CN115144514A - Agricultural chemical residue detection and analysis equipment and method based on chromatography-mass spectrometry - Google Patents

Agricultural chemical residue detection and analysis equipment and method based on chromatography-mass spectrometry Download PDF

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Publication number
CN115144514A
CN115144514A CN202210877695.6A CN202210877695A CN115144514A CN 115144514 A CN115144514 A CN 115144514A CN 202210877695 A CN202210877695 A CN 202210877695A CN 115144514 A CN115144514 A CN 115144514A
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China
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detection
sample
mounting
area
bottom end
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Inventor
余佳
曹莉
豆叶枝
马涛
李菊颖
张悦清
许静
何健
孔德洋
吴文铸
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Nanjing Institute of Environmental Sciences MEE
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Nanjing Institute of Environmental Sciences MEE
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Priority to CN202210877695.6A priority Critical patent/CN115144514A/en
Publication of CN115144514A publication Critical patent/CN115144514A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/88Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention provides an agricultural chemical residue detection and analysis device and method based on chromatography-mass spectrometry, and belongs to the technical field of soil detection. The intelligent sample collection and analysis device comprises a mounting main body, a sample collection assembly, a sample operation and processing assembly, a sample detection and analysis assembly and an intelligent control module; according to the agricultural chemical residue detection and analysis equipment based on the chromatography-mass spectrometry, the sample collection assembly, the sample operation processing assembly, the sample detection and analysis assembly and the intelligent control module are arranged in a centralized manner, agricultural chemicals in soil in an area to be detected are collected in situ, and the whole collection process is carried out in a relatively closed space, so that when the collected samples are circulated among the equipment, the samples cannot be polluted due to exposure to air, and the detection precision and reliability are improved.

Description

Agricultural chemical residue detection and analysis equipment and method based on chromatography-mass spectrometry
Technical Field
The invention belongs to the technical field of soil detection, and particularly relates to agricultural chemical residue detection and analysis equipment and method based on chromatography-mass spectrometry.
Background
Agricultural toxic chemicals including agricultural chemicals, veterinary drugs, etc. and other agricultural supplies containing toxic substances have become the most dominant factor for water environmental pollution from agricultural non-point sources, in addition to N, P. Chemical fertilizers and pesticides are main control objects of agricultural non-point source pollution, and have great significance in realizing clean agriculture and ecological agriculture. The pesticide plays an irreplaceable role in modern agriculture, can prevent the crop from being affected by weeds and insect pests, and improves the growth efficiency of crops, but the pesticide is a double-edged sword, so that the use of the pesticide can also cause serious threats to the ecological environment and human health while bringing huge economic benefits to people.
The pesticide in China is high in the using amount of agricultural products, the pesticide residue of the agricultural products is inevitably overproof due to the use of the pesticide in a large range, so the pesticide residue problem is a main obstacle hindering agricultural development in China and agricultural product quality safety, one of the key links for controlling the pesticide residue amount in the agricultural products is timely and accurate analysis and detection of the pesticide residue amount so as to monitor the reasonable use of the pesticide, and meanwhile, the target product of the pesticide residue is stopped to be sold on the market, so that agricultural chemical residue detection and analysis equipment is urgently needed.
Disclosure of Invention
Aiming at the problems, the invention provides an agricultural chemical residue detection and analysis device and method based on chromatography-mass spectrometry.
The technical scheme of the invention is as follows: the agricultural chemical residue detection and analysis equipment based on chromatography-mass spectrometry comprises an installation main body, a sample collection assembly, a sample operation and treatment assembly, a sample detection and analysis assembly and an intelligent control module, wherein the installation main body is internally provided with a collection area, a treatment area and a detection area which sequentially penetrate and distribute from left to right;
the sample collecting assembly comprises a vertical mounting frame which is arranged in the collecting area and provided with a rotary threaded rod on the side wall, a transverse mounting frame which is in threaded connection with the rotary threaded rod through a sliding sleeve, a sample collecting head which is arranged at the bottom end of the transverse mounting frame, and a rotary motor which drives the rotary threaded rod to rotate, wherein a collecting opening is formed in the bottom end of the collecting area and at the position opposite to the sample collecting head;
the sample operation processing assembly comprises a storage box, a clamping boss, a falling pipe, a transfer processing barrel, a clamping groove and a plurality of liquid outlet pipes, wherein the storage box is arranged in a processing area, the upper end of the storage box is connected with an external water source, the clamping boss is arranged at the bottom end of the storage box, the falling pipe is arranged at the bottom end of the clamping boss, the two transfer sliding rails are arranged on the front side wall and the rear side wall of the processing area and are distributed along the length direction of the processing area, and the left side and the right side of the processing area extend to the collection area and the detection area respectively, the mounting ring can slide left and right on the transfer sliding rails under the driving of a driving device, the transfer processing barrel is clamped on the mounting ring, a liquid outlet is arranged at the bottom end of the mounting ring, a drain outlet is arranged on the side wall of the mounting ring, the upper end of the transfer processing barrel is arranged in a clamping groove which is distributed opposite to the clamping boss and is communicated with the interior of the transfer processing barrel, an electric opening and closing plate is arranged on the clamping groove, an arc dispersion frame is arranged in the transfer processing barrel, a liquid dispersion frame is arranged at the bottom end of the arc dispersion frame, a plurality of dispersion frame is arranged at the center of the dispersion frame, a plurality of dispersion liquid outlet holes are uniformly arranged in which are arranged at the dispersion frame, and are arranged at the bottom end of the arc dispersion frame, and are arranged at the bottom end of the filter plate;
sample detection analysis subassembly including locate detection mounting bracket on the detection zone, with detect chromatograph and the mass spectrograph that the mounting bracket is connected, locate the detection zone bottom and be located detect the detection box under the mounting bracket.
