CN111060659A - Sample pretreatment device capable of automatically identifying liquid level height and sample treatment device - Google Patents
Sample pretreatment device capable of automatically identifying liquid level height and sample treatment device Download PDFInfo
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- CN111060659A CN111060659A CN201911412573.4A CN201911412573A CN111060659A CN 111060659 A CN111060659 A CN 111060659A CN 201911412573 A CN201911412573 A CN 201911412573A CN 111060659 A CN111060659 A CN 111060659A
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- G—PHYSICS
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- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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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
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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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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Abstract
The invention provides a sample pretreatment device and a sample treatment device capable of automatically identifying liquid level height, and relates to the technical field of analytical chemistry. The sample pretreatment device comprises a main pipe and one or more than one auxiliary pipe connected with the main pipe in parallel, through holes are formed between the adjacent main pipe and the auxiliary pipe, and between the adjacent auxiliary pipe and the auxiliary pipe, and filtering pieces for preventing the adsorbent from escaping are arranged on the through holes; the bottom of the main pipe is connected with a driving piece for driving the bottom to move up and down, and the upper end of the main pipe is connected with a detection piece for identifying the liquid level height; optionally, the main tube is filled with an extraction liquid. Above-mentioned preceding processing apparatus of sample can realize extracting, moving liquid, the collection of sample solution fast, makes sample solution and adsorbent separation effect better, has and can realize the accuracy and move liquid, easy operation, automatic advantage such as with low costs.
Description
Technical Field
The invention relates to the technical field of analytical chemistry, in particular to a sample pretreatment device and a sample treatment device capable of automatically identifying liquid level height.
Background
The detection of chemical and biological components in the fields of food safety, environmental protection, medicine research and development and the like has gradually become a content closely related to the daily life of people. This includes measurement of the blood concentration of the drug, measurement of metabolites in urine after the patient has taken the drug; measuring pesticide residue or other harmful substances in food (such as malachite green and Sudan red), and measuring nutrient substances; and (4) measuring harmful substances in water and air. All the detection processes, no matter what detection means is used, mostly need to be subjected to sample pretreatment, including the processes of sample extraction, enrichment and purification.
The currently used sample pretreatment products mainly comprise a solid phase extraction column type and a QuEChERS form. The QuEChERS form is formed by combining partial abbreviations of Quick (Quick), simple (Easy), Cheap (Cheap), efficient (Effective), durable (Rugged) and Safe (Safe) words, and is a convenient and efficient purification pretreatment technology for detecting pesticide residues in agricultural products. With the development of the field of QuEChERS use, the method becomes a standard sample processing method for detecting pesticide residues in fruits and vegetables globally. In addition, along with the development of the application, the method also relates to more and more fields, such as detection of veterinary drugs in meat, environmental water samples, wine, pollutants in soil, drugs, abuse drugs and the like.
The QuEChERS mechanism is that after a homogenized sample is extracted by acetonitrile, extraction salt is adopted for salting out and layering, and a matrix dispersion mechanism is utilized, and N-Propylethylenediamine (PSA), C18 or other adsorbents are combined with most of interferents such as organic acid, fatty acid and the like in a matrix for removal, so that the purification purpose is achieved. In order to improve the wide adaptability of the QuEChERS method to detection of pesticide residues with various samples and various chemical properties, the original QuEChERS (also called original QuEChERS) is improved in the U.S. standard (AOAC2007.01) and the european standard (EN15662) so as to ensure that pesticide residues sensitive to pH are effectively extracted and a good recovery rate is obtained. In the QuEChERS operation, an acetic acid-sodium acetate buffer system or a citrate buffer system is used for adjusting the pH to be weakly acidic, so that the chemical property change of most pesticides which are unstable to acid or alkali can be avoided.
QuEChERS has the characteristics of simple program, high efficiency and high sensitivity. However, the current QuEChERS technique is mainly performed independently in each centrifuge tube. In the extraction or purification step, the adsorbent in the centrifugal tube is mixed with the extraction solution or the purification solution by oscillation, and then the solid-liquid separation of the solid adsorbent and the solution is realized by centrifugation. However, the centrifugal operation is complicated, and the centrifugal process requires a long time, and there are problems that the adsorbent particles enter the upper layer liquid during the solid-liquid separation after the centrifugation, and the like. In addition, the prior QuEChERS needs to transfer the liquid in the previous step to the container in the next step by using a pipetting mode among the steps, so that the operation is more, and the automation cost is higher.
Disclosure of Invention
In view of the above, the present invention is directed to provide a sample pretreatment apparatus capable of automatically identifying a liquid level height, which can rapidly implement processes of oscillation mixing and solid-liquid separation related to processes of extraction, pipetting, purification and collection of a sample solution, avoid using a long-time centrifugal operation, and has the advantages of being capable of implementing accurate pipetting, simple in operation, low in automation cost, and the like.
The invention provides a sample pretreatment device capable of automatically identifying liquid level height, which comprises a main pipe and one or more auxiliary pipes connected with the main pipe in parallel, wherein through holes are formed between the adjacent main pipe and the auxiliary pipes, and between the auxiliary pipes, the bottom of the main pipe is connected with a driving piece for driving the bottom to move up and down, and the upper end of the main pipe is connected with a detection piece for identifying liquid level height; optionally, the main tube is filled with an extraction liquid.
The sample pretreatment device capable of automatically identifying the liquid level height is composed of a plurality of parallel tubes, wherein the tubes are connected through holes, one of the tubes is a main tube, the other tubes are auxiliary tubes, the adjacent tube is a first-stage auxiliary tube for distinguishing different auxiliary tubes, the adjacent tube is a second-stage auxiliary tube, the adjacent tube is a third-stage auxiliary tube, and the adjacent tubes are named in sequence for distinguishing different auxiliary tubes. It should be noted that the numbers of "first, second, or third stage" and the like are only for distinguishing, and the attached pipes with different numbers may be the same or different.
