CN106290696B - Thin-layer chromatography system and chromatography method - Google Patents
Thin-layer chromatography system and chromatography method Download PDFInfo
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- CN106290696B CN106290696B CN201510348775.2A CN201510348775A CN106290696B CN 106290696 B CN106290696 B CN 106290696B CN 201510348775 A CN201510348775 A CN 201510348775A CN 106290696 B CN106290696 B CN 106290696B
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Abstract
The invention discloses a thin layer chromatography system and a chromatography method, wherein the method is carried out by utilizing the thin layer chromatography system and comprises the following steps: spotting by using a thin-layer chromatography plate; vertically and fixedly placing the thin layer chromatography plate by utilizing the first clamping groove and the second clamping groove; covering the upper cover; placing a prepared spreading agent into the cylinder body through a spreading agent containing container, wherein the spreading agent enters the bottom of the cylinder body through a capillary flow guide pipe of a first spreading agent groove and starts a steam saturation process; observing the steam saturation display, and controlling the amount of the expanding agent in the cylinder body through a first control valve and a second control valve; stopping the adjustment of the deployed dose when the saturation reaches the desired value; and (5) carrying out analysis detection on the thin-layer chromatography plate. Therefore, the controllable steam saturation in the chromatography process can be realized, and the developing solvent is added into the closed container, so that the experimental effect and safety are ensured.
Description
Technical Field
The invention belongs to the field of chromatographic analysis, and particularly relates to a thin-layer chromatography system and a chromatography method.
Background
Thin-layer chromatography belongs to common means in the field of pharmacy or chemical synthesis, and has the advantages of rapidness, convenience, low cost and the like for monitoring the reaction process in real time, qualitatively observing reaction products and the like, however, at present, a conventional chromatographic cylinder can only be used for placing a chromatographic plate, an organic solvent is needed in the chromatographic process, and the solvent is volatile in manual operation, so that loss is caused, physical and mental health of experimenters is not facilitated, and environment pollution is caused. On the other hand, the steam saturation in the chromatographic process is uncontrollable, and the chromatographic separation effect is easily influenced.
Therefore, the current thin layer chromatography methods are still to be further improved.
Disclosure of Invention
The present invention aims to solve at least to some extent one of the technical problems of the prior art or at least to provide a useful commercial choice. Therefore, the invention aims to provide a thin-layer chromatography system and a chromatography method, by utilizing the system, the controllability of the steam saturation in the chromatography process can be realized, and a developing solvent is added into a closed container, so that the experimental effect and the safety are ensured.
Thus, in one aspect of the invention, the invention provides a thin layer chromatography system. According to an embodiment of the invention, the system comprises:
the upper cover is provided with at least one first clamping groove;
the thin-layer chromatography plate comprises a cylinder body, wherein an open end is arranged above the cylinder body and is connected with an upper cover, the cylinder body comprises a cylinder body bottom and a cylinder body side wall, the cylinder body bottom is provided with at least one second clamping groove used for being matched with the first clamping groove to fix the thin-layer chromatography plate, the upper part of the cylinder body side wall is provided with a first developing agent groove, the wall of the first developing agent groove is provided with at least one capillary hole, the capillary hole is connected with a capillary guide pipe, the capillary guide pipe extends to the cylinder body bottom, and the cylinder body bottom is provided with a liquid outlet and a first control valve connected with the liquid outlet; and
the developing agent containing container is provided with a first regulator and an injection pipe, and the injection pipe penetrates through the upper cover to be connected with the first developing agent groove; the first regulator comprises a steam saturation display and a second control valve, the steam saturation display is provided with an induction probe, and the induction probe is arranged in the cylinder body.
Therefore, the thin-layer chromatography system according to the embodiment of the invention vertically and fixedly places the thin-layer chromatography plate by utilizing the first clamping groove on the upper cover and the second clamping groove at the bottom of the cylinder body, thereby ensuring that the developing solvent can vertically move upwards along the thin-layer plate; the spreading agent slowly and uniformly flows into the cylinder body through the first spreading agent groove and the capillary flow guide pipe thereof, and a steam saturation process is started in the flowing process of the spreading agent; and observing the steam saturation display, controlling the amount of the developing agent in the cylinder body through the first control valve and the second control valve, and stopping the adjustment of the developing agent when the saturation reaches a required value.