Further, deposit and be equipped with the installation reinforcement between case and the processing area, the installation reinforcement including fixed locating processing area inner wall and lateral wall be equipped with the installation regulation post that the groove was erected in the slip along vertical direction, with the slip erect groove sliding connection and upper end be equipped with place the draw-in groove and the bottom be equipped with the horizontal mounting panel, one end of slip horizontal groove and the slip erect groove sliding connection and the other end with slip horizontal groove sliding connection's enhancement mediation pole, enhancement mediation pole accessible drive arrangement slides in the slip horizontal groove, will deposit the case and place in placing the draw-in groove, support and place, strengthen mediation pole one end and slide in the slip horizontal groove through drive arrangement drive, simultaneously, the other end is erected the inslot at the slip and is followed up, makes horizontal mounting panel slide from top to bottom in the slip vertical groove, can accomplish the regulation of depositing the case and placing the position, when needs clear up its inside, only need make horizontal mounting panel erect the inslot at the slip can downwards, simple structure, convenient operation.
Further, it is equipped with folding seal assembly to transport a processing bobbin end, folding seal assembly including locate transport a processing bobbin end sealed folding cover, locate sealed folding cover's fixed connection ring, be used for connecting transport a processing bobbin end with fixed connection ring's first electric telescopic handle, liquid outlet department are equipped with the solenoid valve, when transporting a processing section of thick bamboo and remove to detecting the box directly on along transporting the slide rail, extend through first electric telescopic handle, drive sealed folding cover downstream, until fixed connection ring and detection box butt, then, open the solenoid valve for the sample is in relative confined environment, and falls to the in-process that detects the box under, does not contact with the outside air, guarantees that the sample can not appear polluting, improves the accuracy of testing result.
Further, arc scattering frame department is equipped with the ultrasonic vibration motor, through the drive of ultrasonic vibration motor, can accelerate the falling speed of soil sample through arc scattering frame, avoids soil sample to pile up, improves work efficiency.
Further, it is equipped with the mounting groove to detect box center department, be equipped with the partition stopper in the mounting groove, evenly be equipped with a plurality of detection grooves on the partition stopper, and every it has a plurality of closed membrane lamellas to detect groove entrance lateral wall along circumference is articulated, through separating a plurality of detection groove structures that the stopper set up, can conveniently carry out batch detection to a plurality of samples simultaneously, shortens check-out time, improves the reliability and the precision that detect, through it has a plurality of closed membrane lamellas to articulate along circumference at every detection groove entrance lateral wall, can make before the detection and during the testing process, the testing sample is in relative confined environment, avoids exposing in the air because of the sample, causes the sample to appear polluting, leads to the testing result inaccurate.
Furthermore, detect the box bottom and be hollow structure, and detect the box and be connected with the condenser through the connecting pipe, and detect box inner wall subsides and be equipped with heat preservation and thermometer, through being in suitable low temperature environment with the testing sample all the time, avoid causing the residue to volatilize in the sample because of external factor, cause the detection concentration to descend, reduce the reliability of detection device work.
Further, detect the mounting bracket include through second electric telescopic handle and detection zone upper wall connection's vertical installation mobile jib, locate the installation lantern ring, the edge of vertical installation mobile jib outer wall installation lantern ring circumferencial direction evenly distributed and with detect a plurality of installation branches of groove one-to-one, every installation branch bottom all is connected with the test probe of chromatograph and mass spectrograph, adjusts the position of vertical installation mobile jib through second electric telescopic handle, reaches the purpose of test probe position, makes steady operation between each equipment, each other does not influence.