The specific sizes of the main pipe and the auxiliary pipe are not limited, and can be reasonably selected and adjusted according to actual requirements such as the amount of samples to be processed and the like.
When the sample pretreatment device is used for treating the sample solution, the sample solution and the extraction solution are injected into the main pipe and are mixed in an oscillating way. After the sample solution in the main pipe is extracted, the driving piece at the bottom of the main pipe pushes the sample solution in the main pipe to move upwards, the detection piece can detect the liquid level height, the piston rising height, the cross-sectional area inside the main pipe and the like are calculated, so that the liquid with a certain volume can be accurately transferred to the auxiliary pipe, and then the sample solution is directly collected from the auxiliary pipe.
The operation process comprises a plurality of steps of extraction, liquid transfer and collection, and can realize automatic operation, and compared with the traditional manual use mode of the centrifugal tube type QuEChERS, the operation has great efficiency advantage.
Above-mentioned sample pretreatment device can realize extracting, moving liquid of sample solution fast, collect the process that the relevant oscillation in-process mixes and solid-liquid separation, has avoided using the centrifugal operation who spends longer time, possesses the function of liquid level height discernment moreover, has and can realize accurate moving liquid, easy operation, automatic advantage such as with low costs.
Furthermore, on the basis of the technical scheme provided by the invention, the main pipe and/or the auxiliary pipe are/is filled with an adsorbent, and a filter piece for preventing the adsorbent from passing through is arranged on a through hole between the auxiliary pipe and the auxiliary pipe; optionally, a filter for preventing the adsorbent from passing through is arranged on the through hole between the main pipe and the auxiliary pipe.
It should be noted that "the main pipe and/or the accessory pipe is filled with the adsorbent" can be understood as three explanations: (1) the main pipe is filled with an adsorbent; (2) the adsorption agent is filled in the auxiliary pipe; (2) the main pipe and the auxiliary pipe are both filled with adsorbents.
When the extracted sample solution needs to be purified, the main pipe and/or the accessory pipe is filled with an adsorbent, so that the sample pretreatment device can have a purification function, and the function of the sample treatment device can be optimized.
The through hole between the accessory pipe and the accessory pipe is provided with the filtering piece for preventing the adsorbent from passing through, so that the adsorbent can not enter the accessory pipe at the last stage no matter the adsorbent is filled in the main pipe and/or the accessory pipe. Therefore, a filter member for preventing the passage of the adsorbent may be optionally provided, either with or without the through hole between the main tube and the auxiliary tube.
However, if only the main tube is connected to one of the auxiliary tubes, the adsorbent is filled in the main tube, and a filter member for preventing the adsorbent from passing through the through hole is required to be disposed in the through hole between the main tube and the auxiliary tube, so that impurities, the adsorbent and the like in the main tube are blocked by the filter member in the through hole and cannot enter the auxiliary tube.
Further, on the basis of the technical scheme provided by the invention, the height of the bottom end of the detection piece is flush with that of the bottom end of the through hole.
Through adopting above-mentioned scheme, when the liquid level of the sample solution in being responsible for contacted the bottom of surveying the piece, can make the sensor produce the signal to realize the discernment of initial liquid level height, and the bottom height of surveying the piece highly flushes with the bottom height of through-hole, the piston distance that rises and the inside cross-sectional area of being responsible for are the volume that liquid shifted, and simple quick realization accurate shifts the liquid of certain volume.
When the height of the bottom end of the detecting piece is not level with the height of the bottom end of the through hole. For example: when the bottom height of the detection piece is lower than that of the through hole, the height difference is recorded, and the volume of the transferred liquid is obtained through calculation with the liquid level height, the piston lifting height and the numerical value of the cross section area inside the main pipe. Or for example: when the bottom height of the detection piece is higher than that of the through hole, a distance detector is selected, the distance between the detector and the initial liquid level and the distance between the detector and the bottom end of the through hole are recorded, and the volume of the transferred liquid is obtained through calculation with the liquid level height, the piston lifting height and the numerical value of the cross section area of the inner part of the main pipe. Thus, the bottom height of the detection piece is flush with that of the through hole, and liquid with a certain volume can be transferred more conveniently and simply.
Further, on the basis of the technical scheme provided by the invention, the main pipe and the auxiliary pipe are both hollow columnar structures with sealed bottoms, and the hollow columnar structures comprise any one of a cylindrical structure, a triangular column structure, a square column structure or a pentagonal column structure.
The hollow columnar structures of the main pipe and the auxiliary pipe are limited, and the structures with regular shapes, such as a conventional cylindrical structure, a triangular column structure, a square column structure or a pentagonal column structure, can be selected, so that the manufacturing difficulty and the manufacturing cost can be reduced.
Further, on the basis of the technical scheme provided by the invention, the main pipe is of a hollow cylindrical structure, the height is 0.1-3cm, and the inner diameter is 1-5 cm.
The height of the main tube is typically, but not limited to, 0.1cm, 1cm, 1.5cm, 2cm or 3 cm.
The internal diameter of the main tube is typically, but not limited to, 1cm, 2cm, 3cm, 4cm or 5 cm.
The appearance of the preferred main pipe is a cylindrical structure, and the hollow interior is also a cylindrical structure, so that compared with other structures, the cylindrical structure is more convenient to manufacture; the hollow interior is cylindrical, the internal space is relatively large, and more adsorbent or extracting solution can be filled.
