CN112198324B - Full-automatic QuECHERS experimental device and experimental method - Google Patents

Abstract

The invention discloses a full-automatic QuECHERS experimental device and an experimental method. The full-automatic QuECHERS experimental device comprises a multifunctional mechanical arm, a screw cap module, a liquid adding module, a centrifugal module, a salt adding module, a ceramic homogenizing submodule, a nitrogen blowing concentration module, a vortex mixing module and a vibration module, and can automatically complete the actions of sample transferring, adding of extraction liquid, extraction salt and ceramic homogeneous protons, vibration mixing, centrifugal separation and vortex mixing; the method for carrying out the experiment by adopting the full-automatic QuECHERS experimental device mainly integrates the processes of sample liquid adding extraction, centrifugal separation, solid phase extraction and nitrogen blowing concentration, saves time, reduces manual operation, improves automation and reduces errors.

Description

Full-automatic QuECHERS experimental device and experimental method

Technical Field

The invention relates to a QuECHERS pretreatment technology, in particular to a full-automatic QuECHERS experimental device and an experimental method.

Background

The development of agricultural industrialization leads the production of agricultural products to depend on exogenous substances such as pesticides, antibiotics, hormones and the like more and more, the dosage of the pesticides in the agricultural products in China is high, and the unreasonable use of the substances can lead the pesticide residue in the agricultural products to exceed the standard, thus affecting the edible safety of consumers, causing the pathogenic, abnormal development and the like of the consumers in serious cases, and even directly causing poisoning and death. The over-standard pesticide residue also affects the trade of agricultural products, countries in the world pay high attention to the problem of pesticide residue, and more strict limit standards are stipulated for the pesticide residue in various agricultural and sideline products, so that the export of agricultural products in China faces a serious challenge.

Pesticide residues are a general term for the parents of pesticides and all derivatives with toxicological significance, such as impurities, metabolic conversion products and reactants, which remain in organisms, agricultural products and the environment due to the application of pesticides. The pretreatment technology is the key in pesticide residue analysis and detection, and the pretreatment technology determines the accuracy of an analysis result to a great extent. Sample pretreatment techniques are important for the detection of minute quantities of complex components in complex matrices. The sample pretreatment is the bottleneck of the current analytical chemistry, and is one of the difficulties and hot problems of the research of the analytical chemistry. Because the number of samples is extremely large, the content of analytes is lower and lower, and the matrix is more and more complex, the development of an online sample pretreatment technology with high flux, high selectivity and high efficiency is urgently required. At present, a lot of pretreatment equipment such as extraction, separation, concentration and the like exist in the market, but the equipment has independence, does not have integrated operation, still needs to consume manpower and time, and urgently needs integrated pretreatment equipment which integrates the functions of extraction, purification, concentration and the like, is small and exquisite, is simple and convenient and is easy to be directly combined with other analysis instruments.

QuECHERS (Quick, Easy, Cheap, Rugged, Safe) is a rapid sample pretreatment technology for agricultural product detection recently developed internationally, and was developed by the American Ministry of agriculture in 2003. The principle is similar to that of high performance liquid chromatography and solid phase extraction, and the adsorbent packing and the impurities in the matrix are interacted to adsorb the impurities so as to achieve the purpose of impurity removal and purification. Specifically, after a homogenized sample is extracted by acetonitrile, extraction salt is adopted for salting out and layering, a matrix dispersion extraction mechanism is utilized, PSA or other adsorbents are combined with most of interferents (organic acid, fatty acid, carbohydrate and the like) in the matrix, and the interferents are removed in a centrifugal mode, so that the purification purpose is achieved.

Compared with the traditional pretreatment analysis method, the QuECHERS method has the advantages of low sample consumption, less glassware, simple experimental process, reduced workload, improved working efficiency, reduced experimental error caused by factors, no need of a large amount of organic reagents, effective avoidance of secondary pollution to the environment and the like.

Although the QuECHERS method has the advantages, a large amount of time and personnel are still needed, and the problems of poor integration degree and automation degree exist.

Disclosure of Invention

The invention aims to provide a full-automatic QuECHERS experimental device which can replace manpower, effectively improve the accuracy and the efficiency of experiments, avoid human errors, has high integration level and high automation degree, and a method for carrying out experiments by using the full-automatic QuECHERS experimental device.

In order to achieve the purpose, the technical scheme provided by the invention is as follows:

in one aspect, the present invention provides a full-automatic queechers experimental apparatus, wherein: the device comprises a sample and test tube module for simultaneously placing a sample tube, a purification tube and a finished product tube, wherein a sample to be processed is stored in the sample tube;

the multifunctional mechanical arm is provided with a mechanical claw for grabbing and carrying the sample tube or the purification tube or the finished tube and a liquid transfer device, and the liquid transfer device is configured to transfer liquid in the sample tube into the purification tube or transfer liquid in the purification tube into the finished tube;

the screwing module is matched with the multifunctional mechanical arm to realize the unscrewing and screwing of the tube cap of the sample tube, the tube cap of the purification tube or the tube cap of the finished product tube;

a liquid adding module configured to add an extraction liquid into the sample tube;

the sample adding module comprises a salt adding module and a ceramic homogenizing submodule which are used for adding extraction salt and ceramic homogenizing protons into the sample tube respectively;

the oscillation module and the centrifugation module are respectively used for realizing the oscillation and centrifugation of the sample in the sample tube;

the vortex mixing module is used for carrying out vortex mixing on liquid in the purification pipe; and

and the nitrogen blowing concentration module blows nitrogen into the liquid in the finished product pipe to realize anaerobic concentration and enrichment.

The nitrogen blowing concentration module comprises a water bath, a nitrogen blowing instrument and a microprocessor control device for controlling the nitrogen blowing instrument to work;

the nitrogen blowing instrument comprises a gas nozzle, wherein the gas nozzle is configured to blow nitrogen into the finished product pipe, and the blowing direction of the nitrogen is obliquely downward blown to the pipe wall of the finished product pipe;

and in the nitrogen blowing concentration process, the finished product pipe is immersed in a water bath kettle, and the temperature of the liquid in the finished product pipe is controlled by the water bath temperature in the water bath kettle.

The technical scheme of the invention also comprises a suction head module and a suction head recovery box;

the suction head module is provided with a suction head bearing plate, a suction head containing box is arranged on the suction head bearing plate, and a plurality of disposable suction heads are placed in the suction head containing box;

the liquid transfer device can suck the disposable suction head and then suck the liquid in the purification tube through the disposable suction head to transfer the liquid into the finished tube.

The technical scheme of the invention also comprises an XYZ three-axis module which is composed of an X-axis assembly, a Y-axis assembly and a Z-axis assembly;

the Z-axis assembly comprises a Z-axis sliding block and a Z-axis guide rail which are connected with each other, and a Z-axis motor which controls the Z-axis sliding block to move up and down on the Z-axis guide rail, and the multifunctional mechanical arm is arranged on the Z-axis sliding block;

the Z shaft assembly is installed on the Y shaft assembly, the Y shaft assembly is installed on the X shaft assembly, and the X shaft assembly and the Y shaft assembly are used for achieving translation of the multifunctional mechanical arm in the front-back direction and the left-right direction.

The multifunctional mechanical arm comprises a telescopic block connected with a Z-axis sliding block, wherein the telescopic block can move up and down on the Z-axis sliding block in a telescopic manner;

the gripper is connected with Z axle slider, and move liquid device and install on flexible piece, and the gripper during operation moves liquid device and upwards retracts along with flexible piece.

The liquid adding module comprises eight switching valves with eight channels and liquid injection devices, wherein the eight liquid injection devices are arranged at each channel of the switching valves with eight channels in a one-to-one correspondence mode.

