CN221061817U - Solid phase extraction auxiliary device - Google Patents

Abstract

The utility model discloses a solid phase extraction auxiliary device, which relates to the technical field of solid phase extraction, and structurally comprises an auxiliary tube; the lower part of auxiliary pipe is the back taper, the top of auxiliary pipe is equipped with the import, and the bottom is equipped with the export, the diameter of import is greater than the export. According to the solid-phase extraction auxiliary device provided by the utility model, the auxiliary pipe is sleeved at the bottom of the solid-phase extraction column, so that the rapid solid-phase extraction is realized, and the time can be shortened by about 50%; the pollution of volatile liquid in the waste liquid cylinder and the environment to the outlet of the solid phase extraction column is basically isolated, so that the purity of the extracted substance to be detected is higher, and the detection result is more accurate.

Description

Solid phase extraction auxiliary device

Technical Field

The utility model relates to the technical field of solid phase extraction, in particular to a solid phase extraction auxiliary device.

Background

The solid phase extraction technology (Solid Phase Extraction, SPE for short) is developed by combining a liquid-solid extraction column and a liquid chromatography technology, and is mainly used for separating, purifying and concentrating samples. Compared with the traditional liquid-liquid extraction method, the solid-phase extraction technology can improve the recovery rate of the analyte, more effectively separate the analyte from the interference component, reduce the pretreatment process of the sample, and has simple operation, time saving and labor saving. The solid phase extraction technology is widely applied to the fields of medicine, food, environment, commercial inspection, chemical industry and the like.

The more commonly used solid phase extraction method is to make the liquid sample solution pass through the solid adsorbent, so that the substance to be detected is kept in the solid phase extractant according to the difference of the acting force of the component to be detected and the coexistent interfering component on the solid phase extractant, then the impurity is washed out by selecting a proper solvent, and finally the substance to be detected is quickly eluted by a small amount of solvent, thereby achieving the purposes of quick separation, purification and concentration. Of course, the solid phase extractant can be used for selectively adsorbing the interference impurities to flow out the tested substances; or simultaneously adsorbing impurities and the substance to be detected, and then selectively eluting the substance to be detected by using a proper solvent.

In the existing solid phase extraction mode, a solid phase extraction column is placed on a bracket, a liquid sample is poured into the solid phase extraction column, the liquid sample flows through a solid phase extractant, and residual liquid is dripped into a waste liquid jar or a clean test tube/reaction tube positioned below from an outlet at the bottom of the solid phase extraction column. The solid phase extraction can be classified into a positive pressure method, a negative pressure method and a gravity method according to the column passing manner. The positive pressure method and the negative pressure method, although greatly improving the column passing speed and shortening the solid phase extraction time, all require additional equipment and are inconvenient for the application of on-site quick detection. In the gravity method, as the name implies, the inlet and outlet of the column are both open to the atmosphere, and the liquid flowing through the solid phase extraction column is pushed mainly by its own weight. Thus, the gravity flow rate through the column decreases as the liquid level in the column decreases. Generally, even if a 1-5mL solid phase extraction column is used, purification and concentration of 10 samples are operated by a gravity method, the column passing time is tens of minutes to hours, and for a sample with high viscosity, such as edible oil, the column passing time is longer under the condition of no pressurization or depressurization; if the number of the samples is increased again, the timeliness of the result of the sample to be detected can be prolonged intactly.

Generally, a container (i.e., a waste liquid tank) for collecting hazardous waste liquid generated in a solid phase extraction process is not cleaned in a laboratory, and is not necessary for cleaning, and only hazardous/waste liquid in the container is required to be transferred to a container specially used for storing and transferring the hazardous waste liquid. Therefore, in the practical high-flux and high-frequency detection application, the volatile organic impurities remained in the waste liquid cylinder, such as organic acid in edible oil, can pollute the column body and the lower liquid outlet of the solid-phase extraction column along with the volatilization of the organic waste liquid in the waste liquid cylinder, and can be reintroduced into the sample during elution, thus causing certain interference to the final detection result.

Disclosure of Invention

In order to solve the problems of the prior art, the utility model provides a solid phase extraction auxiliary device, which is realized by the following technical scheme.

A solid phase extraction auxiliary device comprises an auxiliary pipe; the lower part of auxiliary pipe is the back taper, the top of auxiliary pipe is equipped with the import, and the bottom is equipped with the export, the diameter of import is greater than the export.

