ISOLATION, IDENTIFICATION, AND CHARACTERIZATION OF 17-OXO DEXAMETHASONE, AN OXIDATIVE DEGRADATION IMPURITY OF DEXAMETHASONE USING FLASH CHROMATOGRAPHY AND NMR/HRMS/IR

What is it about?

This paper describes isolation, identification, and characterization of oxidative impurity of dexamethasone (17-oxo dexamethasone) in the drug substance using flash chromatography, high-resolution mass spectrometry (HRMS), 1H nuclear magnetic resonance (NMR), 13C NMR, and infrared (IR).

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Photo by National Cancer Institute on Unsplash

Photo by National Cancer Institute on Unsplash

Why is it important?

Some formulations of dexamethasone available in the market require gamma-radiation sterilized dexamethasone active pharmaceutical ingredient (API). A new impurity was detected in the gamma-radiation sterilized dexamethasone API and determined using gradient ultra performance liquid chromatography (UPLC) method with UV detection. This impurity was identified as the major peroxide degradation impurity of dexamethasone. This impurity standard was consequently isolated via oxidative degradation followed by flash liquid chromatography (LC) method. Using high-resolution mass spectrometry (HRMS), nuclear magnetic resonance (NMR), and infrared (IR) study the impurity was identified as 17-oxo dexamethasone (dexamethasone 17-ketone).