WO2022121614A1 - 一种全自动样品前处理实验装置及实验方法 - Google Patents

一种全自动样品前处理实验装置及实验方法 Download PDF

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Publication number
WO2022121614A1
WO2022121614A1 PCT/CN2021/129966 CN2021129966W WO2022121614A1 WO 2022121614 A1 WO2022121614 A1 WO 2022121614A1 CN 2021129966 W CN2021129966 W CN 2021129966W WO 2022121614 A1 WO2022121614 A1 WO 2022121614A1
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WIPO (PCT)
Prior art keywords
tube
module
purification
sample
axis
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PCT/CN2021/129966
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English (en)
French (fr)
Inventor
杨富成
李朝文
郑劲林
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北京慧荣和科技有限公司
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Publication of WO2022121614A1 publication Critical patent/WO2022121614A1/zh

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/0099—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor comprising robots or similar manipulators
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N2035/00465—Separating and mixing arrangements
    • G01N2035/00534—Mixing by a special element, e.g. stirrer

Definitions

  • the present application relates to QuECHERS pretreatment technology, in particular to a fully automatic sample pretreatment experimental device and experimental method.
  • Pesticide residues refer to the general term for all derivatives of pesticide parent and toxicologically significant impurities, metabolic transformation products and reactants remaining in organisms, agricultural products and the environment due to the application of pesticides.
  • Pretreatment technology is the key to pesticide residue analysis and detection, and pretreatment technology largely determines the accuracy of the analysis results.
  • sample preparation techniques are very important. Sample pretreatment is the current bottleneck of analytical chemistry and one of the difficult and hot issues in analytical chemistry research. Due to the extremely large number of samples, lower and lower analyte content, and more and more complex matrices, it is urgent to develop high-throughput, high-selectivity, and high-efficiency online sample pretreatment technologies.
  • QuECHERS Quick, Easy, Cheap, Rugged, Safe
  • the principle is similar to that of high performance liquid chromatography and solid phase extraction, both of which use adsorbent fillers to interact with impurities in the matrix to adsorb impurities to achieve the purpose of impurity removal and purification.
  • the matrix dispersion extraction mechanism is used, and PSA or other adsorbents are used with most of the interfering substances in the matrix (organic acids, fatty acids, carbohydrates, etc.). Compounds, etc.) are combined and removed by centrifugation, so as to achieve the purpose of purification.
  • the QuECHERS method Compared with the traditional pretreatment analysis method, the QuECHERS method has the advantages of low sample consumption, less use of glassware, simple experimental process, reduced workload, improved work efficiency, and reduced experimental errors caused by considered factors.
  • the organic reagents can effectively avoid secondary pollution to the environment and other advantages.
  • the purpose of this application is to provide a fully automatic QuECHERS experimental device that can replace manual labor, effectively improve experimental accuracy and experimental efficiency, avoid human errors, and have a high degree of integration and automation. method.
  • the application provides a fully automatic QuECHERS experimental device, wherein: a sample and test tube module for placing a sample tube, a purification tube and a finished product tube at the same time, and the sample tube is stored with a sample to be processed;
  • the multifunctional robotic arm is provided with a gripper for grasping and transporting a sample tube or a purification tube or a finished tube, and a pipetting device.
  • the pipetting device is configured to transfer the liquid in the sample tube into the purification tube or transfer the liquid in the purification tube into the finished tube.
  • Cap screwing module which cooperates with the multifunctional robotic arm to unscrew and tighten the cap of the sample tube, the cap of the purification tube or the cap of the finished tube;
  • the liquid addition module is configured to add the extraction liquid to the sample tube
  • the sample adding module includes a salt adding module and a ceramic homogeneous sub-module for adding extraction salt and ceramic homogeneous protons into the sample tube respectively;
  • the shaking module and the centrifugation module are respectively used to realize the shaking and centrifugation of the sample in the sample tube;
  • Nitrogen blowing and enrichment module blowing nitrogen into the liquid in the finished product pipe to achieve anaerobic concentration and enrichment.
  • the nitrogen blowing concentration module described in the technical solution of the present application includes a water bath, a nitrogen blowing instrument, and a microprocessor control device for controlling the operation of the nitrogen blowing instrument;
  • the nitrogen blowing instrument includes a gas nozzle, and the gas nozzle is configured to blow nitrogen into the finished pipe and the blowing direction is slanted downward to the pipe wall of the finished pipe;
  • the finished pipe is immersed in a water bath to control the liquid temperature in the finished pipe through the temperature of the water bath in the water bath.
  • the technical solution of the present application also includes a tip module and a tip recovery box;
  • the suction head module is provided with a suction head carrying plate, a suction head accommodating box is arranged on the suction head carrying plate, and a plurality of disposable suction heads are placed in the suction head accommodating box;
  • the pipetting device can suck the disposable tip and then use the disposable tip to suck the liquid in the purification tube and transfer it to the finished tube.
  • the technical solution described in this application also includes an XYZ three-axis module consisting of an X-axis assembly, a Y-axis assembly and a Z-axis assembly set;
  • the Z-axis assembly includes the interconnected Z-axis slider and Z-axis guide rail, as well as the Z-axis motor that controls the Z-axis slider to move up and down on the Z-axis guide rail, and the multi-functional robotic arm is mounted on the Z-axis slider;
  • the Z-axis assembly is installed on the Y-axis assembly, and the Y-axis assembly is installed on the X-axis assembly.
  • the X-axis assembly and the Y-axis assembly are used to realize the translation of the multi-functional manipulator in the front-rear direction and the left-right direction.
  • the multifunctional mechanical arm described in the technical solution of the present application includes a telescopic block connected with the Z-axis slider, and the telescopic block can telescopically move up and down on the Z-axis slider;
  • the mechanical claw is connected with the Z-axis slider, and the pipetting device is installed on the telescopic block.
  • the pipetting device retracts upward with the telescopic block.
  • the liquid filling module module described in the technical solution of the present application includes an eight-channel switching valve and a liquid injection device.
  • the number of liquid injection devices is eight, and the eight liquid injection devices are installed at each channel of the eight-channel switching valve in a one-to-one correspondence.
  • the salt adding module described in the technical solution of the present application is provided with a salt silo, a rotating body and a driving unit for driving the rotating body to rotate in sequence from top to bottom.
  • the hopper is connected with the salt silo or the salt feeding port as the rotor rotates;
  • the rotating body is provided with an adjusting block for adjusting the size of the hopper.
  • the ceramic homogeneous sub-module described in the technical solution of the present application includes a turntable, a turntable motor for driving the turntable to rotate, and a support plate;
  • the turntable is provided with a plurality of storage holes for storing ceramic homogeneous protons in the circumferential direction;
  • the support plate is arranged below the turntable, and the support plate is provided with a blanking hole communicated with the storage hole;
  • a toggle lever is hingedly installed on the support plate, and the toggle lever rotates to block or open the blanking hole.
  • the support plate described in the technical solution of the present application is provided with a blanking sensor for detecting the falling of ceramic homogeneous protons at a position below the blanking hole.
  • the capping module described in the technical solution of the present application includes an opening and closing cap assembly, and the opening and closing cap assembly is provided with a sample tube capping station, a purification tube and a finished tube capping station.
  • a friction self-locking sleeve for fixing the sample tube, the purification tube and the finished tube is respectively installed at the screw capping station of the finished tube and the friction self-locking sleeve is connected with a driving motor.
  • the cap-screwing module described in the technical solution of the present application further includes a translation guide rail, a cap-screwing slider disposed on the translation guide rail, and a translation motor for driving the cap-screwing slider to translate on the translation guide rail;
  • the opening and closing cover assembly is fixedly installed on the screwing cover slider.
  • the oscillating module described in the technical solution of the present application includes an oscillating base plate, an oscillating motor is fixedly arranged on the oscillating base plate, and a vertical sliding block is connected to the oscillating motor through a cam;
  • the vertical slider is fixedly connected with fasteners for clamping the sample tube or purification tube test tube; a baffle cylinder is hinged, and a baffle is hinged with the baffle cylinder;
  • the baffle is configured to cooperate with the test tube fastener to press the sample tube or purification tube;
  • the baffle cylinder is used to allow the baffle to compress the sample or purge tube or to flip away from the sample or purge tube.
  • the vortex module described in the technical solution of the present application includes a test tube pressing component and a test tube rotating component;
  • the test tube pressing assembly includes a pressing slider, a pressing cylinder for controlling the up and down movement of the pressing slider, a pressing plate and a pressing plate connected with the pressing plate;
  • the test tube rotating assembly includes a whirlpool motor and a whirlpool, the whirlpool is connected with the whirlpool motor through a whirlpool bearing, and a test tube tube for carrying a purification tube is connected to the whirlpool;
  • the platen is configured to compress the purge tube.
  • the technical solution of the present application also includes an ice bath module
  • the ice bath module includes a heat exchanger, a cooling fan, a test tube placement station, a coolant circulation pump and a cold storage block;
  • the present application provides an experimental method using the above-mentioned fully automatic QuECHERS experimental device, comprising the following steps:
  • Step 1 Add liquid and sample to the sample tube
  • the multi-functional robotic arm moves to the sample tube rack on the XYZ three-axis module, and the mechanical claw grabs the sample tube to the sample tube capping station of the capping module. Unscrew the cover;
  • the opening and closing cover assembly moves on the translation rail.
  • the liquid adding module first adds the extraction liquid to the sample tube, and then the opening and closing cover assembly continues to move to the salt adding module.
  • the salt adding module adds the extraction salt to the sample tube, and the cover is opened and closed The assembly continues to move to the ceramic homogenizer module, which adds ceramic homogenizers to the sample tube.
  • Step 2 Shake and mix the liquid in the sample tube and centrifuge
  • the opening and closing cover assembly is translated back to the original position, and the cap of the sample tube is tightened with the mechanical claw.
  • the multi-functional mechanical arm moves on the XYZ three-axis module, and the mechanical claw grasps the sample tube and sends it to the shaking module for shaking and mixing. ;
  • the mechanical claw cooperates with the opening and closing cover assembly to unscrew the cap of the sample tube
  • the multifunctional manipulator moves on the XYZ three-axis module, and the mechanical claw grabs the purification tube and sends it to the purification tube and finished tube capping station of the capping module;
  • the multifunctional mechanical arm continues to move on the XYZ three-axis module, and the mechanical claw grabs the purification tube and sends it to the vortex mixing module for vortex mixing;
  • the multi-functional robotic arm sends the purification tube to the purification tube and finished tube screwing station of the capping module
  • the multi-functional manipulator moves on the XYZ three-axis module, and the manipulator grabs the finished pipe and sends it to the purification pipe and finished pipe unscrewing station of the unscrewing module;
  • the pipetting device drives the disposable tip to extract the supernatant in the purification tube to the finished product tube;
  • the sixth step nitrogen blowing concentration
  • the multi-functional robotic arm transports the sample tube from the sample adding and test tube module to the cap-screwing module.
