CN111638114A - Full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation and pretreatment method thereof - Google Patents
Full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation and pretreatment method thereof Download PDFInfo
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- CN111638114A CN111638114A CN201910155621.XA CN201910155621A CN111638114A CN 111638114 A CN111638114 A CN 111638114A CN 201910155621 A CN201910155621 A CN 201910155621A CN 111638114 A CN111638114 A CN 111638114A
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- 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
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- 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
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
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- 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
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
- G01N2001/4027—Concentrating samples by thermal techniques; Phase changes evaporation leaving a concentrated sample
Abstract
The application discloses full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation and pretreatment method thereof, this all-in-one machine includes: the automatic addressing liquid-transfering device, medicine residue extraction system, purification system and concentration system; the drug residue extraction system is used for carrying out in-situ crushing, in-situ solid-liquid mixing and magnetic solid-liquid separation on a sample to be detected to obtain an extracting solution; the purification system is used for purifying the extracting solution to obtain a purified solution; the concentration system is used for carrying out in-situ filtration, concentration and redissolution on the purified liquid to obtain a detection liquid; the automatic addressing liquid-transfering device is used for moving the extracting solution and the purifying solution. The all-in-one machine is simple in structure, reasonable in design and convenient to use.
Description
Technical Field
The application relates to a full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation and a pretreatment method thereof, belonging to the field of QuEChERS pretreatment.
Background
"people take food as the day and take food as the first, food safety is a big thing about the national times of life, and is highly concerned by all the circles of society. At the present stage, although the food safety condition of China is gradually good, food safety events still occur at all times, such as the problem that pesticide residues in exposed food exceed standards in recent years seriously.
At present, the problems of multiple types and complex matrix of food required by people in China in daily life exist, and great challenge is brought to the safety detection of food quality. In order to realize the rapid and accurate determination of drug residues in a large quantity of different types of food, a reasonable and rapid pretreatment technology is a key.
QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) is a rapid sample pretreatment technology for food detection recently developed internationally, and developed by the American Ministry of agriculture, professor Anastassiads, which is equal to 2003.
The principle of the technology consists of three steps:
firstly, extracting food traditional Chinese medicine residues by acetonitrile under the assistance of substances such as NaCl and the like;
secondly, adsorbing impurities in the food extracting solution to be detected by using an adsorbent filler to achieve the aim of purifying the extracting solution;
and finally concentrating, redissolving and detecting on a machine.
According to the standard GB 23200.113-2018 published on 21.06.8.7.21.4.4 gas chromatography-mass spectrometry combined method for determining the residual quantity of 208 pesticides and metabolites thereof in plant-derived foods, the pretreatment process at least comprises the following steps:
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.
However, a fully-automatic pretreatment all-in-one machine based on the QuEChERS sample pretreatment technology is still rarely reported at present. The fundamental reason is that the first step and the second step of the QuEChERS sample pretreatment technology both need to use a centrifuge to realize solid-liquid separation of the extracting solution and the sample matrix. The centrifuge is difficult to be matched with an addressable automatic instrument because the solid-liquid separation can be realized only by high-speed rotation.
Plum sensitivity and the like of agricultural product processing research institute of Chinese agricultural academy of sciences invent a full-automatic QuEChERS pretreatment all-in-one machine and a pretreatment method thereof (patent number: 201410073673.X), and firstly provides a full-automatic pretreatment all-in-one machine of a QuEChERS sample pretreatment technology. The natural sedimentation is used for replacing a centrifugal machine to realize solid-liquid separation of the extracting solution and the sample matrix, the solid-liquid separation effect is poor, the effect of purifying the filler to adsorb impurities in the extracting solution is poor, and the accuracy of a detection result is seriously influenced.
Disclosure of Invention
According to an aspect of the application, a full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation is provided, and the all-in-one machine is simple in structure, reasonable in design and convenient to use.
Full-automatic QuEChERS pretreatment all-in-one based on magnetic separation, its characterized in that includes: the automatic addressing liquid-transfering device, medicine residue extraction system, purification system and concentration system;
the drug residue extraction system is used for carrying out in-situ crushing, in-situ solid-liquid mixing and magnetic solid-liquid separation on a sample to be detected to obtain an extracting solution;
the purification system is used for purifying the extracting solution to obtain a purified solution;
the concentration system is used for carrying out in-situ filtration, concentration and in-situ redissolution on the purified liquid to obtain a detection liquid;
the automatic addressing liquid-transfering device is used for moving the extracting solution and the purifying solution.
