Thin layer chromatography extraction device, combined system and extraction method

Abstract

To provide a thin layer chromatography extraction device that uses a simpler device structure, can quickly collect, prepare and analyze samples, improves the extraction efficiency, and reduces costs.SOLUTION: A thin layer chromatography extraction device is provided including: a sampler having a solvent inlet and a solvent outlet; solvent injection means in communication with the solvent inlet; and a filter that is detachably attached to the solvent outlet. The solvent outlet has a sharp edge for cutting down a prescribe volume of an adsorbent from an adsorbent layer of a thin layer chromatography plate, the cut-down adsorbent being kept between the solvent inlet and the solvent outlet.SELECTED DRAWING: Figure 1

Description

[Technical field]

[0001] The present invention relates to the field of solution analysis, and more particularly to a thin-layer chromatography extraction device, a thin-layer chromatography-mass spectrometry combined system, and a thin-layer chromatography extraction method. [Background technology]

[0002] Thin layer chromatography (TLC) is a chromatographic technique for separating mixtures. In general, the mixture is separated using thin layer chromatography, then the thin layer is manually scraped off from the separated thin layer chromatography plate with a plate scraper, followed by solvent extraction, filtration and purification to obtain the separated analytes, and finally the separated analytes are transferred to a detection device such as a mass spectrometer for further detection, thus achieving the separation and detection of organic compounds, but the operation is complicated.

[0003] Patent Document 1 discloses a surface extraction interface system that can extract and measure the material composition of an object surface in real time online, specifically, the surface extraction interface system seals the extraction target area from other areas by contacting or cutting into the surface of the adsorbent through a seal assembly, and continuously transfers the extraction solvent to the area from the solvent inlet, and the extracted solvent flows out again from the solvent outlet on the same side nearby and enters a mass spectrometer for detection, thereby extracting and detecting the analyte on the surface of the area in real time. However, the device structure and pipe connection of the surface extraction interface system are complicated, and the extraction time for one area is long, while the adoption of a method in which the solvent passes only through the surface layer of the adsorbent layer on the same side for continuous extraction may cause the substrate material of the thin layer chromatography plate (e.g., silica gel adsorbent) to easily collapse, which may cause clogging of the pipes or frequent replacement of the internal filter material.

[0004] Therefore, an improved technical solution is needed to solve the above problems of traditional thin layer chromatography extraction. [Prior art documents] [Patent documents]

[0005] [Patent Document 1] CN107430048A Summary of the Invention

[0006] In view of the above problems of the prior art, the technical solution of the present invention provides a thin layer chromatography extraction device that uses a simpler device structure and can quickly collect, prepare and analyze samples. [Means for solving the problem]

[0007] A first aspect of the present invention provides a thin layer chromatography extraction device comprising a sampler having a solvent inlet and a solvent outlet, a solvent injection means communicating with the solvent inlet, and a filter removable from the solvent outlet, the solvent outlet having a sharp edge for cutting out a predetermined volume of adsorbent from an adsorbent layer of a thin layer chromatography plate, and the cut out adsorbent is held between the solvent inlet and the solvent outlet. Effect of the Invention

[0008] According to this technical solution, for the adsorption layer obtained after thin-layer chromatography separation, the user presses the area that needs to be further detected with the sampler of the thin-layer chromatography extraction device provided by the present invention, and after the sharp edge is cut into the adsorption layer of the thin-layer chromatography plate by pressure, lift the sampler to obtain a predetermined volume of cut adsorption agent, and then injects solvent into the solvent inlet of the sampler by the solvent injection means, so that the solvent passes through the adsorption agent in the through cavity of the sampler to extract the analyte in the adsorption agent, and the solvent with the analyte after extraction flows out from the solvent outlet of the sampler and passes through the filter, and after the large granular impurities (generally the substrate material of the thin-layer chromatography plate) are removed, it can be directly injected into the subsequent detection device for detection. The thin-layer chromatography extraction device has high extraction efficiency, simple structure, convenient operation, and is more suitable for sampling inspection of a specific area of ​​the adsorption layer after thin-layer chromatography separation in daily detection.

[0009] In a preferred technical solution, the filter is a chip type filter.