In addition, the thin layer chromatography system according to the embodiment of the invention may also have the following additional technical features:
in some embodiments of the present invention, the first developer tank is disposed at a distance of 1/5 to 1/4 of the height of the cylinder from the open end of the cylinder. Therefore, the steam saturation process of the expanding agent can be performed when the expanding agent flows into the cylinder body, and the uniformity of the steam saturation of the cylinder body from top to bottom can be guaranteed.
In some embodiments of the invention, the first developer tank is concave. Therefore, the developing solvent flows out through the capillary holes on the first developing solvent groove when entering the first developing solvent groove through the holding container.
In some embodiments of the invention, the capillary flow-guide is semicircular and open on one side. Thus, the developer flowing out of the capillary holes flows uniformly to the bottom of the cylinder by the capillary flow guide tube, and the vapor is formed to diffuse into the cylinder space by the opening of the capillary flow guide tube. Therefore, the quick and uniform formation of saturated steam in the cylinder body by the developing agent can be guaranteed.
In some embodiments of the invention, the cylinder is a non-transparent cylinder. This makes the system of the invention further suitable for the separation of light-sensitive substances.
In some embodiments of the invention, the cylinder body has a viewing window thereon, and the viewing window further has a height scale. Thus, the state of the thin-layer chromatography plate and the state of the developer running on the thin-layer chromatography plate can be observed. The parameters of chromatographic reaction progress time, rf value of the thin layer chromatography plate and the like can be quantitatively controlled through the height scale. Thereby making the chromatographic process controllable and repeatable.
In some embodiments of the invention, the second blocking grooves on the bottom of the cylinder body correspond to the first blocking grooves on the upper cover in one-to-one correspondence in number and position. Thus, the thin-layer chromatography plate can be placed vertically. Thereby allowing the developer to travel vertically up the thin-layer chromatography plate.
In some embodiments of the present invention, the first detent groove and the second detent groove are both snap-fit type detent grooves. Therefore, the thin-layer chromatography plate can be fixed well, and the phenomenon that the thin-layer chromatography system collapses or inclines to influence an experimental result due to accidents is avoided.
In another aspect of the invention, the invention provides a method of chromatography using the thin layer chromatography system described above. According to an embodiment of the invention, the chromatography method comprises:
(1) Spotting by using a thin-layer chromatography plate;
(2) Vertically and fixedly placing the thin layer chromatography plate by utilizing the first clamping groove and the second clamping groove, and covering an upper cover;
(3) Placing a prepared spreading agent into the cylinder body through a spreading agent containing container, so that the spreading agent enters the bottom of the cylinder body through a capillary flow guide pipe of a first spreading agent groove and starts a steam saturation process;
(4) Observing a steam saturation display, and controlling the amount of the expanding agent in the cylinder body through a first control valve and a second control valve;
(5) When the saturation reaches the required value, stopping the adjustment of the unfolded dose; and
(6) And (5) carrying out analysis detection on the thin-layer chromatography plate.
Therefore, according to the chromatography method provided by the embodiment of the invention, a plurality of thin-layer chromatography plates can be placed according to the experiment requirement, and the saturated steam in the cylinder body is controlled and adjusted, so that the chromatography process can be completed quickly, effectively and controllably, and the safety of the experiment operation can be ensured.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
FIG. 1 is a schematic diagram of the structure of a thin layer chromatography system according to one embodiment of the invention;
FIG. 2 is a schematic diagram of the structure of a first developer tank in a thin layer chromatography system according to one embodiment of the invention;
FIG. 3 is a schematic diagram of the structure of capillary flow-guide tubes in a thin layer chromatography system according to one embodiment of the invention; and
FIG. 4 is a schematic partial structure view of a thin layer chromatography system according to one embodiment of the invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative and intended to explain the present invention and should not be construed as limiting the present invention.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are not to be considered limiting of the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood according to specific situations by those of ordinary skill in the art.
In the present invention, unless otherwise expressly stated or limited, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through an intermediate. Also, a first feature "on," "above," and "over" a second feature may be directly on or obliquely above the second feature, or simply mean that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
In one aspect of the invention, a thin layer chromatography system is provided.
The thin layer chromatography system of the embodiment of the present invention is described in detail below with reference to fig. 1 to 4:
according to an embodiment of the invention, a thin layer chromatography system comprises: an upper cap 1000, a cylinder 2000 and a developer container 3000.