The salt adding module is provided with a salt bin, a rotating body and a driving unit for driving the rotating body to rotate from top to bottom in sequence, the bottom of the salt adding module is provided with a salt adding port, the rotating body is provided with a hopper, and the hopper is communicated with the salt bin or the salt adding port along with the rotation of the rotating body;

the rotating body is internally provided with an adjusting block for adjusting the size of the hopper.

The ceramic homogenizing submodule in the technical scheme of the invention comprises a turntable, a turntable motor for driving the turntable to rotate and a supporting plate;

a plurality of storage holes for storing ceramic uniform protons are uniformly arranged on the rotary table in the circumferential direction;

the supporting plate is arranged below the turntable and provided with a blanking hole communicated with the storage hole;

the supporting plate is hinged with a shifting lever, and the shifting lever rotates to block or open the blanking hole.

According to the technical scheme, a blanking sensor for detecting falling of the ceramic homogenized particles is arranged below the blanking hole on the supporting plate.

The screw cap module comprises an opening and closing cap component, the opening and closing cap component is provided with a sample tube screw cap station, a purification tube and a finished product tube screw cap station, friction self-locking sleeves used for fixing the sample tube, the purification tube and the finished product tube are respectively arranged at the sample tube screw cap station, the purification tube and the finished product tube screw cap station, and the friction self-locking sleeves are connected with a driving motor.

The screw capping module further comprises a translation guide rail, a screw capping sliding block arranged on the translation guide rail and a translation motor for driving the screw capping sliding block to translate on the translation guide rail;

the opening and closing cover component is fixedly arranged on the screwing cover sliding block.

The oscillation module comprises an oscillation substrate, an oscillation motor is fixedly arranged on the oscillation substrate, and the oscillation motor is connected with a vertical sliding block through a cam in a matching manner;

the vertical sliding block is fixedly connected with a fastener for clamping a sample tube or a purification tube test tube; the baffle cylinder is hinged with a baffle plate, and the baffle plate cylinder is hinged with a baffle plate;

the baffle is configured to press the sample tube or the purge tube in cooperation with the test tube fastener;

the baffle cylinder is used for realizing that the baffle compresses the sample tube or the purifying tube or turns over to be far away from the sample tube or the purifying tube.

The vortex mixing module comprises a test tube pressing component and a test tube rotating component;

the test tube pressing assembly comprises a pressing sliding block, a pressing cylinder for controlling the pressing sliding block to move up and down, a pressing plate and a pressing plate connected with the pressing plate;

the test tube rotating assembly comprises a vortex motor and a vortex disc, the vortex disc is connected with the vortex motor through a vortex bearing, and a test tube barrel for bearing the purifying tube is connected to the vortex disc;

the platen is configured to compress the purge tube.

The technical scheme of the invention also comprises an ice bath module;

the ice bath module comprises a heat exchanger, a cooling fan, a test tube placing station, a cooling liquid circulating pump and a cooling capacity storage block;

also provided with a refrigeration sheet and heat insulation cotton.

On the other hand, the invention provides an experimental method adopting the full-automatic QuECHERS experimental device, which comprises the following steps:

the first step is as follows: adding liquid and sample into sample tube

(1) The multifunctional mechanical arm moves to the sample tube rack on the XYZ triaxial module, the mechanical claw grabs the sample tube to a sample tube screw-capping station of the screw-capping module, and the cover opening and closing assembly is matched with the mechanical claw to screw off a tube cap of the sample tube;

(2) the opening and closing cover assembly moves on the translation guide rail, the liquid adding module firstly adds extraction liquid into the sample tube, then the opening and closing cover assembly continuously moves to the salt adding module, the salt adding module adds extraction salt into the sample tube, the opening and closing cover assembly continuously moves to the ceramic homogenizing submodule, and the ceramic homogenizing submodule adds ceramic uniform protons into the sample tube;

the second step is that: shaking, mixing and centrifuging the liquid in the sample tube

(1) The cover opening and closing assembly is translated and returned to the initial position, the tube cover of the sample tube is screwed by matching with the mechanical claw, the multifunctional mechanical arm moves on the XYZ three-axis module, and the mechanical claw grabs the sample tube and sends the sample tube to the oscillation module for oscillation and uniform mixing;

(2) the multifunctional mechanical arm continuously moves on the XYZ three-axis module, and the mechanical claw grabs the sample tube and conveys the sample tube to the centrifugal module for centrifugation;

(3) the mechanical claw grabs the sample tube and moves the sample tube to a sample tube screw-capping station of the screw-capping module;

the third step: first pipetting

(1) The mechanical claw is matched with the opening and closing cover component to unscrew the tube cover of the sample tube;

(2) the multifunctional mechanical arm moves on the XYZ three-axis module, and the mechanical claw grabs the purifying tube and sends the purifying tube to a purifying tube of a screw capping module and a finished product tube screw capping station;

(3) the mechanical claw is matched with the opening and closing cover component to unscrew the pipe cover of the purification pipe;

(4) the liquid transferring device transfers the supernatant liquid in the sample tube into the purifying tube;

(5) the mechanical claw is matched with the opening and closing cover component to screw down the pipe cover of the purifying pipe;

the fourth step: vortex mixing

(1) The multifunctional mechanical arm continuously moves on the XYZ triaxial module, and the mechanical claw grabs the purifying pipe and sends the purifying pipe to the vortex mixing module for vortex mixing;

(2) the multifunctional mechanical arm sends the purifying pipe to a purifying pipe of the screw capping module and a finished product pipe screw capping station;

(3) the mechanical claw is matched with the opening and closing cover component to unscrew the pipe cover of the purification pipe;

the fifth step: second pipetting

(1) The multifunctional mechanical arm moves on the XYZ three-axis module, and the mechanical claw grabs the finished product tube and sends the finished product tube to a purification tube of the screw capping module and a screw capping station of the finished product tube;

(2) the mechanical claw is matched with the opening and closing cover component to unscrew a pipe cover of the finished pipe;

(3) the multifunctional mechanical arm moves, the liquid transfer device is moved to the position above the sucker module, and the disposable sucker is sucked by the liquid transfer device;

(4) the liquid transfer device drives the disposable suction head to pump the supernatant in the purifying tube to the finished product tube;

(5) screwing down pipe covers of the purification pipe and the finished product pipe, and respectively conveying the purification pipe and the finished product pipe to a purification pipe frame and a finished product pipe frame;

and a sixth step: nitrogen-blown concentration

(1) And blowing nitrogen into the finished product pipe to perform nitrogen blowing concentration on the liquid in the finished product pipe.

In conclusion, the invention has the following beneficial effects:

(1) when the device is used for an experiment, the multifunctional mechanical arm carries a sample tube to the position of the screw cap module by the sample adding and test tube module, the mechanical claw and the screw cap assembly are matched to screw the tube cap of the sample tube, extract liquor, extraction salt and ceramic uniform protons are sequentially added into the sample tube through the liquid adding module, the salt adding module and the ceramic homogenizing submodule, the tube cap is screwed, and the sample tube is vibrated and centrifuged through the vibrating module and the centrifuging module; the liquid transfer device transfers the supernatant in the sample tube into the purification tube, then the vortex mixing module performs vortex mixing, and then transfers the supernatant in the purification tube into the finished product tube to perform anaerobic concentration and enrichment through the nitrogen blowing concentration module (the screwing and unscrewing actions on the tube cover of the sample tube, the tube cover of the purification tube and the tube cover of the finished product tube in the whole process are omitted and not described in detail).

The whole process has high experiment automation degree, high experiment efficiency and high reliability; meanwhile, a nitrogen blowing concentration module is innovatively added, a finished product pipe does not need to be manually conveyed to a special nitrogen blowing instrument for concentration, and the full automation of the experimental process is realized.

