CN111803997A - Full-automatic oscillation extraction and purification device and pretreatment method - Google Patents
Full-automatic oscillation extraction and purification device and pretreatment method Download PDFInfo
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- CN111803997A CN111803997A CN201910284888.9A CN201910284888A CN111803997A CN 111803997 A CN111803997 A CN 111803997A CN 201910284888 A CN201910284888 A CN 201910284888A CN 111803997 A CN111803997 A CN 111803997A
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- 238000000605 extraction Methods 0.000 title claims abstract description 76
- 238000000746 purification Methods 0.000 title claims abstract description 73
- 230000010355 oscillation Effects 0.000 title claims abstract description 39
- 238000002203 pretreatment Methods 0.000 title claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 104
- 239000000243 solution Substances 0.000 claims abstract description 47
- 238000001914 filtration Methods 0.000 claims abstract description 30
- 238000011065 in-situ storage Methods 0.000 claims abstract description 20
- 238000002347 injection Methods 0.000 claims abstract description 6
- 239000007924 injection Substances 0.000 claims abstract description 6
- 238000012546 transfer Methods 0.000 claims abstract description 6
- 239000000523 sample Substances 0.000 claims description 39
- 239000012521 purified sample Substances 0.000 claims description 28
- 239000002904 solvent Substances 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 23
- 239000012528 membrane Substances 0.000 claims description 21
- 230000002209 hydrophobic effect Effects 0.000 claims description 18
- 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
- 239000007789 gas Substances 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 238000000034 method Methods 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
- 238000011084 recovery Methods 0.000 claims description 7
- 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
- 238000012856 packing Methods 0.000 claims description 3
- 239000005871 repellent Substances 0.000 claims description 2
- 239000000945 filler Substances 0.000 description 9
- 239000006228 supernatant Substances 0.000 description 7
- 235000013305 food Nutrition 0.000 description 6
- 238000003780 insertion Methods 0.000 description 5
- 230000037431 insertion Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 3
- 238000010926 purge 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
- 238000010586 diagram Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000003640 drug residue Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000002627 tracheal intubation Methods 0.000 description 2
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 description 1
- 230000004075 alteration Effects 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
- 239000006185 dispersion Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 238000001172 liquid--solid extraction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002207 metabolite Substances 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
- 238000012545 processing Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method 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
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- 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
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- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Pathology (AREA)
- Immunology (AREA)
- General Physics & Mathematics (AREA)
- Biochemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Acoustics & Sound (AREA)
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Abstract
The application discloses full-automatic oscillation extraction and purification device and pretreatment method, include: the device comprises a first bottle rack with an automatic rotating and addressing function, a vibration extraction system, a purification system and a filtering and liquid-recovering system; the oscillation extraction system includes: the device comprises a vibrator, a first bottle rack, an extraction bottle and a first mechanical arm; the extraction bottle is arranged on the first bottle rack and stops at the liquid level to be filled after rotating along with the first bottle rack; the liquid injection position to be injected is in the liquid transfer range of the first mechanical arm; the oscillator is arranged on the first bottle rack; and oscillating and standing the sample in situ in an extraction bottle to obtain an extracting solution. The device is particularly suitable for pre-treating a sample to be detected according to the national standard GB23200.113-2018, and has high extraction and purification speed and high automation degree.
Description
Technical Field
The application relates to a full-automatic oscillation extraction and purification device and a pretreatment method, and belongs to the field of sample pretreatment.
Background
In the process of analyzing and detecting the drug residues in foods such as fruits, grains and the like, the foods are generally firstly crushed, then the liquid-solid extraction method is adopted to extract the food traditional Chinese medicine residues into the extracting solution under the action of continuous oscillation, and the extracting solution to be purified is obtained by centrifugation. Then further purifying the extract by using techniques such as dispersed solid phase extraction purification and the like.
