JPH058519Y2 - - Google Patents

Description

[Detailed Description of the Invention] (Industrial Application Field) The present invention relates to an elution stop device used in column chromatography operations.

(Prior art) Column chromatography is frequently used as a method to isolate a specific substance from a mixture, whether natural or synthetic, or to separate a fraction containing that substance at a higher concentration. It is being done. Generally, in this operation, a column is filled with a stationary phase such as silica gel or synthetic resin, or a carrier that holds the stationary phase, and then water, an organic solvent, or a mobile phase prepared by mixing these is added. , an equilibrium system of a stationary phase and a mobile phase is used. A sample is introduced into this glass column, and elution from the column is controlled to separate target components through the interaction between the mobile phase flowing through the column at an appropriate flow rate and the stationary phase.

However, during operation, if the supply of mobile phase solvent is cut off for some reason and the packing material is exposed to air, the air bubbles that have gotten between the packing materials cannot be easily removed even if the solvent is replenished again. , resulting in deterioration of column separation performance.

The reason for this deterioration in separation performance is
Separation bands of sample components may occur due to the presence of air bubbles that reduce the contact area between the sample components and the stationary phase or mobile phase, or between the stationary phase and the mobile phase, or because the packing state of the column becomes non-uniform. For example, the spread of Bubbles can be removed to some extent by physical means such as stirring the filler, but in this case, the separation bands of sample components are disturbed, resulting in a decrease in separation performance. After all, once air bubbles are mixed in, it is difficult to avoid deterioration in the separation performance of the column, regardless of whether they are removed or not, and the more precise separation is attempted, the greater the effect.

(Problems that the invention aims to solve) The present invention automatically elutes the solvent from the column in response to the occurrence of the mobile phase solvent running out, which is the cause of deterioration of column performance. The purpose of the present invention is to provide a column elution stopper that can stop column elution.

(Means for Solving the Problems) A column elution stop device according to the present invention includes a cylinder part provided with a solvent inlet connected to a solvent reservoir and a solvent outlet connected to a column, and a solvent flow in the cylinder part. A solvent reservoir is connected to the inlet and installed at a higher position than the cylinder, and according to the siphon principle, the solvent supplied from the solvent reservoir moves up and down in the cylinder in a confidential manner according to the inflow pressure. The present invention is characterized by comprising a piston portion that is movably provided and that closes at least one of the solvent inlet and the solvent outlet by descending within the cylinder portion.

(Function) In the present invention, the mobile phase solvent flows down toward the cylinder part 1 from the solvent reservoir 5 installed at a high position basically according to the siphon principle. This downward pressure of the mobile phase solvent also acts as a force to push up the piston part 2, and the piston part 2, which can move up and down, stabilizes at a position where its own weight and the pushing up force are balanced, and then the movement in the solvent reservoir becomes stable. As the amount of phase solvent decreases, the position decreases. Then, when the amount of mobile phase solvent decreases to a predetermined position, such as when the solvent reservoir 5 becomes empty, the piston portion 2 lowers to a position where it closes the solvent inlet 3 or the solvent outlet 4.

In this state, although the supply of the mobile phase solvent to the column 8 is cut off, the elution port 10 is open, but as described above, the solvent inlet or solvent outlet of the cylinder section 1 is Since they are sealed airtight, air will not flow into the cylinder or column, and when the internal pressure in column 8 and the external pressure eventually reach an equilibrium state, elution from column 8 will be completed. Stop at. In other words, since elution is stopped when the mobile phase solvent is sufficiently present in the column, the packing material 7 is not exposed to air.

(Example) Hereinafter, an example of the present invention will be described according to the drawings.

FIG. 2 is a sectional view of the column elution stop device according to the example. In the figure, a piston part 2 made of the same material is attached to a glass cylinder part 1, and the inside of the cylinder part 1 has an inner wall surface,
Airtightness is maintained by rubbing the outer wall surfaces of the piston portion 2 together. The cylinder part 1 is provided with a solvent inlet 3 on its side wall surface, and a solvent outlet 4 on its bottom surface, which is the lower end.