The solid phase extraction auxiliary device provided by the utility model is generally used for adsorbing and staying substances to be detected in a solid phase extraction column. The device can accelerate the sample passing through the solid phase extraction column, and remarkably shortens the extraction time; but also effectively avoids the influence of volatile organic impurities on the outlet at the bottom of the solid-phase extraction column, and solves the problem of interference of residual organic impurities in the recovered substances to be detected.

The use method of the solid phase extraction auxiliary device comprises the steps of placing an auxiliary pipe in a vertical state or holding the auxiliary pipe vertically by the same hand; the solid phase extraction column is downwards inserted into the auxiliary tube, approximate sealing is formed between the outer wall of the solid phase extraction column and the inner wall of the auxiliary tube, and the auxiliary tube is placed above the waste liquid cylinder; adding an organic reagent or a sample solution to be purified, slowly passing through the solid phase extractant under the action of gravity and capillary adsorption of the solid phase extractant, and dripping the organic reagent or the sample solution to be purified into the auxiliary tube dropwise from the bottom of the solid phase extraction column; when the effluent liquid is accumulated in the auxiliary pipe to a certain amount, continuously dripping the effluent liquid from the outlet of the auxiliary pipe into the waste liquid cylinder, and simultaneously continuously and rapidly dripping new solution from the bottom of the solid phase extraction column into the auxiliary pipe; the organic reagent in the solid phase extraction column or the sample solution to be purified is completely subjected to the solid phase extraction agent to complete 1 extraction step.

In the conventional solid phase extraction operation process, a solid phase extraction column is fixed above a waste liquid container, an organic reagent or a sample solution to be purified is directly added, and the extraction steps are completed after the organic reagent or the sample solution to be purified completely flows out of the solid phase extraction column. After a large number of comparison experiments, it is found that when the conventional solid phase extraction operation (namely no additional equipment is provided and the reagent or the sample solution is pushed by gravity of the reagent or the sample solution to pass through the column) is adopted, the speed of dropping liquid at the bottom of the solid phase extraction column is very slow; the device of the utility model is adopted to carry out solid phase extraction, the liquid level descending speed in the solid phase extraction column is obviously accelerated by naked eyes, and the liquid dropping speed at the bottom of the solid phase extraction column is obviously accelerated, namely the extraction speed is obviously accelerated. Through measurement and calculation, the time required by the solid phase extraction by adopting the device can be shortened by about 50 percent.

When the micro sample is subjected to solid phase extraction, the speed difference between the conventional solid phase extraction and the operation by adopting the device is larger due to the small volume of the liquid and the influence of surface tension, viscosity and adsorption. This means that the effect of shortening the solid phase extraction time of the device is more remarkable when the solid phase extraction of the trace sample is performed.

Although the above technical effects are observed, the mechanism of action thereof is still in need of further study. The whole liquid extraction process and its presumed principle are:

(1) When the first liquid drops from the liquid outlet of the extraction column to the outlet of the auxiliary pipe, the liquid does not drop out of the outlet immediately because the caliber of the outlet of the auxiliary pipe is smaller and the outlet of the auxiliary pipe is in an inverted cone shape, so that a temporary liquid seal is formed at the outlet of the auxiliary pipe;

After the bottom of the solid phase extraction column is hermetically connected with the auxiliary pipe, a sealed space is formed inside the auxiliary pipe, and at the moment, the air pressure in the sealed space is temporarily equal to the atmospheric pressure;

(2) The organic solvent in the first drop of liquid forms an aerosol layer around the outlet of the auxiliary pipe, so that the friction force between the liquid and the inner wall of the auxiliary pipe is reduced; the second drop of liquid continuously drops due to self gravity and inertia, and after the second drop of liquid drops to the outlet of the auxiliary pipe, a small amount of air in the auxiliary pipe is flushed into the liquid at the outlet part due to the gravity of the liquid at the outlet part and the impact force of the second drop of liquid, and flows out from the outlet of the auxiliary pipe along with the liquid;

(3) As the liquid and a small amount of air in the auxiliary pipe flow out from the outlet in a short time, negative pressure is formed in the auxiliary pipe in a short time; liquid in the extraction column rapidly passes through the filler under the pushing of atmospheric pressure and continuously drops to the outlet part of the auxiliary pipe from the liquid outlet, the liquid at the outlet part of the auxiliary pipe is pushed by the atmospheric pressure and rises at the same time, and the external air enters from the outlet of the auxiliary pipe at the same time; finally, temporary air pressure balance is achieved again;

(4) Along with the continuous dripping of the subsequent third drop and fourth drop of liquid into the auxiliary pipe from the liquid outlet of the extraction column, the liquid flows out from the outlet of the auxiliary pipe under the action of self gravity, drop impact force and the like.

