A pre-compressed solid-phase extraction column tube with adjustable compression amount and its usage method

Abstract

The present invention discloses a pre-compressed solid-phase extraction column tube with adjustable compression amount and its usage method. The pre-compressed solid-phase extraction column tube includes a screw cap, a column tube, and a piston device sleeved inside the screw cap and the column tube. The screw cap and the column tube are connected by threads. A round hole is provided at the center of the screw cap. The piston device includes a piston main body and a cylindrical section arranged at the upper end of the piston main body. An integral column bed is arranged inside the column tube. A lower sieve plate is arranged at the bottom of the integral column bed, and an upper sieve plate is arranged at the top. The top of the upper sieve plate is connected to the bottom of the piston main body. The cylindrical section passes through the round hole of the screw cap and is arranged at the top of the screw cap. A first Luer connector for connecting a syringe is arranged at the top of the cylindrical section. A through hole for liquid flow is arranged inside the piston main body. The pre-compressed solid-phase extraction column tube with adjustable compression amount proposed by the present invention can overcome the problem of shrinkage of the elastic integral column bed to a certain extent by using a mechanical space compensation method, and expand the selection and application range of integral column materials.

Description

Technical Field:

[0001] The present invention relates to the technical field of solid-phase extraction, and particularly relates to a pre-compressed solid-phase extraction column tube with adjustable compression amount and a using method thereof. Background Art:

[0002] The monolithic column is a new type of porous separation and enrichment material, which can be widely used as the filler of solid-phase extraction columns and chromatographic separation columns. The monolithic column has a connected three-dimensional network microstructure. When the in-situ polymerization is completed, the liquid substances (usually called porogens) that do not participate in the polymerization reaction in the raw material mixture are filled in the internal network pores of the monolithic column. In the subsequent preparation process, solvents such as acetonitrile, methanol, and isopropanol are required to wash out the porogens before a usable monolithic column can be made. The materials constituting the network structure of the monolithic column may have different hardnesses and elasticities. When the monolithic column material has a high rigidity, after the solvent in the voids volatilizes, the monolithic column material can still maintain the three-dimensional network structure and scale, without affecting the performance and use effect of the monolithic column; while some materials have good stretchability, and the monolithic column made can maintain a complete shape and scale only when it is filled with solvent inside. When the solvent is lost or volatilized, the interior of the pores will deform due to lack of support, and the entire column bed structure will shrink. When it exceeds a certain degree, the spatial structure will collapse, resulting in disordered local cracking or detachment from the column tube, and the entire column will be scrapped and can no longer be used as the stationary phase of liquid chromatography or solid-phase extraction. This phenomenon limits the application of some elastic materials as monolithic column materials. To address this problem, the domestic and foreign research and application fields mainly adopt methods to prevent the solvent in the monolithic column bed from volatilizing as much as possible, such as sealing both ends of the monolithic column or immersing the entire column in a solvent to prevent drying. Although these measures have certain effects, there are still inconveniences. Summary of the Invention:

[0003] To solve the problems existing in the prior art, the present invention proposes a pre-compressed solid-phase extraction column tube with adjustable compression amount and a using method thereof. The present invention pre-applies a pressure in the longitudinal direction of the monolithic column bed by mechanical force to extrude the column bed to a certain extent, so as to offset the remaining amount of column bed shrinkage, thereby preventing cracking after the column bed dries. Using the mechanical space compensation method can overcome the problem of column bed shrinkage of elastic monolithic columns to a certain extent, and can be applied to various solid-phase extraction fillers with a certain elasticity, so as to expand the selection and application range of monolithic column materials.

[0004] The object of the present invention is to provide a pre-compressed solid-phase extraction column tube with adjustable compression amount, which includes a screw cap, a column tube, and a piston device sleeved inside the screw cap and the column tube. The screw cap and the column tube are connected by threads. A round hole is provided in the center of the screw cap. The piston device includes a piston body and a cylindrical section arranged at the upper end of the piston body. An integral column bed is arranged inside the column tube. A lower sieve plate is arranged at the bottom of the integral column bed, and an upper sieve plate is arranged at the top. The top of the upper sieve plate is connected to the bottom of the piston body. The cylindrical section passes through the round hole of the screw cap and is arranged at the top end of the screw cap. A first Luer connector for connecting a syringe is arranged at the top of the cylindrical section. A through hole for liquid to flow through is arranged inside the piston body. The column tube proposed by the present invention is a cylindrical column tube.