Further, on the basis of the technical scheme provided by the invention, the auxiliary pipe is of a hollow square columnar structure, and the side length is 1-5 cm.
The side length of the accessory tube is typically, but not limited to, 1cm, 2cm, 3cm, 4cm or 5 cm.
The preferred accessory pipe is a hollow square column structure, and the inner space is also a square structure, so that the accessory pipe and the main pipe with a cylindrical structure can be better matched in parallel for use, and the processing and forming are convenient.
Further, on the basis of the technical scheme provided by the invention, the main pipe and the auxiliary pipes are made of polypropylene, polyethylene, polyformaldehyde, polyvinyl chloride, polystyrene, metal, graphite or a mixture of the materials in any proportion.
In a preferred embodiment of the present invention, a top cover is detachably connected to the top of the main pipe, and the detecting member is penetratingly disposed on the top cover.
The top cover is made of one or a mixture of polypropylene, polyethylene, polyformaldehyde and polyvinyl chloride in any proportion.
Set up the detachable top cap at the top of being responsible for, survey the piece and run through and set up on the top cap, make to survey the piece and can take off with the top cap together, conveniently add sample solution, extract or adsorbent etc. in being responsible for.
In a preferred embodiment of the invention, the probe members are disposed on opposite sides of the main pipe wall. The detection piece is arranged on the side face of the pipe wall of the main pipe, the detection piece does not need to be taken out frequently, only the top cover needs to be opened, and a sample solution, an extracting solution or an adsorbent and the like are added, so that damage of the detection piece caused by frequent taking out and placing operations is reduced.
Further, on the basis of the technical scheme provided by the invention, the detection piece comprises two electrodes which are arranged in parallel, and the two electrodes are connected with a sensor capable of sensing the liquid level height;
furthermore, the electrode is made of a conductive material, and is preferably a metal or a metal alloy;
further, the sensor is a capacitive sensor.
The electrode is made of conductive material, can be conductive non-metal material or metal material, and is preferably metal or metal alloy.
The electrodes may be, but are not limited to, iron wire, copper wire, nickel wire, or alloys of the above metals. The capacitance type sensor has the advantages of high impedance, low power, good temperature stability, simple structure, strong adaptability and the like, and the liquid level change detection is more sensitive and accurate.
Furthermore, on the basis of the technical scheme provided by the invention, a detachable inner plug is arranged below the top cover, at least two layers of filtering pieces are arranged in the inner plug, and the filtering pieces are hermetically connected with the inner plug; optionally, an adsorbent is packed between the two filter layers.
By adopting the scheme, the inner plug is internally provided with at least two layers of filtering pieces, so that fine particles such as impurities and the like remained after the sample solution is extracted can be better filtered and removed; the adsorbent can be selectively filled between the two layers of filter elements, the adsorbent cannot pass through the filter elements at the moment, so that the sample solution in the main pipe is purified by contacting the filter elements with the adsorbent, the inner plug is taken out after the purification is finished, and then the inner plug with the adsorbent is replaced. Therefore, when the sample solution is extracted without adsorbent purification and only the particle impurities are removed by simple filtration, only the inner plug with the filter element needs to be inserted. If the sample solution needs adsorbent purification after extraction, the adsorbent is filled in the inner plug, compared with the method that the adsorbent is directly filled in the main pipe and the auxiliary pipe, the adsorbent is not convenient to take out, and the inner plug is simpler and more convenient to use once.
Further, on the basis of the technical scheme provided by the invention, the particle size of the adsorbent is 5-100 μm; preferably, the adsorbent is one or more of anhydrous sodium sulfate, anhydrous magnesium sulfate, sodium acetate, sodium chloride, C18 bonded silica gel, graphitized carbon, N-propyl ethylenediamine bonded silica gel or polystyrene divinylbenzene high polymer.
The particle size of the adsorbent is typically, but not limited to, 5 μm, 10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm or 100 μm.
The larger the particle size of the adsorbent is, the smaller the specific surface area is, the capacity of the adsorbent for adsorbing interferents such as organic acid, fatty acid and the like is reduced, and the impurity removal effect is poor; the smaller the particle size of the adsorbent is, the less the effect of adsorbing impurities is improved, and the preparation and subsequent solid-liquid separation are difficult. The particle size range of the adsorbent is optimized, so that the effect of adsorbing impurities in a sample solution can be improved, and the difficulty of subsequent treatment and the sample treatment cost are reduced.
The specific shape of the adsorbent is not particularly limited, and may be irregular, spherical, square, elliptical, triangular, or the like. The spherical adsorbent is preferably spherical, and the specific surface area of the spherical adsorbent is larger under the same particle size, so that the binding area of the adsorbent and interferents such as organic acid, fatty acid and the like can be further increased, and the impurity adsorption effect can be improved.
Further, on the basis of the technical scheme provided by the invention, the filter element is a sieve plate and/or a filter membrane.
It should be noted that "the filter elements are sieve plates and/or filter membranes" can be understood as three explanations: (1) the filtering piece is a sieve plate; (2) the filter element is a filter membrane; (2) the filtering member is formed by combining a sieve plate and a filtering membrane.
Furthermore, the aperture of the sieve plate is 0.22-20 μm, and the thickness is 0.5-5 mm. The pore size of the sieve plate may be, but is not limited to, 0.22 μm, 1 μm, 5 μm, 10 μm, 15 μm, 18 μm, or 20 μm; the thickness of the screen plate may be, but is not limited to, 0.5mm, 1mm, 2mm, 3mm, 4mm, or 5 mm. The sieve plate preferably has a pore size and a thickness such that the sieve plate is better able to block the escape of the adsorbent.
