A method has been developed for the qualitative and quantitative analysis of complex isotopic mixtures of tritium-labelled amino acids and peptides by using high resolution(3)H NMR spectroscopy at 266.8 MHz. Determined were tritium distribution in alanine, glycine, tryptophan and 4-hydroxyproline amino acids, as well as in glycine and valine residues of peptides. Approaches have been worked out for the determination of spin coupling constants and isotope chemical shifts for the strongly coupled nonequivalent atoms of the methylene groups.
SummarySynthesis of tritium labelled BIBN 4096 -1-piperidine--a h-CGRP-antagonist for the treatment of migraine is described. Selective tritiation of a heterocyclic aromatic fragment in the presence of aromatic ring in a precursor of BIBN4096 was successfully carried out using the solid state catalytic exchange method. Subsequent completion of the synthesis sequence gave the final [3 H]BIBN4096 with a specific activity of >170 Ci/mmol.
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