a positioning block.

[0013] Preferably, the inner contour of the guide groove is polygonal.

[0014] Preferably, the inner wall of the inner groove is provided with a sealing ring that contacts the second sealing block, and the sealing ring is symmetrically arranged in two places along the second sealing block. The lower surface of the second sealing block has a sealing gasket that matches the communication port.

[0015] Preferably, the second sealing block is arc-shaped, and an adjusting slider extending above the first sealing block is fixed to the upper end of the inner wall of the second sealing block, and a groove is provided on the inner wall of the inner groove to cooperate with the adjusting slider.

[0016] Preferably, the upper end of the inner side of the threaded groove is provided with an inclined surface.

[0017] Preferably, the solvent bottle has a filling port, and a bottle cap is connected to the filling port by a thread.

[0018] A detection method, employing a pre-processing device, further includes the following steps:

[0019] Step A: Unscrew the threaded groove to inject different solvents into the inside of the multiple solvent bottles respectively, and then tighten the threaded groove to seal the filling port of the solvent bottle, and place the solvent bottle inside the solvent chamber;

[0020] Step B: Rotate the solvent bottle so that the threaded groove on the lower surface of the solvent bottle engages with the threaded block. The push rod pushes the first sealing block upward, and the first sealing block moves upward to open the seal on the threaded groove. The first sealing block pushes the adjusting slider to move the second sealing block upward, and the second sealing block opens the seal on the connecting port so that the solvent bottle can communicate with the inside of the liquid inlet.

[0021] Step C: The pump inside the liquid chromatograph is connected to the inlet via a hose to draw solvent from the inside of the solvent bottle and mix it in the mixer to form the mobile phase in the required proportion.

[0022] Step D: Weigh a well-mixed vegetable sample and place it in a centrifuge tube. Add acetonitrile and extract the sample by shaking in a shaker. Then add sodium chloride to the centrifuge tube and centrifuge.

[0023] Step E: Weigh a portion of the supernatant and place it in a purification tube containing anhydrous magnesium sulfate. Centrifuge the tube and then filter the supernatant to obtain the sample solution to be tested.

[0024] Step F: During detection, the mixed mobile phase carries the sample to be tested into the chromatographic column to achieve isocratic elution separation, and then enters the mass spectrometer to detect fluopyram and its metabolites.

[0025] Compared with the prior art, the beneficial effects of the present invention are:

[0026] This invention, by incorporating a sealing assembly, threaded groove, threaded block, and top rod, avoids the problems associated with traditional top-discharge solvent bottles that require a long connecting hose. This hose is susceptible to misalignment or even detachment under tension. In this invention, the solvent bottle is installed inside the solvent chamber without the need for an additional hose, ensuring a stable flow of solvent into the liquid chromatograph. Furthermore, the double seal effectively prevents leakage due to loosening at the inlet interface, guaranteeing a stable supply of mobile phase to the liquid chromatograph and ensuring stable detection of fluopyram. Attached Figure Description

[0027] Figure 1 This is a schematic diagram of the structure of the present invention;

[0028] Figure 2 This is a schematic diagram of the solvent bottle and liquid inlet fitting structure of the present invention;

[0029] Figure 3 This is a schematic diagram of the threaded groove structure of the present invention;

[0030] Figure 4 This is a schematic diagram of the top rod mounting structure of the present invention;

[0031] Figure 5 This is a schematic cross-sectional view of the solvent bottle of the present invention;

[0032] Figure 6 For the present invention Figure 5 A magnified structural diagram at point A;

[0033] Figure 7 This is a cross-sectional view of the mounting block of the present invention;

[0034] Figure 8 This is a schematic cross-sectional view of the first sealing block of the present invention;

[0035] Figure 9 This is a schematic diagram of the second sealing block structure of the present invention.

