Full-automatic magnetic separation extraction-solid phase extraction combined all-in-one machine
阅读说明：本技术 全自动磁分离提取-固相萃取联用一体机 (Full-automatic magnetic separation extraction-solid phase extraction combined all-in-one machine ) 是由 李晋成 刘欢 韩刚 于 2019-03-01 设计创作，主要内容包括：本申请公开了一种全自动磁分离提取-固相萃取联用一体机及其方法,该一体机包括：自动寻址移液装置、药残提取系统、提取液浓缩系统、固相萃取系统和洗脱液浓缩系统；药残提取系统用于对待检测样品进行原位破碎、原位固液混合和磁性固液分离后,得到提取液；提取液浓缩系统用于对提取液进行浓缩、复溶,得到提取复溶液；固相萃取系统用于对提取复溶液进行固相萃取,得到洗脱液；洗脱液浓缩系统用于对洗脱液进行浓缩、复溶得到检测液；自动寻址移液装置用于移动提取液、净化液和洗脱液。该一体机结构简单,结构简单、使用方便,提高样品前处理效率。(The application discloses full-automatic magnetic separation draws-solid phase extraction all-in-one and method thereof, this all-in-one includes: the device comprises an automatic addressing liquid-transferring device, a drug residue extraction system, an extracting solution concentration system, a solid phase extraction system and an eluent 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 extracting solution concentrating system is used for concentrating and redissolving the extracting solution to obtain an extracting redissolution; the solid phase extraction system is used for carrying out solid phase extraction on the extracted complex solution to obtain eluent; the eluent concentration system is used for concentrating and redissolving the eluent to obtain a detection solution; the automatic addressing liquid-transfering device is used for moving extracting solution, purifying solution and eluent. The all-in-one machine is simple in structure, convenient to use and capable of improving the pretreatment efficiency of samples.)
1. The utility model provides a full-automatic magnetic separation draws-solid phase extraction and unites all-in-one which characterized in that includes: the device comprises an automatic addressing liquid-transferring device, a drug residue extraction system, an extracting solution concentration system, a solid phase extraction system and an eluent 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 extracting solution concentrating system is used for concentrating and in-situ redissolving the extracting solution to obtain an extracting redissolution;
the solid phase extraction system is used for carrying out solid phase extraction on the extraction redissolved solution to obtain an eluent;
the eluent concentration system is used for concentrating and in-situ redissolving the eluent to obtain a detection solution;
the automatic addressing liquid-transfering device is used for moving the extracting solution, the purifying solution and the eluent.
2. The integrated machine of claim 1, wherein the drug residue extraction system comprises: the device comprises an electromagnetic module, an extraction sample bottle and a magnetic extraction 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 fully-automatic magnetic separation extraction-solid phase extraction combined all-in-one machine comprises: a cleaning system, the cleaning system comprising: a cleaning container for cleaning a pipetting needle of the auto-addressing pipetting device and/or a tool bit of a homogenizer;
preferably, the magnetic filler contains at least 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 extract concentrating 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: concentrating the gas needle;
the concentrated gas needle is arranged in the concentrated sample bottle and used for drying liquid;
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 fully-automatic magnetic separation extraction-solid phase extraction combined all-in-one machine comprises: the automatic addressing liquid-transferring device, the drug residue extraction system, the extracting solution concentration system, the solid phase extraction system and the eluent concentration system are accommodated in the light-shielding box;
preferably, the solid phase extraction system comprises: the device comprises a solid phase extraction device and an eluent container, wherein the solid phase extraction device is used for automatically completing the activation, sample loading, leaching and elution of a solid phase extraction column; the eluent container is arranged at an eluent outlet of the solid phase extraction device and is used for containing the eluent;
preferably, the eluent concentration system comprises: the device comprises a heating device, a liquid level sensor and a sample loading bottle;
the liquid level sensor is used for detecting the liquid level in the sample feeding sample bottle and is in control connection with the heating device;
the sample loading bottle comprises: concentrating the gas needle;
the concentrated gas needle is arranged in the sample loading sample bottle and used for drying liquid.
