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Analysis of amino acids and polyamines by HPLC and CZE
Kubíčková, Anna ; Coufal, Pavel (advisor) ; Pacáková, Věra (referee) ; Flieger, Miroslav (referee)
(EN) This work is focused on two specific classes of amines. First group comprises of cyclic polyaminocarboxylates from the DOTA (1,4,7,10-tetraazacyclododecane- 1,4,7,10-tetraacetic acid) family, which are important reaction intermediates in magnetic resonance imaging (MRI) contrast agent synthesis. In the development of new contrast agents, carboxyl groups are very often protected with tert-butyl ester groups. Among these derivatives, tBu3DO3A is of the highest importance. Therefore, reverse-phase high performance liquid chromatographic (RP-HPLC) and non- aqueous capillary zone electrophoretic (CZE) methods were evaluated for qualitative and quantitative analysis of tBu3DO3A (1,4,7,10-tetraazacyclododecan-1,4,7- tris(tert-butylacetate) and two typical reaction by-products, i.e. tBu4DOTA (1,4,7,10- tetraazacyclododecan-1,4,7,10-tetrakis(tert-butylacetate) and tBu2DO2A (1,4,7,10- tetraazacyclododecan-1,4-bis(tert-butylacetate). These optimized methods were successfully applied to monitoring of real reaction mixtures during synthesis of a new MRI contrast agent. No further sample pretreatment was necessary. In the second part of the thesis, proteinogenic amino acids and polyamines were used as model analytes for development of a new post-column solid-phase reactor suitable for on-line derivatization...
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