(2) In the process of nitrogen-blowing anaerobic concentration and enrichment, nitrogen is blown to the liquid surface in a finished tube rapidly and continuously by using a nitrogen blowing instrument, so that a solvent in the liquid is rapidly evaporated and separated, thereby realizing the concentration of a sample, on one hand, the purity of the liquid sample is maintained, and the effect of rapid separation and purification is achieved; on the other hand, nitrogen can play a role in isolating oxygen and preventing oxidation.

The setting of nitrogen gas appearance gas nozzle blowing direction for the nitrogen gas stream that the gas nozzle blew out forms the heliciform air current in the concentration pipe, effectively increases and sweeps the area, has slowed down the air current impulsive force, makes solvent in the liquid in the finished tube evenly volatilize and do not splash.

Before the liquid transfer device moves the supernatant in the purifying tube to the finished tube, the disposable suction head in the suction head module can be sucked firstly, the supernatant is sucked by the disposable suction head to be moved to the finished tube, and the phenomenon that the liquid transfer device has residue to pollute the supernatant in the purifying tube after moving the liquid sample in the sample tube is avoided, so that the experimental result is influenced.

The setting of XYZ triaxial module can realize the removal of multi-functional arm front and back, left and right sides and upper and lower direction, and then has guaranteed that multi-functional arm snatchs sample cell or purifying tube or finished product pipe can move to suitable position towards a plurality of directions, has reduced artificial transport. And Z axle motor can drive the slider and reciprocate, and when the gripper snatched sample cell or purge tube or finished product pipe, the liquid-transfering device was in the state of upwards retracting, and the liquid-transfering device during operation was in the state of stretching out downwards, and gripper and liquid-transfering device can not mutual interference.

When the liquid adding module adds the extraction liquid into the sample tube, liquid adding devices can be correspondingly and uniformly installed in each channel of the eight-channel switching valve one by one, and supply of eight kinds of solution can be realized.

The whole salt adding action is completed by controlling the rotating body to rotate by the driving unit to drive the hopper to rotate, namely, salt in the salt bin falls into the hopper when the hopper is communicated with the salt bin, and the salt falls into the sample tube when the hopper rotates to be communicated with the salt adding port, so that the salt adding is not required to be manually operated, and the automation of the salt adding work is completed. The adjustable hopper size of regulating block, and then make the salt addition volume controllable adjustable.

When the equal proton of pottery is added to the pottery homogeneity submodule piece, also rotate through carousel motor drive carousel, it is intraductal to deposit the automatic sample that falls into via the blanking hole of the equal proton of downthehole pottery, whether blanking sensor response has the pottery homogeneity son to fall down and feed back to carousel motor drive carousel and rotate, need not manual operation, degree of automation is high.

And the setting of friction self-locking cover in the screw capping module has avoided second driving motor drive screw capping module during operation sample pipe or purge tube or finished product pipe to skid motionlessly on the screw capping module, and it is unsuccessful that the test tube lid is screwed up to appear, and easy pine takes off, leads to the experiment to need to stop, the condition of manual intervention.

Drawings

FIG. 1 is a schematic diagram of the internal structure of a full-automatic QuECHERS experimental device according to the present invention;

FIG. 2 is a top view of the interior of a fully automated QuECHERS assay device of the present invention;

FIG. 3 is a schematic diagram of the operation of a fully automatic QuECHERS experimental apparatus;

FIG. 4 is a schematic diagram of a sample and cuvette module according to an embodiment;

FIG. 5 is a schematic structural diagram of an XYZ triaxial module in the embodiment;

FIG. 6 is a schematic structural diagram of a Z-axis module in the XYZ triaxial module in the embodiment;

FIG. 7 is a schematic structural view of the multi-functional robot arm in the embodiment;

FIG. 8 is a schematic structural view of a screw-on module in the embodiment;

figure 9 is a partial cross-sectional view of the screw-on module of the embodiment;

FIG. 10 is a schematic view of a sample addition module in an example;

FIG. 11 is a sectional view of a salting module in an embodiment;

FIG. 12 is a schematic structural diagram of a ceramic homogenizing submodule in an embodiment;

FIG. 13 is a schematic structural diagram of an oscillation module according to an embodiment;

FIG. 14 is a schematic structural view of a centrifuge module according to an embodiment;

FIG. 15 is a schematic view of a vortex blending module in an embodiment;

FIG. 16 is a diagram showing the connection between the vortex mixer module and the purge tube in the example;

FIG. 17 is a schematic view of a tip module according to an embodiment;

FIG. 18 is a schematic diagram of nitrogen purge concentration module in the embodiment;

FIG. 19 is a schematic diagram of the ice bath module in the example.

In the figure:

01. a sample and tube module; 101. a sample pipe frame; 201. a purification pipe frame; 301. a finished pipe frame; 401. a tube support;

02. an XYZ triaxial module; 102. an X-axis assembly; 202. a Y-axis assembly; 302. a Z-axis assembly; 3021. a Z-axis motor; 3022. a Z-axis guide rail; 3023. a Z-axis slide block;

03. a multifunctional mechanical arm; 103. a telescopic block; 203. a pipetting device; 303. a gripper;

04. screwing the cover module; 104. a translation motor; 204. screwing a cover slide block; 304. a translation guide rail; 404. opening and closing the cover assembly; 4041. a sample tube screw-capping station; 4042. the cleaning pipe and the finished product pipe are screwed on the station; 4043. a friction self-locking sleeve; 4044. a drive motor;

05. a liquid adding module;

06. a sample adding module; 106. a liquid adding head; 206. a sample adding support;

07. a salt adding module; 107. a salt bin; 207. a rotation driving unit; 307. a rotating body; 3071. a hopper; 407. an adjusting block; 507. adding salt;

08. a ceramic homogenizing submodule; 108. a turntable motor; 208. a turntable; 2081. a storage hole; 308. a support plate; 3081. a blanking hole; 408. a blanking sensor; 508. a deflector rod;

09. a vibration module; 109. a baffle plate; 209. a baffle cylinder; 309. a vibration motor; 409. a test tube fastener; 509. a vertical slider; 609. oscillating the substrate; 709. a shock-absorbing foot pad;

10. a centrifuge module; 110. a door slide rail; 210. a door opening and closing cylinder; 310. a centrifugal rotor; 410. a taking and placing port;

11. a vortex blending module; 111. pressing a plate; 211. a platen; 311. a pressing cylinder; 411. pressing the sliding block; 511. testing the tube barrel; 611. a vortex motor; 711. a vortex bearing; 811. a swirling disc;

12. a suction head module; 112. a suction head bearing plate; 212. a suction head box; 312. a disposable tip; 412. an internal standard solution cup; 512. a fixed block;

13. an ice bath module; 113. a heat exchanger; 213. a cold storage block; 313. heat insulation cotton; 413. a coolant circulation pump; 513. a refrigeration plate; 613. and a test tube placing station.

Detailed Description

The present invention will be described in further detail with reference to the accompanying drawings.