3. The integrated machine of 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 integrated machine of claim 3, wherein the drug residue extraction system comprises: the electromagnetic module, the extracted sample bottle and the homogenizer are all placed on the first disk.
5. The integrated machine of claim 2, wherein the integrated machine 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 integrated machine of claim 2, wherein the integrated machine comprises: a conduit system, the conduit system comprising: the device comprises a cleaning liquid bottle, a waste liquid bottle and a solvent distributor, wherein the bottom of the cleaning liquid bottle is respectively connected with the waste liquid bottle; the top of the cleaning liquid bottle is respectively connected with a cleaning liquid container;
the solvent distributor is arranged at the bottle mouth of the cleaning liquid bottle and is used for metering the discharged liquid.
7. The integrated machine of claim 2, wherein the extract concentrating system comprises: the second tray, the heating device, the concentrated sample bottle and the liquid level sensor are arranged on the second tray.
8. The integrated machine of claim 2, wherein the integrated machine comprises: a conduit system, the conduit system comprising: a first reconstituted solution bottle and a solvent dispenser; the first compound solution bottle is connected with the concentrated sample bottle pipeline;
the solvent distributor is arranged at the bottle mouth of the first compound solution bottle and is used for metering the effluent liquid.
9. The integrated machine of claim 2, wherein the eluent concentration system comprises: the heating device, the sample loading bottle and the liquid level sensor are arranged on the fourth tray;
preferably, the fully-automatic magnetic separation extraction-solid phase extraction combined all-in-one machine comprises: a conduit system, the conduit system comprising: a second reconstituted solution bottle and a solvent dispenser; the second compound solution bottle is connected with the sample loading bottle pipeline;
the solvent distributor is arranged at the bottle mouth of the second compound solution bottle and is used for metering the effluent liquid.
10. The pretreatment method of the full-automatic magnetic separation extraction-solid phase extraction combined all-in-one machine as claimed in any one of claims 1 to 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;
concentrating and in-situ redissolving the extracting solution to obtain an extracted redissolution;
carrying out solid phase extraction on the extracted complex solution to obtain an eluent;
and concentrating and re-dissolving the eluent in situ to obtain a detection solution.
Technical Field
The application relates to a full-automatic magnetic separation extraction-solid phase extraction combined all-in-one machine and a method thereof, belonging to the field of automatic solid phase extraction purification 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 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, and a full-automatic sample pretreatment technology is a great challenge.
Solid phase extraction is a pretreatment technique combining liquid-solid extraction and liquid chromatography, and has been widely used for separation, purification, and concentration of food sample extract.
Food has the problems of multiple types, complex matrix and the like, and most detection standards require solid-phase extraction to purify a sample extracting solution before on-line detection. For example, the detection method of the residual amount of urotropine in imported and exported animal derived food according to the national standard SN/T2226-2008 standards for the inspection and quarantine industry of the entry and exit of the people's republic of China, namely liquid chromatography-mass spectrometry/mass spectrometry, comprises the following approximate pretreatment processes: weighing animal-derived food to be detected in a plastic centrifuge tube, adding acetonitrile and anhydrous sodium sulfate, covering a centrifuge tube cover, violently shaking and centrifuging; adding buffer solution after concentration, purifying by an oasis MCX solid phase extraction column, and collecting eluent; thirdly, the eluent is transferred into a centrifuge tube, nitrogen is blown to be nearly dry, in-situ redissolution is carried out, and the eluent is filtered through a microporous filter membrane and is tested on a machine.
The traditional food detection and extraction process comprises two steps of solvent extraction and centrifugal separation, and the whole process can be completed only by depending on a plurality of devices such as a homogenizer, a centrifuge and the like. In order to realize the automatic completion of the sample extraction-solid phase extraction purification process, a homogenizer, a centrifuge, a solid phase extraction device and other equipment are integrated into one device. However, since the centrifuge needs to rotate at a high speed to separate solid from liquid, it is difficult to match with a pipetting needle capable of addressing automatically. How to integrate the centrifuge and the solid phase extraction device into a fully automatic device is still a great challenge, and the fundamental difficulty is how to integrate the solid-liquid separation function realized by the centrifuge and the solid phase extraction device into a fully automatic device.