3 and 4 are cross-sectional views of column elution stop devices according to different embodiments, and in FIG. 3, both the solvent inlet 3 and the solvent outlet 4 are connected to the side wall surface of the cylinder part 1. On the other hand, in FIG. 4, both are provided on the bottom surface of the cylinder portion 1. As described above, in the present invention, any structure may be used as long as it can close one or both of the solvent inlet 3 and the solvent outlet 4 when the piston part 2 descends inside the cylinder part. Also in the case of FIG. 4, the mobile phase solvent 6 in the solvent reservoir 5
flows down according to the siphon principle and flows into the cylinder portion 2 from the inlet 3. And solvent reservoir 5
As the mobile phase solvent 6 decreases, the downstream pressure decreases and the piston part 2 descends, eventually blocking the solvent inlet 3 and solvent outlet 4 provided at the bottom of the cylinder part 1 at the same time.

FIG. 1 is an explanatory diagram showing an example of the configuration of column chromatography using the column elution stopper shown in FIG. 2. In the figure, a mobile phase solvent 6 prepared in advance in a solvent reservoir 5 is placed in the cylinder part 1 of the elution stopper.
The solvent is supplied from the inlet 3 via the inlet tip 12 according to the siphon principle. The solvent 6 is further supplied through the solvent outlet 4 to a glass column 8 packed with a stationary phase or a carrier holding the stationary phase. Thus, under normal conditions, the piston portion 2 is positioned above the inlet 3 in balance with the pressure of the solvent 6 supplied from the solvent reservoir 5.

In order to achieve a balance between the two, it is useful to consider the size, shape, and installation height of the solvent reservoir 5, or to adjust the weight of the piston section 2. Well, if there is a concern that the balance will be lost, a stopper 11 to prevent the piston part 2 from falling off as shown in Fig. 3 is provided in order to prevent the piston part 2 from jumping out from the cylinder part 1 due to the pressure of the solvent 6. This is desirable.

In the glass column 8 , the mobile phase solvent 6 is introduced through the supply port 9 . The solvent 6 spreads the adsorption zone downward and is eluted from the elution port 10.

The column chromatography system including the elution stop device of the present invention is used in a configuration in which only the inlet tip 12 of the solvent reservoir 5 and the elution port 10 of the column 8 are open to the outside.

Note that the supply port 9 is desirably located slightly below the liquid level of the mobile phase solvent 6 in the gallium 8 in order to prevent the air inside the column 8 from flowing back into the elution stopper.

Now, in this state, if the supply of mobile phase solvent 6 to the elution stopper is cut off for some reason,
The pressure pushing up the piston part 2 is lost. On the other hand, the elution proceeds to a certain extent, and as the mobile phase solvent 6 in the column 8 gradually decreases, the piston part 2 also descends.

As a result, the outer wall surface of the piston portion 2 closes the inlet port 3. When the piston part 2 is at the lowest point, the outlet port 4 may be closed together with the inlet port 3.

When the piston portion 2 blocks one or both of the inlet 3 and the outlet 4, the supply of the mobile phase solvent 6 to the column 8 is stopped. As a result, the supply port 9 is effectively sealed, so that the internal pressure and external pressure of the column 8 eventually reach an equilibrium state, and elution from the column 8 is stopped. Note that elution from the column continues until the internal pressure and external pressure of column 8 reach an equilibrium state.
In order to prevent the packing material 7 from being exposed to air thereby, it is desirable that the liquid level of the mobile phase solvent 6 in the column 8 be at least 1 cm above the upper end of the packing material 7.

(Effects of the invention) According to the invention, when the mobile phase solvent runs out, elution from the column can be automatically stopped. This can prevent air bubbles from entering the column and prevent the separation performance of the column from deteriorating. The elution stop device according to the present invention has a simple structure, can be easily attached to an existing column chromatography device, and can be improved. Moreover, since it can be left alone during long hours of work, it does not require much manpower, and work efficiency can be improved.

[Brief explanation of the drawing]

FIG. 1 is an explanatory diagram showing a configuration example of column chromatography using a column elution stopper according to the present invention, and FIGS. 2 to 4 are sectional views of column elution stoppers according to various embodiments. 1... Cylinder part, 2... Piston part, 3...
...Solvent inlet, 4...Solvent outlet, 5...Solvent reservoir, 6...Mobile phase solvent, 7...Filling material, 8...Glass column, 9...Solvent supply port, 10...Elution port.

Claims (1)

[Scope of utility model registration request] a cylinder part provided with a solvent inlet connected to the solvent reservoir and a solvent outlet connected to the column; a solvent reservoir connected to the solvent inlet of the cylinder part and installed at a higher position than the cylinder part; and a siphon. According to the principle of A column elution stop device comprising: a piston portion that closes at least one of an outlet and a piston portion.