[0010] According to this technical proposal, a tip-type filter (Syringe Filter) refers to a tubular structure that resembles the tip of a syringe and has a wide-diameter filtration chamber and a narrow-diameter syringe outlet. A filtration structure (e.g., a filtration membrane, a screen, a fine hole, etc.) is installed at the wide diameter, so that the fluid flows into the wide diameter and is filtered, and then merges and flows out through the narrow diameter. In particular, a disposable tip-type filter can be adopted, in which case there is no need to replace the filter material, the possibility of clogging the pipes is low, and the risk of cross-contamination between samples can be reduced.

[0011] In a preferred technical solution, the filter is connected to the solvent outlet and is a syringe tip with an inner diameter of 0.05-0.5 mm.

[0012] According to this technical solution, the syringe tip is a long and thin needle structure attached to the tip of the syringe, and the large granular substrate material cannot pass through the syringe tip with an inner diameter of 0.05-0.5 mm, and the extracted solvent can be directly filtered by the syringe tip and simultaneously merged into a small flux. In addition, there is no need to install a filtering chamber or filtering material, especially a wide-bore chamber, so that the solvent can be avoided from being present in a large amount in the wide-bore chamber, which would cause sample dilution.

[0013] In a preferred technical solution, the thin layer chromatography extraction device is used as a sampling device for a mass spectrometer, and the solvent outlet is used to communicate with the sampling port of the mass spectrometer.

[0014] According to this technical solution, the combination of thin layer chromatography and mass spectrometry makes it easier to analyze and detect the substance composition of a complex mixture, thin layer chromatography can separate the components of the mixture, and different substances after separation are located in different areas of the adsorption layer of the chromatography plate, which is the thin layer chromatography extraction layer, and are pressed and cut by the sampler of the thin layer chromatography extraction device of the present invention to obtain an adsorbent with an analyte in a predetermined area, and after the solvent permeates the adsorbent to complete the extraction, it flows out from the solvent outlet, and after filtering, it directly flows into the mass spectrometry device to detect the substance components, so that the separation and detection of the complex mixture can be easily realized. In particular, the thin layer chromatography extraction device can be directly used in combination with a mass spectrometry device equipped with an analysis ion source, which can further improve the efficiency of substance analysis.

[0015] In a preferred technical solution, the solvent injection means is a syringe, the outlet of which is removably connected to the solvent inlet of the sampler.

[0016] According to this technical solution, the syringe refers to a syringe structure having a piston and a syringe outlet without a syringe tip. The small-diameter outlet at the tip of the syringe is easy to install, the syringe structure is simple, and it is suitable for mass production. In addition, the solvent injection means, the sampler, and the filter are all detachable structures, so that it can be applied to more detection situations.

[0017] In a preferred technical solution, the solvent injection means is a liquid pump.

[0018] According to this technical proposal, the liquid pump serves as a solvent injection means and can automatically pump in the solvent according to the settings, eliminating the need for manual operation and enabling precise control of the amount of extraction solvent pumped in.

[0019] In the preferred technical solution, the sharp edge is annular and has an inner diameter of 0.1-10 mm.

[0020] According to this technical solution, the annular edge with an inner diameter of 0.1-10 mm is pressed against the adsorption layer, and then the cut edge of the cut annular adsorbent is fastened to the inner wall of the annular edge. Then, a solvent injection means and a filter are respectively attached to both sides of the sampler, and the extraction solvent can be injected into the sampler to perform extraction.

[0021] As a preferred technical solution, the sampler further includes a throttle provided between the solvent outlet and the solvent inlet.

[0022] According to this technical solution, the throttle hole prevents the backflow from the solvent outlet to the solvent inlet, and only allows the fluid to flow in one direction from the solvent inlet to the solvent outlet. Furthermore, the sharp edge is located away from the solvent inlet, which prevents the impurity granules in the sampler from flowing back from the solvent inlet to the solvent injection means.

[0023] A second aspect of the present invention provides a thin-layer chromatography-mass spectrometry combined system, comprising the thin-layer chromatography extraction device in the above technical solution.

[0024] A third aspect of the present invention is a sampling step in which the sharp edge of the sampler is pressed against the adsorbent layer of the thin layer chromatography plate and then lifted to cut out a predetermined volume of the adsorbent; an extraction step of injecting a solvent into the sampler to extract the analytes in the sorbent; and a filtration step of filtering the solvent in which the analyte has been extracted, obtained in the extraction step.