At present, the invention of a full-automatic sample pretreatment machine based on solid-phase extraction is only 'a full-automatic rapid solvent extraction-solid-phase extraction combined instrument and an extraction method thereof' invented by Chenjian steel and the like (patent number: 201210388539. X). The patent uses rapid solvent extraction to realize automatic rapid extraction of a sample matrix, and automatic solid-phase extraction to realize automatic rapid purification of the sample matrix; the patent avoids the solid-liquid separation by using a centrifugal machine, but the defects of extraction under the condition of high temperature and high pressure, large volume of required extraction solvent and the like exist in the rapid solvent extraction, and the application of the rapid solvent extraction in food detection is severely limited.
Disclosure of Invention
According to an aspect of the application, based on acetonitrile can make to wait to examine in the sample protein denaturation cluster and with including ferroferric oxide magnetic particle parcel form magnetism wait to examine sample solid part, can realize solid-liquid separation's principle under the effect of external magnet, provide a full-automatic magnetic separation and draw-solid phase extraction and unite all-in-one, this all-in-one simple structure, convenient to use improve sample pretreatment efficiency.
The full-automatic magnetic separation extraction-solid phase extraction combined all-in-one machine is characterized in that,
the method comprises the following steps: the device comprises an automatic addressing liquid-transferring device, a drug residue extraction system, an extracting solution concentration system, a solid phase extraction system and an eluent 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 extracting solution concentrating system is used for concentrating and in-situ redissolving the extracting solution to obtain an extracting redissolution;
the solid phase extraction system is used for carrying out solid phase extraction on the extraction redissolved solution to obtain an eluent;
the eluent concentration system is used for concentrating and redissolving the eluent to obtain a detection solution;
the automatic addressing liquid-transfering device is used for moving the extracting solution, the purifying solution and the eluent.
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 the electromagnetic module is conducted and acting on the acetonitrile to denature and agglomerate protein in a sample to be detected and wrap ferroferric oxide magnetic particles in the sample to be detected to form a magnetic solid part of the sample to be detected.
Optionally, the drug residue extraction system comprises: the homogenizer is used for carrying out in-situ crushing 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 disk; the electromagnetic module, the extracted sample bottle and the homogenizer are all placed on the first disk.
Optionally, the fully-automatic magnetic separation extraction-solid phase extraction combined all-in-one machine 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 fully-automatic magnetic separation extraction-solid phase extraction combined all-in-one machine 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 fully-automatic magnetic separation extraction-solid phase extraction combined all-in-one machine includes: a conduit system, the conduit system comprising: the device comprises a cleaning liquid bottle, a waste liquid bottle and a solvent distributor, wherein the bottom of the cleaning liquid bottle is respectively connected with the waste liquid bottle; the top of the cleaning liquid bottle is respectively connected with a cleaning liquid container;
the solvent distributor is arranged at the bottle mouth of the cleaning liquid bottle and is used for metering the discharged liquid.
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.
Optionally, the draw solution 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: concentrating the gas needle;
the concentrated gas needle is arranged in the concentrated sample bottle and used for blowing dry liquid.
Optionally, the draw solution concentration system comprises: the second tray, the heating device, the concentrated sample bottle and the liquid level sensor are arranged on the second tray.
Optionally, the fully-automatic magnetic separation extraction-solid phase extraction combined all-in-one machine includes: a conduit system, the conduit system comprising: a first reconstituted solution bottle and a solvent dispenser; the first compound solution bottle is connected with the concentrated sample bottle pipeline;
the solvent distributor is arranged at the bottle mouth of the first compound solution bottle and is used for metering the effluent 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 fully-automatic magnetic separation extraction-solid phase extraction combined all-in-one machine includes: the automatic addressing liquid-transferring device, the drug residue extraction system, the extracting solution concentration system, the solid phase extraction system and the eluent concentration system are accommodated in the light-shielding box.
