阅读说明：本技术 一种有机物固相萃取组合装置 (Organic matter solid phase extraction composite set ) 是由 戴媛媛 高燕 王宏 董玉波 张雪 张晶伟 刘克奉 于 2019-09-04 设计创作，主要内容包括：本发明涉及一种有机物固相萃取组合装置,包括萃取柱、固定盖板、储液密封缸以及上样注射器,所述储液密封缸上设多个萃取柱,所述多个萃取柱共同扣装有一固定盖板,固定盖板外圈上制有环状注射凹槽,固定盖板的侧壁上均固装有限位块,所述固定盖板上表面中部通过轴承同轴安装上样注射器,所述上样注射器下部一侧连通设置有出液管,所述出液管端部置于环状注射凹槽内,所述出液管侧壁上固装一扇形限位指针板,所述扇形指针板的端部还铰装一限位卡扣,所述限位卡扣与固定盖板侧壁上限位块相适配。本发明通过旋转上样注射器,带动出液管在环状注射凹槽内旋转,与每个萃取柱完成对接连通实现定位定量上样,无需重复吸样上样,操作方便、节省人力。(The invention relates to an organic matter solid-phase extraction combination device which comprises extraction columns, a fixed cover plate, a liquid storage sealed cylinder and a sample loading injector, wherein a plurality of extraction columns are arranged on the liquid storage sealed cylinder, the extraction columns are jointly buckled with the fixed cover plate, an annular injection groove is formed in the outer ring of the fixed cover plate, limit blocks are fixedly arranged on the side wall of the fixed cover plate, the sample loading injector is coaxially arranged in the middle of the upper surface of the fixed cover plate through a bearing, a liquid outlet pipe is communicated with one side of the lower part of the sample loading injector, the end part of the liquid outlet pipe is arranged in the annular injection groove, a fan-shaped limit pointer plate is fixedly arranged on the side wall of the liquid outlet pipe, a limit buckle is hinged to the end part of the fan-shaped pointer plate, and the limit buckle is matched. According to the invention, the liquid outlet pipe is driven to rotate in the annular injection groove by rotating the sample loading injector, and is in butt joint communication with each extraction column to realize positioning and quantitative sample loading, repeated sample suction and sample loading are not required, the operation is convenient, and the labor is saved.)

1. The utility model provides an organic matter solid phase extraction composite set which characterized in that: the sampling device comprises extraction columns, a fixed cover plate, a liquid storage sealing cylinder and a sampling injector, wherein a plurality of extraction columns are arranged on the outer circumference of the upper surface of the liquid storage sealing cylinder at equal intervals through small column shafts, the middle part of the upper surface of the liquid storage sealing cylinder is coaxially provided with a fixed column, a fixed cover plate is jointly installed on the top ends of the extraction columns through the fixed column, an annular injection groove is integrally formed on the upper surface of the fixed cover plate at a circumferential position corresponding to the plurality of extraction columns in a surrounding mode, a plurality of injection liquid inlets are arranged in the annular injection groove at equal intervals, the injection liquid inlets are fixedly clamped with column ports at the top ends of the extraction columns, limiting blocks with the same number as that of the injection liquid inlets are fixedly installed on the side wall of the fixed cover plate at positions corresponding to the injection liquid inlets in a radial outward mode, the middle part of the upper surface of the fixed cover plate is coaxially provided with the sampling injector through a bearing, one side of the, the end part of the liquid outlet pipe is arranged in the annular injection groove, a fan-shaped limiting pointer plate is fixedly arranged on the side wall of the liquid outlet pipe close to the upper surface of the notch of the annular injection groove, a limiting buckle is further hinged to the end part of the fan-shaped pointer plate, the limiting buckle is matched with a limiting block on the side wall of the fixed cover plate, the liquid outlet pipe is driven to rotate in the annular injection groove by a rotary sample loading injector, and the rotary sample loading injector is in butt joint communication with each extraction column to realize positioning and quantitative sample loading.

2. The organic solid-phase extraction assembly device of claim 1, wherein: the liquid outlet pipe is an inclined L-shaped liquid outlet pipe, and a sealing ring is further arranged at the liquid outlet of the liquid outlet pipe.

3. The organic solid-phase extraction assembly device of claim 2, wherein: the inclination angle of the liquid outlet pipe is 15-30 degrees.

