Abstract
Severe peak asymmetry —fronting— was observed for oxycodone during elution at 30°C from a C 18 HPLC column using a mobile phase consisting of 14.9% MeOH, 84.5% 0.05 M KH 2PO 4 (pH 3.0), 0.5% MTBE, and 0.1% TEA. Investigation using deuterium-labeled oxycodone and analysis by LC/MS showed that gem–diol and hemiketal adducts of oxycodone formed as a result of the equilibrium addition of water and methanol to the C-6 ketone on oxycodone. As a result of slow equilibrium kinetics at room temperature in aqueous solution, the gem–diol and methyl hemiketal eluted as an unresolved broad band in front of the oxycodone peak. Decreasing the column temperature to 0°C decreased the rates of interconversion and allowed the resolution and separation of these species from each other and from oxycodone. Increasing the column temperature to 60°C increased the rates of interconversion with the result that the three species eluted as a single, homogenous peak with greatly improved peak symmetry.(Abstract is approximately 157 words)
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