The automatic addressing liquid-transfering device can transfer liquid among the medicine residue extraction system, the purification system and the concentration system in sequence in a one-way mode.
Optionally, the drug residue extraction system comprises: the device comprises an electromagnetic module, an extraction sample bottle and magnetic filler, wherein the magnetic filler is contained in the extraction sample bottle;
the sample to be detected is contained in the extraction sample bottle;
the electromagnetic module is used for generating magnetic force when being conducted and acting on the magnetic filler.
Optionally, the drug residue extraction system comprises: the homogenizer is used for carrying out the in-situ crushing and the in-situ solid-liquid mixing on the sample to be detected in the extracted sample bottle;
the homogenizer is an automatic addressing homogenizer.
Optionally, the drug residue extraction system comprises: a first tray body; the electromagnetic module, the sample extraction bottle and the homogenizer are all arranged on the first disk body.
Optionally, the full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation includes: a conduit system, the conduit system comprising: the extraction liquid bottle is connected with the extraction sample bottle through a pipeline; the solvent distributor is arranged at the bottle mouth of the extraction liquid bottle and is used for metering the effluent liquid.
Optionally, the full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation includes: a cleaning system, the cleaning system comprising: a washing container for washing a pipetting needle of the auto-addressing pipetting device and/or a cutter head of the homogenizer.
Optionally, the full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation includes: a conduit system, the conduit system comprising: the bottom of the cleaning container is connected with the waste liquid bottle; the top of the cleaning container is connected with the cleaning solution bottle;
the solvent distributor is arranged at the bottle mouth of the cleaning liquid bottle and is used for metering the discharged liquid.
Optionally, the purification system comprises: a purifying sample bottle and a purifying column, wherein the purifying sample bottle is used for containing the extracting solution; and the liquid absorbing end of the purifying column is immersed under the liquid level of the purifying sample bottle and is used for purifying the extracting solution to obtain the purifying solution.
Optionally, the purification system comprises: and the purification sample bottles are placed on the second tray body.
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; and a filter material layer is arranged in the second end of the cylindrical pipe.
Optionally, the purification column comprises: the piston is arranged at one end of the push rod and the needle head, and the needle head is sleeved on the liquid outlet.
Optionally, the periphery of the filter material layer is fixedly connected with the inner wall of the trunk tube.
Optionally, the filtering material layer comprises at least one pair of porous sieve plates and purifying filler, the porous sieve plates are arranged at intervals, and the purifying filler is filled between the porous sieve plates arranged in pairs.
Optionally, the scavenging filler comprises or consists of magnesium sulfate, PSA and GCB.
Optionally, the magnetic filler comprises: a magnetic substance;
preferably, the magnetic substance is ferroferric oxide magnetic particles;
more preferably, the magnetic filler is: the mixture consists of ferroferric oxide magnetic particles, magnesium sulfate, sodium chloride, sodium citrate and disodium hydrogen citrate.
Optionally, the concentration system comprises: the device comprises a heating device, a concentrated sample bottle and a liquid level sensor; the liquid level sensor is used for detecting the liquid level in the concentrated sample bottle and is in control connection with the heating device;
the concentrated sample bottle includes: a filter membrane and a concentrated gas needle;
dividing the inner cavity of the concentrated sample bottle into a sample introduction side and a concentrated side along the longitudinal direction of the concentrated sample bottle, wherein the bottom surface of the concentrated side is provided with the filter membrane and is spaced from the bottom surface of the concentrated sample bottle;
filtering the purified liquid in the concentration side and then carrying out in-situ liquid recovery in the sample introduction side; the concentrated gas needle is arranged on the sample injection side and the concentrated side respectively and used for blow-drying liquid.
Optionally, the concentration system comprises: and the heating device, the concentrated sample bottle and the liquid level sensor are arranged on the third tray body.
Optionally, the full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation includes: a conduit system, the conduit system comprising: a reconstituted solution bottle and a solvent dispenser; the re-solution bottle is connected with the sample injection side pipeline;
the solvent distributor is arranged at the bottle mouth of the redissolution bottle and is used for metering the discharged liquid.
Optionally, the automatically addressed pipetting device comprises: the liquid transferring device comprises an internal suction pump and a liquid transferring needle, wherein one end of the liquid transferring needle extends into liquid to be transferred, and the other end of the liquid transferring needle is connected with the internal suction pump.