According to one embodiment of the present invention, the upper cover 1000 has at least one first catching groove 100; the upper part of the cylinder body 2000 is provided with an open end 200, the open end 200 is connected with the upper cover 1000, the cylinder body 2000 comprises a cylinder body bottom 300 and a cylinder body side wall 400, the cylinder body bottom 300 is provided with at least one second clamping groove 310 for matching and fixing a thin layer chromatography plate with the first clamping groove, the upper part of the cylinder body side wall 400 is provided with a first spreading agent groove 410, the wall of the first spreading agent groove 410 is provided with at least one capillary hole 411, the capillary hole 411 is connected with a capillary guide pipe 412, the capillary guide pipe 412 extends to the cylinder body bottom 300, and the cylinder body bottom 300 is provided with a liquid outlet 320 and a first control valve 330 connected with the liquid outlet; the developer holding container 3000 has a first adjustor 500 and an injection pipe 600, and the injection pipe 600 is connected to the first developer tank 410 through an upper cover 1000; the first regulator 500 comprises a steam saturation display 510 and a second control valve 520, wherein the steam saturation display 510 is provided with an inductive probe 511, and the inductive probe 511 is arranged in the cylinder body 2000.
Thus, the thin layer chromatography system according to the embodiment of the present invention vertically fixes the thin layer chromatography plate by using the first retaining groove 100 of the upper cover 1000 and the second retaining groove 310 of the bottom 300 of the cylinder body, thereby ensuring that the developing solvent can vertically move up the thin layer plate; the first developer tank 410 and the capillary guide pipe 412 thereof enable the developer to slowly and uniformly flow into the cylinder body, and the vapor saturation process is started in the flowing process; observing the vapor saturation display 510, the amount of the developer inside the cylinder is controlled by the first control valve 330 and the second control valve 520, and when the saturation reaches a required value, the adjustment with the amount of the developer is stopped.
According to an embodiment of the present invention, the first developer tank 410 is disposed at a distance of 1/5 to 1/4 of the cylinder height from the open end 200 of the cylinder. Therefore, the steam saturation process of the expanding agent can be performed when the expanding agent flows into the cylinder body, and the uniformity of the steam saturation of the cylinder body from top to bottom can be guaranteed.
According to an embodiment of the present invention, the first developer tank 410 has a concave shape. Thus, the developer enters the first developer tank 410 through the receiving container and flows out through the capillary 411 formed thereon.
According to the embodiment of the present invention, the capillary flow-guide tube 412 is semicircular and is open at one side. Thus, the developer flowing out of the capillary holes 411 flows uniformly to the cylinder bottom 300 through the capillary flow guide 412, and vapor is formed to diffuse into the cylinder space through the opening of the capillary flow guide 412. Therefore, the quick and uniform formation of saturated steam in the cylinder body by the developing agent can be guaranteed.
According to an embodiment of the present invention, the cylinder 2000 is a non-transparent cylinder. This makes the system of the invention further suitable for the separation of light-sensitive substances.
According to an embodiment of the present invention, the cylinder 2000 has a window thereon, and the window further has a height scale 700. Thus, the state of the thin layer chromatography plate and the state of the developer running on the thin layer chromatography plate can be observed. The parameters of chromatographic reaction progress time, rf value of the thin layer chromatography plate and the like can be quantitatively controlled through the height scale. Thereby making the chromatographic process controllable and repeatable.
According to the embodiment of the present invention, the second catching grooves 310 of the cylinder bottom 300 correspond to the first catching grooves 100 of the upper cover 1000 in one-to-one correspondence in number and position. Thus, the thin-layer chromatography plate can be placed vertically. Thereby allowing the developer to travel vertically up the thin-layer chromatography plate.
According to an embodiment of the present invention, the first and second detent grooves 100 and 310 are snap-fit type detent grooves. Therefore, the thin-layer chromatography plate can be fixed well, and the phenomenon that the thin-layer chromatography system collapses or inclines to influence an experimental result due to accidents is avoided.
In another aspect of the invention, the invention provides a method of chromatography using the thin layer chromatography system described above. According to an embodiment of the invention, the chromatography method comprises:
(1) Spotting by using a thin-layer chromatography plate;
(2) Vertically and fixedly placing the thin layer chromatography plate by using the first clamping groove 100 and the second clamping groove 310, and covering an upper cover;
(3) Placing a prepared developing solvent into the cylinder body through the developing solvent containing container 3000, so that the developing solvent enters the bottom 300 of the cylinder body through the capillary flow guide pipe 412 of the first developing solvent tank 410 and starts a steam saturation process;
(4) Observing the vapor saturation display 510, controlling the amount of the developing agent inside the cylinder through the first control valve 330 and the second control valve 520;
(5) Stopping the adjustment of the spread dose when the saturation reaches the desired value; and
(6) And (5) carrying out analysis detection on the thin-layer chromatography plate.