  • the salt module and the ceramic homogenizer module sequentially add the extraction liquid, the extraction salt and the ceramic homogenizer to the sample tube, tighten the tube cap, shake and centrifuge through the shaking module and the centrifugal module; the pipetting device transfers the supernatant in the sample tube into the purification tube , and then the vortex mixing module performs vortex mixing, and then the supernatant in the purification tube is transferred to the finished product tube for anaerobic concentration and enrichment through the nitrogen blowing concentration module (the cap of the sample tube, the cap of the purification tube and the The tightening and unscrewing actions of the tube cover of the finished tube are omitted and not described in detail).
  • the whole process experiment has a high degree of automation, high experimental efficiency and high reliability; at the same time, a nitrogen blowing concentration module is innovatively added, which does not require manual delivery of the finished tube to a special nitrogen blowing instrument for concentration, realizing the full automation of the experimental process.
  • the nitrogen blower is used to blow nitrogen rapidly and continuously to the liquid surface of the finished tube, so that the solvent in the liquid can be rapidly evaporated and separated, so as to realize the concentration of the sample, on the one hand, keep the liquid sample
  • nitrogen can play the role of isolating oxygen and prevent oxidation.
  • the setting of the blowing direction of the gas nozzle of the nitrogen blower makes the nitrogen flow blown from the gas nozzle form a spiral airflow in the concentrating tube, which effectively increases the purging area, slows down the airflow impulse, and makes the solvent in the finished tube evenly volatilize without splashing.
  • the setting of the XYZ three-axis module can realize the movement of the multi-functional manipulator in the front and rear, left and right, and up and down directions, thereby ensuring that the multi-functional manipulator grabs the sample tube or the purification tube or the finished tube can be transported to the appropriate position in multiple directions, reducing the manual transportation.
  • the Z-axis motor can drive the slider to move up and down.
  • the liquid adding device When adding the extraction liquid to the sample tube, the liquid adding device can be installed in each channel of the eight-channel switching valve in a one-to-one correspondence, which can realize the supply of eight kinds of solutions.
  • the whole action of adding salt is completed by the drive unit controlling the rotation of the rotating body to drive the hopper to rotate, that is, when the hopper is connected to the salt silo, the salt in the salt silo falls into the hopper, and when the hopper is rotated to communicate with the salt-adding port, the salt falls into the sample tube without manual operation.
  • the adjustment block can adjust the size of the hopper, so that the amount of salt added is controllable and adjustable.
  • the turntable When adding ceramic homogenizers to the ceramic homogenizer module, the turntable is also driven by the turntable motor to rotate, and the ceramic homogenizers in the storage hole automatically fall into the sample tube through the blanking hole.
  • the turntable is driven to rotate without manual operation, and the degree of automation is high.
  • the setting of the friction self-locking sleeve in the capping module prevents the sample tube, purification tube or finished tube from slipping on the capping module when the second drive motor drives the capping module to work. detachment, resulting in the need to stop the test and human intervention.
  • Fig. 1 is the internal structure schematic diagram of a kind of automatic QuECHERS experimental device of the present application
  • Fig. 2 is the internal top view of a kind of automatic QuECHERS experimental device of the present application
  • Figure 3 is a working principle diagram of a fully automatic QuECHERS experimental device
  • Fig. 4 is the schematic diagram of the sample and test tube module in the embodiment
  • Fig. 5 is the structural representation of XYZ three-axis module in the embodiment
  • Fig. 6 is the structural representation of the Z-axis assembly in the XYZ three-axis module in the embodiment
  • Fig. 7 is the structural representation of the multifunctional mechanical arm in the embodiment.
  • FIG. 8 is a schematic structural diagram of a cap-screwing module in an embodiment
  • FIG. 9 is a partial cross-sectional view of the cap-screwing module in the embodiment.
  • Fig. 10 is the schematic diagram of the sample adding module in the embodiment.
  • FIG. 11 is a cross-sectional view of a salting module in an embodiment
  • FIG. 12 is a schematic structural diagram of a ceramic homogeneous sub-module in an embodiment
  • FIG. 13 is a schematic structural diagram of an oscillation module in an embodiment
  • FIG. 14 is a schematic structural diagram of a centrifugal module in an embodiment
  • FIG. 15 is a schematic diagram of a vortex mixing module in an embodiment
  • Fig. 16 is the connection diagram of the vortex mixing module and the purification pipe in the embodiment
  • Figure 17 is a schematic diagram of a tip module in an embodiment
  • Fig. 18 is the nitrogen blowing schematic diagram of nitrogen blowing concentration module in the embodiment.
  • FIG. 19 is a schematic structural diagram of an ice bath module in an embodiment.
  • sample and test tube module 101, sample tube rack; 201, purification tube rack; 301, finished tube rack; 401, tube holder;
  • XYZ three-axis module 102, X-axis assembly; 202, Y-axis assembly; 302, Z-axis assembly; 3021, Z-axis motor; 3022, Z-axis guide rail; 3023, Z-axis slider;
  • Multifunctional mechanical arm 103. Telescopic block; 203. Liquid pipetting device; 303. Mechanical claw;
  • cap screwing module 104, translation motor; 204, cap screwing slider; 304, translation guide rail; 404, opening and closing cap assembly; 4041, sample tube screw capping station; 4042, purification tube and finished tube screw capping station ;4043, friction self-locking sleeve; 4044, drive motor;
  • Sample adding module 106. Liquid adding head; 206. Sample adding bracket;
  • Centrifugal module 110, door slide rail; 210, door opening and closing cylinder; 310, centrifugal rotor; 410, pick and place port;
  • Vortex mixing module 111, pressing plate; 211, pressing plate; 311, pressing cylinder; 411, pressing slider; 511, test tube; 611, vortex motor; 711, vortex bearing; 811, vortex disc;
  • tip module 112, tip carrier plate; 212, tip box; 312, disposable tip; 412, internal standard solution cup; 512, fixing block;
  • This application provides a fully automatic QuECHERS experimental device, as shown in Figures 1 and 2, including a sample and test tube module 01, an XYZ three-axis module 02, a multi-functional robotic arm 03, a cap screwing module 04, a liquid adding module 05,
  • the salt adding module 07, the ceramic homogenizer module 08, the shaking module 09, the centrifugation module 10, the vortex mixing module 11 and the nitrogen blowing concentration module also include a bottom plate and a bracket.
  • the sample and test tube module 01 includes a sample tube rack 101, a purification tube rack 201 and a finished tube rack 301.
  • the sample tube rack 101, the purification tube rack 201 and the finished tube rack 301 are arranged in order in the horizontal direction and pass through the tubes.
  • the bracket 401 is fixedly installed on the bottom plate, and the specific installation method is as follows: the tube bracket 401 is fixedly connected to the bottom plate by screws, and the tube bracket 401 is provided with a positioning groove. There are positioning pins matching with the positioning grooves.
  • the sample tube rack 101, the purification tube rack 201 and the finished tube rack 301 are inserted into the corresponding positioning grooves through the positioning pins to complete the fixed connection with the tube support 401, and the sample tube rack 101.
  • the purification pipe rack 201 and the finished pipe rack 301 are fixedly installed on the pipe rack 401 in a drawer type; the sample pipe rack 101, the purification pipe rack 201 and the finished pipe rack 301 are all provided with multiple test tube fixing positions; the sample pipe rack 101 is used for A plurality of sample tubes are accommodated, and the samples to be processed are contained in the sample tubes; the purification tube rack 201 and the finished tube rack 301 respectively accommodate a plurality of purification tubes and finished tubes (hereinafter, the sample tubes, purification tubes and finished tubes may be collectively referred to as test tubes).
  • FIG. 5 shows the XYZ three-axis module 02 in the accompanying drawings.
  • the XYZ three-axis module 02 is mounted on the bracket, including the X-axis assembly 102, the Y-axis assembly 202 and the Z-axis assembly 302;
  • the X-axis assembly 102 includes two horizontal X-axis guide rails installed in parallel on the bracket.
  • the two X-axis guide rails are connected by connecting rods and driven synchronously. Both X-axis guide rails are provided with X-axis sliders, and the connecting rods cooperate with each other.
  • the X-axis guide rail drive motor is connected; when the X-axis guide rail drive motor is turned on, the X-axis guide rail drive motor drives the movement of the connecting rod, and the connecting rod synchronously drives the movement of the two X-axis guide rails, so that the X-axis slider moves relatively horizontally on the X-axis guide rail.
  • the Y-axis assembly 202 is provided with a Y-axis guide rail horizontally, but the Y-axis guide rail and the X-axis guide rail are arranged in a vertical direction; 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 method is set as the Y-axis guide rail.
  • the two ends of the X-axis are fixedly connected to the X-axis sliders on the two X-axis guide rails.
  • the shaft assembly 202 further includes a Y-axis guide rail driving motor for driving the Y-axis guide rail to move, and is used for driving the Y-axis guide rail to move.
  • the Y-axis guide rail is matched with a Y-axis slider that can move relative to the Y-axis guide along the length of the Y-axis guide.
  • the Z-axis assembly 302 is fixedly connected to the Y-axis slider, and can follow the Y-axis slider along the length of the Y-axis guide. Move; 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 vertically; the Z-axis guide rail 3022 is matched with a relative Z-axis guide rail. 3022 Z-axis slider 3023 that moves up and down.
  • the multi-functional robotic arm 03 is fixedly installed on the Z-axis slider 3023, and drives the X-axis guide rail drive motor.
  • the X-axis slider moves along the length of the X-axis guide rail (hereinafter referred to as the front-rear direction), driving the Y-axis assembly 202 and sliding with the Y-axis.
  • the Z-axis assembly 302 that is fixedly connected to the block and the multi-functional mechanical arm 03 connected to the Z-axis assembly 302 move together in the front and rear directions; the Y-axis guide rail drive motor is driven, and the Y-axis slider moves along the length of the Y-axis guide rail (hereinafter referred to as the left-right direction).
  • Fig. 7 is a schematic diagram of the structure of the multifunctional mechanical arm 03.
  • the multifunctional mechanical arm 03 includes a telescopic block 103, a pipetting device 203 and a mechanical claw 303 for grasping test tubes, and also includes a Z-axis slider fixed to Attached mounting plate.
  • Both the telescopic block 103 and the mechanical claw 303 are fixedly connected to the Z-axis slider 3023 through the mounting plate; the pipetting device 203 is installed on the telescopic block 103, when the mechanical claw 303 grabs the test tube, the pipetting device 203 retracts upward with the telescopic block 103 Back, when the pipetting device 103 picks up the sample liquid, the pipetting device 103 extends along with the telescopic block 103; the pipetting device 103 can use a pipette.
  • the cap-screwing module 04 includes a translation motor 104 , a translation guide rail 304 driven by the translation motor 104 , and a cap-screwing slider 204 that is installed in cooperation with the translation guide rail 304 and slides relatively on the translation guide rail 304 .
