CN111803997B - Full-automatic oscillation extraction and purification device and pretreatment method - Google Patents
Full-automatic oscillation extraction and purification device and pretreatment method Download PDFInfo
- Publication number
- CN111803997B CN111803997B CN201910284888.9A CN201910284888A CN111803997B CN 111803997 B CN111803997 B CN 111803997B CN 201910284888 A CN201910284888 A CN 201910284888A CN 111803997 B CN111803997 B CN 111803997B
- Authority
- CN
- China
- Prior art keywords
- bottle
- mechanical arm
- extraction
- liquid
- needle
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000000605 extraction Methods 0.000 title claims abstract description 74
- 238000000746 purification Methods 0.000 title claims abstract description 49
- 230000010355 oscillation Effects 0.000 title claims abstract description 25
- 238000002203 pretreatment Methods 0.000 title claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 104
- 238000001914 filtration Methods 0.000 claims abstract description 29
- 238000011065 in-situ storage Methods 0.000 claims abstract description 20
- 238000011084 recovery Methods 0.000 claims abstract description 14
- 239000000523 sample Substances 0.000 claims description 42
- 238000005406 washing Methods 0.000 claims description 22
- 239000012528 membrane Substances 0.000 claims description 21
- 239000012521 purified sample Substances 0.000 claims description 21
- 239000002904 solvent Substances 0.000 claims description 21
- 230000002209 hydrophobic effect Effects 0.000 claims description 19
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 14
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical group CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 12
- 238000003780 insertion Methods 0.000 claims description 10
- 230000037431 insertion Effects 0.000 claims description 10
- 239000000945 filler Substances 0.000 claims description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 7
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 4
- 238000001514 detection method Methods 0.000 claims description 4
- 235000019262 disodium citrate Nutrition 0.000 claims description 4
- 239000002526 disodium citrate Substances 0.000 claims description 4
- 229940079896 disodium hydrogen citrate Drugs 0.000 claims description 4
- CEYULKASIQJZGP-UHFFFAOYSA-L disodium;2-(carboxymethyl)-2-hydroxybutanedioate Chemical compound [Na+].[Na+].[O-]C(=O)CC(O)(C(=O)O)CC([O-])=O CEYULKASIQJZGP-UHFFFAOYSA-L 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- 235000002639 sodium chloride Nutrition 0.000 claims description 4
- 239000001509 sodium citrate Substances 0.000 claims description 4
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 4
- 235000011083 sodium citrates Nutrition 0.000 claims description 4
- 230000009514 concussion Effects 0.000 claims description 2
- 230000035939 shock Effects 0.000 claims 1
- 239000000243 solution Substances 0.000 description 37
- 238000000034 method Methods 0.000 description 8
- 235000013305 food Nutrition 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000010926 purge Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 238000012856 packing Methods 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 3
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000012864 cross contamination Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000003640 drug residue Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000009885 systemic effect Effects 0.000 description 2
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000001172 liquid--solid extraction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000003805 vibration mixing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0261—Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
-
- 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
- G01N1/34—Purifying; Cleaning
-
- 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
- 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
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
-
- 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
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
- G01N2001/4088—Concentrating samples by other techniques involving separation of suspended solids filtration
Abstract
The application discloses a full-automatic oscillation extraction and purification device and a pretreatment method, comprising the following steps: the device comprises a first bottle rack with an automatic rotary addressing function, an oscillation extraction system, a purification system and a filtration liquid recovery system; the oscillation extraction system comprises: the device comprises an oscillator, a first bottle rack, an extraction bottle and a first mechanical arm; the extraction bottle is arranged on the first bottle rack and stops on the liquid level to be injected after rotating along with the first bottle rack; the liquid level to be injected is in the liquid transferring range of the first mechanical arm; the oscillator is arranged on the first bottle rack; and (3) carrying out in-situ oscillation and standing on the sample in an extraction bottle to obtain an extracting solution. The device is particularly suitable for pretreatment of samples to be detected according to national standard GB 23200.113-2018, and has high extraction and purification speed and high automation degree.
Description
Technical Field
The application relates to a full-automatic oscillation extraction purification device and a pretreatment method, and belongs to the field of sample pretreatment.
Background
In the process of analyzing and detecting medicine residues in foods such as fruits, grains and the like, the foods are generally crushed, then the liquid-solid extraction method is adopted, the traditional Chinese medicine residues in the foods are extracted into an extracting solution under the continuous oscillation action, and the extracting solution to be purified is obtained by centrifugation. And then further purifying the extracting solution by using technologies such as dispersion solid phase extraction purification and the like.