Furthermore, the aperture of the filter membrane is 0.2-1 μm. The pore size of the filter may be, but is not limited to, 0.2 μm, 0.4 μm, 0.6 μm, 0.8 μm or 1 μm.
Further, the sieve plate and the filter membrane are made of one or more of polytetrafluoroethylene, polypropylene, polyether sulfone, nylon or polyvinylidene fluoride.
Further, on the basis of the technical scheme provided by the invention, the driving piece is a piston, and the piston is connected with the inner wall of the main pipe in a sealing and sliding manner; preferably, the piston is made of polypropylene, polyethylene, polyformaldehyde, polyvinyl chloride, polystyrene, metal, graphite or a mixture of the materials in any proportion.
The piston is selected as a driving piece, the piston is connected with the inner wall of the main pipe in a sealing and sliding mode, and the piston is externally connected with a motor and a control system, so that the accurate moving distance of the piston is accurately controlled, and the accurate moving of the liquid is realized.
Further, on the basis of the technical scheme provided by the invention, when the sample pretreatment device is mainly formed by connecting the main pipe and an auxiliary pipe in parallel, the through hole is close to the top end of the auxiliary pipe, and the adsorbent is filled in the inner plug and/or the cavity of the main pipe.
In a preferred embodiment of the present invention, the sample pretreatment device mainly comprises a main pipe and an auxiliary pipe connected in parallel, wherein a through hole is close to the top end of the auxiliary pipe, and a sieve plate is arranged on the through hole; the top of the main pipe is covered with a top cover, the electrodes are vertically arranged on two sides of the inner wall of the main pipe in parallel, an inner plug is arranged below the top cover, and the adsorbent is filled in the inner plug; the bottom of the main pipe is connected with a piston.
In a preferred embodiment of the present invention, the sample pretreatment device comprises a main pipe and an auxiliary pipe connected in parallel, wherein a through hole is near to the top end of the auxiliary pipe, and a sieve plate is arranged on the through hole; the top of the main pipe is covered with a top cover, the electrode vertically penetrates through the top cover in parallel, and the adsorbent is filled in the cavity of the main pipe; the bottom of the main pipe is connected with a piston.
In a preferred embodiment of the present invention, the sample pretreatment device comprises a main pipe and an auxiliary pipe connected in parallel, wherein a through hole is near to the top end of the auxiliary pipe, and a sieve plate and a filter membrane are arranged on the through hole; the top of the main pipe is covered with a top cover, the electrode vertically penetrates through the top cover in parallel, and the adsorbent is filled in the cavity of the main pipe; the bottom of the main pipe is connected with a piston.
When sample pretreatment device mainly comprises being responsible for and an accessory tube, sample solution draws and purifies the back in being responsible for, and the piston promotes the sample solution upward movement who is responsible for in, and when the liquid level of sample solution contacted the bottom of electrode, discernment initial liquid level height, the piston continues upward movement a section distance, realizes that the liquid of specific volume shifts to the accessory tube in, and impurity and adsorbent etc. in the main pipe can be blockked by sieve and the filter membrane on the through-hole and can't get into the accessory tube, collect sample solution in the accessory tube.
Further, on the basis of the technical scheme provided by the invention, when the sample pretreatment device comprises a main pipe and two auxiliary pipes which are connected in parallel (the auxiliary pipe close to the main pipe is named as a primary auxiliary pipe, and the auxiliary pipe far away from the main pipe is named as a secondary auxiliary pipe), a through hole between the main pipe and the auxiliary pipe is close to the top end of the auxiliary pipe, the through hole between the auxiliary pipe and the auxiliary pipe is close to the bottom end of the auxiliary pipe, and an adsorbent is filled in a cavity of the auxiliary pipe close to the main pipe.
In a preferred embodiment of the present invention, the sample pretreatment device comprises a main pipe and two auxiliary pipes connected in parallel, the top of the main pipe is covered with a top cover, and the bottom of the main pipe is connected with a piston; a through hole (a sieve plate is arranged on the through hole) between the main pipe and the first-stage auxiliary pipe is close to the top end, a through hole (a sieve plate and a filter membrane are arranged on the through hole) between the first-stage auxiliary pipe and the second-stage auxiliary pipe is close to the bottom end, and an adsorbent is filled in a cavity of the first-stage auxiliary pipe; the inner wall of the top of the primary auxiliary pipe is connected with a plug in a sealing and sliding manner.
In a preferred embodiment of the invention, the sample pretreatment device comprises a main pipe and two auxiliary pipes which are connected in parallel, the top of the main pipe is covered with a top cover, an electrode vertically penetrates through the top cover in parallel, and the bottom of the main pipe is connected with a piston; a through hole (a sieve plate and a filter membrane are arranged on the through hole) between the main pipe and the first-stage auxiliary pipe is close to the top end, a through hole (a sieve plate is arranged on the through hole) between the first-stage auxiliary pipe and the second-stage auxiliary pipe is close to the bottom end, and an adsorbent is filled in a cavity of the first-stage auxiliary pipe; the inner wall of the top of the primary auxiliary pipe is connected with a plug in a sealing and sliding manner.
The sample pretreatment device mainly comprises a main pipe, a first-stage attached pipe and a second-stage attached pipe, wherein after sample solution is extracted and completed in the main pipe, a piston pushes the sample solution in the main pipe to move upwards, when the liquid level of the sample solution contacts the bottom end of an electrode, the initial liquid level height is identified, the piston continues to move upwards for a certain distance, the liquid with a specific volume is transferred into the first-stage attached pipe (impurities in the main pipe are blocked by a sieve plate and a filter membrane on a through hole and cannot enter the first-stage attached pipe), the adsorbent in the first-stage attached pipe purifies the sample solution, then a plug at the top of the first-stage attached pipe moves downwards, the liquid in the first-stage attached pipe is transferred into the second-stage attached pipe (the adsorbent in the first-stage attached pipe is blocked by the sieve plate on the through hole and cannot enter the second.
