CN210487696U - Device for capillary tube affinity monolithic column on-line specific adsorption - Google Patents
Device for capillary tube affinity monolithic column on-line specific adsorption Download PDFInfo
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- CN210487696U CN210487696U CN201921193586.2U CN201921193586U CN210487696U CN 210487696 U CN210487696 U CN 210487696U CN 201921193586 U CN201921193586 U CN 201921193586U CN 210487696 U CN210487696 U CN 210487696U
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Abstract
The utility model relates to a device for capillary affinity monolithic column is adsorbed to online specificity belongs to analytical chemistry instrument equipment field, including setting up the fixed subassembly on capillary affinity monolithic column, the introduction end of fixed subassembly is provided with the sample introduction hookup part that is used for with the sampling tube exit end hookup of first dimension chromatogram, and the exit end of fixed subassembly is provided with and is used for deriving the hookup subassembly with the eluant that second dimension chromatogram sampling subassembly introduction end is connected. The device can be flexibly connected with the sampling process of the first-dimension chromatogram, the sampling process of the second-dimension chromatogram, the enrichment process and the elution process.
Description
Technical Field
The utility model relates to a device for capillary affinity monolithic column is adsorbed to online specificity belongs to analytical chemistry instrument equipment field.
Background
With the popularization of microanalysis, a specific adsorption enrichment technology on a column becomes important day by day, and the method is well applied to High Performance Liquid Chromatography (HPLC) analysis. At present, in the conventional HPLC, the enrichment on the column is mainly based on the spontaneous adsorption of solute in a stationary phase, the self-enrichment and concentration effects of locally accumulated filler are generated in the column head sample injection process, and the sample consumption is larger. The capillary affinity monolithic column is a third-generation chromatographic separation medium after a capillary packed column and a capillary open tubular column are taken as a continuous stationary phase for in-situ polymerization in the column, has various properties of good net structure, good permeability, high mass transfer speed, stable structure, high column efficiency, easy surface modification, easy preparation and the like, and has become the key point of micro-flow chromatographic research.
The on-line combination of the capillary inner solid phase micro-extraction technology and the liquid chromatogram ensures that the use level of an analysis sample is reduced from a vertical liter level to a milliliter level or even a micro-upgrade level, realizes the on-line concentration and separation of the sample, and is applied to ultra-micro and trace analysis. On-line micro-column specific adsorption research reports are more, wherein most of the on-line micro-column specific adsorption research reports are applied to liquid chromatography, the on-line specific adsorption column is directly connected with a sample injection device, and on-line continuous sample injection, enrichment and elution analysis of a capillary column are realized through switching of two six-way valve assemblies; the chemical bonding method is applied to coat the inner wall of a quartz capillary electrophoresis column, and documents report a novel capillary electrophoresis coating column, a hyperbranched polyether coating is adopted to modify a capillary, so that organophosphorus pesticide is adsorbed on the capillary in an online specific manner, and the method is mainly applied to online enrichment analysis of capillary electrophoresis, but has no specificity. At present, a capillary column is generally and directly arranged on a six-way valve structure, the length of an online specific adsorption column is limited by the structure of the six-way valve device, the length of an enrichment column is large, the requirements on the polymerization degree and permeability of the whole column are high, and the enrichment elution time is long. There are also reports of a device for capillary column immobilization, the device is integrally formed by adopting a polyetheretherketone PEEK material, the immobilized capillary column has a length of 2 cm, and can be used for on-line specific adsorption of micro-column HPLC, but the length and the diameter are fixed, and flexible transformation or update cannot be performed according to actual needs.
At present, with the development of capillary micro-separation technology, the demand of on-line specific adsorption of micro-columns is increasing. The existing device for capillary column immobilization is structurally solidified and difficult to adjust according to actual needs, brings great inconvenience to the column enrichment operation of the micro-column in the practical analysis and application process, and needs to develop a simple, convenient and practical device for capillary column online specificity adsorption urgently.
Disclosure of Invention
An object of the utility model is to provide a be used for the online specificity of capillary affinity monolithic column absorbent device, the device can link up with advancing kind, enrichment, elution and the second dimension chromatogram of first dimension chromatogram respectively comparatively nimbly and mutually.
The technical scheme of the utility model lies in: the utility model provides a device for online specificity of capillary affinity monolithic column adsorbs, is including setting up the fixed subassembly on capillary affinity monolithic column, the introduction end of fixed subassembly is provided with the sample introduction hookup part that is used for with the hookup of first dimension chromatogram's sampling tube exit end, and the exit end of fixed subassembly is provided with and is used for deriving the hookup subassembly with the eluant that second dimension chromatogram sampling subassembly introduction end is connected.