Optionally, the full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation includes: the light shielding box, the automatic addressing liquid-transferring device, the medicine residue extracting system, the purifying system and the concentrating system are accommodated and arranged in the light shielding box.
According to another aspect of the application, a pretreatment method of the full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation is provided, and comprises the following steps:
carrying out in-situ crushing, in-situ solid-liquid mixing and magnetic solid-liquid separation on a sample to be detected 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.
In the present application, the term "magnetic substance" refers to a magnetic substance that can be used in a process of extracting a target substance from a substrate to be detected, and that can denature protein in the substrate to be detected into a mass when acetonitrile is used as a solvent, and the magnetic substance wraps the mass of the protein-denatured substance to form a solid portion of a magnetic sample to be detected, and can achieve solid-liquid separation under the action of an external magnetic field, for example, a magnetic substance disclosed in CN 106442818A and having a capability of separating substances such as a minced fillet sample to be detected.
The beneficial effects that this application can produce include:
1) the application provides a full-automatic QuEChERS pretreatment all-in-one based on magnetic separation, based on acetonitrile can make in the sample matrix protein denaturation cluster, through stirring the mixture parcel ferroferric oxide magnetic particle in the cluster material, can realize the principle of solid-liquid separation under the external magnet effect, adopt this magnetic separation means to replace centrifuge to realize the solid-liquid separation of QuEChERS pretreatment, adopt syringe formula dispersion solid phase extraction purification post to realize the mixture of extract and purification filler, adsorb and the edulcoration. The all-in-one machine can fully automatically complete the pretreatment steps of homogeneous extraction, magnetic separation, dispersed solid phase extraction purification, concentration, redissolution and the like of a sample to be detected, can realize high flux and full-automatic sample pretreatment of drug residues in food, and has stronger practicability.
2) The full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation, that this application provided, pretreatment edulcoration is effectual, and the testing result rate of accuracy is high.
Drawings
Fig. 1 is a schematic structural diagram of a fully-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation according to an embodiment of the present application;
FIG. 2 is a schematic cross-sectional front view of a purification column according to an embodiment of the present application;
FIG. 3 is a schematic cross-sectional front view of a concentrated sample bottle according to an embodiment of the present disclosure;
list of parts and reference numerals:
| name of component | Reference numerals | Name of component | Reference numerals |
| Magnetic filler | 1 | Composite |
13 |
| |
2 | |
14 |
| |
3 | |
15 |
| Liquid-transfering needle washing container | 4 | Waste |
16 |
| Homogenizer |
5 | |
17 |
| |
6 | |
18 |
| Cleaning fluid delivery conduit | 7 | |
19 |
| Liquid transferring needle | 8 | |
20 |
| Extracting solution conveying conduit | 9 | |
21 |
| |
10 | |
22 |
| Extracting |
11 | |
23 |
| |
12 | Light- |
24 |
| |
181 | |
211 |
| Porous sieve plate | 182 | |
212 |
| Purifying filler | 183 | |
213 |
| |
184 | |
214 |
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 QuEChERS pretreatment all-in-one machine based on magnetic separation provided by the application comprises: the automatic addressing liquid-transfering device, medicine residue extraction system, purification system and concentration system; in a drug residue extraction system, a sample to be detected is subjected to in-situ crushing, solid-liquid mixing and magnetic solid-liquid separation to obtain an extracting solution; the extracting solution is moved into a purifying system through an automatic addressing liquid-transferring device to purify the extracting solution to obtain a purified solution; and (4) moving the purified liquid to a concentration system through an automatic addressing liquid-transferring device to concentrate and redissolve the purified liquid to obtain a detection liquid. And (4) performing on-machine detection on the detection liquid to obtain a detection result.
The medicine residue extraction system comprises a magnetic separation module, the magnetic separation module comprises a magnetic filler 1 and an electromagnetic module, the magnetic filler 1 is in contact with a sample to be detected and an extracting solution, acetonitrile can extract a target object in the sample to be detected, simultaneously, protein in the sample to be detected is denatured into a group, and a magnetic substance is wrapped in the group to form a magnetic solid part to be detected, the electromagnetic module is started to form a magnetic field and adsorb the magnetic solid part to be detected, so that the solid part to be detected is positioned at the bottom of a container, and solid-liquid separation is realized.
By adopting the device, the whole detection pretreatment process can be completed without manual operation, and the pretreatment efficiency is high.
Optionally, a washing system is included for automatically washing the auto-addressed pipetting device.