The above drug residue analysis and detection process has been forced to be established as a national standard. For example, in the national standard GB23200.113-2018 food safety national standard plant-derived food, the gas chromatography-mass spectrometry combined method for measuring the residual quantity of 208 pesticides and metabolites thereof at least comprises the following pretreatment processes:
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 homogeneous proton, covering a centrifuge tube cover, violently shaking and centrifuging;
secondly, sucking a certain amount of supernatant liquid, adding the supernatant liquid into a plastic centrifuge tube containing magnesium sulfate and PSA, adding the magnesium sulfate, the PSA and the GCB into the plastic centrifuge tube for a sample with a darker color, and centrifuging after uniformly mixing in a vortex manner;
thirdly, accurately sucking a certain amount of supernatant into a test tube, blowing nitrogen into a water bath at 40 ℃ until the supernatant is nearly dry, redissolving the supernatant, passing the redissolved supernatant through a microporous filter membrane, and measuring the supernatant by a machine.
Disclosure of Invention
According to an aspect of the application, a full-automatic oscillation extraction and purification device is provided, the device can effectively improve sample treatment efficiency, shorten treatment time, and automatically and gradually complete each operation of pretreatment.
Full-automatic oscillation extraction and purification device is characterized by comprising: the device comprises a first bottle rack with an automatic rotating and addressing function, a vibration extraction system, a purification system and a filtering and liquid-recovering system;
the oscillation extraction system includes: the device comprises a vibrator, a first bottle rack, an extraction bottle and a first mechanical arm; the extraction bottle is arranged on the first bottle rack and stops at the liquid level to be filled after rotating along with the first bottle rack; the liquid injection position to be injected is within the liquid transfer range of the first mechanical arm; the oscillator is arranged on the first bottle rack;
and carrying out in-situ oscillation and in-situ filtration by using a hydrophobic porous filter membrane on the sample in the extraction bottle to obtain an extracting solution.
Optionally, the oscillation extracting system includes: the first bottle rack, 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 liquid transferring range of the first mechanical arm;
the first liquid inlet needle is arranged on the liquid taking end of the first mechanical arm;
after the first mechanical arm moves the first liquid inlet needle to the first needle washing container for needle washing, taking the solvent from the solvent bottle and then moving the solvent into the extraction bottle;
optionally, the solvent is acetonitrile.
Optionally, the extraction bottle comprises: the water-repellent bottle comprises a bottle cap, an inner inserting tube, a hydrophobic porous filter membrane and a bottle body, wherein one end of the inner inserting tube is sleeved with the hydrophobic porous filter membrane and extends into the bottle body, the other end of the inner inserting tube is an open end which is inserted into the bottle cap, and the open end is exposed on the surface of the bottle cap;
preferably, the sample and extraction pad are contained in a cavity between the inner cannula and the vial;
preferably, the extraction packing is: magnesium sulfate, sodium chloride, sodium citrate, and disodium hydrogen citrate.
Optionally, the purification system comprises: a purifying column and a second mechanical arm;
the purification column and the filtration 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 absorb the extracting solution;
and the second mechanical arm pushes the piston in the purification column to purify the extracting solution to obtain the purified solution.
Optionally, the purification column comprises: the piston, the cylindrical tube and the filter material layer; the piston is accommodated in the column tube and slides along the inner wall of the column tube; the first end of the cylindrical pipe is open, and the second end of the cylindrical pipe is provided with a liquid outlet; the second end of the cylindrical pipe is internally provided with the filter material layer.
Optionally, the filtration and rehydration system comprises: the device comprises a second bottle rack, a third mechanical arm, at least one purified sample bottle, a needle type filter and a heating device, wherein the purified sample bottle is inserted into the second bottle rack and rotates to a liquid position to be moved along with the second bottle rack;
the liquid level to be moved of the second bottle rack is positioned 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 purification sample bottle, and the purification liquid is moved into the needle filter by the purification column;
the heating device heats the purified sample bottle.
Optionally, the filtration and rehydration system comprises: the second bottle rack is arranged on the third tray 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.