Furthermore, the fixed assembly comprises a protective sleeve sleeved on the capillary affinity integral column, two ends of the protective sleeve are respectively connected with a fixed tube, the other end of the fixed tube is respectively provided with a fixed tube conical screw, and the fixed tube conical screw are sleeved on the capillary affinity integral column.
Furthermore, the sample introduction connecting part comprises a sample introduction end conical screw connected with the outlet end of the sampling tube of the first dimension chromatogram, a capillary tube sleeve is arranged in the sample introduction end conical screw, and the other end of the capillary tube sleeve extends into the fixed tube conical screw on the sample introduction end side and the fixed tube and is sleeved on the capillary affinity monolithic column.
Furthermore, the eluent guiding-out connection component comprises an outlet end conical screw connected with the inlet end of the second-dimension chromatographic sampling tube, a capillary tube sleeve is arranged in the outlet end conical screw, and the other end of the capillary tube sleeve extends into the fixed tube conical screw and the fixed tube on the outlet end side and is sleeved on the capillary affinity monolithic column.
Furthermore, both ends of the protective sleeve are respectively in threaded connection with a fixed pipe, and the fixed pipe is in threaded connection with a conical screw of the fixed pipe.
Further, the both ends of protective case are provided with the transparent polymerization plastic tubing of screw thread matched with fixed pipe respectively, the one end inside of fixed pipe be provided with fixed pipe taper screw matched with screw thread, the other end of fixed pipe be provided with protective case assorted threaded PEEK pipe, the center of fixed pipe be equipped with be used for with PEEK pipe matched with microchannel.
Further, the capillary affinity monolithic column has an outer diameter of 365 microns, the capillary sleeve is a PEEK tube, the tube outer diameter is 1/16 inches, and the inner diameter is 500 microns.
Furthermore, the sample inlet end taper screw and the fixed tube taper screw are respectively 1/16-inch PEEK joints commonly used for liquid chromatography.
Further, the outlet end conical screw is an 1/16 inch PEEK fitting commonly used in liquid chromatography.
Compared with the prior art, the utility model has the advantages of it is following: the device can be flexibly connected with the sample injection, enrichment and elution of the first-dimension chromatogram and the sample injection process of the second-dimension chromatogram respectively through a sample injection connecting part and an eluent leading-out connecting component; the conical screw of the capillary affinity monolithic column fixing component and the size of the fixing pipe thereof are matched with the capillary affinity monolithic column, so that the capillary affinity monolithic column can be tightly fixed under high pressure; the two ends of the protective sleeve can be respectively connected with the fixed pipes on the two sides through threads, the embedding depth can be adjusted according to the length of the capillary affinity integral column, the operation is simple, the problem that the conventional capillary column online specificity adsorption device cannot adopt a capillary column with the length different from that of the fixed pipe due to the fixed length of the fixed groove is solved, and the applicability is better.
Drawings
Fig. 1 is a schematic structural view of the present invention;
in the figure: 1-sampling end conical screw; 2-capillary sleeve; 3-fixing the conical screw of the pipe; 4-fixing the tube; 5-protecting the sleeve; 6-capillary affinity monolithic column; 7-a fixed tube; 8-fixing the pipe conical screw; 9-capillary sleeve; 10-outlet end conical screw.
Detailed Description
In order to make the aforementioned features and advantages of the present invention more comprehensible, embodiments accompanied with figures are described in detail below, but the present invention is not limited thereto.
Refer to FIG. 1
The utility model provides a device for online specificity of capillary affinity monolithic column adsorbs, is including setting up the fixed subassembly on capillary affinity monolithic column 6, the introduction end of fixed subassembly is provided with the sample introduction hookup part that is used for with the sampling tube exit end hookup of first dimension chromatogram, and the exit end of fixed subassembly is provided with and is used for deriving the hookup subassembly with the eluant that second dimension chromatogram sampling subassembly introduction end is connected.
In this embodiment, fixed subassembly is including arranging protective case 5 on capillary affinity monolithic column in the cover, the both ends of protective case are connected with fixed pipe 4, 7 respectively, the other end of fixed pipe is provided with fixed pipe conical screw 3, 8 respectively, and the conical surface of fixed pipe conical screw is towards fixed pipe, fixed pipe and fixed pipe conical screw cover are arranged on capillary affinity monolithic column in. The dimensions of the fixed tube conical screws 3, 8 and the fixed tubes 4, 7 are matched to the capillary affinity monolith column in order to tightly fix the capillary affinity monolith column at high pressure.