4. The organic solid-phase extraction assembly device of claim 1, wherein: the liquid storage sealing cylinder comprises an upper cover and a shell to form a closed whole, the shell is cylindrical, the upper cover is detachably and hermetically mounted at the top end of the shell, a plurality of small cylindrical shafts are arranged on the outer circumference of the upper cover at equal intervals, and the small cylindrical shafts are of a through tubular structure, are communicated with the inside of the shell and are used for inserting the solid-phase extraction column.

5. The organic solid-phase extraction assembly device of claim 1, wherein: a plurality of support columns are installed between the fixed cover plate at the outer ring position of the extraction column and the upper cover of the liquid storage sealing cylinder at intervals.

6. The organic solid-phase extraction assembly device of claim 1, wherein: the extraction column comprises a column opening, a column body and a sieve plate, the column opening is positioned at the upper end of the column body, a connecting piece is further embedded in the column opening, the lower part of the column body is filled with a filler, the sieve plate is positioned at the lower part of the filler at the lower end of the column body and is made of polypropylene or glass fiber, and a valve is further arranged on the column body at the lower part of the sieve plate.

7. The organic solid-phase extraction assembly device of claim 6, wherein: the filler is specially treated silica gel filler.

8. The organic solid-phase extraction assembly device of claim 6, wherein: the column mouth position of extraction column still can coaxial inlay the rubber buffer, the cock body external diameter of rubber buffer is unanimous with the internal diameter of extraction column.

9. The organic solid-phase extraction assembly device of claim 1, wherein: the solid phase extraction combination device also comprises a liquid collecting bottle and a vacuum pump, wherein the liquid collecting bottle is provided with two communicating holes, one communicating hole is connected with the liquid storage sealed cylinder, and the other communicating hole is communicated with the vacuum pump.

Technical Field

The invention belongs to the technical field of analytical chemistry sample pretreatment, relates to a solid phase extraction device, and particularly relates to an organic matter solid phase extraction combination device.

Background

Organic matter is the material basis for life production, and all living organisms contain organic compounds. Organic substances are various and can be divided into hydrocarbons and hydrocarbon derivatives. Metabolism in the body of an organism and genetic phenomena in the organism are involved in the conversion of organic compounds. Solid Phase Extraction (SPE) is to adsorb organic compounds in liquid sample by using solid adsorbent, separate the organic compounds from the matrix and interfering compounds of the sample, and then elute or heat-desorb the organic compounds by using eluent to achieve the purpose of separating and enriching the organic compounds. Solid phase extraction generally involves four steps. Activating, removing impurities in the solid phase extraction column and creating a certain solvent environment; loading, dissolving the sample with a certain solvent, transferring and retaining the components on the solid phase extraction column; leaching to remove interferents to the maximum extent; eluting, eluting the tested substance with small volume of solvent, and collecting. On the technical condition basis of current solid phase extraction, still there are many weak points in convenience and functionality that use, most solid phase extraction device complex operation, relatively consumption time, can't independently accomplish alone, influence work efficiency, the inconvenient use of adjusting of extraction device simultaneously, can't carry out accurate control to the environment of extraction, lead to the extraction quality to descend, it is very inconvenient, wherein advance kind process operation heavy and complicated, if can only artifical a bit will wait that the extract moves to the extraction post and absorb the appearance a little, waste time and energy, the inefficiency, and the volume of transferring at every turn is different, and advance the appearance and all need the ration to inhale the appearance and again the appearance of getting into the appearance at every turn.

The following patent documents related to the present application were found by search, and the contents thereof are as follows:

1. the utility model provides an autoinjection solid phase extraction device (CN209049057U), includes extraction post and autoinjection subassembly, the autoinjection subassembly includes communicating pipe and the holding piece that is used for the holding to treat the extract, the holding piece is installed in the top of extraction post, communicating pipe intercommunication holding piece and extraction post.

2. A solid phase extraction liquid filler (CN209148617U) comprises a sample liquid injector, a plurality of three-way pipe joints which are sequentially communicated in series and a plurality of branch injection pipes which are in one-to-one correspondence with the three-way pipe joints, wherein a needle head of the sample liquid injector is coaxially provided with a bolt, the bolt is in threaded sealing connection with an inlet of the three-way pipe joint at the front end, an outlet of the three-way pipe joint at the tail end is sealed, a liquid outlet of the sample liquid injector is communicated with a main pipe of each three-way pipe joint to form a main infusion passage, a branch pipe of each three-way pipe joint is communicated with the corresponding branch injection pipe through a pipeline to form an infusion branch passage, a vent hole is arranged on the branch injection pipe and close to the liquid inlet of the branch injection pipe, a column head which is matched with a solid phase extraction small column is arranged at the liquid outlet, the column cap is internally provided with a through hole for communicating the branch injection tube with the solid phase extraction small column.