Medicine residue extraction system:
the drug residue extraction system comprises: the device comprises a first disc body 3 with controllable magnetism, an extraction sample bottle 2 containing acetonitrile, a homogenizer and magnetic packing 1.
Placing an extraction sample bottle 2 on the first tray body 3, accommodating a sample to be detected in the extraction sample bottle 2, and completing sample in-situ crushing, magnetic solid-liquid separation and extracting solution extraction in the extraction sample bottle 2. The in-situ crushing is carried out by a homogenizer which has an automatic addressing function and can carry out homogenizing treatment on each extracted sample bottle 2 on the first disc body 3 one by one. Thereby realizing the sample crushing and solid-liquid mixing and stirring treatment in the sample extraction bottle 2.
After stirring one sample, the homogenizer automatically moves to a cleaning container for knife washing treatment. And then moving to a second sample for homogenization treatment.
The sample extracting solution is a liquid phase obtained by homogenizing a sample, dissolving the sample in acetonitrile and carrying out solid-liquid separation. During solid-liquid separation, in order to avoid using a centrifugal machine and further reduce the volume of the device, magnetic separation is adopted to realize solid-liquid separation. The magnetic separation comprises adding an extracting solution (usually acetonitrile) and a magnetic filler 1 to a sample to be detected, homogenizing, crushing the sample to be detected during the homogenization process, and fully mixing the sample to be detected with the magnetic filler 1. And homogenizing to obtain a solid part of the magnetic sample to be detected. The electromagnet module arranged on the first disc body 3 is started, so that the first disc body 3 generates attraction force to the solid part of the sample to be detected, and solid-liquid separation is realized after the first disc body is still.
After solid-liquid separation, a liquid phase can be obtained as an extracting solution, the obtained extracting solution contains the information substance to be detected, and the liquid phase is transferred to the purified sample bottle 17 by a common liquid transferring device such as a pipette or a liquid transferring gun which can be automatically addressed.
Optionally, the magnetic filler comprises at least a magnetic substance;
preferably, the magnetic substance is ferroferric oxide magnetic particles;
more preferably, the magnetic filler is: the mixture consists of ferroferric oxide magnetic particles, magnesium sulfate, sodium chloride, sodium citrate and disodium hydrogen citrate.
A purification system:
the purification system comprises: a clean sample bottle 17, a second tray 19 and a clean column 18.
The purifying sample bottle 17 is placed on the second tray body 19, the purifying column 18 is arranged on the upper part of the purifying sample bottle 17, and the needle 184 of the purifying column 18 extends into the extracting solution.
Referring to fig. 2, the purification column 18 comprises a push rod, a piston 181, a column tube, and a layer of filter material. One end of the push rod is provided with a piston 181, and the piston 181 is accommodated in the column tube and slides along the inner wall of the column tube. The first end of the cylindrical tube is open, and the second end is provided with a liquid outlet. The liquid outlet may be covered with a needle 184. And a filter material layer is arranged in the second end of the cylindrical pipe.
In use, the piston 181 in the purifying column 18 is pulled to suck the extracting solution into the filter material layer to mix with the purifying filler 183, and the piston 181 in the purifying column 18 is pushed to push the extracting solution out of the filter material layer and flow back to the purifying sample bottle 17. The pressure of the liquid to be purified is automatically adjusted by adopting the piston 181, so that the liquid can be rapidly, simply and conveniently purified. The device cost is reduced, a solid phase extraction device is not used, and the purification efficiency is improved.
Optionally, the periphery of the filter material layer is fixedly connected with the inner wall of the column casing pipe.
Optionally, the filtering material layer includes at least one pair of porous sieve plates 182 and purifying fillers 183, the porous sieve plates 182 are arranged at intervals, and the purifying fillers 183 are filled between the porous sieve plates 182 arranged in pairs.
Optionally, an upper cover is mounted on the other end of the push rod.
Alternatively, the purge column 18 can be automatically raised and lowered by means of a robot arm, and the piston pushing and pulling can be automatically performed. Alternatively, scavenging filler 183 may be a variety of commonly used materials, such as octadecyl bonded silica gel particles (C18), ethylenediamine-N-Propylsilane (PSA), and the like. Preferably the PSA particle size is 40-63 μm, the pore diameter is
Preferably, scavenging filler 183 is sulfuric acidMagnesium, PSA, and Graphitized Carbon (GCB) mixtures or similar combination mixtures.
A concentration system:
the concentration system includes: a third plate 20 with heating function, a concentrated sample bottle 21 and a liquid level sensor 22.