[0036] In the diagram: 1. Liquid chromatograph body; 2. Solvent chamber; 3. Solvent bottle; 4. Inlet; 41. Threaded block; 42. Top rod; 5. Bottle cap; 6. Sealing assembly; 61. Mounting block; 611. Inner groove; 612. Stop block; 62. First spring; 63. Guide tube; 64. Connecting port; 65. First sealing block; 651. Protrusion; 652. Guide groove; 66. Sealing ring; 67. Second sealing block; 671. Adjusting slider; 68. Second spring; 7. Threaded groove; 8. Inclined surface. Detailed Implementation

[0037] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0038] Example 1

[0039] Please see Figures 1-9 The present invention provides a technical solution: a pretreatment device based on fluopyram, comprising:

[0040] The liquid chromatograph body 1 is equipped with a solvent chamber 2.

[0041] Solvent bottle 3 is located inside solvent chamber 2, and the bottom of the inside of solvent chamber 2 has a liquid inlet 4 that matches solvent bottle 3, so that liquid can enter into the inside of solvent bottle 3 through the inner hole inside the liquid inlet 4.

[0042] A threaded groove 7 is formed at the lower inner end of the solvent bottle 3, and a sealing component 6 is provided inside the threaded groove 7 to seal it.

[0043] A threaded block 41 is fixed to the upper surface of the inlet 4 to cooperate with the threaded groove 7, and the inner side of the inlet 4 has a push rod 42 that drives the sealing assembly 6 to open so that the inlet 4 communicates with the inside of the solvent bottle 3.

[0044] This design eliminates the need for additional hoses when installing solvent bottle 3 into solvent chamber 2, avoiding the problems of long hoses, easy pull-off, or improper installation in traditional liquid dispensing methods. The threaded fit in this device ensures a stable connection, and the push rod 42 automatically drives the sealing assembly 6 to open, connecting solvent bottle 3 with the inside of inlet 4, ensuring a stable flow of solvent into the liquid chromatograph body 1 and reducing the risk of leakage.

[0045] Preferably, the push rod 42 is cylindrical, and the push rod 42 is fixed to the inside of the liquid inlet 4 by a support rod;

[0046] It can stably apply a pushing force to the sealing assembly 6, ensuring the reliability and consistency of the opening action.

[0047] Preferably, the sealing assembly 6 includes a mounting block 61, a communication port 64, a first sealing block 65, a second spring 68, and a second sealing block 67. The mounting block 61 is fixed to the bottom inner side of the solvent bottle 3 to correspond to the threaded groove 7, and the lower inner side of the mounting block 61 is provided with a communication port 64 to communicate between the threaded groove 7 and the interior of the solvent bottle 3. An inner groove 611 is provided on the inner side of the mounting block 61 along its height direction. The second spring 68 and the second sealing block 67 are sequentially arranged inside the inner groove 611, and the second sealing block 67 corresponds to the communication port 64 to seal the communication port 64. The first sealing block 65 is connected to the lower inner side of the mounting block 61 through an elastic guide structure to seal the threaded groove 7. When the first sealing block 65 is pushed by the push rod 42, it drives the second sealing block 67 to move and open the communication port 64.

[0048] The first sealing block 65 seals the threaded groove 7, and the second sealing block 67 seals the connecting port 64. When the push rod 42 pushes the first sealing block 65, it can drive the second sealing block 67 to open, realizing the sequential release of the two seals. This ensures a reliable seal when the solvent bottle 3 is not installed, and also realizes automatic connection after installation, effectively preventing solvent leakage.

[0049] Preferably, the elastic guide structure includes a first spring 62, a guide cylinder 63, a protrusion 651, and a guide groove 652. The guide cylinder 63 is fixed to the middle of the inner side of the mounting block 61, and the first sealing block 65 is provided with a guide groove 652 that cooperates with the guide cylinder 63. The first spring 62 is provided inside the guide groove 652. The outer surface of the first sealing block 65 extends outward to form the protrusion 651. The inner wall of the mounting block 61 has a stop 612 that cooperates with the protrusion 651 to form a positioning.