Furthermore, each it is articulated between installation branch and the installation lantern ring outer wall, vertical installation mobile jib outer wall just is located installation lantern ring lower extreme position department and is equipped with the regulation gusset plate, just adjust gusset plate upper end and every be equipped with third electric telescopic handle between the installation branch, adjust and be equipped with a plurality of gusset rods between gusset plate lower extreme and the vertical installation mobile jib outer wall, adjust the position of vertical installation mobile jib through second electric telescopic handle, reach the purpose of coarse adjustment test probe position, finely tune test probe's position through third electric telescopic handle, guarantee that each test probe can be sufficient and the sample contact, avoid appearing the phenomenon that the testing result became invalid to improve test structure's reliability.
The invention also discloses an agricultural chemical residue detection and analysis method based on the chromatography-mass spectrometry, and the agricultural chemical residue detection and analysis equipment based on the chromatography-mass spectrometry comprises the following steps:
s1, moving an installation main body to an area needing to collect a sample, starting a rotating motor, driving a rotating threaded rod to rotate clockwise through the rotating motor, driving a transverse installation rack to move downwards through a sliding sleeve, synchronously descending a sample collection head at the moment, closing the rotating motor when the sample collection head moves downwards through a collection port and contacts with the sample collection area, collecting the sample through the collection head, restarting the rotating motor after collection is finished, and driving the rotating threaded rod to rotate anticlockwise through the rotating motor, so that the sample collection head moves upwards;
s2, after the sample collection is finished, driving the mounting ring to move on a transfer slide rail through a driving device, when the sample reaches the lower end of the collection head, closing the driving device, driving a rotary threaded rod to rotate through a rotary motor, enabling the sample collection head to move downwards to the upper end of a transfer treatment cylinder, opening an electric opening and closing plate, enabling the collected sample to fall to an arc-shaped dispersion frame through a clamping groove, dispersing the collected soil to all positions of the transfer treatment cylinder through dispersion pipes distributed along all directions on the arc-shaped dispersion frame, closing the electric opening and closing plate, driving the mounting ring to move on the transfer slide rail to the lower end of a storage box through the driving device, closing the driving device, enabling a clamping boss to be in contact with a clamping groove, enabling a relatively closed space to be formed between the clamping boss and the clamping groove, opening the electric opening and closing plate, enabling a water body in the storage box to flow into a dispersion layer through the dispersion pipes and through dispersion liquid adding holes, and enabling agricultural chemicals in the soil sample to be dissolved in the water body to form slurry through stirring and uniformly mixed by a stirring element;
s3, when a collected sample needs to be detected, the mounting ring is driven to move on the transfer slide rail through the driving device, when the transfer processing barrel moves to the position right above the detection box, the first electric telescopic rod is started to extend to drive the fixed connecting ring to move downwards, when the fixed connecting ring is in contact with the position right above the detection box, the first electric telescopic rod is closed, a relatively closed structure is formed through the sealing folding sleeve, then the electromagnetic valve is opened, so that the sample is in a relatively closed environment and drops downwards after being filtered by the filter plate, and under the action of the falling gravity of the slurry sample, each closed membrane flap is impacted to be opened, so that the slurry sample falls into each detection groove;
s4, after the thick liquid sample is whole to fall, start the upwards compression of first electric telescopic handle, it shifts up to drive fixed go-between, move on transporting the slide rail through drive arrangement drive collar, make and transport a processing section of thick bamboo and detection box separation, then, start second electric telescopic handle downwardly extending, and drive and adjust vertical installation mobile jib downstream, roughly adjust the position of test probe in proper order, and simultaneously, start third electric telescopic handle and extend and carry out the fine tuning to test probe' S position, when each test probe chromatograph and mass spectrograph distribute the whereabouts to each detection groove, detect the sample can.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the agricultural chemical residue detection and analysis equipment based on the chromatography-mass spectrometry, the sample collection assembly, the sample operation processing assembly, the sample detection and analysis assembly and the intelligent control module are arranged in a centralized manner, agricultural chemicals in soil in an area to be detected are collected in situ, and the whole collection process is carried out in a relatively closed space, so that when the collected samples are circulated among the equipment, the samples cannot be polluted due to exposure to air, and the detection precision and reliability are improved.