[0025] As a preferred technical solution, the thin layer chromatography extraction method includes: The method further includes a detection step of transferring the solvent filtered in the filtering step to a mass spectrometer for detection. [Brief description of the drawings]

[0026] [Figure 1] FIG. 1 is a structural schematic diagram of a thin-layer chromatography extraction device according to a first embodiment of the present invention. [Diagram 2] FIG. 1 is a structural schematic diagram of a preferred filter in a thin layer chromatography extraction device according to a first embodiment of the present invention; [Diagram 3] FIG. 2 is a schematic diagram showing the structure of yet another preferred filter in a thin layer chromatography extraction device according to the first embodiment of the present invention. [Figure 4] FIG. 1 is a partially enlarged view of a thin layer chromatography extraction device according to a first embodiment of the present invention. [Diagram 5] FIG. 2 is a structural schematic diagram of a thin-layer chromatography-mass spectrometry combined system according to a second embodiment of the present invention. [Figure 6] 1 is a flowchart of a thin layer chromatography extraction method according to a third embodiment of the present invention. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0027] Hereinafter, the embodiments of the present invention will be described with reference to the drawings. Those skilled in the art will understand that these embodiments are merely for illustrating the technical principles of the present invention, and are not intended to limit the scope of the present invention.

[0028] [First embodiment] FIG. 1 is a structural schematic diagram of a thin layer chromatography extraction apparatus according to an embodiment of the present invention, and the thin layer chromatography extraction apparatus 100 includes a sampler 2, a solvent injection means 3, and a filter 1.

[0029] Here, the sampler 2 is formed as a through cavity structure, and the opposing sides of the cavity structure have two through openings, one of which is a solvent inlet 21 and the other is a solvent outlet 22. In particular, the inner wall of the cavity at the solvent outlet end of the sampler 2 is formed as a sharp edge 221 for cutting and removing a predetermined volume of adsorbent from the adsorption layer of the thin-layer chromatography plate, and the sharp edge 221 here refers to a sharp edge formed by extending outward so that the inner wall of the solvent outlet 22 itself becomes gradually thinner, and does not mean that both inner walls are formed into a pointed structure so as to be wrapped inward.

[0030] In this embodiment, the shape of the sharp edge 221 of the solvent outlet 22 is not limited, but the user may make the sharp edge 221 a cutting structure of any volume and shape according to the size and shape of the adsorbent sample. Preferably, the sharp edge 221 is annular, with an inner diameter of 0.1-10 mm. If the sharp edge 221 is an annular edge with an inner diameter of 0.1-10 mm, after pressing and cutting the adsorbent layer, the cut annular adsorbent is clamped to the inner wall of the annular edge by the edge performing the cutting, and later, the solvent injection means 3 and the filter 1 are attached to both ends of the sampler 2, respectively, and the extraction solvent is injected into the sampler 2, so that extraction can be performed.

[0031] The solvent injection means 3 is provided at the solvent inlet end of the sampler 2 and is used to inject a certain amount of extraction solvent into the sampler 2. The solvent injection means 3 may be any liquid extraction / injection means, such as a piston reciprocating pump, a liquid pump, a peristaltic pump, a syringe, etc. In some preferred embodiments, the solvent injection means 3 is a syringe (not shown in FIG. 1), and the syringe referred to in this embodiment is a syringe structure having a piston and a syringe outlet without a syringe tip, and the outlet of the syringe is usually a small-diameter pipe for easy detachable connection to the solvent inlet 21 of the sampler 2. Therefore, the structure of the syringe is simple and suitable for mass production. In addition, the solvent injection means 3, the sampler 2, and the filter 1 are all detachable structures, which makes it more portable and applicable to more detection situations. In another preferred embodiment, the solvent injection means 3 is a liquid pump, and the liquid pump as the solvent injection means 3 can automatically push the solvent according to the settings, eliminating the need for manual operation and allowing the amount of extraction solvent pushed in to be precisely controlled.

[0032] Alternatively, the solvent injection means 3 may be directly connected to a solvent storage device. By extracting the solvent from the solvent storage device and injecting it directly into the sampler 2, the trouble of refilling the solvent after it is used up is eliminated, making the use of the solvent more convenient in a fixed location (e.g., a laboratory). Alternatively, the solvent injection means 3 may be portable and pre-loaded with one or more doses of solvent, thereby adapting to more mobile detection situations.