[0005] Existing copolymer monolithic columns have the problem of being prone to dry cracking, which affects the characterization and application of the monolithic columns. To solve this problem, in addition to adjusting polymerization parameters to increase the strength of the monolithic column structure and prevent the column bed from drying and shrinking, the pre-compressed solid-phase extraction column tube with adjustable compression amount proposed by the present invention can solve the problems of removing porogens from the monolithic column and compensating for the column bed shrinkage during the drying process of the column bed, preventing phenomena such as cracks in the column bed and detachment from the column tube to adapt to the elastic monolithic column. Using a mechanical space compensation method can overcome the problem of column bed shrinkage of the elastic monolithic column to a certain extent and expand the selection and application range of monolithic column materials.

[0006] The cylindrical monolithic column bed after polymerization is located at the bottom of the cylindrical column tube, and upper and lower sieve plates made of porous sintered materials are respectively arranged above and below it to limit its position; among them, the upper sieve plate at the upper end of the monolithic column bed is fixed to the bottom of the movable piston body. There is a through hole for liquid to flow through in the middle of the piston body, and the piston body is pressed downward by the screw cap at the top.

[0007] The technical principle of the pre-compressed solid-phase extraction column tube with adjustable compression amount proposed by the present invention is as follows: After the monolithic column prepared from an elastic material is polymerized, during the process of flushing to remove the porogens therein, the spatial network structure may shrink and crack due to the loss of the support of the internal filling liquid. If the column bed is gradually compressed inward in one direction during the process of removing the porogens, and the compression amount is gradually increased as the porogens are removed, the shrinkage phenomenon of the column bed can be controlled to proceed orderly in one direction, preventing the occurrence of disordered internal gaps, voids, and detachment from the pipe wall.

[0008] Preferably, an internal thread of the screw cap is arranged inside the screw cap, and an external thread of the pipe wall is arranged on the outer wall of the column tube. The screw cap and the column tube are connected by the internal thread of the screw cap and the external thread of the pipe wall. The screw cap and the column tube are connected by threads, and there is a certain margin between the internal thread of the screw cap and the external thread of the pipe wall, and the height of the screw cap can be adjusted within a certain range by rotating the angle of the screw cap.

[0009] Preferably, a scale is provided on the outer wall of the column tube, and a scale pointer for jointly identifying the screwing-in amount of the screw cap with the scale is provided on the screw cap.

[0010] Preferably, the through hole is a tapered through hole. There is a through hole inside the piston body for the liquid to flow through. The lower part of the through hole expands into a tapered through hole. The circular sieve plate (upper sieve plate) is stuck in the tapered through hole at the bottom of the piston body, and the upper sieve plate and the bottom edge of the piston body form a plane.

[0011] Preferably, a second Luer connector for connecting an on-line device or a vacuum assistance device is provided at the bottom of the column tube. The solid phase extraction column prepared by the adjustable compression amount pre-compressed solid phase extraction column tube proposed by the present invention can be connected to an on-line device through the first Luer connector or the second Luer connector and used as an on-line solid phase extraction column. It can also be used as an off-line solid phase extraction column by connecting an empty syringe to the first Luer connector at the upper end and a vacuum assistance device to the second Luer connector at the lower end.

[0012] Preferably, a sealing ring for sealing is provided at the lower end of the piston body. The column tube is a hollow cylindrical shape, open at the upper part and basically closed at the lower part. The lower outlet is in the specification of a Luer connector. In the combined state, the cylindrical section at the upper part of the piston body passes through the circular hole in the center of the screw cap, and the first Luer connector at its upper end extends outside the screw cap. The sealing ring on the outer edge of the lower part of the piston body forms an interference fit with the inner wall of the column tube to achieve sealing. The bottom edge of the piston body and the upper sieve plate stuck at the bottom of the piston body together press on the top of the overall column bed, and the lower part of the column bed is supported by the lower sieve plate.

[0013] Preferably, the piston body is a cylindrical piston body, and the diameter of the cylindrical section is smaller than the diameter of the cylindrical piston body.