3. A novel solid phase extraction device (CN208678438U) comprises a cylinder body, a lower bracket, an upper bracket, a centrifuge tube, an upper cover, support legs, an evacuated rubber tube, a cannula head, an SPE column, a plug and a pressure gauge; a lower support and an upper support are arranged in the cylinder body, a plurality of centrifuge tubes are inserted into the lower support and the upper support, the centrifuge tubes are common 10ml centrifuge tubes with round bottoms or pointed bottoms, and the top of the centrifuge tubes is provided with a threaded screw cap which can be freely taken down and used for hermetically storing samples; the cylinder body on be provided with the upper cover, the bottom of upper cover is provided with the stabilizer blade, is provided with on the upper cover and manages to find time rubber tube, a plurality of cannula head and manometer, insert in the cannula head and be equipped with SPE post or end cap.

Through comparison of technical features, the technical structures of the above-mentioned patent publications and the present invention are different, and the creativity and novelty of the present invention application are not affected.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provide a novel solid phase extraction combined device, which purifies a target object by utilizing the difference of the adsorbed capacities of analytes in different media, effectively separates the target object from interferents and greatly enhances the detection capacity of the analytes, particularly trace analytes. Effectively improves the solid phase extraction recovery rate, has outstanding high selectivity and high sensitivity, and overcomes the defects of low selectivity and poor flexibility of the solid phase extraction.

The technical problem to be solved by the invention is realized by adopting the following technical scheme:

an organic solid-phase extraction combination device comprises extraction columns, a fixed cover plate, a liquid storage sealing cylinder and a sample loading injector, wherein a plurality of extraction columns are arranged on the outer circumference of the upper surface of the liquid storage sealing cylinder at equal intervals through small column shafts, a fixed column is coaxially arranged in the middle of the upper surface of the liquid storage sealing cylinder, a fixed cover plate is jointly installed at the top ends of the extraction columns through the fixed column, an annular injection groove is integrally formed in the upper surface of the fixed cover plate corresponding to a circumferential position formed by surrounding the extraction columns, a plurality of injection liquid inlets are arranged in the annular injection groove at equal intervals, the injection liquid inlets are fixedly clamped with column ports at the top ends of the extraction columns, limiting blocks with the same number as that of the injection liquid inlets are fixedly installed on the side wall of the fixed cover plate corresponding to each injection liquid inlet radially outwards, and the sample loading injector is coaxially installed in the middle of the upper surface of the fixed cover plate through a bearing, the sample loading injector is characterized in that an inclined liquid outlet pipe is communicated with one side of the lower portion of the sample loading injector, the end of the liquid outlet pipe is arranged in the annular injection groove, a fan-shaped limiting pointer plate is fixedly installed on the side wall of the liquid outlet pipe close to the upper surface of the notch of the annular injection groove, a limiting buckle is hinged to the end of the fan-shaped pointer plate, the limiting buckle is matched with a limiting block on the side wall of the fixed cover plate, the sample loading injector is rotated to drive the liquid outlet pipe to rotate in the annular injection groove, and the sample loading injector is in butt joint communication with each extraction column to achieve positioning and.

Moreover, the liquid outlet pipe is an inclined L-shaped liquid outlet pipe, and a sealing ring is further arranged at the liquid outlet of the liquid outlet pipe.

Moreover, the inclination angle of the liquid outlet pipe is 15-30 degrees.

And the liquid storage sealing cylinder comprises an upper cover and a shell to form a closed whole, the shell is cylindrical, the upper cover is detachably and hermetically arranged at the top end of the shell, a plurality of small cylindrical shafts are arranged on the outer circumference of the upper cover at equal intervals, and the small cylindrical shafts are of a through tubular structure, are communicated with the inside of the shell and are used for inserting the solid-phase extraction column.

And a plurality of support columns are arranged between the fixed cover plate at the outer ring position of the extraction column and the upper cover of the liquid storage sealing cylinder at intervals.

And the extraction column comprises a column opening, a column body and a sieve plate, wherein the column opening is positioned at the upper end of the column body, a connecting piece is embedded in the column opening, the lower part of the column body is filled with a filler, the sieve plate is positioned at the lower part of the filler at the lower end of the column body and is made of polypropylene or glass fiber, and the column body at the lower part of the sieve plate is also provided with a valve.