[0033] The filter 1 may be detachably installed at the solvent outlet end of the sampler 2, and the filter 1 may be any filtering device having a filtering membrane, fine pores, or mesh structure for filtering large granular substrate materials. For example, in some embodiments, the filter 1 may be a filter material that is directly attached to the solvent outlet 22 of the sampler 2 and matches the shape of the solvent outlet 22 of the sampler 2 to filter the solvent flowing out of the sampler 2. In other embodiments, the filter 1 may be a separately installed filtering chamber structure, and the solvent flowing out of the solvent outlet 22 of the sampler 2 enters the filtering chamber of the filter 1, is filtered by the filtering device in the chamber, and then flows out of the outlet of the chamber. Preferably, the inlet end of the filter 1 is consistent with the aperture of the solvent outlet 22 of the sampler 2, and the other end is formed as a busbar with a small aperture, so that the extracted solvent is filtered and then merged, and is easily injected into the subsequent detection device as a small flux.

[0034] FIG. 2 is a schematic diagram showing the structure of a preferred filter in a thin layer chromatography extraction device according to an embodiment of the present invention.

[0035] As shown in FIG. 2, the filter 1 is a chip-type filter 11. Here, the chip-type filter 11 is a tubular structure having a wide-diameter filtration chamber 111 and a narrow-diameter syringe outlet 112, which is similar to the tip of a syringe. A filtration structure (e.g., a filtration membrane, a screen, a fine hole, etc.) is installed in the filtration chamber 111, so that the flow rate of the solvent after extraction can be reduced in the wide-diameter filtration chamber 111, which makes it convenient for the solvent to be filtered by the filtration structure and then flow out through a narrow-diameter bath. In particular, a disposable chip-type filter 11 can be adopted, in which case there is no need to replace the filter material, the possibility of clogging is low, and the risk of cross-contamination between samples can be reduced.

[0036] FIG. 3 is a schematic diagram showing the structure of another preferred filter in a thin layer chromatography extraction device according to an embodiment of the present invention.

[0037] As shown in FIG. 3, the filter 1 is connected to the solvent outlet 22 and is a syringe tip 12 with an inner diameter of 0.05-0.5 mm. The syringe tip 12 is a long and thin needle tube 121 structure attached to the tip of the syringe, one end of the syringe tip 12 is fitted into the solvent outlet 22 of the sampler 2, and the other end is formed as a long and thin needle tube 121, where the inner diameter refers to the inner diameter of the long and thin needle tube 121. Since large granular substrate material cannot pass through the syringe tip 12 with an inner diameter of 0.05-0.5 mm, the extracted solvent is directly filtered by the syringe tip 12 and merges to form a small flux. This eliminates the need to install a filtration chamber 111 and a filtration material, and can avoid dilution of the sample by excess solvent in the filtration chamber 111.

[0038] In this embodiment, for a mixture having a complex composition, first, multiple components in the mixture are separated by thin layer chromatography, and the separated adsorption layer of the thin layer chromatography plate is further subjected to extraction processing by the thin layer chromatography extraction device 100, and then transferred to a subsequent detection device for substance detection. Specifically, for the separated adsorption layer, the sampler 2 of the thin layer chromatography extraction device 100 presses and cuts the area that needs to be further detected, and a predetermined volume of adsorbent is taken, and then the filter 1 is attached to the solvent outlet end of the sampler 2, and the solvent is injected into the solvent inlet end of the sampler 2 by the solvent injection means 3, so that the adsorbent is extracted so that the solvent permeates the adsorbent, and the extracted solvent flows out from the solvent outlet 22 on the opposite side and flows into the filter 1 to be filtered, and the filtered solvent is directly injected into the subsequent detection device for detection.

[0039] In the thin layer chromatography extraction device according to this embodiment, instead of in-line extraction, the adsorbent can be cut out from the thin layer chromatography plate, and the extracted solvent can be directly transferred to the subsequent detection device without a complex pipeline system, so the device is simple and has high operational flexibility, which is more suitable for sampling inspection of a specific area of ​​the adsorbent layer after thin layer chromatography separation in daily detection. In addition, since the solvent is directly passed through the adsorbent layer of the thin layer chromatography plate to perform extraction, there is no need to repeat extraction. In addition, a disposable chip-type filter can be adopted, which can reduce the risk of clogging of the pipeline due to the cracking of the substrate material.