The above principle of action is estimated based on the actual states of the liquid and the liquid surface in the auxiliary pipe, and the specific principle thereof needs to be further studied.

In order to achieve the above technical effects of the present invention, the aperture of the outlet at the bottom of the auxiliary tube needs to be small enough to allow the droplets falling from the solid phase extraction column to form a liquid seal at the outlet.

In the solid phase extraction, other auxiliary clamps are generally used for clamping the solid phase extraction column. The core of the solid phase extraction auxiliary device provided by the utility model is that an auxiliary pipe is inserted below the solid phase extraction column. Therefore, as long as the above functional requirements of the auxiliary tube are satisfied, the fixing manner of the auxiliary tube itself may be determined according to the actual situation (for example, the number of test groups), and may be fixed by a tool such as a ready-made jig or a hole plate frame, or may be held by hand.

It should be noted that, at present, the commercialization degree of the solid phase extraction column is very high, and there are a large number of solid phase extraction columns with different thicknesses and lengths according to the requirements in the market. These commercial solid phase extraction columns are typically plastic in nature and may be glass if they are self-made. Therefore, the solid phase extraction auxiliary device provided by the utility model needs to use materials which have certain ductility and can wrap and attach the solid phase extraction column, such as soft plastics and the like; or the sealing structure is arranged on the auxiliary pipe to realize the attaching sealing of the solid phase extraction column. The final purpose of the solid phase extraction column is to insert the solid phase extraction column into the auxiliary tube, and then the inverted cone-shaped part at the lower part of the auxiliary tube can be automatically attached to the bottom end of the solid phase extraction column to form a completely sealed or nearly completely sealed state.

By using the device, the solid phase extraction column is completely sealed or nearly completely sealed by the auxiliary pipe, and the outlet at the bottom end of the solid phase extraction column is positioned in the auxiliary pipe, so that the pollution of the waste liquid cylinder and volatile liquid in the environment to the outlet of the solid phase extraction column is basically isolated, the purity of the extracted substance to be detected is higher, and the detection result is more accurate. The diameter of the outlet at the bottom of the auxiliary tube is very small, and substantially no volatile waste liquid enters the interior of the auxiliary tube from the outlet.

Preferably, the top end of the auxiliary tube is provided with a sealing structure.

More preferably, the sealing structure is a structure composed of an elastic material.

More preferably, the sealing structure is a rubber ring arranged at the inlet position.

In order to achieve the purpose of attaching the outer wall of the solid phase extraction column to the inner wall of the auxiliary tube, a sealing structure is arranged at the top end of the auxiliary tube. It should be noted that, this sealing structure may be realized by selecting materials for the auxiliary tube, or may be realized by a physical structure. For example, soft plastic can be selected as the material, and when the solid phase extraction column extrudes the auxiliary tube, the wall of the auxiliary tube made of soft plastic is deformed and then is naturally attached to the outer wall of the solid phase extraction column. For example, a rubber ring with a sealing function is additionally arranged at the top end of the auxiliary pipe, and the rubber ring is deformed by extrusion, so that the sealing purpose can be achieved.

Preferably, the device further comprises a bracket, and the auxiliary tube is positioned on the bracket. In order to facilitate the vertical fixation of the auxiliary pipe, a bracket can be additionally arranged for matching use.

Preferably, the number of the auxiliary tubes is not less than 2, and is regularly arranged on the bracket.

Preferably, the auxiliary tube is detachably arranged with the bracket.

More preferably, the auxiliary tube and the bracket are detachably arranged through a thread structure.

More preferably, the bracket comprises a first support plate and a second support plate which are arranged up and down, wherein a first through hole is formed in the first support plate, and a second through hole corresponding to the first through hole is formed in the second support plate; the aperture of the first through hole is larger than that of the second through hole; the apertures of the first through hole and the second through hole are smaller than the maximum diameter of the inverted cone-shaped part of the auxiliary pipe, or the aperture of the first through hole is not smaller than the outer diameter of the solid phase extraction column.