[0050] The first sealing block 65 can move smoothly under the action of the push rod 42, and automatically reset and seal after disassembly by relying on the first spring 62. The protrusion 651 and the stop block 612 cooperate to limit the movement, prevent the first sealing block 65 from moving excessively, and improve the reliability of the sealing assembly 6.

[0051] Preferably, the inner contour of the guide groove 652 is polygonal;

[0052] It can prevent the first sealing block 65 from rotating circumferentially relative to the guide cylinder 63, and ensure the linearity and stability of its axial movement.

[0053] Preferably, the inner wall of the inner groove 611 is provided with a sealing ring 66 that contacts the second sealing block 67. The sealing ring 66 is symmetrically arranged in two places along the second sealing block 67. The lower surface of the second sealing block 67 has a sealing gasket that cooperates with the communication port 64.

[0054] The sealing performance between the second sealing block 67 and the inner groove 611 and the connecting port 64 is significantly enhanced, further reducing the possibility of solvent leakage and improving the overall sealing reliability of the device.

[0055] Preferably, the second sealing block 67 is arc-shaped, and an adjusting slider 671 extending above the first sealing block 65 is fixed to the upper end of the inner wall of the second sealing block 67. The inner wall of the inner groove 611 is provided with a groove that cooperates with the adjusting slider 671.

[0056] It is easy to be reliably pushed by the first sealing block 65, thus realizing the sequential opening of the two-stage seal.

[0057] Preferably, an inclined surface 8 is provided at the upper end of the inner side of the threaded groove 7;

[0058] This allows residual solvent at the connection port 64 to flow more effectively into the liquid inlet 4, reducing residue.

[0059] Preferably, the solvent bottle 3 is provided with a liquid filling port, and a bottle cap 5 is connected to the liquid filling port by a thread;

[0060] It facilitates rapid sealing after solvent is injected into the bottle, preventing solvent evaporation, contamination, or leakage.

[0061] A detection method, employing a pre-processing device, further includes the following steps:

[0062] Step A: Unscrew the threaded groove 7 to inject different solvents into the inside of multiple solvent bottles 3 respectively, and then tighten the threaded groove 7 onto the solvent bottle 3 to seal its filling port, and place the solvent bottle 3 inside the solvent chamber 2.

[0063] Step B: Rotate the solvent bottle 3 so that the threaded groove 7 on the lower surface of the solvent bottle 3 engages with the threaded block 41. The push rod 42 pushes the first sealing block 65 upward, and the first sealing block 65 moves upward to open the seal on the threaded groove 7. The first sealing block 65 pushes the adjusting slider 671 to drive the second sealing block 67 to move upward. The second sealing block 67 seals and opens the communication port 64 so that the solvent bottle 3 communicates with the inside of the liquid inlet 4.

[0064] Step C: The pump inside the liquid chromatograph body 1 is connected to the inlet 4 via a hose to draw the solvent inside the solvent bottle 3 and mix it in the mixer to form the mobile phase of the required proportion.

[0065] Step D: Weigh a well-mixed vegetable sample and place it in a centrifuge tube. Add acetonitrile and extract the sample by shaking in a shaker. Then add sodium chloride to the centrifuge tube and centrifuge.

[0066] Step E: Weigh a portion of the supernatant and place it in a purification tube containing anhydrous magnesium sulfate. Centrifuge the tube and then filter the supernatant to obtain the sample solution to be tested.

[0067] Step F: During detection, the mixed mobile phase carries the sample to be tested into the chromatographic column to achieve isocratic elution separation, and then enters the mass spectrometer to detect fluopyram and its metabolites;

[0068] The solvent bottle 3 is quickly installed and automatically connected by screw thread engagement, eliminating the traditional tubing insertion step, simplifying the operation process, and avoiding the risk of tubing detachment. At the same time, combined with the sample pretreatment and liquid chromatography-mass spectrometry detection process in step AF, it can stably and reliably provide the mobile phase to the liquid chromatograph body 1, realizing isocratic elution separation and mass spectrometry detection of components such as fluopyram, improving the accuracy and repeatability of detection.