[0040] FIG. 4 is a partially enlarged view of the thin layer chromatography extraction device according to an embodiment of the present invention.

[0041] As shown in Fig. 4, in the thin layer chromatography extraction apparatus 100, the sampler 2 further includes a throttle port 31 provided between the solvent outlet 22 and the solvent inlet 21. The throttle port 31 may be a mechanism such as a check valve that regulates the one-way flow of the solvent from the solvent inlet 21 to the solvent outlet 22 and prevents the solvent from flowing back from the solvent outlet 22 to the solvent inlet 21, and since a sharp edge 221 is provided at the solvent outlet 22, it is possible to prevent the impurity granules (generally the substrate material of the adsorbent) in the sampler 2 from entering the solvent injection means 3 with the backflow of the solvent and contaminating the solvent.

[0042] In this embodiment, the sampler 2 of the thin layer chromatography extraction apparatus 100 can directly sample a specific area in the adsorption layer after thin layer chromatography separation, and perform solvent extraction by passing through the adsorbent. At the same time, the structural design of the filtration device can filter out large granules of substrate material in the solvent after extraction, and finally realize the confluence of the solvent at the outlet of the filter 1, which can be injected into the subsequent detection device for further detection of the analyte.

[0043] [Second embodiment] FIG. 5 is a structural schematic diagram of a thin-layer chromatography-mass spectrometry combined system according to a second embodiment of the present invention.

[0044] As shown in FIG. 5, the combined thin layer chromatography-mass spectrometry system includes a thin layer chromatography extraction device 100, in which the thin layer chromatography extraction device 100 is used as a sampling device for a mass spectrometer 200, and the solvent outlet 22 is provided for communication with a sampling port 201 of the mass spectrometer 200.

[0045] In addition, Figure 5 illustrates an example in which filter 1 is a syringe tip 12 and the sampling port of mass spectrometer 200 is connected to the outlet of filter 1 of thin layer chromatography extraction apparatus 100, but the present invention is not limited to this, and any combined thin layer chromatography-mass spectrometry system formed by mass spectrometer 200 being connected to any of the thin layer chromatography extraction apparatuses 100 in the first embodiment is included within the scope of protection of the present invention.

[0046] In this embodiment, the thin layer chromatography extraction apparatus 100 and the mass spectrometer 200 are used in combination, so that the composition of a complex mixture can be more easily detected. Thin layer chromatography can separate different components in a mixed substance, and the separated analytes are located in different regions on the adsorption layer of the thin layer chromatography plate, and the adsorbent in a predetermined region is obtained by pressing and cutting with the sampler 2 of the thin layer chromatography extraction apparatus 100 of the present invention, and the solvent permeates the adsorbent and extracts it, then flows out from the solvent outlet 22, and after filtration, it is directly transferred to the sampling port 201 of the mass spectrometer 200 to detect the substance components, which makes it easy to separate and detect a complex mixture. In particular, the mass spectrometer may be a mass spectrometer for direct analysis, but the efficiency of substance analysis can be further improved by using the thin layer chromatography extraction apparatus of this embodiment in combination with a mass spectrometer equipped with a direct analysis ion source.

[0047] [Third embodiment] FIG. 6 is a flow chart of a thin layer chromatography extraction method according to a third embodiment of the present invention. As shown in FIG. 6, the thin layer chromatography extraction method includes: A sampling step S1 in which the sharp edge of the sampler is pressed against the adsorbent layer of the thin layer chromatography plate and then lifted up to cut out a predetermined volume of the adsorbent; an extraction step S2 of injecting a solvent into the sampler to extract the analytes in the sorbent; and a filtering step S3 of filtering the solvent in which the analyte has been extracted, obtained in the extraction step.

[0048] Preferably, the thin layer chromatography extraction method further includes a detection step S4 of transferring the solvent filtered by the filtering step S3 to a mass spectrometer 200 for detection.