Optionally, the solid phase extraction system comprises: the device comprises a solid phase extraction device and an eluent container, wherein the solid phase extraction device is used for automatically completing the activation, sample loading, leaching and elution of a solid phase extraction column; the eluent container is arranged at an eluent outlet of the solid phase extraction device and is used for containing the eluent.
Optionally, the eluent concentration system comprises: the device comprises a heating device, a liquid level sensor and a sample loading bottle;
the liquid level sensor is used for detecting the liquid level in the sample feeding sample bottle and is in control connection with the heating device;
the sample loading bottle comprises: concentrating the gas needle;
the concentrated gas needle is arranged in the sample loading sample bottle and used for drying liquid.
Optionally, the eluent concentration system comprises: and the heating device, the sample loading bottle and the liquid level sensor are arranged on the fourth tray.
Optionally, the fully-automatic magnetic separation extraction-solid phase extraction combined all-in-one machine includes: a conduit system, the conduit system comprising: a second reconstituted solution bottle and a solvent dispenser; the second compound solution bottle is connected with the sample loading bottle pipeline;
the solvent distributor is arranged at the bottle mouth of the second compound solution bottle and is used for metering the effluent liquid.
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.
According to another aspect of the application, a pretreatment method of a full-automatic magnetic separation extraction-solid phase extraction combined all-in-one machine is provided, which 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;
concentrating and in-situ redissolving the extracting solution to obtain an extracted redissolution;
carrying out solid phase extraction on the extracted complex solution to obtain an eluent;
and concentrating and re-dissolving the eluent in situ to obtain a detection solution.
The beneficial effects that this application can produce include:
1) the utility model provides a full-automatic magnetic separation draws-solid phase extraction allies oneself with uses all-in-one, can make to wait to examine in the sample protein denaturation cluster and with including ferroferric oxide magnetic particle parcel formation magnetism examine the sample solid part, can realize the principle of solid-liquid separation under the effect of external magnet, this application adopts the magnetic separation means to replace centrifuge to realize the solid-liquid separation of sample and extract, adopt the solid-phase extraction to realize the purification of extract, it can accomplish automatically and wait to detect the homogeneity of sample and draw, magnetism solid-liquid separation, solid-phase extraction purifies, concentration, preliminary treatment steps such as redissolution, can realize the remaining high flux of medicine in the food, full-automatic sample pretreatment, the practicality is stronger.
2) The utility model provides a full-automatic magnetic separation draws-solid phase extraction allies oneself with all-in-one adopts isotropic symmetry and the liquid-transfering device that has the automatic addressing function, realizes the automatic movement of liquid in each processing step, improves pretreatment efficiency. The all-in-one machine is particularly suitable for automatic solid phase extraction pretreatment.
Drawings
FIG. 1 is a schematic diagram of a fully automatic magnetic separation extraction-solid phase extraction integrated machine 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
Third delivery pipe
13
Sample extracting bottle
2
First compound solution bottle
14
First disk
3
Fourth delivery pipe
15
Liquid-transfering needle washing container
4
Second compound solution bottle
16
Homogenizer cutter washing container
5
Waste liquid bottle
17
Homogenizer
6
Fifth delivery pipe
18
First delivery pipe
7
Second plate
19
Liquid transferring needle
8
Concentrated sample bottle
20
Second delivery pipe
9
Liquid level inductor
21
Solvent dispenser
10
Third plate
22
Cleaning solution bottle
11
Solid phase extraction device
23
Extracting liquid bottle
12
Fourth plate
24
----
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Sample loading bottle
25
Internal suction pump
26
Light-proof box
27
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 present application provides a full-automatic magnetic separation extraction-solid phase extraction all-in-one that unites, includes: the device comprises an automatic addressing liquid-transferring device, a drug residue extraction system, an extracting solution concentration system, a solid phase extraction system and an eluent 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 to an extracting solution concentration system through an automatic addressing liquid-transferring device to be concentrated and redissolved in situ to obtain an extracting complex solution; moving the extracted re-solution to a solid phase extraction system through an automatic addressing liquid-transferring device to perform solid phase extraction on the extracted re-solution to obtain eluent; and moving the eluent to an eluent concentration system through an automatic addressing liquid-transferring device for concentration and in-situ redissolution to obtain a detection solution. 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, after the magnetic filler 1 is contacted 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 can be denatured into a group, and a magnetic substance is wrapped to form a magnetic solid part to be detected, the electromagnetic module is started and adsorbs 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, the pretreatment efficiency is high, the whole equipment is not low, and the size is small.
