RP-HPLC and non-aqueous CZE methods were evaluated for qualitative and quantitative analysis of esterified macrocyclic compounds of the DOTA family (DOTA=1,4,7,10-tetraazacyclododecan-1,4,7,10-tetraacetic acid). This group of compounds represents important reaction intermediates in synthesis of magnetic resonance contrast agents. Calibration curves in the concentration range from 1.0 x 10(-5) to 1.0 x 10(-3) mol/L were plotted and the experimental data were critically compared in terms of their repeatability, linearity, LOD and LOQ. The optimized methods were successfully applied to the analysis of a real reaction mixture without any further pretreatment.
- MeSH
- elektroforéza kapilární přístrojové vybavení metody MeSH
- estery analýza chemie MeSH
- heterocyklické sloučeniny monocyklické analýza chemie MeSH
- kontrastní látky chemická syntéza chemie MeSH
- magnetická rezonanční spektroskopie MeSH
- molekulární struktura MeSH
- vysokoúčinná kapalinová chromatografie přístrojové vybavení metody MeSH
- Publikační typ
- časopisecké články MeSH
- práce podpořená grantem MeSH
- srovnávací studie MeSH
Polycarboxylate derivatives of cyclen are potential La (III) ion carriers for application in medicine, e.g. in magnetic resonance imaging (MRI). The compounds are prepared in multistep syntheses and hence the development of efficient separation and analytical methods for the determination of purity of the products and intermediates is desirable. This work was focused on HPLC methods suitable for the purpose. Out of the four modified stationary phases, only the pentafluorophenylpropyl modification, offering mix-mode interactions, was found suitable. The effect of the mobile phase composition was investigated using aqueous methanol, acetonitrile and buffers of different pH. The best results were obtained with a methanolwater mixture (85:15, v/v). UV detection is unsuitable for the purpose because of its low absorption coefficients, even at short wavelengths. A new type of contactless conductivity detector provided a better sensitivity than the UV detector.