The invention provides a full-automatic QuECHERS experimental device, which comprises a sample and test tube module 01, an XYZ triaxial module 02, a multifunctional mechanical arm 03, a screw cap module 04, a liquid adding module 05, a salt adding module 07, a ceramic homogenizing submodule 08, a shaking module 09, a centrifugal module 10, a vortex mixing module 11, a nitrogen blowing concentration module, a bottom plate and a support as shown in figures 1 and 2. Wherein, as shown in fig. 4, sample and test tube module 01 includes sample pipe support 101, purification pipe support 201 and finished product pipe support 301, and sample pipe support 101, purification pipe support 201 and finished product pipe support 301 horizontal direction arrange in proper order and through pipe support 401 fixed mounting on the bottom plate, and concrete mounting means is: the pipe support 401 is fixedly connected to the bottom plate through screw threads, a positioning groove is formed in the pipe support 401, positioning pins matched with the positioning grooves are arranged on the sample pipe support 101, the purification pipe support 201 and the finished product pipe support 301, the sample pipe support 101, the purification pipe support 201 and the finished product pipe support 301 are inserted into the corresponding positioning grooves through the positioning pins to complete the fixed connection with the pipe support 401, and the sample pipe support 101, the purification pipe support 201 and the finished product pipe support 301 are fixedly installed on the pipe support 401 in a drawer type; the sample pipe frame 101, the purification pipe frame 201 and the finished product pipe frame 301 are all provided with a plurality of test tube fixing positions; the sample tube rack 101 is used for accommodating a plurality of sample tubes, and the sample tubes are filled with samples to be processed; the purge tube rack 201 and the product tube rack 301 accommodate a plurality of purge tubes and product tubes, respectively (hereinafter, sample tubes, purge tubes, and product tubes may be collectively referred to as test tubes).

Fig. 5 illustrates a schematic representation of the XYZ tri-axial module 02, as can be seen in fig. 1 and 5, the XYZ tri-axial module 02 is mounted on a support, comprising the X-axis assembly 102, the Y-axis assembly 202 and the Z-axis assembly 302; the X-axis assembly 102 comprises two horizontal X-axis guide rails which are arranged on the bracket in parallel, the two X-axis guide rails are connected by a connecting rod and driven synchronously, X-axis sliding blocks are arranged on the two X-axis guide rails in a matched mode, and the connecting rod is connected with an X-axis guide rail driving motor in a matched mode; and opening the X-axis guide rail driving motor, driving the connecting rod to move by the X-axis guide rail driving motor, and synchronously driving the two X-axis guide rails to move by the connecting rod, so that the X-axis sliding block relatively moves horizontally on the X-axis guide rails. The Y-axis assembly 202 is horizontally provided with a Y-axis guide rail, but the Y-axis guide rail is arranged in the direction vertical to the X-axis guide rail; the Y-axis assembly 202 can slide on the X-axis guide rail along the length direction of the X-axis guide rail, and the specific mode is that two ends of the Y-axis guide rail are correspondingly and fixedly connected to X-axis sliding blocks on the two X-axis guide rails, the X-axis guide rail moves, and when the X-axis sliding blocks move relative to the X-axis guide rail, the Y-axis assembly 202 is driven to move along the X-axis sliding rail direction; the Y-axis assembly 202 further includes a Y-axis rail drive motor for driving the movement of the Y-axis rail. A Y-axis sliding block which can move along the length direction of the Y-axis guide rail relative to the Y-axis guide rail is arranged on the Y-axis guide rail in a matched mode, and the Z-axis assembly 302 is fixedly connected to the Y-axis sliding block and can move along the length direction of the Y-axis guide rail along with the Y-axis sliding block; as shown in fig. 6, the Z-axis assembly 302 includes a Z-axis motor 3021 and a Z-axis guide rail 3022 driven by the Z-axis motor 3021, and the Z-axis guide rail 3022 is arranged in a vertical direction; a Z-axis slider 3023 that moves up and down with respect to the Z-axis guide 3022 is fitted to the Z-axis guide 3022.

The multifunctional mechanical arm 03 is fixedly arranged on a Z-axis sliding block 3023 and drives an X-axis guide rail driving motor, the X-axis sliding block moves along the length direction (hereinafter referred to as the front-back direction) of the X-axis guide rail to drive the Y-axis assembly 202, the Z-axis assembly 302 fixedly connected with the Y-axis sliding block and the multifunctional mechanical arm 03 connected with the Z-axis assembly 302 to move in the front-back direction; a Y-axis guide rail driving motor is driven, a Y-axis sliding block moves along the length direction (hereinafter referred to as the left-right direction) of the Y-axis guide rail, and drives the Z-axis assembly 302 and the multifunctional mechanical arm 03 connected with the Z-axis assembly 302 to move in the left-right direction together; the Z-axis motor 3021 is driven, and the Z-axis slider 3023 moves in the longitudinal direction (hereinafter referred to as the vertical direction) of the Z-axis guide rail 3022, thereby driving the multifunctional robot arm 03 to move in the vertical direction together.

Fig. 7 is a schematic structural diagram of the multifunctional mechanical arm 03, and as shown in fig. 7, the multifunctional mechanical arm 03 comprises a telescopic block 103, a pipetting device 203, a mechanical claw 303 for gripping a test tube, and a mounting plate fixedly connected with a Z-axis slide block. The telescopic block 103 and the mechanical claw 303 are fixedly connected with the Z-axis sliding block 3023 through a mounting plate; the liquid transfer device 203 is arranged on the telescopic block 103, when the mechanical claw 303 grabs the test tube to work, the liquid transfer device 203 retracts upwards along with the telescopic block 103, and when the liquid transfer device 103 transfers the sample liquid, the liquid transfer device 103 extends out along with the telescopic block 103; the pipetting device 103 may employ a pipette.

As shown in fig. 8, the screw-capping module 04 includes the translation motor 104, a translation guide rail 304 driven by the translation motor 104, and the screw-capping slider 204 installed in cooperation with the translation guide rail 304 and relatively sliding on the translation guide rail 304, and further includes an opening and closing cap assembly 404 fixedly installed on the screw-capping slider 204; the translation motor 104 works to drive the screw capping slide block 204 to move along the length direction of the translation guide rail 304 relative to the translation guide rail 304, and further drive the cover opening and closing assembly 404 to move along the length direction of the translation guide rail 304; the opening and closing cap assembly 404 is provided with a sample tube screw-capping station 4041, a purification tube and a finished tube screw-capping station 4042; friction self-locking sleeves 4043 for fixing the sample tube, the purification tube and the finished product tube are respectively installed at the sample tube screwing-cover station 4041, the purification tube and the finished product tube screwing-cover station 4042, the friction self-locking sleeves 4043 are connected with a driving motor 4044, and the specific connection installation mode is shown in fig. 9. The test tube is fixed in sample cell screw capping station 4041 or the friction self-locking cover 4043 of purge tube and finished product tube screw capping station 4042, and driving motor 4044 drive friction self-locking cover 4043 rotates, and the test tube can follow the friction from the rotation of self-locking cover 4043 under the drive of the frictional force with friction self-locking cover 4043.

The liquid adding module 05 comprises an eight-channel switching valve and a liquid injecting device, the liquid injecting device comprises a stepping motor, a precise screw rod and a microsyringe, and the stepping motor drives the precise screw rod to drive the microsyringe to supply extraction liquid; the liquid injection device is provided with eight liquid injection devices, the eight liquid injection devices are correspondingly arranged at eight channels of the eight-channel switching valve one by one, different extraction liquids can be added into different liquid injection devices, the eight-channel switching valve is used for switching different extraction liquid channels, and the supply of eight extraction liquids can be realized at most. In addition, the liquid adding module 05 of the invention can be provided with an automatic cleaning device (not shown in the figure), and the automatic cleaning is carried out after the eight-channel switching valve is controlled by an intelligent control program to switch the extraction liquid; the microsyringe can be controlled to supply a maximum of 25ml at a time to meet the requirements of the instrument.