(2) The arrangement of the electric opening and closing plate and the folding sealing assembly ensures that a detected sample is in a relatively closed environment and does not contact with the outside air, so that the sample is prevented from being polluted, the accuracy of a detection result is improved, meanwhile, the transfer treatment cylinder disclosed by the invention slides in each area of the installation main body through the transfer slide rail, so that the continuous work among all devices is coordinated, the whole process does not need excessive manpower participation, the automation degree is high, and the workload of workers is reduced.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention;
FIG. 2 is a schematic view of the construction of the mounting stiffener of the present invention;
FIG. 3 is a schematic structural view of the folding seal assembly of the present invention;
FIG. 4 is a schematic view showing the internal structure of the cartridge when the closure flap of the present invention is opened;
FIG. 5 is a schematic view showing the internal structure of the cartridge when the closure flap of the present invention is closed;
FIG. 6 is a schematic structural view of the test mount of the present invention;
wherein, 1-installation main body, 10-collection area, 100-collection port, 11-treatment area, 12-detection area, 2-sample collection assembly, 20-vertical installation rack, 200-rotary threaded rod, 21-transverse installation rack, 210-sliding sleeve, 22-sample collection head, 23-rotary motor, 3-sample operation treatment assembly, 30-storage box, 31-clamping boss, 32-drop tube, 33-transfer slide rail, 34-installation ring, 35-transfer treatment cylinder, 350-liquid outlet, 3500-electromagnetic valve, 351-sewage outlet, 352-clamping groove, 3520-electric opening and closing plate, 353-arc dispersion rack, 354-liquid dispersion layer, 355-liquid dispersion pipe, 356-through port, 357-liquid dispersion addition hole 358-filter plate, 36-stirring element, 37-mounting reinforcement, 370-mounting adjusting column, 3700-sliding vertical slot, 371-transverse mounting plate, 3710-placing clamping slot, 3711-sliding transverse slot, 372-strengthening adjusting rod, 38-ultrasonic vibration motor, 4-sample detection and analysis component, 40-detection mounting frame, 400-second electric telescopic rod, 401-vertical mounting main rod, 402-mounting collar, 403-mounting support rod, 404-adjusting reinforcing plate, 405-third electric telescopic rod, 406-reinforcing rod, 41-chromatograph, 42-mass spectrometer, 44-detection box, 440-mounting slot, 441-separating plug, 442-detection slot, 443-sealing membrane flap, 444-heat-insulating layer, thermal-insulating layer, etc, 445-thermometer, 45-condenser, 5-intelligent control module, 6-folding sealing component, 60-sealing folding sleeve, 61-fixed connecting ring, 62-first electric telescopic rod.
Detailed Description
In order to further understand the contents of the present invention, the present invention is described in detail by examples below.
Example 1
As shown in fig. 1, the agricultural chemical residue detection and analysis device based on chromatography-mass spectrometry comprises an installation main body 1, a sample collection assembly 2, a sample operation processing assembly 3, a sample detection and analysis assembly 4 and an intelligent control module 5, wherein the installation main body 1 is internally provided with a collection area 10, a processing area 11 and a detection area 12 which are sequentially distributed in a penetrating manner from left to right, the sample collection assembly 2 is arranged in the collection area 10, the sample operation processing assembly 3 is arranged in the processing area 11, the sample detection and analysis assembly 4 is arranged in the detection area 12, and the intelligent control module 5 is arranged on the side wall of the installation main body 1;
the sample collecting assembly 2 comprises a vertical mounting rack 20 which is arranged in the collecting area 10 and provided with a rotary threaded rod 200 on the side wall, a transverse mounting rack 21 which is in threaded connection with the rotary threaded rod 200 through a sliding sleeve 210, a sample collecting head 22 which is arranged at the bottom end of the transverse mounting rack 21, and a rotary motor 23 which drives the rotary threaded rod 200 to rotate, wherein a collecting opening 100 is arranged at the bottom end of the collecting area 10 and at the position opposite to the sample collecting head 22;
the sample operation processing assembly 3 comprises a storage box 30 which is arranged in a processing area 11 and the upper end of which is connected with an external water source, a clamping boss 31 which is arranged at the bottom end of the storage box 30, a falling pipe 32 which is arranged at the bottom end of the clamping boss 31, two transfer slide rails 33 which are arranged on the front side wall and the rear side wall of the processing area 11 and distributed along the length direction of the processing area 11 and the left side and the right side of which respectively extend to an acquisition area 10 and a detection area 12, a mounting ring 34 which can slide left and right on the transfer slide rails 33 under the drive of a drive device, a transfer processing cylinder 35 which is clamped on the mounting ring 34 and