[0014] The present invention also protects the application of a pre-compressed solid-phase extraction column tube with adjustable compression amount in solid-phase extraction. The specific usage method of the pre-compressed solid-phase extraction column tube with adjustable compression amount is as follows: When preparing the monolithic column, remove the screw cap, the inner main tube and the spring, block the lower end of the outer column tube with a Luer plug, and place the outer column tube vertically. Add the prepared liquid polymer monomer mixture into the outer column tube, block the upper end of the outer column tube with a sealing cap, and place it at a certain temperature for in-situ polymerization reaction to prepare the monolithic column bed. After the polymerization reaction is completed, remove the sealing cap on the upper part of the outer column tube, install the piston and the screw cap, connect the pipeline of the rinsing agent tank or the infusion pump to the first Luer connector at the upper end of the column tube, and connect the pipeline leading to the waste liquid tank to the second Luer connector at the lower end of the column tube. During the process of rinsing to remove the porogen, the screw cap can be gradually screwed in by a mechanical device or manually to increase the screw-in amount, and the piston is compressed downward to compensate for the longitudinal shrinkage of the monolithic column bed until the preset scale is reached. Then, fix the screw cap with glue to prevent it from rotating further. The two ends of the column tube can be sealed with caps and plugs that meet the Luer connector standard to prevent the monolithic column bed from drying out completely. The elastic material solid-phase extraction monolithic column prepared with the pre-compressed solid-phase extraction column tube with adjustable compression amount can be used for off-line solid-phase extraction operation in the following manner: Before use, remove the caps and plugs at both ends of the column tube, connect an empty syringe to the first Luer connector at the upper end of the solid-phase extraction column, connect the second Luer connector at the lower end to a vacuum-assisted device, rinse and activate the column bed with an appropriate volume of a suitable solvent, and then perform sample loading, elution and elution in the same operation mode as a conventional solid-phase extraction column. The prepared elastic material solid-phase extraction monolithic column can also be connected to an on-line solid-phase extraction device through the first Luer connector and the second Luer connector for on-line solid-phase extraction.

[0015] Compared with the prior art, the present invention has the following advantages: The pre-compressed solid-phase extraction column tube with adjustable compression amount proposed by the present invention can compensate for the shrinkage of the monolithic column bed during the process of removing the porogen and column bed drying, preventing phenomena such as cracks in the column bed and detachment from the column tube to adapt to the elastic monolithic column. Using 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. BRIEF DESCRIPTION OF THE DRAWINGS:

[0016] Figure 1 is a schematic structural diagram of the pre-compressed solid-phase extraction column tube with adjustable compression amount of the present invention;

[0017] Figure 2 is Figure 1 a cross-sectional view taken along the longitudinal direction;

[0018] Figure 3 is Figure 1 a schematic exploded view of the structure of

[0019] Description of the reference numerals: 1. Screw cap; 2. First Luer connector; 3. Cylindrical section; 4. Piston body; 5. Sealing ring; 6. Upper sieve plate; 7. Monolithic column bed; 8. Lower sieve plate; 9. Scale; 10. Column tube; 11. Second Luer connector; 12. Scale pointer; 13. Internal thread of the screw cap; 14. External thread of the tube wall. Detailed implementation manners:

[0020] Next, in combination with the embodiments of the present invention, the technical solutions of the present invention will be clearly and completely described. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts belong to the protection scope of the present invention. Unless otherwise specified, the equipment and reagents used in the present invention are conventional commercially available products in the technical field.

[0021] The pre-compressed solid-phase extraction column tube with adjustable compression amount proposed by the present invention is composed of three parts, namely the upper screw cap 1, the internal piston device, and the lower column tube 10. The screw cap 1 and the column tube 10 are connected by threads, and there is a certain margin in the threads, and the height of the screw cap 1 can be adjusted within a certain range by rotating the angle. A pointer (pointer mark) is engraved on the screw cap 1 to jointly identify the screwing-in amount of the screw cap with the scale on the outer wall of the column tube. The piston device is an integral body. The upper part is a Luer connector specification (first Luer connector) that can be connected to a syringe. There is a cylindrical section 3 with a smaller diameter downward, and then a cylindrical piston body 4 below. There are two raised sealing rings 5 at the lower end of the piston body 4. A through hole through which liquid can flow is provided inside the piston body 4. The lower part of the through hole expands into a tapered through hole. The upper sieve plate 6 is stuck in the tapered through hole at the bottom of the piston body 4. The upper sieve plate 6 and the bottom edge of the piston body 4 form a plane. The column tube 10 is a hollow cylindrical shape, with an open upper part and a basically closed lower part. The lower outlet is a Luer connector specification (second Luer connector). In the combined state, the cylindrical section 3 at the upper part of the piston body 4 passes through the round hole in the center of the screw cap 1, and the first Luer connector 2 at its upper end extends out of the screw cap 1. The sealing ring 5 on the outer edge of the lower part of the piston body 4 forms an interference fit with the inner wall of the column tube 10 to achieve sealing. The bottom edge of the piston body 4 and the upper sieve plate 6 stuck at the bottom of the piston body 4 together press on the top of the monolithic column bed 7. The lower part of the monolithic column bed 7 is supported by the lower sieve plate 8.