In this embodiment, the sample introduction coupling part comprises a sample introduction end conical screw 1 for being coupled with the outlet end of the sampling tube of the first dimension chromatogram, the conical surface of the sample introduction end conical screw faces outwards, a capillary sleeve 2 is arranged in the sample introduction end conical screw, and the other end of the capillary sleeve extends into a fixed tube conical screw 3 and a fixed tube 4 on the sample introduction end side and is sleeved on the capillary affinity monolithic column. The length of the capillary tube housing 2 can be flexibly changed according to the size of the device.
In this embodiment, the eluent leading-out coupling assembly includes an outlet-end conical screw 10 for coupling with an inlet end of the second dimension chromatography sampling tube, a conical surface of the outlet-end conical screw faces outward, a capillary tube 9 is disposed in the outlet-end conical screw, and the other end of the capillary tube extends into a fixed tube conical screw 8 and a fixed tube 7 on the outlet end side and is sleeved on the capillary affinity monolithic column. The length of the capillary tube sleeve 9 can be flexibly changed according to the size of the device.
In this embodiment, both ends of the protective sleeve are screwed with the fixed tube respectively, and the embedding depth can be adjusted so as to protect the capillary affinity monolithic column. The fixed pipe is in threaded connection with the conical screw of the fixed pipe.
In this embodiment, the both ends of protective sleeve are provided with the transparent polymerization plastic tubing with the screw thread matched with of fixed pipe respectively, the fixed pipe of protective sleeve can pass through the rotation embedding, and capillary affinity monolithic column passes from the protective sleeve, and its embedding degree of depth can be adjusted according to the length of affinity monolithic column, has avoided the restriction of fixed dimension to capillary column and capillary direct exposure and easy impaired problem.
In this embodiment, the inside screw thread that is provided with and solid fixed tube conical screw matched with of one end of solid fixed tube, the other end of solid fixed tube be provided with protective case assorted screw thread the PEEK pipe, the center of solid fixed tube be equipped with be used for with advance kind and the PEEK pipe matched with microchannel that the eluant was derived to be used for pinning solid capillary affinity column.
In this embodiment, the capillary affinity monolithic column has an outer diameter of 365 microns, the capillary sleeve is a PEEK tube, the outer diameter of the PEEK tube is 1/16 inches, and the inner diameter of the PEEK tube is 500 microns. Can resist the corrosion of organic reagents and acid-base reagents and can resist the high pressure of a liquid chromatography mobile phase.
In this embodiment, the sample introduction end conical screw, the outlet end conical screw, and the fixing tube conical screw are respectively 1/16 inch PEEK connectors that are commonly used in liquid chromatography.
In order to describe the on-line specific adsorption of a target object by a capillary affinity monolithic column, an affinity monolithic column formed by polymerizing polyhedral oligomeric silsesquioxane (POSS-MA), ethylene glycol dimethacrylate (EDMA) and aptamer (Apt) by ochratoxin A (OTA) serving as a model compound is selected for an experiment, and the method specifically comprises the following steps:
(1) preparing Tris-HCl binding buffer solution;
(2) loading the capillary affinity monolithic column into the on-line specificity adsorption device, wherein conical screws at two ends are respectively arranged at the output position of the six-way valve sample tube in the first dimension and the sample injection position of the six-way valve sample tube in the second dimension;
(3) introducing the prepared Tris-HCl binding buffer solution into an affinity monolithic column for balancing for 30 min;
(4) filling 100 mu L of OTA standard solution prepared by combining buffer solution into a quantitative ring;
(5) switching the six-way valve, taking the binding buffer solution as a mobile phase, and introducing the OTA solution into the affinity monolithic column through a liquid phase pump at room temperature;
(6) washing the affinity monolithic column with a binding buffer solution to remove target substances which are not specifically bound;
(7) eluting the target substance from the affinity monolithic column by using methanol as eluent, and introducing the eluent into a sampling loop of a second-dimensional chromatogram with the volume of 20 mu L;
(8) switching the six-way valve of the second dimension chromatogram, injecting the eluent into a liquid chromatogram instrument, carrying out chromatographic separation under an isocratic mode, wherein the flow rate is 1.0 mL/min, and carrying out separation detection by using 2% acetic acid-water solution/acetonitrile = 38/62 (v/v) as a mobile phase.