Referring to fig. 3, the concentrated sample bottle 21 includes: a permeable filter membrane 212, a concentrated gas needle 211. The concentrated sample bottle 21 has an inner cavity divided into a sample introduction side 213 and a concentrated side 214 along the longitudinal direction thereof, and a bottom region of the sample introduction side 213 extends to below the concentrated side 214. A permeable filter 212 is inserted across the concentrated sample vial 21 on the bottom of the concentrated side 214. The open ends of the sample inlet side 213 and the concentrate side 214 are provided with concentrate gas needles 211.
A concentrated sample bottle 21 is placed on the third tray 20. The purified liquid is moved into the concentration side 214 of the concentrated sample bottle 21 by the pipetting device with the automatic addressing function, and the purified liquid is filtered under the action of gravity. The concentrated gas needle 211 blows gas into the liquid in the sample inlet 213 and the concentrated side 214 simultaneously and heats the concentrated sample bottle 21 to accelerate the evaporation process until the liquid is dried or the volume is set. After drying, a redissolution is introduced into the sample introduction side 213 through the redissolution conveying conduit 13, and the dry sample is subjected to in-situ redissolution.
The heating device is in control connection with the liquid level sensor 22, so that the heating temperature can be automatically controlled according to the change condition of the liquid level, and full-automatic evaporation is realized.
The automatic addressing liquid-transfering device includes internal suction pump 23 and liquid-transfering needle, one end of the liquid-transfering needle is extended into the liquid to be transferred, and its another end is connected with internal suction pump 23, and on the side wall of the liquid-transfering needle a scale is set, so that it is convenient to control liquid-transfering quantity. After the internal suction pump 23 is switched on and one end of the pipetting needle sucks liquid to the required scale, the pipetting needle can be controlled by a mechanical arm and other parts to move into a liquid bottle to be placed.
A cleaning system:
optionally, the washing system is further included, and the washing system is used for washing devices needing washing, such as the automatic addressing pipetting device and the homogenizer, and the washing system comprises: a pipette needle washing container 4 and a homogenizer knife washing container 5, wherein the pipette needle washing container 4 is used for washing a pipette device; the homogenizer knife washing container 5 is used for washing a homogenizer knife head.
Optionally, a light shielding box 24 is further included, and an automatic addressing pipetting device, a drug residue extraction system, a purification system and a concentration system are accommodated in the light shielding box 24. Through setting up the light-shading box 24, avoid the interference and the influence of light to sample pretreatment, be favorable to improving and detect the precision.
A pipeline system:
optionally, a piping system is further included, the piping system comprising: an extraction liquid bottle 11, a cleaning liquid bottle 12, a waste liquid bottle 15 and a re-solution bottle 14. The extraction liquid bottle 11 is connected with the extraction sample bottle 2 through a pipeline. The re-solution bottle 14 is connected with the sample inlet side 213 of the concentrated sample bottle 21 through a pipeline.
The bottoms of the liquid-transferring needle washing container 4 and the homogenizer knife washing container 5 are respectively connected with a waste liquid bottle 15; the top parts of the liquid-transferring needle washing container 4 and the homogenizer knife washing container 5 are respectively connected with a cleaning liquid container. And introducing cleaning liquid into the pipette needle washing container 4 and the homogenizer knife washing container 5 or removing the cleaning liquid according to the requirement.
The number of extraction sample bottles 2, purification sample bottles 17, and concentration sample bottles 21 may be determined as necessary.
In the embodiment, the pipette tips are cleaned in the pipette tip washing container 4 after use, the pipette tip washing container 4 is disposed on the first tray 3, the pipette tip washing container 4 is connected to the cleaning solution bottle 12 by the cleaning solution delivery conduit 7, and the liquid outlet of the homogenizer knife washing container 5 is connected to the waste solution bottle 15 by the waste solution drainage conduit 16.
The homogenizer is to utilize homogenizer to wash sword container 5 and wash after the homogeneity, this homogenizer washes sword container 5 and sets up on first disk body 3, and utilize washing liquid conveying pipe 7 and washing liquid bottle 12 through connection on homogenizer washes sword container 5, through connection has the measurement distributor between washing liquid bottle 12 and the washing liquid conveying pipe 7, the liquid outlet of homogenizer washes sword container 5 utilizes waste liquid flowing back pipe 16 to be connected with waste liquid bottle 15, waste liquid bottle 15 sets up in the outside of light-shielding box 24.
