Purification process

Details Purification process Purification process

1996-10-18

1998-10-20

Therkorn, Ernest G.

Liquid purification or separation

Processes

Chromatography

210635, B01D 1508

Patent

active

058242252

DESCRIPTION:

BRIEF SUMMARY
The present invention relates to a process for purifying a crude material by liquid chromatography.
The use of liquid chromatography to isolate a desired compound in essentially pure form from a crude material which contains that compound as a constituent part is known in the art. In this known process, the crude material to be separated is charged to the top of a chromatography column containing a finely divided absorbent solid, the so-called stationary phase, and is effectively washed through this column at a controlled rate by means of a flow of solvent, the so-called mobile phase. As the solvent flows through the column, it carries the crude material along with it, but the various components of the crude material are carried along at differing rates owing to the differing degrees of absorption thereof on the column packing. Thus, as the crude material passes through the column it is gradually separated into its component parts, and by careful selection of the packing material and solvent medium the desired compound can be collected off the column in essentially pure form as a solution in the solvent medium.
A particularly efficient form of liquid chromatography is so-called high performance liquid chromatography (HPLC) in which very finely divided solids, e.g. solids having mean particle diameters in the range of from 5 to 10 microns (.mu.m), are used to pack the column and high pressures, e.g. up to 8000 psi, are employed to drive the solvent through the column so as to achieve a realistic solvent flow rate. The first commercial use of HPLC was as an analytical tool in which only very small quantities of complex organic mixtures were separated in the column. However, more recent developments have enabled HPLC to be used for the isolation/purification of development and even production quantities of a desired compound such as a pharmaceutical product.
The present invention is concerned with the provision of new solvents for use in liquid chromatography techniques, particularly high performance liquid chromatography techniques.
According to one aspect of the present invention there is provided a process for purifying a crude material containing one or more desired compounds in impure form, which process comprises the steps of (1) passing the crude material through a chromatography column packed with a particulate absorbent solid using a solvent comprising at least one fluorine containing compound selected from the (hydro)fluorocarbons and the (hydro)fluorocarbon ethers to transport the said crude material through the packed column, and (2) collecting the one or more desired compounds as they emerge from the column as a solution in the solvent.
According to a further aspect of the present invention there is provided a process for isolating one or more desired compounds from a crude material which contains those compounds as a constituent part, which process comprises the steps of (1) passing the crude material through a chromatography column packed with a particulate absorbent solid using a solvent comprising at least one fluorine containing compound selected from the (hydro)fluorocarbons and the (hydro)fluorocarbon ethers to transport the said crude material through the packed column, and (2) collecting the one or more desired compounds as they emerge from the column as a solution in the solvent.
The present invention also provides for the use of a solvent comprising at least one fluorine containing compound selected from the (hydro)fluorocarbons and the (hydro)fluorocarbon ethers in a liquid chromatography process, particularly a high performance liquid chromatography (HPLC) process.
The crude material to be separated is charged to the inlet end of the packed chromatography column and a supply of the solvent or eluant is then fed to the same end of the packed column. The solvent entrains or dissolves the crude material and carries this material along with it through the column, specifically through the absorbent solid material packing the column. Although the solvent may be allowed to pass passively th

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