Towards the certification of the purity of calibrant reference materials for thyroid hormones: A chicken and egg dilemma

The certification of the purity of CRMs intended for calibration, where no other certified material already exists for comparison, raises principle questions on how to determine the purity of a “first” calibrant in the calibration hierarchy. We developed and certified two calibration CRMs for their purity in thyroid hormones taking into consideration inorganic residues, residual solvents and organic impurities detectable by HPLC–UV and HPLC–MS. IRMM-468 was certified for a thyroxine (T4) mass fraction of 98.6 ± 0.7% and IRMM-469 was certified for a 3,3′,5-triiodothyronine (T3) mass fraction of 97.1 ± 0.7%. The approach we used aims to determine the purity of these two CRMs to the best of our knowledge and taking all scientific aspects properly into account for the estimation of an uncertainty related to the stated purity.