Another aspect of the present application further provides a pretreatment method of the above full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation, which includes the following steps:
carrying out in-situ crushing, in-situ solid-liquid mixing and magnetic solid-liquid separation on a sample to be detected to obtain an extracting solution;
purifying the extracting solution to obtain a purified solution;
and carrying out in-situ filtration, concentration and redissolution on the purified solution to obtain a detection solution.
The method can effectively improve the pretreatment efficiency, realize the integrated use of the automatic addressing device, realize the one-time detection of mass samples and improve the comparability of detection results.
Examples
Referring to fig. 1, the technical solution adopted by the present embodiment is: the device comprises a magnetic filler 1, an extraction sample bottle 2, a first tray body 3, a liquid-transferring needle washing container 4, a homogenizer knife washing container 5, a homogenizer 6, a cleaning liquid conveying conduit 7, a liquid-transferring needle 8, an extracting liquid conveying conduit 9, a solvent distributor 10, an extracting liquid bottle 11, a cleaning liquid bottle 12, a re-dissolving liquid conveying conduit 13, a re-dissolving liquid bottle 14, a waste liquid bottle 15, a waste liquid discharging conduit 16, a purification sample bottle 17, a purification column 18, a second tray body 19, a sample bottle placing tray 20, a sample bottle 21, a liquid level sensor 22, an internal suction pump 23 and a light-proof box 24;
a plurality of sample extracting bottles 2 are arranged on the first disc body 3, and magnetic fillers 1 are arranged in the sample extracting bottles 2;
the second tray body 19 is arranged on one side of the first tray body 3, a plurality of purified sample bottles 17 are arranged on the upper portion of the second tray body 19, the third tray body 20 is arranged on one side of the second tray body 19, a plurality of concentrated sample bottles 21 are arranged on the third tray body 20, the internal suction pump 23 is connected with the pipette needle 8, and the purified sample bottles 20 are connected with the purification column 18;
the purifying column 18 consists of a piston 181, a porous sieve plate 182, a purifying filler 183 and a needle 184, has the function of moving up and down, and the piston 181 can be pulled or pushed up and down;
the homogenizer 6 and the liquid transferring needle 8 are both arranged at one side of the first tray body 3, and the liquid level sensor 22 is arranged at one side of the sample bottle 21;
the inner cavity of the concentrated sample bottle 21 is divided into a sample feeding side 213 and a concentrated side 214 along the longitudinal direction, the bottom of the concentrated side 214 is spaced from the bottom surface of the concentrated sample bottle 21, and the bottom surface of the concentrated side 214 is provided with a permeable filter membrane 212. The inner side walls of the concentration side 214 and the sample introduction side 213 are both provided with concentration gas needles 211, and the concentrated solution can enter the sample introduction side 213 after being filtered by a permeable filter membrane 212. After filtration, the heating device is turned on to heat and evaporate all the liquid in the concentrated sample bottle 21, and the concentrated gas needle 211 is turned on to purge the liquid to accelerate evaporation. After evaporation is completed, the reconstituted solution is transported to the sample introduction side 213 by the reconstituted solution transport conduit 13, and the concentrated substances are reconstituted.
The magnetic filler 1, the extraction sample bottle 2, the first tray body 3, the liquid-transferring needle washing container 4, the homogenizer knife washing container 5, the homogenizer 6, the liquid-transferring needle 8, the purification sample bottle 17, the purification column 18, the second tray body 19, the third tray body 20, the concentrated sample bottle 21, the liquid level sensor 22 and the internal suction pump 23 are all arranged in a light shielding box 24;
the extracting solution bottle 11 is arranged outside the light shielding box 24, a solvent distributor 10 is connected to the port of the extracting solution bottle 11, and the solvent distributor 10 is connected with a plurality of extracting sample bottles 2 by using an extracting solution conveying conduit 9.