Compared with the prior art, the utility model has the beneficial effects that: according to the solid-phase extraction auxiliary device provided by the utility model, the auxiliary pipe is sleeved at the bottom of the solid-phase extraction column, so that the rapid solid-phase extraction is realized, and the time can be shortened by about 50%; the pollution of volatile liquid in the waste liquid cylinder and the environment to the outlet of the solid phase extraction column is basically isolated, so that the purity of the extracted substance to be detected is higher, and the detection result is more accurate.

Drawings

FIG. 1 is a schematic diagram of the internal structure of a solid phase extraction auxiliary device according to an embodiment;

FIG. 2 is a schematic diagram showing the internal structure of a solid phase extraction auxiliary device and a solid phase extraction column according to the embodiment;

FIG. 3 is a schematic view showing a 1 st preferred structure of the solid phase extraction auxiliary device according to the embodiment;

FIG. 4 is a schematic view showing a 2 nd preferred structure of the solid phase extraction auxiliary device according to the embodiment;

FIG. 5 is a schematic view showing a 3 rd preferred structure of the solid phase extraction auxiliary device according to the embodiment;

FIGS. 6 and 7 are schematic views showing a 4 th preferred structure of the solid phase extraction auxiliary device according to the embodiment;

In the figure: 1. an auxiliary tube; 2. an inlet; 3. an outlet; 4. a sealing structure; 5. a bracket; 6. a thread structure; 7. a first support plate; 8. a second support plate; 9. a first through hole; 10. and a second through hole.

Detailed Description

The following description of the embodiments of the present patent will be made clearly and completely with reference to the accompanying drawings, and it is apparent that the described embodiments are only some embodiments of the present patent, but not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the one of ordinary skill in the art based on the embodiments of this patent, are within the scope of protection of this patent.

In the description of this patent, it should be noted that, directions or positional relationships indicated by terms such as "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", "top", etc., are based on directions or positional relationships shown in the drawings, are merely for convenience of description of this patent and for simplification of description, and do not indicate or imply that the apparatus or element to be referred to must have a specific direction, be configured and operated in a specific direction, and thus should not be construed as limiting the patent. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.

In the description of this patent, it should be noted that, unless explicitly stated and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. It is noted that all of the figures are exemplary representations. The specific meaning of the terms in this patent will be understood by those of ordinary skill in the art in a specific context.

The present patent is described in further detail below by way of specific examples of embodiments and with reference to the accompanying drawings.

Examples

As shown in fig. 1 and 2, the solid phase extraction auxiliary device provided in this embodiment includes an auxiliary tube 1; the lower part of the auxiliary pipe 1 is in an inverted cone shape, the top end of the auxiliary pipe 1 is provided with an inlet 2, the bottom end of the auxiliary pipe is provided with an outlet 3, and the diameter of the inlet 2 is larger than that of the outlet 3.

The above-mentioned solid phase extraction auxiliary device is generally used in the case of adsorbing and retaining the substance to be detected in the solid phase extraction column. The auxiliary tube is made of soft plastic, the inlet at the top of the auxiliary tube is used for being inserted into the solid phase extraction column, and the outlet at the bottom of the auxiliary tube is used for flowing out waste liquid. In order to facilitate the formation of a liquid seal from the waste liquid, the diameter of the outlet needs to be set to be smaller.

In the solid phase extraction, as shown in fig. 2, other auxiliary jigs are generally used to clamp the solid phase extraction column. The auxiliary pipe of the solid phase extraction auxiliary device is made of soft plastic, so that the solid phase extraction column is inserted into the auxiliary pipe forcefully, and the auxiliary pipe can be naturally attached to the side wall of the solid phase extraction column by extrusion to form a seal. Therefore, as long as the above functional requirements of the auxiliary tube are satisfied, the fixing manner of the auxiliary tube itself may be determined according to the actual situation (for example, the number of test groups), and may be fixed by a tool such as a ready-made jig or a hole plate frame, or may be held by hand.

The application method of the solid phase extraction auxiliary device comprises the following steps: placing the auxiliary pipe in a vertical state or holding the auxiliary pipe vertically by the same hand; the solid phase extraction column is downwards inserted into the auxiliary tube, a nearly complete sealing state is formed between the outer wall of the solid phase extraction column and the inner wall of the auxiliary tube, and the auxiliary tube is placed above the waste liquid cylinder; adding an organic reagent or a sample solution to be purified, allowing the solution to flow through the solid phase extraction agent, and dropwise dripping the effluent liquid into the auxiliary tube from the bottom of the solid phase extraction column; after the organic reagent or the sample solution to be purified in the solid-phase extraction column flows out completely, the solid-phase extraction column can be taken away for subsequent operation steps; the waste liquid in the auxiliary pipe automatically and continuously drops into the waste liquid cylinder.