is provided with a liquid outlet 350 at the bottom end and a sewage discharge outlet 351 at the side wall, the upper end of the transfer processing cylinder 35 is arranged on a clamping groove 352 which is distributed opposite to the clamping boss 31 and is communicated with the inside of the transfer processing cylinder 35, an electric opening and closing plate 3520 is arranged on the clamping groove 352, an arc-shaped dispersion frame 353 is arranged in the transfer processing cylinder 35, the bottom end of the arc-shaped dispersion frame 353 is provided with dispersion liquid layers 354 and 15 dispersion tubes 355 which are distributed along all directions and the upper end of which penetrates through the arc-shaped liquid outlet 354, a filter plate 358 is arranged at the center of which is arranged on the arc-shaped dispersion tube 35, and is uniformly arranged on the filter plate 358 which is arranged at the bottom end of the mixing cylinder 35;
the sample detection and analysis assembly 4 comprises a detection mounting frame 40 arranged at the upper end of the detection area 12, a chromatograph 41 and a mass spectrometer 42 connected with the detection mounting frame 40, and a detection box 44 arranged at the bottom end of the detection area 12 and positioned right below the detection mounting frame 40;
an ultrasonic vibration motor 38 is arranged at the arc-shaped dispersing frame 353;
as shown in fig. 4 and 5, a mounting groove 440 is formed in the center of the detecting box 44, a separating plug 441 is disposed in the mounting groove 440, a plurality of detecting slots 442 are uniformly disposed on the separating plug 441, and 4 closed flaps 443 are circumferentially hinged to the side wall of the inlet of each detecting slot 442;
the bottom end of the detection box 44 is of a hollow structure, the detection box 44 is connected with a condenser 45 through a connecting pipe, and the inner wall of the detection box 44 is adhered with an insulating layer 444 and a thermometer 445;
as shown in fig. 6, the detection mounting frame 40 includes a vertical mounting main rod 401 connected to the upper wall of the detection area 12 through a second electric telescopic rod 400, a mounting collar 402 disposed on the outer wall of the vertical mounting main rod 400, and 4 mounting support rods 403 uniformly distributed along the circumferential direction of the mounting collar 402 and corresponding to the detection grooves 442 one by one, and the bottom end of each mounting support rod 403 is connected to the detection probes of the chromatograph 41 and the mass spectrometer 42;
each installation branch 403 is articulated between the outer wall of installation lantern ring 402, and vertical installation mobile jib 401 outer wall just is located installation lantern ring 402 lower extreme position department and is equipped with regulation gusset plate 404, and adjusts and is equipped with third electric telescopic handle 405 between gusset plate 404 upper end and every installation branch 403, adjusts and is equipped with a plurality of gusset rods 406 between gusset plate 404 lower extreme and the vertical installation mobile jib 401 outer wall.
Example 2
The present embodiment is different from embodiment 1 in that:
as shown in fig. 2, an installation reinforcing member 37 is disposed between the storage box 30 and the processing area 11, the installation reinforcing member 37 includes an installation adjusting column 370 fixedly disposed on the inner wall of the processing area 11 and having a side wall provided with a sliding vertical groove 3700 in the vertical direction, a transverse mounting plate 371 slidably connected with the sliding vertical groove 3700 and having a placement clamping groove 3710 at the upper end and a sliding transverse groove 3711 at the bottom end, a reinforcement adjusting rod 372 having one end slidably connected with the sliding vertical groove 3700 and having the other end slidably connected with the sliding transverse groove 3711, and the reinforcement adjusting rod 372 can slide in the sliding transverse groove 3711 through a driving device.
Example 3
The present embodiment is different from embodiment 2 in that:
as shown in fig. 3, a folding sealing assembly 6 is disposed at the bottom end of the transferring treatment cylinder 35, the folding sealing assembly 6 includes a sealing folding sleeve 60 disposed at the bottom end of the transferring treatment cylinder 35, a fixed connection ring 61 disposed on the sealing folding sleeve 60, and a first electric telescopic rod 62 for connecting the bottom end of the transferring treatment cylinder 35 and the fixed connection ring 61, and an electromagnetic valve 3500 is disposed at the liquid outlet 350.
The rotating motor 23, the electromagnetic valve 3500, the electric opening and closing plate 3520, the stirring element 36, the ultrasonic vibration motor 38, the second electric telescopic rod 400, the third electric telescopic rod 405, the chromatograph 41, the mass spectrometer 42, the thermometer 445, the condenser 45, the intelligent control module 5 and the first electric telescopic rod 62 used in this embodiment are all products of the prior art, and those skilled in the art can select the products according to the needs, so that the technical scheme of the present invention can be satisfied, and no special limitation is made herein.