The above-described drug residue analysis and detection process has been forced to be formulated as a national standard. The gas chromatograph-mass spectrometer combined method for measuring the residual quantity of 208 pesticides and metabolites in national standard plant source food of national standard for food safety of national standard GB 23200.113-2018 comprises the following pretreatment processes:
(1) weighing a sample to be detected in a plastic centrifuge tube, adding acetonitrile, magnesium sulfate, sodium chloride, sodium citrate, disodium hydrogen citrate and 1 ceramic proton, covering a centrifuge tube cover, and centrifuging after intense shaking;
(2) absorbing a certain amount of supernatant, adding the supernatant into a plastic centrifuge tube containing magnesium sulfate and PSA, adding the magnesium sulfate, the PSA and GCB into the plastic centrifuge tube for the darker sample, and centrifuging after vortex mixing;
(3) accurately sucking a certain amount of supernatant in a test tube, blowing nitrogen in a water bath at 40 ℃ until the supernatant is nearly dry, re-dissolving, passing through a microporous filter membrane, and performing on-machine measurement.
Disclosure of Invention
According to one aspect of the application, a full-automatic oscillation extraction and purification device is provided, which can effectively improve the sample treatment efficiency, shorten the treatment time and automatically and gradually finish all the pretreatment operations.
Full-automatic concussion draws purifier, its characterized in that includes: the device comprises a first bottle rack with an automatic rotary addressing function, an oscillation extraction system, a purification system and a filtration liquid recovery system;
the oscillation extraction system comprises: the device comprises an oscillator, a first bottle rack, an extraction bottle and a first mechanical arm; the extraction bottle is arranged on the first bottle rack, rotates along with the first bottle rack and then stops on the liquid level to be injected; the liquid level to be injected is in the liquid transferring range of the first mechanical arm; the oscillator is arranged on the first bottle rack;
and (3) carrying out in-situ vibration and in-situ filtration on the sample in the extraction bottle through a hydrophobic porous filter membrane to obtain an extracting solution.
Optionally, the oscillation extracting system includes: the first liquid inlet needle, the first tray body, the solvent bottle and the first needle washing container are arranged on the first tray body;
the solvent bottle and the first needle washing container are arranged in the pipetting range of the first mechanical arm;
the first liquid inlet needle is arranged on the liquid taking end of the first mechanical arm;
the first mechanical arm moves the first liquid inlet needle into the first needle washing container to wash the needle, and then takes the solvent from the solvent bottle and moves the solvent into the extraction bottle;
optionally, the solvent is acetonitrile.
Optionally, the extraction bottle comprises: the bottle comprises a bottle cap, an inner insertion tube, a hydrophobic porous filter membrane and a bottle body, wherein one end of the inner insertion tube is sleeved with the hydrophobic porous filter membrane and extends into the bottle body, and the other end of the inner insertion tube is an open end inserted into the bottle cap and exposes the open end on the surface of the bottle cap;
preferably, sample and extraction filler are contained in a cavity between the inner cannula and the vial;
preferably, the extraction filler is: magnesium sulfate, sodium chloride, sodium citrate, disodium hydrogen citrate.
Optionally, the purification system comprises: a purifying column and a second mechanical arm;
the purifying column and the filtering liquid recovery system are arranged in the grabbing range of the second mechanical arm; the second mechanical arm grabs the purifying column and pulls a piston in the purifying column to suck the extracting solution;
and the second mechanical arm pushes the piston in the purifying column to purify the extracting solution to obtain purified solution.
Optionally, the purification column comprises: a piston, a cylinder tube, and a layer of filter material; the piston is accommodated in the column tube and slides along the inner wall of the column tube; the first end of the cylinder tube is open, and the second end of the cylinder tube is provided with a liquid outlet; the second end of the barrel is internally provided with the filter material layer.
Optionally, the filtration and reconstitution system comprises: the device comprises a second bottle rack, a third mechanical arm, at least one purifying sample bottle, a needle filter and a heating device, wherein the purifying sample bottle is inserted on the second bottle rack and rotates to a liquid level to be moved along with the second bottle rack;
the liquid level to be moved of the second bottle rack is in the liquid moving range of the third mechanical arm and the second mechanical arm;
the needle filter is inserted into the liquid inlet of the purifying sample bottle, and the purifying liquid is moved into the needle filter by the purifying column;
the heating device heats the purified sample bottle.
Optionally, the filtration and reconstitution system comprises: the second bottle rack is arranged on the third disc body;
the concentrated gas needle blows gas to the purified sample bottle;
the liquid level sensor monitors the liquid level in the purge sample bottle.