Optionally, the filtration and rehydration system comprises: the second liquid inlet needle is mounted on the liquid transfer end of the third mechanical arm;
the second needle washing container, the re-solution bottle and the third mechanical arm are arranged on the fourth tray body;
the second needle washing container and the re-solution bottle are arranged in the pipetting range of the third mechanical arm.
According to yet another aspect of the present application, there is provided a pretreatment method including the steps of:
carrying out in-situ oscillation and in-situ filtration by a hydrophobic porous filter membrane on a sample 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 solution to obtain a detection solution.
The beneficial effects that this application can produce include:
1) the application provides a full-automatic oscillation extraction purifier adopts hydrophobicity porous filter membrane to filter and replaces centrifuge to realize oscillating the solid-liquid separation who draws the step, adopts syringe formula dispersion solid phase extraction purifier to realize the solid-liquid separation who purifies the step. Can realize the required pretreatment step of full-automatic sample that waits to detect through the device, solution realizes shifting through the arm between each device, can realize once adding the sample, can accomplish according to the preface to vibrate and draw, disperse pretreatment steps such as solid phase extraction purification, automatic move the liquid, can realize that medicine remains high flux, full-automatic sample pretreatment in the food, the practicality is stronger.
2) The full-automatic oscillation extraction and purification device provided by the application is particularly suitable for pre-treating a sample to be detected according to the national standard GB23200.113-2018, and is high in extraction and purification speed and high in automation degree.
Drawings
FIG. 1 is a schematic structural diagram of a fully-automatic oscillation extraction purification device according to an embodiment of the present application;
FIG. 2 is a schematic diagram of an extraction bottle according to an embodiment of the present disclosure;
FIG. 3 is a schematic view of a purification column according to one embodiment of the present application;
list of parts and reference numerals:
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
Referring to fig. 1, the full-automatic oscillation extraction and purification device that this application provided includes: the bottle rack with the automatic rotating and addressing functions, the mechanical arm, the vibration extraction system, the purification system and the filtration complex liquid system are arranged on the bottle rack;
the oscillation extraction system is used for carrying out in-situ oscillation extraction on the sample to obtain an extracting solution;
the bottle rack and the mechanical arm are used for conveying liquid among the vibration extraction system, the purification system and the filtration liquid recovery system.
The bottle rack and the mechanical arm with the automatic rotation addressing function can be conventional devices. The mechanical arm can realize the actions of rotation, extension, bending movement, extrusion, push-pull and the like. The automatic rotary addressing bottle rack can complete rotation and stop at the liquid level to be filled. The oscillation extraction system, the purification system and the filtration complex liquid system are common systems which can be used for realizing the functions.
The application provides the device cooperatees through adopting arm and bottleholder, realizes carrying out liquid transportation between each step processing system, realizes the liquid treatment process full automation of multistep. The production efficiency is improved.
Vibrate extraction system
Specifically, the oscillation extraction system includes: the device comprises a vibrator 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 at the liquid level to be filled after rotating along with the first bottle rack 3; the liquid injection position is in the liquid transfer range of the first mechanical arm 8; the oscillator 2 is arranged on the first bottle rack 3, and the extracting bottle 4 is oscillated.
Optionally, the first mechanical arm 8 pipettes into the extraction bottle 4 at the filling position.
The taking range of the first mechanical arm 8 means that the taking and placing of the extraction bottle 4 can be realized through the first mechanical arm 8 according to control.
Specifically, the oscillation extraction system comprises a first tray body 1, a solvent bottle 5 and a first needle washing container 6, wherein a 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 wash vessel 6 are mounted within the pipetting range of the first mechanical arm 8.
Specifically, shake extraction system and include first liquid inlet needle 7, first liquid inlet needle 7 sets up on the liquid end of getting of first robotic arm 8, accomplishes through first liquid inlet needle 7 and moves the liquid.
