CN113813647A - Pre-compression solid phase extraction column tube with adjustable compression amount and use method thereof - Google Patents
Pre-compression solid phase extraction column tube with adjustable compression amount and use method thereof Download PDFInfo
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- CN113813647A CN113813647A CN202111006979.XA CN202111006979A CN113813647A CN 113813647 A CN113813647 A CN 113813647A CN 202111006979 A CN202111006979 A CN 202111006979A CN 113813647 A CN113813647 A CN 113813647A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/22—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the construction of the column
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Abstract
The invention discloses a precompression type solid phase extraction column tube with adjustable compression amount and a using method thereof. This precompression type solid phase extraction column tube, including spiral cover, the column tube, the piston device inside spiral cover and column tube is located to the cover, spiral cover and column tube pass through threaded connection, the spiral cover center is provided with the round hole, piston device includes the piston main part and sets up in the cylinder section of piston main part upper end, be provided with whole post column bed in the column tube, whole post column bed bottom is provided with down the sieve, the top is provided with the sieve, go up the sieve top and be connected with the bottom of piston main part, the round hole that the cylinder section passed the spiral cover sets up in the spiral cover top, cylinder section top is provided with the first luer joint that is used for connecting the syringe, the inside through-hole that supplies the liquid circulation that is provided with of piston main part. The precompression type solid phase extraction column tube with adjustable compression amount provided by the invention can overcome the problem of shrinkage of an elastic monolithic column bed to a certain extent by using a mechanical space compensation method, and expands the selection and application range of monolithic column materials.
Description
The technical field is as follows:
the invention relates to the technical field of solid phase extraction, in particular to a precompression type solid phase extraction column tube with adjustable compression amount and a using method thereof.
Background art:
the monolithic column is a novel porous separation and enrichment material and can be widely applied to the packing of solid-phase extraction columns and chromatographic separation columns. The monolithic column has a connected three-dimensional reticular microstructure, when in-situ polymerization is completed, liquid substances (generally called pore-forming agents) which do not participate in polymerization reaction in the raw material mixture are filled in network pores inside the monolithic column, and the pore-forming agents need to be washed out by solvents such as acetonitrile, methanol, isopropanol and the like in the following preparation process, so that the usable monolithic column can be prepared. The materials comprising the monolithic column network may have different stiffness and elasticity. When the rigidity of the monolithic column material is higher and the solvent in the gaps is volatilized, the monolithic column material can still maintain the three-dimensional reticular structure and dimension, and the performance and the use effect of the monolithic column are not influenced; and some materials have better elasticity, the integral column prepared can maintain complete shape and dimension when the integral column is filled with the solvent, when the solvent is lost or volatilized, the inside of a pore can deform due to lack of support, the whole column bed structure can shrink, the collapse of a space structure can occur to a certain degree, disordered local cracking or separation from a column tube is caused, the whole column can be scrapped, and the integral column can not be used as a stationary phase of liquid chromatography or solid phase extraction. This phenomenon limits the use of some elastomeric materials as monolithic column materials. In order to solve the problem, the research and application fields at home and abroad mainly adopt a mode of preventing the solvent of the monolithic column bed from volatilizing as much as possible, such as plugging two ends of the monolithic column or soaking the monolithic column in the solvent to prevent drying. These measures, although effective to some extent, still have inconveniences.
The invention content is as follows:
the invention provides a precompression type solid phase extraction column tube with adjustable compression amount and a using method thereof, which aim to solve the problems in the prior art.
The invention aims to provide a precompression type solid phase extraction column tube with adjustable compression amount, which comprises a screw cap, a column tube and a piston device sleeved inside the screw cap and the column tube, wherein the screw cap is connected with the column tube through threads, a round hole is formed in the center of the screw cap, the piston device comprises a piston main body and a cylindrical section arranged at the upper end of the piston main body, an integral column bed is arranged in the column tube, a lower sieve plate is arranged at the bottom of the integral column bed, an upper sieve plate is arranged at the top of the integral column bed, the top of the upper sieve plate is connected with the bottom of the piston main body, the cylindrical section penetrates through the round hole of the screw cap and is arranged at the top end of the screw cap, a first Ruhr joint used for connecting an injector is arranged at the top of the cylindrical section, and a through hole for liquid circulation is formed in the piston main body. The column tube provided by the invention is a cylindrical column tube.