Optionally, the filtration and reconstitution system comprises: the second liquid inlet needle is arranged on the liquid transferring end of the third mechanical arm;
the second needle washing container, the compound solution bottle and the third mechanical arm are arranged on the fourth tray body;
the second needle washing container and the compound solution bottle are in the pipetting range of the third mechanical arm.
According to yet another aspect of the present application, there is provided a pretreatment method comprising the steps of:
carrying out in-situ vibration and in-situ filtration on the sample by using a hydrophobic porous filter membrane to obtain an extracting solution;
purifying the extracting solution to obtain a purified solution;
and carrying out in-situ filtration, concentration and in-situ redissolution on the purified liquid to obtain detection liquid.
The application has the beneficial effects that:
1) According to the full-automatic vibration extraction purification device provided by the application, the hydrophobic porous filter membrane is adopted to replace a centrifugal machine to realize solid-liquid separation in the vibration extraction step, and the injector type dispersion solid-phase extraction purification device is adopted to realize solid-liquid separation in the purification step. The device can realize the required pretreatment steps of the full-automatic sample to be detected, the solution is transferred between the devices through the mechanical arm, the sample can be added once, the pretreatment steps of vibration extraction, dispersion solid phase extraction purification, automatic pipetting and the like can be sequentially completed, the high-flux full-automatic pretreatment of the food and the drug residues can be realized, and the practicability is higher.
2) The full-automatic oscillation extraction and purification device provided by the application is particularly suitable for pretreatment of samples to be detected according to the national standard GB 23200.113-2018, and has the advantages of high extraction and purification speed and high automation degree.
Drawings
FIG. 1 is a schematic diagram of a full-automatic oscillation extraction and purification device according to an embodiment of the present application;
FIG. 2 is a schematic view of an extraction bottle according to one embodiment of the present application;
FIG. 3 is a schematic view showing the structure of a purifying column according to an embodiment of the present application;
list of parts and reference numerals:
Detailed Description
The present application is described in detail below with reference to examples, but the present application is not limited to these examples.
Referring to fig. 1, the full-automatic oscillation extracting and purifying device provided by the application comprises: the bottle rack with the automatic rotary addressing function, the mechanical arm, the vibration extraction system, the purification system and the filtration liquid recovery system;
the vibration extraction system is used for carrying out in-situ vibration extraction on the sample to obtain an extracting solution;
the bottle rack and the mechanical arm carry out liquid conveying among the vibration extraction system, the purification system and the filtration liquid recovery system.
The bottle rack and the mechanical arm with the automatic rotary addressing function can be the conventional common device. The mechanical arm can realize the actions of rotation, expansion, bending movement, extrusion, push-pull and the like. The automatic rotation addressing bottle rack can complete rotation and stop at the liquid level to be injected. The vibration extraction system, the purification system and the filtration liquid recovery system are common systems which can be used for realizing the functions.
The device provided by the application realizes liquid transportation among the processing systems of each step by adopting the matching of the mechanical arm and the bottle rack, and realizes the whole-course automation of the multi-step liquid processing process. The production efficiency is improved.
Vibration extraction system
Specifically, the oscillation extraction system includes: the device comprises an oscillator 2, a first bottle rack 3, an extraction bottle 4 and a first mechanical arm 8; the extraction bottle 4 is arranged on the first bottle rack 3 and stops on the liquid level to be injected after rotating along with the first bottle rack 3; the liquid level to be injected is within the liquid transferring range of the first mechanical arm 8; the oscillator 2 is arranged on the first bottle rack 3, and oscillates the extracting bottle 4.
Optionally, the first mechanical arm 8 pipettes the extraction bottle 4 above the level to be filled.
The taking range of the first mechanical arm 8 means that the picking and placing of the extraction bottle 4 can be realized through the first mechanical arm 8 according to control.
Specifically, the shake extraction system comprises a first tray body 1, a solvent bottle 5 and a first needle washing container 6, wherein the first bottle rack 3, the solvent bottle 5 and the first needle washing container 6 are arranged on the first tray body 1; the solvent bottle 5 and the first needle washing container 6 are mounted within the pipetting range of the first mechanical arm 8.
Specifically, shake extraction system includes first feed liquor needle 7, and first feed liquor needle 7 sets up on the liquid-taking end of first arm 8, accomplishes the pipettor through first feed liquor needle 7.
Camera fig. 2, in particular, the extraction bottle 4 comprises: the inner cannula 42, the hydrophobic porous filter membrane 43 and the bottle body 44, wherein one end of the inner cannula 42 is sleeved with the hydrophobic porous filter membrane 43 and extends into the bottle body 44, and the other end of the inner cannula is inserted into the bottle cap 41 and exposes an open end on the surface of the bottle cap 41.