The sample adding module 06 comprises a salt adding module 07 and a ceramic homogenizing submodule 08 which are used for respectively adding extraction salt and ceramic homogenizing protons into the sample tube, and further comprises a sample adding bracket 206; the salt adding module 07 and the ceramic homogenizing submodule 08 are both arranged on the sample adding bracket 206; the sample adding bracket 206 is also provided with a sample adding head 106, the sample adding head 106 is communicated with the sample adding module 05, namely a microsyringe in the sample adding module 05 is communicated with the sample adding head 106 through a pipeline (not shown in the figure), and an extract liquid pushed out by the microsyringe flows to the sample adding head 106 through the pipeline for liquid adding; referring to fig. 1 and 10, the sample-adding bracket 206 is fixedly mounted on the bottom plate, and the screw-capping module 04 is sleeved by the sample-adding bracket 206, that is, the translation guide rail 304 of the screw-capping module 04 is located below the sample-adding module 06, the sample-adding head 106, the salt-adding module 07 and the ceramic homogenizing submodule 08 are sequentially mounted on the sample-adding bracket 206 along the length direction of the translation guide rail 304, and the cover-opening and closing assembly 404 moves along the length direction of the translation guide rail 304 and can sequentially move to a position below the sample-adding head 106, a position below the salt-adding module 07 and a position below the ceramic homogenizing submodule 08.

The structural schematic diagram of the salt adding module 07 is shown in fig. 11, and the salt adding module includes a salt bin 107, a rotating body 307, and a driving unit 207 for driving the rotating body 307 to rotate, and the bottom of the salt adding module 07 is further provided with a salt adding port 507. The specific implementation mode is as follows: the salt adding module 07 comprises a cylindrical barrel, the hollow cylindrical barrel is provided with a salt bin 107 inside, the top of the cylindrical barrel is provided with a blocking cover in a matching way, and extracted salt can be added into the salt bin 107 by opening the blocking cover; the bottom of the cylindrical barrel is connected with the rotating body 307, a hopper 3071 is arranged on the rotating body 307, and the hopper 3071 can rotate along with the rotating body 307; a salt outlet part is connected to the lower side of the rotating body 307, a salt adding port 507 is formed in the salt outlet part, and when the hopper 3071 rotates along with the rotating body 307, the opening of the hopper 3071 can rotate to the salt bin 107 to be communicated or be communicated with the salt adding port 507; an adjusting block 407 is further arranged in the rotating body 307, and the size of the hopper 3071 can be adjusted by the adjusting block 407, so that the amount of the added extraction salt falling from the hopper 3071 through the salt adding port 507 can be adjusted.

The working principle of the salt adding module 07 is as follows: the driving unit 207 drives the rotating body 307 to rotate until the hopper 3071 is communicated with the salt bin 107 (namely the opening of the hopper 3071 is upward), the blocking cover is opened, the extraction salt is added into the salt bin 107 and enters the hopper 3071, then the driving unit 207 drives the rotating body 307 to rotate, the rotation is generally 180 degrees, the hopper 3071 rotates along with the rotation until the opening of the hopper 3071 is communicated with the salt adding port 507, at the moment, the extraction salt in the hopper 3071 falls through the salt adding port 507 under the action of gravity to add salt, then the hopper 3071 resets under the action of a spring, and the next salt adding is waited; when the salt adding amount needs to be adjusted, the adjustment block 407 can be directly adjusted to change the size of the hopper 3071.

As shown in fig. 12, the ceramic homogenizing submodule 08 includes a turntable 208, a turntable motor 108 for driving the turntable 208 to rotate, and a supporting plate 308; the supporting plate 308 is fixedly connected with the sample adding support 206, a plurality of storage holes 2081 used for storing ceramic protons are arranged on the turntable 208 in the circumferential direction, blanking holes 3081 which can be communicated with the storage holes 2081 are formed in the supporting plate 308, and when the turntable 208 rotates, each storage hole 2081 can rotate until the blanking holes 3081 are communicated with the blanking holes 3081; a shifting lever 508 is hinged on the supporting plate 308, the shifting lever 508 can rotate around a hinged shaft hinged with the supporting plate 308, and the shifting lever 508 rotates and is positioned below the blanking hole 3081 to abut against the supporting plate 308 and block the blanking hole 3081; a blanking sensor 408 is also mounted on the support plate 308 for detecting whether any ceramic protons fall from the blanking hole 3081.

The working principle of the ceramic homogenizing submodule 08 is as follows: when the device does not work, the deflector rod 508 blocks the blanking hole 3081 on the turntable 308; when ceramic protons need to be added into the sample tube, the screw-on module 04 moves to a position below the ceramic homogenizing submodule 08, the screw-on module 04 triggers the shift lever 508, the shift lever 508 rotates to open the blanking hole 3081, and the ceramic protons added into the storage hole 2081 fall into the sample tube on the screw-on module 04 through the blanking hole 3081; when the falling motion of the ceramic homogeneous protons is not detected by the blanking sensor 408, the turntable motor 108 drives the turntable 208 to rotate until the other storage hole 2081 is communicated with the blanking hole 3081, the falling motion of the ceramic homogeneous protons is not detected by the blanking sensor 408, and the turntable 208 rotates until the falling motion of the ceramic homogeneous protons is detected by the blanking sensor 408.

Fig. 13 shows a structure of the oscillating module 09, which includes an oscillating substrate 609, an oscillating motor 309 is mounted on the oscillating substrate 609, the oscillating motor 309 is connected to the vertical slider 509 through a cam, that is, the oscillating motor 309 is connected to a cam, the cam abuts against the vertical slider 509, the cam is driven by the oscillating motor 309 to rotate, and the vertical slider 509 is driven to reciprocate up and down in the rotating process; the oscillation module 09 further comprises a baffle cylinder 209, a baffle 109 connected with the baffle cylinder 209, and a test tube fastener 409 fixedly connected to the vertical sliding block 509; the baffle cylinder 209 is hinged with the baffle 109 and the vertical slide 509, and the baffle 109 is used for pressing or loosening the test tube fastened by the test tube fastener 409. Shock module 09 still can set up shock attenuation callus on the sole 709 shock attenuation, and shock attenuation callus on the sole 709 direct mount can vibrate base plate 609 below.

The operating principle of the oscillation module 09 is as follows: initially, the oscillating motor 309 and the baffle cylinder 209 do not work, and the baffle 109 is in a vertical state; when multifunctional machine arm 03 snatchs the test tube and moves to test tube fastener 409 department, baffle cylinder 209 extension, baffle 109 rotates into the test tube that test tube fastener 409 department was pushed down to horizontal state, then vibrates motor 309 work and drives vertical slider 509 up-and-down reciprocating motion, and test tube fastener 409 is followed up-and-down reciprocating motion and is accomplished the vibration action.

As shown in fig. 14, the centrifugal module 10 includes a centrifugal cover, the centrifugal cover is provided with a pick-and-place port 410, a door slide rail 110 is installed at the pick-and-place port 410, and a door opening and closing (not shown) is installed in a matching manner, the door opening and closing is connected to a door opening and closing cylinder 210, the door opening and closing cylinder 210 extends out to drive the door opening and closing to slide on the door slide rail 110 to close the pick-and-place port 410, and the door opening and closing cylinder 210 retracts to drive the door opening and closing to slide on the door slide rail 110 to open the; be provided with centrifuge rotor 310 in the centrifugal protecting cover, centrifuge rotor 310 has the locate function on the circumference, gets when putting the test tube, and the test tube location is getting under mouthful 410 and open the switch door.

As shown in fig. 15, the vortex blending module 11 includes a test tube compressing assembly and a test tube rotating assembly, the test tube compressing assembly includes a mounting frame, a pressing plate 111, a pressing plate 211, a compressing cylinder 311, and a compressing slider 411; the pressing plate 211 is fixedly connected to the pressing plate 111, the pressing plate 111 is hinged to the pressing slider 411, and the pressing plate 111 can rotate 90 degrees from a vertical state to be in a horizontal state; the compressing slider 411 is connected with the mounting frame in a sliding manner, specifically, a guide post is mounted on the mounting frame, the compressing slider 411 is sleeved on the guide post, and the compressing cylinder 311 is connected with the compressing slider 411 for controlling the compressing slider 411 to move up and down. Test tube rotating assembly includes vortex motor 611, vortex plate 811, and test tube barrel 511, and fig. 16 shows the mounting structure of test tube rotating assembly, vortex plate 811 is connected with vortex motor 611 through vortex bearing 711 and eccentric shaft (not shown), and test tube barrel 511 is mounted on vortex plate 811.