  • the opening and closing cap assembly 404 is provided with a sample tube capping station 4041, a purification tube and a finished tube capping station 4042; the sample tube capping station 4041, the purification tube and the finished tube capping station 4042 are respectively installed and useful
  • the friction self-locking sleeve 4043 for fixing the sample tube, the purification tube and the finished tube is connected with a driving motor 4044, and the specific connection and installation method is shown in FIG. 9 .
  • the test tube is fixed in the friction self-locking sleeve 4043 of the sample tube capping station 4041 or the purification tube and finished tube capping station 4042.
  • the drive motor 4044 drives the friction self-locking sleeve 4043 to rotate, and the test tube can be in the friction self-locking sleeve 4043. Driven by the frictional force, the self-locking sleeve 4043 rotates with the frictional force.
  • the liquid filling module 05 includes an eight-channel switching valve and a liquid injection device.
  • the liquid injection device includes a stepper motor, a precision lead screw and a micro-sampler.
  • the stepper motor drives the precision lead screw to drive the micro-sampler to supply the extraction liquid;
  • liquid adding module 05 of the present application can also be provided with an automatic cleaning device (not shown in the figure), which can be automatically cleaned after switching the extraction liquid by controlling the eight-channel switching valve through the intelligent control program; 25ml supply to meet the requirements of the instrument.
  • an automatic cleaning device not shown in the figure
  • the sample addition module 06 includes a salt addition module 07 and a ceramic homogenizer module 08 for adding extraction salts and ceramic homogenizers into the sample tube respectively, and also includes a sample addition support 206; the salt addition module 07 and the ceramic homogenizer module 08 are installed in the sample addition On the bracket 206; a liquid addition head 106 is also provided on the sample addition support 206, and the liquid addition head 106 communicates with the liquid addition module 05, that is, the micro-injector in the liquid addition module 05 and the liquid addition head 106 pass through the pipeline (Fig. (not shown in the figure) is connected, and the extraction liquid pushed out by the micro-injector flows to the liquid addition head 106 through the pipeline for liquid addition; as shown in FIG. 1 and FIG.
  • the sample holder 206 covers the screw cap module 04, that is, the translation guide rail 304 of the screw cap module 04 is located below the sample addition module 06, and the liquid addition head 106, the salt addition module 07 and the ceramic homogenizer module 08 follow the length of the translation guide rail 304 in sequence.
  • the opening and closing cover assembly 404 moves along the length direction of the translation guide rail 304 and can be moved to the position below the liquid feeding head 106, the position below the salt feeding module 07 and the position below the ceramic homogenizer module 08 successively.
  • Figure 11 shows a schematic diagram of the structure of the salting module 07, including a salt silo 107, a rotating body 307, and a driving unit 207 for driving the rotating body 307 to rotate.
  • the salt adding module 07 includes a cylindrical cylinder, the cylindrical cylinder is hollow and the interior is a salt silo 107 , and a blocking cover is installed on the top of the cylindrical cylinder.
  • extraction can be added to the salt silos 107 Salt;
  • the bottom of the cylindrical cylinder is connected with the rotating body 307, and the rotating body 307 is equipped with a hopper 3071, and the hopper 3071 can rotate with the rotating body 307;
  • a salt outlet is connected at the lower position of the rotating body 307, and the salt outlet is provided with a salt feeding part.
  • Port 507 when the hopper 3071 rotates with the rotating body 307, the opening of the hopper 3071 can be rotated to communicate with the salt bin 107 or communicate with the salt feeding port 507; the rotating body 307 is also provided with an adjusting block 407, and the adjusting block 407 can adjust the hopper The size of the hopper 3071 can be adjusted so that the amount of the extracted salt dropped and added by the hopper 3071 through the salt adding port 507 can be adjusted.
  • the driving unit 207 first drives the rotating body 307 to rotate to the state where the hopper 3071 is connected to the salt bin 107 (that is, the opening of the hopper 3071 faces upwards), opens the blocking cover, adds the extraction salt into the salt bin 107, and extracts the salt.
  • the salt enters the hopper 3071, and then the driving unit 207 drives the rotating body 307 to rotate, generally 180°, and the hopper 3071 rotates until the opening of the hopper 3071 is connected to the salt feeding port 507.
  • the extracted salt in the hopper 3071 is under the action of gravity
  • the salt is added by dropping through the salt-adding port 507, and then the hopper 3071 is reset under the action of the spring, waiting for the next salt-adding; 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 to complete.
  • the ceramic homogeneous sub-module 08 includes a turntable 208 , a turntable motor 108 for driving the turntable 208 to rotate, and a support plate 308 ; the support plate 308 is fixedly connected to the sample loading bracket 206 , and the turntable 208 is arranged in a circumferential direction.
  • the storage hole 2081 of the ceramic homogenizer is provided on the support plate 308 with a blanking hole 3081 that can communicate with the storage hole 2081. When the turntable 208 rotates, each storage hole 2081 can be rotated until the blanking hole 3081 is in the blanking hole 3081.
  • a lever 508 is hinged on the support plate 308, the lever 508 can be rotated around the hinge shaft where it is hinged with the support plate 308, and the lever 508 rotates under the blanking hole 3081 and collides with the support plate 308 and causes the blanking hole 3081 is blocked;
  • a blanking sensor 408 is also installed on the support plate 308 to detect whether there are ceramic homogeneous particles falling from the blanking hole 3081 .
  • the working principle of the ceramic homogenizer module 08 when it is not working, the lever 508 blocks the blanking hole 3081 on the turntable 308; when the ceramic homogenizer needs to be added to the sample tube, the screw cap module 04 moves to the bottom of the ceramic homogenizer module 08 At the position, the cap-screwing module 04 triggers the lever 508, the lever 508 rotates to open the blanking hole 3081, and the ceramic homogeneous particles added in the storage hole 2081 will fall into the sample tube on the cap-screwing module 04 through the blanking hole 3081; If the material sensor 408 does not detect the falling action of the ceramic homogenizer, the turntable motor 108 will drive the turntable 208 to rotate until the other storage hole 2081 is connected with the blanking hole 3081. Continue until the drop sensor 408 detects the fall of the ceramic homogenizer.
  • Fig. 13 shows the structure of the oscillation module 09, including the oscillation base plate 609, the oscillation motor 309 is installed on the oscillation base plate 609, and the oscillation motor 309 is connected with the vertical slider 509 through a cam, that is, the oscillation motor 309 is connected with a cam, and the cam is connected with the vertical slider 509.
  • the block 509 abuts, the cam rotates under the driving of the vibration motor 309, and drives the vertical slider 509 to reciprocate up and down during the rotation;
  • the vibration module 09 also includes a baffle cylinder 209 and a baffle cylinder 209 connected to the baffle cylinder 109, and also includes The test tube fastener 409 fixedly connected to the vertical slider 509;
  • the baffle cylinder 209 is hinged with the baffle 109 and the vertical slider 509, and the baffle 109 is used to compress or loosen the test tube fastened by the test tube fastener 409 .
  • the shock module 09 can also be provided with a shock-absorbing foot pad 709 for shock absorption, and the shock-absorbing foot pad 709 can be directly installed under the shock base plate 609 .
  • the working principle of the vibration module 09 Initially, the vibration motor 309 and the baffle cylinder 209 do not work, and the baffle 109 is in a vertical state; when the multifunctional machine mechanical arm 03 grabs the test tube and moves it to the test tube fastener 409, the blocking The plate cylinder 209 is extended, the baffle plate 109 rotates into a horizontal state and presses the test tube at the test tube fastener 409, and then the vibration motor 309 works to drive the vertical slider 509 to reciprocate up and down, and the test tube fastener 409 reciprocates up and down to complete the vibration. action.
  • the centrifugal module 10 includes a centrifugal cover, a pick-and-place port 410 is provided on the centrifugal cover, and a door slide rail 110 is installed at the pick-and-place port 410 , and a switch door (not shown in the figure) is installed in conjunction with the switch door (not shown in the figure).
  • the door is connected with a door opening and closing cylinder 210.
  • the opening and closing air cylinder 210 extends to drive the opening and closing door to slide on the door slide rail 110 to close the pick-and-place opening 410.
  • the discharge port 410; a centrifugal rotor 310 is arranged in the centrifugal protective cover, and the centrifugal rotor 310 has a positioning function on the circumference.
  • the vortex module 11 includes a test tube pressing component and a test tube rotating component.
  • the test tube pressing component includes a mounting frame, a pressing plate 111, a pressing plate 211, a pressing cylinder 311, and a pressing slider 411; the pressing plate 211 is fixedly connected On the pressing plate 111, the pressing plate 111 is hingedly mounted on the pressing slider 411, and the pressing plate 111 can be rotated 90 degrees from a vertical state to a horizontal state;
  • the pressing slide block 411 is sleeved on the guide post, and the pressing cylinder 311 is connected with the pressing slide block 411 to control the up and down movement of the pressing slide block 411 .
  • the test tube rotation assembly includes a vortex motor 611, a vortex disk 811, and a test tube barrel 511.
  • Figure 16 shows the installation structure of the test tube rotation assembly.
  • the vortex disk 811 is connected to the vortex motor 611 through a vortex bearing 711 and an eccentric shaft (not shown in the figure).
  • the test tube cartridge 511 is mounted on the vortex disk 811 .
  • the working principle of the vortex mixing module 11 the test tube is first moved into the test tube tube 511 to contact the vortex plate 811, the pressing cylinder 311 drives the pressing slider 411 to move downward, the pressing plate 111 turns 90 degrees and then moves downward, the pressing plate 111 is turned from the vertical state to the horizontal state, the pressure plate 211 is then turned over until the plate mouth is aligned with the test tube in the test tube tube 511 and pressed, and the vortex motor 611 is activated to drive the eccentric shaft to rotate, and the eccentric shaft drives the vortex plate 811 to rotate, and then Complete the vortexing of the liquid in the test tube.
  • the tip module 12 includes a tip carrying plate 112 on which a tip accommodating box 212 is set, and a fixing block 512 for pressing and fixing the tip accommodating box 212 is also provided.
  • a plurality of disposable tips 312 are placed in the box 212; the pipetting device 203 can first suck a disposable tip 312 and then suck the liquid in the test tube into the disposable tips 312; a tip recovery box is also provided on the bottom plate , the tip recovery box is located below the purification tube rack 201 in the sample and test tube module 01 , and the used disposable tips 312 can be moved into the tip recovery box through the pipetting device 203 .
  • An internal standard solution cup 412 is also provided on the tip module 12 , and an internal standard solution can be added to the internal standard solution cup 412 , which is aspirated and added to the corresponding test tube through the pipetting device 203 .
  • the nitrogen blowing concentration module includes a water bath, a nitrogen blowing instrument, and a microprocessor control device that controls the work of the nitrogen blowing instrument.
  • the nitrogen blowing instrument includes a gas nozzle;
  • Figure 18 shows the nitrogen blowing concentration module performs nitrogen blowing concentration and enrichment on the liquid in the finished pipe. Schematic diagram, the gas nozzle is set obliquely downward, the nitrogen blowing instrument blows nitrogen through the gas nozzle and blows the nitrogen to the pipe wall of the finished pipe, the finished pipe is immersed in the water bath, and the temperature of the liquid in the finished pipe is controlled by the temperature of the water bath in the water bath.