Further, on the basis of the technical scheme provided by the invention, the extracting solution is a mixed solution formed by mixing acetonitrile and water according to any proportion.
The invention also provides a sample processing device which comprises the sample preprocessing device capable of automatically identifying the liquid level height.
The invention also provides a sample pretreatment method, which adopts the sample pretreatment device capable of automatically identifying the liquid level height or the sample treatment device to carry out sample pretreatment.
Wherein the sample pretreatment comprises the treatment processes of sample extraction, enrichment, purification or collection and the like.
The invention adopts the technical scheme and has the following beneficial effects:
(1) the sample pretreatment device capable of automatically identifying the liquid level height can quickly realize the processes of relevant oscillation mixing and solid-liquid separation in the processes of extraction, liquid transfer and collection of a sample solution, and has the advantages of simple operation and low automation cost;
(2) the sample pretreatment device capable of automatically identifying the liquid level height avoids the use of long-time centrifugal operation, has the function of identifying the liquid level height, and has the advantage of realizing accurate liquid transfer.
Drawings
FIG. 1 is a schematic sectional view showing a sample pretreatment apparatus according to example 1;
FIG. 2 is a schematic sectional view of a sample pretreatment apparatus according to example 2;
FIG. 3 is a schematic diagram showing a cross-sectional view and an exploded structure of a sample pretreatment apparatus in example 3;
fig. 4 is a schematic diagram showing a cross-sectional view and an exploded structure of the sample pretreatment apparatus in example 4.
Reference numerals:
1. a main pipe; 11. a top cover; 12. an electrode; 13. a piston; 14. an inner plug; 141. a third screen deck; 142. a fourth sieve plate; 2. a primary auxiliary pipe; 21. a first through hole; 22. a first screen deck; 23. a plug; 3. a secondary auxiliary pipe; 31. a second through hole; 32, a first step of removing the first layer; a second screen deck; 4. a sample solution.
Detailed Description
Unless defined otherwise, all scientific and technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A sample pretreatment device capable of automatically identifying liquid level height is shown in figure 1 and is formed by connecting a main pipe 1, a first-stage auxiliary pipe 2 and a second-stage auxiliary pipe 3 which are made of polypropylene materials in parallel, wherein through holes are formed between the main pipe 1 and the first-stage auxiliary pipe 2 and between the first-stage auxiliary pipe 2 and the second-stage auxiliary pipe 3; the top of the main pipe 1 is covered with a top cover 11, and the top cover 11 is connected with an electrode 12; the bottom of the main pipe 1 is connected with a piston 13.
The main pipe 1 is a hollow cylindrical structure, the hollow interior is also a cylindrical structure, the axis is vertically arranged, and the inner diameter is 5 cm. Be responsible for 1 top cover and have top cap 11 (polypropylene material), top cap 11 is one end open-ended cylindric groove structure, and the opening is vertical downwards, and the bottom surface thickness of recess is 5mm, is responsible for 1 top and the bottom surface butt of recess. Two independent and parallel electrodes 12 vertically penetrate through the top surface of the top cover 11, the two electrodes 12 are metal wires with the length of 1cm, a capacitive sensor (not shown in the drawing) is connected to the top end of each metal wire, and the bottom end of each metal wire penetrates into the cavity of the main pipe 1. The bottom of the main pipe 1 is sealed and connected with a piston 13 in a sliding mode, the piston 13 is of a cylindrical structure, the thickness of the piston is 5mm, the piston is made of polypropylene materials, and the piston 13 is connected with a motor and a control system.
Be responsible for 1 and have parallelly connected one-level to attach pipe 2 and second grade and attach pipe 3, one-level attaches pipe 2 and second grade and attaches pipe 3 and all be located the right side of being responsible for 1, and the height that is responsible for 1 all is higher than one-level and attaches pipe 2 and second grade and attach pipe 3, and one-level attaches pipe 2 and second grade and attaches pipe 3 highly the same. The one-level attaches pipe 2 and second grade and attaches pipe 3 and be cavity square column structure, and cavity inside is cylindric structure, vertical setting, and the inside internal diameter of cavity is 3 cm. A first through hole 21 is arranged between the main pipe 1 and the first-stage auxiliary pipe 2, the cross section of the first through hole 21 is circular, and the axis is horizontally arranged; the inner diameter of the first through hole 21 is 5mm, the upper edge of the first through hole is 5mm away from the upper edge of the pipe wall of the first-stage attached pipe 2, and the lower edge of the first through hole is flush with the bottom ends of the two electrodes 12. A second through hole 31 is arranged between the first-stage auxiliary pipe 2 and the second-stage auxiliary pipe 3, the cross section of the second through hole 31 is circular, and the axis is horizontally arranged; the inner diameter of the second through hole 31 is 5mm, and the lower edge is flush with the bottom of the secondary auxiliary pipe 3.
The top of one-level accessory pipe 2 is sealed and is slided and be connected with stopper 23, and stopper 23 is flat round platform column structure, and thickness is 3mm, is made by the polypropylene material, and stopper 23 outer even has the motor.
The first through hole 21 is provided with a first sieve plate 22, the first sieve plate 22 is a disc-shaped structure with filter holes, the axis is superposed with the axis of the first through hole 21, the aperture of the filter holes is 5 mu m, the outer diameter of the filter holes is larger than that of the first through hole 21, and the first sieve plate 22 is made of polytetrafluoroethylene.