In use, the sample to be treated and the extraction filler are first placed in the cavity between the hydrophobic porous filter membrane 43 and the vial 44. The extraction liquid is injected into the open end by the first mechanical arm 8. The extracting solution is fully contacted with the sample and the extracting filler through the hydrophobic porous filter membrane 43, and the hydrophobic porous filter membrane is subjected to in-situ filtration after shaking to obtain the extracting solution.
Purification system
Specifically, the purification system includes: a purifying column 11 and a second mechanical arm 12; the purifying column 11 and the filtering liquid recovery system are in the grabbing range of the second mechanical arm 12. After the second mechanical arm 12 grabs the purifying column 11 and pulls the purifying column 11 to suck the extracting solution, the second mechanical arm 12 pushes the piston 113 in the purifying column 11 to move the purified extracting solution into the purifying sample bottle 15.
Optionally, the purification system comprises: a second tray 9 and a purifying column 11 placing tray, wherein the purifying column 11 is placed on the purifying column 11 placing tray; the second mechanical arm 12 and the purifying column 11 placing plate are placed on the second plate body 9.
Referring to fig. 3, the purification column 11 includes: a piston 113, a column tube 112, and a filter material layer; the piston 113 is accommodated in the column tube 112 and slides along the inner wall of the column tube 112; the first end of the cylinder 112 is open, and the second end is provided with a liquid outlet 116; a layer of filter material is disposed within the second end of the barrel 112.
Optionally, the periphery of the layer of filter material is fixedly connected to the inner wall of the shaft tube 112.
Optionally, the filter material layer includes at least a pair of porous screen plates 114 and a purification packing 115, the porous screen plates 114 are arranged at intervals, and the purification packing 115 is filled between the porous screen plates 114 arranged in pairs.
And (3) filtering a liquid recovery system:
specifically, the filtration and reconstitution system comprises: the second bottle rack 14, the third mechanical arm 22, at least one purified sample bottle 15, a needle filter 18 and a heating device, wherein the purified sample bottle 15 is inserted on the second bottle rack 14 and rotates along with the second bottle to a liquid level to be moved. The liquid level to be moved is within the liquid-moving range of the third mechanical arm 22 and the second mechanical arm 12; a needle filter 18 is inserted into the liquid inlet of the purified sample bottle 15. The heating means heats the purge sample bottle 15.
Optionally, the filtration reconstitution system comprises: a concentrated air needle 17, a liquid level sensor 16 and a third disk 13, wherein a second bottle rack 14 is arranged on the third disk 13; after the concentrated air needle 17 extends into the purified sample bottle 15, air is blown into the purified sample bottle 15; the level sensor 16 monitors the level of liquid in the purge sample bottle 15.
Optionally, the filtration reconstitution system comprises: the fourth tray 19, the second needle washing container 20, the double solution bottle 21 and the second liquid inlet needle 23, wherein the second liquid inlet needle 23 is arranged on the liquid transferring end of the third mechanical arm 22; the second needle washing container 20, the reconstitution flask 21 and the third robot arm 22 are arranged on the fourth disc 19. The second needle washing container 20 and the double solution bottle 21 are in the pipetting range of the third mechanical arm 22.
Optionally, the method comprises: the internal suction pump 24 and the light-proof box 25, the oscillation extraction system, the purification system and the filtration liquid recovery system are accommodated in the light-proof box 25, and the internal suction pump 24 is communicated with a liquid transfer device on the mechanical arm.
Further, the solvent bottle 5 contains acetonitrile or other solvents required for pretreatment.
Further, the composition of the extracted filler is: magnesium sulfate, sodium chloride, sodium citrate, a mixture of disodium hydrogen citrate, or a similar combination mixture.
Further, the composition of the purification packing 115 in the purification column 11 is: magnesium sulfate, PSA and GCB mixtures or similar combination mixtures.
Further, the first robot arm 8 and the third robot arm 22 may be rotated or moved up and down according to the automatic addressing result.
Further, the second mechanical arm 12 has automatic addressing functions of automatic rotation, up-and-down movement, and push-pull of the piston 113.
In another aspect of the present application, a pretreatment method is provided, including the steps of:
carrying out in-situ vibration mixing and in-situ filtration on the sample by a hydrophobic porous filter membrane to obtain an extracting solution;
purifying the extracting solution to obtain a purified solution;
and carrying out in-situ filtration, concentration and in-situ redissolution on the purified liquid to obtain detection liquid.