Example 4
The embodiment discloses an agricultural chemical residue detection and analysis method based on chromatography-mass spectrometry, and the agricultural chemical residue detection and analysis device based on chromatography-mass spectrometry of the embodiment 3 comprises the following steps:
s1, moving an installation main body 1 to an area needing to collect a sample, starting a rotary motor 23, driving a rotary threaded rod 200 to rotate clockwise through the rotary motor 23, enabling a sliding sleeve 210 to drive a transverse installation frame 21 to move downwards, enabling a sample collection head 22 to descend synchronously, when the sample collection head 22 moves downwards through a collection port 100 and contacts with the sample collection area, closing the rotary motor 23, collecting the sample through the collection head 22, restarting the rotary motor 23 after collection is finished, and driving the rotary threaded rod 200 to rotate anticlockwise through the rotary motor 23, so as to enable the sample collection head 22 to move upwards;
s2, after a sample collection area is finished, driving the mounting ring 34 to move on the transfer slide rail 33 through a driving device, when the sample collection area reaches the lower end of the collection head 22, closing the driving device, driving the rotary threaded rod 200 to rotate through the rotary motor 23, enabling the sample collection head 22 to move downwards to the upper end of the transfer treatment cylinder 35, opening the electric opening and closing plate 3520, enabling the collected sample to fall to the arc-shaped dispersion frame 353 through the clamping groove 352, dispersing the collected soil to all positions of the transfer treatment cylinder 35 through the dispersion pipes 355 distributed in all directions on the arc-shaped dispersion frame 353, closing the electric opening and closing plate 3520, driving the mounting ring 34 to move to the lower end of the storage box 30 on the transfer slide rail 33 through the driving device, closing the driving device, enabling the clamping boss 31 to be in contact with the clamping groove 352 at the moment, enabling relatively closed spaces to be formed between the clamping boss 31 and the clamping groove 352, opening the electric opening and closing plate 3520, enabling water in the storage box 30 to flow into the dispersion liquid through the through pipes 32 and through the dispersion liquid adding holes 357, uniformly mixing, enabling chemical products in the sample to fall into the soil to be dissolved into the water body in the agricultural slurry through the stirring element 36, and forming a water body dissolved in the agricultural slurry;
s3, when a collected sample needs to be detected, the mounting ring 34 is driven by the driving device to move on the transfer slide rail 33, when the transfer treatment barrel 35 moves to the position right above the detection box 44, the first electric telescopic rod 62 is started to extend to drive the fixed connecting ring 61 to move downwards, when the fixed connecting ring 61 is in contact with the position right above the detection box 44, the first electric telescopic rod 62 is closed, a relatively closed structure is formed through the sealing folding sleeve 60, then the electromagnetic valve 3500 is opened to enable the sample to be in a relatively closed environment, the sample falls downwards after being filtered by the filter plate 358, and under the action of falling gravity of the slurry sample, each closed membrane valve 443 is impacted to be opened, so that the slurry sample falls into each detection groove 442;
s4, after the slurry sample falls completely, start first electric telescopic handle 62 and upwards compress, drive fixed go-between 61 and shift up, move on transporting slide rail 33 through drive arrangement drive collar 34, make and transport a processing section of thick bamboo 35 and detect box 44 separation, then, start second electric telescopic handle 400 downwardly extending, and drive and adjust vertical installation mobile jib 401 and move down, roughly adjust the position of test probe in proper order, and simultaneously, start third electric telescopic handle 405 and extend and carry out fine tuning to the position of test probe, when each test probe chromatograph 41 and mass spectrometer 42 distribute and fall to each detection groove 442, detect the sample can.