The working principle of the specific embodiment is as follows:
1. placing food to be detected and magnetic filler 1 into an extraction sample bottle 2, pumping a certain amount of extracting solution in an extracting solution bottle 11 into the extraction sample bottle 2 through an extracting solution conveying conduit 9 by a solvent distributor 10, homogenizing the food in the extraction sample bottle 2 by a homogenizer 6, cleaning the homogenizer 6 by a homogenizer cutter cleaning container 5 before and after homogenization, pumping a certain amount of cleaning solution in a cleaning solution bottle 12 into the homogenizer cutter cleaning container 5 through a cleaning solution conveying conduit 7 by the solvent distributor 10 to clean a cutter head, so as to avoid cross contamination, the waste liquid of the knife washing is discharged into a waste liquid bottle 15 through a waste liquid discharge conduit 16, the bottom of the first disk body 3 at the bottom of the sample extracting bottle 2 is provided with an electromagnet module, the electromagnet at the bottom of the first disc body 3 is electrified to generate magnetic adsorption to the solid part of the sample to be detected, so that the extraction solution and the solid in the sample extraction bottle 2 can be quickly separated;
2. the method comprises the following steps that a certain volume of extracting solution in an extracting sample bottle 2 is transferred into a purifying sample bottle 17 by using a liquid transferring needle 8, the liquid transferring needle 8 needs to be cleaned in a liquid transferring needle washing needle container 4 before and after use, a certain amount of cleaning solution in a cleaning solution bottle 12 is pumped into the liquid transferring needle washing needle container 4 through a cleaning solution conveying conduit 7 by a solvent distributor 10 to clean the liquid transferring needle so as to avoid cross contamination, needle washing waste liquid is discharged into a waste liquid bottle 15 through a waste liquid discharging conduit 16, a purifying column 18 is arranged at the upper part of the purifying sample bottle 17, the purifying column 18 can automatically move downwards, a piston in the purifying column 18 is pulled to suck the extracting solution to be mixed with a purifying filler, and the piston in the purifying column 18 is pushed to push the extracting solution back to the purifying sample;
3. a volume of the draw solution in the purified sample vial 17 is transferred to the concentrate side 214 of the concentrated sample vial 21 by means of the pipette needle 8, followed by the concentrated gas. The pipette tip 8 is cleaned in the pipette tip container 4 before and after use, a certain amount of cleaning solution in the cleaning solution bottle 12 is pumped into the pipette tip container 4 by the solvent distributor through the cleaning solution delivery conduit 7 to clean the pipette tip, so as to avoid cross contamination, and the waste solution from the pipette tip is discharged into the waste solution bottle 15 through the waste solution discharge conduit 16. In addition, the third tray 20 at the bottom of the concentrated sample bottle 21 has a controllable heating function and is provided with a liquid level sensor 22, so that the real-time monitoring is realized and the extract in the concentrated sample bottle 21 is ensured to be dried to a set volume or completely dried;
4. a certain amount of the redissolution in the redissolution bottle 14 of the metering distributor is pumped into the sample injection side 213 through the redissolution conveying conduit 13, and the detection liquid obtained by filtering the concentrated side 214 is redissolved and then can be tested on the machine.
After adopting above-mentioned structure, this embodiment beneficial effect does: the full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation can denature proteins in a matrix into clusters based on acetonitrile and wrap ferroferric oxide magnetic particles to form a magnetic sample solid part to be detected, and can realize the principle of solid-liquid separation under the action of an external magnet.
Although the present application has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application.
Claims (10)
1. The utility model provides a full-automatic QuEChERS pretreatment all-in-one based on magnetic separation which characterized in that includes: the automatic addressing liquid-transfering device, medicine residue extraction system, purification system and concentration system;
the drug residue extraction system is used for carrying out in-situ crushing, in-situ solid-liquid mixing and magnetic solid-liquid separation on a sample to be detected to obtain an extracting solution;
the purification system is used for purifying the extracting solution to obtain a purified solution;
the concentration system is used for carrying out in-situ filtration, concentration and in-situ redissolution on the purified liquid to obtain a detection liquid;
the automatic addressing liquid-transfering device is used for moving the extracting solution and the purifying solution.