Examples
Referring to fig. 1, the full-automatic oscillation extraction and purification device comprises a first tray 1, an oscillator 2, a first bottle rack 3, an extraction bottle 4, a solvent bottle 5, a first needle washing container 6, a first liquid inlet needle 7, a first mechanical arm 8, a second tray 9, a purification column 11 placing tray, a purification column 11, a second mechanical arm 12, a third tray 13, a second bottle rack 14, a purification sample bottle 15, a liquid level sensor 16, a concentrated gas needle 17, a needle filter 18, a fourth tray 19, a second needle washing container 20, a double solution bottle 21, a third mechanical arm 22, a second liquid inlet needle 23, an internal suction pump 24 and a light shielding box 25.
The first tray body 1 is provided with a first bottle rack 3 with a rotary addressing function, an oscillator 2 is arranged at the bottom of the first bottle rack 3, a plurality of extraction bottles 4 are inserted into the first bottle rack 3, and extraction fillers are arranged in the extraction bottles 4.
Referring to fig. 2, the extraction bottle 4 includes: a cap 41, an inner cannula 42, a hydrophobic porous filter membrane 43 and a vial 44. One end of the inner cannula 42 is inserted on the bottle cap 41, the other end is sleeved with a hydrophobic porous filter membrane 43, and one end of the inner cannula 42 provided with the filter membrane extends into the bottle body 44. The first mechanical arm 8 is arranged near the extraction bottle 4, and liquid can be injected into the extraction bottle 4 on the liquid level to be injected through the telescopic first mechanical arm 8. The extraction bottle 4 can be inserted on the first bottle holder 3 and is stopped by the rotation of the first bottle holder 3 at the liquid level to be injected. The oscillator 2 is mounted on the first bottle holder 3 and oscillates the first bottle holder 3.
The second disk body 9 sets up in one side of first disk body 1, is equipped with purifying column and places dish 10 and purifying column 11 on, places several purifying column 11 on the purifying column placing dish 10, and the second arm 12 of being convenient for takes purifying column 11. The second mechanical arm 12 is disposed on one side of the purifying column placing tray 10, and the purifying column placing tray 10 is located within the grabbing range of the second mechanical arm 12. The purifying column 11 is vertically placed on the purifying column placing tray 10.
Referring to fig. 3, the purification column 11 includes: an upper cover 111, a column tube 112, a piston 113, and porous screen plates 114 provided in pairs at both ends of the purification packing 115; a drain 116 is provided at one end of the barrel 112. The other end of the barrel 112 is open, and a piston 113 extends into the barrel 112 and is connected to the upper cover 111.
The third disk body 13 sets up in one side of second disk body 9, sets up the second bottle holder 14 that has rotatory addressing function on the third disk body 13, is equipped with a plurality of purification sample bottle 15 on the second bottle holder 14, and the third arm 22 of being convenient for pours into the liquid into purification sample bottle 15. A liquid level sensor 16 is placed on one side of each of the purge sample bottles 15 to monitor the liquid level in the purge sample bottles 15 in real time.
The fourth tray 19 is arranged on one side of the third tray 13, and is provided with a second needle washing container 20, a double solution bottle 21, a third mechanical arm 22 and a second liquid inlet needle 23; when the second bottle holder 14 is rotated to the liquid level to be filled, the purge sample bottle 15 is within the pickup range of the third robot arm 22. The double solution bottle 21 and the second liquid inlet needle 23 are also in the picking range of the third mechanical arm 22.
The first tray 1, the oscillator 2, the first bottle holder 3, the extraction bottle 4, the solvent bottle 5, the first needle washing container 6, the first liquid inlet needle 7, the first mechanical arm 8, the second tray 9, the purification column 11 holding tray, the purification column 11, the second mechanical arm 12, the third tray 13, the second bottle holder 14, the purification sample bottle 15, the liquid level sensor 16, the concentrated gas needle 17, the needle filter 18, the fourth tray 19, the second needle washing container 20, the double solution bottle 21, the third mechanical arm 22, the second liquid inlet needle 23 and the internal suction pump 24 are all placed in the light-shielding box 25.
In this embodiment, the working process of the device is as follows:
1. the sample to be tested and the extraction filler are manually placed in a cavity between an inner insertion tube 42 and a bottle body 44 of an extraction bottle 4, the inner insertion tube 42 with a bottle cap 41 is covered, a hydrophobic porous filter membrane 43 is arranged at the bottom of the inner insertion tube 42, the extraction bottle 4 needing sample injection is conveyed to a sample injection position by rotating a first bottle rack 3, a first liquid inlet needle 7 connected with a first mechanical arm 8 moves downwards to be inserted into a solvent bottle 5, and a certain amount of extraction liquid in the solvent bottle 5 is moved into the extraction bottle 4 by a systemic pump 24 connected with the first liquid inlet needle 7.