[0069] Example 2

[0070] A pretreatment device based on fluopyram is the same as that in Example 1.

[0071] A preliminary detection method based on fluopyram:

[0072] Weigh 5 g of a well-mixed vegetable sample (tomato, radish, cabbage) into a 50 mL centrifuge tube, add 10 mL of acetonitrile to the centrifuge tube, tighten the cap, and extract by shaking at 250 r / min for 30 min in a shaker.

[0073] Remove the centrifuge tube, add 2 g of sodium chloride, tighten the cap, vortex at 2500 r / min for 5 min, centrifuge at 4000 r / min for 5 min, transfer about 1.5 mL of supernatant to a 2 mL purification tube containing 150 mg anhydrous magnesium sulfate, 50 mg PSA, and 50 mg C18, vortex at 2500 r / min for 5 min, centrifuge at 3000 r / min for 5 min, and filter the supernatant through a 0.22 µm organic filter membrane into a sample vial for LC-MS / MS analysis.

[0074] Instrumental analysis conditions:

[0075] Chromatographic column: Shim-pack XR-ODS II (2.0 mm × 75 mm × 2.2 µm); column temperature: 40℃; flow rate: 0.3 mL / min; injection volume: 1 μL; isocratic elution; mobile phase: A (0.1% formic acid aqueous solution): B (acetonitrile) = 20:80; data acquisition time: 3 min;

[0076] Mass spectrometry conditions:

[0077] Ion source: ESI+ (fluopyram), ESI- (M700F008, M700F048); Interface voltage: 4.0 kV; Interface temperature: 300℃; DL tube temperature: 250℃; Heating block temperature: 400℃; Nebulizing gas flow rate: 3 L / min; Heating gas flow rate: 10 L / min; Drying gas flow rate: 10 L / min; Collision gas: Argon; Monitoring mode: MRM multiple reaction monitoring mode.

[0078] This invention provides a method for determining the residues of fluopyram and its metabolites in various matrices of tomatoes, radishes, and cabbages using liquid chromatography-tandem mass spectrometry. This method significantly shortens the initial extraction steps and detection time, thereby improving detection efficiency. The method is simple, rapid, and has high sensitivity and accuracy.

[0079] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A pretreatment device based on fluopyram, characterized in that, include: The liquid chromatograph body (1) is provided with a solvent chamber (2). A solvent bottle (3) is disposed inside the solvent chamber (2), and the bottom of the inner side of the solvent chamber (2) has a liquid inlet (4) that cooperates with the solvent bottle (3) so that liquid can enter the inside of the solvent bottle (3) through the inner hole of the liquid inlet (4); A threaded groove (7) is provided at the lower inner end of the solvent bottle (3), and a sealing component (6) is provided inside the threaded groove (7) to seal it. A threaded block (41) is fixed to the upper surface of the inlet (4) to cooperate with the threaded groove (7), and the inside of the inlet (4) has a push rod (42) for driving the sealing assembly (6) to open so that the inlet (4) communicates with the inside of the solvent bottle (3).

2. The pretreatment device based on fluopyram according to claim 1, characterized in that: The top rod (42) is cylindrical and is fixed to the inside of the liquid inlet (4) by a support rod.

