Fully automatic process for the quick, specific, and selective quantitative determination of low concentrated substances in highly heterogeneous substance mixtures, and automatic column-chromatographic process for enrichment, pre-purification and concentration of substances in heterogeneous liquid substance mixtures

摘要

The system on which the method is based is composed of a solvent purification and degassing system of modular structure, a highly effective prepurifying and derivatising system, a subsequent high- resolution chromatography system and a final quantifying detector system. The overall system is synchronised by a process control system which consists of two independent time programs, of which one controls the prepurifying system and the start of the second program, and the second controls the high-resolution chromatography system including the detector devices. The solvent purification and degassing are based on two liquid reservoirs which are connected via different filters and are sealed from the atmosphere. Degassing takes place in the primary reservoir, while the solvents in the secondary reservoirs are in the degassed and purified form. In the prepurifying and/or derivatising system, the substance mixture containing the analyte is charged to a column. Interfering substances are eliminated by "forward elution". The analyte fraction is then transferred, largely selectively, into a mixing section in which the medium of the analyte fraction or the analyte itself is changed in such a way that the analyte is retained on a subsequent column. After a "forward elution" of interfering substances from this column, if necessary, the analyte fraction is eluted backwards and passed to a downstream high-resolution chromatography system. The analyte is quantified by a downstream detector system. In the second method, an analyte is chromatographed out of a highly heterogeneous substance mixture by column chromatography. This is accomplished by charging the substance mixture in "forward flow" to a column and eluting it forwards after elution of interfering substances. By means of a downstream mixing section, it is possible to modify the analyte fraction or the analyte itself, in order to retain the analyte on the second column. After a further elution of interfering substances, the analyte fraction, which was retained in a narrow zone, is eluted from the second column in "backward flow" and fed to a downstream chromatography system or detection system. An electronic circuit greatly reduces the manual effort and leads to high reproducibility. IMAGE