Therefore, according to the chromatography method provided by the embodiment of the invention, a plurality of thin-layer chromatography plates can be placed according to experimental needs, and the chromatography process can be completed quickly, effectively and controllably by controlling and adjusting saturated steam in the cylinder body. And the safety of experimental operation can be ensured.
The scheme of the invention will be explained with reference to the examples. It will be appreciated by those skilled in the art that the following examples are illustrative of the invention only and should not be taken as limiting the scope of the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1:
by using the thin layer chromatography system shown in fig. 1, the chromatographic detection is performed on the sample to be chromatographed according to the chromatography method of the invention, which comprises the following steps:
(1) Spotting by using a thin-layer chromatography plate;
(2) Vertically and fixedly placing the thin layer chromatography plate by using the first clamping groove 100 and the second clamping groove 310, and covering an upper cover;
(3) Placing the prepared developing solvent into the cylinder body through the developing solvent containing container 3000, so that the developing solvent enters the bottom 300 of the cylinder body through the capillary flow guide pipe 412 of the first developing solvent tank 410 and starts a steam saturation process;
(4) Observing the vapor saturation display 510, controlling the amount of the developing agent in the cylinders via the first control valve 330 and the second control valve 520;
(5) Stopping the adjustment of the spread dose when the saturation reaches the desired value; and
(6) And (5) carrying out analysis detection on the thin-layer chromatography plate.
As a result, the sample to be chromatographed is efficiently separated on the thin-layer chromatography plate. According to the result, the chromatographic detection is carried out by using the chromatographic method, and the result is accurate and reliable.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are exemplary and not to be construed as limiting the present invention, and that changes, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (5)
1. A thin layer chromatography system, comprising:
the upper cover is provided with at least one first clamping groove;
the upper part of the cylinder body is provided with an opening end, the opening end is connected with the upper cover, the cylinder body comprises a cylinder body bottom and a cylinder body side wall, the bottom of the cylinder body is provided with at least one second clamping groove used for fixing a thin layer chromatography plate in a matching way with the first clamping groove, the upper part of the cylinder body side wall is provided with a first spreading agent groove, the wall of the first spreading agent groove is provided with at least one capillary hole, the capillary hole is connected with a capillary guide pipe, the capillary guide pipe extends to the bottom of the cylinder body, and the bottom of the cylinder body is provided with a liquid outlet and a first control valve connected with the liquid outlet; and
the spreading agent containing container is provided with a first regulator and an injection pipe, the injection pipe penetrates through the upper cover to be connected with the first spreading agent groove, the first regulator comprises a steam saturation display and a second control valve, the steam saturation display is provided with an induction probe, the induction probe is arranged in the cylinder body,
the first spreading agent groove is arranged at the position which is 1/5-1/4 of the height of the cylinder body away from the opening end of the cylinder body;
the capillary guide pipe is semicircular, and one side of the capillary guide pipe is open;
the second clamping grooves at the bottom of the cylinder body are the same as the first clamping grooves of the upper cover in number and correspond to the first clamping grooves of the upper cover in position one by one;
the first clamping groove and the second clamping groove are both buckle type clamping grooves.
2. The thin layer chromatography system of claim 1, wherein the first developer tank is concave.
3. The thin layer chromatography system of claim 1, wherein the cylinder is a non-transparent cylinder.
4. The thin layer chromatography system of claim 3, wherein the cylinder has a window thereon, the window having a height scale.
5. A method of performing chromatography using the thin layer chromatography system of any one of claims 1-4, comprising:
(1) Spotting by using a thin-layer chromatography plate;
(2) Vertically and fixedly placing the thin layer chromatography plate by using the first clamping groove and the second clamping groove, and covering an upper cover;
(3) Placing a prepared spreading agent into the cylinder body through a spreading agent containing container, so that the spreading agent enters the bottom of the cylinder body through a capillary flow guide pipe of a first spreading agent groove and starts a steam saturation process;
(4) Observing a steam saturation display, and controlling the amount of the expanding agent in the cylinder body through a first control valve and a second control valve;
(5) When the saturation reaches the required value, stopping the adjustment of the unfolded dose; and
(6) And (4) analyzing and detecting the thin layer chromatography plate.
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