The invention discloses a precompression type solid phase extraction column tube with adjustable compression amount, which solves the problem that the prior copolymer monolithic column is easy to crack, influences the characteristics and the application of the monolithic column, and can compensate the removal of a pore-forming agent from the monolithic column and the column bed shrinkage in the column bed drying process and prevent the column bed from cracking, separating and the like in order to adapt to the monolithic column with elasticity, besides adjusting polymerization parameters to increase the strength of the monolithic column structure and prevent the column bed from drying shrinkage. The mechanical space compensation method can overcome the problem of shrinkage of the elastic monolithic column bed to a certain extent, and expand the selection and application range of monolithic column materials.
The cylindrical monolithic column bed after polymerization is positioned at the bottom of the cylindrical column tube, and an upper sieve plate and a lower sieve plate made of porous sintered materials are respectively arranged above and below the cylindrical monolithic column bed to limit the positions of the upper sieve plate and the lower sieve plate; wherein the upper sieve plate at the upper end of the integral column bed is fixed at the bottom of the movable piston main body, a through hole for liquid circulation is arranged in the middle of the piston main body, and the piston main body is pressed downwards by a threaded screw cap at the top end.
The technical principle of the precompression type solid phase extraction column tube with adjustable compression amount provided by the invention is as follows: after the monolithic column prepared from the elastic material is polymerized, shrinkage and cracking may occur due to the loss of the support of the internal filling liquid due to the space network structure in the process of washing and removing the porogenic agent. If the column bed is gradually compressed inwards in one direction in the process of removing the pore-foaming agent, the compression amount is gradually increased along with the removal of the pore-foaming agent, so that the shrinkage phenomenon of the column bed can be orderly controlled in one direction, and the conditions of disordered internal gaps, cavities and separation from the tube wall are prevented.
Preferably, a spiral cover internal thread is arranged in the spiral cover, a pipe wall external thread is arranged on the outer wall of the column pipe, and the spiral cover and the column pipe are connected through the spiral cover internal thread and the pipe wall external thread. Lean on threaded connection between spiral cover and the column casing, and spiral cover internal thread and pipe wall external screw thread have certain surplus, can be in certain extent through rotatory spiral cover angle modulation spiral cover's height.
Preferably, the column tube outer wall be provided with the scale, the spiral cover on be provided with and be used for with the scale mark spiral cover the volume of precessing the scale pointer.
Preferably, the through hole is a tapered through hole. The piston main body is internally provided with a through hole through which liquid can flow, the lower part of the through hole is enlarged into a conical through hole, a circular sieve plate (an upper sieve plate) is clamped in the conical through hole at the bottom of the piston main body, and the upper sieve plate and the bottom edge of the piston main body form a plane.
Preferably, the bottom of the column tube is provided with a second luer connector connected with a line device or a vacuum auxiliary device. The solid phase extraction column prepared by the precompression type solid phase extraction column tube with the adjustable compression amount can be connected with a line device through a first luer connector or a second luer connector and used as an online solid phase extraction column, and the first luer connector at the upper end can be connected with an empty injector, and the second luer connector at the lower end can be connected with a vacuum auxiliary device and used as an offline solid phase extraction column.
Preferably, the lower end of the piston main body is provided with a sealing ring for sealing. The column tube is a hollow cylinder, the upper opening and the lower part are basically closed, and the lower outlet is in the specification of a luer connector. In a combined state, the cylindrical section at the upper part of the piston main body penetrates through a circular hole in the center of the spiral cover, the first Ruhr joint at the upper end of the cylindrical section extends out of the spiral cover, a sealing ring at the outer edge of the lower part of the piston main body forms interference fit with the inner wall of the column tube to realize sealing, the bottom edge of the piston main body and an upper sieve plate clamped at the bottom of the piston main body press the top end of the integral column bed together, and the lower part of the column bed is supported by a lower sieve plate.
Preferably, the piston body is a cylindrical piston body, and the diameter of the cylindrical section is smaller than that of the cylindrical piston body.