Camera fig. 2, in particular, the extraction bottle 4 comprises: an inner cannula 42, a hydrophobic porous filter membrane 43 and a 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, the other end is inserted into the bottle cap 41, and the surface of the bottle cap 41 is exposed to an open end.
When in use, the sample to be treated and the extraction filler are firstly placed in the cavity between the hydrophobic porous filter membrane 43 and the bottle body 44. The extraction liquid is injected into the open end by the first robot arm 8. The extracting solution is fully contacted with the sample and the extracting filler through the hydrophobic porous filter membrane 43, and after oscillation, the hydrophobic porous filter membrane is filtered in situ to obtain the extracting solution.
Purification system
Specifically, the purification system includes: a purge column 11 and a second robot arm 12; the purifying column 11 and the filtering liquid recovery system are arranged in the grabbing range of the second mechanical arm 12. After the second mechanical arm 12 grabs the purifying column 11, the second mechanical arm 12 pushes the piston 113 in the purifying column 11 after the purifying column 11 is pulled to suck the extracting solution, and the purified extracting solution is moved into the purifying sample bottle 15.
Optionally, the purification system comprises: the second tray body 9 and the purification column 11 placing tray, and the purification column 11 is placed on the purification column 11 placing tray; the second mechanical arm 12 and the purification column 11 placing tray are placed on the second tray body 9.
Referring to fig. 3, the purification column 11 includes: a piston 113, a shaft tube 112, a layer of filter material; the piston 113 is accommodated in the trunk pipe 112 and slides along the inner wall of the trunk pipe 112; the first end of the trunk tube 112 is open, and the second end is provided with a liquid outlet 116; a layer of filtration material is disposed within the second end of the barrel 112.
Optionally, the periphery of the layer of filter material is fixedly attached to the inner wall of the shaft tube 112.
Optionally, the filtering material layer includes at least one pair of porous sieve plates 114 and a purifying filler 115, the porous sieve plates 114 are arranged at intervals, and the purifying filler 115 is filled between the porous sieve plates 114 arranged in pairs.
And (3) a filtering complex liquid system:
specifically, filtration complex liquid system includes: a second bottle rack 14, a 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 position to be pipetted is within the pipetting range of the third mechanical arm 22 and the second mechanical arm 12; the needle filter 18 is inserted into the liquid inlet of the purified sample bottle 15. The heating device heats the purified sample bottle 15.
Optionally, the filtration and rehydration system comprises: the concentrated gas needle 17, the liquid level sensor 16 and the third tray body 13, and the second bottle rack 14 is arranged on the third tray body 13; after the concentrated gas needle 17 extends into the purified sample bottle 15, the purified sample bottle 15 is blown with gas; a level sensor 16 monitors the level of liquid in the decontaminated sample vial 15.
Optionally, the filtration and rehydration system comprises: the fourth tray body 19, the second needle washing container 20, the re-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 reconstituted solution bottle 21 and the third mechanical arm 22 are arranged on the fourth tray body 19. The second needle washing container 20 and the reconstituted solution bottle 21 are located within the pipetting range of the third mechanical arm 22.
Optionally, comprising: interior aspiration pump 24 and light-resistant case 25 vibrate extraction system, clean system and filtration complex liquid system and hold and set up in light-resistant case 25, interior aspiration pump 24 communicates with the liquid-transfering device on the arm.
Further, the solvent contained in the solvent bottle 5 is acetonitrile or other solvent required for pretreatment.
Further, the composition of the extraction filler is as follows: magnesium sulfate, sodium chloride, sodium citrate, disodium hydrogen citrate, or similar combination mixtures.
Further, the composition of the purification filler 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 rotate or move up and down according to the auto addressing result.
Further, the second robot arm 12 has an automatically addressable function of automatically rotating, moving up and down, and pushing and pulling the piston 113.
Another aspect of the present application further provides a pretreatment method, including the following steps:
carrying out in-situ oscillation mixing and in-situ filtration by a hydrophobic porous filter membrane on a sample 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 solution to obtain a detection solution.
