JPH04303765A - Counter current distribution chromatograph - Google Patents

Abstract

PURPOSE:To use a short coil to make the distribution condition of the whole coil uniform and achieve high separation performance even if the coil is short. CONSTITUTION:A rotor 26 is rotatably supported by a rotor support base 28 and a drum 30 is rotatably mounted at the position separated from its rotation center on the rotor 26. The drum 30 revolutes by the rotation of the rotor 26 and synchronizes with the rotation of the rotor 26 to autorotate. Coils 10a, 10b are double-spirally wound on the rotor 26. Pieces of inlet tubing 22g, 22b and other pieces of outlet tubing 24a, 24b of the coils 10a, 10b are connected to a six-way valve 20, a flow passage of a movement phase 2 supplied by a liquid supply pump 6 is connected to either of the pieces of the inlet tubing 22a, 22b through an injector 8 and a piece of tubing 25 introduced to a fluxion collector and the like is connected to either of the outlet passages 24a, 24b.

Description

[Detailed description of the invention]

0001

[Field of Industrial Application] The present invention relates to a countercurrent distribution chromatography device equipped with a coil for liquid-liquid distribution chromatography filled with a stationary phase and into which a mobile phase is fed from one end. be.

0002

[Prior Art] Countercurrent distribution chromatography devices include a static equilibrium system in which a coil filled with a stationary phase is kept stationary, and a dynamic system in which a coil filled with a stationary phase is rotated around a central axis. There is an equilibrium system. A dynamic equilibrium system is better for increasing distribution efficiency. There are various types of dynamic equilibrium countercurrent distribution chromatography devices, but one that uses a planetary coil centrifuge without a rotating seal is superior in terms of preventing contamination and liquid leakage.

On the other hand, high performance liquid chromatography (HP
LC) employs recycling chromatography in which sample components separated by one column are returned to the same column via a switching valve or guided to another column. However, there is no known countercurrent distribution chromatography device, particularly a countercurrent distribution chromatography device using a planetary coil centrifuge, in which a recycling channel is configured. In countercurrent partition chromatography, increasing the number of theoretical plates and improving separation requires long coils. For this reason, the coil is wound in multiple layers around the drum that rotates the coil.

0004

[Problem to be Solved by the Invention] When a coil is wound in multiple layers around a drum that rotates on its own axis, the ratio β (=r/R) of the coil's orbital radius R to its rotational radius r at the entrance and exit of the coil.
are different, and the distribution of sample components is also different.
There is a limit to the length of the coil that can be wound around the drum. An object of the present invention is to use a short coil in a countercurrent distribution chromatography apparatus to make distribution conditions uniform throughout the coil, and to achieve high separation performance even with a short coil.

[0005]

SUMMARY OF THE INVENTION In the present invention, a recycle channel is provided in a countercurrent distribution chromatography apparatus.

[0006]

DESCRIPTION OF THE PREFERRED EMBODIMENTS FIG. 1 shows an embodiment in which a recycle channel is provided in an apparatus equipped with one coil 10 for countercurrent distribution chromatography. The coil 10 for countercurrent distribution chromatography is wound around a drum, and as the drum rotates, the coil 10 rotates, and is a coil that utilizes a planetary coil centrifuge without a rotating seal. Such coil 10 may be any of the various coils used in dynamic equilibrium systems of countercurrent partition chromatography;
Also included are the various coils shown, for example, in US Pat. No. 4,058,460.

The mobile phase 2 is transferred to the coil 10 by the liquid feeding pump 6.
An injector 8 for injecting the sample is arranged in a flow path from the pump 6 to the coil 10. coil 1
A detector 12 is disposed in the outlet flow path of the coil 10 to detect the sample separated by 0, and the eluate flow path from the detector 12 includes a recycle flow path for guiding the eluate to a flow-out flow path 16 or a recycle flow path. Recycle valve 1 to switch whether to lead to 18
4 are provided. The recycle channel 18 is connected to the mobile phase supply channel 4 that supplies the mobile phase 2.

The operation of the embodiment shown in FIG. 1 will be explained as follows.
When the sample injected from the injector 8 is separated by the coil 10 while the recycle valve 14 is connected to the flow-out channel side, and the target component is detected by the detector 12, the recycle valve 14 is connected to the flow-out channel side. Switching to the recycling flow path 18 side, the target component is returned to the coil 10 via the liquid sending pump 6 again, and separated by the coil 10 again. This increases the apparent number of theoretical plates even if the coil 10 is short.

