Carbon‐14 (¹⁴C)–labelled active pharmaceutical ingredients (APIs) and investigational medicinal products (IMPs) are required for phase 0/I to phase III mass balance and micro‐dosing clinical trials. In some cases, this may involve the synthesis of ¹⁴C‐labelled peptides, and the analysis can be performed by accelerated mass spectrometry (AMS). The ¹⁴C‐peptide is typically prepared by the solid‐phase peptide synthesis (SPPS) approach using custom‐made glassware for the key coupling steps. Further modification of the purified ¹⁴C‐peptide can then be performed.
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