Examples
Referring to fig. 1, the full-automatic oscillation extraction and purification device comprises a first tray body 1, an oscillator 2, a first bottle holder 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 body 9, a purification column 11 placing tray, a purification column 11, a second mechanical arm 12, a third tray body 13, a second bottle holder 14, a purification sample bottle 15, a liquid level sensor 16, a concentrated gas needle 17, a needle filter 18, a fourth tray body 19, a second needle washing container 20, a re-dissolving liquid bottle 21, a third mechanical arm 22, a second liquid inlet needle 23, an internal suction pump 24 and a light-proof box 25.
Be equipped with the first bottle frame 3 that has rotatory addressing function on the first disk body 1, first bottle frame 3 bottom is equipped with oscillator 2, inserts on the first bottle frame 3 and establishes the several and draw bottle 4, is equipped with in the bottle 4 of drawing and draws the filler.
Referring to fig. 2, the extraction bottle 4 includes: a bottle cap 41, an inner cannula 42, a hydrophobic porous filter membrane 43 and a bottle body 44. One end of the inner insertion tube 42 is inserted into the bottle cap 41, the other end is sleeved with a hydrophobic porous filter membrane 43, and the end of the inner insertion tube 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 injection position through stretching the first mechanical arm 8. The extraction bottle 4 can be inserted on the first bottle rack 3 and is rotated by the first bottle rack 3 to stop at the liquid level to be filled. The oscillator 2 is installed on the first bottle rack 3 and generates oscillation to the first bottle rack 3.
Second disk body 9 sets up in one side of first disk body 1, is equipped with the purification post and places dish 10 and purification post 11, and the purification post is placed and is laid several purification post 11 on the dish 10, and the second arm 12 of being convenient for takes purification post 11. The second mechanical arm 12 is arranged on one side of the purification column placing plate 10, and the purification column placing plate 10 is located in the grabbing range of the second mechanical arm 12. The purification column 11 is placed upright on the purification column placing tray 10.
Referring to fig. 3, the purification column 11 includes: an upper cover 111, a column body pipe 112, a piston 113, and a porous sieve plate 114 arranged at two ends of a purifying filler 115 in pairs; one end of the shaft tube 112 is provided with a drain port 116. The other end of the trunk tube 112 is open, and the piston 113 extends into the trunk tube 112 and is connected to the upper cover 111.
The third tray body 13 is arranged on one side of the second tray body 9, a second bottle rack 14 with a rotary addressing function is arranged on the third tray body 13, and a plurality of purification sample bottles 15 are arranged on the second bottle rack 14, so that the third mechanical arm 22 can conveniently inject liquid into the purification sample bottles 15. A liquid level sensor 16 is placed on one side of each purge sample bottle 15 to monitor the liquid level in the purge sample bottle 15 in real time.
The fourth tray body 19 is arranged on one side of the third tray body 13, and is provided with a second needle washing container 20, a re-solution bottle 21, a third mechanical arm 22 and a second liquid inlet needle 23; when the second bottle holder 14 rotates to the liquid injection position, the purified sample bottle 15 is located in the taking range of the third mechanical arm 22. The re-solution bottle 21 and the second liquid inlet needle 23 are also positioned in the pick-up range of the third mechanical arm 22.
The first tray body 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 body 9, the purification column 11 placing tray, the purification column 11, the second mechanical arm 12, the third tray body 13, the second bottle holder 14, the purification sample bottle 15, the liquid level sensor 16, the concentrated gas needle 17, the needle type filter 18, the fourth tray body 19, the second needle washing container 20, the re-dissolving liquid bottle 21, the third mechanical arm 22, the second liquid inlet needle 23 and the internal suction pump 24 are all arranged in the light avoiding box 25.