Moreover, the filler is specially treated silica gel filler.

And the position of the column port of the extraction column can be coaxially embedded with a rubber plug, and the outer diameter of the plug body of the rubber plug is consistent with the inner diameter of the extraction column.

And the solid phase extraction combination device also comprises a liquid collecting bottle and a vacuum pump, wherein the liquid collecting bottle is provided with two communicating holes, one communicating hole is connected with the liquid storage sealed cylinder, and the other communicating hole is communicated with the vacuum pump.

The invention has the advantages and positive effects that:

1. the sample feeding device is novel in structure and simple to operate, the sample feeding injector is rotated to drive the liquid outlet pipe to rotate in the annular injection groove, the liquid outlet pipe is in butt joint communication with each extraction column to achieve quantitative sample feeding, and the limit buckle at the end of the fan-shaped pointer plate is in fit connection with the limit block on the side wall of the fixed cover plate to achieve rotary positioning, so that the purpose of one-time sample suction, multiple rotary positioning and quantitative sample feeding is achieved, the sample feeding efficiency is greatly improved, and manpower is saved.

2. The extraction column and the filler are designed integrally, the stability is good, the extraction column can be matched with corresponding elution solvents, different samples can be treated respectively, and the selectivity is strong.

Drawings

FIG. 1 is a schematic structural view of the present invention;

FIG. 2 is a schematic view of a loading syringe according to the present invention;

FIG. 3 is a schematic view of the structure of the extraction column of the present invention.

Detailed Description

The present invention will be described in further detail with reference to the following embodiments, which are illustrative only and not limiting, and the scope of the present invention is not limited thereby.

An organic solid-phase extraction combination device comprises extraction columns 13, a fixed cover plate 5, a liquid storage sealed cylinder 9 and a sampling injector 1, wherein a plurality of extraction columns are arranged on the outer circumference of the upper surface of the liquid storage sealed cylinder at equal intervals through small column shafts 11, a fixed column is coaxially arranged in the middle of the upper surface of the liquid storage sealed cylinder, a fixed cover plate is jointly installed on the top ends of the extraction columns through the fixed column, an annular injection groove 3 is integrally formed in the upper surface of the fixed cover plate corresponding to a circumferential position formed by enclosing the extraction columns, a plurality of injection ports are arranged in the annular injection groove at equal intervals, the injection ports are communicated with column ports at the top ends of the extraction columns, limiting blocks 6 with the same number as that of injection ports are fixedly installed on the side wall of the fixed cover plate corresponding to each injection port radially outwards, and the sampling injector is coaxially installed in the middle of the upper surface of the fixed cover plate through a bearing 2, an inclined liquid outlet pipe 17 is communicated with one side of the lower portion of the sample loading injector, the end portion of the liquid outlet pipe is arranged in the annular injection groove, a fan-shaped limiting pointer plate 16 is fixedly installed on the side wall, close to the upper surface of the notch of the annular injection groove, of the liquid outlet pipe, a limiting buckle 15 is hinged to the end portion of the fan-shaped pointer plate, the limiting buckle is matched with a limiting block on the side wall of the fixed cover plate, sample loading in a positioning mode is achieved, the sample loading injector is rotated to drive the liquid outlet pipe to rotate in the annular injection groove and can be communicated with each extraction column in a butt joint mode, and therefore sample loading in a positioning and quantifying mode can be achieved.

The sample loading injector comprises an injector body, a liquid outlet pipe, a fan-shaped limiting pointer plate and a limiting buckle, wherein the injector body is composed of a piston shaft 18 and a cylinder 19, scales are arranged on the cylinder, the piston shaft is coaxially and slidably mounted in the cylinder, one side of an end pipe at the lower end of the cylinder is integrally provided with the liquid outlet pipe, the liquid outlet pipe is an inclined L-shaped liquid outlet pipe, a sealing ring is further arranged at the liquid outlet of the liquid outlet pipe with the inclination angle of 15-30 degrees to realize better sealing and butt joint communication with an injection liquid inlet, in order to enable the sample loading injector to realize positioning, rotating and sample loading, the side wall of the liquid outlet pipe is further horizontally and fixedly provided with the fan-shaped limiting pointer plate, and one end of the fan-shaped limiting pointer plate is hinged with the buckle matched with a limiting block.