  • the temperature of the water bath is controlled from 30°C to 60°C, and good enrichment effect can be obtained by nitrogen purging;
  • the gas nozzle is set in a specific direction, and the blown nitrogen flow forms a spiral airflow in the finished tube, which is effective Increase the purging area, slow down the airflow, and make the solvent evaporate evenly without splashing;
  • the nitrogen blower with this principle has products on the market, which can be directly purchased and used, such as the NS-12S nitrogen blower.
  • the application also includes an ice bath module 13.
  • the ice bath module 13 includes a test tube placing station 613 for placing the test tubes, and also includes a cold storage block 213 located at the test tube placing station 613 And the thermal insulation cotton 313 wrapping the cold storage block 213, when the test tube is located at the test tube placement station 613, the cold storage block 213 surrounds the test tube to transfer cold energy to the test tube, and the thermal insulation cotton 313 separates the outside heat from the cold storage.
  • the temperature of the block 213 changes rapidly to improve the cooling efficiency;
  • the ice bath module 13 also includes a cooling liquid circulation pump 413, a cooling liquid 513 is arranged on the cooling liquid circulation pump 413, and the cooling storage block 213 is located on the cooling sheet 513, and the cooling sheet 513 makes the cooling As the temperature of the storage block 213 decreases, a temperature probe can be designed to detect the temperature;
  • the ice bath module 13 also includes a heat exchanger 113 and a cooling fan (not shown in the figure), and the cooling fan is installed on the heat exchanger 113 through a mounting
  • the circulation pump 413 transports the heat of the cooling fins 513 to the heat exchanger 113, and the cooling fan conducts air cooling and heat dissipation.
  • the application also provides an experimental method of an automatic QuECHERS experimental device, as shown in Figure 3, its working principle and working steps include liquid addition, sample addition, shaking, centrifugation, pipetting, vortex mixing, pipetting and nitrogen Blow concentration; wherein the liquid addition operation includes the following steps:
  • the XYZ three-axis module 02 moves to control the multi-functional robotic arm 03 to move forward and backward, left and right or up and down to the top of the sample tube rack 101.
  • the mechanical claw 303 grabs a sample tube containing the sample to be tested, and controls the movement of the XYZ three-axis module.
  • the mechanical claw 303 removes the sample tube to the sample tube capping station 4041 of the cap opening and closing assembly 404, the mechanical claw 303 grabs the cap of the sample tube, and then opens and closes the cap
  • the drive motor 4044 of the assembly 404 works, and drives the friction self-locking sleeve 4043 to rotate and drives the sample tube to rotate until the cap of the sample tube is opened; at this time, the translation motor 104 of the cap-screwing module 04 works, and drives the translation guide 304 to drive the cap-screwing slide. Block 204 is actuated.
  • the opening and closing cover assembly 404 moves along the translation guide rail 304 until the sample tube whose cap is unscrewed is located under the liquid filling head 106, the liquid addition module 05 is opened, and the liquid injection device of the liquid addition module 05 injects the extraction liquid Add to the sample tube via the dosing head 106 .
  • the sample loading procedure includes the following steps:
  • the translation motor 104 works, and the opening and closing cover assembly 404 continues to move until the sample tube moves to the salt addition port 507 of the salt addition module 07.
  • the extraction salt has been added to the salt tank 107, and then the rotating drive unit 207 works to drive the rotating body 307 rotates, the extracted salt in the hopper 3071 rotates and falls into the sample tube through the salt addition port 507 to complete the addition of the extracted salt; the translation motor 104 works, and the opening and closing cover assembly 404 continues to move until the opening and closing cover assembly 404 moves to the ceramic level.
  • the lever 508 is opened at the lever 508 of the proton module 08, and the ceramic homogeneous particles in the storage hole 2081 fall into the sample tube through the blanking hole 3081 to complete the loading of the ceramic homogeneous particles.
  • the shaking and centrifugation operations include the following steps:
  • the translation motor 104 works, and the opening and closing cover assembly 404 moves until the opening and closing cover assembly 404 returns to the original position.
  • the mechanical claw 303 and the frictional self-locking sleeve 4043 driven by the driving motor 4044 cooperate to tighten the cap of the sample tube to the original position.
  • the multifunctional mechanical arm 03 moves until the sample tube is moved to the vibration module 09, the sample tube is fixed by the test tube fastener 409, the baffle 109 presses the sample tube, and the vibration motor
  • the operation of 309 drives the vertical slider 509 to reciprocate up and down, and drives the oscillating substrate 609 and the sample tube to reciprocate up and down to complete the oscillating operation.
  • the mechanical claw 303 grabs the sample tube, and the multifunctional mechanical arm 03 moves on the XYZ three-axis module 02 until the sample tube is moved into the centrifugation module 10 for centrifugation.
  • the door opening and closing cylinder 210 works to open the opening and closing door, position the sample tube directly below the pick-and-place port 410, and then close the opening and closing door to perform the centrifugation operation on the sample tube.
  • the first pipetting operation involves the following steps:
  • the mechanical claw 303 grabs the sample tube and is moved by the multifunctional mechanical arm 03 to the sample tube screw capping station 4041 of the opening and closing cover assembly 404.
  • the cover is unscrewed, and then the mechanical claw 303 moves to the purification pipe rack 201 to grab the purification pipe, and the multi-functional mechanical arm 03 moves to remove the purification pipe to the purification pipe and finished pipe screw capping station 4042 of the opening and closing cover assembly 404,
  • the mechanical claw 303 cooperates with the opening and closing cover assembly 404 to unscrew the cap of the purification tube.
  • the pipetting device 203 starts to work.
  • the pipetting device 203 moves to the sample tube to absorb the supernatant in the sample tube and move it into the purification tube. Finally, The mechanical claw 303 cooperates with the opening and closing cover assembly 404 to tighten the caps of the sample tube and the purification tube successively, so far the first pipetting work is completed, that is, the supernatant in the sample tube is transferred into the purification tube.
  • the vortex mixing steps are as follows:
  • the mechanical claw 303 grabs the purification tube, moves it to the vortex mixing module 11, and places the purification tube in the test tube 511.
  • the pressing cylinder 311 works so that the pressure plate 211 presses the purification tube, and the vortex motor 611 drives the vortex plate 811 to rotate. , thus completing the vortex mixing of the purification tube.
  • the purification tube after the vortex mixing operation needs to be sent back to the purification tube and finished tube screw capping station 4042 of the opening and closing cap assembly 404 by the multifunctional robotic arm 03 for the second pipetting action.
  • the mechanical claw 303 needs to cooperate with the opening and closing cover assembly 404 to unscrew the cap of the purification tube, and then the multi-functional robotic arm 03 moves and grabs the finished tube, moves the finished tube to the purification tube and unscrews the cap of the finished tube At station 4042, unscrew the cap of the finished tube; then the multi-functional robotic arm moves to the tip module 12, the pipetting device 203 picks up a disposable tip 312 and then moves it to the purification tube, and the pipetting device 203 works, one time The suction head 312 sucks the supernatant in the purification tube and moves it into the finished tube; finally, the mechanical claw 303 cooperates with the opening and closing cover assembly 404 to successively complete the tightening action of the cap of the purification tube and the cap of the finished tube.
  • the multifunctional robotic arm 03 moves, and the disposable tip 312 can be thrown into the tip recovery box.
  • the nitrogen blowing concentration operation includes the following steps:
  • the multi-functional robotic arm 03 moves the finished product tube to the nitrogen blowing concentration module 14, unscrews the tube cover of the finished product tube, and then opens the nitrogen blowing instrument in the nitrogen blowing concentration module 14, and the nitrogen blowing instrument blows nitrogen into the finished product tube for concentration and enrichment.
  • the water bath pot 214 can be heated to a temperature control range of 30°C to 60°C, and the temperature in the finished tube can be controlled by heat transfer to improve the concentration and enrichment efficiency.