[0022] In a pre-compressed solid-phase extraction column tube with adjustable compression amount, the polymerized cylindrical monolithic column bed 7 is located at the bottom of the cylindrical column tube 10, and upper and lower sieve plates 6 and 8 made of porous sintered material are respectively arranged above and below it to limit its position; among them, the upper sieve plate 6 at the upper end of the monolithic column bed 7 is fixed to the bottom of the movable piston body 4, there is a through hole for liquid flow in the middle of the piston body 4, and the piston body 4 is pressed down by the threaded cap 1 at the top; the cap 1 can adjust the downward compression distance of the piston body 4 by the number of turns of rotation through its threaded fit with the column tube 10, and there are scales on the outer wall of the column tube 10 to mark the amount of the cap screwed in. When flushing the monolithic column, connect the pipeline from the flushing agent tank or the infusion pump to the first Luer connector 2 at the upper end of the column tube, and connect the pipeline leading to the waste liquid tank to the second Luer connector 11 at the lower end of the column tube. During the process of flushing and removing the porogen, the amount of the cap screwed in can be gradually increased by machine or manually to compensate for the longitudinal contraction of the monolithic column bed 7 by pressing down the piston body 4 until the preset scale is reached, and then fix the cap 1 with glue to prevent it from rotating further. Caps and plugs conforming to the Luer connector standard can be used to seal both ends of the column tube to prevent the monolithic column bed from drying out completely.

[0023] Example 1

[0024] As Figures 1-3 shown, a pre-compressed solid-phase extraction column tube with adjustable compression amount includes a cap 1, a column tube 10, and a piston device sleeved inside the cap 1 and the column tube 10. The cap 1 and the column tube 10 are connected by threads. A round hole is provided in the center of the cap 1. The piston device includes a piston body 4 and a cylindrical section 3 arranged at the upper end of the piston body 4. A monolithic column bed 7 is arranged inside the column tube 10. A lower sieve plate 8 is arranged at the bottom of the monolithic column bed 7, and an upper sieve plate 6 is arranged at the top. The top of the upper sieve plate 6 is connected to the bottom of the piston body 4. The cylindrical section 3 passes through the round hole of the cap 1 and is arranged at the top of the cap 1. A first Luer connector 2 for connecting a syringe is arranged at the top of the cylindrical section 3, and a through hole for liquid flow is arranged inside the piston body 4.

[0025] In this embodiment, it is preferred that the column tube 10 is a cylindrical column tube, the piston body 4 is a cylindrical piston body, and the diameter of the cylindrical section 3 is smaller than the diameter of the cylindrical piston body 4. The monolithic column bed is made of a porous monolithic material with a certain elasticity. The polymerized cylindrical monolithic column bed 7 is located at the bottom of the cylindrical column tube, and upper and lower sieve plates 6 and 8 made of porous sintered material are respectively arranged above and below it to limit its position; among them, the upper sieve plate 6 at the upper end of the monolithic column bed 7 is fixed to the bottom of the movable piston body 4, there is a through hole for liquid flow in the middle of the piston body 4, and the piston body 4 is pressed down by the threaded cap at the top.

[0026] The inner part of the screw cap 1 is provided with an internal screw thread 13 of the screw cap, and the outer wall of the column tube 10 is provided with an external screw thread 14 of the tube wall. The screw cap 1 and the column tube 10 are connected through the internal screw thread 13 of the screw cap and the external screw thread 14 of the tube wall. The screw cap and the column tube are connected by threads, and there is a certain margin between the internal screw thread of the screw cap and the external screw thread of the tube wall, so that the height of the screw cap can be adjusted within a certain range by rotating the angle of the screw cap.

[0027] The outer wall of the column tube 10 is provided with a scale 9, and the screw cap 1 is provided with a scale pointer 12 for jointly identifying the screwing-in amount of the screw cap with the scale. In the present invention, the through hole is preferably a tapered through hole. There is a through hole inside the piston body through which liquid can flow. The lower part of the through hole expands into a tapered through hole. The circular sieve plate (upper sieve plate) is stuck in the tapered through hole at the bottom of the piston body, and the upper sieve plate and the bottom edge of the piston body form a plane.