After the extracting solution submerges the sample, the oscillator is started to oscillate the extracting bottle 4, and the sample is oscillated and uniformly mixed in situ. Before and after use, the first liquid inlet needle 7 needs to be cleaned by the first needle cleaning container 6 so as to avoid cross contamination.
Standing after shaking, allowing the extracted solution after extracting the sample to enter the inner cannula 42 through the hydrophobic porous filter membrane 43, and retaining the solid sample between the bottle body and the outer wall of the inner cannula 42 to realize solid-liquid separation to obtain the extracted solution to be purified;
2. the second mechanical arm 12 removes the purifying column 11 from the purifying column placing tray 10, the second mechanical arm 12 moves the purifying column 11 and inserts into the inner insertion tube 42 of the extracting bottle 4, and the second mechanical arm 12 pulls the piston 113 of the purifying column 11 to suck a certain volume of extracting solution to be purified;
3. the second bottle rack 14 rotates to convey the purified sample bottle 15 needing sample injection to a position to be injected, the second mechanical arm 12 moves the purifying column 11 to the position above the purified sample bottle 15 to be injected and moves downwards, the liquid outlet 116 of the purifying column 11 is fixedly inserted with the needle filter 18 above the purified sample bottle 15 to be injected, the second mechanical arm 12 pushes the piston 113 of the purifying column 11 to inject the extracting solution to be purified into the purified sample bottle 15 through the liquid outlet 116 and the needle filter 18, the purified sample bottle 15 is provided with the liquid level sensor 16, the volume of the extracting solution entering the purified sample bottle 15 is monitored in real time and ensured to be a set volume, and after the set volume is reached, the second mechanical arm 12 stops pushing the piston 113 of the purifying column 11;
4. the second mechanical arm 12 moves the purifying column 11 and the needle filter 18 into the purifying column placing tray 10;
5. a concentrated gas needle 17 is arranged on one side of the purified sample bottle 15, in addition, a second bottle rack 14 at the bottom of the purified sample bottle 15 has a controllable heating function and is provided with a liquid level sensor 16, and the real-time monitoring and ensuring that the extracting solution in the purified sample bottle 15 is dried to a set volume or thoroughly dried;
6. the second bottle rack 14 rotates to convey the purified sample bottle 15 needing sample injection to a position to be re-dissolved, a second liquid inlet needle 23 connected with a third mechanical arm 22 moves downwards to be inserted into the re-solution bottle 21, and a certain amount of re-solution in the re-solution bottle 21 is moved into the purified sample bottle 15 by a systemic pump 24 connected with the second liquid inlet needle 23 to be re-dissolved, and then the machine can be started. The second liquid inlet needle 23 is cleaned in the second needle washing container 20 before and after use to avoid cross contamination.
While the application has been described in terms of preferred embodiments, it will be understood by those skilled in the art that various changes and modifications can be made without departing from the scope of the application, and it is intended that the application is not limited to the specific embodiments disclosed.
Claims (7)
1. Full-automatic concussion draws purifier, its characterized in that includes: the device comprises a first bottle rack with an automatic rotary addressing function, an oscillation extraction system, a purification system and a filtration liquid recovery system;
the oscillation extraction system comprises: the device comprises an oscillator, an extraction bottle and a first mechanical arm; the extraction bottle is arranged on the first bottle rack, rotates along with the first bottle rack and then stops on the liquid level to be injected;
the liquid level to be injected is in the liquid transferring range of the first mechanical arm;
the oscillator is arranged on the first bottle rack;
the sample is subjected to in-situ vibration and in-situ filtration by a hydrophobic porous filter membrane in the extraction bottle to obtain an extracting solution;
the oscillation extraction system comprises: the first liquid inlet needle, the first tray body, the solvent bottle and the first needle washing container are arranged on the first tray body;
the solvent bottle and the first needle washing container are arranged in the pipetting range of the first mechanical arm;
the first liquid inlet needle is arranged on the liquid taking end of the first mechanical arm;
the first mechanical arm moves the first liquid inlet needle into the first needle washing container to wash the needle, and then takes the solvent from the solvent bottle and moves the solvent into the extraction bottle;
the purification system includes: a purifying column and a second mechanical arm;
the purifying column and the filtering liquid recovery system are arranged in the grabbing range of the second mechanical arm; the second mechanical arm grabs the purifying column and pulls a piston in the purifying column to suck the extracting solution;
the second mechanical arm pushes a piston in the purifying column to purify the extracting solution to obtain purified solution;
the filtration and liquid recovery system comprises: the device comprises a second bottle rack, a third mechanical arm, at least one purifying sample bottle, a needle filter and a heating device, wherein the purifying sample bottle is inserted on the second bottle rack and rotates to a liquid level to be moved along with the second bottle rack;
the liquid level to be moved of the second bottle rack is in the liquid moving range of the third mechanical arm and the second mechanical arm;
the needle filter is inserted into the liquid inlet of the purifying sample bottle, and the purifying liquid is moved into the needle filter by the purifying column;
the heating device heats the purified sample bottle;
the filtration and liquid recovery system further comprises: the second bottle rack is arranged on the third disc body;
the concentrated gas needle blows gas to the purified sample bottle;
the liquid level sensor monitors the liquid level in the purified sample bottle;
the filtration and liquid recovery system comprises: the second liquid inlet needle is arranged on the liquid transferring end of the third mechanical arm;
the second needle washing container, the compound solution bottle and the third mechanical arm are arranged on the fourth tray body;
the second needle washing container and the compound solution bottle are in the pipetting range of the third mechanical arm.