The placement positions of the drug residue extraction system, the extracting solution concentration system, the solid phase extraction system and the eluent concentration system are not limited, and the exchange of substances among the systems is carried out by an automatic addressing liquid-transferring device.
Medicine residue extraction system:
the drug residue extraction system comprises: a magnetically controllable first tray 3, an extraction sample vial 2, a homogenizer 6 and a magnetic packing 1.
Placing the extraction sample bottle 2 on the first plate 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 adopting a homogenizer 6, and the homogenizer 6 has an automatic addressing function and can carry out homogenizing treatment on each extracted sample bottle 2 on the first disc 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 6 automatically moves to a knife washing container for knife washing treatment. And then moving to the second sample, and repeating the operation.
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 the steps of adding extracting solution and magnetic fillers 1 into a sample to be detected, homogenizing to obtain a solid part of the sample to be detected, and starting an electromagnet module arranged on a first disc 3 to enable the first disc 3 to generate attraction force on the solid part of the sample to be detected, so that solid-liquid separation is realized.
After solid-liquid separation, a liquid phase is obtained as an extracting solution, the obtained extracting solution contains the information substance to be detected, and the liquid phase is transferred to the concentrated sample bottle 20 by a common liquid transferring device such as a liquid transferring needle or a liquid transferring gun which can be automatically addressed.
Alternatively, the magnetic filler 1 contains at least a magnetic substance;
preferably, the magnetic substance is ferroferric oxide magnetic particles;
more preferably, the magnetic filler 1 is: the mixture consists of ferroferric oxide magnetic particles, magnesium sulfate, sodium chloride, sodium citrate and disodium hydrogen citrate.
An extracting solution concentrating system:
the extract concentration system includes: a second tray 19, a concentrated sample bottle 20, a level sensor 21.
The extract is moved into the concentrated sample vial 20 by an automatically addressed pipetting device. The concentrated sample bottle 20 is connected with concentrated gas to blow the extracting solution dry or accelerate the evaporation process. The concentrated gas needle blows gas to the liquid of the concentrated sample bottle 20 and heats the concentrated sample bottle 20 to accelerate the evaporation process, and the liquid level is detected by the liquid level sensor 21 arranged at one side of the concentrated sample bottle 20 in the evaporation process. Until the liquid is blown dry or the volume is evaporated to a predetermined value. And adding a redissolution solvent into the sample, and performing redissolution to obtain an extracted redissolution.
The heating device is in control connection with the liquid level sensor 21, 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 26, liquid-transfering needle 8, and the one end of liquid-transfering needle 8 is stretched into and is waited to move and get in the liquid, and the other end is connected with internal suction pump 26, sets up the scale on the lateral wall of liquid-transfering needle 8, is convenient for control the liquid-transfering quantity. After the internal suction pump 26 is switched on, one end of the pipetting needle 8 sucks liquid to the required scale, and the pipetting needle 8 can be controlled by a mechanical arm and other parts to move into the liquid bottle to be placed.
Solid phase extraction system
The solid phase extraction system comprises: a third tray 22, a solid phase extraction device 23, an eluent container, and a device capable of automatically completing the functions of activating, loading, leaching and eluting the solid phase extraction column by the solid phase extraction device 23. An eluent container is arranged at an eluent outlet of the solid phase extraction device 23 and is used for containing eluent, so that the eluent can be conveniently moved into the sample loading bottle 25 through an automatic addressing liquid-moving device.