In this embodiment, the device works as follows:
1. the sample to be detected 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 first bottle frame 3 rotates to convey the extraction bottle 4 to be sample-fed to a position to be sample-fed, a first liquid inlet needle 7 connected with a first mechanical arm 8 moves downwards to be inserted into a solvent bottle 5, and an inner suction pump 24 connected with the first liquid inlet needle 7 moves a certain amount of the extraction liquid in the solvent bottle 5 into the extraction bottle 4.
After the extracting solution submerges the sample, the oscillator is started to oscillate the extracting bottle 4, and the sample is oscillated and mixed in situ. The first liquid inlet needle 7 needs to be cleaned by the first needle cleaning container 6 before and after use, so that cross contamination is avoided.
Standing after oscillation, allowing the extracting solution after sample extraction to enter the inner intubation 42 through the hydrophobic porous filter membrane 43, and allowing the solid sample to be retained between the bottle body and the outer wall of the inner intubation 42 to realize solid-liquid separation to obtain the extracting solution to be purified;
2. the second mechanical arm 12 takes the purifying column 11 out of the purifying column placing tray 10, the second mechanical arm 12 moves the purifying column 11 and inserts the purifying column 11 into the inner inserting tube 42 of the solvent 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 a purified sample bottle 15 needing sample introduction to a position to be subjected to sample introduction, the second mechanical arm 12 moves the purifying column 11 to the position above the purified sample bottle 15 to be subjected to sample introduction and moves downwards, the liquid discharge port 116 of the purifying column 11 is fixedly inserted into the needle filter 18 above the purified sample bottle 15 to be subjected to sample introduction, the second mechanical arm 12 pushes the piston 113 of the purifying column 11 to inject an extracting solution to be purified into the purified sample bottle 15 through the liquid discharge port 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 and ensured to be a set volume in real time, and after the set volume is reached, the second mechanical arm 12 stops pushing the piston 113 of;
4. the second robot arm 12 moves the purification cartridge 11 and the needle filter 18 into the purification cartridge placing tray 10;
5. a concentrated gas needle 17 is arranged on one side of the purified sample bottle 15, and 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 21, so that the real-time monitoring is realized, and the extract in the purified sample bottle 15 is ensured to be dried to a set volume or completely dried;
6. the second bottle rack 14 rotates to convey the purified sample bottle 15 to be fed to the position to be redissolved, the second liquid inlet needle 23 connected with the third mechanical arm 22 moves downwards to be inserted into the redissolution bottle 21, and the inner suction pump 24 connected with the second liquid inlet needle 23 moves a certain amount of redissolution in the redissolution bottle 21 into the purified sample bottle 15 for redissolution, so that the machine can be operated. Before and after use, the second liquid inlet needle 23 is cleaned in the second needle washing container 20 to avoid cross contamination.
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (10)
1. The utility model provides a full-automatic oscillation draws purifier which characterized in that includes: the device comprises a first bottle rack with an automatic rotating and addressing function, a vibration extraction system, a purification system and a filtering and liquid-recovering system;
the oscillation extraction system includes: the device comprises a vibrator, an extraction bottle and a first mechanical arm; the extraction bottle is arranged on the first bottle rack and stops at the liquid level to be filled after rotating along with the first bottle rack;
the liquid injection position to be injected is within the liquid transfer range of the first mechanical arm;
the oscillator is arranged on the first bottle rack;
and carrying out in-situ oscillation and in-situ filtration by using a hydrophobic porous filter membrane on the sample in the extraction bottle to obtain an extracting solution.
2. The fully automatic oscillation extraction purification device of claim 1, wherein the oscillation extraction system comprises: the first bottle rack, 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 liquid transferring range of the first mechanical arm;
the first liquid inlet needle is arranged on the liquid taking end of the first mechanical arm;
after the first mechanical arm moves the first liquid inlet needle to the first needle washing container for needle washing, taking the solvent from the solvent bottle and then moving the solvent into the extraction bottle;
3. the full-automatic oscillation extraction and purification device of claim 2, wherein the solvent is acetonitrile.