[0049] Specifically, see Figures 1 and 6. First, the mixture is subjected to detection by thin layer chromatography to complete the separation of the components of the mixture. After performing a sampling step S1 for the separated adsorption layer, the sharp edge 221 of the sampler 2 of the thin layer chromatography extraction device 100 is used to press the area of ​​the adsorption layer of the thin layer chromatography plate that needs further detection, thereby cutting out a predetermined volume of the adsorbent and holding it within the sharp edge 221 of the solvent outlet 22 of the sampler 2, a filter 1 is attached to the solvent outlet end of the sampler 2, a solvent is injected into the solvent inlet end of the sampler 2 by the solvent injection means 3, the adsorbent is extracted so that the solvent permeates the adsorbent, an extraction step S2 is performed so that the solvent carrying the analyte flows out from the solvent outlet 22 of the sampler 2 by extraction, and a filtration step S3 is performed in which the solvent carrying the analyte enters the filter 1 installed at the solvent outlet end of the sampler 2 and is filtered. The specific filtration method may be mesh filtration, membrane filtration or small diameter pipe filtration, and the filtered solvent finally flows from the outlet of the filter 1 into the sampling port of the mass spectrometer 200 for detection by performing the filtration step S3.

[0050] Although the technical solutions of the present invention have been described above with reference to the drawings, it is obvious to those skilled in the art that the scope of protection of the present invention is not limited to these specific embodiments. Without departing from the principles of the present invention, those skilled in the art may make equivalent modifications or replacements to the relevant technical features, and all such modified or replaced technical solutions fall within the scope of protection of the present invention. [Explanation of symbols]

[0051] 100-thin layer chromatography extraction apparatus; 200-mass spectrometer; 201-sampling port; 1-filter; 11-tip type filter; 111-filtration chamber; 112-syringe outlet; 12-syringe tip; 121-long thin needle tube; 2-sampler; 21-solvent inlet; 22-solvent outlet; 221-sharp edge; 3-solvent injection means; 31-aperture.

Claims

1. 1. A thin layer chromatography extraction apparatus comprising: a sampler having a solvent inlet and a solvent outlet; a solvent injection means communicating with the solvent inlet; a filter detachably provided at the solvent outlet, A thin layer chromatography extraction device characterized in that the solvent outlet has a sharp edge for cutting out a predetermined volume of adsorbent from an adsorbent layer of a thin layer chromatography plate, and the cut out adsorbent is retained between the solvent inlet and the solvent outlet.

2. 2. The thin layer chromatography extraction device according to claim 1, wherein the filter is a chip-type filter.

3. 2. The thin layer chromatography extraction apparatus according to claim 1, wherein the filter is connected to the solvent outlet and is a syringe tip having an inner diameter of 0.05-0.5 mm.

4. The thin layer chromatography extraction device according to any one of claims 1 to 3, characterized in that the thin layer chromatography extraction device is used as a sampling device for a mass spectrometer, and the solvent outlet is connected to a sampling port of the mass spectrometer.

5. 4. The thin layer chromatography extraction apparatus according to claim 1, wherein the solvent injection means is a syringe, and the outlet of the syringe is removably connected to the solvent inlet of the sampler.

6. 4. The thin layer chromatography extraction apparatus according to claim 1, wherein the solvent injection means is a liquid pump.

7. 2. The thin layer chromatography extraction device according to claim 1, wherein the sharp edge is annular and has an inner diameter of 0.1-10 mm.

8. 2. The thin layer chromatography extraction apparatus according to claim 1, wherein the sampler further comprises a throttle port provided between the solvent outlet and the solvent inlet.

9. A thin-layer chromatography-mass spectrometry combined system comprising the thin-layer chromatography extraction device according to any one of claims 1 to 3 and 7 to 8.

10. 1. A thin layer chromatography extraction method comprising the steps of: a sampling step in which the sharp edge of the sampler is pressed against the adsorbent layer of the thin layer chromatography plate and then lifted to cut out a predetermined volume of the adsorbent; an extraction step of injecting a solvent into the sampler to extract the analytes in the sorbent; and a filtration step of filtering the solvent in which the analyte has been extracted, obtained in the extraction step.

11. The thin layer chromatography extraction method according to claim 10, further comprising a detection step of transferring the solvent filtered by the filtering step to a mass spectrometer for detection.

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