The solid phase extraction device 23 in the present application may be an existing conventional device.
The solid phase extraction device 23, the eluent container, can be placed on the third tray 22.
Eluent concentration system
The eluent concentration system comprises: a fourth tray 24, a liquid level sensor 21 and a sample loading bottle 25.
The eluent is moved by an automatically addressed pipetting device into the sample loading vial 25. The sample loading bottle 25 is connected with concentrated gas to blow the eluent or accelerate the evaporation process. The concentrated gas needle blows gas to the liquid of the sample bottle 25 and can heat the concentrated sample bottle 20 through the heating device arranged on the fourth tray 24 to accelerate the evaporation process, and the liquid level is detected through the liquid level sensor 21 arranged on one side of the concentrated sample bottle 20 in the evaporation process. Until the liquid is blown dry or the volume is evaporated to a predetermined value. And adding a redissolution solvent into the sample, and performing redissolution to obtain a detection solution. The heating means is not limited to being mounted on the fourth plate 24.
The heating device is in control connection with the liquid level sensor 21, so that the heating temperature can be automatically controlled according to the change condition of the liquid level, and full-automatic evaporation is realized.
A cleaning system:
optionally, a cleaning system is further included, the cleaning system is used for cleaning the automatic addressing pipetting device, the homogenizer 6 and other devices needing cleaning, and the cleaning 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 cutter washing container 5 is used for washing the cutter head of the homogenizer 6.
In the embodiment, the pipette needles 8 of the automatic addressing pipetting device are cleaned in the pipette needle washing container 4 after use, the pipette needle washing container 4 is arranged on the first tray 3, the pipette needle washing container 4 is communicated with the cleaning solution bottle 11 by the first conveying pipe 7, and the liquid outlet of the homogenizer knife washing container 5 is connected with the waste solution bottle 17 by the waste solution drainage conduit.
The homogenizer 6 after homogenizing all will utilize homogenizer to wash sword container 5 and wash, this homogenizer washes sword container 5 and sets up on first dish 3, and utilizes first conveyer pipe 7 and washing liquid bottle 11 through connection on the homogenizer washes sword container 5, through connection has the measurement distributor between washing liquid bottle 11 and the first conveyer pipe 7, the liquid outlet of homogenizer washes sword container 5 utilizes waste liquid flowing back pipe 18 to be connected with waste liquid bottle 17, waste liquid bottle 17 sets up in the outside of dodging case 27.
Optionally, a light shielding box 27 is further included, and an automatic addressing liquid transferring device, a drug residue extraction system, an extract concentration system, a solid phase extraction system and an eluent concentration system are accommodated in the light shielding box 27. Through setting up the light-shading box 27, 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 12, a cleaning liquid bottle 11, a waste liquid bottle 17, a first re-solution bottle 14 and a second re-solution bottle 16. Solvent distributors 10 are arranged at the outlets of the extraction liquid bottle 12, the cleaning liquid bottle 11, the first re-dissolution liquid bottle 14 and the second re-dissolution liquid bottle 16, so that the amount of the effluent liquid can be conveniently measured.
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 17; 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 extraction liquid bottle 12 is connected with the extraction sample bottle 2 through a pipeline. The first reconstituted solution bottle 14 is connected with the concentrated sample bottle 20 through a pipeline.
The second compound solution bottle 16 is connected with the sample loading bottle 25 through a pipeline.
The number of extraction sample bottles 2, concentration sample bottles 20, and loading sample bottles 25 may be determined as necessary.
Another aspect of the present application further provides a pretreatment method of the above full-automatic magnetic separation extraction-solid phase extraction combined all-in-one machine, including 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;
concentrating the extracting solution, and redissolving in situ to obtain a re-extracted solution;
carrying out solid phase extraction on the extracted complex solution to obtain an eluent;
and concentrating and re-dissolving the eluent in situ 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.