The second through hole 31 is provided with a second sieve plate 32 and a filter membrane (not shown in the figure), the second sieve plate 32 is a disk-shaped structure with filter holes, the axis of the second sieve plate is coincident with the axis of the second through hole 31, the aperture of the filter holes is 5 μm, and the aperture of the filter membrane is 0.22 μm. The filtering membrane is attached to the second sieve plate 32, the second sieve plate 32 is made of polytetrafluoroethylene, and the filtering membrane is made of nylon.
The use principle of the embodiment is as follows: after the top cover 11 is opened, the sample solution 4 and the extracting solution are injected into the main pipe 1, meanwhile, the adsorbent is added into the first-stage auxiliary pipe 2, and the mixture is oscillated and mixed after the top cover 11 is replaced. After the sample solution 4 in the main pipe 1 is extracted, the piston 13 pushes the sample solution 4 in the main pipe 1 to move upwards, when the liquid level of the sample solution 4 in the main pipe 1 contacts the bottom end of the electrode 12, the capacitive sensor can generate a signal, the height of the initial liquid level is identified, the piston 13 continues to move upwards for a certain distance, the sample solution 4 with a specific volume is transferred to the first-stage auxiliary pipe 2 through the first through hole 21, and the adsorbent in the first-stage auxiliary pipe 2 purifies the sample solution 4. After the purification is completed, the plug 23 moves downwards, so that the sample solution 4 in the first-stage accessory pipe 2 is transferred to the second-stage accessory pipe 3 through the second through hole 31, and the sample solution 4 is directly collected by a pipettor from the second-stage accessory pipe 3.
Example 2
A sample pretreatment device capable of automatically identifying the liquid level height is different from the sample pretreatment device of the embodiment 1 as shown in figure 2:
(1) the two metal wire electrodes 12 are respectively positioned at two sides of the pipe wall of the main pipe 1 and can be contacted with the solution in the main pipe 1, one metal wire electrode 12 is inserted in the first through hole 21, the other metal wire electrode 12 is inserted in the side wall of the main pipe 1 opposite to the first through hole 21, and the lengths of the two metal wire electrodes 12 are both 10 mm;
(2) the inner diameter of the main pipe 1 is 4cm, the thickness of the bottom surface of the groove of the top cover 11 is 3mm, the side length of the periphery of the first-stage auxiliary pipe 2 and the second-stage auxiliary pipe 3 is 2cm, and 200mg of C18, 150mg of PSA and 50mg of graphitized carbon adsorbent are added into the first-stage auxiliary pipe 2.
Except for the above differences, the structures and the connection relations of the rest of the components are the same as those of the embodiment 1 (the plug 23 on the primary auxiliary pipe 2 is not shown in fig. 2).
The principle of use of this embodiment is the same as that of embodiment 1.
Example 3
A sample pretreatment device capable of automatically identifying liquid level height is shown in figure 3, and is formed by connecting a main pipe 1 and a primary auxiliary pipe 2 which are made of polypropylene materials in parallel, wherein a first through hole 21 is arranged between the main pipe 1 and the primary auxiliary pipe 2; the top of the main pipe 1 is covered with a top cover 11, and the top cover 11 is connected with an electrode 12; an inner plug 14 is arranged below the top cover 11, and a piston 13 is connected to the bottom of the main pipe 1.
The main pipe 1 is a hollow cylindrical structure, the hollow interior is also a cylindrical structure, the axis is vertically arranged, and the inner diameter is 3 cm. Be responsible for 1 top cover and have top cap 11, top cap 11 is one end open-ended cylindric groove structure, and the opening is vertical downwards, and the bottom surface thickness of recess is 5mm, is responsible for 1 top and the bottom surface butt of recess. Two independent and parallel electrodes 12 vertically penetrate through the top surface of the top cover 11, and the two electrodes 12 are both metal wires with the length of 1 cm. The bottom of the main pipe 1 is sealed and connected with a piston 13 in a sliding mode, and the piston 13 is of a cylindrical structure and is 7mm thick.
An inner plug 14 is embedded in the cavity of the main pipe 1 below the top cover 11. The inner plug 14 is a hollow cylindrical structure, is vertically arranged, and has an axis coincident with that of the main pipe 1, and the bottom of the inner plug is abutted against the side wall of the main pipe 1 (the inner diameter of the upper part of the side wall of the main pipe 1 is slightly increased, so that the outer diameter of the inner plug 14 is larger than the inner diameter of the pipe wall of the lower part of the main pipe 1 and is abutted against the pipe wall of the upper part of the main pipe 1, and the inner plug 14 is clamped and embedded in the main pipe 1. The lower end of the inner plug 14 is provided with a third sieve plate 141 and a fourth sieve plate 142, and the third sieve plate 141 and the fourth sieve plate 142 are arranged at intervals up and down. The third sieve plate 141 and the fourth sieve plate 142 are both disc-shaped structures with filter holes, the axis of the disc-shaped structures is coincident with the axis of the inner plug 14, and the aperture of each filter hole is 5 μm. The circumferential outer walls of the third sieve plate 141 and the fourth sieve plate 142 are connected with the inner wall of the inner plug 14 in a sealing way, and the third sieve plate 141 and the fourth sieve plate 142 are both made of polytetrafluoroethylene.