The invention also protects the application of the precompression type solid phase extraction column tube with adjustable compression amount in solid phase extraction. The specific application method of the precompression type solid phase extraction column tube with adjustable compression amount is as follows: when the integral column is prepared, the screw cap, the inner main pipe and the spring are taken down, the lower end of the outer column pipe is plugged by the luer plug, and the outer column pipe is vertically placed. Adding the prepared liquid polymerization monomer mixture into the outer column tube, sealing the upper end of the outer column tube by a sealing cover, and carrying out in-situ polymerization reaction at a certain temperature to prepare the integral column bed. After the polymerization reaction is completed, the sealing cover on the upper portion of the outer column tube is removed, the piston and the screw cap are mounted, the pipeline of the flushing agent tank or the infusion pump is connected to the first Ruhr connector at the upper end of the column tube, and the pipeline leading to the waste liquid tank is connected to the second Ruhr connector at the lower end of the column tube. In the process of washing and removing the pore-forming agent, the screwing amount of the screw cap can be gradually increased through a mechanical device or manually, the piston is compressed downwards to compensate the longitudinal shrinkage of the integral column bed until the preset scale is reached, then the screw cap is fixed by dispensing to prevent the continuous rotation of the integral column bed, and the two ends of the column tube can be sealed by using the sealing caps and the plugs which meet the standard of a luer connector to prevent the integral column bed from being completely dried. The elastic material solid phase extraction monolithic column prepared by the precompression type solid phase extraction column tube with the adjustable compression amount can be used for off-line solid phase extraction operation in the following mode: before use, the sealing caps and the end caps at two ends of the column tube are removed, a first luer connector at the upper end of the solid phase extraction column is connected with an empty syringe, a second luer connector at the lower end of the solid phase extraction column is connected with a vacuum auxiliary device, a certain volume of proper solvent is used for washing and activating the column bed, and then the loading, leaching and elution are carried out according to the operation mode of the conventional solid phase extraction column. The prepared elastic material solid phase extraction monolithic column can also be connected to an online solid phase extraction device through a first luer connector and a second luer connector for online solid phase extraction.
Compared with the prior art, the invention has the following advantages: the precompression type solid phase extraction column tube with adjustable compression amount can compensate the shrinkage of the whole column bed in the process of pore-forming agent removal and column bed drying, and prevent the column bed from cracking, separating from the column tube and the like so as to adapt to the elastic whole column. The mechanical space compensation method can overcome the problem of shrinkage of the elastic monolithic column bed to a certain extent, and expand the selection and application range of monolithic column materials.
Description of the drawings:
FIG. 1 is a schematic diagram of a pre-compression solid phase extraction column tube with adjustable compression according to the present invention;
FIG. 2 is a cross-sectional view of FIG. 1 taken in the longitudinal direction;
FIG. 3 is an exploded view of FIG. 1;
description of reference numerals: 1. screwing a cover; 2. a first luer fitting; 3. a cylindrical section; 4. a piston body; 5. a seal ring; 6. an upper sieve plate; 7. a monolithic column bed; 8. a lower sieve plate; 9. calibration; 10. a column tube; 11. a second luer fitting; 12. a scale pointer 13 and a screw cap internal thread; 14. and the pipe wall is externally threaded.
The specific implementation mode is as follows:
the technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood 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. The equipment and reagents used in the present invention are, unless otherwise specified, conventional commercial products in the art.
The pre-compression solid phase extraction column tube with adjustable compression amount consists of three parts, namely an upper screw cap 1, an inner piston device and a lower column tube 10. The screw cap 1 is connected with the column tube 10 through threads, and the threads have certain allowance, so that the height of the screw cap 1 can be adjusted through a rotation angle within a certain range. The screw cap 1 is marked with a pointer (pointer mark) which is used for marking the screw amount of the screw cap together with the scale on the outer wall of the column tube. The piston device is a whole, the upper part of the piston device is in a luer connector specification (first luer connector) capable of being connected with a syringe, a cylindrical section 3 with a smaller diameter is arranged downwards, then a cylindrical piston main body 4 is arranged downwards, the lower end of the piston main body 4 is provided with two raised sealing rings 5, a through hole through which liquid can flow is arranged in the piston main body 4, the lower part of the through hole is enlarged to be a tapered through hole, an upper sieve plate 6 is clamped in the tapered through hole at the bottom of the piston main body 4, and the upper sieve plate 6 and the bottom edge of the piston main body 4 form a plane. The column tube 10 is a hollow cylinder, the upper opening of which is substantially closed at the lower part, and the lower outlet of which is of luer fitting specification (second luer fitting). In a combined state, the cylindrical section 3 at the upper part of the piston main body 4 penetrates through a circular hole in the center of the screw cap 1, the first Ruhr joint 2 at the upper end of the cylindrical section extends out of the screw cap 1, the sealing ring 5 at the outer edge of the lower part of the piston main body 4 and the inner wall of the column tube 10 form interference fit to realize sealing, the bottom edge of the piston main body 4 and the upper sieve plate 6 clamped at the bottom of the piston main body 4 press the top end of the integral column bed 7 together, and the lower part of the integral column bed 7 is supported by the lower sieve plate 8.