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Abstract

本申请公开了一种全自动样品前处理实验装置及实验方法。其中全自动QuECHERS实验装置包括多功能机械臂、拧盖模块、加液模块、离心模块、加盐模块、陶瓷均质子模块、氮吹浓缩模块、漩涡混匀模块以及震荡模块，可自动化完成样品移取，萃取液、萃取盐和陶瓷均质子的添加，震荡混匀，离心分离和漩涡混匀动作；采用全自动QuECHERS实验装置进行实验的方法，主要是集样品加液萃取、离心分离、固相萃取和氮吹浓缩过程为一体，节约时间、减少人为操作，提高自动化，减少误差。

Description

一种全自动样品前处理实验装置及实验方法 技术领域
本申请涉及QuECHERS前处理技术,尤其涉及一种全自动样品前处理实验装置及实验方法。
背景技术
农业产业化的发展使农产品的生产越来越依赖于农药、抗生素和激素等外源物质，我国农药在农产品的用量居高不下，而这些物质的不合理使用必将导致农产品中的农药残留超标，影响消费者食用安全，严重时会造成消费者致病、发育不正常等，甚至直接导致中毒死亡。农药残留超标也会影响农产品的贸易，世界各国对农药残留问题高度重视，对各种农副产品中农业残留都规定了越来越严格的限量标准，使中国农产品出口面临严峻的挑战。
农药残留是指由于农药的应用而残存于生物体、农产品和环境中的农药亲体及具有毒理学意义的杂质、代谢转化产物和反应物等所有衍生物的总称。前处理技术是农药残留分析检测中的关键，前处理技术在很大程度上决定了分析结果的准确与否。要在复杂的基质中检测微量复杂的组分，样品前处理技术非常重要。样品前处理是目前分析化学的瓶颈，是分析化学研究的难点和热点问题之一。由于样品数量极多，且分析物含量越来越低，基体越来越复杂，迫切要求发展高通量、高选择性、高效率的在线样品前处理技术。目前市场上有很多前处理设备，例如提取、分离、浓缩等等，但是设备都具有独立性，没有一体式操作，仍然需要耗费人力和时间，急需一种集萃取、纯化、浓缩等功能为一体，小巧、简便且易于与其他分析仪器直接联用的一体式前处理设备。
QuECHERS(Quick、Easy、Cheap、Rugged、Safe)是近年来国际上最新发展起来的一种用于农产品检测的快速样品前处理技术，由美国农业部Anastassiades教授等于2003年开发的。原理与高效液相 色谱和固相萃取相似，都是利用吸附剂填料与基质中的杂质相互作用，吸附杂质从而达到除杂净化的目的。具体而言是均质后的样品经乙腈提取后，采用萃取盐盐析分层后，利用基质分散萃取机理，采用PSA或其他吸附剂与基质中绝大部分干扰物(有机酸、脂肪酸、碳水化合物等)结合，通过离心方式去除，从而达到净化目的。
QuECHERS方法相比于传统前处理分析方法，具有样品用量低，对玻璃器皿的使用少，实验过程简单，降低了工作量，提高了工作效率，降低了认为因素造成的实验误差，因不需要大量的有机试剂可以有效避免对环境的二次污染等优势。
虽然QuECHERS方法有以上众多优势，但是仍然需要大量的时间和人员，存在集成度和自动化程度差等问题。
发明内容
本申请的目的是提供一种能够代替人工、有效提高实验准确性和实验效率、避免人为误差且集成度高、自动化程度高的全自动QuECHERS实验装置，以及使用该全自动QuECHERS实验装置进行实验的方法。
为了实现上述目的，本申请提供的技术方案如下：
一方面，本申请提供了一种全自动QuECHERS实验装置，其中：包括同时置放样品管、净化管和成品管的样品及试管模块，样品管内存放有待处理样品；
多功能机械臂，设置有抓取、搬运样品管或净化管或成品管用机械爪以及移液装置，移液装置配置成将样品管内液体移取到净化管内或将净化管内液体移取到成品管内；
拧盖模块，配合多功能机械臂实现样品管的管盖、净化管的管盖或成品管的管盖的拧开与拧紧；
加液模块，配置成向样品管内添加萃取液；
加样模块，包括分别向样品管内添加萃取盐和陶瓷均质子的加盐模块和陶瓷均质子模块；
震荡模块以及离心模块分别用于实现样品管内样品震荡和离心 的；
还包括用于对净化管内液体进行漩涡混匀的漩涡混匀模块；以及
氮吹浓缩模块，对成品管内液体吹入氮气实现无氧浓缩富集。
本申请的技术方案所述的氮吹浓缩模块包括水浴锅、氮吹仪以及控制氮吹仪工作的微处理器控制装置；
氮吹仪包括气体喷嘴，气体喷嘴配置成向成品管内吹入氮气且吹气方向斜向下吹向成品管的管壁；
氮吹浓缩过程中成品管浸在水浴锅中通过水浴锅内水浴温度控制成品管内液体温度。
本申请的技术方案还包括吸头模块和吸头回收盒；
吸头模块设置有吸头承载板，吸头承载板上设置有吸头容纳盒，吸头容纳盒内放置有多个一次性吸头；
移液装置可吸取一次性吸头后再通过一次性吸头吸取净化管内液体移取至成品管内。
本申请所述的技术方案还包括由X轴组件、Y轴组件和Z轴组件集合组成的XYZ三轴模块；
Z轴组件包括相互连接的Z轴滑块和Z轴导轨，以及控制Z轴滑块在Z轴导轨上上下移动的Z轴电机，多功能机械臂安装在Z轴滑块上；
Z轴组件安装在Y轴组件上，且Y轴组件又安装在X轴组件上，X轴组件和Y轴组件用于实现多功能机械臂前后方向和左右方向的平移。
本申请的技术方案所述的多功能机械臂包括与Z轴滑块连接的伸缩块，伸缩块可在Z轴滑块上上下伸缩运动；
机械爪与Z轴滑块连接，移液装置安装在伸缩块上，机械爪工作时，移液装置随伸缩块向上缩回。
本申请的技术方案所述的加液模块模块包括八通道切换阀和注液装置，注液装置设置为八个，八个注液装置一一对应安装在八通道切换阀的各个通道处。
本申请的技术方案所述的加盐模块由上到下依次设置有盐仓、转 动体和驱动转动体转动的驱动单元，在加盐模块底部设置有加盐口，转动体上开设有料斗，料斗随着转动体转动与盐仓或者加盐口连通；
转动体内设置有用于调节料斗大小的调节块。
本申请的技术方案所述的陶瓷均质子模块包括转盘、驱动转盘转动的转盘电机以及支撑板；
转盘上周向均列有多个用于存放陶瓷均质子的存放孔；
支撑板设置在转盘下方，且支撑板上开设有与存放孔相通的落料孔；
支撑板上铰接安装有拨杆，拨杆转动实现对落料孔的堵塞或打开。
本申请的技术方案所述的支撑板上于落料孔下方位置处安装有用于检测陶瓷均质子落下的落料传感器。
本申请的技术方案所述的拧盖模块包括开合盖组件，开合盖组件设置有样品管拧盖工位、净化管和成品管拧盖工位，在样品管拧盖工位、净化管和成品管拧盖工位处分别安装有用于固定样品管、净化管和成品管的摩擦自锁套，摩擦自锁套连接有驱动电机。
本申请的技术方案所述的拧盖模块还包括平移导轨、设置在平移导轨上的拧盖滑块以及驱动拧盖滑块在平移导轨上平移的平移电机；
开合盖组件固定安装在拧盖滑块上。
本申请的技术方案所述的震荡模块包括震荡基板，震荡基板上固定设置有震荡电机，震荡电机通过凸轮配合连接有垂直滑块；
垂直滑块固定连接有用于夹固样品管或净化管试管紧固件；铰接有挡板气缸，与挡板气缸铰接有挡板；
挡板配置成配合试管紧固件压住样品管或净化管；
挡板气缸用于实现挡板压紧样品管或净化管或者翻转远离样品管或净化管。
本申请的技术方案所述的漩涡模块包括试管压紧组件以及试管转动组件；
试管压紧组件包括压紧滑块以及控制压紧滑块上下移动的压紧气缸，还包括压板以及和压板连接的压盘；
试管转动组件包括漩涡电机和漩涡盘，漩涡盘通过漩涡轴承与漩涡电机连接，在漩涡盘上连接有用于承载净化管的试管筒；
压盘配置成压紧净化管。
本申请的技术方案还包括冰浴模块；
冰浴模块包括热交换器、散热风扇、试管置放工位、冷却液循环泵以及冷量存储块；
还设置有制冷片和隔热棉。
另一方面，本申请提供了一种采用上述全自动QuECHERS实验装置的实验方法，包括以下步骤：
第一步：向样品管内加液、加样
(1)多功能机械臂在XYZ三轴模块上移动至样品管架处，机械爪抓取样品管到拧盖模块的样品管拧盖工位，开合盖组件配合机械爪把样品管的管盖拧开；
(2)开合盖组件在平移导轨上移动，加液模块先向样品管内添加萃取液，然后开合盖组件继续移动至加盐模块处，加盐模块向样品管内添加萃取盐，开合盖组件继续移动至陶瓷均质子模块，陶瓷均质子模块向样品管内添加陶瓷均质子。
第二步：对样品管内液体震荡混匀并离心
(1)开合盖组件平移返回至最初位置，配合机械爪拧紧样品管的管盖，多功能机械臂在XYZ三轴模块上移动，机械爪抓取样品管送至震荡模块处进行震荡混匀；
(2)多功能机械臂继续在XYZ三轴模块上移动，机械爪抓取样品管送至离心模块处进行离心；
(3)机械爪抓取样品管将样品管移动至拧盖模块的样品管拧盖工位。
第三步：移液
(1)机械爪配合开合盖组件将样品管的管盖拧开；
(2)多功能机械臂在XYZ三轴模块上移动，机械爪抓取净化管送至拧盖模块的净化管和成品管拧盖工位；
(3)机械爪配合开合盖组件将净化管的管盖拧开；
(4)移液装置将样品管内上清液移取至净化管内；
(5)机械爪配合开合盖组件将净化管的管盖拧紧。
第四步：漩涡混匀
(1)多功能机械臂继续在XYZ三轴模块上移动，机械爪抓取净化管送至漩涡混匀模块处进行漩涡混匀；
(2)多功能机械臂将净化管送至拧盖模块的净化管和成品管拧盖工位处；
(3)机械爪配合开合盖组件将净化管的管盖拧开。
第五步：移液
(1)多功能机械臂在XYZ三轴模块上移动，机械爪抓取成品管送至拧盖模块的净化管和成品管拧盖工位；
(2)机械爪配合开合盖组件将成品管的管盖拧开；
(3)多功能机械臂移动，将移液装置移至吸头模块上方，移液装置吸取一次性吸头；
(4)移液装置带动一次性吸头抽取净化管内的上清液至成品管；
(5)拧紧净化管和成品管的管盖，并将净化管和成品管分别送至净化管架和成品管架。
第六步：氮吹浓缩
(1)向成品管内吹入氮气对成品管内液体进行氮吹浓缩。
综上所述，本申请具有以下有益效果:
(1)本装置进行实验时，多功能机械臂由加样和试管模块搬运样品管至拧盖模块处，机械爪和开合盖组件配合拧开样品管的管盖，通过加液模块、加盐模块和陶瓷均质子模块依次向样品管内添加萃取液、萃取盐和陶瓷均质子，拧紧管盖，经由震荡模块和离心模块震荡和离心；移液装置将样品管内上清液移取到净化管内，然后漩涡混匀模块进行漩涡混匀，再将净化管内上清液移取至成品管内经由氮吹浓缩模块进行无氧浓缩富集(整个过程中对样品管的管盖、净化管管盖和成品管的管盖的拧紧和拧开动作省略未细述)。
整个过程实验自动化程度高，实验效率高且可靠性高；同时创新性的添加了氮吹浓缩模块，不需要人工将成品管送到专门的氮吹仪进 行浓缩，实现了实验过程的全自动化。
(2)氮吹无氧浓缩富集过程中，利用氮吹仪将氮气快速、连续的吹向成品管内液体表面，使液体中溶剂迅速蒸发、分离，从而实现样品的浓缩，一方面保持液体样品的纯净，达到快速分离纯化的效果；另一方面氮气可以起到隔绝氧气的作用，防止氧化。
氮吹仪气体喷嘴吹气方向的设置，使得气体喷嘴吹出的氮气流在浓缩管内形成螺旋状气流，有效增加吹扫面积，减缓了气流冲力，使得成品管内液体中溶剂均匀挥发不飞溅。