After a large number of comparison experiments, it is found that when the conventional solid phase extraction operation (namely no additional equipment is provided and the reagent or the sample solution is pushed by gravity of the reagent or the sample solution to pass through the column) is adopted, the speed of dropping liquid at the bottom of the solid phase extraction column is very slow; the device of the utility model is adopted to carry out solid phase extraction, the liquid level descending speed of the sample in the solid phase extraction column is obviously accelerated by naked eyes, and the liquid dropping speed at the bottom of the solid phase extraction column is obviously accelerated, namely the extraction speed is obviously accelerated. Through measurement and calculation, the time required by the solid phase extraction by adopting the device can be shortened by about 50 percent. Because the auxiliary pipe protects the bottom of the solid phase extraction column, the pollution of volatile liquid in the waste liquid cylinder and the environment to the column body and the liquid outlet of the solid phase extraction column is basically isolated, and the volatile waste liquid can not diffuse into the auxiliary pipe from the outlet at the bottom of the auxiliary pipe, so that the influence of volatile organic impurities on the outlet at the bottom of the solid phase extraction column can be effectively avoided, and the problem of residual organic impurity interference in the recovered substance to be detected is solved.

Preferably, as shown in fig. 3, the top end of the auxiliary tube 1 is provided with a sealing structure 4, and optionally, the sealing structure 4 is a rubber ring arranged at the position of the inlet 2.

Preferably, as shown in fig. 4, the solid phase extraction auxiliary device provided in this embodiment further includes a support 5, and the auxiliary tube 1 is located on the support 5;

Alternatively, the number of the auxiliary pipes 1 is not less than 2, and is regularly arranged on the bracket 5.

Preferably, as shown in fig. 5, the auxiliary tube 1 and the bracket 5 are detachably arranged through a screw structure 6.

Preferably, as shown in fig. 6 and 7, the bracket 5 comprises a first support plate 7 and a second support plate 8 which are arranged up and down, the first support plate 7 is provided with a first through hole 9, and the second support plate 8 is provided with a second through hole 10 corresponding to the first through hole 9; the aperture of the first through hole 9 is larger than that of the second through hole 10; the apertures of the first through hole 9 and the second through hole 10 are smaller than the maximum diameter of the inverted cone portion of the auxiliary tube 1, or the aperture of the first through hole 9 is not smaller than the outer diameter of the solid phase extraction column.

The above examples describe in detail the practice of the utility model, but the utility model is not limited to the specific details of the above embodiments. Many simple modifications and variations of the technical solution of the present utility model are possible within the scope of the claims and technical idea of the present utility model, which simple modifications are all within the scope of the present utility model.

Claims (9)

1. The solid phase extraction auxiliary device is characterized by comprising an auxiliary pipe; the lower part of auxiliary pipe is the back taper, the top of auxiliary pipe is equipped with the import, and the bottom is equipped with the export, the diameter of import is greater than the export.

2. The solid phase extraction auxiliary device according to claim 1, wherein the top end of the auxiliary tube is provided with a sealing structure.

3. The solid phase extraction auxiliary device according to claim 2, wherein the sealing structure is a structure composed of an elastic material.

4. The solid phase extraction auxiliary device according to claim 2, wherein the sealing structure is a rubber ring arranged at the inlet position.

5. The solid phase extraction aid according to any one of claims 1-4, further comprising a support, the aid tube being located on the support.

6. The solid phase extraction auxiliary apparatus according to claim 5, wherein the number of auxiliary tubes is not less than 2 and is regularly arranged on the rack.

7. The solid phase extraction auxiliary device according to claim 5, wherein the auxiliary tube is detachably arranged between the support and the support.

8. The solid phase extraction auxiliary device according to claim 7, wherein the auxiliary tube and the bracket are detachably arranged through a thread structure.

9. The solid phase extraction auxiliary device according to claim 5, wherein the bracket comprises a first support plate and a second support plate which are arranged up and down, a first through hole is formed in the first support plate, and a second through hole corresponding to the first through hole is formed in the second support plate; the aperture of the first through hole is larger than that of the second through hole; the apertures of the first through hole and the second through hole are smaller than the maximum diameter of the inverted cone-shaped part of the auxiliary pipe, or the aperture of the first through hole is not smaller than the outer diameter of the solid phase extraction column.