The first-level accessory pipe 2 is of a hollow square columnar structure (the bottom is sealed), the inside of the hollow is of a cylindrical structure, the axis direction is vertical, and the inner diameter is 2 cm. A first through hole 21 is arranged between the main pipe 1 and the first-stage auxiliary pipe 2, the cross section of the first through hole 21 is circular, and the axis is horizontally arranged; the inner diameter of the first through hole 21 is 5mm, the upper edge of the first through hole is 5mm away from the upper edge of the pipe wall of the first-stage attached pipe 2, the lower edge of the first through hole is flush with the bottom ends of the two electrodes 12, and the lower edge of the first through hole 21 is higher than the top end of the third sieve plate 141.
A first sieve plate 22 is arranged in the first through hole 21, the first sieve plate 22 is a disc-shaped structure with filter holes, the axis of the first sieve plate is overlapped with the axis of the first through hole 21, and the aperture of each filter hole is 5 mu m.
The use principle of the embodiment is as follows: after the top cover 11 is opened and the inner plug 14 is removed, the sample solution 4 and the extraction liquid are injected into the main pipe 1, and at the same time, the adsorbent is filled between the third sieve plate 141 and the fourth sieve plate 142 of the inner plug 14, and the inner plug 14 and the top cover 11 are returned to mix by shaking. After the sample solution 4 in the main pipe 1 is extracted, the piston 13 pushes the sample solution 4 in the main pipe 1 to move upwards, after the sample solution 4 contacts the bottom end of the inner plug 14, the sample solution 4 enters the inner plug 14 through the fourth sieve plate 142, the adsorbent in the inner plug 14 purifies the sample solution 4, the sample solution 4 continues to move upwards through the third sieve plate 141 after being purified, when the liquid level of the sample solution 4 in the main pipe 1 contacts the bottom end of the electrode 12, the capacitive sensor can generate a signal to identify the height of the initial liquid level, the piston 13 continues to move upwards for a certain distance, the sample solution 4 with a specific volume is transferred into the first-stage auxiliary pipe 2 through the first through hole 21, and the sample solution 4 is directly collected by a pipettor from the inside of the first-stage auxiliary pipe 2.
Example 4
A sample pretreatment device capable of automatically identifying the liquid level height is different from the sample pretreatment device of the embodiment 3 as shown in figure 4:
(1) the two metal wire electrodes 12 are respectively positioned at two sides of the pipe wall of the main pipe 1 and can be contacted with the solution in the main pipe 1, one metal wire electrode 12 is inserted in the first through hole 21, the other metal wire electrode 12 is inserted in the side wall of the main pipe 1 opposite to the first through hole 21, and the lengths of the two metal wire electrodes 12 are both 10 mm;
(2) the inner diameter of the main pipe 1 is 4cm, the thickness of the bottom surface of the groove of the top cover 11 is 5mm, and 200mg of C18, 150mg of PSA and 50mg of graphitized carbon adsorbent are added into the inner plug 14.
Except for the above differences, the structures and the connection relationships of the remaining components are the same as those of embodiment 3.
The principle of use of this embodiment is the same as embodiment 3.
Example 5
A sample pretreatment method adopts the sample pretreatment device capable of automatically identifying the liquid level height in the embodiment 1, and comprises the following steps of extraction, purification and liquid transfer:
(1) adding 10g of homogenized corn sample into a main pipe 1 containing 6g of anhydrous magnesium sulfate and 1.5g of sodium acetate, adding 10ml of acetonitrile extraction solution into the main pipe 1, covering a top cover 11, and then oscillating and mixing to extract effective components in the corn sample;
(2) the motor drives the piston 13 at the bottom of the main pipe 1 to move from bottom to top, and drives the solution in the main pipe 1 to rise to meet the electrodes 12 (two metal wires); at the moment, the two independent metal wires are conducted by the conductive solution, so that an external sensor receives a signal, senses the upper liquid level position of the solution and identifies the identification of the initial liquid level height;
(3) the control system starts to send a command to the motor, the driving piston 13 is stopped after rising to a certain distance, and the lower end of the metal wire is flush with the lower edge of the through hole, so that Xml of sample solution 4 with a specific volume can be transferred to the primary attached pipe 2 (filled with 100mg of C18, 100mg of PSA and 50mg of graphitized carbon adsorbent) through the first through hole 21 (filtered by the first sieve plate 22);
(4) the draw solution flowing into the first-stage appendage 2 is purified by the adsorbent therein in the oscillation mode of operation. Then, the motor drives the plug 23 on the upper part of the first-stage attached tube 2 to move from top to bottom, drives the liquid in the first-stage attached tube 2 to flow into the second-stage attached tube 3 through the second through hole 31 between the first-stage attached tube 2 and the second-stage attached tube 3, and flows into the second-stage attached tube 3 after being filtered by the second sieve plate 32 and the filter membrane (because the lower edge of the second through hole 31 is flush with the bottom of the second-stage attached tube 3, Xml of sample solution 4 with a specific volume can flow into the second-stage attached tube.
Example 6
A sample pretreatment method adopts the sample pretreatment device capable of automatically identifying the liquid level height in the embodiment 3, and comprises the following steps of extraction, purification and liquid transfer:
(5) adding 10g of homogenized Chinese cabbage sample into a main pipe 1 containing 6g of anhydrous magnesium sulfate and 1.5g of sodium acetate, adding 10ml of acetonitrile extraction solution into the main pipe 1, covering a top cover 11, and then oscillating and mixing to extract effective components in the Chinese cabbage sample;
(6) the motor drives the piston 13 at the bottom of the main pipe 1 to move from bottom to top, the solution in the main pipe 1 is driven to pass through the adsorbents (300mg C18, 100mg PSA and 100mg graphitized carbon adsorbents) in the inner plug 14 at the upper part of the main pipe 1 for purification, and the solution meets the electrode 12 (two metal wires) when rising to the upper surface of the inner plug 14; at the moment, the two independent metal wires are conducted by the conductive solution, so that an external sensor receives a signal, senses the upper liquid level position of the solution and identifies the identification of the initial liquid level height;
(7) the control system starts to send a command to the motor, the driving piston 13 is stopped after rising to a certain distance, and the lower end of the metal wire is flush with the lower edge of the through hole, so that sample solution 4 with a specific volume of Xml can be transferred into the first-stage auxiliary pipe 2 through the first through hole 21 (filtered by the first sieve plate 22), and the moving of the Xml with a fixed volume is realized.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and the like that are within the spirit and principle of the present invention are included in the present invention.