移液装置将净化管内上清液移取至成品管内之前，可以先吸取吸头模块中的一次性吸头，通过一次性吸头吸取上清液移取至成品管内，避免移液装置在移取样品管内液体样品后有残留而污染净化管内上清液，影响实验结果。
XYZ三轴模块的设置，可实现多功能机械臂前后、左右和上下方向的移动，进而保证了多功能机械臂抓取样品管或净化管或成品管可朝多个方向搬运至合适位置，减少了人工的搬运。而Z轴电机可驱动滑块上下移动，机械爪抓取样品管或净化管或成品管时，移液装置处于向上缩回状态，移液装置工作时，处于向下伸出状态，机械爪和移液装置不会相互干扰。
加液模块向样品管内添加萃取液时，可以在八通道切换阀的各个通道内一一对应均安装加液装置，可实现八种溶液的供给。
整个加盐动作由驱动单元控制转动体旋转带动料斗旋转完成，即料斗与盐仓连通时盐仓内盐落入料斗，料斗旋转至与加盐口相通时盐落入样品管，不需人工操作加盐，完成了加盐工作的自动化。调节块可调节料斗大小，进而使得加盐量可控可调。
陶瓷均质子模块添加陶瓷均质子时，亦是通过转盘电机驱动转盘转动，存放孔内陶瓷均质子自动经由落料孔落入样品管内，落料传感器感应是否有陶瓷均质子落下来反馈至转盘电机驱动转盘转动，无需人工操作，自动化程度高。
而拧盖模块中摩擦自锁套的设置，避免了第二驱动电机驱动拧盖模块工作时样品管或净化管或成品管在拧盖模块上打滑不动，出现试 管盖拧紧不成功，容易松脱，导致试验需停止，人为进行干预的情况。
附图说明
图1是本申请一种全自动QuECHERS实验装置的内部结构示意图；
图2是本申请一种全自动QuECHERS实验装置的内部俯视图；
图3是一种全自动QuECHERS实验装置的工作原理图；
图4是实施例中样品及试管模块的示意图；
图5是实施例中XYZ三轴模块的结构示意图；
图6是实施例中XYZ三轴模块中Z轴组件的结构示意图；
图7是实施例中多功能机械臂的结构示意图；
图8是实施例中拧盖模块的结构示意图；
图9是实施例中拧盖模块的局部剖视图；
图10是实施例中加样模块的示意图；
图11是实施例中加盐模块的剖视图；
图12是实施例中陶瓷均质子模块的结构示意图；
图13是实施例中震荡模块的结构示意图；
图14是实施例中离心模块的结构示意图；
图15是实施例中漩涡混匀模块的示意图；
图16是实施例中漩涡混匀模块和净化管连接关系图；
图17是实施例中吸头模块的示意图；
图18是实施例中氮吹浓缩模块的氮吹示意图；
图19是实施例中冰浴模块的结构示意图。
图中：
01、样品及试管模块；101、样品管架；201、净化管架；301、成品管架；401、管支架；
02、XYZ三轴模块；102、X轴组件；202、Y轴组件；302、Z轴组件；3021、Z轴电机；3022、Z轴导轨；3023、Z轴滑块；
03、多功能机械臂；103、伸缩块；203、移液装置；303、机械爪；
04、拧盖模块；104、平移电机；204、拧盖滑块；304、平移导 轨；404、开合盖组件；4041、样品管拧盖工位；4042、净化管和成品管拧盖工位；4043、摩擦自锁套；4044、驱动电机；
05、加液模块；
06、加样模块；106、加液头；206、加样支架；
07、加盐模块；107、盐仓；207、转动驱动单元；307、转动体；3071、料斗；407、调节块；507、加盐口；
08、陶瓷均质子模块；108、转盘电机；208、转盘；2081、存放孔；308、支撑板；3081、落料孔；408、落料传感器；508、拨杆；
09、震荡模块；109、挡板；209、挡板气缸；309、震荡电机；409、试管紧固件；509、垂直滑块；609、震荡基板；709、减震脚垫；
10、离心模块；110、门滑轨；210、开关门气缸；310、离心转子；410、取放口；
11、漩涡混匀模块；111、压板；211、压盘；311、压紧气缸；411、压紧滑块；511、试管筒；611、漩涡电机；711、漩涡轴承；811、漩涡盘；
12、吸头模块；112、吸头承载板；212、吸头盒；312、一次性吸头；412、内标溶液杯；512、固定块；
13、冰浴模块；113、热交换器；213、冷量存储块；313、隔热棉；413、冷却液循环泵；513、制冷片；613、试管置放工位。
具体实施方式
以下结合附图对本申请作进一步详细说明。
本申请提供了一种全自动QuECHERS实验装置，如图1和图2所示，包括样品及试管模块01、XYZ三轴模块02、多功能机械臂03、拧盖模块04、加液模块05、加盐模块07、陶瓷均质子模块08、震荡模块09、离心模块10、漩涡混匀模块11以及氮吹浓缩模块，还包括底板和支架。其中，如图4所示，样品及试管模块01包括样品管架101、净化管架201和成品管架301，样品管架101、净化管架201和成品管架301水平方向依次排列并通过管支架401固定安装在底板上，具体安装方式为：管支架401通过螺钉螺纹固定连接在底板上， 管支架401上设置有定位凹槽，在样品管架101、净化管架201和成品管架301上均设置有与定位凹槽匹配的定位销，样品管架101、净化管架201和成品管架301通过定位销插入对应的定位凹槽内完成与管支架401的固定连接，且样品管架101、净化管架201和成品管架301为抽屉式固定安装在管支架401上；样品管架101、净化管架201和成品管架301均设置多个试管固定位置；样品管架101用于容纳多个样品管，且样品管内盛装有待处理样品；净化管架201和成品管架301分别容纳多个净化管和成品管(以下可将样品管、净化管和成品管统称为试管)。
图5对XYZ三轴模块02进行了附图展示，由图1和图5可看出，XYZ三轴模块02安装在支架上，包括X轴组件102、Y轴组件202和Z轴组件302；X轴组件102包括两根平行安装在支架上的水平向X轴导轨，两根X轴导轨由连接杆连接并同步驱动，两根X轴导轨上均配合设置有X轴滑块，连接杆配合连接有X轴导轨驱动电机；打开X轴导轨驱动电机，X轴导轨驱动电机带动连杆运动，连杆同步驱动两根X轴导轨运动，使得X轴滑块在X轴导轨上相对水平移动。Y轴组件202水平设置有一根Y轴导轨，但Y轴导轨与X轴导轨垂直方向设置；Y轴组件202可在X轴导轨上沿X轴导轨长度方向滑动，具体方式设置为，Y轴导轨的两端对应固定连接在两根X轴导轨上的X轴滑块上，X轴导轨运动，X轴滑块相对X轴导轨移动时，带动Y轴组件202沿X轴滑轨方向移动；Y轴组件202还包括驱动Y轴导轨运动的Y轴导轨驱动电机，用于驱动Y轴导轨运动。Y轴导轨上配合设置有可相对Y轴导轨沿Y轴导轨长度方向移动的Y轴滑块，Z轴组件302固定连接在Y轴滑块上，可随Y轴滑块沿Y轴导轨长度方向移动；如图6所示，Z轴组件302包括Z轴电机3021以及Z轴电机3021驱动的Z轴导轨3022，Z轴导轨3022竖直方向设置；Z轴导轨3022上配合设置有相对Z轴导轨3022上下移动的Z轴滑块3023。
多功能机械臂03固定安装在Z轴滑块3023上，驱动X轴导轨驱动电机，X轴滑块沿X轴导轨长度方向(以下称前后方向)移动，带动Y轴组件202以及与Y轴滑块固定连接的Z轴组件302以及与Z轴 组件302连接的多功能机械臂03一起前后方向移动；驱动Y轴导轨驱动电机，Y轴滑块沿Y轴导轨长度方向(以下简称左右方向)移动，带动Z轴组件302以及与Z轴组件302连接的多功能机械臂03一起左右方向移动；驱动Z轴电机3021，Z轴滑块3023沿Z轴导轨3022长度方向(以下称上下方向)移动，带动多功能机械臂03一起上下方向移动。
图7是多功能机械臂03的结构示意图，由图7所述，多功能机械臂03包括伸缩块103、移液装置203和用于抓取试管的机械爪303还包括与Z轴滑块固定连接的安装板。伸缩块103和机械爪303均通过安装板与Z轴滑块3023固定连接；移液装置203安装在伸缩块103上，机械爪303抓取试管工作时，移液装置203随伸缩块103向上缩回，移液装置103移取样品液体时，移液装置103随伸缩块103伸出；移液装置103可采用吸液管。
由图8所述，拧盖模块04包括平移电机104、平移电机104驱动的平移导轨304以及与平移导轨304配合安装且在平移导轨304上相对滑动的拧盖滑块204，还包括固定安装在拧盖滑块204上的开合盖组件404；平移电机104工作，带动拧盖滑块204相对平移导轨304沿平移导轨304长度方向移动，进而带动开合盖组件404沿平移导轨304长度方向移动；开合盖组件404设置有样品管拧盖工位4041、净化管和成品管拧盖工位4042；在样品管拧盖工位4041、净化管和成品管拧盖工位4042处分别安装有用于固定样品管、净化管和成品管的摩擦自锁套4043，摩擦自锁套4043连接有驱动电机4044，具体连接安装方式如图9所示。试管固定在样品管拧盖工位4041或净化管和成品管拧盖工位4042的摩擦自锁套4043内，驱动电机4044驱动摩擦自锁套4043转动，试管可在和摩擦自锁套4043的摩擦力的带动下跟随摩擦自锁套4043转动。
加液模块05包括八通道切换阀和注液装置，注液装置包括步进电机、精密丝杠和微量进样器，步进电机驱动精密丝杠带动微量进样器进行萃取液的供给；注液装置设置八个，八个注液装置一一对应安装在八通道切换阀的八个通道处，可以在不同的注液装置中加入不同 的萃取液，用八通道切换阀切换不同的萃取液通道，最多可实现八种萃取液的供给。此外，本申请的加液模块05还可以设置自动清洗装置(图中未表示出)，通过智能控制程序控制八通道切换阀切换萃取液后进行自动清洗；微量进样器可控制在一次最大为25ml的供给量来满足仪器的使用要求。
加样模块06包括分别向样品管内添加萃取盐和陶瓷均质子的加盐模块07和陶瓷均质子模块08，还包括加样支架206；加盐模块07和陶瓷均质子模块08均安装在加样支架206上；在加样支架206上还设置有加液头106，加液头106与加液模块05连通，即加液模块05内的微量进样器与加液头106通过管路(图中未表示出)连通，微量进样器推出的萃取液经由管路流到加液头106处进行加液；结合图1和图10所示，加样支架206固定安装在底板上，且加样支架206套住拧盖模块04，即拧盖模块04的平移导轨304位于加样模块06的下方，加液头106、加盐模块07和陶瓷均质子模块08按序沿平移导轨304的长度方向安装在加样支架206上，开合盖组件404沿平移导轨304长度方向移动，可先后移动到加液头106下方位置、加盐模块07下方位置以及陶瓷均质子模块08的下侧位置。
加盐模块07的结构示意图如图11所示，包括盐仓107、转动体307、驱动转动体307转动的驱动单元207，在加盐模块07底部还开设加盐口507。具体实施方式为：加盐模块07包括柱形筒体，柱形筒体中空设置内部为盐仓107，柱形筒体顶部配合安装有堵盖，打开堵盖，可以向盐仓107内添加萃取盐；柱形筒体底部与转动体307连接，转动体307上料斗3071，料斗3071可随转动体307转动；在转动体307下侧位置处连接有出盐部，出盐部开设有加盐口507，料斗3071随着转动体307转动时，料斗3071的开口可转动至于盐仓107连通或与加盐口507连通；在转动体307内还设置有调节块407，调节块407可以调节料斗3071的大小，进而使得料斗3071经由加盐口507掉落加的萃取盐的量可调。