The working principle of the vortex mixing module 11 is as follows: the test tube moves earlier in test tube barrel 511 and vortex dish 811 butt, compresses tightly cylinder 311 and drives and compress tightly slider 411 downstream, and 90 degrees downstream are overturned again to the clamp plate 111 earlier, and clamp plate 111 overturns to the horizontality by vertical state, and pressure disk 211 overturns thereupon to the test tube that the dish mouth aimed at in test tube barrel 511 and compresses tightly, and vortex motor 611 starts, drives the eccentric shaft and rotates, and the eccentric shaft drives vortex dish 811 again and rotates, and then accomplishes the vortex mixing operation of the interior liquid of test tube.

The suction head module 12, as shown in fig. 17, comprises a suction head bearing plate 112, a suction head containing box 212 is arranged on the suction head bearing plate 112, a fixing block 512 for pressing and fixing the suction head containing box 212 is also arranged, and a plurality of disposable suction heads 312 are arranged in the suction head containing box 212; the pipetting device 203 may aspirate a disposable tip 312 and then aspirate the fluid in the test tube into the disposable tip 312; a tip recovery cassette is also provided on the base plate, which is located below the clean-up tube rack 201 in the sample and tube module 01, into which the used disposable tips 312 can be moved by the pipetting device 203.

An internal standard solution cup 412 is also arranged on the suction head module 12, and an internal standard solution can be added into the internal standard solution cup 412, sucked by the pipetting device 203 and added into a corresponding test tube.

The nitrogen blowing concentration module comprises a water bath, a nitrogen blowing instrument and a microprocessor control device for controlling the nitrogen blowing instrument to work, and the nitrogen blowing instrument comprises a gas nozzle; fig. 18 shows a schematic diagram of nitrogen-blowing concentration and enrichment of the liquid in the finished tube by the nitrogen-blowing concentration module, wherein a gas nozzle is arranged in an obliquely downward direction, nitrogen blown out by a nitrogen blower is obliquely blown downward to the tube wall of the finished tube through the gas nozzle, the finished tube is immersed in a water bath kettle, the temperature of the liquid in the finished tube is controlled by the water bath temperature in the water bath kettle, and the water bath temperature is controlled from 30 ℃ to 60 ℃ at a certain temperature of a sample, so that a good enrichment effect can be obtained by nitrogen-blowing; the gas nozzle is arranged in a specific direction, and the blown nitrogen flow forms a spiral air flow in the finished product pipe, so that the blowing area is effectively increased, the air flow chongli is slowed down, and the solvent is uniformly volatilized and does not splash; the nitrogen blowing instrument based on the principle is available on the market and can be directly purchased and used, such as the NS-12S type nitrogen blowing instrument.

Further, the invention also comprises an ice bath module 13, the structural schematic diagram of the ice bath module 13 is shown in fig. 19, and the ice bath module comprises a test tube placing station 613 for placing a test tube, a cold storage block 213 positioned at the test tube placing station 613, and heat insulation cotton 313 wrapping the cold storage block 213, when the test tube is positioned at the test tube placing station 613, the cold storage block 213 surrounds the test tube to transfer cold to the test tube, and the heat insulation cotton 313 separates external hot gas to avoid the rapid temperature change of the cold storage block 213, thereby improving the refrigeration efficiency; the ice bath module 13 further comprises a cooling liquid circulating pump 413, a refrigerating piece 513 is arranged on the cooling liquid circulating pump 413, the refrigerating storage block 213 is located on the refrigerating piece 513, the refrigerating piece 513 enables the temperature of the refrigerating storage block 213 to be reduced, and a temperature probe can be designed to detect the temperature; the ice bath module 13 further includes a heat exchanger 113 and a heat dissipation fan (not shown), the heat dissipation fan is installed on the heat exchanger 113 through a mounting member, heat of the cooling plate 513 is transferred to the heat exchanger 113 by the cooling liquid circulation pump 413, and the heat dissipation fan cools and dissipates the heat.

The invention also provides an experimental method of the full-automatic QuECHERS experimental device, as shown in figure 3, the working principle and the working steps comprise liquid adding, sample adding, shaking, centrifuging, liquid transferring, vortex mixing, liquid transferring and nitrogen blowing concentration; wherein the liquid adding operation comprises the following steps:

firstly, the XYZ triaxial module 02 moves to control the multifunctional mechanical arm 03 to move back and forth, left and right or up and down to the position above the sample tube rack 101, the mechanical claw 303 grabs a sample tube filled with a sample to be detected, the XYZ triaxial module is controlled to move to enable the multifunctional mechanical arm 03 to move to the screw-on cover module 04, the mechanical claw 303 moves the sample tube to the sample tube screw-on cover station 4041 of the open-close cover component 404, the mechanical claw 303 grabs a tube cover of the sample tube, then the driving motor 4044 of the open-close cover component 404 works to drive the friction self-locking sleeve 4043 to rotate to drive the sample tube to rotate until the tube cover of the sample tube; at this time, the translation motor 104 of the screw-capping module 04 operates to drive the translation guide rail 304 to move to drive the screw-capping slider 204 to move, at this time, the cap opening and closing assembly 404 moves along the translation guide rail 304 until the sample tube with the tube cap unscrewed is located below the liquid adding head 106, the liquid adding module 05 is opened, and the liquid injecting device of the liquid adding module 05 injects an extract liquid into the sample tube through the liquid adding head 106.

The sample adding step comprises the following steps:

the translation motor 104 works, the cover opening and closing assembly 404 continues to move until the sample tube moves to a position below a salt adding port 507 of the salt adding module 07, at the moment, extraction salt is added in the salt bin 107, then the rotation driving unit 207 works to drive the rotating body 307 to rotate, and the extraction salt in the hopper 3071 rotates to fall into the sample tube through the salt adding port 507 to finish the sample adding of the extraction salt; the translation motor 104 works, the cover opening and closing assembly 404 continues to move until the cover opening and closing assembly 404 moves to the poking rod 508 of the ceramic homogenizing submodule 08 to open the poking rod 508, and the ceramic protons in the storage hole 2081 fall into the sample tube through the blanking hole 3081 to finish the sample adding of the ceramic protons.

The vibration and centrifugal operation comprises the following steps:

firstly, the translation motor 104 works, the cover opening and closing component 404 moves until the cover opening and closing component 404 is reset to the initial position, and at the moment, the mechanical claw 303 and the friction self-locking sleeve 4043 driven by the driving motor 4044 are matched to screw the tube cover of the sample tube on the sample tube; then gripper 303 snatchs the sample cell after, multi-functional arm 03 removes until moving the sample cell to vibrate module 09, and the sample cell is fixed by test tube fastener 409, and baffle 109 compresses tightly the sample cell, vibrates motor 309 work and drives vertical slider 509 up-and-down reciprocating motion, drives and vibrates base plate 609 and sample cell up-and-down reciprocating motion and accomplishes vibration operation.

After the sample tube finishes the oscillation operation in the oscillation module 09, the gripper 303 grabs the sample tube, the multifunctional mechanical arm 03 moves on the XYZ triaxial module 02 until the sample tube is moved into the centrifugal module 10 for centrifugation, the operation of the door opening and closing cylinder 210 is controlled to open the door, the sample tube is positioned and placed under the access port 410, and then the door opening and closing is closed to perform the centrifugation operation on the sample tube.