Claims (15)
1. A sample pretreatment device capable of automatically identifying liquid level height is characterized by comprising a main pipe (1) and one or more auxiliary pipes connected with the main pipe (1) in parallel, through holes are formed between the adjacent main pipe (1) and the auxiliary pipes and between the auxiliary pipes, the bottom of the main pipe (1) is connected with a driving piece for driving the bottom to move up and down, and the upper end of the main pipe (1) is connected with a detection piece for identifying liquid level height;
optionally, the main tube (1) is filled with an extracting solution.
2. The sample pretreatment device according to claim 1, wherein an adsorbent is filled in the main tube (1) and/or the accessory tube, and a filter member for preventing the adsorbent from passing through is provided in the through hole between the accessory tube and the accessory tube;
optionally, a filter piece for preventing the adsorbent from passing through is arranged on the through hole between the main pipe (1) and the auxiliary pipe.
3. The sample pretreatment apparatus according to claim 1, wherein a bottom height of the probe is flush with a bottom height of the through hole.
4. The sample pretreatment device according to claim 1, wherein the main tube (1) and the auxiliary tube are both hollow columnar structures with sealed bottoms, and the hollow columnar structures comprise any one of a cylindrical structure, a triangular column structure, a square column structure or a pentagonal column structure;
preferably, the main pipe (1) is a hollow cylindrical structure, the height is 0.1-3cm, and the inner diameter is 1-5 cm;
preferably, the auxiliary pipe is of a hollow square columnar structure, and the side length is 1-5 cm;
preferably, the main pipe (1) and the auxiliary pipes are made of polypropylene, polyethylene, polyformaldehyde, polyvinyl chloride, polystyrene, metal, graphite or a mixture of the materials in any proportion.
5. The sample pretreatment device according to claim 1, wherein a top cover (11) is detachably connected to the top of the main pipe (1), and the detector is arranged on the top cover (11) in a penetrating manner;
preferably, the detector elements are arranged on opposite sides of the wall of the main pipe (1).
6. The sample pretreatment device according to claim 5, wherein the detecting member comprises two electrodes (12) arranged in parallel, and the two electrodes (12) are connected with a sensor capable of sensing the liquid level;
preferably, the electrode (12) is made of a conductive material, and further preferably made of metal or metal alloy;
preferably, the sensor is a capacitive sensor.
7. The sample pretreatment device according to claim 5, wherein a detachable inner plug (14) is arranged below the top cover (11), and at least two layers of filter elements are arranged in the inner plug (14) and are in sealing connection with the inner plug; optionally, an adsorbent is packed between the two filter layers.
8. The sample pretreatment apparatus according to claim 1, wherein a particle diameter of the adsorbent is 5 to 100 μm;
preferably, the adsorbent is one or more of anhydrous sodium sulfate, anhydrous magnesium sulfate, sodium acetate, sodium chloride, C18 bonded silica gel, graphitized carbon, N-propyl ethylenediamine bonded silica gel or polystyrene divinylbenzene high polymer.
9. The sample pretreatment apparatus according to claim 1, wherein the filter member is a sieve plate and/or a filter membrane;
preferably, the aperture of the sieve plate is 0.22-20 μm, and the thickness is 0.5-5 mm;
preferably, the pore size of the filter membrane is 0.2-1 μm;
preferably, the sieve plate and the filter membrane are made of one or more of polytetrafluoroethylene, polypropylene, polyether sulfone, nylon or polyvinylidene fluoride.
10. The sample pretreatment device according to claim 1, wherein the driving member is a piston (13), and the piston (13) is connected with the inner wall of the main pipe (1) in a sealing and sliding manner;
preferably, the piston (13) is made of polypropylene, polyethylene, polyformaldehyde, polyvinyl chloride, polystyrene, metal, graphite or a mixture of the materials in any proportion.
11. The sample pretreatment device according to claim 1, wherein the sample pretreatment device is mainly composed of a main tube (1) and an accessory tube connected in parallel, the through hole is close to the top end of the accessory tube, and the adsorbent is filled in the cavity of the main tube (1) and/or the inner plug (14).
12. The apparatus for pretreating sample according to claim 1, wherein when the main tube (1) and the two auxiliary tubes are connected in parallel, the through hole between the main tube (1) and the auxiliary tubes is close to the top end of the auxiliary tubes, the through hole between the auxiliary tubes is close to the bottom end of the auxiliary tubes, and the adsorbent is filled in the cavity of the auxiliary tubes close to the main tube (1).
13. The sample pretreatment apparatus according to claim 1, wherein the extraction liquid is a mixed solution of acetonitrile and water at an arbitrary ratio.
14. A sample processing apparatus, characterized in that the apparatus comprises a sample pre-processing apparatus for automatically identifying a liquid level according to any one of claims 1 to 13.
15. A method for pretreating a sample, comprising the step of pretreating the sample by using the sample pretreatment apparatus for automatically identifying a liquid level according to any one of claims 1 to 13 or the sample pretreatment apparatus according to claim 14.
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