In the precompression type solid phase extraction column tube with adjustable compression amount, a cylindrical monolithic column bed 7 after polymerization is positioned at the bottom of a cylindrical column tube 10, and an upper sieve plate 6 and a lower sieve plate 8 made of porous sintered materials are respectively arranged above and below the column bed to limit the positions of the column bed; wherein, the upper sieve plate 6 at the upper end of the integral column bed 7 is fixed at the bottom of the movable piston main body 4, a through hole for liquid circulation is arranged in the middle of the piston main body 4, and the piston main body 4 is pressed downwards by the threaded screw cap 1 at the top end; the screw cap 1 is matched with the column tube 10 through threads, the downward compression distance of the piston main body 4 can be adjusted through the number of turns of rotation, and the outer wall of the column tube 10 is provided with scales which can mark the screwing amount of the screw cap. When the whole column is washed, a line from a washing agent tank or a liquid transfer pump is connected to a first luer connector 2 at the upper end of the column tube, and a line leading to a waste liquid tank is connected to a second luer connector 11 at the lower end of the column tube. In the process of washing and removing the pore-forming agent, the screwing amount of the screw cap can be gradually increased through a machine or manually, the piston main body 4 is compressed downwards to compensate the longitudinal shrinkage of the integral column bed 7 until the preset scale is reached, then the screw cap 1 is fixed by dispensing to prevent the continuous rotation, and the two ends of the column tube can be sealed by using the sealing caps and the plugs which meet the standard of a luer connector to prevent the integral column bed from being completely dried.
Example 1
As shown in fig. 1-3, a precompression type solid phase extraction column tube of adjustable compression, including spiral cover 1, column tube 10, the piston device of spiral cover 1 and column tube 10 inside is located to the cover, spiral cover 1 and column tube 10 pass through threaded connection, spiral cover 1 center is provided with the round hole, piston device includes piston main part 4 and sets up in the cylinder section 3 of piston main part 4 upper end, be provided with whole post column bed 7 in the column tube 10, whole post column bed 7 bottom is provided with down sieve 8, the top is provided with sieve 6, the top of going up sieve 6 is connected with the bottom of piston main part 4, cylinder section 3 passes the round hole of spiral cover 1 and sets up in spiral cover 1 top, cylinder section 3 top is provided with the first luer 2 that is used for connecting the syringe, piston main part 4 inside is provided with the through-hole that supplies the liquid circulation.
In the present embodiment, the column tube 10 is preferably a cylindrical column tube, the piston body 4 is a cylindrical piston body, and the diameter of the cylindrical section 3 is smaller than that of the cylindrical piston body 4. The monolithic column bed is made of a porous monolithic material with certain elasticity. The cylindrical monolithic column bed 7 after polymerization is positioned at the bottom of the cylindrical column tube, and an upper sieve plate 6 and a lower sieve plate 8 which are made of porous sintered materials are respectively arranged above and below the cylindrical monolithic column bed to limit the positions of the cylindrical monolithic column bed and the cylindrical monolithic column bed; wherein, the upper sieve plate 6 at the upper end of the integral column bed 7 is fixed at the bottom of the movable piston main body 4, a through hole for liquid circulation is arranged in the middle of the piston main body 4, and the piston main body 4 is pressed downwards by a screw thread screw cap at the top end.
Be provided with spiral cover internal thread 13 in the spiral cover 1, the pillar pipe 10 outer wall is provided with pipe wall external screw thread 14, and spiral cover 1 and pillar pipe 10 are connected through spiral cover internal thread 13 and pipe wall external screw thread 14. Lean on threaded connection between spiral cover and the column casing, and spiral cover internal thread and pipe wall external screw thread have certain surplus, can be in certain extent through rotatory spiral cover angle modulation spiral cover's height.
The outer wall of the column tube 10 is provided with scales 9, and the spiral cover 1 is provided with a scale pointer 12 which is used for marking the spiral amount of the spiral cover together with the scales. In the present invention, the through-hole is preferably a tapered through-hole. The piston main body is internally provided with a through hole through which liquid can flow, the lower part of the through hole is enlarged into a conical through hole, a circular sieve plate (an upper sieve plate) is clamped in the conical through hole at the bottom of the piston main body, and the upper sieve plate and the bottom edge of the piston main body form a plane.
The bottom of the vial 10 is provided with a second luer fitting 11 for connection to a line or vacuum assist device. The precompression type solid phase extraction column tube with adjustable compression amount can be connected with a line device through a first luer connector 2 or a second luer connector 11 and used as an online solid phase extraction column, or the first luer connector 2 at the upper end can be connected with an empty injector, and the second luer connector 11 at the lower end can be connected with a vacuum auxiliary device and used as an offline solid phase extraction column.