加盐模块07的工作原理：驱动单元207先驱动转动体307转动至料斗3071与盐仓107连通的状态(即料斗3071开口朝上)，打开 堵盖，向盐仓107内加入萃取盐，萃取盐进入料斗3071中，然后驱动单元207驱动转动体307转动，一般转动180°，料斗3071随之转动直至料斗3071开口与加盐口507连通，此时，料斗3071内的萃取盐在重力作用下经由加盐口507掉落进行加盐，然后料斗3071在弹簧作用下复位，等待下次加盐；需要调节加盐量时，可直接调节调节块407改变料斗3071的大小来完成。
如图12所示，陶瓷均质子模块08包括转盘208、驱动转盘208转动的转盘电机108以及支撑板308；支撑板308与加样支架206固定连接，转盘208上周向均列有多个用于存放陶瓷均质子的存放孔2081，在支撑板308上开设有可以与存放孔2081连通的落料孔3081，转盘208转动时，每个存放孔2081均可转动至落料孔3081处于落料孔3081连通；在支撑板308上铰接有拨杆508，拨杆508可以绕其与支撑板308铰接的铰接轴处转动，拨杆508转动位于落料孔3081下方与支撑板308抵触并将落料孔3081堵住；在支撑板308上还安装有落料传感器408，用于检测是否会有陶瓷均质子由落料孔3081落下。
陶瓷均质子模块08的工作原理：不工作时，拨杆508堵住转盘308上的落料孔3081；当需要向样品管内添加陶瓷均质子时，拧盖模块04移动到陶瓷均质子模块08下方位置处，拧盖模块04触发拨杆508，拨杆508转动打开落料孔3081，添加在存放孔2081内的陶瓷均质子会经由落料孔3081落入拧盖模块04上的样品管内；当落料传感器408没有检测到陶瓷均质子的下落动作，则转盘电机108会驱动转盘208转动直至另一个存放孔2081与落料孔3081相通，落料传感器408没有检测到陶瓷均质子下落，转盘208就一直转直至落料传感器408检测到了陶瓷均质子的下落。
图13示出了震荡模块09的结构，包括震荡基板609，震荡基板609上安装有震荡电机309，震荡电机309与垂直滑块509通过凸轮连接，即震荡电机309连接有凸轮，凸轮与垂直滑块509抵接，凸轮在震荡电机309的带动下转动，转动过程中带动垂直滑块509上下往复运动；震荡模块09还包括挡板气缸209以及与挡板气缸209连接 的挡板109，还包括固定连接在垂直滑块509上的试管紧固件409；挡板气缸209与挡板109以及垂直滑块509均铰接，挡板109用于压紧或松开试管紧固件409紧固的试管。震荡模块09还可设置减震脚垫709减震，减震脚垫709可直接安装在震荡基板609下方。
震荡模块09的工作原理：初始时，震荡电机309和挡板气缸209均不工作，挡板109呈竖直状态；当多功能机机械臂03抓取试管移至试管紧固件409处，挡板气缸209伸长，挡板109旋转成水平状态压住试管紧固件409处的试管，然后震荡电机309工作带动垂直滑块509上下往复运动，试管紧固件409随之上下往复运动完成震荡动作。
如图14所示，离心模块10包括离心护盖，离心护盖上开设取放口410，取放口410处安装有门滑轨110，配合安装有开关门(图中未表示出)，开关门连接有开关门气缸210，开关门气缸210伸出带动开关门在门滑轨110上滑动至闭合取放口410，开关门气缸210缩回带动开关门在门滑轨110上滑动至打开取放口410；离心护盖内设置有离心转子310，离心转子310在圆周上有定位功能，取放试管时，试管定位在取放口410正下方并打开开关门。
如图15所示，漩涡模块11包括试管压紧组件和试管转动组件，试管压紧组件包括安装架、压板111、压盘211、压紧气缸311、压紧滑块411；压盘211固定连接在压板111上，压板111铰接安装在压紧滑块411上，且压板111可由竖直状态转动90度呈水平状态；压紧滑块411与安装架滑动连接，具体为安装架上安装有导向柱，压紧滑块411套设在导向柱上，压紧气缸311与压紧滑块411连接用来控制压紧滑块411上下运动。试管转动组件包括漩涡电机611、漩涡盘811、试管筒511，图16显示了试管转动组件的安装结构，漩涡盘811通过漩涡轴承711以及偏心轴(图中未表示出)与漩涡电机611连接，试管筒511安装在漩涡盘811上。
漩涡混匀模块11的工作原理：试管先移至试管筒511内与漩涡盘811抵接，压紧气缸311带动压紧滑块411向下运动，压板111先翻转90度再向下运动，压板111由竖直状态翻转至水平状态，压盘211随之翻转至盘口对准试管筒511内的试管压紧，漩涡电机611启 动，带动偏心轴转动，偏心轴又带动漩涡盘811转动，进而完成试管内液体的涡旋混匀作业。
吸头模块12如图17所示，包括吸头承载板112，吸头承载板112上设置吸头容纳盒212，还设置有用于压住固定吸头容纳盒212的固定块512，吸头容纳盒212内放置有多个一次性吸头312；移液装置203可先吸取一个一次性吸头312然后将试管内液体吸进一次性吸头312内；在底板上还设置有吸头回收盒，吸头回收盒位于样品及试管模块01中净化管架201的下方，用过的一次性吸头312可通过移液装置203移动至吸头回收盒内。
吸头模块12上还设置内标溶液杯412，内标溶液杯412内可添加内标溶液，经由移液装置203吸取并添加到对应试管内。
氮吹浓缩模块包括水浴锅、氮吹仪以及控制氮吹仪工作的微处理器控制装置，氮吹仪包括气体喷嘴；图18示出了氮吹浓缩模块对成品管内液体进行氮吹浓缩富集的原理图，气体喷嘴斜向下方向设置，氮吹仪吹出氮气经由气体喷嘴斜向下吹向成品管的管壁，成品管浸在水浴锅内通过水浴锅内水浴温度控制成品管内液体温度，样品在一定的温度下，水浴温度控制范围从30℃到60℃，通过氮气吹扫，可获得良好的富集效果；气体喷嘴特定方向设置，吹出的氮气流在成品管内形成螺旋状气流，有效增加吹扫面积，减缓了气流崇礼，使溶剂均匀挥发且不飞溅；该原理的氮吹仪市面上已有产品，可直接购买使用，如NS-12S型号的氮吹仪。
进一步地，该申请还包括冰浴模块13，如图19所示，冰浴模块13包括试管置放工位613，用于置放试管，还包括位于试管置放工位613处的冷量存储块213以及包裹冷量存储块213的隔热棉313，试管位于试管置放工位613时，冷量存储块213将试管包围对试管传递冷量，隔热棉313将外界热气隔开避免了冷量存储块213的温度快速变化，提高制冷效率；冰浴模块13还包括冷却液循环泵413，冷却液循环泵413上设置制冷片513，冷量存储块213位于制冷片513上，制冷片513使冷量存储块213温度降低，可设计温度探头探测温度；冰浴模块13还包括热交换器113以及散热风扇(图中未表示出)， 散热风扇通过安装件安装在热交换器113上，冷却液循环泵413吧制冷片513的热量输送至热交换器113上，散热风扇对其进行风冷散热。
本申请还提供了一种全自动QuECHERS实验装置的实验方法，如图3所示，其工作原理和工作步骤包括加液、加样、震荡、离心、移液、漩涡混匀、移液和氮吹浓缩；其中加液操作包括以下步骤：
首先，XYZ三轴模块02运动，控制多功能机械臂03前后、左右或上下移动至样品管架101上方，机械爪303抓取一个装有待测样品的样品管，控制XYZ三轴模块运动，使得多功能机械臂03移动至拧盖模块04，机械爪303移取样品管至开合盖组件404的样品管拧盖工位4041，机械爪303抓住样品管的管盖，然后开合盖组件404的驱动电机4044工作，驱动摩擦自锁套4043转动带动样品管转动，直至样品管的管盖打开；此时，拧盖模块04的平移电机104工作，驱动平移导轨304动作带动拧盖滑块204动作，此时开合盖组件404沿平移导轨304移动，直至拧开管盖的样品管位于加液头106下，打开加液模块05，加液模块05的注液装置注出萃取液经由加液头106加入到样品管内。
加样步骤包括以下步骤：
平移电机104工作，开合盖组件404继续移动，直至样品管移动至加盐模块07的加盐口507下，此时盐仓107内已添加有萃取盐，然后转动驱动单元207工作带动转动体307转动，料斗3071内的萃取盐转动经由加盐口507落入至样品管内完成萃取盐的加样；平移电机104工作，开合盖组件404继续移动，直至开合盖组件404移动至陶瓷均质子模块08的拨杆508处打开拨杆508，存放孔2081内的陶瓷均质子则通过落料孔3081落入样品管内完成陶瓷均质子的加样。
所述震荡、离心操作包括以下步骤：
首先，平移电机104工作，开合盖组件404移动，直至开合盖组件404复位至最初位置，此时机械爪303和驱动电机4044驱动的摩擦自锁套4043配合将样品管的管盖拧紧到样品管上；然后机械爪303抓取样品管后，多功能机械臂03移动直至将样品管移至震荡模块09，样品管被试管紧固件409固定，挡板109压紧样品管，震荡电机309 工作带动垂直滑块509上下往复运动，带动震荡基板609连带样品管上下往复运动完成震荡作业。
当样品管在震荡模块09完成震荡作业后，机械爪303抓取样品管，多功能机械臂03在XYZ三轴模块02上移动直至将样品管移至离心模块10内进行离心，主要是先控制开关门气缸210工作打开开关门，将样品管定位放置在取放口410正下方，然后关紧开关门对样品管进行离心作业。
第一次移液操作包括以下步骤：
样品管完成离心作业后，机械爪303抓取样品管被多功能机械臂03移至开合盖组件404的样品管拧盖工位4041，机械爪303配合开合盖组件404将样品盖的管盖拧开，然后机械爪303移至净化管架201处抓取净化管，多功能机械臂03移动将净化管移取至开合盖组件404的净化管和成品管拧盖工位4042处，机械爪303配合开合盖组件404将净化管的管盖拧开，此时，移液装置203开始工作，移液装置203移至样品管处吸取样品管内的上清液移至净化管内，最后机械爪303配合开合盖组件404先后将样品管和净化管的管盖拧紧，至此完成第一次的移液工作，即将样品管内上清液移取至净化管内。
样品管内上清液移至净化管内后，需要对净化管内液体进行漩涡混匀，漩涡混匀步骤如下：
机械爪303抓取净化管将其移至漩涡混匀模块11处并将净化管置于试管筒511内，压紧气缸311工作使得压盘211压紧净化管，漩涡电机611带动漩涡盘811转动，从而完成净化管的漩涡混匀。
完成漩涡混匀作业的净化管需要被多功能机械臂03送回至开合盖组件404的净化管和成品管拧盖工位4042，以便进行第二次移液动作。
第二次移液时，需机械爪303配合开合盖组件404将净化管的管盖拧开，然后多功能机械臂03移动并抓取成品管将成品管移至净化管和成品管拧盖工位4042处，拧开成品管管盖；然后多功能机械臂移动至吸头模块12处，移液装置203吸取一个一次性吸头312再移至净化管处，移液装置203工作，一次性吸头312吸取净化管内的上 清液并被移动至成品管内；最后，机械爪303配合开合盖组件404先后完成净化管的管盖和成品管的管盖拧紧动作。