Claims (9)

1. The agricultural chemical residue detection and analysis equipment based on chromatography-mass spectrometry is characterized by comprising an installation main body (1) in which a collection area (10), a treatment area (11) and a detection area (12) are sequentially distributed from left to right, a sample collection assembly (2) arranged in the collection area (10), a sample operation treatment assembly (3) arranged in the treatment area (11), a sample detection and analysis assembly (4) arranged in the detection area (12) and an intelligent control module (5) arranged on the side wall of the installation main body (1);
the sample collecting assembly (2) comprises a vertical mounting rack (20) which is arranged in a collecting area (10) and provided with a rotary threaded rod (200) on the side wall, a transverse mounting rack (21) which is in threaded connection with the rotary threaded rod (200) through a sliding sleeve (210), a sample collecting head (22) which is arranged at the bottom end of the transverse mounting rack (21), and a rotary motor (23) which drives the rotary threaded rod (200) to rotate, wherein a collecting port (100) is formed in the bottom end of the collecting area (10) and in the position opposite to the sample collecting head (22);
the sample operation processing assembly (3) comprises a storage box (30) arranged in a processing area (11) and connected with an external water source at the upper end, a clamping boss (31) arranged at the bottom end of the storage box (30), a drop-in pipe (32) arranged at the bottom end of the clamping boss (31), two transfer slide rails (33) which are arranged on the front side wall and the rear side wall of the processing area (11) and distributed along the length direction of the processing area (11) and extend to the acquisition area (10) and the detection area (12) from the left side to the right side respectively, a mounting ring (34) which can slide left and right on the transfer slide rails (33) under the driving of a driving device, a transfer processing cylinder (35) clamped on the mounting ring (34) and provided with a liquid layer (350) at the bottom end and a drain outlet (351) at the side wall, wherein the upper end of the transfer processing cylinder (35) is arranged on a clamping groove (352) which is relatively distributed with the clamping boss (31) and communicated with the inside of the transfer processing cylinder (35), an electric bulk material plate (3520) is arranged on the clamping groove (352), an arc-shaped bulk material distribution frame (353) is arranged in the transfer processing cylinder (35), a plurality of arc-shaped bulk material distribution frames (354) and a plurality of bulk material distribution pipes (354) penetrating through holes (356) are arranged at the bottom end of which penetrate through the bulk material distribution pipe (356) along the distribution pipe, and a plurality of bulk material distribution pipe (356) which penetrate through the bulk material distribution pipe distribution frame (356) and pass through the bulk material distribution frame (356) and are arranged at the bottom end, a plurality of liquid adding holes (357) are uniformly formed in the liquid dispersion layer (354), a stirring element (36) is arranged in the transfer treatment cylinder (35) and positioned at the bottom end of the arc-shaped dispersion frame (353), and a filter plate (358) is arranged at the liquid outlet (350);
sample detection analysis subassembly (4) including locate detection mounting bracket (40) of detection zone (12) upper end, with chromatograph (41) and mass spectrometer (42) that detection mounting bracket (40) are connected, locate detection zone (12) bottom and be located detect detection box (44) under mounting bracket (40).
2. The agricultural chemical residue detection and analysis equipment based on chromatography-mass spectrometry combination of claim 1, wherein an installation reinforcing member (37) is arranged between the storage box (30) and the processing area (11), the installation reinforcing member (37) comprises an installation adjusting column (370) fixedly arranged on the inner wall of the processing area (11) and provided with a sliding vertical groove (3700) on the side wall along the vertical direction, a transverse mounting plate (372) connected with the sliding vertical groove (3700) in a sliding manner and provided with a placement clamping groove (3710) at the upper end and a sliding transverse groove (3711) at the bottom end, and a reinforcing adjusting rod (372) with one end connected with the sliding vertical groove (3700) in a sliding manner and the other end connected with the sliding transverse groove (3711), and the reinforcing adjusting rod (372) can slide in the sliding transverse groove (3711) through a driving device.
3. The device for detecting and analyzing agricultural chemical residue based on chromatography-mass spectrometry as claimed in claim 1, wherein the bottom end of the transfer treatment cylinder (35) is provided with a folding sealing assembly (6), the folding sealing assembly (6) comprises a sealing folding sleeve (60) arranged at the bottom end of the transfer treatment cylinder (35), a fixed connecting ring (61) arranged on the sealing folding sleeve (60), a first electric telescopic rod (62) for connecting the bottom end of the transfer treatment cylinder (35) and the fixed connecting ring (61), and a solenoid valve (3500) is arranged at the liquid outlet (350).
4. The chromatography-mass spectrometry-based agrochemical residue detection and analysis apparatus according to claim 1, wherein an ultrasonic vibration motor (38) is provided at the arc-shaped dispersion frame (353).
5. The apparatus for detecting and analyzing residue of agricultural chemicals based on combined chromatography and mass spectrometry as claimed in claim 1, wherein a mounting groove (440) is formed at the center of the cartridge (44), a separation plug (441) is formed in the mounting groove (440), a plurality of detection grooves (442) are uniformly formed in the separation plug (441), and a plurality of closed flaps (443) are circumferentially hinged to the side wall of the inlet of each detection groove (442).
6. The agricultural chemical residue detection and analysis device based on chromatography-mass spectrometry of claim 5, wherein the bottom end of the detection box (44) is a hollow structure, the detection box (44) is connected with a condenser (45) through a connecting pipe, and an insulating layer (444) and a thermometer (445) are attached to the inner wall of the detection box (44).