[0028] The bottom of the column tube 10 is provided with a second Luer connector 11 for connecting an on-line device or a vacuum assist device. The pre-compressed solid-phase extraction column tube with adjustable compression amount proposed by the present invention can be connected to an on-line device through the first Luer connector 2 or the second Luer connector 11 and used as an on-line solid-phase extraction column. It can also be used as an off-line solid-phase extraction column by connecting an empty syringe to the first Luer connector 2 at the upper end and a vacuum assist device to the second Luer connector 11 at the lower end.

[0029] In this embodiment, the column tube 10 is a hollow cylindrical shape, with an upper opening and a basically closed lower part. The lower outlet is in the specification of a Luer connector. The lower end of the piston body 4 is provided with a sealing ring 5 for sealing. In the combined state, the cylindrical section 3 at the upper part of the piston body 4 passes through the round hole in the center of the screw cap 1, and the first Luer connector 2 at its upper end extends out of the screw cap 1. The sealing ring 5 on the outer edge of the lower part of the piston body 4 forms an interference fit with the inner wall of the column tube 10 to achieve sealing. The bottom edge of the piston body 4 and the upper sieve plate 6 stuck at the bottom of the piston body 4 together press on the top of the overall column bed 7. The lower part of the overall column bed 7 is supported by the lower sieve plate 8.

[0030] The technical principle of the pre-compressed solid-phase extraction column tube with adjustable compression amount proposed by the present invention is as follows: After the overall column made of an elastic material is polymerized, during the process of washing and removing the porogen therein, the spatial network structure may shrink and crack due to the loss of the support of the internal filling liquid. If the column bed is gradually compressed inward in one direction during the process of removing the porogen and the compression amount is gradually increased as the porogen is removed, the shrinkage phenomenon of the column bed can be controlled to proceed orderly in one direction, preventing the occurrence of disordered internal gaps, voids and detachment from the tube wall.

[0031] The solid-phase extraction overall column of the pre-compressed solid-phase extraction column tube with adjustable compression amount proposed by the present invention can be connected to an on-line device through a Luer connector and used as an on-line solid-phase extraction column. It can also be used as an off-line solid-phase extraction column by connecting an empty syringe at the upper end and a vacuum assist device at the lower end.

[0032] The description of the above embodiments is only used to help understand the technical solution and its core idea of the present invention. It should be noted that for those skilled in the art of this technology, without departing from the principle of the present invention, several improvements and modifications can be made to the present invention, and these improvements and modifications also fall within the protection scope of the claims of the present invention.

Claims

1. A pre-compression type solid-phase extraction column tube with adjustable compression amount, characterized in that, It includes a screw cap, a column tube, and a piston device sleeved inside the screw cap and the column tube. The screw cap and the column tube are connected by threads. A round hole is provided at the center of the screw cap. The piston device includes a piston body and a cylindrical section arranged at the upper end of the piston body. An elastic monolithic column bed is arranged inside the column tube. A lower sieve plate is arranged at the bottom of the monolithic column bed, and an upper sieve plate is arranged at the top. The top of the upper sieve plate is connected to the bottom of the piston body. The cylindrical section passes through the round hole of the screw cap and is arranged at the top of the screw cap. A first Luer connector for connecting a syringe is arranged at the top of the cylindrical section. A tapered through hole for liquid flow is arranged inside the piston body.

2. The pre-compressed solid-phase extraction column tube with adjustable compression amount according to claim 1, wherein Internal screw threads are provided inside the screw cap, and external screw threads are provided on the outer wall of the column tube. The screw cap and the column tube are connected by the internal screw threads of the screw cap and the external screw threads of the tube wall.

3. The pre-compressed solid-phase extraction column tube with adjustable compression amount according to claim 1, characterized in that, Scales are provided on the outer wall of the column tube, and a scale pointer for jointly marking the screwing-in amount of the screw cap with the scales is arranged on the screw cap.

4. The pre-compressed solid-phase extraction column tube with adjustable compression amount according to claim 1, wherein A second Luer connector for connecting an on-line device or a vacuum assist device is arranged at the bottom of the column tube.

5. The pre-compressed solid-phase extraction column tube with adjustable compression amount according to claim 1, characterized in that, A sealing ring for sealing is arranged at the lower end of the piston body.

6. The pre-compressed solid-phase extraction column tube with adjustable compression amount according to claim 1, characterized in that, The piston body is a cylindrical piston body, and the diameter of the cylindrical section is smaller than the diameter of the cylindrical piston body.

7. Application of the pre-compressed solid phase extraction column tube with adjustable compression amount according to claim 1 in solid phase extraction.

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