The first pipetting operation comprises the following steps:

after the sample tube finishes centrifugal operation, the mechanical claw 303 grabs the sample tube and is moved to a sample tube screw-on station 4041 of the cover opening and closing component 404 by the multifunctional mechanical arm 03, the mechanical claw 303 cooperates with the cover opening and closing component 404 to screw off the tube cover of the sample cover, then the mechanical claw 303 moves to the purification tube rack 201 to grab the purification tube, the multifunctional mechanical arm 03 moves to move the purification tube to the purification tube of the cover opening and closing component 404 and the product tube screw-on station 4042, the mechanical claw 303 cooperates with the cover opening and closing component 404 to screw off the tube cover of the purification tube, at the moment, the pipetting device 203 starts to work, the pipetting device 203 moves to the sample tube to suck the supernatant in the sample tube and moves into the purification tube, finally, the mechanical claw 303 cooperates with the cover opening and closing component 404 to screw down the tube covers of the sample tube and the purification tube successively, so far, the first pipetting work is completed, and the supernatant in the sample tube.

After supernatant in the sample tube is moved into the purification tube, vortex mixing needs to be carried out on liquid in the purification tube, and the vortex mixing steps are as follows:

the mechanical claw 303 grabs the purification tube and moves the purification tube to the vortex mixing module 11, the purification tube is placed in the test tube barrel 511, the pressing cylinder 311 works to enable the pressure plate 211 to press the purification tube, and the vortex motor 611 drives the vortex disk 811 to rotate, so that vortex mixing of the purification tube is completed.

The purge tube that completes the vortex mixing operation needs to be returned by the multifunctional robot arm 03 to the purge tube and production tube screw-capping station 4042 of the retractable lid assembly 404 for a second pipetting action.

During the second pipetting, the mechanical claw 303 is matched with the opening and closing cover assembly 404 to unscrew the tube cover of the purification tube, then the multifunctional mechanical arm 03 moves and grabs the finished tube, the finished tube is moved to the purification tube and finished tube screwing station 4042, and the finished tube cover is unscrewed; then the multifunctional mechanical arm moves to the suction head module 12, the liquid-moving device 203 sucks one disposable suction head 312 and then moves to the position of a purification tube, the liquid-moving device 203 works, and the disposable suction head 312 sucks the supernatant in the purification tube and moves the supernatant into a finished tube; finally, the gripper 303 cooperates with the opening and closing cap assembly 404 to sequentially complete the tightening of the tube caps of the purification tubes and the tube caps of the finished tubes.

After the second pipetting action is completed, the multi-function robotic arm 03 moves to drop the disposable tips 312 into a tip retrieval box.

The nitrogen-blowing concentration operation comprises the following steps:

the multifunctional mechanical arm 03 moves the finished product pipe to the nitrogen blowing concentration module, unscrews a pipe cover of the finished product pipe, opens a nitrogen blowing instrument in the nitrogen blowing concentration module, and blows nitrogen into the finished product pipe by the nitrogen blowing instrument for concentration and enrichment; in the process, the water bath kettle can be heated until the water bath temperature is controlled within the range of 30 ℃ to 60 ℃, and the temperature in the finished product pipe is controlled by heat transfer, so that the concentration and enrichment efficiency is improved.

The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may occur to those skilled in the art without departing from the principle of the invention, and are considered to be within the scope of the invention.

Claims (12)

1. A full-automatic QuECHERS experimental apparatus is characterized in that: comprises a sample and test tube module (01) for simultaneously placing a sample tube, a purification tube and a finished product tube, wherein the sample tube is internally provided with a sample to be processed;

the multifunctional mechanical arm (03) is provided with a mechanical claw (303) for grabbing and carrying the sample tube or the purification tube or the finished tube and a liquid transfer device (203), and the liquid transfer device (203) is configured to transfer liquid in the sample tube into the purification tube or transfer liquid in the purification tube into the finished tube;

the screwing and capping module (04) is matched with the multifunctional mechanical arm (03) to realize screwing and unscrewing of a tube cap of the sample tube, a tube cap of the purification tube or a tube cap of the finished product tube;

a liquid adding module (05) configured to add an extraction liquid into the sample tube;

the sample adding module (06) comprises a salt adding module (07) and a ceramic homogenizing submodule (08) which are used for respectively adding extraction salt and ceramic homogenizing protons into the sample tube;

the oscillation module (09) and the centrifugation module (10) are respectively used for realizing sample oscillation and centrifugation in the sample tube;

the device also comprises a vortex mixing module (11) for mixing liquid in the purification pipe in a vortex manner; and

the nitrogen blowing concentration module is used for blowing nitrogen into the liquid in the finished product pipe to realize anaerobic concentration and enrichment;

the ice bath module (13) comprises a heat exchanger (113), a cooling fan, a test tube placing station (613), a cooling liquid circulating pump (413), a cold storage block (213), a refrigerating sheet (513) and heat insulation cotton (313);

the ceramic homogenizing submodule (08) comprises a rotary disc (208), a rotary disc motor (108) for driving the rotary disc (208) to rotate and a supporting plate (308); a plurality of storage holes (2081) for storing ceramic uniform protons are uniformly arranged on the circumferential direction of the rotary table (208); the supporting plate (308) is arranged below the turntable (208), and the supporting plate (308) is provided with a blanking hole (3081) communicated with the storage hole (2081); the supporting plate (308) is hinged with a shifting lever (508), and the shifting lever (508) rotates to block or open the blanking hole (3081); a blanking sensor (408) for detecting the falling of the ceramic homogenizers is arranged on the supporting plate (308) at the position below the blanking hole (3081).

2. The full-automatic QuECHERS experimental device according to claim 1, wherein:

the nitrogen blowing concentration module comprises a water bath, a nitrogen blowing instrument and a microprocessor control device for controlling the nitrogen blowing instrument to work;

the nitrogen blowing instrument comprises a gas nozzle, wherein the gas nozzle is configured to blow nitrogen into the finished product pipe, and the blowing direction of the nitrogen is obliquely downward blown to the pipe wall of the finished product pipe;

and in the nitrogen blowing concentration process, the finished product pipe is immersed in a water bath kettle, and the temperature of the liquid in the finished product pipe is controlled by the water bath temperature in the water bath kettle.

3. The full-automatic QuECHERS experimental device according to claim 1, wherein: the device also comprises a sucker module (12) and a sucker recovery box;

the suction head module (12) is provided with a suction head bearing plate (112), a suction head containing box (212) is arranged on the suction head bearing plate (112), and a plurality of disposable suction heads (312) are placed in the suction head containing box (212);

the liquid transfer device (203) can suck the disposable sucker (312), and then the liquid in the purification tube is sucked by the disposable sucker (312) and transferred to the finished product tube.

4. The full-automatic QuECHERS experimental device according to claim 1, wherein:

the device also comprises an XYZ three-axis module (02) which is composed of an X-axis assembly (102), a Y-axis assembly (202) and a Z-axis assembly (302) in a set manner;

the Z-axis assembly (302) comprises a Z-axis slider (3023) and a Z-axis guide rail (3022) which are connected with each other, and a Z-axis motor (3021) which controls the Z-axis slider (3023) to move up and down on the Z-axis guide rail (3022), and the multifunctional mechanical arm (03) is arranged on the Z-axis slider (3023);

the Z shaft assembly (302) is installed on the Y shaft assembly (202), the Y shaft assembly (202) is installed on the X shaft assembly (102), and the X shaft assembly (102) and the Y shaft assembly (202) are used for achieving translation of the multifunctional mechanical arm (03) in the front-back direction and the left-right direction.