In this embodiment, the column tube 10 is a hollow cylinder, the upper opening of which is substantially closed at the lower part, and the lower outlet of which is in the luer fitting specification. The lower end of the piston body 4 is provided with a sealing ring 5 for sealing. In a combined state, the cylindrical section 3 at the upper part of the piston main body 4 penetrates through a circular hole in the center of the screw cap 1, the first Ruhr joint 2 at the upper end of the cylindrical section extends out of the screw cap 1, the sealing ring 5 at the outer edge of the lower part of the piston main body 4 and the inner wall of the column tube 10 form interference fit to realize sealing, the bottom edge of the piston main body 4 and the upper sieve plate 6 clamped at the bottom of the piston main body 4 press the top end of the integral column bed 7 together, and the lower part of the integral column bed 7 is supported by the lower sieve plate 8.
The technical principle of the precompression type solid phase extraction column tube with adjustable compression amount provided by the invention is as follows: after the monolithic column prepared from the elastic material is polymerized, shrinkage and cracking may occur due to the loss of the support of the internal filling liquid due to the space network structure in the process of washing and removing the porogenic agent. If the column bed is gradually compressed inwards in one direction in the process of removing the pore-foaming agent, the compression amount is gradually increased along with the removal of the pore-foaming agent, so that the shrinkage phenomenon of the column bed can be orderly controlled in one direction, and the conditions of disordered internal gaps, cavities and separation from the tube wall are prevented.
The solid phase extraction monolithic column of the precompression type solid phase extraction column tube with adjustable compression amount can be connected with a line device through a luer connector and used as an online solid phase extraction column, and can also be connected with an empty injector at the upper end and connected with a vacuum auxiliary device at the lower end and used as an offline solid phase extraction column.
The above embodiments are only for the purpose of helping understanding the technical solution of the present invention and the core idea thereof, and it should be noted that those skilled in the art can make several improvements and modifications to the present invention without departing from the principle of the present invention, and these improvements and modifications also fall within the protection scope of the claims of the present invention.
Claims (8)
1. The utility model provides an adjustable precompression type solid phase extraction column tube of compression volume which characterized in that, includes spiral cover, column tube, the piston device of cover locating spiral cover and column tube inside, spiral cover and column tube pass through threaded connection, spiral cover center be provided with the round hole, the piston device include piston main part and set up in the cylinder section of piston main part upper end, the column tube in be provided with whole post column bed, whole post column bed bottom be provided with down the sieve, the top is provided with the sieve, last sieve top be connected with the bottom of piston main part, the round hole that the cylinder section passed the spiral cover sets up in the spiral cover top, cylinder section top be provided with the first luer joint who is used for connecting the syringe, piston main part inside be provided with the through-hole that supplies the liquid circulation.
2. The compression-adjustable precompression-type solid phase extraction column as claimed in claim 1, wherein the cap has internal screw threads and the outer wall of the column has external screw threads, and the cap and the column are connected via the internal screw threads.
3. The adjustable compression pre-compression solid phase extraction column of claim 1, wherein the column has a scale on its outer wall, and the screw cap has a scale pointer for indicating the screw amount of the screw cap together with the scale.
4. The adjustable compression pre-compressed solid phase extraction column of claim 1, wherein the through-hole is a tapered through-hole.
5. The adjustable compression pre-compressed solid phase extraction column of claim 1, wherein the bottom of the column is provided with a second luer fitting for connection to a wire or vacuum assist device.
6. The adjustable compression pre-compressed solid phase extraction column of claim 1, wherein the piston body is provided with a sealing ring at the lower end for sealing.
7. The adjustable compression pre-compression solid phase extraction column of claim 1, wherein the piston body is a cylindrical piston body and the diameter of the cylindrical section is less than the diameter of the cylindrical piston body.
8. Use of the adjustable compression precompression solid phase extraction column of claim 1 for solid phase extraction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111006979.XA CN113813647A (en) | 2021-08-30 | 2021-08-30 | Pre-compression solid phase extraction column tube with adjustable compression amount and use method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111006979.XA CN113813647A (en) | 2021-08-30 | 2021-08-30 | Pre-compression solid phase extraction column tube with adjustable compression amount and use method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113813647A true CN113813647A (en) | 2021-12-21 |
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ID=78913776
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111006979.XA Pending CN113813647A (en) | 2021-08-30 | 2021-08-30 | Pre-compression solid phase extraction column tube with adjustable compression amount and use method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113813647A (en) |
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2021
- 2021-08-30 CN CN202111006979.XA patent/CN113813647A/en active Pending
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