2. The full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation as claimed in claim 1, wherein the drug residue extraction system comprises: the device comprises an electromagnetic module, an extraction sample bottle and magnetic filler, wherein the magnetic filler is contained in the extraction sample bottle;
the sample to be detected is contained in the extraction sample bottle;
the electromagnetic module is used for generating magnetic force when being conducted and acting on the magnetic filler;
preferably, the full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation comprises: a cleaning system, the cleaning system comprising: a cleaning vessel for cleaning a pipetting needle and/or homogenizer head of the auto-addressing pipetting device;
preferably, the purification system comprises: a purifying sample bottle and a purifying column, wherein the purifying sample bottle is used for containing the extracting solution; the liquid absorbing end of the purifying column is immersed under the liquid level of the purifying sample bottle and is used for purifying the extracting solution to obtain the purifying solution;
preferably, the concentration system comprises: the device comprises a heating device, a concentrated sample bottle and a liquid level sensor; the liquid level sensor is used for detecting the liquid level in the concentrated sample bottle and is in control connection with the heating device;
the concentrated sample bottle includes: a filter membrane and a concentrated gas needle;
dividing the inner cavity of the concentrated sample bottle into a sample introduction side and a concentrated side along the longitudinal direction of the concentrated sample bottle, wherein the bottom surface of the concentrated side is provided with the filter membrane and is spaced from the bottom surface of the concentrated sample bottle;
filtering the purified solution in the concentration side and then carrying out in-situ solution recovery in the sample injection side;
the concentrated gas needle is arranged on the sample introduction side and the concentrated side respectively and used for drying liquid;
preferably, the magnetic filler comprises: a magnetic substance;
preferably, the magnetic substance is ferroferric oxide magnetic particles;
more preferably, the magnetic filler is: a mixture consisting of ferroferric oxide magnetic particles, magnesium sulfate, sodium chloride, sodium citrate and disodium hydrogen citrate;
preferably, the automatically addressed pipetting device comprises: the liquid transferring device comprises an internal suction pump and a liquid transferring needle, wherein one end of the liquid transferring needle extends into liquid to be transferred, and the other end of the liquid transferring needle is connected with the internal suction pump;
preferably, the full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation comprises: the light shielding box, the automatic addressing liquid-transferring device, the medicine residue extracting system, the purifying system and the concentrating system are accommodated and arranged in the light shielding box.
3. The full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation as claimed in claim 2, wherein the drug residue extraction system comprises: the homogenizer is used for carrying out the in-situ crushing and the in-situ solid-liquid mixing on the sample to be detected in the extracted sample bottle;
the homogenizer is an automatic addressing homogenizer.
4. The full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation as claimed in claim 3, wherein the drug residue extraction system comprises: a first tray body; the electromagnetic module, the sample extraction bottle and the homogenizer are all arranged on the first disk body.
5. The fully-automatic QuEChERS pre-processing all-in-one machine based on magnetic separation as claimed in claim 2, wherein the fully-automatic QuEChERS pre-processing all-in-one machine based on magnetic separation comprises: a conduit system, the conduit system comprising: the extraction liquid bottle is connected with the extraction sample bottle through a pipeline; the solvent distributor is arranged at the bottle mouth of the extraction liquid bottle and is used for metering the effluent liquid.
6. The fully-automatic QuEChERS pre-processing all-in-one machine based on magnetic separation as claimed in claim 2, wherein the fully-automatic QuEChERS pre-processing all-in-one machine based on magnetic separation comprises: a conduit system, the conduit system comprising: the bottom of the cleaning container is connected with the waste liquid bottle; the top of the cleaning container is connected with the cleaning solution bottle;
the solvent distributor is arranged at the bottle mouth of the cleaning liquid bottle and is used for metering the discharged liquid.
7. The fully automated QuEChERS pre-processing all-in-one machine based on magnetic separation of claim 2, wherein the purification system comprises: the purification sample bottles are placed on the second tray body;
preferably, 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; and a filter material layer is arranged in the second end of the cylindrical pipe.
8. The fully automated QuEChERS pre-processing all-in-one machine based on magnetic separation of claim 7, wherein the purification column comprises: the piston is arranged at one end of the push rod and the needle head, and the needle head is sleeved on the liquid outlet;
preferably, the periphery of the filter material layer is fixedly connected with the inner wall of the cylindrical barrel;
preferably, the filtering material layer comprises at least one pair of porous sieve plates and purifying filler, the porous sieve plates are arranged at intervals, and the purifying filler is filled between the porous sieve plates arranged in pairs;
preferably, the scavenging filler comprises magnesium sulfate, PSA and GCB.
9. The fully automated QuEChERS pre-processing all-in-one machine based on magnetic separation of claim 2, wherein the concentration system comprises: the heating device, the concentrated sample bottle and the liquid level sensor are arranged on the third tray body;
preferably, the full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation comprises: a conduit system, the conduit system comprising: a reconstituted solution bottle and a solvent dispenser; the re-solution bottle is connected with the sample injection side pipeline;
the solvent distributor is arranged at the bottle mouth of the redissolution bottle and is used for metering the discharged liquid.
10. The pretreatment method of the full-automatic QuEChERS pretreatment all-in-one machine based on magnetic separation according to any one of claims 1-9, characterized by comprising the following steps:
carrying out in-situ crushing, in-situ solid-liquid mixing and magnetic solid-liquid separation on a sample to be detected 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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