The buffer solution component concentration is 10 mmol/L Tris-HCl, 120 mmol/L NaCl, 5 mmol/LKCl, 20 mmol/L CaCl2The pH was 8.50.
Under the on-line loading condition of the affinity monolithic column, the pump flow rate is 0.02 mL/min, and the backpressure valve is 250 psi.
The above-mentioned affinity monolithic column was cleaned on-line with a pump flow rate of 0.1 mL/min and a backpressure valve of 500 psi.
The above-mentioned conditions for on-line elution of the affinity monolith were 0.02 mL/min pump flow rate and 250 psi back pressure valve.
The above-mentioned separation column for liquid chromatography for on-line separation is C18Column, packing size 5 μm, column size 4.6mm i.d.. times.250 mm.
The above is only the preferred embodiment of the present invention, and all the equivalent changes and modifications made according to the claims of the present invention should be covered by the present invention.
Claims (9)
1. The utility model provides a device for online specificity of capillary affinity monolithic column adsorbs which characterized in that, is including setting up the fixed subassembly on capillary affinity monolithic column, the appearance end of fixed subassembly is provided with the sample appearance hookup part that is used for with the hookup of first dimension chromatogram's sampling tube exit end, and the exit end of fixed subassembly is provided with and is used for deriving the hookup subassembly with the eluant that second dimension chromatogram sampling subassembly appearance end is connected.
2. The device for on-line specific adsorption of a capillary affinity monolithic column according to claim 1, wherein the fixing assembly comprises a protective sleeve sleeved on the capillary affinity monolithic column, two ends of the protective sleeve are respectively connected with a fixing tube, the other end of the fixing tube is respectively provided with a fixing tube conical screw, and the fixing tube conical screw are sleeved on the capillary affinity monolithic column.
3. The device according to claim 2, wherein the sample introduction coupling member comprises a sample introduction end taper screw for coupling with an outlet end of the sampling tube of the first dimension chromatogram, a capillary sleeve is arranged in the sample introduction end taper screw, and the other end of the capillary sleeve extends into the fixed tube taper screw and the fixed tube on the sample introduction end side and is sleeved on the capillary affinity monolithic column.
4. The device for on-line specific adsorption of capillary affinity monolithic column according to claim 2 or 3, wherein the eluent leading-out coupling component comprises an outlet end conical screw for coupling with the inlet end of the second dimension chromatography sampling tube, a capillary sleeve is arranged in the outlet end conical screw, and the other end of the capillary sleeve extends into the fixed tube conical screw and the fixed tube on the outlet end side and is sleeved on the capillary affinity monolithic column.
5. The device for capillary affinity monolithic column on-line specific adsorption according to claim 2, wherein both ends of the protective sleeve are respectively screwed with a fixed tube, and the fixed tube is in threaded connection with a conical screw of the fixed tube.
6. The device for the on-line specific adsorption of the capillary affinity monolithic column according to claim 2 or 5, wherein the two ends of the protective sleeve are respectively provided with a transparent polymeric plastic tube which is matched with the thread of the fixed tube, the inner part of one end of the fixed tube is provided with the thread which is matched with the conical screw of the fixed tube, the other end of the fixed tube is provided with a PEEK tube which is matched with the thread of the protective sleeve, and the center of the fixed tube is provided with a micro-channel which is matched with the PEEK tube.
7. The device for on-line specific adsorption of capillary affinity monolithic column according to claim 4, wherein the outer diameter of capillary affinity monolithic column is 365 microns, the capillary sleeve is PEEK tube, the outer diameter of the tube is 1/16 inches, and the inner diameter of the tube is 500 microns.
8. The device of claim 3, wherein the tapered screw at the sample inlet and the tapered screw at the fixing tube are respectively 1/16 inches PEEK joints commonly used in liquid chromatography.
9. The apparatus of claim 4, wherein the outlet-end taper screw is 1/16-inch PEEK joint commonly used in liquid chromatography.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921193586.2U CN210487696U (en) | 2019-07-26 | 2019-07-26 | Device for capillary tube affinity monolithic column on-line specific adsorption |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921193586.2U CN210487696U (en) | 2019-07-26 | 2019-07-26 | Device for capillary tube affinity monolithic column on-line specific adsorption |
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| CN210487696U true CN210487696U (en) | 2020-05-08 |
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