7. The device for detecting and analyzing agricultural chemical residue based on chromatography-mass spectrometry as claimed in claim 5, wherein the detection mounting frame (40) comprises a vertical mounting main rod (401) connected with the upper wall of the detection zone (12) through a second electric telescopic rod (400), a mounting collar (402) arranged on the outer wall of the vertical mounting main rod (400), and a plurality of mounting struts (403) which are uniformly distributed along the circumferential direction of the mounting collar (402) and correspond to the detection grooves (442) one by one, and the bottom end of each mounting strut (403) is connected with the detection probes of the chromatograph (41) and the mass spectrometer (42).
8. The apparatus for detecting and analyzing residue of agricultural chemicals based on chromatography-mass spectrometry of claim 7, wherein each of the mounting struts (403) is hinged to the outer wall of the mounting collar (402), an adjusting reinforcing plate (404) is provided on the outer wall of the vertical mounting strut (401) and at the lower end of the mounting collar (402), a third electric telescopic rod (405) is provided between the upper end of the adjusting reinforcing plate (404) and each of the mounting struts (403), and a plurality of reinforcing rods (406) are provided between the lower end of the adjusting reinforcing plate (404) and the outer wall of the vertical mounting strut (401).
9. The method for detecting and analyzing the residual agricultural chemical based on the chromatography-mass spectrometry is based on the equipment for detecting and analyzing the residual agricultural chemical based on the chromatography-mass spectrometry of any one of claims 1 to 8, and is characterized by comprising the following steps of:
s1, moving an installation main body (1) to an area needing to collect a sample, starting a rotating motor (23), driving a rotating threaded rod (200) to rotate clockwise through the rotating motor (23), enabling a sliding sleeve (210) to drive a transverse installation rack (21) to move downwards, and enabling a sample collection head (22) to descend synchronously at the moment;
s2, after the sample collection is finished, the mounting ring (34) is driven to move on the transfer sliding rail (33) through the driving device, when the sample collection is finished, the driving device is closed, the rotary threaded rod (200) is driven to rotate through the rotary motor (23), the sample collection head (22) is enabled to move downwards to the upper end of the transfer processing cylinder (35), the electric opening and closing plate (3520) is opened, the collected sample is dropped to the arc-shaped dispersing frame (353) through the clamping groove (352), the collected soil is dispersed to all parts of the transfer processing cylinder (35) through the bulk material pipes (355) distributed along all directions on the arc-shaped dispersing frame (353), and the electric opening and closing plate (3520) is closed, the mounting ring (34) is driven by the driving device to move on the transfer slide rail (33) to the position right below the storage box (30), the driving device is closed, at the moment, the clamping boss (31) is in contact with the clamping groove (352), a relatively closed space is formed between the clamping boss and the clamping groove, the electric opening and closing plate (3520) is opened, water in the storage box (30) flows into the liquid dispersion layer (354) through the falling pipe (32) and the through hole (356), the water is dispersed into the soil sample through the liquid dispersion adding holes (357), at the moment, the water is uniformly stirred by the stirring element (36), and the agricultural chemicals in the soil sample are dissolved into the water to form slurry;
s3, when a collected sample needs to be detected, the mounting ring (34) is driven to move on the transfer sliding rail (33) through the driving device, when the transfer processing barrel (35) moves to the upper end of the detection box (44), the first electric telescopic rod (62) is started to extend to drive the fixed connecting ring (61) to move downwards, when the fixed connecting ring (61) is in contact with the upper end of the detection box (44), the first electric telescopic rod (62) is closed, a relatively closed structure is formed through the sealing folding sleeve (60), then the electromagnetic valve (3500) is opened to enable the sample to be in a relatively closed environment and to fall downwards after being filtered through the filter plate (358), and each closed membrane flap (443) is impacted under the action of falling gravity of the slurry sample to enable the slurry sample to fall into each detection groove (442);
s4, after the slurry sample falls completely, start first electric telescopic handle (62) upwards to compress, drive fixed go-between (61) and move up, move on transporting slide rail (33) through drive arrangement drive collar (34), make and transport a processing section of thick bamboo (35) and detect box (44) separation, then, start second electric telescopic handle (400) downwardly extending, and drive and adjust vertical installation mobile jib (401) and move down, carry out the coarse adjustment to the position of test probe in proper order, simultaneously, start third electric telescopic handle (405) and extend and carry out fine tuning to the position of test probe, when each test probe chromatograph (41) and mass spectrograph (42) distribute and fall to each detection groove (442), detect the sample can.
CN202210877695.6A 2022-07-25 2022-07-25 Agricultural chemical residue detection and analysis equipment and method based on chromatography-mass spectrometry Pending CN115144514A (en)

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