FIG. 2 shows a second embodiment in which an alternative recycle channel in which two coils 10a and 10b are connected via a six-way valve 20 is applied to a countercurrent distribution chromatography apparatus. When the six-way valve 20 is set as shown in FIG. 2(A), the mobile phase sent by the liquid pump 6 enters one coil 10a, passes through the detector 12a, enters the other coil 10b from the six-way valve 20, A flow path is formed through which the liquid waste passes through the detector 12b.

The operation of the embodiment shown in FIG. 2 will be explained as follows.
Assume that the hexagonal valve 20 is set as shown in (A), the mobile phase is sent by the liquid pump 6, and the sample is injected from the injector 8. Assuming that 9 is the target component, the target component is first separated by the coil 10a and detected by the detector 12a. By monitoring the detector 12a, when it is found that the target component is introduced into the next coil 10b via the detector 12a, the six-way valve 20 is switched to the position (B). As a result, the mobile phase is sent directly to the coil 10b via the six-way valve 20, and the target component 9 is sent to the coil 10b.
b, passes through the detector 12b, and is sent to the coil 10a again. When it is confirmed by monitoring the detector 12b that the target component has been introduced into the coil 10a, the six-way valve 20 is returned to the position (A). By repeating this operation, the number of theoretical plates can be increased.

Comparing the recycle channel in FIG. 1 with the alternative recycle channel in FIG. 2, the embodiment in FIG. 1 requires only one coil, so the configuration is simple, but it is generally used in countercurrent partition chromatography. Liquid feed pump 6
Since the volume of the pump head is large, the sample band becomes wider, and it is thought that the number of theoretical plates does not improve much. On the other hand, in the embodiment shown in FIG. 2, the spread of the sample band is small and the number of theoretical plates is improved. However, since two coils are required, the flow path becomes complicated, especially in a dynamic equilibrium system using a planetary coil centrifuge. Therefore, an apparatus for realizing the alternative recycling method shown in FIG. 2 will be described next. 2
One way to realize a countercurrent distribution chromatography device with two coils is to wind two coils around one drum, and another is to use a separate drum for each coil. It is.

FIGS. 3 to 5 show an embodiment in which two coils are wound on one drum. In FIG. 3, the rotor 26 is rotatably supported by a rotor support base 28,
A drum 30 is rotatably attached to the rotor 26 at a position offset from its center of rotation. 32 is a cylindrical tube through which two pipes pass. The rotor 26 is rotated by a drive device (not shown), and the rotation causes the drum 3 to
0 revolves. The drum 30 also rotates in synchronization with the rotation of the rotor 26. In the figure, the coils form two pipes 22a and 22b from the outside of the left side of the rotor 26, and the coils connect to the rotor 26.
6, is guided from left to right through the cylindrical tube 32, enters the rotation center axis of the drum 30 from the right end of the drum 30, and is wound around the drum 30 as coils 10a and 10b. The leftward extending portions of the coils 10a and 10b are guided from the left end of the drum 30 through the rotational center of the drum 30 to the rotational center of the rotor 26, and are guided from left to right in the rotational axis of the rotor 26 as shown in the figure. The outlet pipes 24a and 24b are taken out from the central axis of the pipe 26. Inlet pipes 22a and 22b and outlet pipes 24a and 24
b is connected to the six-way valve 20, and the flow path of the mobile phase 2 sent by the liquid pump 6 is connected to either the inlet pipe 22a or 22b via the six-way valve via the injector 8, and is led to a fraction collector or the like. Piping 25 is connected to either outlet channel 24a or 24b by a six-way valve 20. Each of the outlet channels 24a and 24b is provided with a detector as shown in FIG. 2, but illustration thereof is omitted.

This countercurrent chromatography apparatus utilizes a planetary coil centrifuge that does not use a rotating seal, and so that the coils 10a and 10b can rotate without intertwining the pipes, pipes 22a, 22b, 24a, and 24b are used. A flexible material such as polytetrafluoroethylene is used.

A specific example of the coils 10a and 10b shown in FIG. 3 is shown in FIG. FIGS. 4A to 4C show the process of winding two coils 10a and 10b around the drum 30. Two hollow tubes of the same thickness are wound around the drum 30 in a double spiral. The two coils 10a and 10b are formed by winding the coils around the coils 10a and 10b. The drum 30 with two coils wound around it is shown in Figure 4 (
As shown in D) and (E), the piping attached to the rotor 26 and connected to the inlet and outlet of the coil is passed through the cylindrical tube 32 installed on the rotor 26. 3 and FIGS. 4(D) and 4(E) are the same, but the left and right sides are reversed.

FIG. 5 shows the behavior of the piping when the rotor 26 of the embodiment shown in FIG. 3 rotates. Piping indicated by a solid line indicates that it passes through the front side of the page, and piping indicated by a broken line indicates that it passes through the back side of the page. (A)
Although it is 1/2 rotation from to (E), the pipes can rotate without getting entangled with each other. While the rotor 26 rotates once, the drum 30 rotates twice in the same direction as the rotor 26.