2. The full-automatic oscillation extraction and purification device of claim 1, wherein the solvent is acetonitrile.
3. The full-automatic oscillation extraction and purification device of claim 1, wherein the extraction bottle comprises: the bottle cap comprises a bottle cap body, an inner insertion tube, a hydrophobic porous filter membrane and a bottle body, wherein one end of the inner insertion tube is sleeved with the hydrophobic porous filter membrane and extends into the bottle body, and the other end of the inner insertion tube is an open end inserted into the bottle cap body and exposes out of the open end on the surface of the bottle cap body.
4. A fully automatic shock extraction purification apparatus according to claim 3, the sample and extraction filler being contained in a cavity between the inner cannula and the vial.
5. The full-automatic oscillation extraction and purification device according to claim 4, wherein the extraction filler is: magnesium sulfate, sodium chloride, sodium citrate, disodium hydrogen citrate.
6. The full-automatic oscillation extraction purification apparatus of claim 1, wherein the purification column comprises: a piston, a cylinder tube, and a layer of filter material; the piston is accommodated in the column tube and slides along the inner wall of the column tube; the first end of the cylinder tube is open, and the second end of the cylinder tube is provided with a liquid outlet; the second end of the barrel is internally provided with the filter material layer.
7. A pretreatment method for the apparatus according to any one of claims 1 to 6, comprising the steps of:
carrying out in-situ vibration and in-situ filtration on the sample by using a hydrophobic porous filter membrane to obtain an extracting solution;
purifying the extracting solution to obtain a purified solution;
and carrying out in-situ filtration, concentration and in-situ redissolution on the purified liquid to obtain detection liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910284888.9A CN111803997B (en) | 2019-04-10 | 2019-04-10 | Full-automatic oscillation extraction and purification device and pretreatment method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910284888.9A CN111803997B (en) | 2019-04-10 | 2019-04-10 | Full-automatic oscillation extraction and purification device and pretreatment method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111803997A CN111803997A (en) | 2020-10-23 |
| CN111803997B true CN111803997B (en) | 2023-11-17 |
Family
ID=72844235
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910284888.9A Active CN111803997B (en) | 2019-04-10 | 2019-04-10 | Full-automatic oscillation extraction and purification device and pretreatment method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111803997B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112198324B (en) * | 2020-12-07 | 2021-06-15 | 北京慧荣和科技有限公司 | Full-automatic QuECHERS experimental device and experimental method |
| CN113375995A (en) * | 2021-06-29 | 2021-09-10 | 上海汇像信息技术有限公司 | Full-automatic filtration system |
| CN114252311A (en) * | 2021-10-27 | 2022-03-29 | 上海市农产品质量安全中心 | Method for carrying out in-situ rapid detection pretreatment on pesticide residues in vegetables and fruits |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201053935Y (en) * | 2007-07-11 | 2008-04-30 | 重庆麦迪克科技开发有限公司 | Automatic centrifuging sample feeding device |
| JP2013003003A (en) * | 2011-06-17 | 2013-01-07 | Nissin Foods Holdings Co Ltd | Residual pesticide automatic preprocessing system and residual pesticide extraction method employing the same |
| CN105233527A (en) * | 2015-11-06 | 2016-01-13 | 青岛顺昕电子科技有限公司 | Full-automatic oscillation extraction instrument |
| WO2016026286A1 (en) * | 2014-08-19 | 2016-02-25 | 行政院农业委员会农业药物毒物试验所 | Quick extraction kit for agricultural product pesticide residue detection procedure and method for obtaining stock solution of detection solution from agricultural product sample |
| CN205483729U (en) * | 2016-02-24 | 2016-08-17 | 中国水产科学研究院长江水产研究所 | Drug residue extraction element in fish tissue |
| CN106770786A (en) * | 2017-01-11 | 2017-05-31 | 重庆市农业科学院 | A kind of garden stuff pesticide residue detects fast purification device |