3. The pretreatment device based on fluopyram according to claim 1, characterized in that: The sealing assembly (6) includes a mounting block (61), a connecting port (64), a first sealing block (65), a second spring (68), and a second sealing block (67). The mounting block (61) is fixed to the bottom of the inner side of the solvent bottle (3) to correspond to the threaded groove (7). The lower inner side of the mounting block (61) is provided with a connecting port (64) to connect the threaded groove (7) with the inside of the solvent bottle (3). The inner side of the mounting block (61) is provided with an inner groove (611) along its height direction. The second spring (68) and the second sealing block (67) are sequentially arranged inside the inner groove (611), and the second sealing block (67) corresponds to the connecting port (64) to seal the connecting port (64). The first sealing block (65) is connected to the lower end of the inner side of the mounting block (61) through an elastic guide structure to seal the threaded groove (7). When the first sealing block (65) is pushed by the push rod (42), it drives the second sealing block (67) to move to open the connecting port (64).

4. The pretreatment device based on fluopyram according to claim 3, characterized in that: The elastic guide structure includes a first spring (62), a guide cylinder (63), a protrusion (651), and a guide groove (652). The guide cylinder (63) is fixed to the middle of the inner side of the mounting block (61), and the first sealing block (65) is provided with a guide groove (652) that cooperates with the guide cylinder (63). The first spring (62) is located inside the guide groove (652). The outer surface of the first sealing block (65) extends outward to form a protrusion (651). The inner wall of the mounting block (61) has a stop (612) that cooperates with the protrusion (651) to form a positioning.

5. The pretreatment device based on fluopyram according to claim 4, characterized in that: The inner contour of the guide groove (652) is polygonal.

6. The pretreatment device based on fluopyram according to claim 3, characterized in that: The inner wall of the inner groove (611) is provided with a sealing ring (66) that contacts the second sealing block (67). The sealing ring (66) is symmetrically arranged in two places along the second sealing block (67). The lower surface of the second sealing block (67) has a sealing gasket that cooperates with the communication port (64).

7. The pretreatment device based on fluopyram according to claim 3, characterized in that: The second sealing block (67) is arc-shaped. An adjusting slider (671) extending above the first sealing block (65) is fixed on the upper end of the inner wall of the second sealing block (67). The inner wall of the inner groove (611) is provided with a sliding groove that cooperates with the adjusting slider (671).

8. The pretreatment device based on fluopyram according to claim 1, characterized in that: An inclined surface (8) is provided on the upper inner side of the threaded groove (7).

9. The pretreatment device based on fluopyram according to claim 1, characterized in that: The solvent bottle (3) has a liquid filling port, and a bottle cap (5) is connected to the liquid filling port by a thread.

10. A detection method, employing the pretreatment apparatus according to any one of claims 1-9, characterized in that, It also includes the following steps: Step A: Unscrew the threaded groove (7) to inject different solvents into the inside of multiple solvent bottles (3) respectively, and then screw the threaded groove (7) onto the solvent bottle (3) to seal its filling port, and place the solvent bottle (3) inside the solvent chamber (2); Step B: Rotate the solvent bottle (3) so that the threaded groove (7) on the lower surface of the solvent bottle (3) engages with the threaded block (41). The push rod (42) pushes the first sealing block (65) upward. The first sealing block (65) moves upward to open the seal of the threaded groove (7). The first sealing block (65) pushes the adjusting slider (671) to drive the second sealing block (67) upward. The second sealing block (67) opens the seal of the connecting port (64) so ​​that the solvent bottle (3) communicates with the inside of the liquid inlet (4). Step C: The pump inside the liquid chromatograph body (1) is connected to the inlet (4) through a hose to draw the solvent inside the solvent bottle (3) and mix it in the mixer to form the mobile phase of the required ratio. Step D: Weigh a well-mixed vegetable sample and place it in a centrifuge tube. Add acetonitrile and extract the sample by shaking in a shaker. Then add sodium chloride to the centrifuge tube and centrifuge. Step E: Weigh a portion of the supernatant and place it in a purification tube containing anhydrous magnesium sulfate. Centrifuge the tube and then filter the supernatant to obtain the sample solution to be tested. Step F: During detection, the mixed mobile phase carries the sample to be tested into the chromatographic column to achieve isocratic elution separation, and then enters the mass spectrometer to detect fluopyram and its metabolites.

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