Liquid purification or separation – Processes – Chromatography
Reexamination Certificate
1999-10-28
2001-03-06
Therkorn, Ernest G. (Department: 1723)
Liquid purification or separation
Processes
Chromatography
C210S198200, C095S082000, C096S101000, C422S070000
Reexamination Certificate
active
06197198
ABSTRACT:
REFERENCE TO RELATED APPLICATIONS
This application is a 371 of PCT/EP98/00535 filed Feb. 2, 1998.
BACKGROUND OF THE INVENTION
The invention relates to a device or equipment as well as to a method for the simultaneous, fractionating operation of several parallel chromatography columns. The equipment and the method can be utilized in a particularly advantageous manner in research, within the context of organic synthesis for simultaneous, parallel separation, isolation, and purification of many chemical compounds, such as new active ingredients for medicaments, and especially on the semi-preparative scale.
Column chromatography is a typical method for separating substance mixtures in organic synthesis, especially in the form of a liquid-solid chromatography. Modern pharmaceutical research, therefore, would be unthinkable without column chromatography as a method for isolating and subsequently identifying synthesized organic substances. Since the identification a new type of active ingredient continues to be a difficult and expensive enterprise which necessitates the synthesis of a large number of chemical compounds, the need for innovations with respect to equipment and method still persists. The role of so-called combinatorial synthesis is becoming increasingly important for both the search for as well as the optimization of guide structures, in order to produce chemical compounds within smaller and smaller periods of time. To the extent that systematic molecular variation by way of combinatorial synthesis results in a plurality of different compounds extremely quickly, other methods applied within the context of searching for active ingredients—for example methods for separating substance mixtures or for isolating and purifying individual substances—must also stay apace with the heightened synthesis capacity. For example, although it still was sufficient for classical synthesis procedures to subject the synthesized compounds to a chromatography individually and, if necessary, sequentially, modern synthesis methods with a higher capacity as well as combinatorial chemistry also require a heightened output capacity during the separation of substance mixtures or during the isolation and purification of synthesized compounds, and especially on a semi-preparative scale.
SUMMARY OF THE INVENTION
The object thus was to provide a simple and efficient device for the simultaneous parallel execution of column chromatographies, especially for the semi-preparative scale.
The object is achieved by means of the device or equipment which are stated in the claims as well as by means of the method for column chromatography described.
Accordingly, the invention particularly concerns a device for the simultaneous parallel execution of a particular number n of column chromatographies, in which the device is characterized by
a) a mounting base, preferably in the form of a base trough
which serves to accommodate one or several removable test tube racks (fraction collectors), wherein these test tube racks are adapted in their measurements, either individually or collectively, to the internal dimensions of the mounting base, preferably the base trough, such that an arrangement of m rows lying at a distance from one another with n test tubes standing at a distance in juxtaposition can be effected,
wherein the mounting base, preferably the base trough, optionally can have an additional solvent drain arranged on one or both of the ends (in “position 0” and/or “end-position”);
b) a slide rail which is arranged parallel to each longitudinal side of the mounting base, preferably a base trough, with a controllable, motor-driven carriage;
c) a movable bridge which is arranged on the carriage—by means of which said bridge can be moved across the mounting base at a distance—, and which serves as a support for the fixed or, optionally, interchangeable accommodation of a plurality of chromatographic columns (“column support bridge”);
d) a number n of chromatographic columns which are arranged in rows on the column support bridge parallel to the end of the mounting base, preferably a base trough, in such a way that the positions of the dropper tips of the line of chromatographic columns to be traversed is aligned with the positions of the test tubes in the individual rows, in the process of which the chromatographic columns can be designed for working under pressure;
e) a solvent container for accommodating an eluting agent or, optionally, several solvent containers for accommodating various eluting agents, in which the solvent container or containers also optionally can be designed as pressure containers and in which the solvent container or containers also can be arranged to be mounted on the column support bridge above the chromatographic columns;
f) fixed or flexible supply tubes for introducing the eluting agent or agents from the solvent container or containers into the chromatography columns;
g) a motor drive for moving the carriage with the column support bridge on the slide rails and an electronic control device for automatic control, in particular of the time interval, the rate of feed, and the position of the column support bridge along the mounting base, preferably along the base trough;
in which the number n refers to the chromatographic columns arranged on the column support bridge and represents a number larger than 5;
and in which the number m refers to the possible test tube rows which can be traversed by the column support bridge.
The particular dimensions of the device or the individual components, as well as the exact arrangement of the components can be embodied in accordance with the needs and desires of the respective user. In this way, the structural design and production of the inventive device can be accomplished without particular difficulty. Aside from the components described above, more components which are tailored to further user requirements or to other requirements (such as safety regulations) can be provided, if desired. For example, the mounting base, designed as a base trough, can be fitted with a suctioning device for suctioning the solvent vapors from the mounting base or trough area and its surroundings. Moreover, if desired, the entire device can also be equipped with a shrouding cover or an object suctioner, to the extent that the dimensioning of the device makes it impossible to work in conventional laboratory hoods. The mounting base itself comprises two parallel longitudinal walls as well as two perpendicular lateral walls (ends, or a top and a bottom), as well as a floor plate connected tightly to the lateral walls to form a base trough. The mounting base or trough is securely connected to the slide rails which are arranged parallel to the longitudinal walls of the mounting base or trough. In this way, the carriage moving inside can be moved precisely to a particular position along the mounting base or trough. The test tube racks (fraction collectors) which can be placed into the mounting base or trough are designed in the usual manner and are suited for accommodating test tubes with various diameters which are commercially available. If desired, the test tube rack can be fitted with a suitable cover which serves as a funnel and as a splash guard. Furthermore, a test tube rack which prevents the transposition of test tubes is advantageous because the subsequent processing of the samples can be facilitated. The chromatographic columns are likewise columns having the desired dimensions which comprise standard commercial sizes, such as glass tubes with a thread which can be sealed at the top by means of threaded caps or in some other suitable manner so as to be pressure-tight. The actuator for moving the carriage on the slide rails and the electronic control device are constructed in a conventional manner or in the manner typical for the market. The electronic control device serves to regulate automatically the time interval, the rate of feed, and the position of the column support bridge above the test tubes as well as to shut down the device automatically after the prede
Gundlach Frank
Messinger Josef
Sinner Ernst
Evenson, McKeown, Edwards & Lenahan P.L.L.C.
Solvay Pharmaceuticals GmbH
Therkorn Ernest G.
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