4. The full-automatic oscillation extraction and purification device of claim 1, wherein the extraction bottle comprises: the water-repellent bottle comprises a bottle cap, an inner inserting tube, a hydrophobic porous filter membrane and a bottle body, wherein one end of the inner inserting tube is sleeved with the hydrophobic porous filter membrane and extends into the bottle body, the other end of the inner inserting tube is an open end which is inserted into the bottle cap, and the open end is exposed on the surface of the bottle cap;
preferably, the sample and extraction packing are contained in a cavity between the inner cannula and the vial;
preferably, the extraction packing is: magnesium sulfate, sodium chloride, sodium citrate, and disodium hydrogen citrate.
5. The fully automatic oscillation extraction purification device of claim 1, wherein the purification system comprises: a purifying column and a second mechanical arm;
the purification column and the filtration 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 absorb the extracting solution;
and the second mechanical arm pushes the piston in the purification column to purify the extracting solution to obtain the purified solution.
6. The full-automatic oscillation extraction purification device of claim 5, wherein the purification column comprises: the piston, the cylindrical tube and the filter material layer; the piston is accommodated in the column tube and slides along the inner wall of the column tube; the first end of the cylindrical pipe is open, and the second end of the cylindrical pipe is provided with a liquid outlet; the second end of the cylindrical pipe is internally provided with the filter material layer.
7. The full-automatic oscillation extraction and purification device of claim 5, wherein the filtration and liquid recovery system comprises: the device comprises a second bottle rack, a third mechanical arm, at least one purified sample bottle, a needle type filter and a heating device, wherein the purified sample bottle is inserted into the second bottle rack and rotates to a liquid position to be moved along with the second bottle rack;
the liquid level to be moved of the second bottle rack is positioned 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 purification sample bottle, and the purification liquid is moved into the needle filter by the purification column;
the heating device heats the purified sample bottle.
8. The full-automatic oscillation extraction and purification device of claim 7, wherein the filtration and liquid recovery system comprises: the second bottle rack is arranged on the third tray 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.
9. The full-automatic oscillation extraction and purification device of claim 7, wherein the filtration and liquid recovery system comprises: the second liquid inlet needle is mounted on the liquid transfer end of the third mechanical arm;
the second needle washing container, the re-solution bottle and the third mechanical arm are arranged on the fourth tray body;
the second needle washing container and the re-solution bottle are arranged in the pipetting range of the third mechanical arm.
10. A method of pre-treatment for use in an apparatus as claimed in any one of claims 1 to 9, comprising the steps of:
carrying out in-situ oscillation and in-situ filtration by a hydrophobic porous filter membrane on a sample 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 solution to obtain a detection solution.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112198324A (en) * | 2020-12-07 | 2021-01-08 | 北京慧荣和科技有限公司 | Full-automatic QuECHERS experimental device and experimental method |
| CN112578062A (en) * | 2020-12-24 | 2021-03-30 | 中国农业科学院农业质量标准与检测技术研究所 | High flux dioxin sample pretreatment purifier |
| 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 (9)
| 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 |
| US20090298129A1 (en) * | 2006-01-18 | 2009-12-03 | Simon Jonathon Spence | Systems and methods for processing samples in a closed container, and related devices |
| 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 |
-
2019
- 2019-04-10 CN CN201910284888.9A patent/CN111803997B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090298129A1 (en) * | 2006-01-18 | 2009-12-03 | Simon Jonathon Spence | Systems and methods for processing samples in a closed container, and related devices |
| 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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112198324A (en) * | 2020-12-07 | 2021-01-08 | 北京慧荣和科技有限公司 | Full-automatic QuECHERS experimental device and experimental method |
| CN112578062A (en) * | 2020-12-24 | 2021-03-30 | 中国农业科学院农业质量标准与检测技术研究所 | High flux dioxin sample pretreatment purifier |
| 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 |
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|---|---|
| CN111803997B (en) | 2023-11-17 |
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