JPH02179473A - Counter current chromatograph - Google Patents

Abstract

PURPOSE:To simplify balance adjustment and to make it possible to change the number of separating stages and separating capacity in response to purposes by a constitution wherein specimen separating pipes are wound around a plurality of rotary shafts which are provided on the concentric circles of the rotary surface of a rotary supporting body at an equal interval. CONSTITUTION:Rotary supporting plates 3A and 3B are linked and rotated with a horizontal shaft 2 as the center. Rotating shafts 4A and 4B which can be rotated on their axes are horizontally supported at symmetrical positions on the concentric circumference of the rotary surface between the plates 3A and 3B. The supporting plates 3A and 3B are revolved with a rotating motor 5. The shafts 4A and 4B are linked to the plates 3A and 3B with a rotating means and rotated at the same speed. Specimen separating pipes 8A and 8B are made to extend from a specimen introducing/ discharging part 10. The pipes are wound around the shafts 4A and 4B through the shaft 2 and the shafts 4A and 4B and fixed. The pipes are guided to the introducing/ discharging part 10 through the shaft 2 and the shafts 4A and 4B again. A flow-path reversing and switching valve 13 which is provided between the discharging part 10 and the passing position of the shaft 2 switches and connects the flow paths of the separating pipes 8A and 8B in parallel and in series.

Description

DETAILED DESCRIPTION OF THE INVENTION (a) Field of Industrial Application This invention relates to a countercurrent chromatograph. More specifically, the present invention relates to a countercurrent chromatograph that can rapidly perform liquid-liquid partition chromatography using centrifugal force.

(b) Prior art Chromatography, which does not use solid fillers and separates samples by utilizing the difference in partition coefficient between two immiscible liquids, is known as liquid-liquid partition chromatography. One of them is the countercurrent distribution method.

In order to efficiently carry out the self-flow distribution method and shorten the separation time as much as possible, a flow-through centrifuge is used to remove the liquid.
A so-called countercurrent chromatograph that constitutes a liquid distribution system is known (Japanese Patent Publication No. 5g-29871, etc.).

An example of the basic structure of such a countercurrent chromatograph is shown in FIG. In the figure, 2 is a horizontal axis for revolution, 3A and 3B are rotating supports that constitute a rotating surface around this horizontal axis 2, and 4
is a rotating shaft rotatably supported between the rotating supports 3A and 313; 5 is a motor for rotating the rotating supports; 6 and 6'
1 and 2 respectively show a guide gear and a planetary gear that rotate the rotating shaft 4 in the same direction and at the same rotational speed in conjunction with the rotation of the rotating support. Further, it is wound around the rotation axis 4 in large numbers via a cylindrical holder 7, and is wound around the holder 6 from the sample introduction part through the center axis 2 and the rotation axis 4, and then again inside the rotation axis 4 and the center axis. P'l extending through 2 to the sample discharge part
' A sample separation tube 8 made by FE is attached.

A counterweight 14 was attached to the rotating surface of the rotating supports 3A and 3B at a position symmetrical to the rotating shaft 4 via another rotating shaft 4' for maintaining balance during rotation. .

In such a conventional countercurrent chromatograph, the motor 5 is driven to cause the wound sample separation tube 8 to revolve around the horizontal axis 2 and rotate around the rotation axis 4 in the same direction, resulting in planetary rotation. A steady state of phase separation is ensured for the two immiscible liquids (for example, water-butanol) that are filled and introduced into the separation tube 8. Therefore,
By introducing the sample, chromatographic separation is performed primarily within the long, wound sample separation tube 8 by countercurrent distribution. Since the rotation of the horizontal axis and the rotation axis are performed in synchronization, there is no twisting due to the rotation of the separation tube 8, and the planetary rotation interlocking of the wound sample separation tube can be performed without using a rotary seal. can be done.

(c) Problems to be Solved by the Invention However, in the conventional countercurrent chromatograph described above, it is necessary to arrange a counterweight as described above at a target position of the wound sample separation tube. Since this counterweight is used to ensure balance during planetary rotation, it is necessary to change the weight accordingly when the specific gravity or volume ratio of the two-phase liquid system in the opposing sample separation tube changes. However, it has been extremely difficult in practice to change the weight in such a way as to eliminate this change when the balance changes.

Furthermore, in such a countercurrent chromatograph, the number of separation stages and separation procedure are ultimately limited by the size of the cylindrical holder 7, but it is also desirable to further increase the number of stages and capacity depending on the purpose. Ta.

This invention was made under such circumstances.
The object of the present invention is to provide a countercurrent chromatograph in which balance adjustment during planetary rotation can be easily performed, and the number of separation stages and separation capacity can be changed or increased depending on the purpose.

(d) Means for Solving the Problems Thus, according to the present invention, (a) a pair of rotating supports that rotate in conjunction with each other about a horizontal axis to constitute opposing rotating surfaces; (b) the above rotating supports; (c) a plurality of rotational shafts each disposed parallel to the horizontal axis and rotatably supported at a plurality of equally spaced positions on a concentric circumference of the rotational surface of the rotational support; (c) the rotational support; a revolution means for rotating the body; and a rotation means for rotating the rotation axes at the same rotational speed in conjunction with the revolution of the rotation support; a plurality of sample separation tubes each wound around and fixed around the rotation axis via the horizontal axis and the rotation axis, and guided to the sample introduction/discharge section via the rotation axis and the horizontal axis, and (e) each of the above. a parallel-to-series switching means for a flow path, which is interposed between the sample introduction/discharge part and the horizontal axis passing position in the sample separation tube, and is capable of switching and connecting the plurality of sample separation tubes in series. A countercurrent chromatograph is provided.

Flexible and chemically stable tubes are suitable for each sample separation tube in this invention, and tubes made of fluororesin such as P'rFE (polytetrafluoroethylene) are suitable. .

Further, as the series-parallel switching means for the flow paths, various switching means can be applied, such as a combination of three-way valves and a valve switching type. Note that the separation channel may be provided with a channel reversal switching means for reversing the liquid feeding direction.

Further, the number of rotation axes arranged between a pair of rotating supports and serving as winding axes of each sample separation tube may be two or more, and should be arranged at least at equal intervals on the concentric circumference of the rotating surface. All you need is one. However, it is preferable that the number of turns of the sample separation tubes to be wound around each axis of rotation is the same in order to maintain strict balance.

(E) Function According to the countercurrent chromatograph of the present invention, a sample separation tube is wound around each of a plurality of rotation axes provided at equal intervals on the concentric circumference of the rotation surface of the rotation support. Because there are
These are balanced, and the balance of planetary rotation can be ensured without adding a counterweight as in the conventional case.

In addition, since a series-parallel switching means is provided, each of the sample separation tube systems mentioned above can be made into one continuous separation system by this switching, and the number of separation stages can be increased without impairing the balance during rotation. , it becomes possible to increase the separation capacity depending on the purpose.

(f) Example Reference numeral 1 shown in FIG. 1 is a configuration explanatory diagram showing one embodiment of a countercurrent chromatograph of the present invention, and FIG. 2 is a partial perspective view for explaining the basic configuration.

As shown in the figure, the countercurrent chromatograph 1 of the present invention is
A pair of rotational support plates 3A and 3B are provided, which rotate in conjunction with each other around a horizontal axis 2 made of a hollow body, and these rotational support plates 3A,
A pair of rod-shaped rotation shafts 4A and 4B are horizontally supported between the rotary shafts 3B and at symmetrical positions on the concentric circumference of the rotation plane, respectively, so as to be rotatable on their own axis. Then, the rotation motor 5 (0 to 8
00 rpm variable), rotary pulleys 51 and 53, a timing belt 52, and a fixed gear 54 that fixes the rotary pulley 53 and the support plate to constitute a revolution means for rotating (revolving) the rotary support plate around a horizontal axis, Further, the guide gear 6 and the planetary gear 6' held around the horizontal axis constitute an autorotation means for rotating the respective autorotation shafts 4A and 4B. Here, since the gear ratio of 6°/6' is set to tit, it is set so that the rotation axis rotates in the same direction at the same speed as the rotational speed (angular speed) due to revolution.

A cylindrical holder 7 is provided around each rotation axis 4A, 4B.
are fixed, and each cylindrical holder 7 has an inner diameter of 1
Sample separation tube 8A made of 6jIx PTFE tube,
8B is wound in six layers. In the figure, 8I indicates the wound layer of the sample separation tube.

Here, the sample separation tubes 8A and 8B each extend from the sample introduction/discharge section 10, pass through the hollow part of the horizontal shaft 2, and extend from one end to the other end to the ends of the rotation shafts 4A and 4B, respectively. The sample is wound in multiple layers around the cylindrical holder through the hollow part as described above, and is again guided to the sample introduction/discharge section 10 via the rotation shafts 4A, 4B and the horizontal shaft 2 in the reverse order as described above. Each has an independent liquid reciprocating path (total length: 16
0m).

A parallel/series switching means 9 consisting of a six-way switching valve 91 that can switch and connect these sample separation tubes 8A and 8B in series is interposed between the sample introduction/discharge section 10 and the horizontal axis passing position. It becomes. The sample introduction/discharge section IO is composed of a sample injection section 11 and a drain 12, and numeral 13 in the figure is a flow path reversal switching valve for switching the liquid feeding direction of each sample separation tube.

The operation of the countercurrent chromatograph I will be explained below.

First, with the hexagonal switching valve 91 set to the solid line position, a liquid intended as a stationary phase is introduced from the sample introduction/discharge section 10 to fill the sample separation tubes 8A and 8B with the stationary phase liquid.

In this state, the liquid intended as the mobile phase is transferred to the sample separation tube 8A.
8B, and by driving the rotary motor 5, the revolution and rotation axes 4A of the rotary supports '3A, 3B.

Winding F by interlocking the rotation of 4B! 8! are interlocked with planetary rotation at a constant speed. As a result, at first the stationary phase liquid filled inside flows out to the drain 12, but when equilibrium is reached, only the mobile phase liquid flows out and the stationary phase does not flow out, and a stable state remains in each separation tube 8A, 8B. A two-phase system will be maintained. Therefore, by injecting the sample from the injection part 11 in this state, each sample component is separated based on the difference in distribution coefficient through the separation tubes 8A and 8B, and is sequentially discharged from the drain. And these wound layers 81°8I
are arranged in symmetrical positions around the horizontal axis 2, so as long as the same phase system is used, even if the specific gravity of this two-phase system is changed, mutual balance is maintained, and smooth planetary rotation is maintained at a steady state. It can be done in a specific manner.

By injecting another sample into the separation tubes 8A and 8B, it is also possible to separate two types of samples at the same time.

On the other hand, by setting the hexagonal switching valve 91 to the broken line position, the separation tubes 8A and 8B are connected in series, and in this state, by injecting the stationary phase from the sample introduction/discharge section IO through one of the separation tubes 8B, The stationary phase is introduced into the separation tube 8A through the separation tube 8B, and the drain 1 on the separation tube 8B side is
It is discharged from 2. After filling the stationary phase with this introduction, by supplying the mobile phase in the same manner as above,
A two-phase liquid system is set within one separation pipe system in which separation pipes 8B and 8A are connected. Therefore, by injecting the sample from the sample injection part 2 on the separation tube 8B side, it is possible to perform countercurrent distribution, which doubles the number of separation stages and separation capacity, allowing for separation and purification of a larger amount of sample and analysis with high resolution. It becomes possible to do so.

In addition, in the above-described embodiment, the separation tube has two winding layers.
Although the example has been described in which two or more, for example, three or four, are provided, the same effect can be obtained.

(G) Effects of the Invention According to the countercurrent chromatograph of the present invention, smooth planetary rotation of the sample separation tube can be performed in a well-balanced manner without adding a counterweight. Moreover, since it is equipped with a flow path system consisting of multiple wound layers of sample separation tubes, it is possible to perform countercurrent distribution separation analysis and separation and purification of different samples simultaneously, and even for the same sample, it is possible to perform parallel separation and purification. In comparison, a large amount of separation and purification can be performed.

Moreover, the parallel-serial flow path switching means allows these plurality of sample separation tubes to be connected in series depending on the purpose, making it possible to easily separate a larger amount of samples and perform high-precision analysis.

Therefore, the countercurrent chromatograph of this invention can be used in chemistry, pharmacy,
It is extremely useful as a separation/analysis device in various fields such as medicine and biology.

[Brief explanation of the drawing]

FIG. 1 is a configuration explanatory diagram showing one embodiment of a countercurrent chromatograph of the present invention, FIG. 2 is a partial perspective view of the same, and FIG. 3 is a configuration explanatory diagram illustrating a conventional countercurrent chromatograph. . I... Winding layer, 9... Parallel-series switching means, 1... Six-way switching valve, 0... Sample introduction/discharge section, l. ...Sample injection part, 12 ...Drain, 3 ...Flow path reversal switching valve. ! ...Countercurrent chromatograph, 2...Horizontal axis, 3A, 3B...Rotating support plate, 4A, 4B...Rotating axis, 5... ... Rotating motor, 51.53 ... Rotating pulley, 52 ... Timing belt, 54 ... Fixed gear, 6 ... Guide gear, 6'・・・・・・Planet gear, 7・・・・・・
Cylindrical holder, 8A, 8B... Sample separation tube, ■ Fig. ζ Fig.

Claims (1)

[Scope of Claims] 1. (a) a pair of rotating supports that rotate in conjunction with each other about a horizontal axis to form opposing rotating surfaces; (b) each of the rotating supports is arranged parallel to the horizontal axis between the rotating supports; (c) a revolution means for rotating the rotary support; and (c) a revolution means for rotating the rotary support; (d) an autorotating means for rotating the shafts at the same rotational speed in conjunction with the revolution of the rotating support; (d) a rotating means extending from each of the sample introduction/discharging sections and passing through the horizontal axis and the autorotation axis of the rotating support; a plurality of sample separation tubes that are wound and fixed around the rotational axis and guided to the sample introduction/discharge section through the rotational axis and the horizontal axis, and (e) the sample introduction/discharge section in each of the above sample separation tubes. A countercurrent chromatograph comprising: parallel-to-series switching means for flow paths, which is interposed between the sample separation tubes and the horizontal axis passage position, and is capable of switching and connecting the plurality of sample separation tubes in series.