| CN206671024U (en) * | 2017-04-10 | 2017-11-24 | 贵州出入境检验检疫局检验检疫综合技术中心 | A kind of automatically QuECHERS purifications, concentration and derivatization device |
| CN210205955U (en) * | 2019-04-10 | 2020-03-31 | 中国水产科学研究院 | Full-automatic oscillation extraction and purification device |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2007282135C1 (en) * | 2006-01-18 | 2012-05-24 | Coimmune, Inc. | Systems and methods for processing samples in a closed container, and related devices |
-
2019
- 2019-04-10 CN CN201910284888.9A patent/CN111803997B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201053935Y (en) * | 2007-07-11 | 2008-04-30 | 重庆麦迪克科技开发有限公司 | Automatic centrifuging sample feeding device |
| JP2013003003A (en) * | 2011-06-17 | 2013-01-07 | Nissin Foods Holdings Co Ltd | Residual pesticide automatic preprocessing system and residual pesticide extraction method employing the same |
| WO2016026286A1 (en) * | 2014-08-19 | 2016-02-25 | 行政院农业委员会农业药物毒物试验所 | Quick extraction kit for agricultural product pesticide residue detection procedure and method for obtaining stock solution of detection solution from agricultural product sample |
| CN105233527A (en) * | 2015-11-06 | 2016-01-13 | 青岛顺昕电子科技有限公司 | Full-automatic oscillation extraction instrument |
| CN205483729U (en) * | 2016-02-24 | 2016-08-17 | 中国水产科学研究院长江水产研究所 | Drug residue extraction element in fish tissue |
| CN106770786A (en) * | 2017-01-11 | 2017-05-31 | 重庆市农业科学院 | A kind of garden stuff pesticide residue detects fast purification device |
| CN206671024U (en) * | 2017-04-10 | 2017-11-24 | 贵州出入境检验检疫局检验检疫综合技术中心 | A kind of automatically QuECHERS purifications, concentration and derivatization device |
| CN210205955U (en) * | 2019-04-10 | 2020-03-31 | 中国水产科学研究院 | Full-automatic oscillation extraction and purification device |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111803997A (en) | 2020-10-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111803997B (en) | Full-automatic oscillation extraction and purification device and pretreatment method | |
| CN112198324B (en) | Full-automatic QuECHERS experimental device and experimental method | |
| JP7038439B2 (en) | Nucleic acid extraction system | |
| CN105517711B (en) | Centrifuge and method for acting on reaction vessel unit by centrifugal force | |
| CN1114831C (en) | Method and apparatus for liquid treatment utlizing dispenser | |
| US7351378B2 (en) | Nucleic acid extraction device | |
| US5305650A (en) | Automatic preparation apparatus | |
| JP5292267B2 (en) | SAMPLE PROCESSING DEVICE, SAMPLE PROCESSING METHOD, AND REACTION CONTAINER USED FOR THEM | |
| JPH11215978A (en) | Nucleic acid extracting equipment | |
| WO2020027566A1 (en) | Nucleic acid extraction device and operating method therefor | |
| JPH10260118A (en) | Automatic extraction device and automatic concentration-measuring apparatus for component substance in liquid sample | |
| JP2002506384A (en) | Device for selectively filtering sample liquid or droplets of sample liquid under reduced pressure and drying in vacuum, and use of the device | |
| CN210205955U (en) | Full-automatic oscillation extraction and purification device | |
| WO2008059685A1 (en) | Analyzer | |
| JP6198632B2 (en) | Sample preparation equipment for analysis | |
| CN111638276A (en) | Full-automatic magnetic separation extraction-solid phase extraction combined all-in-one machine | |
| JP2001108688A (en) | Device for automatically extracting component substance in liquid sample, device for automatically measuring concentration and method for extracting component substance in liquid sample | |
| CN210198828U (en) | Full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation | |
| CN109470882A (en) | A kind of extraction system | |
| CN111638114A (en) | Full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation and pretreatment method thereof | |
| JP4707086B2 (en) | Water separation apparatus and method for water separation in water-dispersed organic solvent | |
| JPH063233A (en) | Agricultural chemicals residue automatic preliminary treatment device | |
| JP5599488B2 (en) | Sample processing method | |
| JPH11281535A (en) | Apparatus for cleaning cell | |
| JP7333569B2 (en) | Automatic pretreatment device for test samples |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |