Tímea Iványi

Characterisation of reversed-phase liquid chromatographic columns by chromatographic tests. Evaluation of 36 test parameters: repeatability, reproducibility and correlation.

The European Pharmacopoeia (Ph. Eur.) or other official compendia give only a general description of the stationary phase in the description of a liquid chromatographic method. Therefore the selection of a column giving suitable selectivity presents difficulties. Earlier, a test procedure was proposed that allows measurement of a number of parameters which are reported to be representative for stationary phase characteristics. This paper describes how the test procedure was applied on 69 RP-LC C18 columns. Chromatographic parameters obtained as test results were evaluated, and their repeatability, reproducibility and correlation were examined.

Characterisation of reversed-phase liquid chromatographic columns by chromatographic tests. Rational column classification by a minimal number of column test parameters.

The European Pharmacopoeia (Ph. Eur.) and other official compendia give only a general description of the stationary phase in the description of a liquid chromatographic method. Therefore the selection of a column giving suitable selectivity presents difficulties. Earlier, a test procedure was proposed that allows to measure 36 chromatographic parameters which have been described for characterising stationary phases. This procedure was carried out on 69 reversed-phase liquid chromatography (RP-LC) columns. This paper focuses on the classification of RP-LC stationary phases based on chromatographic parameters. A chemometric study was conducted using 24 parameters that could be measured in a repeatable and reproducible way. Principal component analysis was used to classify the columns and to estimate the minimal number of parameters necessary for a rational classification. It is shown that after reducing the number of parameters from 24 to four or three, similar classifications were obtained. The column classifications were compared to the European Pharmacopoeia stationary phase description and to the column properties obtained from the manufacturers.

Minimal number of chromatographic test parameters for the characterisation of reversed-phase liquid chromatographic stationary phases

This paper focuses on the classification or differentiation of RP-HPLC columns based on measured chromatographic properties. A chemometric study has been conducted on a published data set consisting of 85 RP-HPLC columns and on a data set consisting of 47 self-tested columns. Principal component analysis enables determination of the number of parameters necessary for a rational differentiation. The results show that reducing the number of parameters for such differentiation still allows classification of the columns just as a higher number did. It is shown that three test parameters produce a classification similar to that obtained with five parameters.

Synthesis, Conformation and Equilibrium Study of New Piperazine and Azamacrocyclic Ligands with N-(Tetrahydro-2-oxofuran-3-yl) and N-[(Carboxy)(2-hydroxyethyl)methyl] Pendant Arms

New piperazine (1), homopiperazine (2), 1-tosyl-1,4,7-triazacyclononane (3), 1,4,7-triazacyclononane (4), and 1,4,10,13-tetraoxa-7,16-diazacyclooctadecane (5) derivatives 1a−5a with 2-oxotetrahydrofuran-3-yl pendant arms have been synthesized from the parent cyclic polyamines 1−5 and 2-bromobutyrolactone in acetonitrile. Their conformational properties have been studied by molecular mechanics and NMR spectroscopy, and new sets of Karplus parameters for calculation of the vicinal coupling constants of the butyrolactone moieties have been determined. Compounds 1a−5a were hydrolysed to (carboxy)(2-hydroxyethyl)methyl derivatives 1b−5b by treatment with aqueous sodium hydroxide. The protonation and complexation properties of 4b (HOET-NOTA) were studied by pH potentiometry, photometry, and 1H NMR titrations, and the results were compared with the corresponding values for NOTA. It was found that, although complexation of 4b with smaller metal ions was approximately two orders of magnitude weaker, its stability constants with the lanthanides remained unchanged.