完成第二次移液动作后，多功能机械臂03移动，可将一次性吸头312丢至在吸头回收盒内。
氮吹浓缩操作包括以下步骤：
多功能机械臂03将成品管移至氮吹浓缩模块14处，拧开成品管的管盖，然后打开氮吹浓缩模块14内的氮吹仪，氮吹仪向成品管内吹入氮气进行浓缩富集；此过程中，可对水浴锅214进行加热至水浴温度控制范围从30℃到60℃，通过传热控制成品管内温度，提高浓缩富集效率。
以上所述仅是本申请的优选实施方式，本申请的保护范围并不仅局限于上述实施例，凡属于本申请思路下的技术方案均属于本申请的保护范围。应当指出，对于本技术领域的普通技术人员来说，在不脱离本申请原理前提下的若干改进和润饰，这些改进和润饰也应视为本申请的保护范围。

Claims (15)

  1. 一种全自动QuECHERS实验装置，其特征是：包括同时置放样品管、净化管和成品管的样品及试管模块(01)，样品管内存放有待处理样品；
    多功能机械臂(03)，设置有抓取、搬运样品管或净化管或成品管用机械爪(303)以及移液装置(203)，移液装置(203)配置成将样品管内液体移取到净化管内或将净化管内液体移取到成品管内；
    拧盖模块(04)，配合多功能机械臂(03)实现样品管的管盖、净化管的管盖或成品管的管盖的拧开与拧紧；
    加液模块(05)，配置成向样品管内添加萃取液；
    加样模块(06)，包括分别向样品管内添加萃取盐和陶瓷均质子的加盐模块(07)和陶瓷均质子模块(08)；
    震荡模块(09)以及离心模块(10)分别用于实现样品管内样品震荡和离心的；
    还包括用于对净化管内液体进行漩涡混匀的漩涡混匀模块(11)；以及
    氮吹浓缩模块，对成品管内液体吹入氮气实现无氧浓缩富集。
  2. 根据权利要求1所述的全自动QuECHERS实验装置，其特征是：
    氮吹浓缩模块包括水浴锅、氮吹仪以及控制氮吹仪工作的微处理器控制装置；
    氮吹仪包括气体喷嘴，气体喷嘴配置成向成品管内吹入氮气且吹气方向斜向下吹向成品管的管壁；
    氮吹浓缩过程中成品管浸在水浴锅中通过水浴锅内水浴温度控制成品管内液体温度。
  3. 根据权利要求1所述的全自动QuECHERS实验装置，其特征是：还包括吸头模块(12)和吸头回收盒；
    吸头模块(12)设置有吸头承载板(112)，吸头承载板(112)上设置有吸头容纳盒(212)，吸头容纳盒(212)内放置有多个一次性吸头(312)；
    移液装置(203)可吸取一次性吸头(312)后再通过一次性吸头(312)吸取净化管内液体移取至成品管内。
  4. 根据权利要求1所述的全自动QuECHERS实验装置，其特征是：
    还包括由X轴组件(102)、Y轴组件(202)和Z轴组件(302)集合组成的XYZ三轴模块(02)；
    Z轴组件(302)包括相互连接的Z轴滑块(3023)和Z轴导轨(3022)，以及控制Z轴滑块(3023)在Z轴导轨(3022)上上下移动的Z轴电机(3021)，多功能机械臂(03)安装在Z轴滑块(3023)上；
    Z轴组件(302)安装在Y轴组件(202)上，且Y轴组件(202)又安装在X轴组件(102)上，X轴组件(102)和Y轴组件(202)用于实现多功能机械臂(03)前后方向和左右方向的平移。
  5. 根据权利要求4所述的全自动QuECHERS实验装置，其特征是：多功能机械臂(03)包括与Z轴滑块(3023)连接的伸缩块(103)，伸缩块(103)可在Z轴滑块(3023)上上下伸缩运动；
    机械爪(303)与Z轴滑块(3023)连接，移液装置(203)安装在伸缩块(103)上，机械爪(303)工作时，移液装置(203)随伸缩块(103)向上缩回。
  6. 根据权利要求1所述的全自动QuECHERS实验装置，其特征是：加液模块(05)包括八通道切换阀和注液装置，注液装置设置为八个，八个注液装置一一对应安装在八通道切换阀的各个通道处。
  7. 根据权利要求1所述的全自动QuECHERS实验装置，其特征是：加盐模块(07)由上到下依次设置有盐仓(107)、转动体(307)和 驱动转动体(307)转动的驱动单元(207)，在加盐模块(07)底部设置有加盐口(507)，转动体(307)上开设有料斗(3071)，料斗(3071)随着转动体(307)转动与盐仓(107)或者加盐口(507)连通；
    转动体(307)内设置有用于调节料斗(3071)大小的调节块(407)。
  8. 根据权利要求1所述的全自动QuECHERS实验装置，其特征是：陶瓷均质子模块(08)包括转盘(208)、驱动转盘(208)转动的转盘电机(108)以及支撑板(308)；
    转盘(208)上周向均列有多个用于存放陶瓷均质子的存放孔(2081)；
    支撑板(308)设置在转盘(208)下方，且支撑板(308)上开设有与存放孔(2081)相通的落料孔(3081)；
    支撑板(308)上铰接安装有拨杆(508)，拨杆(508)转动实现对落料孔(3081)的堵塞或打开。
  9. 根据权利要求8所述的全自动QuECHERS实验装置，其特征：支撑板(308)上于落料孔(3081)下方位置处安装有用于检测陶瓷均质子落下的落料传感器(408)。
  10. 根据权利要求4所述的全自动QuECHERS实验装置，其特征是：拧盖模块(04)包括开合盖组件(404)，开合盖组件(404)设置有样品管拧盖工位(4041)、净化管和成品管拧盖工位(4042)，在样品管拧盖工位(4041)、净化管和成品管拧盖工位(4042)处分别安装有用于固定样品管、净化管和成品管的摩擦自锁套(4043)，摩擦自锁套(4043)连接有驱动电机(4044)。
  11. 根据权利要求10所述的全自动QuECHERS实验装置，其特征是：拧盖模块(04)还包括平移导轨(304)、设置在平移导轨(304) 上的拧盖滑块(204)以及驱动拧盖滑块(204)在平移导轨(304)上平移的平移电机(104)；
    开合盖组件(404)固定安装在拧盖滑块(204)上。
  12. 根据权利要求1所述的全自动QuECHERS实验装置，其特征是：震荡模块(09)包括震荡基板(609)，震荡基板(609)上固定设置有震荡电机(309)，震荡电机(309)通过凸轮配合连接有垂直滑块(509)；
    垂直滑块(509)固定连接有用于夹固样品管或净化管试管紧固件(409)，并铰接有挡板气缸(209)，与挡板气缸(209)铰接有挡板(109)；
    挡板(109)配置成配合试管紧固件(409)压住样品管或净化管；
    挡板气缸(209)用于实现挡板(109)压紧样品管或净化管或者翻转远离样品管或净化管。
  13. 根据权利要求1所述的全自动QuECHERS实验装置，其特征是：漩涡混匀模块(11)包括试管压紧组件以及试管转动组件；
    试管压紧组件包括压紧滑块(411)以及控制压紧滑块(411)上下移动的压紧气缸(311)，还包括压板(111)以及和压板(111)连接的压盘(211)；
    试管转动组件包括漩涡电机(611)和漩涡盘(811)，漩涡盘(811)通过漩涡轴承(711)与漩涡电机(611)连接，在漩涡盘(811)上连接有用于承载净化管的试管筒(511)；
    压盘(211)配置成压紧净化管。
  14. 根据权利要求1所述的全自动QuECHERS实验装置，其特征是：还包括冰浴模块(13)；
    冰浴模块(13)包括热交换器(113)、散热风扇、试管置放工位(613)、冷却液循环泵(413)以及冷量存储块(213)；
    还设置有制冷片(513)和隔热棉(313)。
  15. 一种采用权利要求11-14任一项所述的全自动QuECHERS实验装置进行实验的实验方法，包括以下步骤：
    第一步：向样品管内加液、加样
    (1)多功能机械臂(03)在XYZ三轴模块(02)上移动至样品管架(101)处，机械爪(303)抓取样品管到拧盖模块(04)的样品管拧盖工位(4041)，开合盖组件(404)配合机械爪(303)把样品管的管盖拧开；
    (2)开合盖组件(404)在平移导轨(304)上移动，加液模块(05)先向样品管内添加萃取液，然后开合盖组件(404)继续移动至加盐模块(07)处，加盐模块(07)向样品管内添加萃取盐，开合盖组件(404)继续移动至陶瓷均质子模块(08)，陶瓷均质子模块(08)向样品管内添加陶瓷均质子；
    第二步：对样品管内液体震荡混匀并离心
    (1)开合盖组件(404)平移返回至最初位置，配合机械爪(303)拧紧样品管的管盖，多功能机械臂(03)在XYZ三轴模块(02)上移动，机械爪(303)抓取样品管送至震荡模块(09)处进行震荡混匀；
    (2)多功能机械臂(03)继续在XYZ三轴模块(02)上移动，机械爪(303)抓取样品管送至离心模块(10)处进行离心；
    (3)机械爪(303)抓取样品管将样品管移动至拧盖模块(04)的样品管拧盖工位(4041)；
    第三步：移液
    (1)机械爪(303)配合开合盖组件(404)将样品管的管盖拧开；
    (2)多功能机械臂(03)在XYZ三轴模块(02)上移动，机械爪(303)抓取净化管送至拧盖模块(04)的净化管和成品管拧盖工位(4042)；
    (3)机械爪(303)配合开合盖组件(404)将净化管的管盖拧开；
    (4)移液装置(203)将样品管内上清液移取至净化管内；
    (5)机械爪(303)配合开合盖组件(404)将净化管的管盖拧紧；
    第四步：漩涡混匀
    (1)多功能机械臂(03)继续在XYZ三轴模块(02)上移动，机械爪(303)抓取净化管送至漩涡混匀模块(11)处进行漩涡混匀；
    (2)多功能机械臂(03)将净化管送至拧盖模块(04)的净化管和成品管拧盖工位(4042)处；
    (3)机械爪(303)配合开合盖组件(404)将净化管的管盖拧开；
    第五步：移液
    (1)多功能机械臂(03)在XYZ三轴模块(02)上移动，机械爪(303)抓取成品管送至拧盖模块(04)的净化管和成品管拧盖工位(4042)；
    (2)机械爪(303)配合开合盖组件(404)将成品管的管盖拧开；
    (3)多功能机械臂(03)移动，将移液装置(203)移至吸头模块(12)上方，移液装置(203)吸取一次性吸头(312)；
    (4)移液装置(203)带动一次性吸头(312)抽取净化管内的上清液至成品管；
    (5)拧紧净化管和成品管的管盖，并将净化管和成品管分别送至净化管架(201)和成品管架(301)；
    第六步：氮吹浓缩
    (1)向成品管内吹入氮气对成品管内液体进行氮吹浓缩。
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