The liquid storage sealing cylinder comprises an upper cover 10 and a shell to form a closed whole, the shell is cylindrical, the upper cover is detachably and hermetically mounted at the top end of the shell, a plurality of small cylindrical shafts are arranged on the outer circumference of the upper cover at equal intervals, and the small cylindrical shafts are of a through tubular structure, are communicated with the inside of the shell and are used for inserting the solid-phase extraction column.

In the specific implementation of the invention, in order to enable the fixed cover plate to better fix the extraction column, a plurality of support columns 14 are installed at intervals between the fixed cover plate at the outer ring position of the extraction column and the upper cover of the liquid storage sealing cylinder.

In the specific implementation of the invention, the extraction column comprises a column mouth, a column body 20 and a sieve plate 22, the column mouth is positioned at the upper end of the column body, a connecting piece 23 is embedded in the column mouth to enable the liquid outlet pipe and the extraction column to be better communicated and connected, the lower part of the column body is filled with a filler 21, the filler is a silica gel filler subjected to special treatment, the sieve plate is positioned at the lower part of the filler at the lower end of the column body and is made of polypropylene or glass fiber, the column body at the lower part of the sieve plate is also provided with a valve 12, the valve is opened, liquid in the column body flows out and enters a liquid storage sealed cylinder, the valve is closed, and the liquid in the column body.

In the specific implementation of the invention, a rubber plug 4 can be coaxially embedded at the position of the column port of the extraction column, and the outer diameter of the plug body of the rubber plug is consistent with the inner diameter of the extraction column.

In the specific implementation of the invention, the solid phase extraction combination device further comprises a liquid collecting bottle 7 and a vacuum pump 8, wherein the liquid collecting bottle is provided with two communicating holes, one of the two communicating holes is connected with the liquid storage sealed cylinder, and the other communicating hole is communicated with the vacuum pump.

In the specific implementation of the invention, the extraction column is a polyethylene syringe type.

During operation, firstly filling materials into an extraction column according to liquid to be extracted, then covering a rubber plug, pulling a piston shaft of a sample injector, filling the cylinder of the sample injector with the liquid to be extracted, installing the sample injector, placing a liquid outlet end of a liquid outlet pipe of the sample injector in an annular injection groove, then pulling out a piston arranged on an injection liquid inlet, clockwise rotating the sample injector to drive the liquid outlet pipe to rotate in the annular injection groove, matching and limiting a buckle of the sample injector with a limiting block when the sample injector rotates to the position of a first extraction column, butt-jointing the liquid outlet pipe of the sample injector and the extraction column at the moment, then pressing the piston shaft of the sample injector downwards for sampling for a certain distance, and rotating the sample injector until the position of a next extraction column is fixed after sampling, simultaneously, the rubber plug is used for sealing and plugging the first extraction column which has finished sampling, the column body of the extraction column is in a sealing state at the moment, the later sampling step is the same as the above step, the descending distance of the piston shaft is the same every time, so that the positioning and quantitative sampling of each extraction column is realized, when extraction is needed, the vacuum pump is started, negative pressure is generated in the liquid collecting bottle, and extraction liquid is absorbed from the liquid storage sealing cylinder, the connecting hole communicated with the liquid storage sealing cylinder on the liquid collecting bottle is positioned at the lower part of the liquid collecting bottle, the communicating hole communicated with the vacuum pump is positioned at the upper part of the liquid collecting bottle, and the extraction liquid is collected by utilizing the principle of an upward air.

The sample feeding device is novel in structure and simple to operate, the sample feeding injector is rotated to drive the liquid outlet pipe to rotate in the annular injection groove, the liquid outlet pipe is in butt joint communication with each extraction column to achieve quantitative sample feeding, and the limit buckle at the end of the fan-shaped pointer plate is in fit connection with the limit block on the side wall of the fixed cover plate to achieve rotary positioning, so that the purpose of one-time sample suction, multiple rotary positioning and quantitative sample feeding is achieved, the sample feeding efficiency is greatly improved, and manpower is saved.

The extraction column and the filler are designed integrally, the stability is good, the extraction column can be matched with corresponding elution solvents, different samples can be treated respectively, and the selectivity is strong.

Although the embodiments of the present invention and the accompanying drawings are disclosed for illustrative purposes, those skilled in the art will appreciate that: various substitutions, changes and modifications are possible without departing from the spirit and scope of the invention and the appended claims, and therefore the scope of the invention is not limited to the disclosure of the embodiments and the accompanying drawings.