FIG. 6 shows an embodiment in which two coils constituting the alternative recycle channel are wound on separate drums. Figure 6 (A) is shown in each drum.
The coil is wound as shown. As shown in (B), the helical directions of the two coils 10a and 10b are the same. Since the directions in which the drums 30a and 30b are attached to the rotor 26 are opposite to each other, each coil 10a and 10
The inlet and outlet directions of b are reversed. Drums 30a, 30
(C) and (D) show the state in which b is attached to the rotor 26.

FIG. 7 shows the rotor 2 in the embodiment of FIG.
6 shows the behavior of the piping when it rotates. In this case as well, the pipes do not get entangled with each other, and the rotor 26
While rotating, the drums 30a and 30b each rotate twice in the same direction as the rotor 26.

FIG. 8 shows an embodiment in which two coils are wound in a double spiral as shown in FIG. 4, and the coils are formed over two drums 30-1 and 30-2. In FIG. 8, the two coils 10a and 10b are represented by one straight line.

FIG. 9 shows an example in which each coil is wound on a separate drum as in the embodiment of FIG. 6, and each coil is formed over two drums, for a total of four drums. . Two drums 30- with one coil 10a
1 and 30-2, and the other two drums 30-3 and 30-4 are used in the other coil 10b.

FIG. 10 shows an example topologically equivalent to FIG. 9. In both Figure 9 and Figure 10, one straight line has two lines.
It represents a set of tubes. In the above embodiments, it is possible to wind the coils in multiple layers around the drum as long as there is no problem in separation.

[0021] In each of the embodiments shown in FIGS. 3 to 10 for realizing an alternative recycling flow path,
Since the two coils are attached to one rotor, their rotation speeds match each other. Furthermore, since the tubes at the inlet and outlet of the coil do not intertwine with each other, there is no need for a rotary seal, and there is no need to rotate the switching valve. Also, especially
If two coils are wound around the same drum as in the embodiment of FIG. 3, it is easy to match the number of turns of the two coils.

[0022]

[Effects of the Invention] In the present invention, since a recycling channel is provided in a countercurrent distribution chromatography device, the volume of the coil only needs to be equal to the band of the target sample, and even if the length of the coil is short, high resolution can be achieved. Realized. Since the coil of a countercurrent distribution chromatograph device is a hollow tube, the flow path resistance is lower than that of a high-performance liquid chromatograph column, so it is possible to use detectors and six-way valves with low pressure resistance. can. Furthermore, since the coil can be shortened, it is easy to make the conditions of the entire coil uniform, for example by keeping β constant over the entire coil.

[Brief explanation of the drawing]

FIG. 1 is a flow path diagram schematically showing one embodiment.

FIG. 2 is a schematic flow path diagram showing an example including an alternative recycling flow path, which is another embodiment.

FIG. 3 is a configuration diagram showing an example.

FIG. 4 is a diagram showing a coil portion of the embodiment of FIG.
A) to (C) are front views showing how to wind the coil, (D)
is a perspective view showing the state in which the coil is attached to the rotor, (
E) is its cross-sectional view.

FIG. 5 is a diagram showing the operation of the embodiment of FIG. 3;

6A and 6B are diagrams showing other examples of coils constituting an alternative recycling channel, in which (A) is a front view showing one coil, (B) is a perspective view showing a pair of coils, and (C) is a perspective view showing a pair of coils.
(D) is a perspective view of the device attached to the rotor, and (D) is a cross-sectional view.

FIG. 7 is a diagram showing the operation of the embodiment of FIG. 6;

FIG. 8 is a diagram showing still another embodiment, in which (A) is a schematic side view and (B) is a schematic perspective view.

FIG. 9 is a diagram showing still another embodiment, in which (A) is a schematic side view and (B) is a schematic perspective view.

FIG. 10 is a diagram showing still another embodiment, in which (A) is a schematic side view and (B) is a schematic perspective view.

[Explanation of symbols]

10, 10a, 10b Coil 26 Rotor 28 Rotor support stand 22a, 22b Coil inlet piping 24a, 24
b Coil outlet piping 30, 30a, 30b, 3
0-1 to 30-4 Drum 14 Recycling valve 20 Six-way valve

Claims (1)

[Claims] Claim 1: At least one set of a detector and a coil for liquid-liquid distribution chromatography filled with a stationary phase and fed with a mobile phase from one end, the flow path being switched to the outlet flow path of one set of detectors. A countercurrent distribution chromatography device equipped with a valve and a recycle channel that guides the eluate that has passed through the detector to the same coil or another set of coils.