5. The full-automatic QuECHERS experimental device according to claim 4, wherein: the multifunctional mechanical arm (03) comprises a telescopic block (103) connected with a Z-axis sliding block (3023), and the telescopic block (103) can move up and down in a telescopic mode on the Z-axis sliding block (3023);

the mechanical claw (303) is connected with the Z-axis slide block (3023), the liquid transfer device (203) is installed on the telescopic block (103), and when the mechanical claw (303) works, the liquid transfer device (203) retracts upwards along with the telescopic block (103).

6. The full-automatic QuECHERS experimental device according to claim 1, wherein: the liquid adding module (05) comprises eight channel switching valves and liquid injection devices, the number of the liquid injection devices is eight, and the eight liquid injection devices are installed at each channel of the eight channel switching valves in a one-to-one correspondence mode.

7. The full-automatic QuECHERS experimental device according to claim 1, wherein: the salt adding module (07) is sequentially provided with a salt bin (107), a rotating body (307) and a driving unit (207) for driving the rotating body (307) to rotate from top to bottom, the bottom of the salt adding module (07) is provided with a salt adding port (507), the rotating body (307) is provided with a hopper (3071), and the hopper (3071) is communicated with the salt bin (107) or the salt adding port (507) along with the rotation of the rotating body (307);

an adjusting block (407) for adjusting the size of the hopper (3071) is provided in the rotating body (307).

8. The full-automatic QuECHERS experimental device according to claim 4, wherein: the screw-capping module (04) comprises a switch cover assembly (404), the switch cover assembly (404) is provided with a sample tube screw-capping station (4041), a purification tube and a finished product tube screw-capping station (4042), friction self-locking sleeves (4043) for fixing the sample tube, the purification tube and the finished product tube are respectively installed at the sample tube screw-capping station (4041), the purification tube and the finished product tube screw-capping station (4042), and the friction self-locking sleeves (4043) are connected with a driving motor (4044).

9. The full-automatic QuECHERS experimental device according to claim 8, wherein: the screw-on capping module (04) further comprises a translation guide rail (304), a screw-on capping slider (204) arranged on the translation guide rail (304), and a translation motor (104) for driving the screw-on capping slider (204) to translate on the translation guide rail (304);

the opening and closing cover assembly (404) is fixedly arranged on the screwing cover sliding block (204).

10. The full-automatic QuECHERS experimental device according to claim 1, wherein: the oscillation module (09) comprises an oscillation substrate (609), an oscillation motor (309) is fixedly arranged on the oscillation substrate (609), and the oscillation motor (309) is connected with a vertical sliding block (509) through a cam in a matching manner;

the vertical sliding block (509) is fixedly connected with a fastener (409) for clamping a sample tube or a purification tube test tube, and is hinged with a baffle cylinder (209) which is hinged with a baffle (109) with the baffle cylinder (209);

the baffle (109) is configured to press against a sample tube or purge tube in cooperation with a test tube fastener (409);

the baffle cylinder (209) is used for realizing that the baffle (109) compresses the sample tube or the purification tube or turns away from the sample tube or the purification tube.

11. The full-automatic QuECHERS experimental device according to claim 1, wherein: the vortex blending module (11) comprises a test tube pressing component and a test tube rotating component;

the test tube pressing component comprises a pressing slide block (411), a pressing cylinder (311) for controlling the pressing slide block (411) to move up and down, a pressing plate (111) and a pressing plate (211) connected with the pressing plate (111);

the test tube rotating assembly comprises a vortex motor (611) and a vortex disc (811), the vortex disc (811) is connected with the vortex motor (611) through a vortex bearing (711), and a test tube barrel (511) used for bearing a purification tube is connected to the vortex disc (811);

the platen (211) is configured to compress the purge tube.

12. An experimental method for performing experiments by using the fully automatic queechers experimental device of any one of claims 9-11, comprising the steps of:

the first step is as follows: adding liquid and sample into sample tube

(1) The multifunctional mechanical arm (03) moves to the sample tube rack (101) on the XYZ triaxial module (02), the mechanical claw (303) grabs the sample tube to a sample tube screw-capping station (4041) of the screw-capping module (04), and the cover opening and closing component (404) is matched with the mechanical claw (303) to unscrew the tube cap of the sample tube;

(2) the opening and closing cover assembly (404) moves on the translation guide rail (304), the liquid adding module (05) firstly adds extraction liquid into the sample tube, then the opening and closing cover assembly (404) continuously moves to the salt adding module (07), the salt adding module (07) adds extraction salt into the sample tube, the opening and closing cover assembly (404) continuously moves to the ceramic homogenizing submodule (08), and the ceramic homogenizing submodule (08) adds ceramic uniform protons into the sample tube;

the second step is that: shaking, mixing and centrifuging the liquid in the sample tube

(1) The opening and closing cover assembly (404) is translated and returned to the initial position, the tube cover of the sample tube is screwed by matching with the mechanical claw (303), the multifunctional mechanical arm (03) moves on the XYZ triaxial module (02), and the mechanical claw (303) grabs the sample tube and sends the sample tube to the oscillation module (09) to oscillate and mix the sample tube uniformly;

(2) the multifunctional mechanical arm (03) continues to move on the XYZ triaxial module (02), and the mechanical claw (303) grabs the sample tube and conveys the sample tube to the centrifugal module (10) for centrifugation;

(3) the mechanical claw (303) grabs the sample tube and moves the sample tube to a sample tube screw-capping station (4041) of the screw-capping module (04);

the third step: pipetting

(1) The mechanical claw (303) is matched with the opening and closing cover component (404) to unscrew the tube cover of the sample tube;

(2) the multifunctional mechanical arm (03) moves on the XYZ triaxial module (02), and the mechanical claw (303) grabs the purifying tube and sends the purifying tube to a purifying tube and finished product tube screwing station (4042) of the screwing module (04);

(3) the mechanical claw (303) is matched with the opening and closing cover assembly (404) to unscrew the pipe cover of the purifying pipe;

(4) a liquid transferring device (203) transfers the supernatant liquid in the sample tube into the purifying tube;

(5) the mechanical claw (303) is matched with the opening and closing cover assembly (404) to screw down the pipe cover of the purifying pipe;

the fourth step: vortex mixing

(1) The multifunctional mechanical arm (03) continues to move on the XYZ triaxial module (02), and the mechanical claw (303) grabs the purifying pipe and sends the purifying pipe to the vortex blending module (11) for vortex blending;

(2) the multifunctional mechanical arm (03) sends the purifying pipe to a purifying pipe and finished product pipe screwing station (4042) of the screwing module (04);

(3) the mechanical claw (303) is matched with the opening and closing cover assembly (404) to unscrew the pipe cover of the purifying pipe;

the fifth step: pipetting

(1) The multifunctional mechanical arm (03) moves on the XYZ triaxial module (02), and the mechanical claw (303) grabs a finished product pipe and sends the finished product pipe to a purification pipe of the screw capping module (04) and a finished product pipe screw capping station (4042);

(2) the mechanical claw (303) is matched with the opening and closing cover assembly (404) to unscrew the pipe cover of the finished pipe;

(3) the multifunctional mechanical arm (03) moves, the liquid transfer device (203) is moved to the position above the sucker module (12), and the liquid transfer device (203) sucks the disposable sucker (312);

(4) the liquid transfer device (203) drives the disposable suction head (312) to draw the supernatant liquid in the purification tube to the finished product tube;

(5) screwing down pipe covers of the purification pipe and the finished product pipe, and respectively conveying the purification pipe and the finished product pipe to a purification pipe rack (201) and a finished product pipe rack (301);

and a sixth step: nitrogen-blown concentration

(1) And blowing nitrogen into the finished product pipe to perform nitrogen blowing concentration on the liquid in the finished product pipe.

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